JWRI Vol.39 No.2 PDF

ISSN 0387-4508
TRANSACTIONS
OF
J W R I
Vol. 39 No. 2
2010
JOINING AND WELDING RESEARCH INSTITUTE
OSAKA UNIVERSITY
JAPAN
Organization and Staff (December 2010)
Director General Dr. NAKATA Kazuhiro
1. Division of Materials Processing System
1) Energy Control of Processing
Professor Dr. TANAKA Manabu
Assistant Professor Dr. TASHIRO Shinichi
2) Energy Transfer Dynamics
Professor Dr. SETSUHARA Yuichi
Assistant Professor Dr. TAKENAKA Kousuke
3) Energy Processing Systems
Professor Dr. NAKATA Kazuhiro
Professor(Supplementary assignment) Dr. TAKAHASHI Yasuo
Assistant Professor Dr. TSUMURA Takuya
Assistant Professor(Supplementary assignment) Dr. MAEDA Masakatsu
Specially Appointed Researcher Dr. ZHANG Di
Specially Appointed Researcher Dr. LIU Hong
Specially Appointed Researcher Dr. LIU Duo
4) Advanced Engineering Science
Guest Professor Dr. NISHIYAMA Hideya
2. Division of Materials Joining Mechanism
1) Welding Mechanism
Associate Professor Dr. SHIBAYANAGI Toshiya
Associate Professor Dr. TAKAHASHI Makoto
Specially Appointed Researcher Dr. AHMED KHODIR Saad
2) Laser Welding and Materials Processing
Professor Dr. KATAYAMA Seiji
Associate Professor Dr. KAWAHITO Yousuke
Specially Appointed Researcher Mr. YOSHIDA Satoru
3) Composite Materials Processing
Professor Dr. KONDOH Katsuyoshi
Visiting Professor Dr. UMEDA Takateru
Assistant Professor Dr. UMEDA Junko
Specially Appointed Researcher Dr. IMAI Hisashi
Specially Appointed Researcher Mr. MURAKI Yoshinori
Specially Appointed Researcher Dr. LI Shufeng
3. Division of Functional Assessment
1) Mathematical Modeling and Computational Analysis
Professor Dr. MURAKAWA Hidekazu
Associate Professor Dr. NAKACHO Keiji
Associate Professor Dr. SERIZAWA Hisashi
Specially Appointed Professor Dr. RASHED Sherif
Specially Appointed Associate Professor Mr. YAMAMOTO Takao
Specially Appointed Researcher Dr. KAWAHARA Atsushi
Specially Appointed Researcher Dr. YAMAZATO Kunihiko
Specially Appointed Researcher Dr. MORISHITA Tashika
2) Dependability and Optimum Design
Professor Dr. KIM You-Chul
Assistant Professor Dr. SAKINO Yoshihiro
Specially Appointed Assistant Professor Dr. HIROHATA Mikihito
3) Materials Diagnosis and Life Assessment
Professor Dr. FUJII Hidetoshi
Specially Appointed Associate Professor Dr. SUN Yufeng
4. Smart Processing Research Center
Director Dr. NAITO Makio
1) Smart Beam Processing
Associate Professor Dr. ABE Nobuyuki
Associate Professor (Lecturer) Dr. TSUKAMOTO Masahiro
2) Smart Coating Processing
Professor Dr. NAITO Makio
Associate Professor Dr. ABE Hiroya
Specially Appointed Associate Professor Dr. OKUMIYA Masataro
Specially Appointed Researcher Dr. KONDO Akira
Specially Appointed Researcher Dr. YAMANAKA Shinya
3) 3D Nano/Micro Structure Control
Associate Professor Dr. KIRIHARA Sousyu
Specially Appointed Researcher Dr. TASAKI Satoko
4) Nano-Sized Particle bonding
Professor Dr. KOMIZO Yuichi
Associate Professor (Lecturer) Dr. TERASAKI Hidenori
Specially Appointed Researcher Dr. ZHANG Xinfang
5) Smart Green Processing
Associate Professor Dr. NISHIKAWA Hiroshi
5. Toyo Tanso “Advanced Carbon Design” Joint Research Chair
Guest Professor Dr. TOJO Tetsuro
Specially Appointed Associate Professor Dr. CHEN Weiwu
Specially Appointed Associate Professor Dr. NAKAMURA Fumishige
Guest Academic Staff Mr. NAKAMURA Masaharu
Guest Researcher Dr. MIYAMOTO Yoshinari
Guest Researcher Dr. MATSUMOTO Taihei
6. Fuji Electric Power Device Smart Joining Joint Research Chair
Guest Professor Dr. UMIDA Hidetoshi
Specially Appointed Professor Dr. TAKEMOTO Tadashi
Associate Professor Dr. NISHIKAWA Hiroshi
Specially Appointed Assistant Professor Mr. SHIMODA Masayoshi
Guest Academic Staff Mr. SHIOKAWA Kunio
Guest Academic Staff Dr. HIDAKA Noboru
Guest Researcher Mr. WATANABE Hirohiko
7. Development Base of Advanced Materials Development and Integration of Novel Structured Metallic and Inorganic Materials
Associate Professor Dr. KOBAYASHI Akira
Specially Appointed Associate Professor Dr. OHARA Satoshi
Specially Appointed Assistant Professor Dr. TERAJIMA Takeshi
Specially Appointed Researcher Dr. TAN Zhenquan
8. Global Collaborative Research Center for Computational Welding Science (CCWS)
Professor Dr. MURAKAWA Hidekazu
Specially Appointed Professor Dr. OKUMOTO Yasuhisa
Guest Professor Dr. TERASAKI Toshio
Associate Professor Dr. NAKACHO Keiji
Associate Professor Dr. SERIZAWA Hisashi
Guest Associate Professor Dr. MA Ninshu
9. Joint Interface Microstructure Characterization Room
Associate Professor Dr. TAKAHASHI Makoto
ISSN 0387-4508
TRANSACTIONS
OF
J W R I
Vol. 39 No. 2
2010
JOINING AND WELDING RESEARCH INSTITUTE
OSAKA UNIVERSITY
JAPAN
Transactions of JWRI, Vol. 39 No. 2, 2010
CONTENTS
Numerical visualization on melting and solidification of micron-sized metallic particles by laser irradiation
TAKASE Kazuyuki, MURAMATSU Toshiharu and SHOBU Takahisa ....................................1
Three-dimensional computational modelling of MIG welding

MURPHY Anthony B ....................................4
Weld pool development and stirring behavior of AlCu4SiMg aluminum alloy during GTA welding hybrid
a longitudinal electromagnetic field
LUO Jian ....................................7
Numerical simulation of molten pool flow for various welding parameters in V-groove GMA pipe welding
CHO Dae-Won, NA Suck-Joo, CHO Min-Hyun and LEE Jong-Sub ....................................9
Three-dimensional simulation of a flow in an arc weld pool by SPH method

SHIGETA Masaya, ITO Masumi, IZAWA Seiichiro and FUKUNISHI Yu .................................. 11
Numerical simulation and vision-based sensing of key-holing process in plasma arc welding
LIU Zuming, WANG Xiaojie and WU Chuan Song ..................................14
A Study on the macro-micro physical properties in pulsed arc plasma

SONG Yonglun, YAN Sibo, XIAO Tianjiao and YANG Xiaohong ..................................17
Evaporation phenomena of magnesium during pulsed-MIG arc welding of aluminum alloy

WANG Jing-Bo, NISHIMURA Hitoshi, KATAYAMA Seiji and MIZUTANI Masami ..................................19
Experimental and numerical study of friction stir welding with double-shaft stir probe
XU Zhongfeng and LU Hao ..................................22
Experimental and numerical studies of material flow during welding by friction stirring
SHIMODA Yoichiro, TSUBAKI Masami, YASUI Toshiaki and FUKUMOTO Masahiro ..................................25
Effects of tool geometry and process conditions on material flow and strength of friction stir spot welded joints
HORIE Shohei, SHINOZAKI Kenjin, YAMAMOTO Motomichi,
KADOI Kota, NAKASHIN Hiroki and NORTH T. H. ..................................28
Study on defect in the intersection of VPPA and FSW

YU Yang, LI Baotian, JIANG Fan and CHEN Shujun ..................................31
Simulations of weld pool dynamics and theis visualization

NA Suck-Joo, CHO Won-Ik and CHO Dae-Won ..................................34
Numerical simulation of laser welding processes with CIP finite volume method
YAMASHITA Susumu, YONEMOTO Yukihiro, YAMADA Tomonori,
KUNUGI Tomoaki and MURAMATSU Toshiharu ..................................37
Modelling of the electron beam welding process applied to aircraft engine components
LAURENT D’Alvise ..................................40
Visualization of fluid flow and heat transfer in resistance spot weld nugget
LI Yongbing, SHEN Qi and CHEN Guanlong ..................................42
Development of welding method for wide gap lap joint of steel sheet using laser welding with hot-wire
YAMAMOTO Motomichi, SHINOZAKI Kenji, KADOI Kota, FUJITA Daigo,
INOUE Takeshi, FUKAHORI Mitsugu and KITAHARA Yoichiro ..................................44
Development of a high-efficiency / high-quality hot-wire laser fillet welding process

KADOI Kota, SHINOZAKI Kenji, YAMAMOTO Motomichi, TAKAYANAGI Daisuke,
NISHIMOTO Akihiro, OWAKI Katsura and INOSE Kotaro ..................................47
Innovation of laser direct joining between metal and plastic

KAWAHITO Yousuke and KATAYAMA Seiji ..................................50
i
High brightness laser cutting of CFRP
JUNG KwangWoon, KATAYAMA Seiji and KAWAHITO Yousuke ..................................53
Characteristics and mechanism on the distortion of friction stir welded aluminum alloy sheet
YAN Dong-yang, WU Ai-ping, SILVANUS Juergen, ZHANG Zeng-lei and SHI Qing-yu ..................................56
The influence of the solid state phase transformation on welding deformation of low alloy high strength steel
YANG Xiao, CHEN Junmei and LU Hao ..................................59
Optimising residual stress measurements through the use of measurement simulation

TRUMAN C. E. and SMITH D. J. ..................................62
Residual stress measurement of large-bore stainless steel pipe with butt-welded joint by inherent strain method
MAEKAWA Akira, NAKACHO Keiji, MA Ninshu and SATO Reiko ..................................65
Residual stress generated by LBW on HT780

KIM You-Chuland and HIROHATA Mikihito ..................................68
Structure optimization of air conditional compressor based on reverse welding deformation model
LI Yongzhi, LU Hao, CHEN Junmei and REN Liping ..................................71
Study on prediction of welding deformation for large-scale structure by T-E-P FEM using 3D shell element
ZHANG Xueyuan, LUO Yu and WANG Yang ..................................73
Fast finite element stress and deformation prediction for large thick-wall welded cylinder with angle-inserting elbow
ZHANG Kerong, ZHANG Jianxun, HUANG Siluo and QIU Yiqiang ..................................76
Thermal elastic plastic analysis for welding problem of large scale models
TANAKA Norihiro, KAWAHARA Atsushi,
SERIZAWA Hisashi and MURAKAWA Hidekazu ..................................79
Comparison on several kinds of T-E-P FEM software for welding

WANG Yang, LUO Yu and ZHANG Xueyuan ..................................82
Finite element simulation of multi-pass welding process with rezoning technique

- Fast prediction for welding deformation and residual stress -
HUANG Hui, ZHAO Yao, YUAN Hua and HU Defang ..................................85
Prediction and measurement of welding distortion of thin shell structure

WANG Jiangchao, MA Ninshu, MURAKAWA Hidekazu, TENG Bugang and YUAN Shijian ..................................88
Investigation on ductility dip cracking susceptibility of filler metal 82 in welding

CHEN Jingqing and LU Hao ..................................91
Prediction of welding deformation for double bottom structure in cargo hold of 50000 DWT multipurpose ship
LI Jing and LUO Yu ..................................94
Microstructure and mechanical properties of overlaying specimens in GMAW hybrid

an additional longitudinal electromagnetic field
LUO Jian ..................................97
Flowing behaviors affected by different parameters and multi-materials in GTA weld pool hybrid
a longitudinal electromagnetic field
LUO Jian ................................100
Concept of inherent strain, inherent stress, inherent deformation and inherent force for prediction of
welding distortion and residual stress
MURAKAWA Hidekazu, DENG Dean and MA Ninshu ................................103
Inherent strain calculation from inverse analysis of measured welding deformation based on python of
ABAQUES CAE
ZHAO Haiyan, NIU Wenchong, WANG Peng,
YU Xingzhe, HE Hongwen and SUGIMURA Tadashi ................................106
ii
Application of inherent deformation and interface element to prediction of welding distortion during
assembly process
DENG Dean, MURAKAWA Hidekazu, MA Ninshu and SERIZAWA Hisashi ................................109
Development of simulation system JWELD for assemble deformation of welded structures

MA Ninshu, CHIMURA Isaku and MURAKAWA Hidekazu ................................ 112
In-situ Observation of martensite transformation and retained austenite in supermartensitic stainless steel
ZHANG Shuoyuan, TERASAKI Hidenori and KOMIZO Yu-ichi ................................ 115
In-situ observation of phase transformation during laser welding processes

YAMADA Tomonori, YONEMOTO Yukihiro, YAMASHITA Susumu,
MURAMATSU Toshiharu and KOMIZO Yu-ichi ................................ 118
Numerical simulation on type IV cracking of ASME P92 steel at high temperature

JING Hongyang, XU Lianyong and ZHAO Lei ................................121
Numerical simulation of austenite retention in triplex stainless steel weld metals

SAIDA Kazuyoshi, ARATA Hayata, OGIWARA Hiroyuki and NISHIMOTO Kazutoshi ................................124
Prediction of hardness in HAZ of low-alloy steel produced by temper bead welding using neural network
YU Lina, NAKABAYASHI Yuma, ITO Shinsuke, KAMEYAMA Masashi,
HIRANO Shinro, CHIGUSA Naoki, SAIDA Kazuyoshi,
MOCHIDUKI Masahito and NISHIMOTO Kazutoshi ................................127
Surface tension of molten iron measured by oscillating droplet method using electromagnetic levitation
- Influence of oxygen adsorption on surface tension -
OZAWA Shumpei, TAKAHASHI Suguru, SUZUKI Shoji,
SUGAWARA Hiroharu, HIBIYA Taketoshi and FUKUYAMA Hiroyuki ................................130
Effect of welding sequences on the microstructure of electron beam welded TA15 titanium alloy and
304 stainless steel joints with copper filller metal
WANG Ting, ZHANG Binggang, CHEN Guoqing and FENG Jicai ................................133
Effect of grain size on solidification cracking susceptibility of type 347 stainless steel during laser welding
SHINOZAKI Kenji, WEN Peng, YAMAMOTO Motomichi,
KADOI Kota, KOHNO Yusuke and KOMORI Takuo ................................136
Image processing analysis of growth of carbide particles promoting SR embrittlement in HAZ of 2 1/4Cr-1Mo steel
KAWAKAMI Hiroshi, TAMAKI Koreaki, SUZUKI Jippei,
TAKAHASI Kanta, IMAE Yousuke and OGUSU Soichiro ................................139
Numerical simulation of impact toughness of welded joints for X80 pipeline steel
ZHANG Jianxun, XIONG Qinren, YANG Zhongna and ZHENG Li ................................141
Numerical analysis of deformation and thermal behavior during ultrasonic Al ribbon bonding
SUZUKI Shinji, OYAMA Yusuke, MAEDA Masakatsu and TAKAHASHI Yasuo ................................143
Visualization of heat and stress flows in thermodynamic crystals fabricated by laser scanning stereolithography
KIRIHARA Soshu, UEHARA Yasunori, TAKINAMI Yohei and TASAKI Satoko ................................145
Visualizations of microwave emissions through pure copper photonic crystals

TAKINAMI Yohei and KIRIHARA Soshu ................................148
Visualizations of terahertz frequency amplifications in water cells introduced into alumina diamond photonic crystals
OHTA Noritoshi, NIKI Toshiki and KIRIHARA Soshu ................................151
Weld process management using data visualization

- Approaches to calculation and display of welding statistical information -
SIMPSON Steve W., HUGHES Peter W. and RADOS Michael ................................154
Nonlinear ultrasound and its applications in quality inspection and damage assessment in metallic materials
JIN-YEON Kim, LAURENCE Jacobs and JIANMIN Qu ................................157
iii
Measurement of fatigue damage parameter by sacrificial test piece and thermography
SAKINO Yoshihiro, SAKAGAMI Takahide and KIM You-Chul ................................159
Role of ambient pressure on splat formation and coating adhesion strength during thermal spraying process
YANG Kun, EBISUNO Yoshinobu, TANAKA Kazuhiro, USAMI Takashi,
FUKUMOTO Masahiro, YASUI Toshiaki and YAMADA Motohiro ................................162
Repair heavy-duty generator rotor shaft by electro spark deposition process

WANG Ruijun, WANG Weiping, Lü Yufen and TIAN Hehong ................................164
Visualization of nugget formation in resistance spot welding of multi-stackup sheets

ZHANG Yansong, SHEN Jie and WANG PC ................................166
Development of wettability evaluation equipment for solder paste using laser displacement method
KOYAMA Shinji, OYA Issei, ISAKA Toshihiro, SHOHJI Ikuo,
NISHIMURO Masashi, HIRAMOTO Kiyoshi and MIYAMOTO Hironaga ................................169
Examination of improvement effect of surface modification of Cu with organic acid on solder paste wettability
using a laser displacement meter
KOYAMA Shinji, AOKI Yukinari and SHOHJI Ikuo ................................172
Effect of welding direction on weld bead formation in high power fiber laser and MAG arc hybrid welding
MURAKAMI Takahiro, SHIN Min-Hyo and NAKATA Kazuhiro ................................175
Numerical analysis on effects of power source characteristics on arc properties in gas tungsten arc
TSUJIMURA Yoshihiro, TASHIRO Shinichi and TANAKA Manabu ................................178
Experimental observation of cleaning action of cathode spots in AC TIG welding of aluminum plates
TASHIRO Shinichi, SAWATO Hiroshi and TANAKA Manabu ................................180
Numerical simulation of heat source properties of pulsed tungsten inert gas arc
ITO Kuniyoshi, TASHIRO Shinichi and TANAKA Manabu ................................182
Numerical analysis of weld pool formation mechanism in TIG welding in consideration of the influence of
emitter material adding to the tungsten cathode
ZENIYA Tasuku . TASHIRO Shinichi, TANAKA Manabu,
YAMAMOTO Eri, YAMAZAKI Kei and SUZUKI Keiichi ................................184
Efficiency comparison between iterative substructure method and commercial software

ZHANG Linjie, ZHANG Jianxun, SERIZAWA Hisashi and MURAKAWA Hidekazu ................................187
Experiment and numerical simulation in temperature distribution and welding distortion in GMA welding
YAMANE Satoshi, YAMAZAKI Takuya, KANETA Tomoaki,
NAKAJIMA Toru and YAMAMOTO Hikaru ................................190
Measurement of dynamical variation in two-dimensional temperature distribution of TIG pulsed-arcs

SAWATO Hiroshi, TASHIRO Shinichi, NAKATA Kazuhiro, TANAKA Manabu,
YAMAMOTO Eri, YAMAZAKI Kei and SUZUKI Keiichi ................................193
Improvement of bead formation in plasma MIG welding process in pure argon atmosphere
KATAYAMA Tsubasa, TASHIRO Shinichi and TANAKA Manabu ................................195
Mechanism of undercut in high speed welding based on moveless TIG welding

LU Zhenyang, HUANG Pengfei, CHEN Shujun and LI Yan ................................197
Numerical analysis the influence of arc shape on metal transfer process

KADOTA Keiji and HIRATA Yoshinori ................................199
In-process monitoring and adaptive control for micro welding of titanium

NAKAMURA Hiroshi, KAWAHITO Yousuke and KATAYAMA Seiji ................................201
Numerical analysis on heat source characteristics of two-electrodes TIG arc

OGINO Yosuke, HIRATA Yoshinori and NOMURA Kazufumi ................................204
iv
Fundamental research on micro discharge process
- Research on discharge of sub-millimeter size process -
MINGON Park, HIRATA Yoshinori and NOMURA Kazufumi ................................207
Influence of magnet configurations on magnetic controlled TIG arc welding

NOMURA Kazufumi, OGINO Yosuke, HAGA Takuya and HIRATA Yoshinori ................................209
Visualization of EM process by FEM

CHUN Yu and HAO Lu ................................ 211
Numerical simulation of fusion zone shape of lotus-type porous metals produced by laser welding
TSUMURA Takuya, NAKAJIMA Hideo and NAKATA Kazuhiro ................................213
Numerical simulation on the coupled arc and pool for GTAW using a unified mathematical model
YONGPING Lei, YAOWU Shi, JIAN Lin,
ZHENYANG Lu, RONGSHI Xiao and H. Murakawa ................................215
Prediction of 475°C embrittlement in stainless steel welds using phase field model
SAIDA Kazuyoshi and NISHIMOTO Kazutoshi ................................218
Metallurgical mechanism of ductility-dip cracking in multipass welds of alloy 690

OKAUCHI Hironori, NOMOTO Yuki, OGIWARA Hiroyuki,
SAIDA Kazuyoshi and NISHIMOTO Kazutoshi ................................221
Interfacial reaction between Sn-3.0Ag-0.5Cu solder / Co-P plating and Ni-Co-P plating
DAITO Tomoya, NISHIKAWA Hiroshi, TAKEMOTO Tadashi and MATSUNAMI Takashi ................................223
Formation of reaction layers at anodically-bonded metallc glass/silicate glass interfaces

TAKAHASHI Makoto, WATATANI Yuuki, IKEUCHI Kenji,
KIMURA Hisamichi and INOUE Akihisa ................................125
The dissymmetry of friction stir welding joints and variable polarity plasma arc welding joints study
CHEN Shujun, WANG Long and YU Yang ................................228
Industrial application of welding temperature field and distortion visualization using FEA
RAPHAEL Thater, WILLIAM Perret, CHRISTOPHER Schwenk,
UWE Alber and MICHAEL Rethmeier ................................231
Prospective design of weld joint between first and side walls in the test blanket module for ITER
NAKAMURA Shinichiro, SERIZAWA Hisashi,
TANIGAWA Hiroyasu and MURAKAWA Hidekazu ................................234
Preliminary numerical research of microstructural fracture behavior in metal by using interface element
TOMIYAMA Seigo, SERIZAWA Hisashi, HAJIMA Tsuyoshi and MURAKAWA Hidekazu ................................237
Thermoreversible colloidal gelation for direct-assembly of nanoparticles

KONDO Akira, ANDATSU Masahiro, ABE Hiroya and NAITO Makio ................................240
Dispersion control of magnetic nanoparticles for functional fluids

YAMANAKA Shinya, ABE Hiroya, NAITO Makio, UESHIMA Yuya and NOMA Junichi ................................243
Molecular dynamics analysis of fcc nanowire under torsional loading

OGAWA Takaki and NAKATANI Akihiro ................................245
Visualization of mechanical properties in alumina dental crowns fabricated by using laser scanning stereolithography
TASAKI Satoko, KIRIHARA Soshu and SOHMURA Taiji ................................248
Combinatorial analysis of plasma-polymer interactions for formation of inorganic-soft materials hybrid structure
TAKENAKA Kosuke, CHO Ken, SETSUHARA Yuichi,
SHIRATANI Masaharu, SEKINE Makoto and HORI Masaru ................................250
Observation of hole formation process in plasma arc drilling

KUSUMOTO Kazuomi, HAO Son and ISHIKAWA Satoshi ................................253
Simulations and visualizations of grid erosion in ion engines
v
- Prediction of ion engine lifetime -
NAKANO Masakatsu ................................256
Materials joining technologies and interface science for integration of novel structured metallic
and inorganic materials
SETSUHARA Yuichi and NAKATA Kazuhiro ................................259
Cooperative researches in Tohoku University

FUKUHARA Mikio ................................262
Approach for the project on advanced materials development and integration of novel structured metallic
and inorganic materials by materials and structures laboratory of Tokyo Institute of Technology
OKADA Kiyoshi ................................264
Synthesis and properties of hybrid-type polymer membranes for fuel cells

YOGO Toshinobu ................................266
Evolution of laser welding to dissimilar materials joining

KATAYAMA Seiji and KAWAHITO Yousuke ................................268
Introduction to vector materials science and bioengineering

YAMASHITA Kimihiro ................................270
Preparation of metal nano particles using electrochemical deposition

- Pt nano patterned electrodes -
SAITO Mikiko, MIZUNO Jun and HOMMA Takayuki ................................273
Fabrication and thermoelectric properties of eco-friendly silicides for thermoelectric power generation
using waste heat
ITOH Takashi ................................276
Fabrication of zirconium oxide solid electrolytes with ordered porous structures by using micro stereolithography
KIRIHARA Soshu and TASAKI Satoko ................................279
Application to catalyst of mayenite consisting of ubiquitous elements

SUZUKI Kenzi ................................281
Arrangement of Pd nanoparticles on SDS-functionalized single-walled carbon nanotubes

TAN Zhenquan, ABE Hiroya, NAITO Makio and OHARA Satoshi ................................284
Nano-carbon structures on silicon carbide

NORIMATSU Wataru and KUSUNOKI Michiko ................................287
Room-temperature Coulomb oscillation of Ni-Nb-Zr-H glassy alloys with nanoscale size clusters
M. Fukuhara, H.Yoshida and A.Inoue ................................289
Superconductivity of Ni0.324Nb0.216Zr0.36H0.1 glassy alloys

YOSHIDA Hajime, FUKUHARA Mikio and INOUE Akihisa ................................291
Enhancement of solderability of Cu60Zr30Ti10 bulk metallic glass by dealloying in hydrofluoric acid solution
NAOI Takehiro, NISHIKAWA Hiroshi, TAKEMOTO Tadashi,
ABE Hiroya, FUKUHRA Mikio and INOUE Akihisa ................................293
Local structures of amorphous (Ni0.6Nb0.4)100-xZrx(x=30, 35, 40) alloys by XAFS

MATSUURA Makoto, KONNO Kazuya, FUKUHARA Mikio,
FUJIMA Nobuhisa and INOUE Akihisa ................................296
Effects of photon irradiation in UV and VUV regions during plasma processing of organic materials
CHO Ken, TAKENAKA Kosuke, SETSUHARA Yuichi,
SHIRATANI Masaharu, SEKINE Makoto and HORI Masaru ................................298
Single layer PDMS flexible parallel wall microvalvets

D. H. Yoon, D. Wakui, T. Sekiguchi and S. Shoji ................................301
vi
Development of a novel integrated iontophoresis electrode consisting of metallic and drug-loaded layers
T. Yoshioka, N. Saito, T. Ikoma, N. Ohashi, H. Haida,
S. Ando, R. Wakita, H. Fukayama, M. Umino and J. Tanaka ................................304
Responses of osteoblast to surface modified bulk metallic glass

NAGAI Akiko, YAMASHITA Kimihiro, MURAYAMA Sayaka, MATSUSHITA Nobuhiro,
OKADA Kiyoshi, ABE Nobuyuki, TSUKAMOTO Masahiro, SON Kunsu,
WANG Xinmin, XIE Guoqiang and INOUE Akihisa ................................306
Joining of ceramic nanocrystals and bio-molecules towards bio-medical applications

OHARA Satoshi, SATO Kazuyoshi, TAN Zhenquan and UMETSU Mitsuo ................................308
Cu-based metallic glass surfacemodified with Cu for soldering

- Productions and applications of Cu clad metallic glass -
TERAJIMA Takeshi, KIMURA Hisamichi and INOUE Akihisa ................................310
Shock-assisted joining between metallic glass and ceramics

ATOU Toshiyuki, MUKOGAWA Shintaro, KIMURA Hisamichi,
ITO Shun and KIKUCHI Masae ................................312
Development of plasma MIG brazing process of advanced materials

TASHIRO Shinichi, KATAYAMA Tsubasa and TANAKA Manabu ................................314
Developments of hybrid in-situ observation system to study the microstructural change of metallic alloys
TERASAKI Hidenori and KOMIZO Yu-ichi ................................316
Measurement of fracture behavior of Zr-based metallic glass by thermography

SAKINO Yoshihiro, IZUMI Yui, KURODA Toshio,
SAKAGAMI Takahide and KIM You-Chul ................................319
Development of amorphous boron carbon oxynitride film for transmission electron microscope with
environmental-cell system
MATSUTANI Takaomi, TSUTSUI Hidenori and KAWAKAKI Tadahiro ................................322
Properties of metallic glass coatings sprayed by gas tunnel type plasma spraying
KOBAYASHI Akira, KURODA Toshio, KIMURA Hisamichi and INOUE Akihisa ................................325
Inter-granular cracking of a splat of zirconia coating fabricated by plasma spraying technique

FUJIMOTO Koji, REFAT El-Sheikhy and KOBAYASHI Akira ................................328
Tungsten coatings on reduced-activation ferritic/martensitic steel by plasma spray technique

- Thermal behavior of Tungsten coatings -
TOKUNAGA Kazutoshi, KOBAYASHI Akira, ARAKI Kuniaki, FUJIWARA Tadashi,
MIYAMOTO Yoshio, NAKAMURA Kazuo, KURUMADA Akira, TOKITANI Masayuki,
MASUZAKI Suguru, EZATO Koichiro, SUZUKI Satoshi,
ENOEDA Mikio and AKIBA Masato ................................331
Behavior of arc plasma for thermal barrier coating preparation

- Plasma plume length determined from light intensity -
KOIKE Kazuo, ONO Norifumi and KOBAYASHI Akira ................................333
Titanium oxide film deposition by vortex air thermal plasma assisted spray pyrolysis deposition
ANDO Yasutaka and KOBAYASHI Akira ................................335
Investigations on frequency shift probes for monitoring of electron conditions in nano-materials processing plasmas
NAKAMURA Keiji and SUGAI Hideo ................................338
Dissimilar laser brazing of single crystal diamond and tungsten carbide

SECHI Yoshihisa and NAKATA Kazuhiro ................................340
Joining mechanism between aluminum and polypropylene resin using insert materials by laser irradiation
HINO Makoto, MITOOKA Yutaka and KATAYAMA Saiji ................................343
vii
Modeling of temperature distribution with metal vapour in pulsed TIG including influence of radiative absorption
IWAO Toru, MORI Yusuke, SAKAI Tadashi, TAKI Hiroyuki,
SHIMOKURA Takuya, TASHIRO Shinichi, TANAKA Manabu and YUMOTO Motoshige ................................346
Control of wire melting behavior using coaxial hybrid solid wire

- Development of pure Ar–MIG welding -
NAKAMURA Terumi, HIRAOKA Kazuo and TANAKA Manabu ................................349
Newly developed novel transparent conductor of Mg(OH)2-C compounds

KUJI Toshiro ................................352
Phase transformation at interface using femtosecond laser irradiation

KANEHIRA Shingo, NISHIMURA Masakazu, MIURA Kiyotaka and HIRAO Kazuyuki ................................354
Laser Micro-machinability of electric field-assisted ion-exchanged glass

MATSUSAKA Souta, TSUKAMOTO Masahiro, ABE Nobuyuki and WATANABE Takehiro ................................357
Dynamic mechanical behavior of Sn-Ag-Cu lead-free solders by tensile test under high strain rate
YASUDA Kiyokazu, SAKINO Yoshihiro, SHOJI Ikuo and TAKEMOTO Tadashi ................................360
Oxide nanosheets and their assemblies for new ceramic joining and smart processing
OSADA Minoru and SASAKI Takayoshi ................................362
Evaluation of magnetite and related iron compounds in the teeth of chiton using X-ray and electron analyses
NUMAKO Chiya, SATO Kazuyoshi, ABE Hiroya and OHARA Satoshi ................................364
Characterication and control of nanoparticle dispersion behavior for smart processing in liquid phase
KAMIYA Hidehiro, IIJIMA Motoyuki, TAKENOUCHI Shun,
IINUMA Chihiro and NAITO Makio ................................366
Developments of real-time monitoring method of welding

MATSUBARA Toshio, TERASAKI Hidenori, OTSUKA Hiroyuki and KOMIZO Yu-ichi ................................369
Image measurement of welding distortion of pipe joint in two-phase flow separator

ITOH Shinsuke, SHIBAHARA Masakazu and MOCHIZUKI Masahito ................................372
Microstructure of Cr3Si coatings on austenitic stainless steel by spark plasma sintering

NISHIMOTO Akio, MIYATA Atsuhiro and AKAMATSU Katsuya ................................375
Modification of thermally sprayed cemented carbide layer by friction stir processing

MORISADA Yoshiaki, FUJII Hidetoshi, MIZUNO Tadashi, ABE Genryu,
NAGAOKA Toru and FUKUSUMI Masao ................................378
Ultimate strength of aluminum alloy plates in compression considering joining locations

OKURA Ichiro ................................381
Development of analytical method for welding mechanics using idealized explicit FEM
SHIBAHARA Masakazu and IKUSHIMA Kazuki ................................384
CONTRIBUTIONS TO OTHER ORGANIZATIONS ..............................................................................................387
viii
Transactions of JWRI, Vol.39 (2010), No. 2
Numerical visualization on melting and solidification of micron-

†
sized metallic particles by laser irradiation
TAKASE Kazuyuki*, MURAMATSU Toshiharu**, SHOBU Takahisa***
KEY WORDS: (Numerical simulation) (Laser welding) (Thermal-hydraulics) (Phase change) (Metallic
particles) (Melting) (Solidification) (temperature) (liquid metal) (repair technology)
1. Introduction ª wD
P «
g

w D gU g , j º» qgw qgint * hgsat (5)
Aiming at the enhancement of safety of currently
operated nuclear reactors, development of a repair « wt wx j »
¬ ¼
technology using laser welding [1] has been performed. An
experimental study on welding of micron-sized metallic
particles on a stainless steel plate by laser irradiation has w
w D l Ul elU l , j
already been carried out. Moreover, an analytical study was
D l Ul el
wt wx j
also begun to predict numerically the experimental results.
The micron-sized metallic particle that is made of iron is
P « l

ª wD w D lU l , j º» q w qint * hsat (6)
heated by the laser irradiation and then melts and finally the l l l
« wt wx j »
solid metallic particle changes perfectly to the liquid metal. ¬ ¼
After a long time, the liquid metal solidified the solid metal
with decreasing the temperature. This paper describes 3. Analytical conditions
visualized numerical simulation results of the melting and
Figure 1 shows the analytical geometry, which represents
solidification behavior of the micron-sized metallic particles
the experimental condition. 12x12 metallic particles are set
that change from the solid to liquid and the liquid to solid.
into a slit on a metallic plate. Each of them is made of iron.
The outer diameter of the metallic particle is 0.04 mm. The
2. Governing equations
size of the slit is 0.48 mm square and 0.05 mm in depth. It
Governing equations consist of gas and liquid phases as briefly simulates any cracks on vessels or components of
follows: nuclear reactors. A laser beam is irradiated from the upper
-Mass conservation; side into the slit. The shape of the laser beam is round as can
w w be seen using red in Fig. 1, and the diameter is 0.48 mm.
wt

D g Ug
wx j

D g U gU g , j *
(1)
w w
wt
D l U l
wx j

D l UlU l , j * (2) I 0.48 mm
Heat flux Metallic particle
-Momentum conservation;
wU g ,i wU g ,i int
1 wP M g ,i
Ug,j 0.05 mm
wt wx j U g wxi D g U g Metallic 5 mm
* wW g ,ij 0.48 mm plate

D g Ug
U g ,i U l ,i D 1
gi (3)
g Ug wx j
Fig. 1 Analytical geometry.
wU l ,i wU l ,i 1 wP M l ,i
int
Ul , j
wt wx j Ul wxi D l Ul Figure 2 shows the phase change model from the solid to
liquid phase and conversely the liquid to solid phase. The
* wW l ,ij

D l Ul
U g ,i U l ,i D 1U wx j
gi (4) phase change behavior of the metallic particles with the laser
irradiation is obtained from the liquid fraction, L f , which is
l l
-Internal energy conservation; specified as the following equation:
† Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding

* Japan Atomic Energy Agency, Tokai,㻌 Ibaraki, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Japan Atomic Energy Agency, Tsuruga,㻌 Fukui, Japan Japan
*** Japan Atomic Energy Agency, Harima,㻌 Hyogo, Japan
1
Numerical visualization on melting and solidification of micron-sized metallic particles by laser irradiation
T TS Temperature (K)
Lf (7) 㻌㻌㻌㻌㻌 500 2200
TL TS
Here, T represents the temperature of the metallic particle, T S
solidification temperature, and T L melting temperature. The
following three states related to T and L f are considered:
i) Solid state (at L f =0); when T<T S ;
ii) Liquid state (at L f =1); when T>T S ; and,
iii) Phase change state; T S <T<T L .
Therefore, change of enthalpy in the material from the
solid to liquid by phase change is calculated from
T
h h0 ³ c p dT H L L f (8) (a) After 0.1 ms
T0
Assumptions and conditions for the numerical analysis are

as follows;
1) Constant heat flux given to the metal powders is 815
MW/m2㻌 and㻌 the heating time of the laser is 0.5 ms;
2) An ambient fluid around the metallic particles and plate is
atmosphere;
3) Only metallic particles melt;
4) T S =1809.9 K and T L =1810 K are defined; and,
5) Two-phase flow simulation with the VOF method is used. (b) After 0.3 ms
䠍
Liquid fraction Lf

Lf
Liquid

㻜

(c) After 0.4 ms
Solid
TS T TL
Temperature T
Fig. 2 Phase change model between solid and liquid phase.
4. Results and discussion

Figure 3 shows predicted temperature distributions. The
melting and solidification processes of the metallic particles (d) After 1 ms
due to the laser irradiation can be visualized numerically.
Here, (a) is a result after 0.1 ms from the start of the Fig. 3 Predicted temperature distributionsat different
calculation, and similarly, (b) is after 0.3 ms, (c) is 0.4 ms, time duration from the start of the calculation.
and (d) is after 1 ms. The laser irradiation is completed at 0.5
ms. In Fig. 3, the blue means 500 K and the red means over 5. Conclusions
2200 K. First, the temperature of the metallic particle goes A computational study on melting and solidification of
up in the heating region where the laser beam is irradiated as micron-sized metallic particles was performed to clarify the
can be seen in Fig. 3(a). Next, the temperature of the metallic possibility of the laser welding simulation. From the
particle rises to the melting temperature (Fig. 3(b)) and the visualized results of the present study, we concluded that the
melting occurs as soon as it exceeds the meting temperature welding simulation is possible and the present numerical
(Fig. 3(c)). With increasing the calculation time, almost all approach will be effective.
the metallic particles in the laser irradiation region melt and
become liquid metal. Moreover, the metallic particles in a 6. Nomenclature
region where the laser is not irradiated are heated by thermal
e : Internal energy [J/kg]
conduction, and melt. The laser irradiation is stopped after
g : Gravity [m/s2]
0.5 ms. According to that, the heat moves from the high
hsat : Saturated enthalpy [J/kg]
temperature region to the low temperature region due to the
Mint : Interfacial stress [kg/m2/s2]
thermal conduction. As a result of this, the liquid metal
P: Pressure [Pa]
region can be expanded. Then, by the thermal conduction to
qint : Interfacial heat flux [W/m3]
the metallic plate and the convection into the atmosphere, the
qw : Wall heat flux [W/m3]
temperature of the liquid metal decreases with time and the
t : Time [s]
solidification takes place (Fig. 3(d)).
U : Velocity [m/s]
2
D : Volume ratio
* ,* +,*-: Gas generation rate [kg/m3/s]
Qt : Eddy viscosity [m2/s]
U : Density [kg/m3]
W : Shear stress tensor [kg/m/s2]
Subscripts
g : Gas
l : Liquid
i, j: Spatial coordinate component
References
[1] S. K. Maiti, et al.: Science&Technology of Welding and
Joining, 8 (2003), pp.377-384.
3
†
Three-dimensional computational modelling of MIG welding
MURPHY Anthony㻌㻌 B*
KEY WORDS: (Computional modelling) (MIG welding) (Gas–metal arc welding) (Arc welding)
(Weldpool) (Droplets) (Arc Plasma) (Weld reinforcement)
1. Introduction three phenomena included in the model. Calculations were

There are several difficulties involved in modelling of performed for parameters typical of one-drop-per-pulse
MIG (metal–inert-gas) welding. The motion of the wire and welding of aluminium, which are given in Table 1.
arc relative to the workpiece has to be taken into account. Figure 1 shows the temperature distribution in a cross-
The geometry is three-dimensional, due to the motion of the section through the electrode, arc and workpiece. The
arc. The flow in the molten weld pool, and in particular the presence of a reinforcement of the weld pool due to
deformation of the surface of the weld pool, require careful droplets is clearly apparent. The arc tends to attach to the
treatment. The transfer of droplets from the wire electrode raised region, and thus this region is the hottest in the weld
to the weld pool also has to be considered. pool.
Computational models of arc welding of varying
degrees of sophistication have been developed, but no Table 1 Parameters used for the calculations
comprehensive treatment of MIG welding that addresses all Parameter Value
the difficulties listed above has yet been developed. In this Arc current 95 A
Wire electrode radius 0.6 mm
paper, I outline progress towards developing such a model
Welding velocity 15 mm s-1 in negative y
and present representative results. I discuss in particular the direction
influence of weld pool surface deformation and of droplets Wire electrode feed rate 72 mm s-1
on the weld depth. Droplet frequency 93 Hz
Workpiece thickness 3 mm (on a 50 mm base)
2. Methods Workpiece and wire Aluminium alloy AA5754,
composition melting temperature 875 K
The equations of conservation of mass, momentum,
energy and charge, together with Maxwell’s equations, are
solved in three-dimensional Cartesian geometry using a
finite volume method. Motion of the wire anode and arc
relative to the workpiece is taken into account using the
method described in [1]. An equilibrium surface method [2]
is used to treat the deformation of the surface of the weld
pool due to the arc and droplet pressure and the addition of
mass through droplet transfer. The mass and momentum
transferred to the weld pool by droplets is calculated on a
time-averaged basis. The temperature and velocity of the
droplets are tracked from the initial detachment to the
bottom of the weld pool [3].
Results are presented for steady-state calculations with
an initially flat workpiece (i.e., bead-on-plate welding),
argon shielding gas and aluminium alloy electrodes. The
thermodynamic and transport properties of argon were
taken from [4].
3. Influence of Molten Weld Pool and Droplets

To determine the shape of the weld pool, it is essential
to take into account flow in the weld pool, deformation of Fig. 1 Temperature distribution in the cross section at
the weld pool surface, and the influence of droplets. The x = 0. The welding velocity is to the left.
results presented in this section have been obtained with all

* CSIRO Materials Science & Engineering, Sydney, Australia Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
4
Three-dimensional computational modelling of MIG welding†
Figure 2 shows a more detailed view of the weld pool

region of Fig. 1, including the flow vectors in the weld pool.
The direction of flow is determined by many factors,
including the Marangoni effect (the change in surface
tension with temperature), the magnetic pinch force and
buoyancy [5]. In this case, the influence of droplet
momentum is dominant, driving flow downwards and
leading to a relatively deep weld pool. This can be seen by
comparing Fig. 2 with Fig. 3, which shows the time-
averaged momentum transferred to the arc and weld pool
by the droplets. Momentum is transferred to the droplet by
the arc (due to the drag forces applied by the rapid plasma
flow), but on reaching the weld pool, the droplet is rapidly
slowed, thereby applying downward momentum to the
molten metal.
Fig. 3 Axial momentum source term applied to the arc

and weld pool to take into account the effect of droplets,
in the cross section at x = 0. The top of the weld pool is at
z = 29.3 mm. The welding velocity is to the left.
Fig. 2 Temperature distribution and velocity vectors in

the weld pool in the cross section at x = 0. The welding
velocity is to the left. The white arrow shows the scale of
the velocity vectors.
4. Comparison with Experiment Fig. 4 Comparison of measured and calculated weld

profiles. The welding direction is into the page.
The calculated weld profile is compared with a
measured profile in Fig. 4. The width of the weld and the
height and shape of the reinforcement predicted by the 5. Conclusions
model are in good agreement with measurements, but the A three-dimensional computational model of MIG
predicted depth of the weld is significantly larger. This is at welding that takes into account all important effects, except
least partly due to fact that the presence of metal vapour is for the influence of metal vapour, has been developed. The
neglected in the calculation. Metal vapour will cool the arc model treats the wire electrode, arc and workpiece self-
by increasing the radiative emission [6]. Further, consistently, and allows the shape of the weld pool,
vaporization of the molten section of the wire and of the including the surface deformation, to be predicted.
droplet will cool the droplet and reduce its volume, thereby The importance of including the arc plasma in the
decreasing the energy and momentum transferred by the computational domain (rather than just the workpiece, with
droplet to the weld pool. Both these changes will lead to a the influence of the arc included through boundary
shallower weld pool. conditions) should be emphasized. The influence of weld
pool surface deformation on the location and size of the
attachment region of the arc, and the momentum of the
droplets and its effect on the weld pool, to give just two
5
examples, can only be treated reliably by including the arc References

in the model. [1] K. Mundra, T. DebRoy and K. M.. Kelkar: Numer. Heat
Transfer, 29 (1996), pp.115-129.
Acknowledgements
[2] J.-W. Kim and S.-J. Na: Weld J., 74 (1995), pp. 141s-152s.
The support provided for the work reported here by
General Motors Holden, and the Commonwealth of [3] C. T. Crowe, M. P. Shama and D. E. Stock: J. Fluid Eng., 99
(1977), pp. 325-332.
Australia, through the Cooperative Research Centre for
Advanced Automotive Technology, is gratefully [4] A. B. Murphy and C. J. Arundell: Plasma Chem. Plasma
acknowledged, as are useful discussions with Dr John Process., 14 (1994), pp. 451-490.
Lowke of CSIRO, Dr Hui-Ping Wang of General Motors [5] M. Tanaka and J. J. Lowke: J. Phys. D: Appl. Phys., 40 (2007),
and Drs Bartosz Protasz and Oleg Volkov of McMaster pp. R21-R23.
University. I thank Associate Professor Fenggui Lu of
[6] A. B. Murphy: J. Phys. D: Appl. Phys. 43 (2010), 434001.
Shanghai Jiao Tong University for providing the measured
weld cross-section.
6
Weld pool development and stirring behavior of AlCu4SiMg

aluminum alloy during GTA welding hybrid a longitudinal
†
electromagnetic field
LUO Jian*
KEY WORDS: (Welding pool) (GTAW) (Magnetic field) (Aluminum alloy) (Development) (Stirring motion)
1. Introduction
(a) (b)
In GTA Welding with a longitudinal electromagnetic
field (LMF-GTAW), the formation, microstructure and
mechanical properties of aluminum alloy are studied. t=0.02s t=0.04s
However, there is still a lack of practical or numerical
detailed understanding of the formation of the welding pool
during LMF-GTAW. For example, the effect of the
longitudinal electromagnetic field on the formation of the
weld pool is not clear yet. The additional electromagnetic
force can not only affect the behavior of welding arc, but
also change the force balance state and heat transfer of metal
molten body of the weld pool. (c) (d)
In this paper, we focus on the need for understanding the
weld pool’s formation is AlCu4SiMg aluminum alloy during
LMF-GTAW by a new mathematic model and finite element t=0.05s t=0.06s
method (FEM).
2. A New Quasi-3D Transient Model

The welding arc and weld pool are described relative to a
cylindrical coordinate, assuming rotational symmetry around
the arc axis owing to the fixed arc in GTAW. The flow is
assumed to be laminar, and a quasi-three-dimensional
transient model is built up. The detailed governing equations, (e) (f)
additional electromagnetical driving body force expression,
boundary conditions and numerical method are given in our
previous paper [1]. The governing equations are solved t=0.08s t=0.1s
(g) (h)
t=0.2s t=0.3s
Fig.1 Diagram of FEM model in LMF-GTAW Fig.2 The gestation period of the LEM-GTA Welding pool
† Received on 30 Sep. 2010 Transactions of JWRI is published by Joining and Welding

* State Key Lab of Mechanical Transimission, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Chonging University, Chongqing 400030, China Japan
7
Weld pool development and stirring behavior of AlCu4SiMg
aluminum alloy during GTA welding hybrid a longitudinal electromagnetic field
(a) (b)
t=0.4 t=0.6
(c) (d)
t=0.8 t=1.0 Fig.4 The stirring speed of LEM-GTA Welding pool

depending on the depth of welding seam
The flowing characteristic of molten metal becomes a

stable circular loop at the end of the gestation period, and the
welding time is about 0.3s. The "step-style" flowing shape
appears in welding pool, as shown in Fig.2h.
The direction of molten metal flowing remains constant
(e) (f) throughout the developing period, shown in Fig.3. The stable
flowing path is from the center of welding pool to the edge
of welding seam, which means the shape of welding seam is
t=1.2 t=1.4 the flat, so called “wide and shallow”. The “step-style” is
disappears at the end of the developing stage. A stable
flowing is formed in welding pool.
The flowing state of welding pool is locally affected by
the additional electromagnetic field. Specially, a stir driving
force forms a stir action in welding pool, shown in Fig. 4.
Compared to the traditional GTAW welding process, LMF-
GTAW has a significant rotation motion about the symmetry
(g) (h) D[LVR]D[LVșGLUHFWLRQ, shown in Fig.1).
Although the molten or solid state aluminum alloy is not
a ferromagnetic material, there also exists the distribution of
t=1.6 t=3.2 welding current flux in the welding pool, so the molten metal
in the welding pool is carried in response to the additional
electromagnetic forces imposed upon it. Under the influence
of the hybrid magnetic field, the maximum stirring speed is
present at the middle of the radius with the same depth. The
radius center region has a stronger electromagnetic driving
force in comparison with the others, due to the fact that the
bigger zonal components of welding current flux is
Fig.3 The developing period of LEM-GTA Welding pool perpendicular to LFM and a lower viscosity or flowing
resistance at higher temperature, which then produces
strong stirring behavior at the middle of radius, resulting the
iteratively by the FEM numerical procedure. The type of electromagnetic stir in welding pool.
material, namely, AlCu4SiMg aluminum alloy (3.9~4.8% Cu,
0.4~0.8% Mg, 0.4~1.0% Mn, 0.6~1.2% Si, Al balance) is 4. Conclusions
calculated. The physical parameters given to a quasi-three- Based on the numerical calculation of a hybrid
dimensional transient model are from the literature [2]. electromagnetic field in the molten metal flowing unified
model, we conclude that LMF affects the flowing state of
3. Results and Discussion molten metal at the welding pool. The welding current fluxes,
Figures 2 and 3 show the two-dimensional fluid flow direction of hybrid electromagnetic and local temperature of
velocities of LMF-GTAW pools during the gestation period molten metal determine the stirring behaviors of the LMF
and at the developing period respectively, the welding attachment during the GTAW process.
current is 100 A and the hybrid electromagnetic field is
0.01T. The direction of molten metal flowing is random in References
Fig.2. [1] Luo J, Luo Q, Lin YH and Xue J: Weld. J., 82(2003), pp 202s-
206s.
[2] Luo J, Jia CS, Wang YS, Xue J and Wu YX: Acta Metall. Sin.,
37(2001), pp212-219.
[3] Govindaraju N and Li BQ: Energy Convers. Manage,
43(2002),pp 335-344.
8
Numerical simulation of molten pool flow for various welding

†
parameters in V-groove GMA pipe welding
CHO Dae-Won*,NA Suck-Joo*, CHO Min-Hyun** and LEEJong-Sub**
KEY WORDS: (Numerical simulation) (Abel inversion) (Molten pool flow) (V-groove Pipe welding)
(Elliptic arc heat flux) (Bead shape)
1. Abstract 3. Arc heat flux modeling in GMAW

Normally many researchers used the axis-symmetric Heat input from arc plasma to cathode is transferred by
arc heat flux model in V-groove Gas Metal Arc welding conduction, radiation and convection. These terms are
simulations. In this study, however, the elliptic arc heat calculated by equation (1), (2) and (3).
flux model was adopted to conduct the 3D numerical keff (Tcb Tca ) Sj
simulations by applying Abel inversion to the arc images Qcond
G
(1) Qrad
2 ³ 4S r
cos M dV j (2)
Vj ij
captured with a CCD camera. Heat transfer and fluid flow
in the weld pool were analyzed to examine the 0.515 § Pcb Ucb ·
0.11 0.5
§ ucb · (3)
temperature distribution, flow velocity fields, and the Qconv ¨ ¸ ¨ Pca Uca ¸ C p (Tcb Tca )
Prca © Pca U ca ¹ © r ¹
solidified weld bead geometry during GMA V-groove
welding of pipes. The model solved the equations of Heat transfer from radiation, however, is less than 5%
conservation of mass, momentum and energy with the of the total heat input, and can be neglected according to a
VOF (Volume of Fluid) method which was adopted to realistic assumption [4]. So it is possible to assume that
calculate the shape of free surfaces. For various welding heat transfer from conduction and convection is
parameters such as welding position, torch angle, size of proportional to the temperature difference between the
gap, wire feed rate, different molten pool flows and bead cathode and the cathode boundary. In addition, the arc
shapes (humping, burn through) could be visualized in the plasma in GMAW is in LTE (local thermodynamic
CFD numerical simulations. The results of simulation equilibrium), where the gas temperature is the same as the
were compared with the experimental data, and showed a electron temperature. Finally, the arc heat flux modeling
good agreement can be completed by the irradiance of arc plasma because
it is linear to the arc temperature [5, 6]. The area matrix
2. Introduction Abel inversion method was used to obtain the irradiance
Previous V-groove or fillet joint simulations used the of arc plasma. Cho obtained arc heat flux model from
axis-symmetry arc heat flux model [1,2]. These studies, Abel inversion and found out that arc shape is elliptic
however, do not consider the effect of material shape, rather than axi-symmetry. [7]
which can deform the arc plasma shape. Y.T.Cho
calculated the arc heat distribution in a V-groove with 4. CFD pipe welding simulation
CCD camera and the area matrix Abel inversion method In this paper, the elliptic arc heat flux model (Eqn.4) is
and found out that the arc heat distribution had elliptic used to conduct numerical simulations. As the material
symmetry [1]. has a 60 degree V-groove, the effective radii for each
Optimizing the parameters in GMA(gas metal arc) viewpoint are 0.89mm and 1.54mm ( V x , V y )[7]. Other
pipe welding needs more effort than that in other cases factors such as arc pressure, electro-magnetic force,
because of the gravity force, which causes a molten pool droplet heat source, surface tension are considered in the
to flow to the ground. So, it is better to use the VOF numerical simulations. The VOF model equation is solved
(Volume of fluid) model than the FEM to check the iteratively by a commercial simulation program FLOW-3D.
molten pool flow. The VOF technique has recently been K AVI § § x2 y2 · · (4)
q ( x, y ) exp ¨ ¨ 2 2 ¸ ¸
used for some cases: in alloying elements in laser-hybrid 2SV xV y ¨ ¨ 2V x 2V y ¸ ¸
© © ¹¹
welding [2] and in laser drilling [3].

㻌 * Dept of Mech. Eng, KAIST, Daejeon, Republic of Korea Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Steel Solutions Group, POSCO, Pohang, Republic of Korea Japan
9
Numerical simulation of molten pool flow for various welding parameters in V-groove GMA pipe welding †
Fig.3 Molten pool flow and fusion zone

in overhead position
Fig.1 V-groove material shape (SS400 steel)
5. Conclusion
Due to different welding positions, molten pool flows
(1) The elliptic symmetry arc heat flux model is
make different bead shapes. Figure 2 shows the molten
proposed for CFD pipe welding simulation
pool flow before solidification and fusion zone in vertical-
(2) For different welding position, molten pool flows and
down position. Figure 3 shows the result in overhead
fusion zones are different.
position.
Reference
[1] Y.T. Cho and S.J. Na: Meas. Sci. Technol. 16(2005),
pp.878-884.
[2] W.I. Cho, S.J. Na, M.H. Cho and J.B. Lee: Proc. LAMP
(2009), pp.251
[3] K.W. Park and S.J. Na: Applied Surface Science, 256
(2010), pp.2392-2399
[4] M. Ushio, D. Fan and M. Tanaka M.: Trans. JWRI. 22
(1993) pp.201–207
Fig.2 Molten pool flow and fusion zone [5] W. L. Wiese: Spectrochimica Acta, 46B (1991) pp. 831–
in vertical-down position 841
[6] C. Yubero, M.S. Dimitrijevic, M.C. Garcia M.C. and M.D.
Calzada: Spectrochimica Acta Part B, 62(2007), pp.169-
176,
[7] D.W. Cho, S.J. Na, M.H. Cho and J.S. Lee: 63rd IIW Doc.
(2010)
10
Three-dimensional simulation of a flow in an arc weld pool by SPH

†
method
SHIGETA Masaya*, ITO Masumi*, IZAWA Seiichiro* and FUKUNISHI Yu*
KEY WORDS: (SPH) (Arc welding) (Weld pool) (Penetration shape) (Marangoni effect)
1. Introduction although the viscosity term is neglected, the fluid behaves

To optimize an arc welding process, precise prediction like a viscous flow because of the numerical viscosity. The
and evaluation of weld penetration are indispensable. detailed model description is found in Ref. [2].
However, it is extremely difficult to measure and directly
observe the molten-metal flow in the weld pool [1]. 3. Computational Condition
Furthermore, the modeling approach is also arduous The computational domain is a cylindrical anode with
because conventional grid-based numerical methods require the diameter of 50 mm and the height of 10 mm. The
a tangled algorithm to simulate the complicated flow in a domain is discretized by 27,504 particles with the diameter
weld pool which includes deformation of its free surface of 1.0 mm. At the side and bottom of the domain, two-
and movement of the solid-liquid interface due to the phase particle layers are set as a solid wall which does not melt. It
transition. is assumed that the position of the cathode is above the
In this study, to overcome that problem, an SPH cylinder along the central axis. The physical properties of
(Smoothed Particle Hydrodynamics) method is adopted for SUS304 are given to all the particles. The 300K uniform
simulating the thermofluid behavior during an arc welding temperature distribution is given to the entire area as an
process, taking into account four dominant flow-driving initial condition. The wall temperature is also fixed at 300K.
forces: the gradient of the surface tension (Marangoni The top surface of the anode is heated in the arc welding.
effect), the gas drag at the surface, the buoyancy, and the The heat flux from an arc to the anode surface is calculated
electromagnetic force (Lorentz force). The numerical based on the temperature distribution numerically obtained
calculations are carried out to demonstrate the individual by Tanaka et al. [3], which affects the surface particles. The
effects of those forces on the flow behavior. Also, the time step is set to be 1.0 ms.
simulation of a weld pool is performed including all of
those forces and the phase transition. In addition, the Table 1 Computational conditions.
influence of the sulfur content on the flow behavior and the Case Force Phase
weld penetration is presented. 1 – Liquid
2 Marangoni (with low sulfur) Liquid
2. Model Description 3 Marangoni (with high sulfur) Liquid
The SPH method is a gridless Lagrangian technique 4 Gas drag on surface Liquid
that expresses the fluid motion by particles that move 5 Buoyancy Liquid
according to Navier-Stokes equation. Additionally, even a 6 Lorentz force Liquid
solid region can be represented by particles that do not 7 All forces (with low sulfur) Solid+Liquid
move. Hence, SPH method offers high adaptability to 8 All forces (with high sulfur) Solid+Liquid
processes with large interface deformation such as a flow in
an arc weld pool. In this method, the mass of each particle 4. Results and Discussion
is given as a continuous function of Kernel W, so that the In this study, eight cases of computation are performed
equation of motion is written as as presented in Table 1. Case 1 is to see the effect of heat
wua §p p · F transfer only. Cases 2-6 are carried out against molten
¦ mb ¨¨ a2 b2 ¸¸ aWab a , (1) metal in order to check whether the SPH method can handle
wt b © U a Ub ¹ ma convective flows driven by the four forces: namely, the
where a and b denote the particle indices, u is the velocity, gradient of surface tension (Marangoni effect), the gas drag
t is the time, p is the pressure, m is the mass of a particle, ȡ on the surface, the buoyancy, and the electromagnetic force
is the density at the position of a particle, and F is the (Lorentz force). Figure 1 presents the computational results
external driving force. The first term of the right hand side of the half domain at t = 2.0 s. Each particle is colored
in Eq.(1) represents the pressure gradient. In this paper, according to its temperature. White corresponds to 2500 K.
† Received on 30 September 2010. 㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 Transactions of JWRI is published by Joining and Welding

* Graduate School of Engineering, Tohoku University, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Sendai, Japan Japan
11
Three-dimensional simulation of a flow in an arc weld pool by SPH method
In Case 2, the fluid heated at the center on the surface approximation and is given to all liquid particles. As a
spreads outward, while in Case 3, the heated fluid is result, the high temperature region is observed only on the
transported downward. These results derive from the surface.
difference in the direction of the surface tension gradient. It Case 6 shows that the fluid heated at the surface flows
is known that Marangoni effect shows two different downward. During the arc welding, the electromagnetic
tendencies depending on the sulfur content in SUS304, i.e. field is generated, and consequently, the Lorentz force acts
the surface tension increases with temperature when the on the fluid inside of the weld pool. In this study, the
sulfur content is low, while it decreases when the sulfur axisymmetric Lorentz force is calculated from the electric
content is high [4]. In the present computation, the specific current density distribution obtained in Ref. [3].
data of Ref. [4] is used. Figure 2 depicts the computational results when all the
In Case 4, the gas drag, which is a frictional force by forces and the phase transition are taken into account, at t =
the shielding gas flow on the surface of the weld pool, is 20.0 s. For the phase change, the latent heat is treated. The
calculated from the velocity distribution obtained in Ref. red particles are at the melting point, 1750 K. The depth of
[3]. Because the drag acts outward to the surface particles, penetration is approximately 4 mm in Case 7, meanwhile
the high temperature region at the surface spreads. the penetration has reached about 8 mm in Case 8. This
In Case 5, the buoyancy caused by the non-uniform difference is obviously attributed to the difference in the
temperature distribution in a weld pool are taken into sulfur contents.
account. The force is calculated using the Boussinesq
㻌㻌㻌 Case 1 㻌㻌㻌㻌 Case 2 Case 3
Case 4 Case 5 Case 6

Fig. 1 Temperature distributions caused by flow driven with only a force (t = 2.0 s).
Case 7 Case 8 Color legend of the images

Fig. 2 Temperature distributions including all the forces and phase transition (t = 20.0 s).
12
5. Conclusions References
In this study, the SPH method was applied to a [1] K. Yamazaki, E. Yamamoto, K. Suzuki, F. Koshiishi, S.
simulation of the thermofluid behavior during an arc welding Miyazako, S. Tashiro, M. Tanaka and K. Nakata: Quarterly
process, taking four dominant flow-driving forces into Journal of the Japan Welding Society, 27 1 (2009), pp.34-40.
(in Japanese)
account. The numerical calculations presented the effect of
each force on the temperature distribution inside the weld [2] M. Shigeta, T. Watanabe, S. Izawa and Y. Fukunishi: Int. J.
pool. Also, the simulation of a weld pool was conducted Emerging Multidisciplinary Fluid Sci., 1 (2009), pp.1-18.
including all the forces and the phase transition. The [3] M. Tanaka, M. Ushio, T. Isa and J.J. Lowke: JSME Int. J.
influences of the sulfur content on the flow behavior and the Series B, 48 (2005), pp.397-404.
weld penetration were shown. The penetration shapes of the
present computation showed a tendency similar to Ref. [3]. [4] T. Zacharia, S.A. David, J.M. Vitek and T. Debroy: Metall.
Trans. B., 21 B (1990), pp.600-603.
Here, we can conclude that SPH method is a method suitable
for a thermofluid simulation of an arc weld pool.
13
Numerical simulation and vision-based sensing of key-holing

†
process in plasma arc welding
LIU Zuming*, WANG Xiaojie*, WU Chuan Song*
KEY WORDS: (Numerical simulation) (Sensing) (Plasma arc welding) (Key-holing process)
1. Introduction 180
160
Efflux plasma voltage (mV)

2000
To overcome the shortcomings of conventional plasma 140
Welding current (A)

arc welding (PAW), the ‘controlled pulse key-holing’ 120
1500
100
strategy is proposed and the waveform-controlled keyhole 80 Welding current
PAW experiment system is developed [1]. During the 60 Efflux plasma voltage
1000
waveform-controlled PAW process, the key-holing process 40
20
takes place, i.e., keyhole establishing, expanding, sustaining, 0 500
contracting and closing, in each pulse cycle. Sensing and -20
-40
describing the keyhole shape and geometry with proper 0
50 51 52 53 54 55 56 57 58 59 60
methods are of great significance for optimizing the
Time (s)
welding process parameters and enhancing the stability of
weld quality [2]. In this study, the key-holing behaviors are Fig.1 The measured welding current and efflux plasma
visualized through both numerical simulation and voltage
experimental measurement.
2. Experimental measurement
The developed waveform-controlled PAW experimental
system consists of the computer, PAW machine, data
acquisition unit, welding current sensor, efflux plasma
voltage sensor and CCD camera. The computer is the
central unit for adjusting welding current, and sampling the Plasma
signals of welding current, efflux plasma voltage and arc
keyhole images. On one hand, a measuring bar mounted
underneath the workpiece to be welded and kept insulated
electrically is employed to detect the efflux plasma voltage
when the keyhole is established. On the other hand, a CCD
camera is aimed at the weld pool from the backside to
capture the keyhole images. Efflux
Figure 1 shows the measured welding current and plasma
efflux plasma voltage signals. At the dropping stage of
welding current from the peak level to the base level, two
sub-stages of current decreasing with different slopes are
added. The signal of the efflux plasma voltage is around Fig.2 The captured images of both the plasma arc and
zero before the keyhole is established, while it exceeds a the efflux plasma
certain value after the keyhole is established. It is clear that
each pulse produces one keyhole during the welding
process. Figure 2 is the images of both the plasma arc transient waveform-controlled PAW process are very
and the efflux plasma captured from a side view. Figure 3 complicated. As a first step, the level-set method is used to
shows an image of keyhole from the backside of the track the keyhole boundary in stationary continuous-current
workpiece. PAW process [3]. As shown in Fig. 4, the level-set function
is defined as a signed distance function M ( x , t ) r d ,
3. Simulation of keyhole shape and size where d is the actual distance from the keyhole boundary,
The modeling and simulation of keyhole behaviors in
* Institute of Materials Joining, Shandong University, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
14
Numerical simulation and vision-based sensing of key-holing process in plasma arc welding
-2
(a)
z, mm
4
0.18 m/s
6
8
-8 -6 -4 -2 0 2 4 6 8
r, mm
-2
Fig.3 The captured image of keyhole at backside (b)
0
x is the space variables, and t is time. The level-set function
has the value of 0 on the keyhole boundary. The plus (minus) 2
sign denotes the outside (inside) of the keyhole boundary.
z, mm
By using the level-set method the keyhole boundary tracking
4
problem can be transformed into a partial differential
equation, which can be numerically solved with other 0.48 m/s
6
governing equations. The general form of the level-set
equation is
8
wM -8 -6 -4 -2 0 2 4 6 8
F M 0 (1)
wt r, mm
where F is the speed function in the normal direction of the -2

(c)
keyhole boundary. To get the function , the fluid flow in
both the plasma and weld pool must be known. The 0
combined volumetric heat source model is used to

numerically analyze the transient temperature field and then 2
z, mm
to determine the weld pool geometry. The algorithm of level-

set theory combined with the transient thermal conduction 4
model is used to determine the evolution of both keyhole and 0.53 m/s
weld pool geometry at different time steps. Figure 5 6
demonstrates the simulated keyhole profile during stationary

PAW under following conditions: stainless steel plate of 6- 8
-8 -6 -4 -2 0 2 4 6 8
mm thickness, welding current 180 A, arc voltage 24.5 V, r, mm
plasma flow rate 3.0 L/min, shield flow rate 20.0 L/min, -2
torch standoff distance 6 mm. It is found that a complete (d)
keyhole is established at 2.5 s for current levels of 180 A. 0
The numerical analysis of keyhole formation is verified by
measuring the efflux plasma voltage signals at the moment of 2
key establishing.
z, mm
Plasma 6
0.45 m/s
torch
8
-8 -6 -4 -2 0 2 4 6 8
ĳ<0 r, mm
Fig.5 Keyhole profiles in stationary PAW at (a) t=1.5 s, (b)

ĳ=0 t=2.5 s, (c) t=2.8 s, (d) t=2.9 s
r
(The direction and length of arrows inside the pool indicate
ĳ>0 respectively the direction and velocity of fluid flow)
Weld
pool 4. Conclusions
A waveform-controlled PAW system is developed to
implement the controlled pulse key-holing strategy. A special
z current waveform is designed with two sub-stages of current
decreasing with different slopes at the dropping edge of
Fig.4 The definition of level-set function pulse, and the mode of one keyhole in each pulse is realized.
The CCD camera and efflux plasma voltage sensor are used
to measure and characterize the keyhole shape and size.
Based on the level-set theory, a numerical model is
developed to describe and simulate the keyhole behaviors in
15
stationary PAW, and is employed to track the evolution References

process of keyhole boundary. [1] C.S. Wu, C.B. Jia and M.A. Chen: China Welding, 19 (2010),
pp.12-16.
Acknowledgments [2] Y.M. Zhang and Y.C. Liu: Automatica, 43 (2007), pp.876-884.
The authors are grateful to the financial support for this
research from the National Natural Science Foundation of [3] X.J. Wang, C.S. Wu and M.A. Chen: Acta Metallurgica Sinica,
46(2008), pp.984-990.
China (Key Program Grant No. 50936003).
16
A Study on the macro-micro physical properties in pulsed arc

†
plasma
SONG Yonglun*, YAN Sibo, XIAO Tianjiao and YANG Xiaohong
KEY WORDS: (Pulsed arc) (High frequency) (Diffusing mode) (TIG welding) (Physical properties)
1. Introduction
Extensive research has been reported on pulsed arc
welding and its effects over the past decades. The
advantage of the pulsed arc summing-up in the literature,
however, mostly concerns weld metallurgy, including
refinement of fusion zone grain size and substructure,
reduced width of HAZ and so on [1]. Mechanical property
improvement of welding joint always was explained as an
evidence of the effects. To deepen the understanding of
pulsed arc physical properties, a study on the effects of
pulsed TIG welding arc is made from lower frequency to
higher frequency up to 80 kHz in both electric and thermal Fig. 2 Arc voltage vs pulse frequency
respects.
3. Micro View of Pulsed TIG Arc
2. Macro View of Pulsed TIG Arc Electron density in arc column is observed by Stark
Welding is carried out using a TIG welding machine broadening spectrum and can be calculated using Stark
(EWM Tetrix 500) as base current source (BCS). A high broadening of the 656.3nm HĮ emission line [3]. Figure 3
frequency current producing device is used as peak current shows a trend of the electron densities in the Ip period with
source (PCS), and it works with BCS synchronously for frequency changing. The electron density goes down at
generating square current waveform.Welding conditions higher frequencies though the input energy from power
are as follows ĭ0 mm, 2% Ce-tungsten electrode with source to arc is increasing. It may indicate that arc column
60º tip angle; Argon shielding gas 10l/min and 4 mm arc diffusing near the tungsten cathode instead of continually
length. Welding parameter setting᧶Ip = 100A, Ib = 50A. lift-up constriction at higher frequency in order to realise
Figure 1 shows the arc profiles changing in the “electric- energy balance.
thermal transfer” mode from a diffuse to a lift-up
attachment with pulse frequency increasing [2], and a ball-
like arc column contracting towards tungsten cathode can
be observed in the higher pulse frequency region. Figure 2
shows a trend of the arc voltage Up and Ub with frequency
changing respectively. The phenomena of Up going up with
the increase of pulse frequency and strong oscillation
appearing and taking 30% of the Ub period during the
changing from Ip to Ib are rather noticeable.
50 1K 2.5K 20K 50K 80K
Fig. 3 Electron density Ne vs pulse frequency
4. Discussion
While energy frequency inputting to the arc near or
reaching to the order of the critical time of energy transfer
based on electron-collision mode[3], a positive potential
Fig. 1 A map of the arc profiles in different pulse drop would be needed in order to transport the energy from
frequancies
* Beijing University of Technology, Beijing, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
College of Mechanical Engneering & Applied Electronics Japan
Technology
17
A Study on the macro-micro physical properties in pulsed arc plasma
5. Conclusions
Based on the above discussion, the following results
may be concluded:
(1) With the increase of pulse frequency, there are 2
diffusing modes in TIG arcs, that is, diffusing
attachment towards anode at lower frequency region
and ball-like diffusing near cathod at higher frequency
region. The phenomenon of continual constriction with
the frequency increasing is not as expectation, only a
Fig. 4 Arc dynamic impedance model slight constriction of the arc at the lower frequency
the arc column into the anode. It would be a reason to region can be identified.
explain the phenomena of Up going up with increase of (2) The electron density distribution with frequency
pulse frequencies. changing may support the profiles of pulsed arc in some
According to the experimental result, the TIG arc may diffusing modes. It may be helpful to understand the
be not the first-order inertial link under the higher physical properties of free burning TIG arcs.
frequency condition, but a second-order link with the
obvious oscillation phenomenon in the view of electricity. Acknowledgement
An arc dynamic impedance model may be shown in Fig. 4, This work is financially supported by the Chinese NSF,
and the corresponding arc dynamic impedance transfer project no. 50375005.
function may be expressed by:
References
[1] T. Senthil Kumar, V. Balasubramanian and M.Y. Sanavullah:
U (s) s Influences of pulsed current tungsten inert gas welding
Z (s) parameters on the tensile properties of AA 6061 aluminium
I (s) 1
Cs s
2 1 (1)
R L alloy, Materials and Design 28 (2007), pp. 2080–2092
[2] J Heberlein, J Mentel and E Pfender: The anode region of
According to the model, the inductance feature may electric arcs: a survey, J. Phys. D: Appl. Phys. 43 (2010),
play a main role at lower frequency region, and the pp.1-31
capacitance feature may play a main role at higher [3] Hans R. Griem: Spectral line broadening by plasmas. New
frequency region. It would be a reason to explain the York: Academic press, (1974), pp.226-231
phenomena of Ub going down.
18
Evaporation phenomena of magnesium during pulsed-MIG arc

†
welding of aluminum alloy
WANG Jing-Bo*, NISHIMURA Hitoshi*, KATAYAMA Seiji** and MIZUTANI Masami**
KEY WORDS: (Evaporation phenomena) (Evaporation rate) (Evaporation flux) (Magnesium)

㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 (Aluminum alloy) (Pulsed-MIG arc welding)
1. Introduction Welding conditions and the chemical compositions of

Welding fumes are frequently formed during pulsed- materials used are shown in Table 1 and Table 2.
MIG arc welding of aluminum alloy using a 5xxx
Table 1 Materials used and welding conditions.
aluminum alloy welding wire because of the evaporation of
magnesium which is present at several percents for the Material Plate A5052 (t 9 mm)
prevention of welding cracks [1]. There are two methods to Wire A5356 (䃥1.2 mm)
evaluate the evaporation phenomena during arc welding. MIG Torch angle Perpendicular to work
The one is to collect the total welding fumes formed during Tip-to-work distance 18 mm
a constant welding period to quantitatively calculate the Shielding gas (Ar) 20 L/min
evaporation rate. The other one is to directly observe the Average current 150 A
droplet behavior with a high-speed video imaging system. Average voltage 20 V
By both methods, unfortunately, it is impossible to evaluate Peak current 335 A
the evaporation phenomena during peak or background Background current 80 A
periods separately. Frequency 180 Hz
This paper presents a novel method for calculating the Welding speed 8.33 mm/s
evaporation rate and flux of magnesium in peak period Welding position Bead on plate
during pulsed-MIG arc welding.
4. Experimental results and discussions
2. Method to visualize droplet behavior
In order to characterize the behavior of the droplet
A high-speed video imaging system was used to
formation and the evaporation phenomena a series of high-
observe the arc morphology and the behavior of droplet
speed video images are examined. One example showing
formation. A diode laser with a center wavelength of 930
the droplet transfer is shown in Fig. 1. Attention, especially,
nm was used for illumination in order to visualize the
should be taken to the time for forming a neck near the
formation of particulate fumes from the droplet surface.
droplet-wire boundary which is about 1 ms from the
beginning of a peak period and is nearly coinciding with the
3. Method to calculate evaporation rate and flux
time for the formation of particulate fumes.
The calculation of the evaporation rate and flux is
conducted by the following three steps. (a) 0 ms (b) 0.25 ms (c) 0.50 ms (d) 0.75 ms (e) 1.00 ms (f) 1.25 ms
(1) An automated robot welding system is used to produce Neck Particulate
a series of droplets by shutting-down the peak current

and stopping the wire feeding at different droplet
growth times in one peak period.
(2) The magnesium contents of the above produced
droplets are analyzed by EDX analyzer. At the same (g) 1.50 ms (h) 1.75 ms (i) 2.00 ms (j) 2.25 ms (k) 2.50 ms (l) 2.75 ms
time, the droplet volumes of these droplets are

measured, and the droplet surface areas are measured
from a series of high-speed video images.
(3) From the relationship between the magnesium content, Particulate Particulate Particulate Particulate Particulate Particulate
droplet volume, droplet surface area and the droplet
growth time, the evaporation rate and flux of Figure 1 A series of high-speed video images showing the droplets
magnesium during peak period are calculated. formed at the welding wire tip (peak: (b)-(g); background: (a), (j)-(l);
transition from peak to background: (h)-(j)).
㻌 †㻌 Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding

㻌 *㻌 Panasonic Welding Systems Co., Ltd., Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
**㻌 JWRI,㻌 Osaka University, Osaka, Japan Japan
19
Evaporation phenomena of magnesium during pulsed-MIG arc welding of aluminum alloy
Table 2 Chemical compositions of materials used.
Chemical compositions (mass %)

Materials Cr Cu Fe Mg Mn Si Ti Zn Al
Plate (A5052) 0.170 0.010 0.270 2.650 0.000 0.080 0.000 0.000 Bal.
Wire (A5356) 0.058 0.001 0.167 4.952 0.055 0.128 0.072 0.002 Bal.
Droplet volume and droplet surface area are measured,

and the magnesium content in the droplet is analyzed. The 8 6
obtained results of droplet volume V drop , droplet surface
area S drop , and magnesium content C Mg , are shown in Fig. 2.
(mm 2 )
About the droplet growth behavior, when the droplet Sdrop
(mm 3)
Mg content, C Mg (mass %)
growth time TS is under 0.5 ms, both the droplet volume 6 5
drop
and droplet surface area increase slightly. From the high-
drop
speed video images, the arc root is seen to spread from the CMg
Droplet surface area, S

droplet bottom to climb toward the wire boundary and the
Dorplet volume, V
droplet itself deforms. Before the arc root spreads up to a 4 4
solid part of the welding wire, the droplet volume increased
only a little. When TS is over 0.5 ms to 1.6 ms, both the
droplet volume and the droplet surface area increase
abruptly. About the magnesium evaporation behavior, when Vdrop
2 3
TS is 0 ms, that is, at the end of the background period or
the beginning of the peak period, the magnesium content in
droplet is 4.63 mass %. With increasing the droplet growth
time TS up to 1.0 ms, the magnesium content decreased to
0 2
4.2 mass %. After that, the magnesium content decreased
very slowly to reach about 4.0 mass % at the end of the 0.0 0.5 1.0 1.5 2.0
peak period of about 1.6 ms. The decrease in magnesium Droplet growth time, TS (ms)
content with increasing TS is considered to be caused by Figure 2 Droplet volume, droplet surface area and
the evaporation of magnesium from the droplet surfaces magnesium content at different droplet growth times.
whose temperatures are reported to nearly reach their
boiling point [2]. From Fig. 2, empirical relationships
between the droplet volume V drop (mm3), droplet surface
area S drop (mm2), magnesium content C Mg (mass %) and TS After the above calculation, the evaporation rates V vap(i)
(ms) are obtained as Equation (1) to (3). (i=1, 2,䡡䡡㻘㻌䡡㼚㻕㻌 and evaporation flux are plotted
accounting for TS. The calculated results are shown in Fig.
V drop =0.844+8TS2/(TS2+18) (1) 3. It is seen that in region I (TS=0-0.2 ms) slight decreases
S drop =3.405+8TS2/(TS2+3.2) (2) both in the evaporation rate and flux are confirmed. This is
C Mg =3.9+0.73e(-TS/0.85) (3) attributed mainly to the evaporation from the anode root
area. In region II, the evaporation rate increases very fast
From equation (1) to (3), the evaporation rate and flux of with increasing TS up to 1.2 ms and the evaporation flux
magnesium during peak period can be calculated as follows. increases slightly and finally reaches a saturated value.
Firstly, one peak period is divided by a time interval ԥTS When TS increases into region III, the increase of the
(=0.01 ms) into TS (i) (i=0, 1, 2, 㺃㺃㺃, n). V drop(i) and C Mg(i) evaporation rate with increasing TS slows down a little and
(i=0, 1, 2, 㺃㺃㺃, n) are calculated from Equation (1) and (2) the evaporation flux decreases slightly. The change from
by inputting TS=ixԥTS. Secondly, the evaporation rate region II to region III is considered to correspond with the
and flux are calculated as follows by putting i=1, 2, 㺃㺃㺃, n. formation of particulate fumes as shown in Figure 1. In
(1) Calculating the mass of magnesium W dMg(i-1) and region III the slow-down of the evaporation rate or the
W dMg(i) at TS (i-1) and TS (i) , respectively. decrease of evaporation flux with increasing TS is thought
(2) Calculating the mass of magnesium W wMg in the to be caused by the evaporation of aluminum accompanied
welding wire melted during ԥTS. with magnesium which is supposed to be included in
(3) Calculating the evaporation rate of magnesium V vap(i) particulate fumes.
[=(W dMg(i-1) +W WMg -W dMg(i) )/ԥTS].
(4) Calculating the evaporation flux by dividing V vap(i) by
Equation (2).
20
5. Conclusions
4 1.0 This study is summarized as follows.
䊠䊡䊢 (1) According to the evaporation behavior of magnesium,
Evaporation flux (g/cm 2/s)

Evaporation rate (g/min)
the peak period is divided into three regions. That is,

3 the region I is from TS=0-0.2 ms, the region II from
TS=0.2-1.2 ms and the region III from TS>1.2 ms.
(2) In region I, both the evaporation rate and flux decrease
2 0.5 slightly, and the evaporation is considered to be
dominated by the evaporation of magnesium from the
anode root area on the droplet surface.
1 (3) In region II and III the evaporations are considered to
be dominated by the evaporation from the whole
Peak period droplet surface. The region III corresponds to the
0 0.0 formation of particulate fumes which is considered to
0.0 0.5 1.0 1.5 2.0 accompany with a small amount of aluminum.
Droplet growth time, TS (ms)
References
Figure 3 Calculated evaporation rate and evaporation [1] J. H. Dudas and F. R. Collins, Welding J., 45 (1966), pp.241s-
flux of magnesium from the droplet surface. 249s.
[2] R. A. Woods, Welding J., 60 (1980), pp.59s-66s.
21
Experimental and numerical study of friction stir welding with

†
double-shaft stir probe
XU Zhongfeng* , LU Hao*
KEY WORDS: (FSW) (Numerical simulation) (Heat source model) (Temperature field)
1. Introduction
Friction stir welding[1] (FSW) is a new developed
solid-state joining technique. FSW has been successful
applied to aerospace, ship manufacturing and automobile
industries. However, due to the disadvantage of the concave-down area
keyhole, which is caused by the probe’s pulling out when center line
circular weld is applied, NASA developed a kind of
double-shaft stir probe. The stir probe can pull out with a Fig. 2 Cross-section of the weld bead
certain velocity from the weldment when the shoulder is
still rotating and advancing along the weld bead. A
Significant process has recently been made on heat
schematic illustrating the process of FSW is shown in Fig.
transfer modeling for FSW. Frigaard, Grong, and
1.
Midling[2] developed a process model for FSW, the heat
input from the tool shoulder is assumed to be the friction
probe heat, and the coefficient of friction or the calculated
temperature during the welding is adjusted to keep the
calculated temperature from exceeding the material
melting point. The Rosenthal equation for modeling
shoulder heat-transfer for thin plates has also been applied in
modeling the heat-transfer in FSW[3]. Because of the
process of the probe’s pulling out, the heat transfer process
will become complicated. Numerical methods are very
convenient for the investigation of the mechanism of FSW.
Therefore, this work mainly studies the weld quality and
Pull
the heat transfer.
V
2. Description of the heat source model

Press Press
In the presented model, the heat at the tool
shoulder/workpiece interface and the heat at the tool
probe/workpiece interface are both considered.
Because the hardness of the probe is larger than
Fig. 1 Schematic diagram of friction stir welding the weldment in the FSW, when the welding is in the
quasi-stable state, we can get the following equation:
d f = Ĳ s hd s
When the stir probe is abreast with the shoulder, the According to the rule of Misses yielding, the
shoulder depresses at a certain velocity so as to replenish rheological shear stress Ĳ s can be calculated by the
the instantaneous cavity caused by the probe’s pulling out following expression:
from the weldment. Figure 2 shows the features of a weld
bead in the vertical direction at the last process. Ĳ s =0.577hR eL (T)
Where d f is infinitesimal friction force, R eL (T) is the
stress value when the material generates 0.2% plastic
strain and is the function of temperature[4], d s is
†㻌 Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding
* Materials Science and Engineering School, Shanghai Jiaotong Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
University, Shanghai 200240, China
Japan
22
Experimental and numerical study of friction stir welding with double-shaft stir probe
infinitesimal contact area. Finally, we can get the equation

of heat flux at the integral point in the tool
shoulder/workpiece interface:
K E =Wh0.577 R eL (T)r
Where K E is surface flux density, W is the angular
velocity of the probe, r is the radial distance from the tool
axis.
The friction at the tool probe/workpiece interface
is simplified for calculating easily. We will treat the heat
Fig. 5 33-D
Fi D view
i off the
th calculated
l l t d ttemperature
t contour
t
as body flux:
Q=0.577 R eL (T) hn / 30[5] At the beginning and at the end of welding, the
Where Q is the body flux density, n is the rotating calculated temperature at the measuring points change a
velocity of the stir probe(r/min). little, which shows the probe’s primary function is to
Therefore, R eL (T) is a very important parameter deform the material around the tool and its secondary
related to the material property. In this experiment, Zwick function is to generate heat.
machine is used for tensile test to get the Stress-Strain
curve under different temperature. 2219 aluminum alloy
strip is used for getting the R eL (T) value, as shown in Fig.
3. Then, the R eL (T) value under different temperature can
be found in the curve, as shown in Fig. 4 .
Fig. 6 Calculated temperature at the beginning
Fig. 3 Shape of samples
Fig. 7 Calculated temperature at the end
Fig. 4 2219 R eL curve at different temperature 4. Conclusions

According to the experiment and simulation results,
3. Temperature distribution of FSW the following conclusions can be obtained:
During this period, the tool traverses along the joint ˄1˅The self-adaption model of heat generation can
line at a constant weld speed. Figure 5 shows the accurately model the heat-transfer process in FSW.
calculated temperature contour and the heat-transfer The difficulty of determining coefficient of friction
process in the weld period can be clearly found. has been settled. In the simulation, we adopt R eL (T)
Additionally, R eL (T) depends on the temperature produced as an important parameter.
by welding. Numerical models of FSW have shown that ˄2˅By the FEM model of FSW welding, nodes will
with the welding temperature increasing, the R eL (T) value experience some time before reaching the top
decreases, resulting in the top temperature of some point temperature. Comparing the stability period of
gradually reaching. Figure 6, 7 show the temperature welding with the probe’s pulling out period, we
curves of three points, 12mm, 16mm, 18mm, away from find that the temperature distribution changes a
the center point at the initial stage and at the end of little. The heat generated at the tool probe
welding respectively. From Fig. 6, it can be found that the /workpiece interface accounts for 20%
calculated temperature contour at 12.0 s is similar to that approximately of the total.
at time 20.0s, which implies that a steady heat transfer is
reached.
23
Acknowledgement friction stir welding of age hardening aluminum alloys,

This project is support by the National Natural Metallurgical and Materials Transactions A 32A (2001).
Science Foundation of China (Grant No. 50975176) [3] M.J. Russell, H.R. Shercliff, Analytical modeling of
microstructure development in friction stir welding,
Proceedings of the first International Symposium on Friction
References
Stir Welding, Thousand Oaks, CA June 1999.
[1] W.M.Thomas, E.D.Nicholas, J.C.Needham, M.G.Murch, P.
[4] Hongke, Li, etal. The sef-adaption heat source model of
Temple-Smith, C.J.Dawes, Friction stir butt welding, Int.
FSW[J].The Welding Transaction, 2006, 27(11):81-85.
Patent Application no. PCT/GB92/02203; GB application no.
[5] Chun Xia, etal. The heat source model of FSW[J]. Hot
9,125,978.8, 1991; US Patent no. 5,460,317, 1995
Working Technology, 2008, 19(37): 108-110,113
[2] Ø. Frigaard, Ø. Grong, O.T. Midling, A process model for
24
Experimental and numerical studies of material flow during

†
welding by friction stirring
SHIMODA Yoichiro*, TSUBAKI Masami*, YASUI Toshiaki*, and FUKUMOTO Masahiro*
KEY WORDS: (Friction Stir Welding) (Material flow) (High speed video camera) (PIV) (FEM model)
1. Introduction high speed video camera (Photron FASTCAM SA5). The

Friction stir welding (FSW) is a solid state welding material flows at advancing side (AS) and retreating side
process invented and patented by TWI in 1991 [1]. The (RS) of the pin were observed from the tool bottom.
weld joint is produced by plastic flow of material induced Particle image velocimetry (PIV) is an optical method of
by friction between a tool and work pieces, and controlled fluid visualization. It is used to obtain instantaneous
by rotating speed of the tool, welding speed, axial force and velocity measurements. In this study, material flow during
the tool shape etc. As qualitative analysis of material flow, welding was measured with PIV method, and the analysis
metallic insert material is set in the position of weld metal conditions were shown in Table 1.
before FSW [2]. In case of dissimilar metals welding, the
material flow was evaluated by X-ray computed Work piece direction x
Rotation Load
tomography [3]. Additionally, direct observation of z
material flow was conducted by using transparent poly- y
vinyl chloride (PVC) as simulation experiments of welding PVC(clear)
between aluminum alloys [4]. However, it is difficult to or
evaluate the material flow quantitatively during welding. PVC(gray)
In this study, quantitative measurement and calculation
of the material flow around the tool pin during welding PVC(gray)
or
were investigated. As simulation experiments of welding PVC(clear)
between aluminum alloys, the material flow of welding High speed video camera
between PVC was measured by particle image velocimetry
(PIV) method with high speed video camera. Also, the (a) Schematic view of welding experiment.
material flow during welding was numerically simulated by
plastic forming software DEFORM-3D. From these studies,
PVC x PVC x
direction and velocity of the material flow during welding (clear) (gray)
Rotation y Rotation y
around tool pin were estimated.
Shoulder Shoulder
2. Direct observation of material flow during welding
Welding experiments were performed by a machining
center (Enshu S400). The welding tool was composed with Observation area Observation area
a shoulder, which was made of tool steel with Ǿ20mm in
diameter, and pin, which was made from WC-Co cemented PVC PVC
(gray) (clear)
carbide with a screw shape and Ǿ5mm in diameter and
4.0mm in length on the top. In this study, transparent PVC Work piece direction Work piece direction
(clear) and PVC (gray) were welded as simulation (b)AS view. (c)RS view.
experiment of welding between aluminum alloys. PVC Fig. 1 Experimental set up for direct observation of FSW.
(clear) and PVC (gray) were both 20mm in width, 50mm in
length and 20mm in thickness. Figure 1 shows the Table 1 Observation and PIV analysis conditions.
arrangement of weld materials and movement of the tool. Shutter speed (frame/s) 1,000
The tool is plunged into the interface between PVC (clear) Analysis image number 400
and PVC (gray) and moves along the weld line. The Interval of analysis image (s) 0.001
rotating speed was 750rpm and the revolution pitch was Scanning area (mm2) 3.4
0.2mm/r. Material flow during welding was observed with a
* Department of Production Systems Engineering, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Toyohashi University of Technology, Toyohashi, Japan Japan
25
Experimental and numerical studies of material flow during welding by friction stirring
3. Numerical model for FSW Low magnification High magnification

In this study, the commercial FEM software DEFORM-
(a) (b)
3DTM was used for welding simulation. This software is a
Lagrangian implicit code designed for metal forming AS (b)
processes. The workpiece was single-block continuum
model (PVC), used in order to avoid contact instabilities Flow1
due to the intermittent contact at the sheet-sheet and sheet-
tool interfaces. The workpieces were meshed with about
100,000 tetrahedral linear elements. The tool was modeled Pin
as rigid body (WC-Co cemented carbide) and meshed for Pin
velocity analysis with about 3,700 tetrahedral elements.
These assumption are reasonable as the yield strength of the (c) (c)
workpiece is significantly lower than the yield strength of
Pin
the rotating tool. Following thermal characteristics of PVC
Velocity (mm/s)
2.0
were used in this simulation: thermal conductivity k=0.17
(W/mK), and thermal capacity c=1.95 (N/(mm2K)). These RS
assumption linearizes the finite element formation for Flow2 1.0
temperature analysis and results in better convergence [5].
A rigid-viscoplastic temperature and strain rate dependent Rotation
material model is employed Work piece direction 0.0
()()
n
σ = cε ε + y
m
(1) Fig. 3 FEM analysis of material flow.
Where c =7.791, n =1.987, m =-0.116 and y =20.052
Figure 4 shows measured and calculated results of material
(MPa) are material constants determined by a numerical
flow velocities by PIV and FEM analysis during welding.
regression based on experimental data [6].
The material flow velocities of PIV analysis ranges from
about 2 to 20 mm/s at AS. The material flow velocities of
4. Results and Discussion
PIV analysis ranges from 1 to 5 mm/s at RS. These are
Figure 2 shows the material flow of the weld with high similar tendencies that of FEM analysis. Additionally, both
speed video camera and analysis of PIV at AS and RS. velocities of PIV and FEM at AS are faster than that flow at
Figure 3 shows FEM analysis of material flow. From PIV RS.
and FEM analysis, material flow was observed different One revolution of welding tool
type of flow direction at RS and RS. At RS, direction of the
material flow (Flow2) was corresponded to the tool rotation. 30
However, material flow (Flow1) at AS was in the reverse (a) AS PIV
25 FEM
Velocity, mm/s
direction of the tool rotation. The material flow from AS to

PIV
RS passed behind the pin. 20
15 FEM
photograph PIV analysis
(a) PVC (b) 10
(clear)
(b) 5
Flow1 10
0
AS
(b) RS PIV
8 FEM
Velocity, mm/s
Pin
PVC Pin PIV
1mm (gray) 6 FEM
(c) PVC (gray) (d) 4
Pin Pin
2
Velocity (mm/s)
(d) 2.0
RS
Flow2
0
PVC 1.0 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4
(clear) Time, s
Rotation Fig. 4 Measured and calculated results of material
Work piece direction 1mm 0.0 flow velocities by PIV and FEM analysis during welding.
Fig. 2 Material flow of weld with high speed video camera Analysis area is Fig. 2, (b), (d) and Fig. 3, (b), (c).
and analysis of PIV.
26
5. Conclusions [2] Schmidt H et al, Material flow in butt friction stir welds in
Material flow by friction string during welding was AA2024-T3, Acta Materialia 54 (2006) 1199-1209.
investigated with experimental and numerical studies. [3] Y. Yasui et al, Macrostructure of butt weld between aluminum
Following results were obtained. and steel by friction stirring, Proc. 6th Int. Symp. on FSW
(2008) 1100-1130.
1. Material flow at RS corresponded to the rotating
[4] T. Shinoda et al, Observation of metal flow phenomenon in
direction of the tool. However, material flow at AS friction stir welding of aluminum alloy, Proc. 7th Int. Symp.
was in the reverse direction of the tool rotation. The on FSW (2008) 1405-1430.
material flow from AS to RS passed behind the pin. [5] G. Buffa et al, Finite element studies on friction stir welding
2. From PIV and FEM analysis, material flow velocities processes of tailored blanks, Computers and Structures 86
at AS are faster than that at RS. (2008) 181-189.
[6] Sharon Y.Soong et al, The effects of thermomechanical
References history and strain rate on antiplasticization of PVC, Polymer
[1] W. M. Thomas, International patent application, No. 49 (2008) 1440-1443.
PCT/GB92, GB Patent Application, No. 9125978.8.6, (1991).
27
Effects of tool geometry and process conditions on material flow

†
and strength of friction stir spot welded joints
HORIE Shohei*, SHINOZAKI Kenjin*, YAMAMOTO Motomichi*, KADOI Kota*,

NAKASHIN Hiroki*, and NORTH T. H.**
KEY WORDS: (FSSW) (Tool geometry) (Material Flow) (Strength) (Mg alloy)
1. Introduction since the stir zone is not grown up enough. However, when
FSSW has been employed in various industries and has the plunging depths from 0 mm to 0.3mm are applied,㻌
rapidly become one of the main processes for joining light when the tool shoulder completely contacts the surface of
materials. Strength of welded joints is a significant issue in upper sheet the rupture load indicates peak values. At this
FSSW researches. Though some reports are published the time, the fracture mode is transited to the thickness
which the key issue is optimization of tool geometry to direction. When further plunging is applied, which is over
obtain the high strength [1-2], the theoretical concept for 0.3 mm the rupture load decreases linearly with the
the tool design has not been established yet. In this study plunging despite the same fracture mode because of the
effects of tool geometry on strength of friction stir spot thinning of the upper sheet. As shown in Figure 2, same
welded joints were investigated in terms of the view of relations are seen using No. 2 and No. 4 tools. However,
material flow during FSSW. the rupture load of welded joints produced by No. 4 tool is
much higher than the other two tools.
2. Experimental Procedure 㻌㻌 Figure 3 shows the cross sectional macro images of the
The material used in this study was AZ31 with 1.6mm welded joints before and after cross tensile test. When No.
thickness. Figure 1 shows a schematic illustration of the 2 tool is used although width of stir zone is slightly bigger
tool geometries. No.1 is a conventional shape which has a than that No.1 tool is used, the unbonded interface is longer
flat shoulder with 10mm diameter and M4 threaded probe. than No. 1 tool. However, the angle formed by hooking and
No.2 has a concave shoulder with 7.5 degree to produce the interface between the upper sheet and the lower sheet is
inward material flow efficiently beneath the rotating sweep. Thus, the interface would not open when cross
shoulder. No.3 has a bigger shoulder with 15mm diameter tensile test is performed and rupture load is increased.
to increase heat input and be expected to make the stir zone When No. 3 tool is used pronounced hooking is formed and
bigger. No.4 tool has a combined shape of No.2 and No.3 tip of the interface between upper and lower sheet toward
tools to benefit from synergetic effects, and spiral slit is the probe keyhole. Thus, the interface is easily opened
fabricated on the shoulder to produce another material flow when the cross tensile test is carried out and rupture load is
beneath the tool shoulder. All tools are designed on the very weak. In direct contrast, when No. 4 tool is used a㻌
basis of material flow models proposed in previous much bigger stir zone is formed than other tools and
researches to produce the large or optimized bonding area rupture load is very high. Although the interface looks like
[3]. A constant plunging rate and dwell time were applied, a probe keyhole, propagation is in the through thickness
which were 2.5mm/s and 4s, respectively. Tool rotational direction. Spiral slit and concave taper on rotating shoulder
was varied from 1000rpm to 3000 rpm. The shoulder produce a strong inward flow. It is presumed that this
plunging depth below the upper sheet surface was varied material flow facilitates stir zone growth and bonding the
from -0.2 mm to 0.65 mm. Cross tension tests and Tensile interface between upper and lower sheet.
Shear tests were carried out according to the Japanese Figure 4 shows the relation between tensile shear load
Industrial Standard (JIS) Z3137 and JIS Z3136 respectively. and plunging depth when No. 2 and No. 4 tools, which
were confirmed increasing of rupture load in cross tensile
3. Results and Discussion test and No. 1 tool are used. In the case that No. 1 and No.
Figure 2 shows the relation between cross tensile load 4 tools are used, rupture load is increased with increasing
and plunging depth in using No.1, No.2 and No.4 tools. In plunging depth. Fracture mode transits from shear direction,
the case that No.1 tool is used, when the plunging depths which cut across the stir zone to mixed mode of thickness
under 0mm are applied the rupture load increases with the direction and zone direction at around 0.3mm plunging
plunging depth and the rupture pass traverses the stir zone depth. As in the case of cross tensile test, rupture road is
* Hiroshima University, Hiroshima, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** University of Toronto, MSE, Toronto, Canada Japan
28
Effects of tool geometry and process conditions on material flow and strength of friction stir spot welded joints
dramatically higher than other two tools in all plunging and lower sheets would be bonded like friction pressure
depths when No. 4 tool is used. As shown Fig. 4, width of welding. High strength joints are produced stably in every
stir zone is much larger than No. 1 and No. 2 tools. And rotational speed by using No. 4 tool. By comparison with
fracture mode is a mixed mode cutting across stir zone with the higher rotational condition using No. 3 and No. 4 tool,
thickness direction. Thus fracture load is dramatically it is presumed that tool slippage occurs at the contact
increased when No. 4 tool is used. interface between rotating shoulder and material. And
Figure 5 shows the relation between tensile shear load efficient material flow just beneath the rotating shoulder
and tool rotational speed when No. 1, No. 3 and No. 4 tools would not occur when No. 3 tool is used under higher
are used. When No. 1 tool is used fracture load increases rotational speed. However, No. 4 tool has a concave taper
with the tool rotational speed. Fracture mode is in the shear inside of the tool shoulder and spiral slit outside, material
direction at all rotation speeds. This means fracture load beneath tool shoulder is forced to transport inwards. Thus
depends on the width of the stir zone. It is well known that strong inward material flow is produced despite high
the growth of stir zone facilitates with increasing tool rotational condition using big size shoulder.
rotational speed during FSSW using general tool shape.
Thus fracture load increases with the tool rotational speed
when No. 1 tool is used. In direct contrast, fracture load
decreases with increasing tool rotational speed when No. 3
tool is used. When No. 3 tool is used under low rotation
condition a hook is not formed and the interface between
upper and lower sheets are bonded widely. Because
material flow around probe periphery does not occur
enough since heat generation is much lower than using
higher rotational condition. However, big size shoulder
produces efficient material flow beneath the rotating
shoulder. Furthermore axial force during FSSW is higher
when No. 3 tool is used. Thus the interface between upper
Fig. 3 Macro future of cross section and fracture pattern

made using No.1, No.2, No.3 and No.4 tool.
Rotational speed, plunging speed and dwell time
are 2250rpm, 2.5mm/s and 4s respectively.
Fig. 1 Geometry of FSSW tool.
Fig. 2 Relationship between plunging depth and Fig. 4 Relationship between plunging depth and tensile
tensile shear load of friction stir spot welded shear load of friction stir spot welded joint made
joint made using different tool geometries. using different tool geometries.
29
4. Conclusions
Novel tool design which is based on material flow models
during FSSW is proposed in this study. This tool is designed
to facilitate the inward material flow beneath a rotating
shoulder and succeeds in increasing both cross tensile load
and tensile shear load drastically.
References
[1] H. Badarinarayan, et al.: Effect of tool geometry on static
strength of friction stir spot-welded aluminum alloy, Int J Mach
Tools Manuf 49 (2009), pp. 142–148.
[2] Y. Tozaki, et al.: Effect of tool geometry on microstructure and
static strength in friction stir spot welded aluminum alloys, Int J
Mach Tools Manuf 47 (2007), pp. 2230–2236.
[3] S.Horie,et al.: Experimental investigation of Material Flow
Fig. 5 Relationship between rotational speed and tensile during Friction Stir Spot Welding, Science and Technology
shear load of friction stir spot welded joint made
using different tool geometries.
30
Study on the formation

mechanism of pore in the intersection of
†
VPPA and FSW
YU Yang *, LI Baotian *, JIANG Fan *, CHEN Shujun *
KEY WORDS: (VPPA) (FSW) (Porosity) (Oxide)
1. Introduction There is a high possibility that sound joints will be obtained

Aluminium alloys are finding increased use in aerospace, by either VPPA or FSW. However, only a limited number
transportation (automotive, shipbuilding) and chemistry of studies have been done on defects in the intersection of
industry due to their high strength-to-weight ratio, and VPPA and FSW. In this paper, several kinds of overlapping
remarkable ability to resist corrosion. The extensive welding seam were prepared, and defects in the overlapping
application of aluminium alloys promotes the development welding seam were detected. The mechanism of defects
of aluminium alloy welding technology; meanwhile the was further explored.
development of aluminium alloy welding technology
extends the application of aluminium alloy. 2. Experiment
Aluminum presents a high hydrogen solubility in the 㻌 The base metal used in this study was a 2219 aluminum
liquid and an important solubility gap between solid and alloy plate of 6 mm in thickness, whose chemical
liquid state. One of the major concerns during welding of compositions are listed in Table 1.
aluminum alloys is the presence of porosity in the weld Table 1 Chemical compositions (wt.%)
metal that can deteriorate mechanical properties, Al Cu Mn Fe Si
particularly tensile strength and elongation[1-3]. Bal. 6.43 0.31 0.30 0.20
Variable polarity plasma arc welding (VPPAW) and
Friction stir welding are two valuable welding processes for The plate was cut and machined into two kinds of
aluminum alloys. Compared with other arc welding rectangular welding samples: one is 400 mm in length and
processes, VPPAW can generate high weld quality and 200 mm in width; the other is 400 mm in length and 400
high productivity at relatively low cost. These attractive mm in width. After cleaned with acetone, two samples with
features are attributed mainly to a fully penetrated keyhole- dimension 400*200mm were longitudinally butt-welded
mode weld pool, inside which hydrogen cannot be trapped, using an FSW machine, and stir-in-plate welding was
and to the removal of tenacious oxide film on the performed on the middle of the 400*400 samples. Then
workpiece surface, which guarantees better fluidity of the bead-on-plate welding was carried out on the plate with the
metal in the weld pool[4]. Friction stir welding (FSW) is a butt-welded seam and plate with stir-in-plate welded seam
relatively new solid state joining process[5] that offers the by VPPA welding machine. Four kinds of overlapping
potential for joints with high fatigue strength, low joints were prepared. For the convenience, the sample with
preparation and little post-ZHOG GUHVVLQJ 2WKHU EHQH¿WV VPPA welded seam which is perpendicular to the butt-
include generally low defect populations (compared with welded FSW seam is named BW+; the sample with VPPA
fusion welding) and the ability to join dissimilar metals. welded seam in which the centerline is consistent with that
Joints without porosity can be produced by either VPPA of butted-welded FSW seam is named by BW-; the sample
or FSW. However complex structure can not be finished by with VPPA welded seam which is perpendicular to the stir-
one kind of welding process. Usually, space vehicle is in-plate welded FSW seam is named SIP+; and the sample
produced with the support of several kinds of welding with VPPA welded seam in which centerline is consistent
processes. with that of butted-welded FSW seam is named by SIP-.
The schematic of overlapping welding is shown in Fig. 1.
Visual and X-ray radiography inspections of the
overlapping joints were performed in order to reveal the
weld defects on the surfaces and in the inner zones of the
welded joint.
The configuration and size of the transverse tensile
specimens were prepared with reference to China National
Fig. 1 Overlapping welding specimens Standard (GB2625-89), as shown in Fig. 2. The room㻌㻌㻌

* Beijing University of Technology, Beijing, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
31
Study on the formation mechanism of pore in the intersection of VPPA and FSW
temperature tensile test was carried out at a crosshead

speed of 1 mm/min using a computer-controlled testing
machine and the tensile properties of each joint were
evaluated using three tensile specimens cut from the same
joint. After the tensile test, the fracture features of the joints
were analyzed by OM and SEM mentioned above.
Fig. 4 Macrostructures of as-welded FSW
4. Discussion
Fig. 2 Tension specimen Comparing the results of X-ray radiography inspections,
pores can be found in the overlapping seam in the form of
3. Results BW+, but there are no pores in the overlapping seam in the
㻌 Table 2 shows the results of X-ray radiography form of SIP+. The main difference between BW+ sample
inspections. and SIP sample is that there are two initial surfaces of the
BW+ sample. Conclusion that the oxide on the sample
Table 2 Results of X-ray radiography inspections surface leads to the formation of porosity in the intersection
BW+ BW- SIP+ SIP- of the BW+ sample can be drawn. With loosened structure,
the oxide can adsorb water vapor easily. The water vapor
defect Pores No pore No pore No pore
can react with the molten metal, and produce hydrogen in
the arc welding process.
Fracture surfaces of the tensile specimens are shown in Figure 5 is the enlarged picture of a tensile fracture, and
Fig. 3(a). There are a lot of circular shape pores located in it is obvious that some particles are located in some pores.
the neighborhood of fusion line at the root of the welding The particles can be identified as aluminium oxide by EDX.
seam. The pores can be identified as hydrogen pores due to Some fracture surfaces appeared as wave forms, as shown
their smooth inner surface. in Fig. 6, is identical with the fracture which tensile
Figure 3(b)show the enlarged fusion-zone of the tensile specimen bearing zigzag line [6]. Zigzag line is recently
fracture, and no pores but many dimples are observed. hypothesized to be due to entrapped oxide particles seeping
from the specimen surface during welding [7], which can
further confirm that the oxide is the source of hydrogen.
(a) macrostructure (b) enlarging of fusion zone

Fig. 3 Tensile fracture surface
Typical microstructure of the cross-section of FSW joints is

illustrated in Fig. 4. The micrograph was taken at the
retreating side of the welded joint. The micrographs shown Fig. 5 pores with particle
in Fig. 5 are for a specimen welded at welding speed of
180mm/min and tool rotational speed of 800 rpm. It is clear
that, beside the BM, the macrostructure of the FSW alloy
consists mainly of three distinct zRQHV W\SLFDOO\ L ¿QH
grained dynamically recrystallised zone DRZ, (ii) thermo-
mechanically affected zone (TMAZ) and (iii) heat-affected
zone (HAZ). The TMAZ experiences both temperature and
deformation during FSW and characterized by a highly
deformed structure. The HAZ is the zone that is believed to
be unaffected by any mechanical effects but only the
thermal effects caused by the frictional heat generated by
the shoulder and tool pin rotation. Fig. 6Zigzag fracture
Although VPPA welding owing special process to avoid the

formation of porosity, but if the hydrogen forms at the root
of molten pool where temperature is low, the molten metal
solid quickly. The hydrogen is trapped in the welding seam.
32
5. Conclusions [2] R. F. Ashton, and R. P.Wesley, Welding Journal. 54(1975).

When an arc welding seam meets with the FSW seam, 95-s to 98-s.
porosity is the usual defect in the intersection of above two [3] M. Katoh, Welding International (UK). 10(1996), 771–777
different welding seams. [4] A. C.Nunes, Welding Journal. 63(1984), 4, 27-s to 35-s.
[5] C.J. Dawes, W.M. Thomas, Welding Journal. 75 (1996), 41–
The entrapped oxide seeping from the specimen surface
45.
leads to the formation of porosity in the intersection of [6] H.J. Liu, Y.C. Chen and J.C. Feng, Scripta Materialia. 55
FSW with VPPA. (2006), 231–234
[7] Y. Sato, F. Yamashita, Y. Sugiura, S. Park, H. Kokawa,
References Scripta Mater. 50 (2004) 365–369.
[1] F. V. Lawrence, Jr. WRC Bulletin. 181(1973), PP. 1–23
33
†
Simulations of weld pool dynamics and theis visualization
NA Suck-Joo *, CHO Won-Ik * and CHO Dae-Won *
KEY WORDS: (Arc welding) (Laser welding) (Hybrid welding) (Fluid dynamics) (Animation)
㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 (Bead formation) (Alloy element mixing)
1. Introduction
Numerical simulations of weld pool dynamics in GMA
welding and laser-GMA hybrid welding can show
information of fluid flow characteristics and alloy element
mixing in detail. The necessary condition for the validity
of simulation results is, however, the accurate description
of complex welding phenomena occurring during heating,
melting, solidification and cooling. This paper introduces
effective ways to describe the heat flux distribution from
arc plasma to the base metal in GTA and GMA welding,
and the laser heat transfer through the surface of keyholes
with arbitrary shapes. The simulation result is visualized
by the animation technique and some meaningful Fig.1㻌 Arc heat flux and bead formation under various
snapshots and compared with the experimental one to shielding gas flow rates in GHTAW
verify the validity of the developed model. The whole
simulation model is then applied to GHTA welding in Figure 2 shows the arc light emissivity, which is the
vacuum, GMA welding of pipes and laser-GMA hybrid result of Abel inversion and a Gaussian fitted line for the
welding of thick plates to understand the weld pool front and side views in GMA pipe welding. To conduct
dynamics of various welding conditions. the Gaussian fitting, the effective radius should be
obtained by taking the integral of arc light emissivity.
2. Arc Welding: GHTAW and Pipe Welding
Previous simulations of arc welding processes
generally adopted the axis-symmetry arc heat flux model
[1]. These studies, however, do not consider the effect of
various conditions such as ambient pressure and joint
shape, which can deform the arc plasma characteristics. In
this study, the arc heat flux model was obtained from the
Abel inversion method [2], and applied for weld pool
㻌㻌
simulations to compare with the results of the generally (a) Front (b) Side
adopted axis-symmetric arc heat flux model in numerical Fig.2㻌 Result of Abel inversion of arc light intensity in
simulations of arc welding processes. 㻌㻌㻌㻌 GMA㻌 pipe welding
Figure 1 shows the arc heat flux distributions
measured by Abel inversion of CCD images of arc light Figure 3 shows the experiment and simulation results
intensity under various shielding gas flow rates in for the different welding positions. Due to the gravity
GHTAW (gas hollow tungsten arc welding), the effect, molten pool behavior affects the variable surface
corresponding characteristic weld pool flows and the profile shapes for different welding positions. In flat and
resulting bead shapes. overhead positions, the molten pool circulated
It is clearly visible that the increase of shielding gas counterclockwise, which makes a uniform bead along the
flow rate results in the intensified and concentrated arc welding direction.
heat flux, which stimulates the strong downward flow
along the center axis. Accordingly the simulated and In the vertical position, however, the molten pool
experimental bead shapes are in a very good agreement cannot circulate well because the gravity force moves the
for different conditions. molten pool to the rear direction, which makes an unstable
bead shape like humping.
* Department of Mechanical Engineering,KAIST, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
㻌 Daejeon,Korea Japan
34
Simulations of weld pool dynamics and its visualization
In particular, the region is rapidly expanded by the

excessive recoil pressure, if the reflected laser beam is
concentrated at the rear part of the keyhole surrounded by
the molten metal. For this reason, complex flows with
relatively high velocity are observed near the keyhole and
can make the keyhole unstable. Meanwhile, it is observed
that clockwise-rotating vortices form a quasi-steady state
(a)Flat position (b)Vertical position flow pattern in the wide molten region located away from
the keyhole. It can be inferred that these vortices are
Fig.3 Result of simulation and experiment for different
driven by the strong flow at the keyhole. Because the
welding positions
vortices extending a relatively wide range of the molten
3. Keyhole Welding: Laser and Laser-Arc Hybrid pool not only have high Cr content but also rotate in the
Welding same direction, they help mix Cr in the molten pool and
The three-dimensional molten pool formed in laser thus Cr is distributed uniformly in the wide molten region.
and laser-arc hybrid welding is analyzed by numerical However, the outer clockwise-rotating vortex with
simulation. All mathematical models for laser and arc relatively high or low Cr content passes through around
welding are combined together without the interaction the solid-liquid interface, and thus Cr can be entrapped
between the arc and laser heat sources. and make a pattern like the teeth of a comb. For the region
The laser model is modified to consider the optical around the keyhole bottom, strong up-and-back flow
geometry of the laser system, and an additional arises and pushes out the flow having high content of
conservation equation having the form of a general scalar alloying elements because of the fast cooling rate and
advection equation is used for simulating the alloy small accompanying molten region. Therefore, low
element distributions [3]. content of alloying elements exists in the keyhole bottom.
Figure 4 shows the temperature and Cr distributions
with the flow patterns in the longitudinal cross sections 4. Conclusions
during hybrid welding. In the figures, maximum
The conclusions of this study can be summarized as
temperature and content values of Cr are set to 1768K and
follows.
8%, respectively. At the keyhole front, where a high
(1) With a CCD camera and Abel inversion method, it is
intensity laser beam is directly irradiated, the material is possible to calculate the effective radius of arc
removed without a thin molten layer, a process that plasma in different arc welding processes.
resembles the laser cutting and drilling process. The laser
beam reflected at the keyhole front reaches the other (2) The arc heat flux models obtained as above could be
position of the keyhole wall and is then absorbed. As effectively applied to the numerical simulations of
shown in the figures, not only can the incident beam reach weld pool in GHTAW and GMA V-groove pipe
welding. The simulated and experimental results of
the keyhole wall easily, but also the reflected beam can be
bead shapes are in good agreement to show a validity
collected around a specific point, if the shape of the
of the proposed models.
keyhole is not smooth but rather has a bulge.
(3) Although the theoretical İ value of 0.08, rather than
the numerically compensated İ value of 0.2, is used
in the simplified Fresnel’s reflection model for the
steel and CO2 laser, the bead shape of laser-arc
hybrid welding could be predicted very accurately by
0.6s numerical simulations.
(4) For the alloying elements in laser-GMA hybrid
welding, a relatively low content of alloying elements
is observed in the low molten region, because the
1.2s flow with a large content of alloying element is
pushed out by the excessive flow at the rear part of
the keyhole.
1.8s Acknowledgement
(a) Temperature (b) Time (c) Cr profile Support by POSCO, the Brain Korea 21 project, and a
Mid-career Researcher Program through NRF grant
Fig.4 Simulation results in longitudinal cross sections funded by the MEST (No. 2010-0027749) is gratefully
during hybrid welding acknowledged.
35
References [3] W.-I.Cho, S.-J.Na, M.-H.Cho and J.-S.Lee: Comput. Mat.

[1]J.H. Cho and S.J. Na: Weld. Jourmal, 88(2009), pp.35s-43s. Sci., 49(2010), pp.792-800
[2] Y.T. Cho and S.J. Na: Meas. Sci. Technol. 16 (2005),
pp.878-884.
36
Numerical simulation of laser welding processes with CIP finite

†
volume method
YAMASHITA Susumu*, YONEMOTO Yukihiro*, YAMADA Tomonori*, KUNUGI

Tomoaki**and MURAMATSU Toshiharu*
KEY WORDS: (Laser welding simulation) (CIP finite volume method) (Multiphase flow) (One fluid model) 㻌
㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 (Marangoni convection)
1. Introduction and gas phases, we employ the one-fluid numerical model.

Quantitative evaluation and controlling the residual In the model, effective flux on each surface is evaluated by
stress which is induced by laser welding is one of the the advection equation of the VOF (volume of fluid)
important subjects for a plant life extension of FBRs (Fast function, ȭ,
Breeder Reactors) and the guarantee of the reliability of the wIk w (uiIk ) wui
repair domain. Numerical simulation is an effective tool for Ik . (2)
deep understanding of their phenomena and it needs to have
wt wxi wxi
high accuracy, robustness and reliability. Recently, in order Based on the local values of ȭ, the appropriate properties
to satisfy those requirements, we have developed the laser and variables are assigned to each control volume within
welding simulation model using some advanced numerical the computational domain. If Y denotes the generic fluid
models; surface capturing scheme, THINC[1] and spatial property (e.g. density, viscosity, specific heat, etc.) the
discretization scheme, VSIAM3[2]. We have conducted corresponding value in each cell is given by
three-dimensional simulations of the laser welding Y (I ) YsI s Y"I " Yg (1 I s I " ), (3)
processes using physical properties of the pure aluminum
and the stress jump across the interface[3], [4]. The where subscripts s, ε and g represent solid, liquid and gas
behavior of the welding pool is qualitatively the same as the phase, respectively and ȭ takes 0 to 1.
experimental one. It is concluded that the present numerical It is known in fact that the expression for the stress jump F i ,
model can be expected as a practical tool to simulate laser across the interface is given by
dV
welding processes.
Fi VNni I ij ni n j Ti (4)
2. Governing Equations dT
A welding pool which is induced by a laser irradiation where n i is the unit vector perpendicular to the fluid/fluid
can be treated as a fluid so that the governing equations can interface, ț㻌 is the curvature, ı is the surface tension
be described by equation of continuity, Navier-Stokes coefficient and I ij is the identity matrix,
equation and energy equation. Assuming the wI / wxi wni
incompressible fluid, those equations can be expressed as
ni ,N . (5)
| wI / wxi | wxi
wu i The second term of the right hand side in the Eq.(4) is the
0,
wxi contribution related to surface tension gradients along the
interface (Marangoni stress).
wu i wu 1 wp 1 w
uj i 2PDij Fi , (1)
wt wx j U wxi U wx j 3. Numerical configuration
Figure 1 represents the computational domain of the
wT wT 1 w § wT · 1 laser welding simulation. The length of x, y and z are 2 cm
ui Ö ¸¸ Q, (the thickness of the aluminum solid plate 1 cm). In this
wt wxi UCQ wxi ¨© wxi ¹ UCQ study, 808080 grid points for each direction are used.
where u i , F i , T, ȡ, ȝ, C Ȟ , Ȝ, Q andȭ represent the The laser heating starts from far left of the plate and is
velocity vector, external force (gravity, surface tension scanning on the aluminum plate with constant velocity, 2
force, etc.) temperature, density, viscosity, specific heat, cm/s. The diameter of the laser spot and the total laser
thermal conductivity and heat source. power are 2 mm and 300W, respectively. The energy input
In order to express the multiphase flows, e.g. solid, liquid from the laser light was modeled as a surface heat flux.
* Japan Atomic Energy Agency, Fukui, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Kyoto University, Kyoto, Japan Japan
37
Numerical simulation of laser welding processes with CIP finite volume method
Currently, spatial intensity of the heat flux on the plate was

distributed as a Gaussian laser-beam distribution and the
profile for the depth direction, Bouguer-Lambert-Beer
law[5-7] was used.
We used a FAVOR (Fractional Area/Volume Obstacle

Representative) method[8] as the expression of the solid
phase and the temperature recovering method is used as the
(a) t = 0.125 s.
Fig.1㻌 Schematic diagram of the laser welding

㻌㻌㻌㻌 simulation. (b) t = 0.33 s.
phase change model. Boundary conditions of the velocity,

pressure and temperature are no-slip, Neumann and
constant temperature conditions, respectively.
The resulting system of pressure equations was solved
by means of a Krylov-Subspace solver. For this purpose the
AMG-BiCGSTAB library was chosen.
We carried out the simulation of the laser welding in air
(combustion and evaporation were not considered). The
physical properties are shown in Table.1.

Figure 2(a)-(d) shows the snap shots of the simulation (c) t = 1.0 s.
of the laser welding on the aluminum plate. At the
irradiation of the laser beam, the temperature increases and,
because the temperature coefficient of the surface tension is
negative for most materials, the surface tension increases
along a line from the irradiation point to the edge of the
melt pool. Thus, as shown in Fig.2(a) and (b), in the
vicinity of the solid/liquid surface swells and the irradiation
point sinks in. After some time proceeding, in Fig. 2(c) and
(d), the bead was formed at the back of the melting pool.
These results indicate that the present numerical model can
be applied to practical laser welding processes.
Table 1 Physical properties of the molten aluminum.

Density [kg/m3] 2357 (d) t = 1.51 s.
Viscosity [Pa s] 1.178e-3 Fig.2㻌 The three-dimensional views of the surface of the 㻌
Thermal conductivity [W/m/K] 93 㻌㻌㻌㻌 laser welding. The blue and red are indicating the
Specific ratio [J/kg/K] 1090 㻌㻌㻌㻌㻌 low and high temperature regions.
Surface tension coefficient [N/m] 0.9
Melting point [K] 933
dıdT [N/m/K] -3.5e-4
38
We carried out the laser welding simulation using a one [1] K. Yokoi: J. Comput. Phys. 226 (2007), pp.1985-2002.
fluid model by CIP finite volume method. Although the [2] F. Xiao: J. Comput. Phys. 195 (2004), pp.629-654.
model considered only thermocapillary and surface tension [3] M. S. Gross, I. Black and W. H. Muller: J. Phys. D: Appl.
Phys.36(2003), pp.929-938.
force as a surface force models, the representative behavior
[4] M. Lappa: CMC, vol.2, no.1 (2005), pp.51-64.
of the laser welding was obtained. Therefore, it is [5] M. Von Allmen: Springer-Verlag, Berlin (1987).
concluded that the model can be applied to practical laser [6] J. F. Ready: Academic Press, New York (1971).
welding problems. In order to investigate the details of the [7] S. I. Anisimov, Ya. A. Imas, G. S. Romanov and Yu. V.
flow of the inside the molten pool, the high resolution Khodyko: National Technical Information Services (1971).
simulation is indispensable. So we parallelized the model [8] W. Hirt et al: 4th Int. Conf. Washington DC (1985).
by means of MPI. After some improvement the numerical
model, massively-parallel computers with more than one
hundred CPUs will be used. Thus, in near the future, details
of the laser welding processes will be revealed and it will
contribute to controlling the residual stress on laser welding
processes.
39
Modelling of the electron beam welding process applied to aircraft

†
engine components
LAURENT D’Alvise*
KEY WORDS: (Welding) (Simulation) (Modelling) (Morfeo) (Software) (Parallel)
1. Introduction ence frame.

A thermo-mechanical model of the electron beam The thermal conductivity and heat capacity are con-
welding process has been developed in Morfeo (Cenaero sidered functions of the temperature. The radiation heat
welding software). It allows predicting the temperature loss and heat transfer with the support are also taken into
evolution, the distortions and residual stresses at the end account. In this welding process, there is no free convec-
of the process. The welding of a blade on an aero engine tion because it takes place in a high vacuum environment,
stator has been studied. around 10-6 bar, to avoid the electron beam scattering
The electron beam welding (EBW) process is exten- with the air.
sively used for assembling titanium and other high In order to avoid a numerical instability, known has
strength components in the aircraft engine industry. For the thermal shock problem, a lumped heat capacity ma-
such applications, it is important to predict distortions trix is used, as suggested in [3]. This numerical instability
and residual stresses after the welding process. appears under some particular conditions when the finite
A transient numerical model of the electron beam element method is used to solve the transient thermal
welding process has been developed in the finite element problem. It has been found that without this lumping
code Morfeo. The modelling of the thermo-mechanical method, the mesh in the region close to the welding zone
problem allows predicting the level of the residual should be highly refined to prevent numerical instabilities,
stresses and distortions at the end of the process. leading to a prohibitive computation time and memory
This numerical model will enable the optimisation of cost on industrial applications.
the welding process in order to improve the design with- Once the temperatures are known, the resulting ther-
out having to perform expensive experimental work. mal and residual stresses are computed by a mechanical
model. In Morfeo, the coupling between the thermal and
2. Numerical model mechanical calculation is staggered. The mechanical
The main objective in the modelling of the welding properties of the material are considered function of the
process is the prediction of the distortions and the ther- temperature.
mal and residual stresses rather than solving the laws of It is very important to emphasise that the greatest influ-
the fluid mechanics in the weld pool and the keyhole. ence on the thermal and residual stresses is due to the
Therefore, a phenomenological approach, based on the variation of the yield strength as a function of the tem-
utilisation of a power density distribution is used to perature [1].
model the welding beam.
In the thermal model, the 3D equivalent heat source is 3. Applications
modelled using a superposition of an ellipsoidal and Figure 1 shows the stator of the compressor stage of
conical shape heat source with Gaussian power density an aircraft engine, made of a titanium alloy. The blades
distribution in order to reproduce the shape of the fusion are assembled on the stator using the electron beam weld-
zone [1, 2]. ing method.
Because the residual stresses are directly related to the The welding of a blade on a section of the stator (il-
high temperature variation, its important to have a good lustrated Fig. 2) has been studied. The welding velocity
representation of the heat flux produced by the electron is assumed constant along the trajectory. The welding
beam. The parameters of the heat source are chosen such trajectory is defined directly from the CAD geometry.
that the simulation results match experimentally meas- Therefore, complex welding paths can be easily defined.
ured temperatures and weld pool shape profile. Figure 3 shows the mesh, generated with the Sim-
Given that the heat flux is defined in a local frame metrix library, used in the welding simulation. The mesh
moving along the welding trajectory, an axes change has has been refined in the welding zone where high thermal
been implemented to get the heat flux values in the refer- and stress gradients are encountered. Figure 4 shows the
temperature computed by Morfeo during the EBW
* Virtual Manufacturing Group, Cenaero Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
40
Modelling of the electron beam welding process applied to aircraft engine components
Fig. 4 Temperature field during the welding

process.
process. The simulation results still need to be validated

Fig. 1 Stator of the compressor stage of an with experimental measurements.
aircraft engine assembled by a EBW technique. An inverse analysis will be performed to determine
accurately the heat source parameters from temperature
measurements on samples.
References
[1] P. Ferro, A. Zambon and F. Bonollo, Investigation of elec-
tron-beam welding in wrought Inconel 706 experimental
and numerical analysis, Materials Science and Engineering
A, vol. 392, pp. 94-105, 2005.
[2] A. Lundbäck, Finite element modelling and simulation of
welding of aerospace components, 2003, Licentiate thesis,
Lulea University, Sweden.
[3] R.H. Wagoner and J.-L. Chenot, Metal forming analysis,
Cambridge University Press, UK, 2001
Fig. 2 Section of the stator.
Fig. 3 Mesh of the stator section.
41
Visualization of fluid flow and heat transfer in resistance spot weld

†
nugget
LI Yongbing *, SHEN Qi and CHEN Guanlong
KEY WORDS: (Resistance Spot Welding) (fluid Flow) (Heat Transfer) (Electromagnetic Stirring) (Modeling)
(Magnetofluidodynamics)
1. Introduction rotational motion in four quarters, and in each quarter of the

Resistance spot welding (RSW) process has been widely nugget, the molten metal flows out of the nugget along the
used in sheet metal joining, especially in automotive BIW faying surface and flows back into the nugget along the
(body in white) assembly. During RSW, a large welding edge of the nugget. Thus, a small dead zone is formed at the
current flows through electrode caps and sheet metals. The center of the nugget. Moreover, the maximum flow velocity
current not only produces resistance heat which can melt appears at the faying surface away from the weld nugget.
the sheet metal to form a nugget, but also induces a large The flow of the molten metal will definitely affect the heat
magnetic field to stir molten metal in the nugget. transfer behavior in the nugget. For traditional models,
Traditional electro-thermal models have been widely used which can not consider the fluid flow in the nugget, the
to predict the nugget growth and heat transfer during RSW, temperature gradient consists of a series of concentric
however, these models could not reveal forced fluid flow ellipses and is large in any direction because of the
and its effect on heat transfer in the nugget. There is still a consistent cooling, as shown in Fig. 2. However, for the
lack of in-depth understanding of the physical behavior in model with magnetic field considered, the strong flow
the weld nugget. substantially disturbs the regular thermal conduction and
In this paper, the fluid flow and heat transfer in RSW mixes the hot and cold metal through mechanical stirring,
are a magneto-hydro-dynamic (MHD) finite element (FE) and greatly reduces the temperature gradient in the nugget,
model, which couples the electric field, thermal field, flow especially in the width direction, as shown in Fig. 3.
field, magnetic field, and is used to investigate the
electromagnetic phenomena in RSW and its effects on the (a)
nugget formation.
2. Numerical Model
A standard RWMA CLASS II electrode (MPE-25Z
CMW® 328) with a flat end surface was utilized in this
work. The material to be welded was 1.6mm thick mild
steel sheet, the welding current was 10,200 ampere, the
welding time was 12 cycles (0.2 s), the ambient temperature
was 21ć, and the temperature of cooling water was 17.8ć.
In order to reduce the complexity of the coupled multi-
physics process, the molten metal in the nugget was
assumed to be incompressible, viscous, laminar, and with
Newtonian fluid. Gravity’s effect on fluid flow was ignored (b)
[1]. The electromagnetic field was viewed as quasi-stable
for low-frequency welding current [2, 3].
The governing equations, boundary conditions,
material models and numerical method are given and
validated in our previous papers [4, 5].
ANSYS/Multiphysics and its parametric design language
were used to realize the coupling of the electric, magnetic,
thermal and flow fields.

Fig. 1 Calculated flow field in the nugget. The unit is m/s.
Figure 1 showed the flow field in the nugget at the
(a) overall view; (b) close-up view of the first quarter.
end of welding cycles. Obviously, the liquid metal makes

* Shanghai Key Laboratory of Digital Autobody Engineering, 㻌 Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Shanghai Jiao Tong University, Shanghai, P.R. China. Japan
42
Visualization of fluid flow and heat transfer in resistance spot weld nugget
0.00 0.05 0.10 0.15 0.20 0.25 0.30

2000 2000
1800 1800
1600 1600
1400 1400
Temperature/oC
1200 1200
1000 Without magnetic field 1000
With magnetic field
800 800
600 600
400 400
200 200
Fig. 2 Calculated nugget with traditional electro-thermal 0 0
model. 0.00 0.05 0.10 0.15 0.20 0.25 0.30
Welding time/s
㻌㻌 Figure 4 showed the evolution of maximum temperature

Fig. 4 This unit is maximum temperature evolutions for
in the nugget throughout the welding process. Obviously,
both kinds of models.
the maximum temperature evolution below the liquidus is
totally the same. Once there is molten metal in the nugget,
4. Conclusions
temperature differences will appear. For traditional models,
A multi-physics FE model is used to model the
the maximum temperature increases almost linearly with
electromagnetic phenomena in RSW. Researches showed
time, however, for the model with magnetic field
that the magnetic force field, which is produced by the
considered, after about 0.18s, the maximum temperature
welding current and the induced magnetic field, is very
does not increase obviously and only makes slight
regular, and causes the molten metal in the nugget to make
fluctuations with the alternating welding current.
regular flow in four cores at high velocity. The flow
dramatically changes the heat transfer in the weld nugget,
and results in a different temperature gradient in the nugget,
which will surely affect the crystallization process of the
liquid nugget.
Acknowledgement
This research is supported by National Natural Science
Foundation of China (Grant No. 50705059)
References
[1] J.A. Khan, L.J. Xu, Y.J. Chao, and Kirkland Broach:
Numerical Heat Transfer Part A, 37 (2000), pp. 425-446
[2]Wang Q., Li G.D.: Basic Theory of Electromagnetic, Beijing,
Fig. 3 Calculated nugget with the MHD model. Science Publishing House (1998)
[3] Jia R.G. and Xue Q.Z.: Electromagnetics, Beijing, Higher
Education Publishing House (2003)
[4] Y.B. Li, Z.Q. Lin, S.J. Hu and G.L. ChenO: Journal of
Applied Physics, 101 (2007), pp. 053506
[5] Li, Y.B., Lin, Z.Q., Lai, X.M., Chen, G.L., Zhang, K.: Science
China Technological Sciences, 53 (2010), pp. 1271-1277
43
Development of welding method for wide gap lap joint of steel sheet
†
using laser welding with hot-wire
YAMAMOTO Motomichi*, SHINOZAKI Kenji*, KADOI Kota*, FUJITA Daigo*,

INOUE Takeshi*, FUKAHORI Mitsugu** and KITAHARA Yoichiro**
KEY WORDS: (Hot-wire) (Laser welding) (Wide gap) (Lap joint) (Steel sheet)
1. Introduction which make the molten pool having a little larger width
In recent years, high strength / ultra-high strength steel than the filler wire diameter, 1.5mm for the spot
sheets are widely used for an automobile body since the diameter and 1.5 m/min for the welding speed in this
demand to reduce automobile body weight and energy study.
consumption is increasing rapidly, moreover lap joints of (2) The adequate wire feeding position and angle which are
high strength / ultra-high strength steel sheets by using laser the anterior region of the molten pool created posterior
welding for body construction is investigated to improve to the penetrated hole, 3mm for the feeding position
the body stiffness. However it is difficult to predict and IURPWKH ODVHU VSRW FHQWHU DQG Û IRU WKH ZLUH IHHGLQJ
control precisely springback behavior during press forming angle in this study.
of high strength / ultra-high strength steel sheets, then a (3) The adequate wire current which makes wire melting in
large gap between lapped sheets is created. In general, laser the region from the upper sheet surface to the gap
welding has only small gap tolerance and the laser welding between the lapped sheets, 102 ~ 116 A in this study.
speed with a filler wire to fill the gap must decrease. In this
study, the new laser welding process, which has a high Table 1 Welding conditions.
welding speed with feeding a filler wire and large gap
tolerance, is proposed and investigated by combining laser
welding and the hot-wire system which has the ability to
control filler wire melting independently from the main heat
input.
2. Experimental procedure
The in-situ observation was carried out using a high-
980 MPa class steel sheets (JIS-G3135-SPFCY, t: 1 speed camera to investigate filler wire melting phenomena
mm) and a 590 MPa class filler wire (JIS-Z3321 YGW23, I and weld bead creation phenomenon during welding. The
1.2 mm) were used. 200 mm long and 50 mm wide observation and evaluation of the bead surface and the
specimens were used for basic investigation, and 220 cross section, and the tensile test were performed after
mm long and 100 mm wide specimens with a 30 mm lapped welding.
region were used for tensile tests. A gap between lapped
sheets was fixed as 1 mm by inserting shim tapes. The weld 3. Result and discussion
bead length was 180 mm and tensile specimens having 30
mm width were cut out in the above welded lapped sheets. Figure 1 shows the high-speed image output during hot-
Table 1 shows the welding conditions. A 3kW fiber wire laser lap welding under the optimum welding
laser, a laser head with a 400 mm focal length and a hot- condition. Figure 2 shows the schematic illustration of
wire heating system produced by Bab-Hitachi Industrial Co. welding phenomenon during developed hot-wire laser lap
were used. The welding speed, the laser power, the filler welding. A penetrated hole initiated and weld metal could
wire feeding speed and the laser irradiation angle were not fill the hole during laser welding without filler wire,
IL[HG DV PPLQ N: PPLQ DQG Û UHVSHFWLYHO\ then the sound bead and joint could not be created. The
The laser spot diameter, the wire feeding angle, the wire developed hot-wire laser welding method can make stable
feeding position and the wire current were changed as wire feeding to fill the hole created by laser irradiation, and
experimental parameters. Filler wire was fed from then the sound joint with a 1 mm gap could be created by
backwards into a welding region. the proposed welding method. The following conditions are
necessary to make stable filler wire feeding and the sound
(1) The adequate laser spot diameter and the welding speed joint.
** Mazda Motor Corporation, Hiroshima, Japan Japan
44
Development of welding method for wide gap lap joint of steel sheet using laser welding with hot-wire
Figure 5 shows the tensile shear test result when the

wire current is varied from 102 A to 120 A. The laser spot
GLDPHWHU LV PP WKH ZLUH IHHGLQJ DQJOH LV Û and the
wire feeding position is 3 mm based on the above
investigations. The fracture path is in the base metal or the
Fig.1 High-speed image during welding (optimum welding). boundary between the base metal and the weld metal since
the welded joint produced using the proposed hot-wire laser
welding method has no serious defect in it. It is clear from
the figure that the stable tensile shear strength can be
obtained in the optimum wire current region.
Fig.2 Schematic illustration of hot-wire laser welding.
Figure 3 shows the cross-sections when the laser spot

GLDPHWHULVPPWKHZLUHIHHGLQJDQJOHLVÛWKHZLUH
feeding position is 3 mm and the wire current is varied.
When the wire current was too low (under 100 A in this
Fig.4 Effect of wire feeding angle on optimum wire current.
study), the lower sheet melting was unstable, then a hole
defect on the upper sheet initiated or filler wire penetrated
into the lower sheet. When the wire current was high (118 ~
120 A in this study), filler wire melted at the upper surface
of the upper sheet, then the excess weld metal was formed
but a serious defect was not created in the weld bead. When
the wire current was too high (over 120 A in this study),
filler wire was melted down before its tip reached the upper
sheet surface, then the sound bead was not created. When
the wire current was adequate (102 ~ 116 A in this study),
stable wire melting was achieved and the sound bead with
adequate cross-section and surface appearance could be
created.
Fig.5 Tensile shear strength of lap welded joints.
4. Conclusions
The hot-wire laser welding method was proposed for the
Fig.3 Cross-sections when wire current is varied. lap joint of the high tensile / ultra-high tensile strength
sheets with a wide gap, and its welding phenomenon was
Figure 4 shows the effect of the wire feeding angle on investigated precisely by using a high-speed camera, then
the optimum wire current. When the wire feeding angle the optimum welding conditions were obtained in this study.
EHFDPH WRR ORZ Û DQG Û LQ WKLV VWXG\ ILOOHU ZLUH The obtained conclusions are as follows.
touched the upper sheet surface at the back of the molten (1) The hot-wire laser system makes the penetrated hole
pool, then stable wire feeding could not be performed. and the molten pool by laser irradiation firstly, and then
When the wire IHHGLQJ DQJOH ZDV WRR KLJK Û LQ WKLV filler wire heated up by energization fills the penetrated
study), the filler wire tip melted down frequently since the hole in the proposed hot-wire laser lap welding method.
reflected laser beam irradiated unsteadily on its surface. The optimum conditions for the 1 mm gap are 1.5mm of
:KHQWKHZLUHIHHGLQJDQJOHZDVÛLQWKLVVWXG\WKHILOOHU the spot diameter, 3 mm of the wire feeding position,
wire tip touched stably the molten pool posterior to the Û RI WKH ZLUH IHHGLQJ DQJOH DQG a $ RI WKH
penetrated hole, then the optimum wire current region wire current for 3kW of laser power, 1.5 m/min of the
became wider. welding speed, 3.8 m/min of the wire feeding speed, 1
45
mm of the base sheet thickness and 1.2 mm of the filler upper sheet surface to the gap between the lapped sheets
wire diameter. are necessary for the stable welding phenomenon and
(2) The laser spot diameter and the welding speed which sound bead creation.
make the molten pool having a little larger width than (3) The stable and high tensile shear strength (500 ~ 600
the filler wire diameter, the wire feeding position and MPa) can be obtained over the wide wire current region
angle which is the anterior region of the molten pool (102 ~ 120 A) using the optimum welding conditions
created posterior to the penetrated hole, and the wire based on the above investigation.
current which makes wire melting in the region from the
46
Development of a high-efficiency / high-quality hot-wire laser fillet

†
welding process
KADOI Kota*, SHINOZAKI Kenji*, YAMAMOTO Motomichi*, TAKAYANAGI Daisuke*,

NISHIMOTO Akihiro*, OWAKI Katsura** and INOSE Kotaro***
KEY WORDS: (Hot wire) (Fillet welding) (Laser welding) (High efficiency)
1. Introduction traveling RQH,QDGGLWLRQWKHODVHUKHDGZDVDOVROHDQHGÛ

The GMA welding process has been widely used for to the traveling direction. Filler wire was fed into the
fillet welding because of its convenient and economical backward part of the laser irradiated area toward the
efficient advantages compared with other welding processes. welding direction.
However, the process conditions for high speed and high In-situ observation was carried out using a high speed
deposition rate often leads to defects like undercut etc. and camera to investigate the melting phenomena of the base
increase the deformation amount due to excessive heat material and the wire during welding. As quantitative
input. Laser and laser-arc hybrid welding are the promising evaluation, throat thickness and leg length were measured
processes to achieve the high welding speed and the low from the cross section of each obtained sample. In order to
deformation. However, to apply laser welding process to characterize the property of the welded joint,
fillet welding requires a high power source for full microstructural analysis and mechanical tests were carried
penetration welds. In addition, it is also necessary to have out.
high positional accuracy and the addition of filler metals for
stable bead formation. It is hard to control the melting 3. Result and discussion
phenomenon of the filler stably since both the filler and the Firstly, we focused on the clarification of the influencing
base material are heated by the laser. On the other hand, in factors on the melting phenomenon of filler wire. Wire
the case of laser-arc hybrid welding, it is difficult to prevent current, wire feeding position (distance from laser center)
forming defects caused by arc phenomenon. and wire feeding angle were applied as the experimental
The aim of this work is to develop the hot-wire laser factors. Figure 1 shows the images taken by a high speed
welding process which has both advantages of high camera on each wire current. 110 A of wire current
efficiency (high deposition rate, high speed etc.) and high indicates the stable melting of filler wire. In the case of the
quality (low heat input and deformation). This process lower current, the wire can reach the molten pool bottom
combines a laser and hot-wire system in which the filler because of the heating insufficiency. On the other hand, the
wire is melted by current heating. Thus, each melting of higher current induces the meltdown of the wire due to the
filler wire and the base material can be controlled excessive heat input. Thus, the adequate wire current value
independently. In this study, influence of welding is required for the stable melting.
conditions on melting phenomena was investigated using an Table 1 Chemical compositions of used materials.
䠯䡅䠩䡊䠬䠯䠟䡑䠝䡈䠰䡅+䠶䡎
in-situ monitoring system using a high speed camera. Cross C
SS400 䠘0.16 䠘0.17 䠘0.73 䠘0.016 䠘0.006 - - -
sections and mechanical properties were evaluated as the YGW11 0.04 0.68 1.55 0.014 0.013 0.03 䠘0.01 0.23
characterization of the welded joint. Table 2 Welding conditions.
Mild steel plate (SS400, thickness: 9 mm) and filler
wire (JIA Z3321 YGW, I 1.4 mm) were used. Table 1
shows the chemical compositions of used materials.
Table 2 indicates the welding conditions. The
conditions relating with laser and filler wire were changed
as experimental parameters. A fiber laser was used as a heat The high speed camera images for each of the wire
source. The laser power and the welding speed were fixed. feeding distances forming the laser spot are indicated in Fig.
Spot diameters of laser were controlled by the distance 2. The stable melting can be confirmed if the fire is fed into
from the focal length of a laser head. A laser head and a 2 mm of the position from the spot center. However, the
wire torch were leaned Û WR WKH vertical direction of the filler wire is melted before touching the base material due
** IHI Inspection & Instrument, Kanagawa, Japan Japan
*** IHI Corporation, Kanagawa, Japan
47
Development of a high-efficiency / high-quality hot-wire laser fillet welding process
Spot diameter: 7.5 mm, Wire feeding position: 2 mm,

Wire feeding angle : 55 °, Wire feeding position: 1.5mm,
Wire feeding speed: 1.8 m/min, Wire feeding angle: 55° Wire current : 84-122 A, Wire feeding speed: 1.1-2.4
m/min
Fig. 1 High speed images on each wire current. Fig. 4 Cross sections of weld bead on each spot diameter.
Spot diameter : 7.5mm, Wire feeding angle : 55 °
to the direct irradiation of laser, when the wire is introduced Wire feeding position: 1.5mm, Wire current :
at the center of the laser spot. On the other hand, the wire is 0~149A
not able to be inserted into the molten pool for more than 3
mm of wire feeding position. These result means that the
filler wire should be introduced into the molten pool
backward without the laser irradiation
In addition, we also investigated the wire melting
phenomena as the function of the wire feeding angle. In the
FDVH RI DQG Û RI WKH IHHGLQJ DQJOH WKH FRQWLQXRXV Fig. 5 Cross sections of weld bead
feeding and the stable melting of filler wire were obtained. on various wire feeding speeds.
+RZHYHU Û RI WKH IHHGLQJ DQJOH led to form the poor
geometry of the bead since the wire tends to touch the solid Regardless of the filler wire addition, the length increases
part at the backward part of the molten pool due to the wire with increasing spot diameter. Besides, those values of no
softening by heating. wire samples are smaller than those of the wire added ones.
As the second step, the phenomenon of bead formation It can be assumed that this is caused by the reflection of the
was evaluated. Figure 3 shows the change of average leg laser beam. The laser beam has a great tendency to reflect
length with spot diameter of laser. Average leg length was on the molten pool surface due to high optical reflectivity of
obtained from both the lengths of vertical (L 1 ) and liquid metal. Thus, the reflected beam contributes to
horizontal (L 2 ). The broken line indicates the laser melting of the base material since the beam irradiates the
irradiated length calculated from the spot diameter. surroundings of the distended geometry of the molten pool.
Figure 4 indicates cross sections of the beads welded
Spot diameter: 7.5 mm, Wire current: 110 A, under identical condition shown in Fig. 3. In the case of 3
Wire feeding speed: 1.8 m/min, Wire feeding angle: 55° mm of the spot diameter, the penetration is deeper
compared with another samples because of the high energy
density. If we apply the laser spot diameter which is more
than 4.5 mm, the dilutions of the base materials are quite
low. In addition, defects like overlaps and undercut at the
welding toe never form in any spot diameters. However,
lack of fusion at the root observed in the samples fabricated
under 6.0 and 7.5 mm diameter of the laser spot due to the
a) 0 mm b) 2 mm
low heat input corresponding to large spot diameter.
Fig. 2 High speed images on each wire feeding position.
Figure 5 also shows cross sections as the function of
wire feeding speed. There is not much difference between
the leg lengths of the weld bead. However, the cross section
geometry transits from triangle to sector. Furthermore,
increasing the wire feeding speed induces to the formation
of larger lack of fusion at the root. Thus, there is a limit to
improving the leg length by the laser beam reflection
changing with only the wire feeding speed. We should
consider the factor interaction between laser energy density,
wire feeding speed and welding speed.
The welded joint fabricated under the optimized
conditions has following properties; average grain size in
the coarse grain zone: 60 μm, dilution ratio: a few percent,
thickness of heat affected zone: 1 mm.
These results reveal that this process includes various
factors influencing on the welding phenomenon. However,
Fig. 3 Leg length change with spot diameter of laser. the parameter optimization contributes to the stable melting
of base materials and the filler wire and the obtained welds
48
indicate attractive properties, namely low heat input and (2) The filler wire should be fed into the molten pool
low dilution. backward without the laser irradiation.
(3) The leg length increases by the addition of filler wire
4. Conclusions compared with the non filler welding due to the laser
In order to develop the high efficiency / high quality beam reflection at the molten pool surface.
fillet welding technique, the welding phenomena on the hot- (4) The formation of lack of fusion at the root must be
wire laser fillet welding were investigated. Obtained caused by the excessive wire feeding and the
conclusions are as follows. insufficiency of the heat input by laser.
(1) The melting of filler wire depends on wire current and (5) The parameter optimization leads to the stationary
there is an optimum vale of the current at each wire welding phenomenon. In addition, the obtained weld
feeding speed. has attractive properties, namely low heat input and low
dilution.
49
Innovation of laser direct joining between metal and plastic†
KAWAHITO Yousuke* and KATAYAMA Seiji*
KEY WORDS: (Metal) (Plastic) (Ceramic) (Laser direct joining) (TEM image) (LD laser)
1. Introduction
Many materials including metals, plastics and ceramics
have been widely used in many industrial applications such
as automobiles, aircrafts and electronic devices. Joining
of these dissimilar materials is necessary and important
from a manufacturing viewpoint. The features of metals
include high strength, high toughness, high heat
conductivity and high heat resistance. Plastics are
characterized by lightweight, high corrosion resistance and
excellent formability. Polyethylene terephthalate (PET) is
known as a typical engineering plastic and commercially
available bottles. On the other hand, ceramics are used
owing to their high hardness and/or good heat resistance.
Silicon nitride ceramics (Si 3 N 4 ), a chemical compound of
silicon and nitrogen, is utilized as a bearing for engines or a
Fig 1 LAMP joints before and after tensile shear test.
rotor blade of turbine.
The dissimilar joining is generally performed using shown in Fig. 2. The TEM image demonstrates that the
adhesive bonds (glues) or mechanical fastering such as metal and the plastic are tightly bonded on the atomic or
bolts and rivets. However, these joining processes have molecular sized level. The base metal and the
some problems in terms of environmental restriction of intermediate layer were identified to be fcc gamma (J)
volatile organic compound (VOC) emission and mass phase and 5 nm-thick Cr-oxide film from these diffraction
production. Therefore, the authors have developed a new patterns, respectively. It was therefore revealed that a
laser direct joining method between metals and plastics strong joint could be produced by atomic, nanostructural or
which is named Laser Assisted Metal and Plastic joining molecular bonding of the metal and the plastic through the
method (LAMP joining method) [1]. oxide film on the metal plate surface. Not only the anchor
The LAMP joints between engineering plastic PET and (mechanical bonding) effect but also Van der Waals
stainless steel SUS304 before and after the tensile shear test interaction force and chemical bonding were considered as
are shown in Fig. 1. The top surface of PET was not bonding mechanisms of LAMP joining.
damaged to be as smooth as what it had been before the In this research, LAMP joining method with a 3-kW
laser irradiation. However, many bubbles of sub- diode laser (LD) was applied to join of Si 3 N 4 ceramic and
millimeter sizes were formed inside the plastic near the PET engineering plastic. The LAMP joining between the
joint. The shear load of the joint was about 3000 N, and ceramic and the plastic was carried out to optimize welding
the base PET was elongated sufficiently as shown in the speed. The obtained joints were evaluated by the tensile
lower photo of Fig. 1. Such strong joints were produced shear test. Furthermore, the joints were observed in
by the laser direct joining process with many small bubbles. details through TEM in order to investigate the joining
The LAMP joints were examined with transmission structure.
electron microscopes (TEM), and these examples are

* JWRI, Osaka University, Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
50
Innovation of laser direct joining between metal and plastic
3. Experimental Results and Discussion

A silicon nitride Si 3 N 4 plate and a PET plate were
overlapped, and then the LD beam was irradiated from the
plastic side. The welding speed was changed from 4 mm/s
to 8 mm/s at the laser power of 500 W. The typical
joining result at 6 mm/s speed is shown in Fig. 4. The top
surface of PET was not damaged and as smooth as it had
been before the laser irradiation as well as the previous
works of LAMP joining [1, 2]. Therefore, LAMP joints
of Si 3 N 4 ceramic and PET engineering plastic were
successfully produced. It was found that many bubbles
were formed inside the plastic near the LAMP joints.
The tensile shear strengths of the LAMP joints were
measured. The shear loads had the peak at about 6 mm/s,
and over 3100 N was achieved. Furthermore, the LAMP
Fig. 2 TEM image and FFT analyses of LAMP joints. joint made at 6 mm/s was observed with TEM. The
observation image is shown in Fig. 5. The bright upper
2. Materials and Experimental Procedures

The ceramic used was silicon nitride plates. The size
is 110 mm x 30 mm with 3 mm thickness. The plastic
used was PET plates. The size is 70 mm x 30 mm with 2
mm thickness. The transmissivity of amorphous PET is
high owing to its transparency. PET is decomposed at
more than 600 K. On the other hand, Si 3 N 4 has much
higher temperature of decomposition than PET.
This study was performed with the objective of
producing a strong LAMP joints of Si 3 N 4 ceramic and PET Fig. 4 Surface appearance of LAMP joint of Si3N4 and PET
produced at 500 W and 6 mm/s, showing bubbles.
engineering plastic. The LAMP joining with a LD beam
was carried out in the air without shielding gas for cooling part is PET polymer and the dark lower area is Si 3 N 4 .
the plastic and keeping the clean surface conditions as The TEM image demonstrates that the ceramic and the
illustrated in Fig. 3. The LD beam is in the line shape plastic are tightly bonded on the atomic or molecular size
whose major axis is 23 mm. The focused position of the level. Moreover, it was found that the PET polymer
LD beam is on the metal surface. Laser power is 500 W
and traveling speed is 4 mm/s to 8 mm/s. To evaluate the
mechanical properties of LAMP joints, SHIMAZU AG- Plastic:PET
10kNE was used as a tensile shear tester.
Fig. 3 Schematic experimental set-up of LAMP joining.

10 nm Ceramic:Si3N4
Fig. 5 TEM image of obtained LAMP joints of Si3N4 and PET.
51
entered the nanoscale hollow formed on the surface of Acknowledgments

Si 3 N 4 . It was therefore considered that the strong joint This work was conducted as part of the Industrial
could be produced by atomic, nanostructural or molecular Technology Research Grant Program “Development of
bonding of the metal and the plastic on the ceramic plate high-quality direct laser joining of metal and plastic by
surface, where not only the anchor (mechanical bonding) laser adaptive control” supported by New Energy and
effect but also Van der Waals interaction force and Industrial Technology Development Organization (NEDO).
chemical bonding were considered as joining or bonding The authors would like to acknowledge whom it may
mechanisms. concern.
[1] Y. Niwa, Y. Kawahito, S. Kubota and S. Katayama, Proc. of
We have successfully produced new LAMP (Laser-
ICALEO 2007, LIA, Orlando, (2007) (CD).
Assisted Ceramic and Plastic) joints between the
[2] S. Katayama and Y. Kawahito, Scripta Materialia, 59-12
commercially available ceramic Si 3 N 4 and the engineering
(2008), pp.1247- 1250.
plastic PET. The joint possessed over 3100 N shear load
strength in 30-mm-width plastic samples of 2 mm in
thickness. The base plastic was elongated because of the
formation of strong joints. Moreover, the TEM image of
the LACP joint demonstrates that the ceramic and the
plastic are tightly bonded on the atomic or molecular size
level.
52
JUNG KwangWoon *, KATAYAMA Seiji ** and KAWAHITO Yousuke **
KEY WORDS: (CFRP) (Laser cutting) (Ultra-high cutting speed) (Heat Affected Zone) (Cutting surface)
㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 (High brightness laser)
1. Introduction
Carbon fiber reinforced plastic (CFRP) with high Table 1 Material properties of CFRP used in experiments
specific strength to weight ratio, outstanding fatigue
resistance and no corrosion as one of composite materials
has been widely applied in automobile, aerospace and
electronics, where it is necessary to reduce energy
consumption and CO2 generation. However, CFRP is
difficult to cut because of the high hardness of carbon fiber
that made PITCH carbonized at high temperatures. The
main cutting techniques of CFRP are abrasive water-jet
machining and mechanical cutting operations by contact
process between tool and material such as micro-cutter
machining, milling machining. But they have several
disadvantages such as moisture absorption, high tool wear
because of mechanical loads and thermal loads, high costs Fig. 1 Schematic experimental set-up for cutting of CFRP
and limited cutting speed. In recent years, laser cutting
experiments with high power density heat source as one of
non-contact process have been conducted to investigate
cutting characteristics of CFRP using pulsed Nd:YAG laser,
disk laser and CO2 laser[1, 2]. During the laser cutting of
CFRP with high laser beam absorptivity, however, a㻌 wider
heat affected zone could be formed because of an increase
in laser heat input at a range of lower speed and also was
affected by material properties of CFRP and laser cutting
parameters including the laser power, the cutting speed, the
pressure of assist gas and the focal position. In this study, Fig. 1 Schematic experimental set-up for cutting of CFRP
therefore, with the objective of obtaining the better cut
quality and narrower HAZ width, laser cutting experiments beam of 8 mm䂩mrad (BPP) was delivered by the optical
were conducted to establish the proper laser cutting fiber of 0.2 mm core diameter. The laser scanner head was
conditions for various CFRP sheets at ultra-high cutting employed in order to accomplish ultra-high cutting speed,
speed using high brightness CW disk laser. and the laser beam was focused by the focal lens of 291.5
mm. The spot size of the laser beam was about 0.3 mm at
2. Experimental procedures the focal point.
Table 1 shows material properties of CFRP sheets used Table 2 indicates laser cutting conditions used mainly
in the experiments. Each CFRP was made by considering for cutting of CFRP. Laser cutting parameters were the
different material properties which include plastic type, laser power of 1 kW, the cutting speed of 500 – 5000 mm/s,
volume of fiber (%), fiber type, manufacturing process㻌 and laser irradiated number of 1 – 80 passes, time interval after
thickness of CFRP. A schematic experimental set-up for laser irradiated of 0 or 1 second, the focal position of ±0
laser cutting of CFRP is given Fig. 1. The CW disk laser mm. Cutting phenomena and behavior of the laser induced
with a maximum power of 16 kW was utilized and the laser plume during the laser cutting were observed by using two

* Graduate School, Osaka University, Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** JWRI, Osaka University, Osaka, Japan Japan
53
high speed video cameras at 10,000 F/s and 5,000 F/s for
laser irradiated part and laser induced plume, respectively.
A He- Ne laser with the maximum power of 50 mW and the
Table 2 Laser cutting conditions used in experiments
Fig. 3 Cut quality and laser induced plume behavior

observation results for cutting of No.4 CFRP
wavelength of 633 nm was employed for illumination. In considering the effect of time interval
addition, HAZ widths and kerf widths for the cut surfaces
and the cross sections of CFRP were evaluated using
optical microscope and scanning electron microscope
(SEM).
3. Results and discussions

In order to investigate the effect of the cutting speed on
the cut quality of CFRP, laser cutting experiments were
conducted by changing the cutting speed from 500 mm/s to
5,000 mm/s.
Figure 2 shows cut quality and plume behavior
observation results of No. 4 CFRP at the laser power of 1
kW, the laser irradiated number of 1 pass and the focal
position of ±0 mm. The results showed that the cut depth
and HAZ width of surface appearances and cross section Fig. 4 SEM photos of cross section of various CFRP with
at 500 mm/s were deeper and wider in comparison with 1kW laser power, 5,000 mm/s cutting speed, 80
those of 5,000 mm/s. In addition, it was observed that the pass laser irradiated number and 1 sec time interval
plume at 500 mm/s was ejected violently on the cut surface
and to the back direction and became lower the height of Figure 3 shows cut quality and plume behavior
the plume than that of 5,000㻌 mm/s. Based on these results, observation results of No. 4 CFRP, considering the effects
by increasing the laser heat input because of the long of time interval on HAZ width for the laser power of 1 kW,
interaction period between laser and material at the lower the cutting speed of 5,000 mm/s, the laser irradiated number
speed, it was noted that HAZ width was considerably wider. of 10 passes. In the case of time interval of 0 sec, wider
HAZ was generated compared with that of 1 sec. These
results can be explained by several causes as follows. First,
the deep-black high temperature stream during the
observation of laser irradiated parts was observed
continuously to remain to stay on the cut surface. Second,
in the case of plume observation results for time interval of
0 sec, as the laser was irradiated continuously, the height of
the plume was going down. From the results, the laser heat
input came to increase. Wider HAZ was attributed to the
phenomena that the heat inside CFRP sheet was
increasingly accumulated in the case of the continuous laser
Fig. 2 Cut quality and plume behavior observation results irradiation.
of No.4 CFRP at different speed In order to evaluate cut quality and cutting possibility
for various CFRP sheets, laser cutting experiments were
54
performed. The results are shown in Fig. 4. Cutting of No.1 4. Conclusions

and No. 7 CFRP was significantly difficult in comparison Laser cutting experiments of various CFRP sheets were
with other CFRP sheets. The reason is attributed to the base performed using a high brightness CW disk laser. At the
plastic of Epoxy and PPS, respectively. No. 2 CFRP with ultra-high cutting speed of 5,000 mm/s, narrower HAZ and
50 % volume of fiber and one-directional fiber type was kerf widths were obtained due to the decrease in laser heat
also difficult in cutting. Cutting of No. 4, No. 5, No. 6 and input for short interaction period. During the multi-passes
No. 8 CFRP with lower volume of fiber was easier than that laser irradiation, time interval was effective to produce
of the other CFRP, and narrower HAZ was obtained. In narrower kerf widths and HAZ on the cut surface and the
addition, as compared with No. 4 and No. 8 CFRP with cross section than no time interval. Moreover, cut quality
long fiber pellet and short fiber pellet, respectively, No. 8 and cutting possibility are known to highly depend on
CFRP with short fiber pellet had narrower HAZ width due plastic type, the volume of fibers, fiber laminated type of
to the effect of heat conduction by the different length of CFRP sheets.
fibers.
References
[1] D. Herzog, P. Jaeschke, O. Meier and H. Haferkamp. IJMTM.,
48 (2008), pp.1464-1473.
[2] Y. Abe, Y. Kawahito and S. Katayama. Preprints of the
national meeting of J.W.S., 86 (2010), pp. 188-189.
55
Characteristics and mechanism on the distortion of friction stir

welded aluminum alloy sheet

YAN㩷㩷 Dong-yang :8Ai-ping 6,/9$186Juergen =+$1*Zeng-lei DQG

6+,Qing-yu

.(<:25'6Friction stir weldingResidual distortionNumerical simulationMechanical loads

,QWURGXFWLRQ average respectively, while the loads in other two directions
As an advanced welding technology, possessing were very low. As shown in Fig. 1a, the main distortion of
the characteristics of low heat input and solid-state joining, sheets after FSW was out-of-plane distortion, which was
friction stir welding (FSW) has been widely used for similar to an anti-saddle pattern. A three-coordinates
joining aluminum alloys [1-2]. Although the residual measuring machine was used to measure the accurate
stresses and distortion are smaller to those of traditional distortion of the friction stir welded sheets [11]. The results
fusion welding, they still can not be ignored, especially showed that the offset between the highest and the lowest
when welding thin sheets with large size. Residual stresses position of sheet was about 8.5 mm.
in FSW have been widely investigated in recent years, and Fusion butt welding experiments were also executed
many conclusions have been obtained [3-9]. But few on the aluminum alloy sheets with the same dimension and
studies about distortion have been published. fixture conditions. The tungsten inert-gas (TIG) welding
Recently, a few papers [10-12] reported that when was utilized with the parameters of 16 V for voltage, 140 A
aluminum alloy sheets with large size were welded by FSW, for current and 4.42 mm/s for welding speed. The distortion
it not only had remarkable out-of-plane distortion, but also shape of the sheets after TIG welding appeared as a saddle
had different distortion patterns from that of the arc welding pattern (Fig.1b), which was opposite to the results of FSW.
with the same fixture conditions[12-13].
Many mechanical analysis models [6-9] have been
developed to predict the residual stresses of FSW, but the
stir tool’s mechanical loads were not considered. The
objective of this study is to investigate the characteristics Fig.1 Distortion pattern after welding, a) FSW, b)TIG
and the reason for unusual distortion patterns of friction stir
welded aluminum sheets, mainly by numerical simulation )LQLWHHOHPHQWPRGHO
based on previous experimental studies. In order to compare the effects of the stir tool
mechanical loads on the distortion, two analysis models are
([SHULPHQWDOSURFHGXUHV established. Model 1 considered the tool mechanical loads,
FSW experiments were carried out to observe the while model 2 did not. Except for the difference on tool’s
distortions with butt welding 6056 aluminum alloy sheets of mechanical loads, there were no other dissimilar conditions
the 600×315×3 mm dimension. The dimensions of the stir between the two models. ABAQUS/Standard software and
tool were 13 mm in diameter of the shoulder, 5 mm in sequentially coupled simulations were used. The geometry
diameter of the pin, and 2.6 mm in length of the pin. The model and the meshing are shown in Fig. 2. All properties
welding parameters were set to 1850 rpm in rotating speed of Al 6056 used in simulation are temperature-dependent,
and 700 mm/min in welding speed. Down load force of the even the yield strength is both temperature and temperature
stir tool was set to 8 kN, and forward tilt angle of the stir history dependent [14-16]. The dimensions of welding
tool was kept at 2° during welding. The welding fixtures sheets and the FSW parameters were similar with
were made up of one backing board and two pressing experiments.
boards. The temperature was measured by thermocouples The total heat input was calculated with the equation of
which were embedded near the stir tool. Force and working 4䰉K 0 ]Z , where Mz was the working torque of the stir
torque of the stir tool were also recorded during the welding tool, and 8.76Nm was used, Z was the tangential speed of
process. The measurements showed that the mechanical
stir tool 䋬 K was the total heat coefficient, which was
loads of stir tool mainly appeared as down force and
working torque, which reached 8086 N and 8.76 Nm in supposed to be 95% in simulation. It was assumed that heat
㩷 5HFHLYHGRQ6HSWHPEHU Transactions of JWRI is published by Joining and Welding
Tsinghua University, Beijing, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
EADS, Innovation Works Germany Japan
56
Characteristics and mechanism on the distortion of friction stir welded aluminum alloy sheet
input from the shoulder was 75% of the total, while the model 1 was consistent with the FSW experimental results
other was generated by the pin. The heat supplied by the in shape, while the distortion shape from the model 2 was
tool shoulder was considered as a surface heat flux which is absolutely opposite. The offset between the highest and the
axi-symmetric and increases linearly with radius, and the lowest position of sheet was 7.41mm and 8.63mm in the
heat generated by the pin was assumed to be a uniform model 1 and the model 2 respectively. These results
volume heat flux [6, 8-9, 17-18] . indicated that the introduction of stir tool’s mechanical
The heat transfer condition on the sheet surfaces which loads had the effect of distortion reduction. The distortion
were not in contact with the fixtures was set as the curves on the line of X=40 mm, X=320 mm, X=560 mm,
convection boundary condition, while on the contacting Y=-310 mm, Y=-116 mm and Y=0 mm on the top surface
surfaces the heat transfer was treated in a way of contact of the sheet from the computation with the model 1 and
heat conduction. The contact conductivity was assumed to experimental results were listed in Fig. 5. The results
be simply temperature-dependent [19]. showed that the distortion trends of the sheet by simulation
The restriction effect of the welding fixtures on the and experimental results were consistent, and this
sheet was set as a contact model, where the condition on consistency was compatible over the whole plate, not for
contacting surfaces was described as Coulomb friction with some local positions. The largest error between the
a coefficient of 0.3, and the interaction force in the normal deformation values was less than 20%, which was
direction was set under the principle of “pressure-over- acceptable in welding mechanical analysis. The distortion
closure”[20]. The down force of the stir tool was imposed comparison confirmed that the model 1 was a reasonable
as a uniform surface pressure onto the upper surface of the model for distortion analysis of FSW.
sheet where the stir tool covered. The working torque was
simplified as shearing friction between the shoulder
surfaces and welded materials, and was treated as
circumferential body forces, and applied on the uppermost
layer integration points of the panels which lay in the region
covered by tool shoulder [21]. Model 2 only has thermal
load during mechanical analysis.
At the end of mechanical simulation, the restrictions of
welding fixtures were removed. Thus the residual distortion
of sheet appeared under unclamped condition.
5HVXOWVDQGGLVFXVVLRQ Fig.5 Deformation comparisons between simulation and

The computed and measured welding temperature experimental results
histories of nodes A(X=300㧘Y=4.5㧘Z=3) and
B(X=300㧘Y=14.5㧘Z=3) are displayed in Fig. 3. The According to the residual transverse plastic strain
computed results showed that the peak temperature in FSW results (Fig. 6) with the two models, mechanical loads of
was only 485ć, which was lower than the melting point of the stir tool not only reduced the residual plastic strain of
6056 aluminum alloy. the weld zone, but also changed the relationship of the
magnitude of transverse plastic strain between top and
bottom of the sheet. When the mechanical loads of the tool
were not considered, like in model 2, the transverse
compression plastic strain on sheet’s top surface was
smaller than that of the bottom surface, so the sheet became
convex in width. But if the model included both thermal
Fig.2 Geometric model and Fig.3 Computed and measured load and stir tool’s mechanical loads, as in model 1, the
mesh
for the welded sheets temperature results transverse compressive plastic strain on sheet’s top surface
was larger than that of the bottom surface. Therefore, the
distortion appeared concave shape in width of sheet.
Fig.4 Distortion pattern with model 1(a) and model 2(b)
The distortion simulation results with the two analysis

Fig.6 Distribution of trans- Fig.7 Distribution of longi-
models are shown in Fig. 4. The patterns are different, anti-
verse residual plastic strain tudinal residual plastic strain
saddle shape for model 1, but saddle shape for model 2.
These results indicated that the distortion obtained from the
57
Curves in Fig. 7 displayed the results of longitudinal 5HIHUHQFH

plastic strain of the weld central line on the top surface with >@:07KRPDV('1LFKRODV-&1HHGKDP0*0XUFK3
the two models, which appeared as compression strain. The 7HPSOHVPLWK&-'DZHV)ULFWLRQ6WLU:HOGLQJ,QWHUQDWLRQDO
strain curves comparison in the figure showed that the 3DWHQW $SSOLFDWLRQ 1R 3&7*% DQG *UHDW %ULWDLQ
3DWHQW$SSOLFDWLRQ1R
values of longitudinal compression strain were reduced >@560LVKUD=<0D0DWHU6FL(QJ5
under the impact of the stir tool’s mechanical loads. This >@0-DPHV00DKRQH\3URFRIVW,QW6\PSRVLXPRQ
result could be approved by the value of longitudinal )ULFWLRQ6WLU:HOGLQJ7KRXVDQG2DNV&$86$-XQH
shrinkage of the weld seam by simulation: the shrinkage
arrived at 0.8 mm with model 2, but this value fell to >@&''RQQH(/LPD-:HJHQHU$3\]DOOD7%XVODSV
0.3mm with model 1. 3URF RI UG ,QW 6\PSRVLXP RQ )ULFWLRQ 6WLU :HOGLQJ .REH
As is known, the materials in the welding zone can’t -DSDQ6HSWHPEHU
expand and shrink freely during traditional fusion welding >@655DMHVK+DQ6XU%DQJ:RRQJ6HRQJ&KDQJ:RRQJ
process under the local thermal load effect, so that some 6HRQJ&KDQJ+HXQJ-X.LPHWDO-0DWHU3URFHVV7HFKQRO
compressive plastic strain still remain after welding. In 䍆 &
FSW process, the plastic strain is not only caused by >@0=+.KDQGNDU$.-DPLO35$QWKRQ\$60LFKDHO
HWDO-0DWHU3URFHVV7HFKQRO
thermal load, but also influenced by stir tool’s loads. There >@7LQJ/L4LQJ\X6KL+RQJNH/L6FL7HFKQRO:HOG-RLQ
are two main functions that these loads of the stir tool affect
on the residual plastic strain. First, the tool’s mechanical >@4LQJ\X6KL7HUU\'LFNHUVRQ+XJK56KHUFOLII3URFWK,QW
loads enhance the mechanical restriction effect on the &RQI RQ 7UHQGV LQ :HOGLQJ 5HVHDUFK 3LQH 0RXQWDLQ
materials around the stir tool, resulting in the lower residual *HRUJLD86$$SULO
plastic strain. Second, the down force of the stir tool >@7/'LFNHUVRQ 4< 6KL +56KHUFOLII 3URF WK ,QW 6\PS
supplies an additional compression, so the dimension of 2Q )ULFWLRQ 6WLU :HOGLQJ 6DOW /DNH &LW\ 8WDK 86$ 0D\
thickness direction in the stir zone was reduced. According
to the volume constancy principle, the compression in >@'$3ULFH6::LOOLDPV$:HVFRWW&-&+DUULVRQ$
5H]DL$6WHXZHU03HHO36WDURQDQG0.RFDN6FL
thickness direction would bring additional expansion in the
7HFKQRO:HOG-RLQ
other two directions. >@4<6KL-6LOYDQXV</LXHWDO6FL7HFKQRO:HOG-RLQ

&RQFOXVLRQV >@65%KLGH30LFKDOHULV03RVDGD-'HORDFK:HOGLQJ
(1) A 3D FEA model considering the stir tool’s mechanical -RXUQDO
loads was developed to study the generation and >@&/7VDL6&3DUN:7&KHQJ:HOGLQJ-RXUQDO
characteristics of the distortion of friction stir welded 㩷㩷㩷
aluminum alloy sheets. >@**ULPYDOO7KHUPRSK\VLFDOSURSHUWLHVRIPDWHULDOV1HZ
(2) The simulation results indicated that the functions of stir 㩷㩷㩷 <RUN
tool’s mechanical loads could change the relationship of >@-(3DUURWW'6$XGUH\7KHUPDO&RQGXFWLYLW\RIVROLGV
㩷㩷㩷 3LRQ/RQGRQ
magnitude of transverse plastic strain between top and >@=/=KDQJ-6LOYDQXV+./L4<6KL6FL7HFKQRO
bottom surface of sheet, which was the key point to the 㩷㩷㩷 :HOG-RLQ
difference of distortion patterns between FSW and >@0=+.KDQGNDU-$.KDQ$35H\QROGV6FL7HFKQRO
fusion welding with the same fixture conditions. 㩷㩷㩷 :HOG-RLQ
(3) Mechanical loads of the stir tool have two main >@79X\VW/''HDOYLVH3URFWK,QW6\PSRQ 䌿䍌 )ULFWLRQ
functions to influence the distribution of residual plastic 㩷㩷 6WLU:HOGLQJ)UDQFH
strain in FSW process, increasing the frictional >@&KXDQVRQJ:X1XPHULFDODQDO\VLVIRUKHDWWUDQVIHULQ
resistance between the welded sheets and backing board, ZHOGLQJSURFHVV+DUELQLQVWLWXWHRIWHFKQRORJ\SUHVV+DUELQ
limiting the expansion of material in stir zone in &KLQD
thickness direction and bringing additional expansion in >@$%$4866WDQGDUG8VHU䌿䍍 V0DQXDOYHU
the plane of sheet. >@7LQJ/L4LQJ\X6KL+RQJNH/L:HL:DQJ=KLSHQJ&DL
,QWHUQDWLRQDO:HOGLQJ-RLQLQJ&RQIHUHQFH.RUHD
&2(;&RQYHQWLRQ&HQWHU6HRXO.RUHD0D\

58
The influence of the solid state phase transformation on welding

deformation of low alloy high strength steel†
YANG Xiao*, CHEN Junmei*, LU Hao*
KEY WORDS: (welding deformation) (phase transformation) (measurement) (prediction) (FEA)
1. Introduction parameters are shown in Table1.

As low alloy high strength steel is widely used in many Table1 Welding parameters
fields such as in shipbuilding and so on, the influence of Current Voltage Speed Gas flow Wire
phase transformation on welding deformation has attracted dia.
researchers’ attention all over the world. In this paper, we 170A 29V 50cm/min 8L/min 1.2mm
did some welding experiments with low alloy high strength
steel AH3201, which is popular with shipbuilding. During
the welding, we measured the deformation in three
positions dynamically with a program based on LabVIEW.
Then we calculated the deformation in the same condition
as that in the experiment on ABAQUS, taking account of
phase transformation, which could be in contrast with the
experiment.
2. Measurement
Fig. 2 Result got in LabVIEW program
Figure 2 shows the displacement in the Z-direction at

three points. We can see the maximum displacement after
cooling for nine minutes occurs in the middie, which is
about 25mm.
Fig. 1 Assembly chart
Figure 1 shows the assembly chart in this

experiment[1]. Two 500mm*150mm*3mm plates placed on
a large plate are to be welded. The plate A is fixed by four
clamps so that it can not move in any direction. The plate B
is not fixed by clamps but by spot welding at the beginning
and the end of the gap, which means that it can deform Fig. 3 Measured displacement at three points
much more freely. Three resistance displacement sensors
are placed next to plate B to get the displacement in the Z- We compound these three plots together, as shown in
direction at three points along the edge of the plate. We Fig. 3. In the experiment, the period for arc heating is from
didn’t measure the displacement in the other two directions 0 to 67th second, and from 67th second to 600th second for
because the plate was too thin to be attached to the sensors. cooling, when we found the displacement didn’t change a
The welding method is CO 2 -GMAW. The welding lot any more. Fig.3 takes on three characteristics.
* Materials Science and Engineering School, Shanghai Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Jiaotong University, Shanghai 200240, China Japan
59
The influence of the solid state phase transformation on welding deformation of low alloy high strength steel
1) The maximum displacement occurs in different The no diffusion-phase transformation can be

positions at different time- at the beginning after heating described by K-M formula:
and in the mid after cooling. Transferred into angle, the X 1 exp[c( M s T )] (2)
maximum angle deformation is about 10 degrees. Notice
that the displacement on plate B was measured in the The parameter c is supposed to be a constant 0.01.
condition that the plate A was fixed and didn’t deform a lot. The expansion coefficient of each phase is different in
the form:
2˅ The plots can be divided into four sections. In the
austenite > ferrite > pearlite > bainite > martensite
first section, the displacement didn’t increase possibly
So it has an influence on welding deformation. The
because the beginning and the end of two plates were not
average expansion coefficient is:
well jointed by spot welding. Then the displacement at
three points increased drastically till heating finished. The D D1 X D 2 (1 X ) (3)
first inflexion appeared at about the 72th second, after which On the other hand, an linear expansion about 1.6%
the displacement decreased at different speeds. The second occurs when austenite transfers to other phases in a lower
inflexion appeared at about the 135th second, after which temperature because of the difference in specific volume[4].
the displacement increased again and reached the steady The corresponding incremental strain is about:
state at last. 'H sv 0.016 X (4)
3˅ The inflexions at three points are almost at the
So the total incremental strain caused by phase
same time. Considering that the temperature history for
transformation at each increment is:
these points in distance of 200mm should have an interval
much more than six seconds, we infer that the occurrence of ǻ H 0.016( X X pre ) 1 (D D pre )(T Tpre ) (5)
each inflexion doesn’t result from something such as phase 2
transformation in the region near the very point only, but
from the temperature field and phase distribution of the
whole model.
3. Calculation
We did a sequential coupled analysis on the same
model based on ABAQUS, taking account of the factor of
phase transformation. During the welding, diffusion and no Fig. 5 Comparison of calculation and experiment
diffusion phase transformation happens in the region near
the weld at different cooling speeds[2]. The diffusion phase Figure 5 shows the calculated result compared with
transformation can be described by the following the experiment result. Figure 6 shows the calculated
Kamamoto model[3]: displacement in the mid point compared with the
Ts T n experiment, with another plot not taking account of phase
X 1 exp[k ( ) ] (1) transformation. We can see the trend of deformation
Ts T f conforms to the experiment, but the values differ a lot. The
X represents the volume percentage of the new phase. displacement taking account of phase transformation is
T s and T f represent the moment phase transformation starts smaller than that of not taking account of phase
and finishes, which are determined by the cooling speed transformation.
and continuous cooling transformation chart as shown in
Fig. 4. The parameters k and n come from previous
experiment result.
Fig. 6 Calculated displacement at the mid point
4. Conclusions
The conclusions of this study are summarized as follows.
(1) In one-side fixed welding of thin plate, the unfixed side
warps a lot, especially at the position in the middie.
Fig. 4 The CCT chart of AH3201 (2) The deformation appears to be an increase-decrease-
increase process, either in the experiment or in the
60
calculation, no matter if we take account of phase [2] Zhao Hongzhuang, Xu Hong, Liu Xianghua and Wang
transformation. Guodong: Review of Numerical Simulation on the Process of
(3) Phase transformation from austenite to phases at a lower Heat Treatment. Heat Treatment, 2004,19(1).
temperature decrease the welding transformation. [3] Wang Qingpeng, Li Wushen, Chen Cuixin and Feng Lingzhi:
Analysis on the Model of Phase Transformation in Welding
Acknowledgement Heat Affected Zone. Welding, 2004(11).
This project is support by the National Natural Science [4] Wang Wenxian, Huo Lixing, Zhang Yufeng and Wang
Foundation of China (Grant No. 50975176) Dongpo: Analysis on the Regulation and Mechanism of the
Influence from Phase Transformation Temperature over
References Welding Residual Stress. China Mechanical Engineering,
[1] Xu Jijin, Chen Ligong, Zhang Min, He Defu and Wu Youjing: 2003,14(3).
Experiment and Measuring System of Double Wires
Submerged Arc Welding with A105-Steel Heavy Plates.
Symposium of 11th National Welding Conference, 2005.
61
Optimising residual stress measurements through the use of

†
measurement simulation
TRUMAN C. E. * and SMITH D. J. *
KEY WORDS: (Residual stress) (Deep hole drilling) (Measurement simulation)
1. Introduction stresses by analysing measured distortions with elasticity

Mechanical strain relaxation (MSR) residual stress theory. In many welded components, however, the high
measurement techniques, and in particular deep hole magnitude and tri-axiality of the residual stress field can
drilling, are now being used to make accurate cause plasticity when a cut is introduced as part of the
measurements of residual stress in environments that have measurement. This plasticity can cause significant
previously caused problems. Conventional application of measurement errors. Deep hole drilling, one principal MSR
these techniques determines through-thickness residual technique, has been advanced in recent years to account for
this plasticity. The research in this paper describes how
deep hole drilling measurements may be optimised - in
terms of reduced measurement errors and more efficient
experimental parameters - by utilising measurement
simulations prior to the actual measurement. Several cases
Fig. 2㻌㻌 Mesh illustrating the DHD drilling and trepanning

Fig. 1㻌㻌 316H offset repair sequence

* Department of Mechanical Engineering, University of Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Bristol, Bristol, UK Japan
62
Optimising residual stress measurements through the use of measurement simulation
studies (all welded components) are considered where

results of finite element predictions of weld residual
stresses are mapped onto bespoke meshes and deep hole
drilling simulations undertaken. These simulations permit
the effects of several measurement parameters to be
explored and optimised. Results are presented which
demonstrate the significant experimental improvements
obtained by utilising a combined measurement-simulation
approach. This extended abstract describes two of the case
studies, with more being considered in the presentation.
2. Case Study 1: 316H Stainless Steel Repair

A three dimensional (3D) finite element analysis (FEA)
was carried out to investigate the influence of trepanning in
the deep-hole drilling (DHD) residual stress measurement
method on the initial residual stress present in a welded
pipe containing a short repair, Fig. 1. Using a mapping
procedure the initial residual stress and equivalent plastic
strain fields from the repair weld simulation were mapped
onto a 3D model with a mesh structure suitable to simulate
the experimental deep hole drilling residual stress
measurement technique, Fig. 2. Deep hole drilling
measurements had been previously obtained. Fig. 3㻌 General arrangement of NeT TG4 specimen
The initial results obtained from the weld residual stress
model and the DHD measurement simulation both utilised a
mixed hardening material model. The direction of the DHD
simulation through the thickness of the repair weld was
from the outer surface towards the inner surface. This
correctly mirrored the experimentally applied measurement
direction.
The study showed, in general, a minimal effect of
trepanning in the DHD measurement method on the
redistribution of the original residual stress present in the
component and verified the applicability of the method on
this particular component. A degree of redistribution was, Fig. 4㻌㻌 Weld residual stress model results, used as initial
however, noticeable close to the outer surface of the state for measurement simulations
component. In particular, the redistribution effect was more
pronounced in the longitudinal residual stress component. 4. Conclusions
Deep hole simulations on the girth-butt welded
3. Case Study 2: 3-pass Slot Weld (NeT TG4) component revealed that the deep-hole method worked well
The TG4 specimen is a 3-pass slot weld in AISI 316LN for practical components with some degree of redistribution
austenitic stainless steel, made using the tungsten-inert-gas effect in the reconstructed DHD simulated residual stress
(or TIG) welding process. The dimensions of the plate are components close to the outer surface. The redistribution
194 x 150 x 18 mm, while the slot is 80 mm long and 6 mm was more apparent in the case of longitudinal stress
deep, and is filled with three superimposed weld passes. component. The study illustrated the influence of the DHD
This specimen provides a natural increase in complexity procedure on the initial residual stress distribution present
over the NeT-TG1 specimen [1]: the weld is made with in a component. The reconstructed residual stress
three passes rather than one, and the volume of weld metal distribution did not reveal the initial peak tensile residual
is much greater, extending over about 1/3 of the depth of stress near the outer surface of the butt-girth welded pipe
the plate. The overall specimen geometry is illustrated in component. Both the initial and the reconstructed residual
Fig. 3. stress distributions were sensitive to the material hardening
In order to systematically study a suite of potential behaviour.
measurement options, with a view to improving accuracy Results of measurement simulations in the TG4 specimen,
and better understanding the influence of potential plasticity some of which are displayed in Fig. 5, highlighted the
issues, the results of a finite element weld simulation [2] of necessity of devising an optimized measurement strategy
the TG4 specimen were used as initial state conditions in a prior to experiment. The specimen contained very high
simulation of the measurement, Fig. 4. magnitude residual stresses, a high degree of tri-axiality and
substantial regions of plastically yielded material.
63
References
[1] C. E. Truman and M. C. Smith: Int. J. Pres. Ves. Pip., 86(1)
(2009), pp 1-2
[2] O. Muránsky et al: ASME Pres. Ves. Pip. Conf. (2010),
PVP2010-25
Fig.5㻌㻌 “Overcoring” results for DHD 㻌

simulation in TG4 specimen
64
Residual stress measurement of large-bore stainless steel pipes with

†
butt-welded joints by inherent strain method
MAEKAWA Akira*, NAKACHO Keiji **, MA Ninshu*** and SATO Reiko****
KEY WORDS: (Welding residual stress) (Austenitic stainless steel) (Butt-welded joint) (Inherent strain
method) (Large-bore pipe) (Three-dimensional stress distribution)
1. Introduction
The inherent strain method [1] is a destructive § ] ·§ [ ·
H *kf ] ,[
A1k ¨¨1 ¸¸¨¨1 ¸¸
technique to measure the residual stress accurately by © Z k ¹© R k ¹ (4)
cutting up the welding structure to be measured. The N N
§ S] · § S[ ·
residual stress is represented by Eq.(1) using inherent ¦¦ Aijk cos¨¨ 2i 1 ¸¸cos¨¨ 2 j 1 ¸¸
strain: i 1 j 1 © 2Z k ¹ © 2 Rk ¹
^V ` >D@>H @^H ` (1) Here H k f 9 , [ is the inherent strain distribution, ȗ, ȟ, Z k ,

R k are local coordinates, A 1k , A ijk are coefficients of
where ^V ` is residual stress, ^H ` is inherent strain, >D @ inherent strain distribution, N=1,2,3 and k=0,1,2,3,4.
is the matrix between elastic stress and strain, and H is > @
the elastic response matrix between inherent strain and 2. Test Pieces
elastic strains. Two kinds of test pieces welded in a butt joint were
The measurement strain ^mH ` is obtained by cutting used: 300A welded pipe joint made of SUS316L with an
outer diameter of 318.5mm and thickness of 33.3mm; and
the welding structure. ^V ` is obtained by substituting the 500A welded pipe joint made of SUS316with an outer
^ `
most probable value Hˆ calculated by Eq.(2) to Eq.(1). diameter of 508.0mm and thickness of 50.0mm. The
welding current and voltage were from 63 to 180 Aand 20
^Hˆ ` §¨© >H @ >H @ ·¸¹>H @ ^ H `
T 1 T
m
(2) V, respectively. Tungsten inert gas (TIG) welding was done
without fixing the ends from 0° to 180°.
The inherent strain method using functional form [2], in 3. Results and Discussion
which the inherent strain distribution was represented by Figures 1 and 2 show the residual stress distributions
the function, enables accurate measurement in spite of for circumferential and axial stress on the inner and outer
fewer measurement points because the distribution of sides in the 0° - 180° cross section. A different bore
inherent strain ^H ` is represented by the appropriate changes the distributions of compressive and tensile stress.
function. This is why the residual stress distribution is more
In this study, the inherent strain method using functional complicated due to the change in magnitude of the bending
form was applied to welded pipe joints. The measurement deformation because the magnitude of thermal expansion
strain was measured at 90° from the welding start position and the shrinkage are different in the circumferential
and then, the residual stress distribution was calculated direction as the bore and wall thickness are each made
assuming that the strain distribution spread uniformly in the larger.
circumferential direction. Here, the third order polynomial Figures 3 and 4 show the residual stress distribution of
function was assumed as an appropriate function for the 300A welded pipe joint. The distributions calculated by
inherent strain distribution. However, the appropriate using two functions with N=3 in Eq.(3) and Eq.(4) are very
function of inherent strain distribution has not been clarified reliable based on statistical and mechanical standpoints [3].
for a large-bore and heavy-walled welded pipe joint. However, more investigation is needed to determine the
Therefore, six kinds of functions were examined to most reliable function. Additional functions with various N
represent the distribution appropriately. values are now being examined.
N N
§ ] ·
i
§ [ ·
j
4. Conclusions
H * ] ,[
f
k ¦¦ Aijk ¨¨1 ¸¸ ¨¨1 ¸¸ (3) The results in this study were summarized as follows:
i 1 j 1 © Zk ¹ © Rk ¹

* Institure of Nuclear Safety System, Inc., Fukui, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** JWRI, Osaka University, Ibaraki, Japan Japan
*** JSOL Corporation, Osaka, Japan
**** Graduate School, Osaka University, Ibaraki, Japan
65
Residual stress measurement of large-bore stainless steel pipes with butt-welded joints by inherent strain method
(MPa) (MPa) (MPa) (MPa)
(a) Circumferential stress (b) Axial stress

Fig.1 Residual stress distribution of 300A welded pipe joint (a) Circumferential stress (b) Axial stress
(0° - 180° cross section, function with N=3 in Eq.(3)).
Fig.2 Residual stress distribution of 500A welded pipe joint
(0° - 180° cross section, function with N=3 in Eq.(3)).
(MPa) (MPa) (MPa)
3.5E+02 4.0E+02 5.0E+02
3.0E+02 3.5E+02
4.0E+02
2.5E+02 3.0E+02
2.0E+02 2.5E+02 3.0E+02
1.5E+02 2.0E+02
2.0E+02
1.5E+02
1.0E+02
1.0E+02 1.0E+02
5.0E+01
5.0E+01
0.0E+00 0.0E+00
0.0E+00
-5.0E+01 -5.0E+01 -1.0E+02
-1.0E+02 -1.0E+02
-2.0E+02
-1.5E+02 -1.5E+02
-2.0E+02 -2.0E+02 -3.0E+02
(a) N=1 in Eq.(3) (b) N=2 in Eq.(3) (c) N=3 in Eq.(3)

(MPa) (MPa) (MPa)
4.0E+02 4.0E+02 5.0E+02
3.5E+02 3.5E+02
4.0E+02
3.0E+02
3.0E+02
2.5E+02 3.0E+02
2.5E+02 2.0E+02
2.0E+02
2.0E+02 1.5E+02
1.5E+02 1.0E+02 1.0E+02
1.0E+02 5.0E+01 0.0E+00

0.0E+00
5.0E+01 -1.0E+02
-5.0E+01
0.0E+00 -1.0E+02 -2.0E+02
-5.0E+01 -1.5E+02
-3.0E+02
-1.0E+02 -2.0E+02
-1.5E+02 -2.5E+02 -4.0E+02
(d) N=1 in Eq.(4) (e) N=2 in Eq.(4) (f) N=3 in Eq.(4)

Fig.3 Circumferential residual stress of 300A welded pipe joint (90° cross section).
(MPa) (MPa) (MPa)
2.5E+02 2.5E+02 2.5E+02
2.0E+02 2.0E+02 2.0E+02
1.5E+02 1.5E+02
1.5E+02
1.0E+02 1.0E+02
1.0E+02
5.0E+0.1
5.0E+01
5.0E+01 0.0E+00
0.0E+00
0.0E+00 -5.0E+01
-5.0E+01
-1.0E+02
-1.0E+02 -5.0E+01
-1.5E+02
-1.5E+02 -1.0E+02
-2.0E+02
-2.0E+02 -1.5E+02 -2.5E+02
(a) N=1 in Eq.(3) (b) N=2 in Eq.(3) (c) N=3 in Eq.(3)

(MPa)
(MPa) (MPa)
2.5E+02
2.0E+02 3.0E+02
2.0E+02 2.5E+02
1.5E+02
1.5E+02 2.0E+02
1.0E+02 1.5E+02
1.0E+02 5.0E+01 1.0E+02
5.0E+01 5.0E+01
0.0E+00
0.0E+00
0.0E+00 -5.0E+01 -5.0E+01
-5.0E+01 -1.0E+02 -1.0E+02
-1.5E+02
-1.5E+02
-1.0E+02 -2.0E+02
-2.0E+02 -2.5E+02
-1.5E+02
-2.5E+02 -3.0E+02
(d) N=1 in Eq.(4) (e) N=2 in Eq.(4) (f) N=3 in Eq.(4)
Fig.4 Axial residual stress of 300A welded pipe joint (90° cross section).
66
(1) The inherent strain method using functional form was References
applied to large-bore and heavy-walled stainless steel [1] Y. Ueda, K. Fukuda, K. Nakacho and S. Endo: J. Soc. Nav.
pipe with butt-welded joint. Archit. Jpn., (1975), pp.499-507.
(2) The shape of the stress distribution had a more complex [2] Y. Ueda and N.X. MA: Quarterly Journal of JWS, 11 (1993),
change when the bore and thickness were larger. pp.189-195.
(3) Six kinds of functions were examined to provide greatly
[3]K. Nakacho, N. Ogawa and T. Ohta: Quarterly Journal of JWS,
reliable distribution of residual stress. 27 (2009), pp.297-306.
67
†
KIM You-Chul*and HIROHATA Mikihito*
KEY WORDS: (Residual stress) (Laser beam welding) (High strength steel) (Phase transformation)
(Thermal elastic-plastic analysis)
1. Introduction Table 1 Chemical compositions and

For improving function and reducing the weight of mechanical properties.
steel structures, use of high strength steel has been tried Chemical compositions (mass%)
frequently. As the joining method for the high strength C Si Mn P S
steel, laser beam welding (LBW) is noted [1]. 0.08 0.22 0.96 0.007 0.002
The characteristics of LBW such as heat input, bead Mechanical properties
width, welding speed and so on are largely different from Yield stress Tensile strength
those of existing arc welding. (MPa) (MPa)
In welding of high strength steel, martensitic 813 840
transformation (phase transformation) occurs in the
relatively low temperature region in the cooling process.
500
It is known that the phase transformation largely affects the
generation of distortion and residual stress [2]. 50 5mm
20
40
It is unknown how residual stress is generated in
welding of the high strength steel by laser beam.
In this paper, in order to elucidate how residual stress x
9mm
is generated by LBW on the high strength steel (HT780), an
experiment is carried out and is simulated by a thermal y
300
elastic-plastic analysis with considering the phase Weld line

transformation.
2. Experiment
20
One-pass bead-on-plate welding is performed on high

40
strength steel by using a fiber laser. As the welding

conditions, the laser power is 6kW and the welding speed is 12
z
Material: HT780
0.6m/min. Unit: mm
The material is HT780 and the thickness is 12mm. y
Table 1 shows the chemical compositions and the
Fig. 1 Test specimen and macrograph.
mechanical properties of the material.
Figure 1 shows the shape of the specimen and an 250
Young’s modulus E (GPa)
example of the macrograph. Experiment

The width of the weld bead is around 5mm and the Heating
penetration depth is around 9mm. 200
Cooling
After the welding, the residual stress is obtained by the Analysis
stress relaxation method. 150 Heating
Cooling
3. Idealization of Mechanical Properties with 100
Considering Phase Transformation
In the welding of high strength steel, the phase Ms=441
50 (ഒ)
transformation occurs in the relatively low temperature Mf=324
range in the cooling process. In that range, the mechanical Mf Ms
properties cannot be specified because the transformation 0
expansion and the transformation superplasticity 0 400 800 1200 1600
(extraordinary ductility) occur. Temperature T (Υ)
It is necessary that the mechanical properties in the
phase transformation range are idealized for simulating the Fig. 2 Temperature dependency of
welding of the high strength steel by FEM. Young’s modulus.
† Received on 30 September 2010㻌㻌 Transactions of JWRI is published by Joining and Welding
* JWRI, Osaka University, Ibaraki, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
68
As an example, Fig. 2 shows the idealized Young’s

2000
modulus proposed by the author [3].
Residual stress ıx (MPa)

Analysis Experiment
For simulating the extraordinary ductility due to the 1500 With PT
transformation superplasticity, Young’s modulus; E at the Without
start temperature of the phase transformation; M s (=441ଇ) 1000
is lowered around zero and it is linearly recovered up to the
finish temperature; M f (=324ଇ) in the cooling process. 500
In the thermal elastic-plastic analysis described below,
0
these mechanical properties are used in the cooling process
Obverse x=30 (mm)
in the elements where the temperature exceeds the A 1 -500
transformation temperature (around 720 ଇ) in the heating f
-50 -25 0 25 50
process, that is, the weld metal and HAZ. In the elements y (mm)
except them, the mechanical properties in the heating
(a) Stress component in welding direction; ıx
process are also used in the cooling process.
2000
4. Thermal Elastic-plastic Analysis
Residual stress ıy (MPa)

Analysis Experiment
The experiment is simulated by the thermal elastic- 1500 With PT
plastic analysis. Without
1000
500
0
z x=30 (mm)
Welding Obverse
direction y
x -500 f
Weld metal -50 -25 0 25 50
y (mm)
(b) Stress component in transverse direction; ıy
Symmetric Fig. 4 Residual stress distribution
condition
HAZ In the case of without PT modelı x is over the yield
stress. However, it is confirmed that the equivalent stress
DJUHHVZLWKWKH\LHOGVWUHVV 2QWKHRWKHUKDQGı x varies
from the yield stress to zero in the case of with PT model.
Fig. 3 Model for thermal elastic-plastic analysis. The experimental result is within the result obtained by the
analysis of with PT model. Considering the accuracy of
Figure 3 shows the analysis model. the stress relaxation method, the experimental result is
The isoparametric solid elements with 8 nodes are substantially simulated by the analysis of with PT model.
used. The stress compRQHQW LQ WKH WUDQVYHUVH GLUHFWLRQ ı y
The half model is adopted. The heat input (the weld (Fig. 4(b)) is noted.
metal) elements are decided by referring to the macrograph In the case of without PT modelı y is tension and the
(Fig. 1). value is around 300MPa. It does not agree with the
The model with considering the phase transformation experimental result which is small compression. On the
by using the above idealized mechanical properties is contrary, the result obtained by the analysis of with PT
defined as ‘with PT’ model. model accurately agrees with the experimental result.
On the other hand, the model without considering the From these results, the validity of the treatment in
phase transformation, i.e., the same mechanical properties mechanics of with PT model idealizing the mechanical
in the heating process are also used in the cooling process, properties with considering the transformation expansion
is defined as ‘without PT’ model. and transformation superplasticity is verified.
The analysis results of these two models are compared The residual stress generated in the weld metal is
to investigate the effect of the phase transformation on the largely affected by the phase transformation in the cooling
residual stress. process although the bead width of LBW (around 5mm) is
extremely narrow. The tensile residual stress generated in
5. Results of Experiment and Analysis the weld metal is largely released by the phase
Figure 4 shows the residual stress distribution transformation.
obtained by the experiment and the analysis.
The stress at the center of the welding direction 6. Conclusions
(x=30(mm)) on the obverse surface is shown in the figure. In order to elucidate how residual stress was generated
The stress component in the welding directioQı x (Fig. by LBW on the high strength steel, one-pass bead-on-plate
4(a)) is noted.
69
welding of HT780 by laser beam was simulated by the compared with that of existing arc welding.
thermal elastic-plastic analysis with using the idealized (3) The tensile residual stress generated in the weld metal
mechanical properties considering the phase transformation. was largely released by the phase transformation.
(1) The residual stress obtained by the experiment could
be simulated by the analysis with high accuracy. The References
validity of the treatment of the mechanical properties in [1] INOSE K., LEE J-Y., NAKANISHI Y. and KIM Y-C. :
the phase transformation range was verified. QJJWS, 26-1(2008), pp. 61-66.
(2) It was known that the residual stress generated in the [2] SATOH K. and TERASAKI T. : Journal of the JWS, 45-
weld metal was largely affected by the phase 7(1976), pp.46-52.
[3] UEDA Y., KIM Y-C., CHEN C. and TANG Y-M. : QJJWS,
transformation in the cooling process although the bead 2-1(1984), pp. 89-97.
width of LBW (around 5mm) was extremely narrow
70
Structure optimization of air conditional compressor based on

†
reverse welding deformation model

LI Yongzhi *, LU Hao *, CHEN Junmei * and REN Liping **
KEY WORDS: (Air conditioning compressor) (Welding deformation) (Blade groove width) (Three-point
welding) (Phase transformation) (Thermal elastic-plastic finite element method)
1. Introduction
The FEM simulation of welding residual stresses and
distortions can provide valuable instructions for the
optimization of welding technology and structures. Under
the welding condition, the phase transformation in solid (a) Geometric model
state not only changes the strain-stress, but also affects the 5x108
thermal elastic-plastic
life evaluation for the structure. In order to accurately 4x108 thermo-mechanic-metallurgical
predict the distortion and stress during welding process, the 3x10 8
numerical analysis is usually performed using the thermal- 2x108

mechanic-metallurgical coupling model, and the effects
Axial stress / Pa
1x108
caused by phase transformation are also considered [1,2]. 0
Recently, significant progress has been made by researchers -1x108

in the modeling of phase transformation behavior of steel -2x108
[3-5]. Mathematical models are gaining acceptance as -3x108
powerful tools for residual stresses and distortions -4x108
prediction and structure optimization. -5x108
0 200 400 600 800 1000 1200 1400 1600
In this paper, a phase transformation model is Temperature/oC
developed to study the material thermo-mechanical (b) Relation between stress and temperature
behavior under a typical welding process. A reverse model Fig. 1 Thermo-mechanic-metallurgical mode results
based on thermal elastic-plastic finite element method is
developed to simulate the three-point welding of
compressor shell and cylinder.
2. Thermo-mechanic-metallurgical model and results The blade

A thermo-mechanic-metallurgical model is developed to groove
study the material thermo-mechanical behavior. The
geometric model is shown in Fig.1(a), and the result is
shown in Fig.1(b), both of the ends are fixed during the
simulation. The result shows that, as the temperature
increases the axial compressive stress becomes bigger, and (a)FEM model
during the cooling stage, axial tensile stress appears in the
model. Differences between the thermal elastic-plastic
model and the thermo-mechanic-metallurgical model
appear at the Ms point. In the thermo-mechanic-
metallurgical model, the axial tensile stress decreases
rapidly because of the transformation strain. But with
further cooling, the stress increased again.
3. Air conditioning compressor model and results

The FEM model of the air conditioning compressor is
shown in Fig.2(a), and the contour of temperature
distribution is shown in Fig.2(b). (b) The contour of temperature distribution
Fig. 2 Air conditioning compressor model
㻌 † Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding
㻌 * Shanghai Jiao Tong University, Shanghai, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Engineering Research Center, Gree Electric Appliances, Inc. of Japan
㻌㻌 Zhuhai, China
71
Structure optimization of air conditioner compressor based on reverse welding deformation model
Three parameters are discussed in our simulation, the

height of the compressor shell, material properties of the
cylinder, and whether the shell is in contact with the
cylinder. Figure 3 shows the width change of the blade
groove with different parameters. The results show that, the
height of the compressor shell has little effect on the width
change of the blade groove. The width change becomes
smaller when cast steel is used for the cylinder. In the
simulation, the Young’s Modulus of the cast steel is smaller
than the shell’s. And the width change can be decreased by (b) Case B (×30)
decreasing the material Young’s Modulus of the cylinder
material. When the shell is in contact with cylinder, the
width change is also decreased.
0.014
0.012
Width Change of the groove/mm
0.010
0.008
0.006
(c) Case C (×30)
height 60mm not contacted
0.004
height 220mm contacted Fig. 4 Contours of radial deformation under different
0.002 height 220mm not contacted conditions
height 220mm not contacted with different materials
0.000
0 5 10 15 20 4. Conclusions
Distance from the end/mm According to the simulation results, the following
Fig. 3 The width change of the blade groove with conclusions can be obtained:
different parameters (1) The height of the compressor shell has little effect
on the width change of the blade groove. The width change
The deformation of the shell with different parameters becomes smaller when cast steel is used for the cylinder.
is shown in Fig. 4. Three different cases are discussed: (2) When the shell and the cylinder are in contacted,
Case A, the shell and the cylinder are in contact, and the deformation of the shell is much smaller. And in the
using the same material properties. experiment, the measured cylinder roundness is 377.41ȝm,
Case B, the shell and the cylinder are not in contact, which is in very good with the case C.
using the same material properties.
Case C, the shell and the cylinder are not in contact, the Acknowledgement
cylinder using different material properties. This project is support by the National Natural Science
The results show that, the deformation of the Foundation of China (Grant No. 50975176)
compressor shell seems like a “flower”. When the shell and
the cylinder are in contact, the deformation of the shell is References
much smaller. The cylinder roundness of these three cases [1] Jun-yan LIU, Hao LU, Jun-mei CHEN, Jinyang LIU. Finite
are 229ȝm䚸416.2ȝm and 397.8ȝm. And in the experiment, element simulation of Satoh test taking into account
the measured cylinder roundness is 377.41ȝm, which is in transformation induced plasticity. Transactions of the China
very good with the case C. Welding Institution, 2008, 29(3):105-109.
[2] Jun-yan LIU 䠈㻴㼍㼛㻌㻸㼁䠈㻶㼡㼚 -mei CHEN. Experimental
analysis of transformation induced plasticity in 9Cr1Mo steel.
Front. Mater. Sci. China 2009, 3(1):61-66.
[3] Caner Simsir, Cemil Hakan Gür. 3D FEM simulation of steel
quenching and investigation of the effect of asymmetric
geometry on residual stress distribution. Journal of materials
processing technology, 2008, 2007:211-221.
[4] Caner Simsir, Cemil Hakan Gür. A FEM based framework for
simulation Application to steel quenching.
(a) Case A (×40)
Computational Materials Science, 2008, 44:588-600.
[5] Moumni, Z., et al. Theoretical and numerical modeling of the
thermo mechanical and metallurgical behavior of steel. Int. J.
Plasticity (2010), doi:10.1016/j.ijplas.2010.07.002.
72
Study on prediction of welding deformation for large-scale

structure by T-E-P FEM using 3D shell element†
ZHANG Xueyuan*, LUO Yu**, WANG Yang*
KEY WORDS: (T-E-P FEM) (Welding deformation) (Large-scale structure) (3D shell element) (Parallel
calculation)
1. Introduction stresses of 3d solid element model agree quite well with

Recently numerical simulations of industrial that of the 3d shell element model.
manufacturing processes have been widely studied, and
various methods of numerical simulation for welding 2.4 Comparison of plastic strain
mechanical behavior have been developed. But the reports Figure 3 displays the plastic strain in the Y-direction
about simulation involving large-scale structures, especially for the 3D solid model and 3D shell model at center cross-
by T-E-P FEM, were still rare. The reason maybe is a huge section in middle of plate. Both are almost the same
amount of computation time. It is possible to save
computation time by replacing 3D solid elements using 3D
shell elements.
In this paper, a bead-on-plate welding is the research
model, and simulations by T-E-P FEM have been
performed using software Abaqus. Through the comparison
of the calculation results using 3D solid and shell element,
the possibility of using 3D shell element to simulate
deformation of large-scale structure is confirmed. Then,
Mesh size effect has been discussed, and parallel
calculation was employed in calculating.
As an example, a typical large-scale hull double
bottom structure is modeling, and 3D shell element T-E-P
FEM was used to simulate welding deformation. The
feasibility of welding deformation prediction by 3D shell
element T-E-P FEM is verified.
2. The Comparison of 3D solid and shell T-E-P FEM

2.1 Research Model Fig.1 Comparison of temperature at center cross-section
The size of model is 1000mm, 500mm and 10mm for
length, width and thickness respectively. The smallest
element is 10mmx2.5mmx2.5mm. Heat input parameter
(Q/h2) is 13.0 (J/mm3), welding speed is 10mm/Sec.
The thermal properties and mechanical properties are
dependent on temperature, which reference to paper [1].
2.2 Comparison of temperature

Figure 1 shows the distribution of temperature by 3D
solid and shell element at center cross-section on the
surface of the plate when welding time is 50 sec. As in Fig.
1, it is found that the distribution of temperature is in good
agreement.
2.3 Residual Stress Analysis

Fig. 2 Comparison of von-mises residual stress at welding
The comparison of von-mises residual stresses is shown
line
2, also it is shown that the von-mises residual
in Fig.
* Graduate School, Shanghai Jiao Tong University, Shanghai, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
㻌㻌㻌 China Japan
** Shanghai Jiao Tong University, Shanghai, China
73
Study on prediction of welding deformation for large-scale structure by T-E-P FEM using 3D shell element
As seen from Table 1, it is clear that the results obtained

from using 3D solid and shell elements are consistent, and
cost time is three times less.
3. Calculation example
As an example, a typical of the hull structure, called
large-scale hull double bottom structure, is modeling, and
3D shell element T-E-P FEM was used to simulate welding
deformation.
3.1 Model and welding conditions

As Fig. 5, the length, the width and the height of the
Double Bottom Structure are 16125mm, 11860mm and
1750mm respectively. The element size is 100mm h
Fig. 3 Comparison of plastic strain at center cross-section 100mm, and the total number of elements is 123512, which
amounts to 426078 degrees of freedom. DS4 was used for
temperature field calculation, and the S4 shell element was
chosen appropriately for simulation of stress field. Material
2.5 Effect of Mesh Sizes properties are the same as above bead-on-plate model.
In order to improve calculation speed, parallel
calculation was performed by establishing a computer
cluster system composed of two server computers.
It takes about 15 hours for completing the
computation of temperature field and stress field with two
Dual-Core Xeon processors with 3.0 GHz clock speed.
3.2 The calculated results

Figure 5 shows the distribution of temperature by 3D
shell element. The six weldments on floor plate and
stiffener are proceeding.
Figure 6 displays welding deformation enlarged 200
times. Transverse and longitudinal shrinkage which most
are concerned is approximately 3.96mm and 2.56 occurring
at the middle of the double bottom.
So, the 3D shell element T-E-P FEM should be a
useful tool for prediction of welding deformation of large-
Fig. 4 Effect of Mesh Sizes on Welding Deformation
scale structure.
As Fig. 4 shows, as the size of the mesh increases, the
peak temperature at welding line will be gradually reduced,
when the size is 100mm, the temperature dropped to 693ć.
If the size is greater than 100mm, residual stresses on
welding bead began to decline. Also, transverse plastic
strain decreases with the mesh size increasing. From these
curves it can be suggested if mesh size is less than 100mm,
calculation results will not be greatly affected.
As a summary, the results of comparison between 3D
solid and shell models are listed in Table 1.
Table 1 The results of comparison between 3D solid

and shell models
Mesh Residual Shrink plastic Cost Fig. 5 Model of Double Bottom Structure and the temperature
size(mm) stress(MPa) age strain time(min) field
Solid 10x2.5x2.5 240.2 0.096 0.00120 140
Shell 2.5x2.5 240.7 0.094 0.00124 30
74
4. Conclusions
The conclusions of this study are summarized as
follows:
(1) Regarding bead-on-plate welding, the calculation
results obtained by 3D solid and shell element T-E-P
FEM are in good agreement.
(2) If mesh size is less than 100mm, calculation results
will not be affected greatly by mesh size
(3) By simulation of a typical of large-scale hull double
bottom structure, the feasibility of 3D shell element T-
E-P FEM was verified.
References
[1] Yu LUO, Hidekazu MURAKAWA and Yukio UEDA: Trans.
Fig. 6 Welding Deformation
Of JWRI, Vol. 26 (1997), No.2.467-475.
75
Fast finite element stress and deformation prediction for large

†
thick-wall welded cylinder with angle-inserting elbow
ZHANG Kerong *, ZHANG Jianxun *, HUANG Siluo**, QIU Yiqiang**
KEY WORDS: (Large thick-wall) (Fast prediction) (Stress evolution) (Roundness change) (Simplified models)
1. Introduction 2. Finite element modeling

During thick-wall vessel welding, due to the serious As shown in Fig. 1, thick-wall welded cylinder with
uneven heating on the thick-wall vessel during welding, angle-inserting elbow is composed of two parts, the wall
larger deformation easily occurs on the joint during welding thickness of both structures are 125mm. The temperature
and cooling. It is necessary to make prediction of the input imposed during each bead is showed in Fig. 2. All
characteristics of structure stress and deformation. parts of the joint are carbon steel 20G, whose properties are
In the numerical calculation of large thick-wall structure shown in Fig. 3. The specific process parameters are shown
welding, the calculation workload can be effectively in Table 1. The 3D finite element mode is shown in Fig. 4.
reduced by appropriate simplification, as in reference [1-2]. Table 1 Technological parameter
Three predictor models based on software ANSYS with
Parameter Value
simplification of bead, moving heat source, and both of
Welding speed / cm/min 16
them respectively are presented. As a result, the
Average time for single welding / min 100
characteristics of stress and deformation have been
predicted fast.
0.30
1650
³s
/G
Material properties
0.24
Pa
1500 -6
68º 0.18 ¢h10-2/ 10 /ć
Temperature T/ ć
Heat input
0.12
-3/[W/(mgć
)]
0.06
¬×10
Ch10-4/[ J/(kg·ć)]
50
0.00 E/GPa
36
0 500 1000 1500 2000
Unit˖mm 2550 Temperature t /ć
2.25 Time t / s Į: Linear expansion coefficient; ı s : Yield strength; E: Elastic modulus; C:
Specific heat; O: Thermal conductivity; ȡ(Density)=7.89×106kg/m3
Fig.1 Structure and groove of welded
Fig.2 Heat input and their duration Fig.3 Material property
cylinder with angle-inserting elbow
3. Comparison of simplified model The regions where the equivalent residual stress under 3
simplified models is up to 80%, 60% and 50% respectively
Three simplified models are established. The welding are compared as shown in Fig. 8. It can be seen that the
order and weld size after the beads is simplified to be 5 and methods of bead and moving heat source simplified have
are described as shown in Fig. 5. The simplification little effect on the overall stress of joint.
methods are given in Table 2. In order to explain the effect of simplification method
The stresses of point A at different locations along the on the stress evolution of joint, the process stress under 3
depth direction of the weld are compared as shown in Fig. 6. simplified models of point A at different moments are
It can be known that, the stress distribution under model A compared as shown in Fig. 9.
is most close to the typical description of stress distribution
of thick-wall vessel in other reference [3]. 4. Fast prediction
Stresses of region B at different locations along the Under the Model C, the computing time under this
vertical direction of weld are compared as shown in Fig. 7. simplified model can be shorten significantly. Therefore,
It can be known that the method of simplified bead is Model C whose bead and moving heat sources are both
obviously better than that of simplified moving heat source simplified is selected for fast prediction of joint stress in
when studying the stress within the same bead plane. this article.

* State key laboratory for mechanical behavior of materials, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Xian Jiaotong University, Xian, China Japan
** The Challenge Petrochemical Machinery Corporation of
㻌㻌 Maoming, Maoming,China.
76
Fast finite element stress and deformation prediction for large thick-wall welded cylinder with angle-inserting elbow
125
50mm Model A
5
100 Model B
Depth h / mm
Model C
4 75
125mm
3 50
2 25
1
0
10mm 135 150 165 180 195 210
Stress ³m MPa
Fig.5 Welding process and size

Fig.4 Finite element model of joint Fig.6 Equivalent stress in depth at point
description for 5 bead
250
Model A
Stress ³m MPa
Model B
200 Model C
150
100
0 150 300 450 600 750 50%ıs 60%ıs 80%

Distance d / mm
Fig.7 Stress with distance to the welding center at region B Fig.8 Equivalent stress with three simplified standards
Figure 10 shows the longitudinal and transverse stress
Table 2 Simplified methods
distribution on the internal and external surface of region B
Model Bead Moving heat source at different locations along the vertical direction of weld. It
A 5 No can be known from the figure, the stress on the external
B 1 Yes surface of the weld is obviously higher than that on the
C 1 No
internal surface.
200
250
60 Outer surface
200
Inner surface
Stress ³/ MPa
Stress ³MPa
Stress ³MPa
Stress ³/ MPa
150 Model A 200 Outer surface

Model A 40
Model B
100 Inner surface
Model B
Model C 150 Model C 20
100
0
100 0
50 -100
50 -20
0 5000 10000 15000 0 150 300 450 600 0 150 300 450 600
0 5000 10000 15000
Distance d / mm Distance d / mm
Time t / s Time t / s
˄a˅Internal surface ˄b˅External surface ˄a˅Longitudinal residual stress ˄b˅Transverse residual stress
Fig.9 Stress cycle on the internal and external weld at point A Fig.10 Stress of the weld with distance from the centerline
For the analysis of deformation characteristics of joints, Figure 12 shows the relative displacement of all points
the roundness change of the left and right ends on the on the elbow outer contour at different moments. At the
cylinder, the roundness change of weld curve, and the beginning of welding, elbow is far from the cylinder, finally
displacement of elbow outer contour are analyzed, the the distance between elbow and cylinder is smaller and the
research area is shown as in Fig. 11. axis curvature of elbow is larger.
Y direction
Elbow outer
contour
Original state
Welding initial
Welding completed
After cooling
Right end
Left end
X direction
Fig.11 Research region of displacement Fig.12 Displacement schematic diagram of elbow axis
Figure 13 shows the roundness change at the two ends Figure 14 expresses the displacement of all the points
of left and right on the cylinder. During cooling, the on the weld at different moments. It can be seen that the
roundness change of the cylinder is just opposite to that in angle between the symmetrical axis of weld and the axis of
the stage of welding. The elliptic deformation of circle at cylinder has an important influence on the deformation of
the left of the cylinder is smaller than that of the circle in the weld.
the right.
77
0 0 0
330 30 330 30 330 30
Original state Original state
Welding initial Original state
300 60 Welding initial 300 60 300 60 Welding completed
Welding completed Welding completed
After cooling
After cooling After cooling Measured results
270 90 270 90 270 90
240 120 240 120 240 120
210 150 210 150 210 150

180 180 180
Fig.14 Displacement schematic diagram of point on

Fig.13 Displacement schematic diagram of point on both ends of thick-wall cylinder
bead
(1) The process peak stress increases in case of simplified [1] J. Zhang a, P. Dong, F. W. Brust and et al. Nuclear
moving heat source model, and the process stress of the Engineering and Design, 195 (2000), pp.171-187.
joint with many beads or a very long welding time is
[2] S. Wen, P. Hilton and D. Farrugia. Journal of Materials
affected more significantly by the simplified bead model.
Processing Technology, 119(2001), pp.203-209.
(2) Under the model whose bead and moving heat sources
are both simplified, the distance between elbow and [3] R. Leggatt. International Journal of Pressure Vessels
cylinder as well as the roundness change of the cylinder, and Piping, 85 (2008), pp. 144-151.
are in a reverse state during welding and cooling.
78
Thermal elastic plastic analysis for welding problem of large scale

†
models
TANAKA Norihiro*, KAWAHARA Atsushi **, SERIZAWA Hisashi **,

MURAKAWA Hidekazu **
KEY WORDS : (Thermal elastic plastic analysis)(Welding)(Residual stress)(Distortion)(Iterative substructure

method)
1. Introduction
It has been more than three decades since the finite
element method was first applied to the welding simulation.
However, due to the poor performance of the computer,
application of the FEM was limited to small scale A B
laboratory models. On the other hand, the need for the
theoretical prediction of the welding distortion and residual
stress, especially in the industries, has kept growing. To
meet this demand, authors developed an FE code which is
specially designed for efficient computation so that
complex and large welded structures or welded parts
produced in industry can be simulated. In this paper, the
idea of iterative substructure method (ISM) [1-5] and its
advantage for large scale problems are discussed. Also, its A B’
ǻ
potential capability is demonstrated through an example
problem with more than million elements.
B
2. Concept of Iterative Substructure Method
If the problem can be separated into a large but constant Fig. 1 Concept of Iterative Substructure Method.
stiffness problem and a small moving nonlinear problem,
the computational time can be reduced by using an iterative
substructure method. As schematically shown in Fig. 1, the
region B which exhibits strong nonlinearity is limited in a
Solve A using stiffness of A’ and save matrix
small region compared to the whole model A to be analyzed. after forward elimination
In ISM, the problem is reformulated as follow.
(1) The region B is the region with strong nonlinearity.
(2) The region (A-B) is the mostly linear region. Extract displacement uǻ on ǻ
(3) The boundary 䂳 is the boundary between regions
(A-B) and B. Solve B under boundary displacement uǻ
(4) The virtual region A’ is the model in the past. The
difference from region A is that its stiffness is
unchanged until updated. Compute unbalance force on ǻ
(5) Solve the region (A-B) using the stiffness of A’ and {A̓-B}+B
solve the region B using current stiffness.
(6) The continuity on the boundary 䂳 is maintained
through the iterative procedure. Convergence check
The detail of the iterative solution procedure is shown in Next step

the following and in Fig. 2.
(a)Solve A using the stiffness of A’ and compute Fig. 2 Flow chart of iteration.
㻌 * Graduate School, Osaka University, Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Osaka University, Osaka, Japan Japan
79
Thermal elastic plastic analysis for welding problem of large scale models
Thickness : 2mm
Welding Line
Length : 100mm Width : 100mm
Fig. 3 Model for analysis.
㻡㻌㻝㻜㻡
Fig. 5 Geometry of weld joint with cross-section.
Thermal analysis
Mechanical analysis
㻡
㻠㻌㻝㻜
Computong time [s]
㻟㻌㻝㻜㻡
㻞㻌㻝㻜㻡
㻝㻌㻝㻜㻡
㻜 Fig. 6 Distribution of axial component of residual stress.

㻜㻞㻌㻝㻜㻡㻠㻌㻝㻜㻡㻢㻌㻝㻜㻡㻤㻌㻝㻜㻡㻝㻌㻝㻜㻢㻝㻚㻞㻌㻝㻜㻢㻝㻚㻠㻌㻝㻜㻢
Number of elements and the model with 1,208,000 elements can be computed in
Fig. 4 Relation between computing time and number of 434,010 seconds (120.5 hours).
elements for thermal and mechanical analysis.
4. Preliminary Computed Results for NRC Round
displacements in the whole model. If the updated
Robin
stiffness of A is used, save the stiffness matrix after
the forward elimination. The second example is the preliminary computation of
(b) Solve B by using the displacement on 䂳 computed in the welding residual stress in the nozzle shown in Fig. 5.
step (a) as the boundary condition. In this way, the This model is proposed by US Nuclear Regulatory
continuity of the displacement on the boundary 䂳 is Commission for International Weld Residual Stress Round
maintained. This solution process is nonlinear and the Robin [6]. As a preliminary analysis, the residual stress
Newton-Raphson iterative method is employed. produced by the welding between the nozzle and the safe
(c) Compute the unbalance force between the reaction end was computed. The outer and the inner diameter of the
forces from (A’-B) and B. safe end are 381 mm and 284.5 mm, respectively. This
(d) To recover the continuity of the traction, feedback the model is divided into 63,000 elements. There are 40 and 27
above unbalance force to step (a) and compute the passes on the outer and the inner sides. In the computation,
only the welding passes on the outer and inner surfaces are
correction for the displacement on the boundary 䂳.
computed using moving heat source and a stationary ring
(e) Repeat steps (a) through (d) until the convergence is
shape heat source (equivalent to axi-symmetric model) is
reached.
used for the rest of the passes. For this computation, the
total computing time for the mechanical analysis is 53.6
3. Capability of ISM for Large Scale Welding Problems hours. The distribution of the axial component of the
The model is a simple bead on plate welding model with residual stress is shown in Fig. 6. Through this preliminary
different width. In all cases, the thickness and the length of computation, it is found that the full computation using a
the plate is fixed as 2 mm and 100 mm, respectively. The moving heat source for all passes can be completed in about
width of the plate is increased from 100 mm to 12,000 mm 8 days.
so that the number of elements is increased from 18,000 to
1,208,000. An example for the case with 18,000 elements is 5. Conclusions
shown in Fig. 3. The relations between computing time and
ISM was developed based on the idea to separate the
the number of elements are shown in Fig. 4. For these
nearly linear region and the nonlinear region in an efficient
computations, Intel Xeon W5590 (Quad Core 3.33GHz,
way. In order to examine the effectiveness of this method,
96GB) was used under single core mode. According to
the bead on plate welding was analyzed as example. From
Fig.4, the mechanical analysis of the model with 18,000
that computation, it is found that the computational time is
elements can be completed in 6,542 seconds (1.8 hours),
drastically reduced by using ISM and its advantage
becomes greater when the number of elements increases.
80
Acknowledgment [3] A. Maekawa, M. Noda, S. Takahashi, T. Oumaya, H.

Serizawa and H. Murakawa: Quarterly Journal of the Japan
The author would like to acknowledge that this research Welding Society, 27 [2], (2009), pp.240-244.
work was partly conducted as a joint research with Institute [4] R. Wang, J. X. Zhang, C. Liu, H. Serizawa and H.
of Nuclear Safety System Inc. Murakawa: Science and Technology of Welding and Joining
14 [5], (2009), pp. 396-403.
References [5] L. J. Zhang, J. X. Zhang, H. Serizawa and H. Murakawa:
Science and Technology of Welding and Joining, 12 [8],
[1] H. Nishikawa, I. Oda, M. Shibahara, H. Serizawa and H. (2007), pp.703-707.
Murakawa: Proceedings of the 14th International Offshore
and Polar Engineering Conference, 4, (2004), pp.126-132. [6] “International Weld Residual Stress Round Robin Problem
Statement,” Version 1.0, US Nuclear Regulatory
[2] H. Nishikawa, H. Serizawa, H. Murakawa: Science and Commission, Office of Nuclear Regulatory Research,
Technology of Welding and Joining, 12[2], (2007), pp.147- Division of Engineering Component Integrity Branch,
152. December 14, (2009).
81
†
WANG Yang *, LUO Yu **,㻌㻌 ZHANG Xueyuan *
KEY WORDS: (Software Comparison) (T-E-P FEM) (Welding Temperature) (Welding Deformation) (Welding
Stress and strain)
1. introduction Comparison of plastic strain

Numerical simulation has been playing a significant Figure 2 displays the plastic strain in Y-direction by
role in manufacturing recently. The general Thermo-elastic- Abaqus, Ansys and Jwrian at center cross-section in middle
plastic (T-E-P) FEM software is now widely used in of the plate.
mechanical process as during welding. However, the Figure 3 is the curve of the temperature history and
research in comparing with in detail results using different plastic strain history at center that coordinate is (200, 0, 5).
T-E-P FEM software is rare. It is necessary to learn all the It is found that plastic strain from Abaqus and Ansys
differences of calculation results by different software for are good in agreement, yet that from Jwrian is a little
industrial applications. smaller than the others.
In this paper, three kinds of software (ANSYS,
ABAQUS and JWRIAN) are employed in T-E-P FEM
analysis for bead-on-plate welding, and temperature field
and stress field are discussed in detail through a series of
calculations. By comparing experimental results which are
published, the differences among results which are obtained
by different T-E-P FEM software are established.
2. Model for Analysis

Bead-on-plate welding is taken as the research model
herein. The length, the width and the thickness of the plate
is 400mm, 400mm and 10mm respectively. The material is
low-carbon steel. The FE model has 2720 solid elements
and 3690 nodes. The smallest size of element is
10mm×2.5mm×2.5mm.
The thermal properties and mechanical properties are
dependent on temperature, which reference to paper [1].
DC3D8 and SOLID 70 are used for temperature Fig. 1 Distribution of temperature at center cross-section
calculation for Abaqus and Ansys, and to simulate the stress
field, C3D8I and SOLID 45 are chosen for Abaqus and
Ansys respectively. In order to simplify calculation, the
moving welding arc is simplified as a cuboid interior
moving heat source.
3. Calculated Results
Comparison of temperature
Figure 1 shows the distribution of temperature at
center cross-section on the surface of plate when welding
time is 21 sec, and total heat input parameter (Q/h2) is 4.06
(J/mm3), welding speed is 10mm/Sec.
From Fig.1, it is clearly seen that temperature results
obtained from three kinds of software are consistent, the
peak temperature has difference a bit.
Fig. 2 Distribution of plastic strain at center cross-section

* Graduate School, Shanghai Jiao Tong University, Shanghai, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
China Japan
** Shanghai Jiao Tong University, Shanghai, China
82
Comparison of residual stress

The comparison of residual stresses in welding
direction(X) on surface at center cross-section is shown in
Fig. 4.
According to Fig.4, it is found that results from
Abaqus resemble those from Ansys, but the distribution
area of residual stress obtained from Jwrian is narrower
than Abaqus and Ansys.
Fig. 5 Relationship between transverse shrinkage and heat

input parameter
Figure 6 shows relationship between angular

distortion and heat input parameter. Seen as Fig.6, if the
heat input parameter Q/h2 is small, the angular distortion
obtained from calculator by the T-E-P FEM softwares are
agreement in experimented data. With the increase of heat
Fig. 3 Temperature and plastic strain histories input parameter Q/h2, the difference between the numerical
results and experimental data increases. Reason may be that
metal melting has not been considered in T-E-P FEM
analysis. In the case of Jwrian, better results can be
obtained in high heat input area compared with the other
software.
Fig. 4 Distribution of residual stresses at center cross-

section
Comparison of deformation Fig. 6 Relationship between angular distortion and heat

The curve of relationship between transverse shrinkage input parameter
and heat input parameter Q/h2 is Fig. 5. As seen from Fig.5,
the results calculated by the T-E-P FEM software agree Comparison of computed time
with the experimental data [2], and also that from Jwrian is a The computed time of temperature field and stress
little smaller than that. field are show in Table 1. From this table, it can be seen
that Abaqus takes the shortest time among the three kinds
of software in the same condition.
Table 1 comparison of computed time

Cost time Abaqus Ansys Jwrian
Temperature filed 7 22 8
(min)
Stress field (min) 36 90 200
83
4. Conclusions (4) If heat input is small, the calculated angular distortion is

The conclusions of this study are summarized as agreement with experiment data, with the increasing of
follows: heat input, the difference increases.
(1) The temperature results obtained from three kinds of (5) Abaqus takes the shortest time among the three kinds of
software are consistent; the peak temperature has a software in the same condition.
small difference.
(2) The calculated results of residual stress accord closely References
each other, but distribution area of Jwrian is narrower [1] Yu LUO, Hidekazu MURAKAWA and Yukio UEDA: Trans.
than Abaqus and Ansys. JWRI, Vol. 26 (1997), No.2.467-475.
(3) The calculated transverse shrinkages agree with the [2] Dean Deng: Doctoral Thesis, Osaka University, 2002, pp.21-
experimental data, yet that from Jwrian is a little small 22.
than experimental data.
84
Finite element simulation of multi-pass welding process with

rezoning technique†
Fast prediction for welding deformation and residual stress
HUANG Hui *, ZHAO Yao *, YUAN Hua *, HU Defang *
KEY WORDS: (Finite element simulation) (Multi-pass welding) (Rezoning technique) (Welding Deformation)
㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 (Residual Stress) (Computational efficiency)
1. Introduction The computational results with and without rezoning

Finite element simulation of welding process has been technique are compared.
widely employed in engineering where welding
deformation and residual stress are considered. One big 3. Results and Discussion
problem during thermal elastic-plastic simulation is the Figure 1 shows the shape and size of a multi-pass
severe demands of hard disk capacity and computation time, welded butt joint. Thermal-mechanical sequentially
especially for large structures with long weld length or coupled analysis procedure is employed in this study. Heat
multi-pass welding. Lindgren proposed an automatic input is simulated by surface and body combined heat
rezoning procedure in simulation of welding based on a source. It is significant to accurately evaluate temperature
graded hexahedral element [1]. Murakawa developed an distribution in prediction of reliable welding deformation
iterative substructure method to perform analysis on large and residual stress. Figure 2 shows temperature history at
scale welding problems [2]. To minimize the number of two specific points in the full model and rezoningmodel.
unknowns in finite element model, a rezoning technique is The results agree well for the two points in transient time.
developed to simulate the multi-pass welding process. The
local nonlinear zone around the pass close to the heat
source is modeled with a dense finite element mesh, while
the region of other passes is modeled with a coarser mesh.
Then the model is redefined pass by pass to represent the
filling of the metal and the motion of the weld arc. Three-
dimensional finite element simulations with and without
rezoning technique are performed to obtain transient
temperature, welding deformation and residual stress. By
comparing the results of the model, computational Fig. 1 Shape and size of the multi-pass welding joint
efficiency and accuracy of the proposed method is
confirmed.
2. Analysis Procedure and Rezoning Technique

In the rezoning model, the deformed geometry after one
welding pass is rebuilt by different nodes and elements, and
exact locations of the new nodes are determined by a large
number of high order simultaneous equations [3]. The
Newton-Raphson method is employed to solve the
equations and just several iterations are needed to achieve
convergence. Variables such as temperature, strain and
stress are mapped from the old mesh to the new mesh after
obtaining the equivalent solving space. The multi-pass
welding process is then simulated pass by pass, with the FE
model changed in the mesh density and the filling of metal.
Thermal and mechanical analyses are implemented by
three-dimensional FEM. The welding joint is also
simulated by thermal elastic-plastic analysis in full model. Fig. 2 Temperature history of two points
* Huazhong University of Science and Technology, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
85
Finite element simulation of multi-pass welding process with rezoning technique
Fig. 3 Angular distortion in each welding pass

Fig. 6 Comparison of simulation time for each welding
pass
Angular distortion at the middle cross section of the

plate normal to the weld line after each welding pass is
shown in Fig. 3. Transverse shrinkage and angular
distortion of the two different models after cooling are
shown in Fig. 4. It can be seen that the simulated results of
rezoning model agree very well with the full model.
Figure 5 shows Mises stress field on the middle

cross-section of the model with and without rezoning
technique. The material in the fusion zone exhibits high
stress level and most of the points have reached the initial
yield strength. The difference of residual stress
distributions between full model and rezoning model is
Fig. 4 Welding deformation of the multi-pass welding joint very small. Computational time for each welding pass is
shown in Fig. 6. The full model requires almost the same
time for each pass since the mesh is not changed during the
simulation. It can be found that computational time
increases by pass in the rezoning model. This can be
explained by the fact that the mesh scale becomes larger as
the pass number increases. The mesh of the rezoning model
for the last welding pass is the same with that of the full
model. Total simulation time of the model with and without
rezoning is listed in Table 1.
Table 1 Total simulation time
Simulation time (h)
(a)
With rezoning 107.8
Without rezoning 168.3
It should be noted that, the first five welding pass can

be simulated in half a model due to the symmet of the
problem. Then the full model can be obtained by reflecting
the half model to fulfill the consecutive passes. It can be
expected that more computational time will be saved
without loss in accuracy. In the present study, mesh
coarsening has not been implemented. The relationship
between coarsening criterion and solution accuracy is
(b) under investigation to gain more reduction in solution time.
Fig. 5 Comparison of Mises stress field on middle cross-
section: (a) without rezoning (b) with rezoning
86
Multi-pass butt joint welding process is simulated by [1] L. E. Lindgren, H. A. Haggblad, J. M. McDillb: a.s.oddy,
three dimensional FEM in both rezoning model and full Comput. Methods Appl. Mech. Engrg. 143(3)(1997), pp.401-
models. Transient temperature, welding deformation and 409.
residual stress calculated in rezoning model agree well with [2] H. Murakawa, I. Oda, S. Ito, H. Serizawa, M. Shibahara and
that of full model. Computational time of the simulation is H. Nishikawa: J. Kansai Soc. N. A. Japan, 243(2005), pp.67-
reduced by 36% with a rezoning technique for the studied 7 0 .
model. Effectiveness and efficiency of the proposed [3] S. B. Brown and H. Song: ASME J. Engrg Industry,
method is confirmed. 155(1993), pp.415-423.
87
Prediction and measurement of welding distortion of thin shell

†
structure
WANG Jiangchao *, MA Ninshu **, MURAKAWA Hidekazu **, TENG Bugang ***
and YUAN Shijian ***
KEY WORDS: (Welding Distortion) (Inherent Deformation) (Shell Structure) (Elastic Analysis)
(Thermal-Elastic-Plastic computation) (Finite Element Method)
1. Introduction
In the manufacturing industry, welding is commonly
used as a main joining process to assemble various parts to
a welded structure. However, welding distortion always
occurs during the welding process because of non-uniform C D 2
expansion and contraction caused by the heating and A
B E 1
cooling cycle at the weld and surrounding base material [1].
Distortion due to welding not only degrades the Top polar Bottom polar
performance of a welded structure but also increases its
production cost. In fact, it is impossible to completely
eliminate welding-induced distortion, but a welded structure
can be produced within a small tolerance through Fig. 2 Position of measuring points
minimizing the welding-induced distortion [2]. Therefore,
prediction and control of welding distortion have become of 3. Computational Approach
critical importance during assembly processes. The computational approach for welding distortion of
the spherical structure is divided into two steps. In the first
2. Experimental procedure step, the inherent deformations in a butt welded joint are
The research object is a spherical structure which estimated by a three dimensional thermal-elastic-plastic
consists of 16 bent thin shells and 2 circular polar plates. FEM. Then, in the second step, welding distortion induced
The spherical structure has been pre-assembled by tack by sequential welding of the spherical structure is computed
welds. The dimensions of this spherical structure are shown by an elastic FEM in which the inherent deformations
in Fig. 1. To evaluate welding distortion, five typical points predicted in the first step are used as the input data.
as shown in Fig. 2 have been selected to measure the
displacements after each welding line. [1] Estimation of inherent deformation using thermal-
elastic-plastic FEM.
The dimensions of a butt welded joint are 400mm×
400mm×1mm, shown in Fig. 3. The base metal is a low
carbon steel and the welding condition is shown in Table. 1.
Fig. 1 Dimensions of the spherical structure
Fig. 3 Dimension and mesh of model

* Graduate School, Osaka University, Suita, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
88
Prediction and measurement of welding distortion of thin shell structure
Table 1 welding condition

Element Number
Current(A) Voltage(V) Velocity(mm/s)
70 20 12
Using the software JWRIAN, temperature field,

displacement and plastic strains are estimated. Figure 4
shows the distribution of longitudinal and transverse plastic
strains along the central cross section of the model.
According to the definition of inherent deformation [3],
integration of plastic strains gives the inherent deformations
as shown in Table. 2. Z
㻜㻚㻜㻝
X Y
㻜
㻙㻜㻚㻜㻝 Fig. 5 Part numbers of spherical structure

㼜㼘㼍㼟㼠㼕㼏㻌㼟㼠㼞㼕㼍㼚
㻙㻜㻚㻜㻞 After the last welding line, the radial displacement

contour diagram of the spherical welded structure is shown
㻙㻜㻚㻜㻟 in Fig. 6 and the radial displacement of the selected points
during sequential welding is shown in Fig. 7. Because of
㻙㻜㻚㻜㻠
the strong constraint of tack welds, the circumferential
㼜㼘㼍㼟㼠㼕㼏㻌㼟㼠㼞㼍㼕㼚㻌䃔㼜㼤 length will be not changed due to welding. As a result, the
㻙㻜㻚㻜㻡
㼜㼘㼍㼟㼠㼕㼏㻌㼟㼠㼞㼍㼕㼚㻌䃔㼜㼥 points B and E have negative radial displacements (inward).
㻙㻜㻚㻜㻢
The points C and D have positive radial displacements
㻙㻠㻜㻙㻞㻜㻜㻞㻜㻠㻜 (outward). The largest deformation of the points B and E
㼥㻌㼏㼛㼛㼞㼐㼕㼚㼍㼠㼑㻌㻔㼙㼙㻕 will occur after the first welding pass and the welding
Fig. 4 Distribution of strains in the central cross section deformation will decrease with the progress of the other
welding lines. The largest deformation at the point C and D
1 1 will occur after the last welding line. The welding
h ³³ h ³³
Gx H xp dydz G y H yp dydz deformation increases after each welding line. The welding
distortion of the point A is the negative radial displacement
h which always increases after each welding line and it
Tx ³H ( z ) /( h 3 / 12)dydz
p
x
2 increases dramatically when welding the circular polar plate.
h In addition, the computational results of typical points have
Ty ³ H y ( z 2 ) /(h / 12)dydz
p 3
a good agreement with the measured results as shown in Fig
8.
Where, G x , G y and H xp , H yp are the inherent deformations
5.0+00
and plastic strains at longitudinal and transverse direction,
4.0+00
respectively. T x ,T y are longitudinal and transverse
3.0+00
bending.
2.0+00
Table 2 Inherent deformations
į x (mm) į y (mm) ș y (rad) ș x (rad) 1.0+00
-0.064313 -0.16865 -0.00001 0.000007 0.0+00
-1.0+00
[2]Elastic analysis with inherent deformation -2.0+00
Based on the inherent strain theory, welding induced
-3.0+00
distortion of the spherical structure can be calculated using
the known inherent deformations. Part numbers of the -4.0+00 Z
spherical structure are shown in Fig. 5. The welding -5.0+00 X
sequence is corresponding to the part member. Y
Component Max Min
Y-Direction Displacement 4.7461mm -4.5452mm
Fig. 6 Welding distortion of spherical structure
89
㻞 4. Conclusions
(1) Welding distortions of a spherical welded structure
㻝
have been predicted by an elastic FEM using the
㼃㼑㼘㼐㼕㼚㼓㻌㻰㼕㼟㼠㼛㼞㼠㼕㼛㼚㻌㻔㼙㼙㻕
㻜 inherent deformation estimated by thermal-elastic-

plastic FEM.
㻙㻝 (2) Computational results are in good agreement with
measurements, furthermore, the welding distortion at the
㻙㻞
different points changes differently after each welding
㻭 line.
㻙㻟㻮
㻯
㻙㻠㻰 References
㻱 [1] G Verhaeghe. Predictive Formulae for Weld Distortion – a
㻙㻡 Critical Review. England, Abington publishing (1999).
㻜㻞㻠㻢㻤㻝㻜㻝㻞㻝㻠㻝㻢
㼣㼑㼘㼐㼕㼚㼓㻌㼜㼍㼟㼟 [2] Dean Deng, Hidekazu Murakawa, Wei Liang. Numerical
Fig.7 Radial displacement (Positive outward) of the Simulation of Welding Distortion in Large Structures. Comput.
Methods Appl. Mech. Engrg. 196(2007) 4613-4627.
selected points during sequential welding
[3] Murakawa Hidekazu, Deng Dean, Rashed Sherif and Sato
㻞 Shinji. Prediction of Distortion Produced on Welded
Structures during Assembly Using Inherent Deformation and
㻝 Interface Element. Proceedings of international conference on
welding science and engineering, 2009, Shanghai, China.
㼃㼑㼘㼐㼕㼚㼓㻌㻰㼕㼟㼠㼛㼞㼠㼕㼛㼚㻌㻔㼙㼙㻕
㻙㻝
㻙㻞
㻙㻟
㻯㼛㼙㼜㼡㼠㼍㼠㼕㼛㼚㼍㼘㻌㼞㼑㼟㼡㼘㼠㻌㼛㼒㻌㻼㼛㼕㼚㼠㻌㻭
㻙㻠㻹㼑㼍㼟㼡㼞㼑㼐㻌㼞㼑㼟㼡㼘㼠㻌㼛㼒㻌㻼㼛㼕㼚㼠㻌㻭
㻯㼛㼙㼜㼡㼠㼍㼠㼕㼛㼚㼍㼘㻌㼞㼑㼟㼡㼘㼠㻌㼛㼒㻌㻼㼛㼕㼚㼠㻌㻯
㻹㼑㼍㼟㼡㼞㼑㼐㻌㼞㼑㼟㼡㼘㼠㻌㼛㼒㻌㻼㼛㼕㼚㼠㻌㻯
㻙㻡
㻜㻞㻠㻢㻤㻝㻜㻝㻞㻝㻠㻝㻢
㼃㼑㼘㼐㼕㼚㼓㻌㻼㼍㼟㼟
Fig. 8 Comparison between computational and measured
result of point A and C
90
Investigation on ductility dip cracking susceptibility of filler metal

†
82 in welding
CHEN Jingqing* and LU Hao*
KEY WORDS: (Ductility dip crack) (Welding) (Inconel600) (Finite element method)
1. Introduction
The Ni-base alloys have widely been used in nuclear
power plant, particularly to variety pipe welding.
Ductility Dip Crack mainly happens in a Ductility Dip
Temperature Range (DTR) below the solidus temperature
when a stroke is exerted[1]. Currently, among all the
Ni-base alloys that have been used, Inconel600 is a kind
of Ni-Cr-Fe alloy with excellent high temperature
strength and corrosion resistance. A significant amount of (a) Welding orientation ˄b˅Shape of samples
research has been performed to identify the mechanisms Fig. 1 Schematic diagram of sample
of DDC. Rines and Wray’s [2] work shows that DDC is 2
formed by void accumulation during shear loading, Samples are heated to 1000 & and held for 10s. And
which has great similarity to creep cracking. Another then cooled to a certain temperature (750ćˈ850ćˈ
hypothesis is studied by Zhang, et al. [3], who believe that 900ćˈ950ćˈ1000ćˈ1050ć), a stroke is loaded after
intergranular precipitate, intergranular sliding and holding the temperature for 10s. The stroke is also held
boundary tortuosity have complex effects on DDC for 10s, later, cooling till room temperature. Along with
susceptibility. And K. C. WU and R. E. [4] Herfert think the surfaces holding at 1100ć, 1150ć, 1200 ć, the
that appearance of DDC is due to grain boundary critical strain of DDC is found.
weakening, as intergranular strength be comes lower then Finally, corroding on the sample surfaces, optical
intragranular strength when heated up to a certain microscope and SEM are used to observe the surface
temperature. This work mainly studies DDC cracks and microstructure.
susceptibility of Filler Metal 82 under different stress 1200
states.
1000
2. DDC susceptibility test in uniaxial stress state 800

Temperature / OC
Filler Metal 82 strip is used for study and overlay 600

welding is performed on steel for 3 layers (12mm),
shown as Fig. 1a. To avoid components fluctuation by 400
steel, only the upper layers are chosen to make samples

by wire cutting. The shape of samples is shown as Fig.
200
1b. Spot welding (diameter about 7mm) in both sides of 0

0 10 20 30 40 50 60 70
samples is required. Time / s
First, Zwick and Gleeble machine are used for Fig. 2 Temperature history loading
tensile test to find the ductility dip range, and
Yield strength and elongation of FM82 decrease with
Stress-Strain curves under different temperature are
increasing temperature, from the figure, the stress-strain
achieved. Later, Strain to Fracture(STF)tests take the
curves have obvious hardening periods from room
temperature history loading, as shown in Fig. 2, at DTR
of DDC. temperature till 850ć. On the other hands, yield
platform appears in the stress-strain curves above 950ć.

* Materials Science and Engineering School, Shanghai Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Jiaotong University, Shanghai 200240, China Japan
91
Investigation on ductility dip cracking susceptibility of filler metal 82 in welding
It indicates that intergranular strength is inferior to 0.16
intragranular strength at lower temperature. For most of 0.14

the deformation happens intergranularly, dislocation 0mm
1mm
0.12
slipping and climbing lead to a hardening period. With 2mm
3mm
temperature increasing, materials strength decreases, till 0.10 4mm
a certain temperature, intragranular strength be comes 0.08
5mm
6mm
inferior to intergranular strength, which results in grain
Strain
Critical strain of DDC
boundary ˄GB˅, sliding the main form of deformation. 0.06
As DDC is due to intergranular cracks at high 0.04

temperature and caused by uncoordinated intergranular
0.02
deformation and voids accumulation, FM82 is much
more susceptible to DDC above 900ć. At high 0.00
temperature above 1100ć, the strengthened 700 800 900 1000 1100 1200 1300 1400
re-crystallization can prevent the crack propagation, Temperature / oC
which reduces the DDC sensitivity effectively. [5] (a) Welding speed of 2mm/s
According to STF results, from 900Υto 1200ćwith 0.16
a stroke rate of 0.5mm/s, the minimum critical strain of 0.14

FM82 is less than 3% and the most sensible temperature
0.12 0mm
is about 1100ć, as Fig. 3 shows. 1mm
0.10 2mm
0.16
Equivalent strain
3mm
4mm
0.08
0.14 5mm
6mm
Critical strain of DDC 0.06 Critical strain of DDC
0.12
0.04
Equivalent strain
0.10
0.02
0.08
0.00
0.06
700 800 900 1000 1100 1200 1300 1400 1500
0.04 Temperature / oC
0.02
700 800 900 1000 1100 1200
(b) Welding speed of 5mm/s
o
Temperature / C Fig. 5 Equivalent strain changing with temperature
Fig. 3 Critical strain at different temperature
gets across the sensitive range. It means that the strain at
this location is higher than critical strain and prone to
3. DDC susceptibility under complex stress state DDC propagation.
FEM model of TIG welding is built up by ABAQUS When raising the welding speed in the case of the
common software with size of 100×100×2mm plate. The same weld width, in light of conductive time, strain
welding parameter used are as follows, current I=100A, changes more behind the temperature peak compared to
voltage U=10V, welding speed Ȟ=2mm/s, and a double speed of 2mm/s. Thus deformation is slight in DTR.
ellipsoid heat source is used. Figure 4 shows the From the curve of equivalent strain increment to
distribution of welding temperature. temperature (Fig. 5b), the position around the weld has
less DDC susceptibility.
According to the simulation results of single-pass
welding, welding strain decreases against distance to the
fusion line. Moreover, optimizing welding parameters,
such as increasing welding speed, can effectively
decrease DDC susceptibility. With the increase of
welding speed, strain changes respectively behind the
temperature peak, which enables deformation to avoid
the sensitive temperature range.
Fig. 4 Temperature distribution of single pass welding

4. Conclusions
According to the experiment and simulation results,
In order to evaluate the DDC susceptibility, the the following conclusions can be obtained:
equivalent strain increment to temperature curve is ˄1˅STF test samples show that the minimum critical
achieved at DTR (900-1350ć). As Fig. 5a shows, when strain of FM82 is less than 3% at 1100Υ. GB weakening
the welding speed is 2mm/s, the curve of 3mm to weld and sliding is the main reason for DDC formation by the
92
tensile test. When deformation is over the critical strain [1]Tang Zhengzhu, Chen PeiYing and Wu Wei. Influence
GB can endure, void accumulation results in crack Mechanism of Nb on Ni-based alloy DDC Susceptibility.
propagation perpendicular to loading. Transactions of the China Welding Institution, 2008, 29(1):
109-112. (in Chinese)
˄2˅By the FEM model of single pass welding, 3mm
[2]Rhinestone, F. N. and P. J. Wray. Investigation of the
from weld center has the most susceptibility at this Intermediate Temperature Ductility-Dip Cracking in
welding condition. Upon the same weld width, Austenitic Stainless Steels and Ni-base Alloys. Welding in
simulation shows that increasing welding speed can the World, 2002. 46(7/8): 32-40.
effectively improve DDC resistance. [3]Zhang. Y. C, Natsuda. H, Matsuda. F. Weldability of
Fe-36%Ni alloy (Report III). Transactions of JWRI, 1985,
14(1): 107-114.
Acknowledgement [4]K.C.Wu and R.E. Herfert. Microstructural Studies of Rense
This project is support by the National Natural Science 41 Simulated Weld Heat-Affected Zone. Welding J,
Foundation of China (Grant No. 50975176) 1967(46):32.
[5]BY F. F. Noecker, J. N. Dupont. Metallurgical Investigation
into Ductility Dip Cracking in Ni-Base Alloys: Part II.
References Welding Research, 2009, 88(3): 62-77.
93
Prediction of welding deformation for double bottom structure in

†
cargo hold of 50000 DWT multipurpose ship
LI Jing*, LUO Yu*
KEY WORDS: (Welding Deformation) (Inherent Deformation) (Accuracy Control) (WSDP)
1. Introduction
Double bottom is a typical unit of hull construction, and This double bottom block is divided into several
the prediction of its welding deformation is essential for components, such as the inner bottom plate, floor plates,
hull structural design and accuracy control of shipbuilding. shell plate, longitudinal girder, which are assembled
Three-dimensional thermal elastic-plastic FEM can separately at five steps as below, and shown in Fig. 1.
simulate the whole welding process, but it takes huge inner bottom plate => longitudinal structure => floor plate
calculation time and is only applicable to welding and stiffener => straight shell plate => curved shell plate.
mechanics behavior analysis of welded joint or small
structures. In this paper, through a large amount of
computation and measurement, a simple calculation formula 3. The Finite Element Model
The finite element model is established by software
of inherent deformation which relies on thickness of plates
HyperMesh. According to symmetry, a half of the
is proposed. Based on the inherent deformation calculated
block structure is meshed with quadrilateral elastic
by the simple formula [1][2], the deformations of the double
shell element [3]. There are 1730 model nodes and 2108
bottom structure in NO.6 Cargo of 50000 DWT
elements. Figure 2 depicts the finite element model
multipurpose ship are predicted by special software WSDP.
and constraints. X axis (longitudinal) is along the bow
The feasibility of inherent deformation database and simple
direction, Y axis (transverse) is along the port
formula is verified for the numerical results and agrees well
direction of the ship and Z axis (vertical) is along the
with the experimental data.
upward direction to the shell plate. 151 fillet welded
2. Production Process of the Double Bottom Structure joints were employed.
The 50000 DWT multipurpose ship is a kind of welded
steel ship with double shell structure. In this paper the block
1C14P/C/S has been taken as specimen of study. The
specimen’s width is 32250mm, length is 11860mm, and the
height is 1750mm. The steel-type of inner bottom plate is
GLDH32, and inner bottom longitudinal is GLAH32 while
in other area is GL-A.
Step1, Step2 Step3

Fig. 2 Finite Element Model of Double Bottom and
Constraints
4. Formula of Inherent deformation
The heat input is the main factor of inherent
deformation. According to the welding technology used in
hull, the total heat input is almost determined by the
Step4 Step5 thickness of plates. Therefore, inherent deformation was
considered as a function of the thickness of plates. The
simplified inherent deformation formulas are proposed as:
Fig. 1 Assembly and Welding Sequence
* Graduate School, Shanghai Jiao Tong University, Shanghai,China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Shanghai Jiao Tong University, Shanghai, China Japan
94
Prediction of welding deformation for double bottom structure in cargo hold of 50000 DWT multipurpose ship
T f 0.016 KEh 2 ( N ) (1) 21

Step 2
G 0.006 Kh (mm) (2)
Displacement along the ship width (mm)

Step 3
18 Step 4
Where T f is Tendon force, į is the transversal shrinkage, Step 5
E is the elastic modulus, h is the thickness of plates and K is 15 Measured Value
the correction coefficient, its value is between 0.6~1.0.
Since the main concern of shipyard is shrinkage of hull 12
structure, in order to simplify the computation, the angular
deformation has been neglected. The welding deformations 9
of this block are predicted using the inherent deformation
calculated by formula (1) and (2). 6
3
5. Calculated Results
Figure 3 displays the distribution of welding 0
deformation along the longitudinal and transverse direction, 0 1 2 3 4 5 6 7 8 9 10 11
Along the ship length, x (m)
and the deformation enlarged 100 times, the dashed line is
the original contours of the structure. (a) Along the ship length
21
Figure 4 expresses the shrinkage curve along the Step 1
Displacement along the ship length (mm)

Step 2
longitudinal and transverse direction at each step. The black Step 3
18
curve depicts the actual displacement obtaining by Step 4
measurement. Step 5
15
Measured Value
12
0
0 2 4 6 8 10 12 14
Along the ship width, x (m)
(b) Along the ship width
Fig. 4 Comparison of experimental and computational
displacement by five steps
As Fig. 4 (a) reveals, the longitudinal shrinkage

gradually increases with the welding sequences carrying on,
(a) Along the ship length and the maximum deformation is approximately 14.5mm
occurring at the middle of the double bottom. It is indicated
by comparison that the computational result agrees well
with the experimental data. The similar conclusion can be
acquired from Fig. 4 (b).
6. Conclusions
Based on the discussion above, we can conclude
the following.
(1) The simple inherent deformation formulas for hull
construction are obtained through a series of
thermal elastic-plastic calculation and production
experience:
Tf 0.016 KEh 2 ( N )
G 0.006 Kh (mm)
Where T f is the Tendon force, į is the transversal
(b) Along the ship width shrinkage, E is elastic modulus, h is the thickness
Fig. 3 Distribution of Welding Deformation of plates and K is the correction coefficient, its
value is between 0.6~1.0.
95
(2) The deformation of the whole structure along the References

longitudinal and transverse direction is 12mm and [1] Y. Ueda, H. Murakawa, N. Ma, Y.Luo, J. Wang:
13mm predicted by software WSDP based on the Computational Methods and FEM program of Welding
inherent strain method. This result agrees well with Deformation and Residual Stress (in Chinese), Sichuan
University Press, (2008), pp.6-7.
the measured value.
(3) The inherent strain method is practical, accurate [2] Y. Luo, H. Lu, Z. Zhu: J. Journal of Marine Technology,
and easy for calculation, so it can be a useful tool 2 (2005) pp.35-39.
for prediction of welding deformation of hull [3] P. Michaleris, A. DeBiccari: J. Welding Research
construction. Supplement, April (1997), pp.172-180.
96
Microstructure and mechanical properties of overlaying specimens

†
in GMAW hybrid an additional longitudinal electromagnetic field
LUO Jian*
KEY WORDS: (Thermal mechanical property) (GMAW) (Magnetic field) (Overlaying welding)
(Microstructure)
1. Introduction
Hot forge moulding has several remarkable advantages,
including high working performances, high precision, high
wear resistance (especially the red hardness) and good
ductile plasticity, the bimetal material used in hot forge
mould is subjected to the rigorous working environment on
the hot forge process. The GMA Welding with a
longitudinal electromagnetic field (LMF-GMAW) is one of
the overlaying welding methods, which is of low cost and
the high performance to manufacture the bimetal thermal
forming mould. However, there is still a lack of practical
detailed understanding of the thermal mechanical property
about the LMF-GMAW work pieces.
In this paper, we focus on the need for understanding Fig. 1 Diagram of the LMF- GMAW overlaying system
the thermal mechanical property of these work pieces with
overlaying hard alloy components on the carbon steel base
by using the LMF-GMAW method. 㸦 d㸧㸦 b㸧
2. A New Experimental Method

The LMF-GMAW overlaying system consists of an
induction coil with 350 turns and a multifunctional
excitation power source, which can provide the coil with a
variable polarity pulse current. The coil is filted on the
torch and it can create a double polarity alternating
electromagnetic field, because the direction of the 10μm 2mm
additional magnetic field is coaxial with the axis of welding 㸦a
arc, so it is called the longitudinal magnetic field. The basic 㸦c㸧
principle of LMF-GMAW overlaying system is
schematically shown in Fig. 1. The based material Q235
carbon steel (0.14~0.22% C, 0.12~0.3% Si, 0.3~0.65% Mn,
P and S controlling content, wt%) is used. The wire is the
Cr-Ni-Mo series flux-cored CO2 arc welding wire, namely
414N (11.47% Cr, 3.02%Ni, 0.707% Mo, 0.055%C,
0.67%Mn, 0.2Si%, 0.013%W, 0.010Nb%, 0.011%V, 10μm
0.054%Cu, 0.006%Co, 0.023%Ti, 0.001%B, 0.089%N,
0.005%As, 0.006%S, 0.016%P, wt%). Fig. 2 Microstructure of the surface deposited layer on
The welding parameters are listed as follows: LMF-GMAW work pieces
welding current is 200A, welding voltage is 28V, hybrid
electromagnetic field is 0.02T, Preheating temperature is
200Υ, Magnetic field frequency is 10Hz, CO 2 shield gas
flowing is 18 L/min, welding speed is 520 mm/min.

* The State Key Lab of Mechanical Transimission, Chonging Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
University, China Japan
97
Microstructure and mechanical properties of overlaying specimens in GMAW hybrid an additional longitudinal
㸦e㸧㸦d㸧 3. Results and Discussion

Figure 2a and b show overlapping specimen and can be
divided into three zones: base metal (seen in Fig. 2c),
transition layer (seen in Fig. 3c) and surface layer (seen in
Fig. 3e). Fig. 2d shows the grain is rough in the heat
affected zone (HAZ), there is little obvious boundary from
the base metal to the transition layer. But there is no
obvious boundary line between the transition layer and the
10μm 10μm surfacing layer shown in Fig. 3d. The microstructure of the
㸦c㸧
㸧 transition layer is made up of some reticular formations,
㸦a㸧
㸧㸦b㸧
㸧
which look like a spiked shape in the grain (shown in Fig.
3c). The microstructures of the surface layer are some
regular lath martensite phases and dispersed hard particles
resulting in a high wear resistance performance (shown in
Fig. 3e).
Figure 4 shows the hardness value of the surface layer
of the LMF-GMAW overlaying specimen is obviously
2mm 10μm higher than that of a conventional GMAW overlaying
specimen. But the hardness of LMF-GMAW overlaying
Fig. 3 Microstructure of the transition deposited layer on specimen increases continuously and smoothly depending
LMF-GMAW work piece on the distance from base metal, this typical hardness
distribution is a very ideal distribution status, especially for
the application of hot forming mould, which indicates that
the gradient deposited layer has a good ductility and joining
strength. So the hardness on the surface layer can be
matched to the wear requirement, which is proved by the
following wear experiment.
The hot compression experiment is used to evaluate the
thermal mechanical property by a GLEEBLE-1500D
machine in the hot forming mould’s application
environment. The thermal mechanical property shows the
deformation resistance of the LMF-GMAW overlaying
specimen is higher than that of general GMAW overlaying
specimen for the same welding condition. The average
difference value of true stress is near 400Mpa between the
LMF-GMAW specimen and GMAW specimen. The
deformation resistance of LMF-GMAW overlaying
specimen is much greater than that of the general GMAW
Fig. 4 Hardness of overlaying workpiece overlaying specimen, in other words, the thermal
mechanical property of LMF-GMAW specimen is much
better than that of general GMAW overlaying specimen,
shown in Fig. 5. After some hot compression experiments,
cracks are generated in the general GMAW specimen, but
not in LMF-GMAW specimen, The different deformation
shapes also show the hybrid additional longitudinal
electromagnetic field can improve ductile plasticity of
overlaying work pieces.
The wear testing result demonstrates that friction loss of
the LMF-GMAW overlay specimen is lower than that of
conventional GMAW overlaying specimen, the friction loss
is decreased by an average 5% value, so the wear resistance
property of the LMF-GMAW overlaying specimen is
significantly improved. It also means that the additional
longitudinal magnetic field can effectively improve the
Fig. 5 True stress- strain curves of overlaying work pieces wear resistance performance of GMAW overlaying work
with a 70% deformation ratio and 5s -1deformation rate pieces, besides the key material factors. The affecting
speed on the condition of 600Υ deformation temperature mechanisms of LMF are given in our previous paper [1].
98
4. Conclusions
Based on the comparison study of microstructure and
mechanical properties between LMF-GMAW specimen and
general GMAW, we conclude that LMF overlaying method
can increase surface hardness, reduce surface friction loss,
improve wear resistance, and enhance the thermal physical
mechanical property of specimens.
References
[1] Luo J, Lin Y, Luo Q and Wu YX, Sci. Technol. Weld. Join.,
(a) LMF-GMAW work piece 9(2004),pp 465-469.
(b) GMAW work piece

Fig. 6 The deformation shape of work pieces after hot
compression experiment
99
Flowing behaviors affected by different parameters and multi-

materials in GTA weld pool hybrid a longitudinal electromagnetic
†
field
LUO Jian*
KEY WORDS: (Welding pool) (GTAW) (Magnetic field) (Flowing behaviors) (Different parameters)
1. Introduction (a (b
The electromagnetic field hybrid arc welding technique
is applied in many manufacturing fields, however there is a
lack of detailed understanding of flowing behavior of t=1.0s t=1.0s
molten metal at a weld pool during GTA welding hybrid of
longitudinal electromagnetic field (LMF-GTAW). For
example, the impact of longitudinal electromagnetic field to
the flowing behaviors of weld pool is not yet clear. Because
the hybrid electromagnetic field can not only affect the
behavior of the welding arc, but also change the driving
force and flowing of molten metal at the weld pool.
In this paper, we focus on the need for understanding
weld pool’s flowing behavior affected by different
parameters and multi-materials in LMF-GTAW using a Fig. 1 The flowing at AlCu4SiMg aluminum alloy welding
numerical simulation research method. pool: (a) GTAW; (b) LMF-GTAW.
2. A New Quasi-3D Transient Model

The weld pool is described relative to a cylindrical
coordinate, assuming rotational symmetry around the arc
axis owing to the fixed arc in GTAW. The flowing is
assumed to be laminar, and a quasi-three-dimensional
t=1.4s t=1.4s
transient model is built up. The key additional
electromagnetic driving body force expression and
simulation procedure are given in our previous paper [1].
The typical materials, namely, AlCu4SiMg aluminum alloy,
Q245R (STB42) carbon steel and 1Cr18Ni9Ti stainless
steel are calculated. The different welding parameters,
including surface tension coefficient welding current,
magnetic induction and magnetic direction, are considered
in the quasi-three-dimensional transient model and
simulation procedure [2]. The basic welding current is 100 Fig. 2 The flowing affected by surface tension coefficient in
A and hybrid electromagnetic field is 0.01T in this paper.
LMF-GTAW: (a) 1. ; (b) -1.

Figure 1 shows that the LMF quells the molten metal 3. Results and Discussion
motion on the depth direction (Z) and increases the radial Figure 2 shows the surface tension coefficient can
motion(R), the velocity on the surface of weld pool and the change the flowing direction, the large surface tension
width. Same conditions are carried out in GTAW and LMF- coefficient (absolute value) makes the radius of the stable
GTAW. circular loop decrease. The centre of circular loop has also
a general exodus, the flowing in homogeneity increases and
the speednear the weld pool’s surface is higher than that of
* The State Key Lab of Mechanical Transimission, Chonging Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
University, China. Japan
100
Flowing behaviors affected by different parameters and multi-materials in GTA weld pool hybrid a longitudinal
other parts that are associated with surface tension (b)
(a) t=1.0s
coefficient absolute value.
Although a strong hybrid electromagnetic field can
make a strong stirring motion, the increased magnetic t=1.0s
induction has little change on the flowing mode or shape on
the ROZ cross-section of weld pool. But the flowing
velocity of molten metal is held in the ROZ plane, as shown
in Fig. 3. The strong stirring behavior is one of reasons.
Undoubtedly, the increased welding current can lead to
fast flowing, shown in Fig. 4. It is also contribute to the
stable flowing path and uniform circular loop. The “step-
style” about the flowing loop disappears at the developing
period of the weld pool. A stable even flowing status is
formed at the welding pool with the big welding current, as
a result of higher temperature.
Fig. 5 Flowing at STB42 carbon steel LMF Weld pool:
(a) (b)
(a) ROZ cross-section; (b) stirring rotation motion.
(a) (b)
t=1.4s t=1.4s
Fig. 3 The flowing affected by magnetic induction in LMF-

Fig. 6 Flowing at 1Cr18Ni9Ti stainless steel LMF weld
GTAW: (a) B=0.02T; (b) B=0.03T. pool: (a) ROZ cross-section; (b) stirring rotation motion.
(a) (b) (b)
(a)
t=0.2s t=0.2s
Fig. 4 The flowing affected by welding current in LMF-

Fig. 7 Flowing at AlCu4SiMg aluminum alloy LMF weld
GTAW: (a) I=150A; (b) B=180A.
pool: (a) ROZ cross-section; (b) stirring rotation motion
with an inverse direction of magnetic field.
101
Compared to the ferrous materials, the non-ferrous

(a) (b) metal (such as aluminum alloy) also has an obvious stirring
rotation motion around their symmetry axis (oz axis). In
t=1.0s t=1.0s particular, the direction of stirring rotation motion is also
changed, but the stirring strength is not changed, while the
direction of the hybrid electromagnetic field changes at
LMF-GTA welding pool, shown in Fig.7b.
Figure 8 shows the temperature field at LMF-GTA
welding pool of AlCu4SiMg aluminum alloy and STB42
carbon steel respectively, when the welding time is 1.0
second. The STB42carbon steel has a higher temperature
than that of AlCu4SiMg aluminum alloy, resulting from
material properties about the heat transfer on traditional or
Fig. 8 The temperature field of LMF-GTAW: (a) STB42 LMF welding process.
carbon steel; (b) AlCu4SiMg aluminum alloy.
4. Conclusions
Figures 5, 6 and 7 shows the flowing at the LMF-GTA The LMF quells the molten metal motion on the
welding pool with different materials, including STB42 direction of depth, increases the radial motion and the
carbon steel, 1Cr18Ni9Ti stainless steel and AlCu4SiMg velocity near the surface of weld pool. The surface tension
aluminum alloy respectively. The 1Cr18Ni9Ti stainless coefficient can change the flowing direction. The increased
steel has the highest flowing velocity due to the lowest magnetic induction can hold the flowing velocity of molten
thermal conductivity properties. metal on the ROZ plane. The 1Cr18Ni9Ti stainless steel
Under the influence of hybrid magnetic field, the has the highest flowing and stirring velocity due to the
maximum stirring speed of 1Cr18Ni9Ti stainless steel is not thermal physical properties in the material.
present at the middle of the radius with the 1.10mm depth
shown in Fig.6b. The curve of stirring velocity is also not of References
the symmetry shape. The peak is close to the welding [1] Luo J, Luo Q, Lin YH and Xue J: Weld. J., 82(2003), pp
seam’s centre because of the thermo-physical properties. 202s-206s.
[2] Luo J, Jia CS, Wang YS, Xue J and Wu YX: Acta Metall. Sin.,
37(2001), pp212-219.
102
Concept of inherent strain, inherent stress, inherent deformation

and inherent force for prediction of welding distortion and residual
†
stress
MURAKAWA Hidekazu *, DENG Dean ** and MA Ninshu ***
KEY WORDS: (Inherent strain)(Inherent stress)(Inherent deformation)(Inherent force)(Prediction)(Elastic

analysis)(Residual stress)(Distortion)
1. Introduction and the transverse inherent strains H x* and H *y . The

There are two methods which can be employed for the shrinkage of an element can be represented by distributed
prediction of welding distortion and residual stress. One is inherent strain as shown in Fig. 1.
the thermal elastic plastic analysis in which the welding is Transverse inherent strain H x* (3)
treated as a transient nonlinear problem [1]. The other is the
inherent strain method in which the distortion and residual Longitudinal inherent strain H *
y
(4)
stress are computed by elastic analysis using the inherent
strain as initial strain [2, 3]. They have both advantages and 4. Inherent Stress in Thin Plate
disadvantages. The latter is advantageous in computational Through the constitutive relation, the inherent strains
time and disadvantageous because the detail of the welding H x* , H *y are transformed into inherent stresses V x* , V *y .
condition may not be fully considered in some cases. The
concept of inherent strain is closely related to those of Transverse inherent stress V x* E
H QH
* *
(5)
1Q 2
QH H
x y
inherent stress, inherent deformation and inherent force. Longitudinal inherent stress V *y E * *
(6)
1Q 2 x y
Since the inherent strain is transformed into the deformation
when the restraint is small and it is transformed into the 5. Inherent Deformation in Thin Plate
stress when the restraint is strong, the framework of FE By integrating the inherent strain over the cross-section
code for welding simulation can be naturally and normal to the welding line and take the average through the
conveniently constructed by combining these concepts. The thickness h , the inherent deformations are obtained.
idea how they are integrated in the FE code is presented in Transverse shrinkage G T* 1h H x* dxdz (7)
this paper. ³
Longitudinal shrinkage G L* (8)
³ H dxdz
1 *
h y
Transverse bending (9)
2. Inherent Strain Produces Residual Stress and T T* ³ zH dxdz
1 *
I x
Distortion Longitudinal bending (10)
T L* ³ zH dxdz
*
The total strain H can be decomposed into the sum of
1
I y
elastic strain H e , plastic strain H p , thermal strain H T , creep where, I 1

³ z dxdz
2
strain H c and that produced through phase transformation H .

t 12
The shrinkage produced by the inherent strain

H He H p HT Hc Ht (1) distributed in an element can be replaced by the inherent
Noting that the deformation and the stress are produced by deformation introduced as the discontinuity of the nodal
the total strain and elastic strain, Eq. (1) can be rearranged displacement as shown in Fig. 2.
to,
H He H p HT Hc Ht H* (2) a
This equation means that the distortion and the residual
stress are produced by the inherent strain H which consists
*
of plastic, thermal, creep and that caused by the

transformation. H x* b
3. Inherent Strain in Thin Plate H *
y
Welding deformations in thin plate such as the
transverse shrinkage, the longitudinal shrinkage and the Fig. 1 Shrinkage represented by inherent strain.
angular distortion are mostly produced by the longitudinal
** Chongqing University, Chongqing, China Japan
*** JSOL Corp. Osaka, Japan
103
Concept of inherent strain, inherent stress, inherent deformation and inherent force for prediction of welding
distortion and residual stress
taken into account through the standard FE formulation.
G y* bH *y That associated with the inherent force FT must be also
taken into account in the force vector and the stiffness
matrix in FEM.
In case of large deformation problem, the strain and the
G x* aH x* total potential energy of the structure at time t 't can be
symbolically described as the following equations.
H (u 'u ) H (u ) '1H '2H (15)
Fig. 2 Shrinkage represented by inherent deformation.
S u 'u S u '1S '2S (16)
6. Inherent Force in Thin Plate where, u and 'u are the displacement and its increment.
Further, the inherent forces can be defined by the '1H , '2H , '1S , '2S are the first and second order terms of
following equations. 'u in the strain and the total potential energy, respectively.
From the first order term '1S , the force vector is derived
Transverse inherent force FT* E ³ H x* dxdz EhG x* (11)
Longitudinal inherent force FL* E H *y dxdz EhG y* (12) while the stiffness matrix is derived from the second order
³ term '2S . Noting that the inherent force (Tendon force) is
³
Transverse inherent moment M T* E zH x* dxdz EIT x* (13)
the concentrated stress described as a delta function, the
Longitudinal inherent moment M L* E ³ zH *y dxdz EIT y* (14) contributions of the tendon force to the large deformation
through the force vector and the stiffness matrix are given
by the following equations.
7. Procedure to Introduce Welding Inherent Strain to
FEM '1S ..... ³ V (u )'1H dv .. ³ V (u )T (u )'T (u )dv
Since the restraint in the welding direction is strong and .. ³ FT T (u )'T (u )ds (17)
that in the transverse direction is very weak, the inherent
strain in the transverse direction mostly transforms into the
deformation and that in the welding direction transforms Tendon f
into the residual stress. Thus it is natural to use the inherent force
z TFT FT
deformation for the transverse shrinkage and the angular V
distortion. For the longitudinal shrinkage and bending, the T
inherent force or moment must be used as shown in Fig. 3.
In this way, the shrinkage in the weld zone can be described y
by using relatively coarse FE mesh as illustrated in Fig.4. x
8. Large deformation Fig. 5 Stress distribution Fig. 6 Force produced by
To predict the distortion of thin wall welded structures, in element. large deformation.
the large deformation must be taken into account. As shown
in Fig. 5, the distribution of the stress in an element which
is facing the welding line is a combination of that is
distributing in an element and that is concentrated at a point
in the form of delta function. The effect of large
deformation associated with the distributed stress can be
FT ahEH *y
aQH *y QF T / hE
aH *
x Fig. 7 Deflection computed under small deformation.
(a) transverse shrinkage (b) longitudinal shrinkage

Fig. 3 Shrinkage represented by inherent deformation and
force.
Tendon force
FT
Transverse shrinkage
aH x* (Q / hE ) FT
FT
Welding line
Fig. 4 Modeling of shrinkage due to welding in FEM. Fig. 8 Deflection computed under large deformation.
104
'2S .... ³ V (u )'2H dv .... ³ V (u ){'T (u )}2 dv References

[1] Y. Ueda and T. Yamakawa: Thermal Stress Analysis of Metals
.. ³ FT {'T (u )}2 ds (18) with Temperature Dependent Mechanical Properties, Trans.
JWS, 2-2 (1971), pp.90-100.
where, T symbolically represents the out of plane rotation due
to the deflection. Figure 6 illustrates the lateral force [2] Y. Ueda, K. Fukuda, K. Nakacho and S. ENDO: Fundamental
produced by the out of plane deformation on the welding Concept in Measurement of Residual Stresses Based on Finite
line. Element Method and Reliability of Estimated Values,
Theoretical and Applies Mechanics, 25 (1977), pp. 539-554.
9. Example of Computed Results [3] H. Murakawa, Y. Luo and Y. Ueda: Inherent Strain as an
Welding distortion of stiffened panels with 12 m length Interface between Computational Welding Mechanics and Its
and 4 m width is computed as both small deformation and Industrial Application, Mathematical Modelling of Weld
large deformation problems. The computed deformations Phenomena 4, Ed. H. Cerjak (1998), 597-619.
are shown in Figs. 7 and 8 for small and large deformation.
10. Conclusions
The idea of combined use of inherent deformation and
inherent force is presented and its effectiveness for large
deformation problems is demonstrated.
105
Inherent strain calculation from inverse analysis of measured

†
welding deformation based on python of ABAQUES CAE
ZHAO Haiyan *, NIU Wenchong *, WANG Peng *, YU Xingzhe *,

HE Hongwen *, SUGIMURA Tadashi **
KEY WORDS: (Inherent strain) (Inverse analysis) (Welding deformation) (Finite Element Analysis)
1. Introduction is different for different welded joints.

To estimate the residual stress, a thermal elastic-plastic
method could be used, but a large number of finite elements 3. Realization of the inverse analysis tool by ABAQUS
and a long calculation time is needed. Inherent strain CAE
generated in welded joints is considered as a source of The inverse analysis tool is realized based on the FEA
welding residual stresses and deformation, which has been software ABAQUS. A guide user interface was developed
used for welding residual stress and deformation prediction as a plug-in module in ABAQUS CAE. The plug-in GUI
[1-2]. Therefore, it is very important to develop the method could ask the user to input the required information and
to obtain the inherent strain. Prof. Ueda proposed a function values interactively. Then the program composed by Python
method for describing and estimating the inherent strain calculates the required matrix, which is transformed to the
distribution [3]. By using this method, the residual stress ABAQUS kernel for Finite Element Analysis. The
deformation could be calculated [4]. For large complex computer language Python was used to develop the
welding structure, it is difficult to calculate the inherent ABAQUS plug-in and finish the matrix calculation of
strain distribution. inherent strain.
In this paper, the “inverse analysis method” was used As If the inverse analysis tool is installed, it can be
to calculate the inherent strain for a large complex structure, selected under the plug-in menu, as showed in Fig. 2. From
and an inverse analysis tool base on the FEA software the user input interface shown in Fig. 3, the welding
ABAQUS CAE was developed to realize the inverse parameters can be input according to different welding
analysis of inherent strain. In the program, a plug-in structures.
technology of ABAQUS CAE and the user customized In this inverse analysis tool, the measured deformation
Python were used for coding. To calculate the inherent from experiments is used, which is saved in a txt file.
strain, the deformations of several numbers of points of the The measured displacement
û`3m [ H A ]3mp ^ A` p
The unknown coefficient vector
welded structure were measured. According to the û`3m Elastic response matrix > H A @3mp ^ A` p
measured results, the inherent strains were calculated by
using the inverse analysis tool. The inherent strain and the Distribution function
induced deformation were calculated for the different ^H ` > P @^ A`
p
p vector P > @
welding structures. The comparison between the calculation
and experiments shows that the inverse analysis tool is able ^V ` > D @^H e ` > D @ ^H ` ^H p `
Predicted residual stress Distribution of inherent strain
to calculate the inherent strain and the accuracy is good
enough for the requirement.
and deformation
Elastic strain-strain matrix > D @ ^H ` p
2. Principle of inverse analysis method for inherent Fig. 1 The principle sketch of the inverse analysis method
strain
The principle flowchart of the developed method is
shown in Figure 1. The measured displacement could be
expressed as the product of elastic response matrix and the
unknown coefficient vector of inherent strain. The elastic
response matrix is related to the welding structure. If the
unknown coefficient vector of the inherent strain is
obtained, the inherent strain can be calculated by
Fig. 2 The plug-in menu of the inverse analysis tool
multiplying the coefficient vector and the distribution
function vector. The distribution function of inherent strain

* Dept. of Mech. Eng., Tsinghua University, Beijing, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Nagasaki R&D Center, Mitsubishi Heavy Industries, Japan Japan
106
Inherent strain calculation from inverse analysis of measured welding deformation based on python of
ABAQUES CAE
Because the inherent strain is calculated from “inverse

analysis” of measured welding deformation, the different
inherent strain distributions (e.g., from different distribution
functions) can have the same welding deformation.
Therefore, the selection of proper distribution function is
very important.
(a) (b)
Fig. 5 Distribution of inherent strain: (a) H x , (b) H y
I I
By using the calculated inherent strain, the

Fig. 3The GUI of user input interface
corresponding deformation of the structure can be
Once the value for calculation is input by the calculated by FEA. Figure 6 shows the calculated
developed GUI, the program can do the rest of the deformation of butt welded joint by the inherent strain from
calculation work automatically, including several pre- the developed tool. The comparison between the calculation
calculations and the elastic response matrix calculation. and experiments shows that the inverse analysis tool is able
From the matrix calculation, the unknown coefficient vector to calculate the inherent strain and the accuracy is good
and the inherent strain distribution can be calculated. The enough for the requirement. Figure 7 shows the influence
tool can save the information of the inherent strain of the number of measured points on the accuracy of
distribution to a readable file. angular distortion. It was found that the calculated error is
reduced with an increasing number of measured points. The
4. An example of inverse analysis method error is small enough when the measured points over 50 in
To verify the inverse analysis tool, experiments were this case.
done for different welding structures such as bead-on-plate
welding, butt welding and T-joint welding. The welding
deformation was measured by using the 3-dimensional
coordinate measurement system. Figure 4 shows the
deformation of butt welding by experiments. From the
figure we can see the obviously angular distortion and
bending deformation, the deformed structure is like a horse
back.
Fig. 6 Calculated results of butt welding deformation by

using the inherent strain from the developed tool
6.00%
5.00%
Relative Error
4.00%
3.00%
2.00%
1.00%
Fig. 4 Experimental results of butt welding deformation 0.00%

0 50 100 150 200
Number of measured points
From the measured welding deformation, the inherent
strain distribution of the butt welded joint is calculated by
using the inverse analysis tool. Figure 5 shows the inherent
strain distribution of the cross section perpendicular to the
Fig. 7 The influence of the number of measured points on
welding line.
the calculated welding deformation
107
5. Conclusions [2].Y. Ueda, K. Fukuda, A measuring theory of three dimensional

(1) The inverse analysis tool of inherent strain from the residual stresses in long welded joints, J. Japan Welding Soc.
measured deformation was developed based on 49(1980), pp.113-122
Python of ABAQUS CAE. [3].Yukio UEDA, Ning Xu MA, Measuring methods of three-
(2) The developed inverse analysis tool is able to dimensional residual stresses with aid of distribution function
calculate the inherent strain with acceptable error, of inherent strain, Trans. JWRI. 23(1994), pp.71-78
and the calculated accuracy is increased by [4]. Michael R. Hill, Drew V. Nelson, The inherent strain method
increasing the measurement points for residual stress determination and its application to a long
welded joint. Structural Integrity of Pressure Vessels, Piping,
References and Components ASME 318 (1995), pp. 343-352
[1]. Y. Ueda, K. Fukuda, New measuring method of three-
dimensional residual stresses based on theory of inherent
strain, J. Soc. Naval Arch. Of Japan, 145(1979), pp.203-211
108
Application of inherent deformation and interface element to

†
prediction of welding distortion during assembly process
DENG Dean *, MURAKAWA Hidekazu **, MA Ninshu ** and SERIZAWA Hisashi **
KEY WORDS: (Inherent Deformation) (Interference Element) (Numerical simulation) (Welding Distortion)
1. Introduction
Fusion welding processes are widely used to assemble both the longitudinal stiffener and the transverse stiffener is
large thin plate structures such as ships, automobiles and 12mm. The size of each mesh is 50mm×50mm. Using this
passenger trains because of the high productivity. However, model, five cases as shown in Table 1 are examined to
welding-induced distortion often inevitably occurs during investigate how the gap and misalignment generate during
the assembly process. Welding distortion not only reduces the assembly, and how welding sequence and gap
fabrication accuracy of a welded structure but also correction affect the final distortion. It is assumed that the
decreases productivity due to correction works. If welding fillet joints and cross-shaped in model A are performed by a
distortion can be predicted using a practical method single-sided welding process. The welding conditions of
beforehand, the prediction will be helpful for taking each joint are the same as Ref.[1].
appropriate measures to control the dimension accuracy. In
this study, an elastic FEM approach to welding distortion Table 1 Simulation cases of Model A
for large and complex welded structures is developed based
on inherent strain theory and interface element formulation Case Detailed information
[1-3]. Welding distortions in two typical structure models A0 Weld all parts at the same time
(model A and model B) are simulated using the proposed
method. Model A is employed to show how the gap and A1 1) Weld transverses/longitudinal stiffeners
misalignment generate during the assembly. Model B is a 2) Correct gaps 3) Weld stiffeners and skin plate
large thin plate structure, and it is used to compare the 1) Weld long. Stiffeners and skin plate 2) Strongly
welding distortions computed by large- deformation theory A2 correct the gaps between trans. stiffeners and skin
and small-deformation theory. plate 3) Weld transverse stiffeners and skin plate 4)
Weld longitudinal stiffeners and Trans. stiffeners.
2. Finite Element Models
1) Weld long. Stiffeners and skin plate 2) Weakly
In this study, a two-step computational procedure [1] is
used to simulate welding distortion occurring during the A3 correct the gaps between trans. stiffeners and skin
assembly process. At the first step, the inherent plate 3) Weld transverse stiffeners and skin plate 4)
deformations of each type joint are estimated by thermal Weld longitudinal stiffeners and transverse
elastic plastic FEM using a small model. In the thermal stiffeners.
elastic plastic FE analysis, the detailed welding conditions 1) Weld Trans. Stiffeners and skin plate 2) Strongly
and temperature dependent thermal physical/mechanical A4 correct the gaps between longitudinal stiffeners and
properties are considered. At the second step, the total skin plate 3) Weld longitudinal stiffeners and skin
distortion of the large model is estimated by the developed plate 4) Weld longitudinal stiffeners and transverse
elastic FEM based on inherent strain theory and interface stiffeners.
element method. In this step, the welding distortion induced
by heat input is simulated by inherent deformation, while
the formation of gap/misalignment, the welding sequence
and the gap correction is modeled by interface elements.
Figure 1 shows the mesh division and boundary
conditions of Model A. This model consists of one skin
plate, two longitudinal stiffeners and two transverse
stiffeners. The length, width and thickness of skin plate are
4000mm, 2000mm and 9mm, respectively. The thickness of
† Received on September 2010 Transactions of JWRI is published by Joining and Welding

* College of Materials Science and Engineering, Chongqing Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
University, China Japan
109
Application of inherent deformation and interface element to prediction of welding distortion during assembly process
Welding line
4000mm
2000mm
GAP
Misalignment
Fig. 1 Finite element model A (Model A)
Fig. 3 Remained gap and misalignment after the transverse

stiffener and the skin plate were weakly positioned
Delecttion distributions along line-1
5
Line 1
0
12000mm
Deflection (mm)
-5
4000mm
-10 Case A-0
CaseA-1
CaseA-2
Fig. 2 Finite element model B (Model B) -15
CaseA-3
CaseA-4
Figure 2 shows the mesh division and the restraint -20
conditions of model B. The length of skin plate is 0 500 1000 1500 2000
X-Coordinate (mm)
2500 3000 3500 4000
12000mm, the width is 4000mm, and the thickness of skin

plate is 6mm. The thickness of both longitudinal stiffeners Fig. 4 Deflection distributions along line 1 (Model A)
and transverse stiffeners is 9mm. The size of each mesh is
100mm×100mm. Because the sink plate is very thin, it can
be expected that buckling distortion will possibly occur
during welding. Using this large model, two cases are
simulated to compare the predictions of welding
deformation calculated by large deformation theory and
small deformation theory. Case B-1 is based on large
deformation theory, while Case B-2 is based on small
deformation theory.
Similar to model A, the welding deformations in each
weld joint of model B are estimated by thermal elastic (a) Large deformation theory (b) small deformation theory
plastic FEM [3]. The net total heat input used in the fillet
joint of model A is 1000 J/mm, while that used in cross- Fig. 5 Deflection distributions of model B
shaped join is 1440J/mm. All fillet joints are performed by
a double-sided welding procedure, while the cross-shaped distributions along line 1 in the five cases. This figure
joints are welded by single-sided welding process. It is indicates that both welding sequence and gap correction
assumed that all parts in model B are fixed by tack weld significantly affect the final welding distortion. Here, it
before welding. should be stressed that the welding conditions (heat inputs)
used in each case are identical regardless of how the gap
3. Simulation Results has been corrected. Generally, the larger gap is, the more
Limited by space, the detailed computational approach heat input is needed. For this issue, we will discuss it in our
is not provided in the present paper. Here, we briefly future researches.
discuss the simulation results of model A and model B. Figure 5 shows the deflection distributions predicted by
Figure 3 shows the remaining gap and misalignment in large deformation theory (Case B-1) and small deformation
Case A-3 after the transverse stiffener and the skin plate theory (Case B-2). It is clear that the deformation mode of
were positioned. Because the initial gap generated between Case B-1 is different from that of Case B-2 especially in the
transverse stiffener and the skin plate was weakly corrected, central panels. Figure 6 compares the deflection
the remained gap can be clearly seen and the maximum distributions along line 1 predicted by the two cases. This
value is approximately 4mm. Figure 4 shows the deflection figure shows that the maximum deflection of Case B-1 is
110
Deflection distributions along line 1 respect to the centerline. Whereas, the deflection along
30
Case B-1 (Large)
line 1 of case B-2 has a symmetrical distribution.
2 (Small)
Case B-1
25
Asymme 4. Conclusions
trical
20
deflectio 1) During the assembly process, besides welding process,
welding sequence and gap correction have a significant
Deflection (mm)
n
15
influence on the final deformation.
10 2) For large thin welded structures, because of the
5
propensity of buckling distortion, it is necessary
consider geometrical nonlinear problem.
0
References
0 2000 4000 6000 8000 10000 12000
-5
X-Coordinate (mm) [1] D. Deng and H. Murakawa, Comput. Methods Appl. Mech.
Engrg. 196, 4613-4627,2007.
Fig. 6 Deflection distributions along line 1 (Model B) [2] H. Murakawa, D. Deng,et.al, Trans. JWRI, Vol.38, No2, 63-69,
2009.
significantly larger than that of Case B-2. Moreover,
because of buckling distortion produced in case B-1, the [3] D. Deng and H. Murakawa, Comput. Mater. Sci, 43, 519-603,
2008.
deflection along line l has an asymmetrical distribution with
111
Development of simulation system JWELD for assembly

†
deformation of welded structures
MA Ninshu *, CHIMURA Isaku * and MURAKAWA Hidekazu **
KEY WORDS: (Welding Deformation) (Assembly Deformation) (Simulation) (Welded Structures)
1. Introduction welded joint but also welded structures built by multiply

Welded structures are generally assembled by multiply weld lines and various welded joints. This system consists
stages such as the weld line fitting stage, tack welding stage of a dedicated FEM solver JWELD, a program JWDB for
and final welding stage. To predict the deformation of management and prediction of inherent deformation data
welded structures produced at all assembly stages, fast and base, and a pre-post processor JVSION [3] as shown in Fig.
accurate simulation software is required by industrial users. 2.
Furthermore, if a data base of welding inherent deformation The pre-processor JVISION/Pre has an interface to
for basic welded joints is created, the welding deformation import the geometry of a welded structure which has been
produced in a welded structure can be easily predicted at used for strength analysis of various commercial FEM
the design stage. Then, various countermeasures before solvers such as NASTRAN, LS-DYNA, IDEAS in current
manufacturing welding structures can be investigated by version and CAD data directly in the next version. The
simulation. multiply weld lines can be automatically identified if a pair
To answer the requests from industrial users, a of parts or an element group or a node group is defined.
dedicated simulation system JWELD is developed based on The deformation of each weld line consists of the
JWRIAN, which is a very fast elastic FEM solver using deformation due to weld line fitting, tack welding and final
inherent strain theory [1] and interface elements arranged welding. The assembly sequences can be easily defined in a
between welded parts [2]. A data base for welding inherent form of table. The system supplies a reference data base for
strain is also included in the system. With the aid of several basic welded joints. Users can also build their own
JWELD, the assemble deformation for large scale welded data base using data base creating program JWDB.
structures with many weld lines can be predicted within
several ten minutes. The effect of assembly sequences of JWELD
multiply weld lines on welding deformation can be easily
visualized by this system. JVISION/Pre
(1) Interface䋽 CAD or FEM mesh
2. Development of Simulation System JWELD (2) Materials and Boundary Conditions
Figure 1 shows a proposed new flow to use the (3) Weld lines
simulation technology for welded structures from design - Weld line fitting JWDB
stage to welding assembly stage. If the welding deformation - Tack welding 䞉Registration
produced in a welded structure can be simulated before - Final welding 䞉Prediction
(4) Assemble sequence
production, the time and the cost of experiments (old
Change Conditions
approach) will be greatly saved.
new JWELD
Simulation for multi-welding lines
Design Welding
Structure Structure Assemble Optimization
Experiment
old
Fig. 1 Simulation stage for a welded structure
JVISION/Post
Comparing with other commercial CAE software which (1) Visualization
(2) Deformation
is mainly applied to predict the welding deformation for a
(3) Export interface
certain welded joint, JWELD is a dedicated and integrated
simulation system which is available not only for a simple Fig. 2 Schematic showing of simulation system JWELD
* JSOL Corp. Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
112
Development of simulation system JWELD for assemble deformation of welded structures
part-
3/t= Tack
6 we ld
s
If a geometry model of a welded structure is built and
the assembly sequences are given, the deformation due to
weld line fitting, tack welding and final welding can be
part
predicted by FEM solver JWELD within very short CPU - 1/t=
6
time. Furthermore, in order to control the deformation, the Part-2
/t4.5 W1
optimization of assemble sequences is being developed and
will be released for next version.
The post processor JVISION/Post can directly show Fig. 4 Deformation due to a single-sided fillet welding
the deformation produced by each weld line. The geometry for a H-section joint
with assembly welding deformation can be exported for the
other purposes of simulation.
3. Verification of Simulation System JWELD

To help users to apply this simulation system, the
welding deformation in basic welded joints much be
verified firstly. Figure 3 shows a single-sided fillet joint
and welding deformation computed by JWELD. The arc
welding conditions and inherent deformation [4] for this
fillet welded joint are shown in Table 1.
Table 1 Arc welding conditions and inherent deformation Fig. 5 Correction deformation of upper flange modeled by
I U v Gx Gy Tx Ty the interface element formulation
(A) (V) (mm/s) [mm] [mm] [rad] [rad]
180 24.0 5.0 0.061 0.11 0.00 0.021 4. Applications of Simulation System JWELD
(1) Welding assembly deformation in a grid structure
The single sided weld line of fillet joint is located on the Figure 6 shows a long grid structure which has ten
right side of flange. Therefore, the deflection on the right parts and nine welding lines. The welding assembly
side of flange is larger than that on the left side. sequences are also shown in Fig.6. The grid made from
steel SS410 is assembled by arc welding process. The
welding current, voltage and welding velocity are 400A,
0 20V, 10mm/sec for three butt weld lines (W1, W2 and W3)
20
50 and 250A, 25V, 10mm/sec for fillet weld lines (W4, W5)
t=6
.5 and (W6, W7, W8, W9), respectively. The welding lines
t=4 line
W4, W5 are double sided fillet welds and weld lines W6,
eld
W W7, W8, W9 are single sided fillet welds. The inherent
400 deformations of these weld lines are predicted using a data
base creating program JWDB. Figure 7 shows the
computed final deformation due to sequential assembly
welding from W1 to W9.
Fig. 3 Deformation due to a single-sided fillet welding (2) Welding assemble deformation in a train car model
Figure 8 shows a simplified FEM model [5] of a train
Figure 4 shows the welding deformation of H type car structure for the computation of welding deformation.
section of fillet welds due to a single-sided weld line (W1) The details are neglected because the limitation of space.
between the lower flange (part-1/t=6) and web (part-
2/t=4.5). If two tack welds between web and upper flange Length=10,000mm part6
(part-3/t=6), the angular distortion due to the weld line Width=1,000mm
part5 W3
(W1) will make the upper flange deform following the web. Height=1,000mm
Thickness=10mm
If there are no any tack welds between the web and upper W5 part4
W8
W2
flange, the gap and misalignment at the interface will part3 W9
produced. If correction of the gap and misalignment in both W6 W4 W1 part2
part9
part10
part1
transverse direction and normal direction are modeled by
W7
the interface element formulation [2] between the upper
part7 part8
flange and the web, the upper flange will deform only in y
direction and z direction as shown in Fig. 5 by two arrows.
Fig. 6 Gird model for computation of welding deformation
113
5. Summary
(1) Integrated simulation system JWELD was developed
for industrial users.
(2) The validity of this system was verified by basic
welded joint models and structural models.
Reference
[1] Y. Ueda, H. Murakawa and N. Ma: Computational Approach
to Welding Deformation and Residual Stress, Sanpo
publication, ISBN978-4-88318-034-9 C3057, 2007
[2] D. Deng and H. Murakawa: FEM Prediction of Buckling
Distortion Induced by Welding in Thin Plate Panel Structures,
Computational Material Science, 41 (2008) 591-607.
[3] JSOL: JVISION User’s Manual, //www.jsol.co.jp/cae/
Fig. 7 Computed welding deformation of gird model [4] JWES: //www-it.jwes.or.jp/nedo01
[5] T. Hisamori and E. Tachibana: Numerical Simulations of A
Train Collision with A Building Structure, Japan Architecture
Society, 2006, p.43-52, http://jweld.jsol.co.jp/
2,550
00
20,0
3,00
0
Fig. 8 Train car model for computation of welding

deformation
114
In-situ Observation of martensite transformation and retained

†
austenite in supermartensitic stainless steel
ZHANG Shuoyuan *, TERASAKI Hidenori ** and KOMIZO Yu-ichi ***
KEY WORDS: (Martensite Transformation) (Retained Austenite) (In situ Observation) (X-ray Diffraction)
(Synchrotron Radiation)
1. Introduction transformation of Supermartensitic steel during cooling was

Supermartensitic steel (14CrNiMo) is a candidate as a observed in-situ by using high temperature laser scanning
weld metal for joining of ultra-high strength steels. For confocal microscopy and X-ray diffraction by Synchrotron
preventing the cold cracking problem, the austenite phase is radiation.
effective due to its nature of hydrogen absorption and the The schematic illustration of the In-situ observation
existing of austenite phases increases toughness of weld system is shown in Figure 1[1]. The In-situ observation
metal. Moreover, the residual stress can be decreased by system consists of High-Temperature Laser Scanning
introducing the martensite transformation expansion. On Confocal Microscopy (HLSCM) system[2, 3] and Time-
the other hand, too much retained austenite could decrease Resolved X-ray Diffraction (TRXRD) system. The High-
the strength of Supermartensitic steel. Hence, determination Temperature Laser Scanning Confocal Microscopy
of the retained austenite is important in Supermartensitic (HLSCM) system was used for direct observation of the
steel. martensite transformation during the thermal cycles.
In this research, martensite transformation of The Time-Resolved X-ray Diffraction (TRXRD)
supermartensitic steel during cooling was observed in-situ systems were performed on the BL46XU beam line with
by using high temperature laser scanning confocal the undulator of third generation synchrotron radiation
microscopy and X-ray diffraction by Synchrotron radiation. source, Spring-8, with the approval of the Japan
The ultra-bright, directional and quasi monochromatic Synchrotron Radiation Research Institute (Hyogo, Japan).
natures of the beam were suitable as the probe for our This research, gives a time resolution of 0.2 seconds by
purpose. using PILATUS 100K detector. The diffraction intensities
at various 2T positions were monitored continuously and in
real time using a detector covering a 2Trange of
approximately form 12° to 28°. In general, two body-
centered cubic (bcc) martensite peaks [110 and 200] and
two face-centered cubic (fcc) austenite peaks [111 and 200]
were identified.

Figure 2 shows the in-situ observation of
morphological development and the diffraction patterns
recorded on the pixel detector for the sample 14Cr5Ni. Fig.
Fig.1 Schematic illustration of in-situ observations 2(a) to (c) correspond to the heating process from the room
experiments system. temperature, while Fig.2(d) to (f) show the martensite
transformation during cooling process. There were four
2. Experimental peaks visible in the diffraction patterns, representing
In this study, for analysis of behavior of retained
D(110), D(200),J(111) andJ(200). The materials consists
austenite in martensite transformation, supermartensitic
of D’-martensite, D(110) and D(200), at room temperature
steel was prepared with different nickel contents. The Ms
of supermartensitic steel of 14Cr9Ni was low, and a large shown in Fig.2(a). As shown in Fig.2(b), J(111) andJ(200)
amount of retained austenite remaind in the specimen reflections were first identified at 758 degree C, indicating
cooled down to room temperature. After the specimens the initiation of transformation from D’- martensite toJ-
were heated from room temperature to 1000 degree C and austenite. Furthermore D(110) and D(200) reflections
cooled down to room temperature. The Martensite disappeared at 907 degree C in Fig.2(c) , which represents
the complete transformation to austenite.
* Graduate School of Engineering, Osaka University, Osaka, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan Japan
** Joining and Welding Research Institute, Osaka University,
Osaka, Japan
115
In-situ Observation of martensite transformation and retained austenite in supermartensitic stainless steel
for all the samples that 2T decreases with increasing time,

during heating process. On the cooling process, 2T
increased with increasing time. It was also shown in the
figure that as the martensite transformation proceeds, in the
higher full width at half maximum (FWHM) and the
intensity ofJ(111) andJ(200) reflections becomes stronger.
Fig. 2 Overview of the In-situ Observation results for

martensite transformation for 14Cr5Ni Using high
temperature laser scanning confocal microscopy and Fig. 4 Intensities of J(111), J(200) and D(110) for the
Synchrotron Radiation X-ray diffraction. The x-y axis last 340s of the cooling to room temperature.
corresponded to that in Fig.1.
Figures 4(a) to (d) show the intensity of D(110), J(111)
andJ(200) as a function of time and temperature for all the
Fig.2(d) shows that due mainly to the variation of the J- samples during cooling process. As the martensite
austenite reflections from a ring pattern to a spot pattern, transformation proceeded, the intensity of D(110) increase
because the austenite grain sizes become larger. As shown with increasing time and decreasing temperature. It is
in Fig.2(e), D(110) reflection first appeard at 199 degree C, interesting to note that simultaneously the intensity of
which corresponds to the beginning of transformation J(111) andJ(200) increased with increasing time and
fromJ-austenite to D-martensite. Subsequently, as the decreasing temperature for the first three samples.
transformation proceeded, J(111) andJ(200) reflections Subsequently, the intensity of J(111) andJ(200) decreased
disappear at 35 degree C, as shown in Fig.2(f). This means with increasing time and decreasing temperature. In
the transformation ofJ-austenite to D-martensite is fully Fig.4(d), the intensity of J(111) andJ(200) increased with
completed. increasing time and decreasing temperature until the room
temperature. A lot of retained austenite has been observed
in this sample. In our previous paper[4], EBSD results
showed that in this sample twin deformation has been
observed and the austenite grain size becomes smaller.
It is generally accepted that ideally perfect crystal and
powder crystal have minimum and maximum diffracting
power respectively, due to the effect of distinction. Thus, at
the initiation of martensite transformation, the intensity of
all the samples increases, mainly because the introduction
of the metal defects in the parent austenite increased the
diffracting power. The intensity of the austenite increases
with increasing metal defects, although the content of
austenite decreases. The content of austenite decreases as
the transformation proceeds. The effect of the intensity of
austenite becomes lower due to increasing diffracting
power by introduction of the metal defects in the austenite,
as a result of decrease intensity of austenite.
Fig. 3 X-ray diffraction sequence for the first 0s to
final 540s for all the samples, 14Cr5Ni, 14Cr6Ni, 4. Conclusions
14Cr8Ni, and 14Cr9Ni. The black corresponds to the Martensite transformation of supermartensitic steel was
peak highest intensities and white the lowest. observed in-situ by using high temperature laser scanning
confocal microscopy and X-ray diffraction by Synchrotron
Figures 3(a) to (d) show the 2T values of the diffraction radiation. The main conclusions obtained are as follows:
peaks plotted as a function of time for all the samples, (1) The reflection of austenite changes from a spot
14Cr5Ni, 14Cr6Ni, 14Cr8Ni, and 14Cr9Ni. It was shown pattern to a ring pattern after martensite
116
transformation. NEDO (New Energy and Industrial Technology

(2) Both the higher full width at half maximum (FWHM) Development Organization) is gratefully acknowledged.
and intensity increased due to the effect of martensite The synchrotron radiation experiments were performed at
transformation. the BL46XU in the SPring-8 with the approval of the Japan
(3) At the initiation of martensite transformation, the Synchrotron Radiation Research Institute (JASRI)
intensity of austenite increased due to increasing (Proposal No. 2008A1959, 2008B2135 & 2009A1944).
diffracting power by introduction of the metal defects
in the austenite. References
[1]Y. Komizo and H. Terasaki: Sci. Technol. Weld. Join.,(2011)
Acknowledgements in press.
This study was carried out as a part of research [2]H. Terasaki and Y. Komizo: Sci. Technol. Weld. Join.,5(2006)
activities of “Fundamental Studies on Technologies for 11, pp. 561-566.
Steel Materials with Enhanced Strength and Functions” by [3]Y. Komizo, et al.: Weld. World,5-6(2008) 52, pp. 56-63.
Consortium of JRCM (The Japan Research and [4]S. Zhang, Y. Komizo, and H. Terasaki: Tetsu-To-
Development Center of Metals). Financial support from Hagane,2(2010) 96, pp. 8-13.
117
In-situ observation of phase transformation during laser welding

†
processes
YAMADA Tomonori*, YONEMOTO Yukihiro*, YAMASHITA Susumu*,

MURAMATSU Toshiharu* and KOMIZO Yu-ichi **
KEY WORDS: (Laser welding) (Weld metal) (In-situ observation) (Nucleation site)
1. Introduction (99.9999%) after evacuating to 1×10-2Pa[1]. In the present

It is known that residual stress is important to keep work, the following thermal cycle was applied to the
structural integrity. Laser welding is effective for a residual samples. To make the austenite grain diameter uniform,
stress decrease because heat input is smaller and have a less heating rate was 13.3oC/sec to 1400oC. Cooling rate was
effect. Therefore, repair technology by laser welding has 5oC /sec between 1400oC and 800oC. To assume the
drawn wide attention for the life extension of FBRs (Fast cooling rate of the laser welding, the sample was cooled by
Breeder Reactors). To establish laser repair technology, the maximal rate (54.5oC/sec) from 800oC.
special attentions should be paid to the morphological To clarify the microstructural evolution mechanism, the
developments. inclusions were investigated from the crystallographic point
In the present work, morphological developments were of view. The foil samples including inclusions were
directly observed using laser scanning confocal microscopy prepared in a focused ion beam (FIB) device and were
during laser weld cooling. observed by a transmission electron microscope (TEM) in
which the accelerated voltage of 200kV was used.
2. Experiments
The tested materials were low carbon Ti-B weld metals
with an oxygen content of 460ppm and machined into
sample discs for observation. Table 1 shows the chemical
compositions of the weld metals used. The compositions of
inclusions were varied by changing aluminium content
while the contents of the other elements kept constant. The
Al/O ratios (mass ratio) were 0.48, 0.73 and 1.52.
Table1 Chemical compositions of weld metals

used(mass%).
Fig. 1 Schematic illustration for optical system in high

temperature laser scanning confocal microscopy.
For in situ observation of phase transformation during
thermal cycle of laser welding, a high temperature laser 3. Results and Discussion
scanning microscope (HLSCM) system was used. This Figure 2 shows the results of in-situ morphological
system consists of LSCM and infrared image furnace (IIF). development observation of transformation for Y2
The sample disc was machined to 5mm diameter and (Al/O=0.73). When sample was cooled to 596oC,
1mm in height and the observed plane was mirror polished. transformation to ferrite from near the inclusions in the
The sample in the high purity alumina crucible was set on austenite grains was observed. The circle shows
the platinum holder connected to a B type thermocouple. morphological change corresponding to acicular ferrite
Figure 1 shows schematic illustration for the sample holder growing. It was clear that morphological change
in an infrared image furnace and the optical system. The corresponding to acicular ferrite growing. It was clear that
high scanning rate (30frame rates) is due to the acoustic the morphological change corresponding to phase
optical deflector and only the focal point can be detected by transformation. This result shows that the grain boundary
the CCD camera without the effects of high temperature did not operate as a nucleation site. When sample was
radiation since a confocal optical system is used. The cooled to 441oC, transformation was finished. Therefore,
atmosphere was filled with high purity argon shielding gas the interface between nucleation site (inclusion) and ferrite

* Japan Atomic Energy Agency Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
118
In-situ observation of phase transformation during laser welding processes
was observed.
Figure 3 shows the HAADF-STEM image, EDS
mapping analysis, EDS spectrum and selected area
diffraction pattern from inclusions in Y2 in which acicular
ferrite was observed. This inclusion was surrounded by a
titanium enriched layer. This layer was identified as TiO by
EDS spectrum and SAD. The TiO has a Baker-Nutting
orientation with acicular ferrite. In this case, the lattice
misfit between TiO and acicular ferrite is 3.0%[2].
Therefore, the TiO on the inclusion surface promotes
intragranular nucleation supplying low interface energy.
Figure 4 shows the corresponding crystal-orientation
maps measured in the Y2(Al/O=0.73) by EBSD analysis.
Inverse pole figure color maps show the distributions of
ferrite and austenite, respectively. The pole figure of ferrite Fig. 3 TEM analysis of inclusion after thermal cycle in
shows {110} and {111}. Moreover, the pole figure of Y2(Al/O=0.73). (a)HAADF-STEM image ; (b)EDS
austenite shows {111} and {101}. From these pole figure, mapping by Ti-K Ș X-ray ; (c)EDS spectrum from the point
{110} ȘFe and {111} Ț Fe , {111} ȘFe and {101} ȚFe were indicated by a cross in the HADDF image; (d) Selected area
parallel, respectively. Therefore, these results suggest that diffraction pattern from the area indicated by a circle in the
they have Kurdjumov-Sachs (K-S) orientation HADDF image and its key diagram.
relationship.
Figure 5 shows the schematic illustration for
orientation relationship between TiO and acicular ferrite,
orientation relationship between acicular ferrite and
austenite. The inclusions which related to acicular ferrite
formation were surrounded by TiO. The B-N orientation
relationship was satisfied between the TiO and acicular
ferrite. The K-S orientation relationship was satisfied
between the acicular ferrite and austenite. Therefore, a
crystal plane of acicular ferrite corresponds to the habit
plane {111} ȚFe and the growth direction was <111> ȘFe .
Fig. 4 The corresponding crystal-orientation map measured

in the Y2(Al/O=0.73) by EBSD analysis.
Fig. 5 Schematic illustration for metallurgical phenomena

around inclusion.
Fig. 2 In-situ observation of morphological development in
Y2(Al/O=0.73). (a)596oC ; (b)574oC ; (c)550oC ; (d)441oC. 4. Conclusions
The phase transformation was observed in-situ during
laser weld cooling in low carbon Ti-B weld metals with
three levels of Al/O ratio. The findings obtained in the
present research are as follows.
(1) Acicular ferrite nucleated intragranularly on inclusions
within the austenite grains in weld metals with low and
medium Al/O ratio.
119
(2) The inclusions which related to acicular ferrite References

formation were surrounded by a TiO layer. [1] H.Terasaki and Y.Komizo: Sci. Technol. Weld. Joining,
(3) The Baker-Nutting orientation relationship was
11(2006), pp.561–566.
satisfied between the TiO layer and acicular ferrite.
(4) It was suggested that the TiO on the inclusion surface [2] T.Yamada, H.Terasaki and Y.Komizo: Tetsu-to-Hagane,
contributes to the heterogeneous nucleation of acicular 95(2009), pp.65-70.
ferrite, supplying low interface energy.
120
Numerical simulation on type IV cracking of ASME P92 steel at

†
high temperature
JING Hongyang**, XU Lianyong**, ZHAO Lei**
KEY WORDS: &reep damage1umerical simulationContinuum damage mechanicsType IV cracking
ASMEP92 steel
1. Introduction angle at 22° in the middle of the specimen, loaded at a

In order to obtain an improvement in thermal efficiency uniform tensile stress in the z-direction with 70 MPa. Based
and a reduction of the CO2 emission in modern ultra- on the uniaxial creep test, a FEM model, as shown in Fig. 1,
supercritical (USC) fossil-fired power, the operating half of the creep specimen is adopted to investigate the
temperature and pressure have to be increased. ASME P92 creep damage development and stress distribution in the
steel (9Cr-1.8W-0.5Mo-NbV in wt%) have been used as welded joint during creep.
structural materials for boiler components at 600 °C and 25
MPa due to its good mechanical properties, especially high
creep rupture strength [1].
Creep cracking often occurs in the fine-grained heat
affected zone (FGHAZ) of welded joints of P92 steel at
high temperature and high pressure, known as Type IV
cracking [2]. It leads to a short creep life of welded joints
compared with that of base metal. Fig. 1 FEM model of the welded creep specimen
In this paper, a fine element method coupled with
continuum damage mechanics is used to investigate the
mechanism of Type IV cracking and factors affecting creep
strength deterioration in the FGHAZ of ASME P92 steel at
650 °C and 70 MPa.
2. Continuum damage mechanics

In the present study, a modified Karchanov-Rabotnov
equation for creep damage is used to calculate the stress
and creep damage distribution of a welded creep specimen
and the constitutive equation is as follows [3]:
d H ij
c
dt
3
2
n 1

BV e S ij 1 U U 1 D
n
(1)
(DV 1 (1 D )V e )
v
dD A
g (2)
1 D
I
dt I 1
(1/ ( I 1))
Dcr 1 (1 g ) (3)
3. FEM model
The welded joint of P92 steel analyzed in this paper is
kept at 650 °C and 70 MPa.The creep specimen of a welded
joint where four different material properties namely BM,
CGHAZ, FGHAZ, and WM are taken into account is a
round bar. The bar has a cross section of 10 mm and a
gauge length of 50 mm with a HAZ width at 2 mm Fig. 2 Contours of creep damage in weld joint with various
(FGHAZ width 1mm, CGHAZ width 1mm) and groove creep times
† Received on 15 October 2010 Transactions of JWRI is published by Joining and Welding

* School of Materials Science and Engineering, Tianjin Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
University, Tianjin, China Japan
** Tianjin Key Laboratory of Advanced Joining Technology,
Tianjin, China
121
Numerical simulation on type IV cracking of ASME P92 steel at high temperature
4. Results and discussions

The FEM result demonstrates that the sample fractures
in the FGHAZ of welded joint at 7100 h, when the D/Dcr of
most elements in the FGHAZ reaches to 100%. It reveals
that with increase in creep time, the creep damage of
FGHAZ is accumulated faster than that of others zones in
welded joint and the first damage elements occur in this
zone, as shown in Fig. 2. The most elements of FGHAZ
reach to the critical damage while the creep damage of
other zones in welded joint is still small. Further, the creep
damage in the inner part of FGHAZ is accumulated faster
that that in the outer part of FGHAZ.
Although the welded joint is loaded by a uniform tensile
stress during creep, there are gradients in the creep strength Fig. 3 Equivalent stress distribution with various creep
of the micro zones in welded joint, which leads to stress times
redistribution during creep, as shown in Fig. 3. Numerical
simulations reveal that the equivalent stress varies with
increase in creep time. At a creep time of 0 h there is no
significant difference in equivalent stresses in the WM,
CGHAZ, FGHAZ, and BM, but after a long creep time the
difference is remarkable. The equivalent stress is low in the
FGHAZ but high in the CGHAZ region adjacent to the
FGHAZ and for the FGHAZ/BM interface, equivalent
stress is low in the FGHAZ but high in the BM region
adjacent to the FGHAZ. The reason is that the constraints
of the CGHAZ and BM on the FGHAZ lead to the stress
concentration.
Figure 4 and Figure 5 show the distribution of stress
triaxiality and maximum principle stress, respectively. The
stress triaxiality and maximum principle stress are high in Fig. 4 Stress triaxiality distribution with various creep times
the FGHAZ while they are low in the CGHAZ. For the
WM/CGHAZ interface, the stress triaxiality and maximum
principle stress increase in both of the CGHAZ and the
WM as the creep time increases. For the CGHAZ/FGHAZ,
the stress triaxiality and maximum principle stress increase
in the FGHAZ but decreases in the CGHAZ. For the
FGHAZ/BM interface, the stress triaxiality and maximum
principle stress increase in the FGHAZ, but decreases in the
BM.
For the CGHAZ/FGHAZ interface or the FGHAZ/BM,
the stress triaxiality and maximum principle stress in
FGHAZ are high and the creep damage is high. The high
creep damage also occurs in the FGHAZ for the
CGHAZ/FGHAZ interface or the FGHAZ/BM interface, Fig. 5 Maximum principle stress distribution with various
where the maximum principle stress and stress triaxiality creep times
are high. It implies that the high maximum principle stress
and high stress triaxiality play an important role on the FEM models with different HAZ widths and various groove
accumulation of creep damage. They may accelerate the angles are calculated. The results reveal that a small groove
growth and coalescence of creep voids and the subsequent angle and a narrow HAZ width can reduce the stress
micro crack formation during creep. The creep damage triaxiality and maximum principle stress in the FGHAZ of
expands from the center of the FGHAZ to the outer surface welded joint of P92 steel, which can suppress the
and the elements reaching to the critical damage also firstly accumulation of creep damage and the development of
occur in the center of FGHAZ. Because the stress triaxiality equivalent creep strain in FGHAZ; as a result Type IV
and maximum principle stress of the center surface are cracking can be suppressed in welded joint of P92 steel.
much higher than those of the outer surface. It is considered that the narrow-gap welding technique
Since the FGHAZ is the key factor to the occurrence of which can produce a small groove angle and a narrow HAZ
Type IV cracking in welded joint of ASME P92 steel, it is should be applied on the welding specification of ASME
necessary to investigate the effect of HAZ width and the P92 steel to decrease the accumulation of creep damage in
effect of groove angle on the creep damage development. the FGHAZ and to suppress Type IV cracking.
122
(1) The creep damage in FGHAZ is severe and the failure [1] C. Petry, and G. Lindet: Modelling creep behaviour and
life of FGHAZ is 7100 h. The stress triaxiality and failure of 9Cr-0.5Mo-1.8W-VNb steel, Int. J. Pres. Ves. Pip.,
maximum principle stress located at the FGHAZ are 86-8 (2009), 486-494.
higher than that of other zones in the welded joint [2] J.A. Francis, W. Mazur, and H.K.D.H. Bhadeshia: Type IV
during creep. It implies that they can accelerate the cracking in ferritic power plant steels, Mater. Sci. Technol.,
creep strain development and creep damage 22-12 (2006), 1387-1395.
accumulation; as a result Type IV cracking is likely to [3] S.-T. Tu, P. Segle, and J.-M. Gong: Creep damage and
occur in this zone. fracture of weldments at high temperature, Int. J. Pres. Ves.
(2) A small groove angle and a narrow HAZ width of the Pip., 81-2 (2004), 199-209.
welded joint are calculated to decrease the maximum
principle stress and stress triaxiality in the FGHAZ,
which leads to a decline in the accumulation of creep
damage and can suppress Type IV cracking in ASME
P92 steel.
123
Numerical simulation of austenite retention in triplex stainless steel

†
weld metals
SAIDA Kazuyoshi*, ARATA Hayata*, OGIWARA Hiroyuki*, NISHIMOTO Kazutoshi*
KEY WORDS: (Triplex stainless steel) (Retained austenite) (Kinetics) (Solidification mode) (Segregation)
(Numerical simulation) (Martensitic transformation) (Ferritic-austenitic transformation)
1. Introduction which is below RT. Microsegregation behaviour in the

Triplex stainless steel, which consists of ferritic, weld metal was computed using a theoretical model in
austenitic and martensitic phases, is one of the most hopeful which solidification segregation and subsequent
welding consumables applied to preheat-free welding of desegregation of alloying elements during the welding
HT980 [1]. It has been shown that the amount of retained process were simulated. Four types of solidification
austenite in the triplex stainless steel weld metal should be modes (A, AF, FA and F modes) were considered in
controlled in an optimal range in order to obtain sufficient calculating the solidification segregation, and the
joint properties of HT980 welds. In the present study, the ferritic-austenitic transformation in the solid was also
kinetics of austenite retention was examined and the amount considered in calculating the desegregation of alloying
of retained austenite was predicted for the various weld elements during cooling after solidification. Assuming
metal compositions and welding conditions in order to that the morphology of a dendritic cell is basically a
obtain basic information on the applicability of such triplex hexagonal prism as illustrated in Fig. 1, the model
stainless steel welding consumables to the preheat-free
analysed here used one-dimensional diffusion in a
welding of HT980.
rectangular triangle. Solidification proceeds one-
2. Materials and Experimental Procedures dimensionally from a cell core to a cell boundary. The
Twenty-three kinds of nominally 13mass%Cr- distribution of solute elements was calculated using the
7mass%Ni triplex stainless steels with varying amounts finite differential method scheme considering the
of Ni and C were used for the base metal. In order to moving boundaries.
obtain the triplex stainless steel weld metals, gas
tungsten arc melt-run welding (GTAW) was conducted
using the following welding conditions: arc current 120
A, arc voltage 14 V and welding speed 1.67-10.0 mm/s.
The amount of retained austenite in the base and weld
metals was measured by X-ray diffraction analysis using
the 5 peaks method.
3. Kinetic Approach to Retention of Austenite

"Retained austenite" is an austenitic phase that does
not transform to a martensitic phase upon cooling from a
high temperature (austenitic region). Therefore, the Fig. 1 Schematic illustration of analysis model
retention of austenite is a complementary event to the
martensitic transformation. Assuming that the retention In the present study, the M s and M f temperatures of
of austenite is governed by the chemical composition in triplex stainless steels was assumed to be expressed by
that location prior to the martensitic transformation, the (unit: K): (1)
retention kinetics of austenite arise from the non- M s = 1263 - 26 Mn - 53 Ni - 32 Cr - 18 Mo - 97 C Cr
uniform distribution of alloying elements due to M f = M s - 100
microsegregation. Austenite is finally retained in a
particular location if the M s temperature in that Figure 2 illustrates the distribution of the M s and M f
locationis below RT. Microsegregation behaviour in the temperatures in a dendritic cell calculated from the
weld metal was computed using a theoretical model in solute concentrations. Austenite is retained in the
* Dept. of Materials & Manufacturing Science. Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Graduate School of Eng., Osaka University, Osaka, Japan Japan
124
Numerical simulation of austenite retention in triplex stainless steel weld metals
with varying alloy compositions. There is a good agreement

between them for all solidification modes. It follows that
the retention of austenite in the triplex stainless steels weld
metal at differing alloy compositions and welding
conditions can be quantitatively predicted by the present
numerical analysis.
Fig. 2 Concept of retention kinetics of austenite based on

distribution of Ms and Mf temperatures
location where the M s temperature in that location drops

below RT, and some amount of austenite is retained in
the transformed martensite at locations where RT is
situated between the M s and M f temperatures. The
fraction of martensite transformed f m at temperature T
(between M s and M f ) can be expressed by:
1 - exp - 0.011 M s - T (a) AF mode
fm = (2)
1 - exp - 0.011 M s - M f
The distribution of solute elements, Cr, Ni, Mo, Mn and

C was calculated for pseudo-binary systems. The
material constants employed for the calculation were
taken from references and computed using Thermo-Calc.
Three kinds of solidification/cooling rates were
determined from the measured thermal cycles during
GTAW while varying the welding velocity from 1.67, to
5.0 and 10.0 mm/s.
4. Analysis Results for retained Austenite

Distribution of M s and M f Temperatures in Dendritic Cell
Figure 3(a) and (b) show the distributions of the M s and
M f temperatures and the volume fraction of retained
(b) FA mode
austenite in a dendritic cell calculated for the weld metals
C1 (AF mode) and A2 (FA mode), respectively. In the case Fig. 3 Calculated distribution of Ms and Mf temperatures
of weld metal C1, the M s and M f temperatures also drop in dendritic cell
toward a cell boundary, however, a ferritic phase (G) exists
at a cell boundary. Retained austenite remains adjacent to a
ferritic phase, and a cell core corresponds to
austenitic+martensitic phases (J0). The amount of
retained austenite in the weld metal is calculated as 31.1%.
In the case of weld metal A2 (FA mode), the M s and M f
temperatures once again decrease toward a cell boundary. A
ferritic phase (G) exists inside a cell, and a martensitic phase
is formed adjacent to a ferritic phase. A cell boundary
corresponds to retained austenite. The amount of retained
austenite in the weld metal is calculated as 12.3%.
Validity of Retention Kinetics of Austenite in Weld Metal

In order to validate the retention kinetics of austenite
proposed in the present study, calculated amounts of
retained austenite were compared with measured values.
Figure 4 shows the relationship between the calculated and
measured amounts of retained austenite in the weld metal Fig. 4 Comparison of amount of retained austenite
between calculated results and measured ones
125
5. Conclusions (3) The calculated amounts of retained austenite in weld

The results obtained may be summarised as follows; metals were approximately consistent with measured
(1) The retention kinetics of austenite were formulated with ones at any alloy composition and welding velocity. It
regard to the various solidification modes, the ferritic- followed that the retention of austenite in the triplex
austenitic and martensitic transformations in the solid, stainless steel weld metals at differing alloy
assuming that austenite retention arose from the non- compositions and welding conditions could be
uniform distribution of alloying elements due to quantitatively predicted by the present numerical
microsegregation. analysis.
(2) The M s and M f temperatures dropped near a cell
boundary. The calculated amounts of retained austenite References
in the weld metal increased with an increase in the Ni [1] K. Saida, K. Nishimoto, K. Ogawa, S. Okaguchi and K.
Fujiwara: ‘Proposal of Welding Consumable of Triplex
and C contents in steels (and with a decrease in cooling Stainless Steel for Ultra High-Strength Steel’, Sci. & Technol.
rate during welding). Welding & Joining, 15-3 (2010), p.185
126
Prediction of hardness in HAZ of low-alloy steel produced by

temper bead welding using neural network†
YU Lina*, NAKABAYASHI Yuma*, ITO Shinsuke*, KAMEYAMA Masashi**,

HIRANO Shinro***, CHIGUSA Naoki***, SAIDA Kazuyoshi*, MOCHIDUKI Masahito*
and NISHIMOTO Kazutoshi*
KEY WORDS: (Hardness prediction) (Temper bead welding) (HAZ) (Neural network) (FEM)
1. Introduction temperature, as follows

Low alloy steel A533B is widely employed in P=T(log t + C) (1)
building PWR reactor vessels. However, the excellent where T is the temperature in degrees Kelvin, t is the
mechanical properties of the base metal will be altered time in hours and C is a material specific constant often
after experiencing thermal cycles imposed by welding approximated as 20 for steel [3].
process, and the increase of hardness always happens in LMP can be used only for the iso-thermal heat
weld heat affected zone (HAZ) [1]. Therefore, post weld treatment with constant tempering temperature.
heat treatment (PWHT) is required to eliminate the Therefore it cannot be applied for tempering during the
residual stress and decrease the hardness. thermal cycle process. In order to apply LMP for thermal
Temper bead welding technique is in practice one of cycle processes, the thermal cycle was divided into such
the effective repair welding methods instead of PWHT minute sections as to be assumed as an iso-thermal heat
when PWHT is difficult to perform [2]. When temper treatment with short holding time. The whole tempering
bead welding is applied, it’s very important to select the effect during thermal cycle process is considered as the
proper thermal cycle during temper bead welding in sum of minute sectioned iso-thermal heat treatment.
order to obtain high tempering effect. Hardness is one of LMP during thermal cycle process can be calculated by
the key criteria to evaluate the tempering effect by following method.
temper bead welding. Therefore a prediction method The LMP of 1st cycle at T 1 with holding time t 1 is
using Neural Network has been investigated to predict equal to that at T 2 with equivalent holding time t 1,2 ,
the hardness in HAZ of A533B, when temper bead shown as
welding is applied. Pଵ = Tଵ (20 + logtଵ ) = Tଶ ൫20 + logtଵ,ଶ ൯ (2)
Thus, the equivalent holding time t 1,2 at T 2 can be
2. Experimental obtained as
The base metal is low alloy steel A533B and the ୘
logtଵ,ଶ = భ (20 + logtଵ ) െ 20 (3)
filler material is Inconel690. Samples (5×5×5mm) were ୘మ
heated by a high frequency induction heating device to Then the LMP of 1st and 2nd pass can be expressed as
simulate as-welded and temper-processed HAZ. The Pଶ = Tଶ [20 + log൫tଵ,ଶ + t ଶ ൯] (4)
multi-pass welded samples (100×33×120mm) were Similarly, the LMP from 1st pass to 3nd pass can be
produced by TIG welding. The 1st layer in the welds obtained as
contained 4 pass beads, and 5 pass and 3 pass in 2nd and Pଷ = Tଷ [20 + log൫t ଶ,ଷ + t ଷ ൯] (5)
3rd layer, respectively. The Vickers hardness was In turn, the LMP from 1st pass to nth pass can be
measured for the specimens after polishing and etching expressed as
with 3㸣 nital solution. The thermal cycles in multi-pass P୬ = T୬ [20 + log൫t ୬ିଵ,୬ + t ୬ ൯] (6)
welds were calculated by House Code FEM software. where T n is the temperature of the nth pass, t n is the
holding time of the nth pass, and t n-1,n is the equivalent
3. Results and discussion holding time from 1st to (n-1)th pass at the temperature of
As to long-term operation in the tempering T n . The LMP during thermal cycle calculated by the
temperature range, the “Larson-Miller parameter (LMP)” newly proposed method is designated as Thermal Cycle
is a useful means for predicting the lifetime of material. Tempering Parameter (TCTP). Figure 1 shows the
LMP which is derived based on the Arrhenius rate relationship between hardness of the specimens and
equation is expressed as a function of time and TCTP of 2 nd and 3 rd thermal cycle. A good linear
* Graduate School of Engineering, Osaka University, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Japan Power Engineering and Inspection Corporation, Japan Japan
*** The Kansai Electric Power Co., Inc., Japan
127
Prediction of hardness in HAZ of low-alloy steel produced by temper bead welding using neural network
(a)

+Y

,62KHDWWUHDWPHQW

7KHUPDO&\FOHSDVV

7KHUPDO&\FOHSDVV

(b)

7&73
Fig.1 Relationship between TCTP and Hardness of multi-pass
thermal cycle
relationship can be seen between the hardness of the

specimens and TCTP. Hardness of the iso-thermal
heat-treated specimens is also on the same line. This
shows that the newly proposed TCTP can be applied to
the hardness change in tempering during both thermal
cycle process and iso-thermal heat treatment.
"Neural Network" (NN) [4], is a mathematical Fig. 2 Hardness prediction system of 2-Pass thermal cycle:
model or computational model that has been used to (a) 3D figure and (b) 2D-Contour figure
model complex relationships between inputs and outputs (Tp1=1350ఁ,CR1=91ఁ/s)
or to find patterns in data. Radial Basis Function (RBF)
is a powerful technique for interpolation of (a)
multidimensional space in NN. The output O(x i ) of the
network is thus
ଶ
O(x୧ ) = σ୬୨ୀଵ w୨ h୨ (x୧ ) = σ୬୨ୀଵ w୨ exp {െ൫x୧ െ c୨ ൯ /r ଶ } (7)
where n is the number of neurons in the hidden layer, c i
is the center vector for neuron i, and w i are the weights of (b)
the linear output neuron. The weights w i , c i , and r are
determined in a manner that optimizes the fit between
O(x i ) and the data.
Based on the experimentally obtained hardness data
base and the relation between hardness and TCTP, the Fig. 3 Peak temperature distribution of (a) 1-Layer and
hardness prediction system of multi-pass thermal cycle (b) 3-Layer multi-pass welding
was constructed. For example, Fig. 2(a) and (b)
respectively represent the calculated 3D and 2D-contour :0
figure of the complex relationship between hardness and (a)
T p2 / CR 2 of 2-pass thermal cycle when T p1 is 1350Υ

and CR 1 is 91Υ/s.

The thermal cycles in welds during multi-pass
welding were calculated by House Code FEM. Figure 3

demonstrates the calculated peak temperature distribution
in the section of 1-layer and 3-layer welds. On the basis %0
of the calculated thermal cycle parameter, the hardness in

the HAZ was calculated, and the predicted hardness (b) :0
distribution is shown in Fig. 4. The predicted hardness

and the experimental results are shown in Fig. 5. The
predicted hardness (red marks) well agreed with the
measured hardness (blue marks), indicating that the

prediction system was useful and effective.
%0
Fig. 4 Hardness distribution in HAZ of multi-pass

welding: (a) 1-layer and (b) 3-layer
128
4. Conclusions
(a) (1) Thermal Cycle Tempering Parameter (TCTP)
calculation method for multi-pass thermal cycles
process has been proposed based on LMP.
(2) On the basis of experimentally obtained hardness
data base and thermal cycle parameters calculated by
FEM, the hardness distribution in HAZ was
predicted using Neural Network.
(3) The predicted hardness was found in good
accordance with the experimental result. It follows
(b)
that the proposed prediction system is effective for
estimating tempering effect in multi-pass welding.
References
[1] J. Liao, K. Ikeuchi, F. Matsuda: Nuclear Engineering and
Design 183 (1998) 9–20.
[2] D. Deng, H. Murakawa: Computational Materials Science
37 (2006) 209–219.
Fig. 5 Comparison between measured and calculated Hv [3] K.G. Samuel, S.K. Ray.: International Journal of Pressure
of (a) 1-layer and (b) 3-layer Vessels and Piping 83 (2006) 405–408.
[4] D. Casasent, X. Chen: Neural Networks 16 (2003) 529–53
129
Surface tension of molten iron measured by oscillating droplet

†
method using electromagnetic levitation
Influence of oxygen adsorption on surface tension
OZAWA Shumpei*, TAKAHASHI Suguru*, SUZUKI Shoji**, SUGAWARA Hiroharu**,

HIBIYA Taketoshi***, and FUKUYAMA Hiroyuki****
KEY WORDS: (Surface tension) (Molten iron) (Oxygen adsorption) (Marangoni convection) (electromagnetic
levitation) (Oscillating droplet method) (High temperature melt) (Undercooling)
1. Introduction induce desorption of oxygen through an adsorption

Surface tension is one of the most important equilibrium mechanism. Although the boomerang shape
thermophysical properties to understand and optimize in a temperature dependence of surface tension is expected for
welding process through numerical simulation because its molten iron, it has not been experimentally confirmed yet
temperature coefficient is a driving force of Marangoni because a conventional technique for a surface tension
convection which affects the shape of a weld pool measurement such as the sessile drop method can assure
dramatically [1]. An accurate surface tension and its only the measurement at a comparatively low temperature
temperature coefficient at high temperature melt are to prevent the contamination of the sample by the
strongly required. measurement device.
The surface tension of molten metals is considerably In this study the surface tension of molten iron was
influenced by oxygen partial pressure, Po2, of the ambient measured by an oscillating droplet method using
atmosphere because oxygen which acts as surfactant is electromagnetic levitation (EML). This technique enables
adsorbed to a melt surface from the atmosphere gas [2]. us to measure the surface tension of molten metals over a
Thus it is very crucial to consider the effect of Po2 on wide temperature range including undercooling condition
surface tension measurement. When Po2 is low, the surface [3]. This technique can assure the Po2 control of the
tension of molten metal generally shows a negative measurement atmosphere. The purpose of this study was to
temperature coefficient. In this case the Marangoni measure an accurate surface tension and its temperature
convection flows radially outward in a weld pool (Fig. 1) coefficient for high temperature molten iron in
[1]. However, the temperature coefficient of surface tension consideration of oxygen partial pressure dependence at a
increases with increasing Po2. Consequently it turns to a wide temperature range.
positive value as long as the molten metal is not oxidized
under comparatively high Po2. In this case, Marangoni 2. Experimental procedure
convection flows radially inward in a weld pool. Even when About 800mg of an electrolytic iron (purity: 99.99%)
Po2 is high, the temperature coefficient is changed from a was electromagnetically levitated and then melted under the
positive value to a negative value like a “boomerang shape” flow condition (2L/min) of the mixed gas of high purity
at higher temperature because the temperature elevation argon and helium to fix the Po2 of 10-2Pa. The sample was
also melted under flow condition of the Ar/He-5%H2 mixed
gas with a moisture content of 2.66 ppm to lower the Po2 by
condensing of the H2O formed from the following reaction;
V V V
1
H 2 + O2 H2O (1)
T’ 2
T T T The Po2 of the inlet gas was confirmed by a zirconia
Marangoni convection T’ oxygen sensor maintained at 1008K. The oscillation
behavior and the temperature of the droplet were observed
from the upper side using a high speed video camera and a
Weld pool
pyrometer. The temperature of the sample was controlled
Fig. 1 relationship between temperature coefficient of by changing the flow rate of Ar and He gases.
surface tension and shape of weld pool
† Received on 30 September 2010 University, Tokyo, Japan

* Department of Aerospace Engineering, Tokyo **** Institute of Multidisciplinary Research for Advanced,
Metropolitan University, Tokyo, Japan Tohoku University, Sendai, Japan
** Department of Human Mechatronics Systems, Tokyo Transactions of JWRI is published by Joining and Welding
Metropolitan University, Tokyo, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
*** Graduate School of System Design and Management, Keio Japan
130
Surface tension of molten iron measured by oscillating droplet method using electromagnetic levitation
The frequencies of the surface oscillations of the m = 0, 䕕 Ar/He-5%H2 (Po2<7㽢10-9Pa )

䕦 Ar/He (Po2=1㽢10-2Pa)
±1, and ±2 for the l = 2 mode were analyzed from the 2400
observed images in consideration of the influence of thetwo
Surface tension V, 10-3N·m-1

I II III
types of droplet rotations, i. e. real rotation and apparent 2200
rotation [4]. The surface tension of molten iron was
3㽢10-10Pa
calculated from the Rayleigh equation [5] calibrated by 2000
the Cummings and Blackburn equation [6]. 4㽢10-14Pa
1800
4㽢10-12Pa
3. Results and discussions 1600
When Ar/He-5%H2 gas was used for the measurement, 7㽢10-9Pa
the oxygen sensor detected the Po2 of 2.0×10-23Pa at the 1400
inlet. However, Po2 varies depending on the sample Melting point
temperature because the equilibrium constant of the 1200
reaction (1) shows temperature dependence; the zirconia 1500 1600 1700 1800 1900 2000 2100 2200 2300 2400
oxygen sensor can not measure the Po2 of the gas Temperature T, K
surrounding the droplet maintained at certain temperature Fig. 2 surface tension of molten iron
but it detects the Po2 of an atmosphere introduced into the
oxygen sensor operated at 1008K. The Po2 of the Ar/He- When the sample temperature rises from 1580K to
5%H2 gas was evaluated as a function of temperature using 1810K, the Po2 of Ar/He-5%H2 gas increased from 4×10-
14
the standard Gibbs energy of formation of H2O, in which Pa to 4×10-12Pa due to the chemical equilibrium of
the equilibrium constant of the reaction (1) is calculated reaction (1). Since higher Po2 normally induces a lower
from the Po2 of 2.0×10-23Pa of the inlet gas at 1008K surface tension of molten metal due to oxygen adsorption at
measured by the oxygen sensor. comparatively low temperature, surface tension becomes
Figure 2 shows surface tension of molten iron lower than that of the pure value as shown at the region I.
measured by the oscillating droplet method using EML What has to be noted is that the temperature elevation
under the flow condition of mixed gases of Ar/He (Po2) and induces not only the increase of the Po2 but also desorption
Ar/He-5%H2 [7]. Uncertainty for the measurement plot was of oxygen due to the temperature dependence of
calculated based on the GUM (ISO Guide to the Expression equilibrium constant for oxygen adsorption under H2-
of Uncertainty in Measurement) [8], in which the coverage containing gas atmosphere at the same time. The amount of
factor of kp=2 was selected. oxygen adsorption is decided from the competition between
We successfully measured the surface tension of molten these two mechanisms. When the oxygen adsorption
iron over a very wide temperature range over 780K becomes small due to high temperature even at high Po2,
including undercooling regions regardless of measurement the surface tension would approach the pure value as shown
atmosphere. When the Po2 of the measurement atmosphere at the region II. When the equilibrium constant of oxygen
is fixed at 10-2 Pa regardless of sample temperature under adsorption becomes zero at high temperature, the surface
the flow condition of high purity Ar and He gases, we tension of molten iron measured under the mixed gas of
succeeded in the experimental observation of a “boomerang Ar/He-5%H2 shows pure value at the region III.
shape” temperature dependence of surface tension of Thus, the temperature dependence of surface tension of
molten iron involving Po2 for the first time; the surface molten metals can not be described as a linear relationship
tension increases as the sample temperature rises up to against temperatures as long as pure surface of it does not
about 2150K, and then it decreases above this temperature appear when the Po2 shows temperature dependence under
because the Po2 becomes less effective due to the reducing gas atmosphere such as H2 and CO. The surface
temperature dependence of oxygen adsorption equilibrium tension of molten metals should be described as functions
constant. The pure surface tension of molten iron free from of temperature and Po2 as is the case for molten silver [4].
oxygen adsorption can be deduced from the negative
temperature coefficient observed above 2150K described as 4. Summary
a dotted line. The surface tension of molten iron was measured by
When the measurement of the surface tension is carried oscillating droplet method using EML under flow
out under the flow condition of mixed gas of Ar/He-5%H2, conditions of mixed gases of Ar/He and Ar/He-5%H2. The
the surface tension decreases as the sample temperature surface tension was measured over wide temperature range
rises. However, it does not appear to change with of about 780K including undercooling condition. The
temperature uniformly but to show a kink at around 1850K. “boomerang shape” temperature dependence of surface
Since the variation of the surface tension at this kink is tension was experimentally confirmed at the Po2 of 10-2Pa.
beyond the uncertainty of the measurement, it is not the The temperature dependence of the surface tension showed
scattering of the measurement originating from the kink at around 1850K under the Ar/He-5%H2 atmosphere
measurement accuracy. This anomalous temperature due to the competition between the temperature dependence
dependence of the surface tension can be explained by the of Po2 and equilibrium constant of oxygen adsorption.
temperature dependence of the Po2 of the mixed gas of
Ar/He-5%H2.
131
Acknowledgements [4] S. Ozawa, T. Koda, M. Adachi, K. Morohoshi, M. Watanabe

This study was funded by Japanese Science and and T. Hibiya: J. Appl. Phys., 106, 034907, (2009), pp. 1-7.
Technology (JST) Agency. One of the authors (SO) wishes [5] Lord Rayleigh: Proceedings of the Royal Society of London
to thank the support from the Cooperative Research 29, (1879), pp. 71-97.
Program of Institute for Joining and Welding Research
Institute, Osaka University. [6] D. L. Cummings and D. A. Blackburn: J. Fluid Mech., 224,
(1991), pp. 395-416.
References [7] S. Ozawa, S. Suzuki, H. Sugawara, T. Hibiya, H. Fukuyama:
[1] C. R. Heiple and J. R. Roper: Welding J, 61, (1982), pp. 97- J. Appl. Phys., submitted.
117.
[8] Guide to the Expression of Uncertainty in Measurement,
[2] K. Mukai, Z. Yuan, K. Nogi and T. Hibiya: ISIJ ISO, (1995).
International 40, (2000), pp. 148-152.
[3] S. Ozawa, K. Morohoshi, T. Hibiya and H. Fukuyama: J
Appl. Phys., 107 014910, (2010), pp. 1-7.
132
Effect of welding sequences on the microstructure of electron beam

welded TA15 titanium alloy and 304 stainless steel joints with
copper filller metal†
WANG Ting*, ZHANG Binggang*, CHEN Guoqing*, and FENG Jicai*
KEY WORDS: (TA15 titanium alloy) (304 stainless steel) ('ual-pass electron beam welding) (:elding
sequence) (0icrostructure) (Intermetallic layer) (Cluster)
1. Introduction 3. Results and Discussion

Composite components of titanium alloy and steel can Macrostructures of the cross sections of the joints under
fully exert the advantages of these two materials different sequences are shown in Fig. 1. It can be seen that
simultaneously[1-2]. Fusion welding of titanium alloy and copper element caused clusters of yellow color located in
steel was difficult to implement because of the production the weld near 304SS in the joint under the first sequence.
of brittle phases in the weld[3-4]. So far, no literature about And another structure in dark gray is also located in the
successful fusion welding of these two alloys has been weld near TA15 in clusters. The joint cracked after welding.
reported. Conversely, pressure welding and brazing can For the joint under the second sequence, the yellow and
eliminate the problems in fusion welding because the base dark gray structures are distributed in the weld and
metals remain in the solid state during joining. Furthermore, d ispersed uniformly. Obviously, this kind of
many successful examples have been reported[5-7]. distribution state of the different structures in the welds is
However, the service conditions may make particular dependent on the welding sequence. For the first sequence,
processes unsuitable [8, 9]. Fe and Cu elements mixed in the weld in the first pass. Fe
In this paper, a copper interlayer sheet was adopted to and Cu are immiscible to each other. So the segregation of
join TA15 titanium alloy and 304 stainless steel by dual- Cu is very serious. But for the second sequence, Ti element
pass electron beam welding. The effect of welding has been melted into the weld in the first pass, so high
sequences on the microstructure and tensile strength of the melting temperature phase Fe-Ti can be considered as
joints were analyzed. nucleating particles and Cu solidified dispersedly in the
second pass.
In order to analyze the reason for the fracture of the joint
2. Experimental
under the first sequence, microstructures of the interface
The chemical compositions of the materials applied in
between TA15 and the weld and the zones I and II of each
this experiment were given in Tables 1, 2. 1 mm thick
joint are examined as shown in Fig. 2 and Fig. 3. There are
copper sheet was adopted as filler metal and embedded in
Cu-Ti intermetallic layers in the interfaces, with thicknesses
the contact face before welding, then fixed by spot welding
of about 75±5ȝP and 90±5ȝP, respectively. This is
using a TIG method.
because the Cu-Ti intermetallic layer is formed in
Dual-pass electron beam welding was used and two
welding sequences were carried out. In one sequence, the
first pass was located on the contact face between stainless Table 1 Chemical composition of TA15 titanium alloy
steel and the copper sheet, and the second pass on the
contact face between titanium alloy and the copper sheet. In
Al Zr Mo V Ti
another sequence, the location of the two passes is contrary. 5.5-7.0 1.5-2.5 0.5-2.0 0.8-2.5 bal
For both of the two passes in the two sequences, the
parameters are 55 kV accelerating voltage, 2450 mA focus
current, 300 mm/min welding speed㸪and 9 mA beam Table 2 Chemical composition of 304 stainless steel
current. C Ni Cr Mn Si Fe
Microstructure observation was with an optical
microscope and scanning electron microscope. Tensile 0.07 8-11 17-19 2.0 1.0 bal
strength was tested under a strain rate of 0.5mm/min.

* SKLP, Harbin Institute of Technology, Harbin, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
133
Effect of welding sequences on the microstructure of electron beam welded TA15 titanium alloy and 304 stainless
steel joints with copper filller metal
a Intermetallic layer a
,
Crack
TA15 304
ȝP
b
b
Intermetallic layer
II TA15

ȝP
Fig. 1 Macrostructures of the cross sections of the joints
under the two welding sequences. (a- The fisrt sequence, b- Fig. 3 Microstructure in zone I and II in the joints under the
The second sequence) two welding sequences. (a- Zone I in the fisrt sequence, b-
Zone II in the second sequence)
a
the last pass for the first sequence. But for the second
sequence, it is formed in the first pass, so it was reheated by
the second pass. Zone I is characterized by three phases, i.e,
dark gray TiCu, light gray TiFe 2 and solid solution of
copper with yellow color. But zone II only contains light
gray TiFe 2 and solid solution of copper with a yellow color.
Comparing the two joints, there is only little solid solution
of copper in zone I near the intermetallic layer, but more in
zone II. Copper is a soft metal, which can accommodate the
deformation, as a result, the heat stress in the region was
ȝP reduced. The more solid solution of copper there is, the
more prominent the reduction effect is. Consequently, a
crack free joint is obtained under the second sequence. The
b tensile strength is 234MPa and the joint fractured in the
intermetallic layer when it was stretched.
4. Conclusions
(1) A crack free electron beam welding joint of TA15 and
304 stainless steel is obtained by using a copper
sheet as filler metal. One important function of copper
is to reduces heat stress in the weld.
(2) The microstructre and property of the joint is affected
by the welding sequence. High quality joints can be
obtained under the welding sequence in which the
ȝP copper distributed uniformly in the weld.
Fig. 2 Intermetallic layers between TA15 and the welds in References

the joints under the two welding sequences. (a- The fisrt [1]. R. R. Boyer: Mater Sci and Eng, A., 213 (1996), pp.103-
sequence, b- The second sequence) 114.
134
[2]. X. J. Yuan, G. M. Sheng, B. Qin: Mater Character, 59 [6]. B. Qin, G. M. Sheng, J. W. Huang, B. Zhou: Mater
(2008), pp.930-936. Character, 51 (2006), pp.32-38.
[3]. A. Elrefaey, W. Tillmann: J. Mater Processing Technol, [7]. P. He, X. Yue, J. H. Zhang: Mater Sci and Eng. A., 486
209 (2008), pp.2746-2752. (2008), pp.171 -176.
[8]. Z. Sun, R. Karppi: J. Mater Processing Technol, 59 (1996),
[4]. X. Yue, P. He, J. C. Feng: Mater Character, 59 (2008),
pp.257-267.
pp.1721-1727.
[9]. M. Ghosh, S. Chatterjee: Mater Sci and Technol, 48 (2002),
[5]. A. Fuji, K. Ameyama, T. H. North: J. Mater Sci, 31 (1996),
pp.393-399.
pp.819-827.
135
Effect of grain size on solidification cracking susceptibility of type

†
347 stainless steel during laser welding
SHINOZAKI Kenji*, WEN Peng**, YAMAMOTO Motomichi*, KADOI Kota*,

KOHNO Yusuke* and KOMORI Takuo*
KEY WORDS: (Grain size) (Solidification cracking) (Stainless steel) (Laser welding) (Fine grain) (In-situ
observation) (Critical strain)
1. Introduction Figure 1 shows the experimental setup of U-type hot

It has been reported that coarse grains can induce a high cracking test [4,5] with the developed vertical in-situ
solidification cracking susceptibility compared with fine observation. The inclination angle of laser welding head
grains. Matsuda et al. evaluated the effect of grain size of was set as 30 degree to avoid the interference between
weld metal on solidification cracking susceptibility of camera and laser head. The fiber laser was used at the
aluminum alloys by using various self-restraint hot cracking power of 1.6kW and the travelling speed of 0.4m/min.
tests [1,2]. In this report, microstructure of weld metal Solidification behavior near the molten pool during laser
indicated the equiaxial grain. On the other hand, the effect welding was obtained with a high speed camera with 7
of grain size of the base metal on solidification cracking times magnification in U-type hot cracking test. By using
susceptibility has not been reported yet. Meanwhile, movie, critical strain of solidification crack was measured.
although some reports have been found on the effect of [6] In this study, gauge length was changed into 0.2, 0.5
grain size on liquation cracking during laser welding of Ni- and 1mm.
base alloys [3], there are few reports found on the effect of
grain size of weld metal in columnar structures on
solidification cracking susceptibility for materials, except
aluminum alloys.
In this paper, the effect of grain size on solidification
cracking was investigated by using a U-type hot cracking
test with in-situ observation method. Firstly, Type 347
stainless steel specimens with different grain sizes were
made by heat treatment. Then, high temperature ductility
curves of the specimens with different grain sizes were
obtained, and cracking susceptibilities were evaluated by
the CST.
2. Materials used and Experimental Procedure

Type 347 stainless steel (100lx30wx5mmt) was used as Fig. 1 Experimental setup of the vertical in-situ observation
the test piece. The chemical composition is shown in Table method
1. The thickness of welding part was machined from 5 to
3mm. The specimen was heated in an electric furnace for 3. Results and Discussion
different holding times to obtain different grain sizes of the Figure 2 shows grain size for the specimens used.
base metal before welding. The holding temperature was Regarding grain size of weld metal, the average width of
1200°C. The holding times were set as 0.5h, 1h, and 4h. the columnar grain was measured as the average grain size.
The measurement area was set in the bead centre.
Table 1 Chemical composition of material used (mass%) &RPSDUHG ZLWK JUDLQ VL]H RI EDVH PHWDO DV ȝPK
ȝPKȝPKȝPKWKHJUDLQVL]HRIZHOG
PHWDO VKRZV DV ȝPK ȝPK ȝPK
ȝPK It can be seen that the grain size of weld metal
is related to the grain size of the base metal.

** Tsinghua University, Beijing, China Japan
136
Effect of grain size on solidification cracking susceptibility of type 347 stainless steel during laser welding
ductility, thus, the more easily solidification cracks occur.

For the specimens of different grain sizes obtained in this
study, the cracking susceptibility was highest for the
specimen-4h in the weld metal.
Holding time at 1200Υ (h)
Fig. 2 Grain sizes compared between base metal and weld

metal
About 6-7 strain-time curves were obtained in each grain

size sample by the in-situ observation measurement method.
The crack initiation strain could be measured in each strain-
time curve. The strain-time curve was change to the strain- Fig. 4 Evaluation of solidification cracking susceptibility
temperature curve using the cooling curve in the weld metal. by high temperature ductility curves
Each plot indicates the crack initiation strain in Fig. 3. By
connecting these plots, the high temperature ductility curves The Trans-Varestraint test has been famous for
of various grain sizes in weld metal were drawn as shown in evaluation of solidification cracking susceptibility,
Fig. 3. For the weld metals with different grain size, the quantitatively. This test can measure BTR, but the lowest
measured critical strains decrease from 2.2 to 0.6% with an ductility is not so accurate.It is clear that solidification
LQFUHDVHLQJUDLQVL]HIURPWRȝP cracking susceptibility can be evaluated more accurately
and quantitatively by means of combining both the critical
strain obtained by U-type hot cracking test with in-situ
observation method and BTR obtained by Trans-Varestraint
test.
4. Conclusions
The effect of columnar grain size on solidification
cracking susceptibility of Type 347 stainless steel was
investigated by using U-type hot cracking test with
developed in-situ observation method. The obtained
conclusions are as follows.
(1) Specimens whose grain sizes of columnar structure in
ZHOGPHWDOYDULHGIURPWRȝPZHUHSUHSDUHGE\
changing the grain size of the base metal using heat
treatment.
(2) Local critical strains of solidification cracking were
measured by four specimens with different grain sizes
RI ZHOG PHWDO IURP WR ȝP +LJK WHPSHUDWXUH
Fig. 3 High temperature ductility curves of used specimens ductility curves were obtained based on various critical
with different grain size strains.
(3) The effect of grain size on solidification cracking
susceptibility was evaluated quantitatively by using the
Figure 4 shows the critical strain rate of temperature
CST of high temperature ductility curves. It was found
drop (CST) based on the high temperature ductility curves
that a specimen of coarse columnar grain size of the
in Fig. 3. The CST of specimen-0h is about 4.7 (×10-4°C-1).
weld metal shows a high solidification cracking
With increasing the grain size, the CST declines
susceptibility comparing with that of fine grain size.
considerably to about 3.8 (×10-4°C-1) for the specimen-0.5h.
Then, the CST drops slowly with increasing the grain size. References
The CST shows about 3.4 (×10-4°C-1) for specimen-4h the [1] Luo X.J.: Study on hot cracking in heat affected zone of
largest grain size used. Therefore, it can be seen that a nickel-base superalloys Inconel718 by laser beam welding. Ph.D.
coarse grain size of base metal induces a high solidification Dissertation of Hiroshima University. Hiroshima Japan.
cracking susceptibility. That is to say, regarding the [2] Nakata K. and Matsuda F. : Quarterly Journal of the JWS,
solidifying weld metal, the larger grain size, the lower 13(1), 1995, 106-115.
137
[3] Matsuda F. Nakata K. Shimokusu Y. Tsukamoto K. and Arai 2008, 49-52.

K.: Transaction of JWRI, 12(1), 1983, 81-87. [6] P. Wen, K. Shinozaki, M. Yamamoto, T. Tamura and N.
[4] M. Yamamoto and K. Shinozaki: Weld. In the World, 9-10, Nemoto: Quarterly Journal of the JWS, 27(2), 2009, 134s-138s
2005, 49-57.
[5] K.Shinozaki and M.Yamamoto: Mate. Sci. Forum, 580-582,
138
Image processing analysis of growth of carbide particles promoting

†
SR embrittlement in HAZ of 2 1/4Cr-1Mo steel
KAWAKAMI Hiroshi *, TAMAKI Koreaki **, SUZUKI Jippei *, TAKAHASI Kanta ***,
IMAE Yousuke *** and OGUSU Soichiro ***
KEY WORDS: (Image processing) (Carbide) (SEM image) (Heat affected zone) (2 1/4Cr-1Mo steel) (SR
embrittlement) (Crack propagation) (Crack initiation) (Cleavage fracture) (Facet)
1. Introduction 3. Image processing

SR treatment (stress relief annealing) improves the Image processing was applied a SEM images of the
toughness of HAZ in 2 1/4Cr-1Mo steel and suppresses the cross section area and the fracture surface. Image
temper embrittlement[1]. However, SR embrittlement processing was carried out by assembling Image dividing,
occurs after long time heating at SR temperature[2]. Brightness&Contrast, Contraction and Expansion
Transition temperature rises when SR embrittlement occurs. treatments. Figure 2 shows an example of an original SEM
Microstructure changes also through SR treatment. image and image after image processing for the carbide
Especially, behavior of precipitation of the carbide particle particles on the fracture surface. Difference of the area
cannot be evaluated easily by manual treatment, because a between manual measurement and image processing for the
lot of particles exists in a microscopic area. Image
processing may help systematic investigation of the
dimension of the carbide particle.
Suitable image processing was developed to measure
shape of the carbide particles in an image of the scanning
electron microscope. The Shape of the carbide particles on
the fracture surface differs from that in the cross section
area when SR embrittlement occurs significantly. Peculiar
phenomena were considered by SEM observation on both
sides of the fracture surface in this study.
2. Specimen
2 1/4Cr-1Mo steel was used in this experiment. The Fig. 2 Example of image processed image with some
synthetic HAZ specimen was produced by a weld thermal carbide particles on fracture surface.
simulator and tempered at 975K. SR embrittlement occurs
from 10h as shown in Fig. 1. The tempered specimen was
fractured at very low absorbed energy with producing
cleavage fracture. The fracture surface and the cross-section
of each specimen were etched by 3% nital to reveal the
contours of carbide particles.
Fig. 3 Schematic diagram of shape of carbide particle

measured after image processing.
Fig. 1 Change of transition temperature vTr30.
* Mie University, Mie, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Professor Emeritus, Mie University, Mie, Japan Japan
*** Graduate School, Mie University, Mie, Japan
139
Image processing analysis of growth of carbide particles promoting SR embrittlement in HAZ of 2 1/4Cr-1Mo steel
centered large carbide is below 1%. Major axis, minor axis

and aspect ratio of the particle were measured by the
digital image after image processing.
Major axis, minor axis and aspect ratio of the particle
were defined as shown in Fig. 3. The particle with aspect
ratio of 1 shows a spherical shape.
4. Experimental results
The relationship between aspect ratio and diameter of
major axis of the carbide particle was measured by image
processing as shown in Fig. 4.
The growth direction of the carbide particle is stable
until 50h because gradient in these figures for cross section
area does not change significantly. This result shows that
the shape of the carbide particle retains the needle shape in
short-time SR treatment. Moreover, the carbide grows as a
polygonal type which has small aspect ratio against
diameter of major axis after 100h. In case of 500h, “p” and
“q” in Fig. 4(g) correspond with the polygonal type and the
needle type, respectively. When SR embrittlement occurs
significantly, coarse particles in the cross-section could not
be observed on the fracture surface and aspect ratio on the
fracture surface is lower than the cross-section. This result
shows coarsened carbide particle promote SR
embrittlement as a site of crack initiation or crack
propagation as shown in Fig. 5[3].
Fig. 5 Broken carbide particles at crack initiation site.
5. Conclusions
Image processing was developed to evaluate the shape
of the carbide particle in a SEM image. Detailed analysis
for the shape of the carbide particle by image processing
shows that coarse carbide particles are broken during crack
initiation and crack propagation.
References
[1] H. Kawakami, K. Tamaki, J. Suzuki, Y. Ichikawa.: Q. J.
Japan Welding Soc., 16 (1998), pp.243-251.
[2] K. Tamaki, H. Kawakami, J. Suzuki, T. Niinomi: Q. J. Japan
Welding Soc., 15 (1997), pp.502-508.
[3] H. Kawakami, K. Tamaki, J. Suzuki, K. Takahashi, Y. Imae,
S. Ogusu: Doc. of IIW, IIW-2302-09(2009), pp.1-13.
Fig. 4 Relationship between aspect ratio and diameter of

major axis of carbide particle.
140
Numerical simulation of impact toughness of welded joints for X80

†
pipeline steel
ZHANG Jianxun*, XIONG Qinren*, **, YANG Zhongna*, ZHENG Li*
KEY WORDS˖
˖(Pipeline steel) (Dynamic impact) (Numerical simulation)
1. Introduction Fig.1.
Issues of impact dynamics exist in various
engineering fields. As dynamic fracture problems were
complex in many experiments, people began to simulate
the whole process of impact dynamics and then analyze
the dynamic response of materials under impact loads in a
better way. Nowadays, nonlinear finite element method has
been widely used in various fields.
With the application of dynamic analysis software
ANSYS/LS-DYNA, a model of impact test specimen is
established and a solid model for the simulation impact test
is also set up in which the dynamic impact process for the
impact test is simulated. The absorbed energy is calculated
during the whole impact test and the difference in impact
toughness caused by the notch located in the weld metal,
HAZ and base metal is analyzed. Study proves that the Fig. 1 Three-dimensional numerical model and FEM
numerical model can be used in prediction and evaluation mesh for the impact testing
of the toughness of welded joints. For welded joints, the density is 7820 kg·m-3; elastic
2. Numerical modeling and meshing modulus and tangent modulus is 200GPa and 2.2GPa,
For impact toughness test, finite element software respectively; Poisson ratio is 0.28; hardening exponent is
LS-DYNA is used to carry out the dynamic numerical 0.13; strain rate parameters are 40 and 5 separately.
simulation of X80 pipeline steel welded joint. The actual Yield strength and failure strain have some effect to
impact test process is completely done according to impact toughness. Therefore, the material properties of
Chinese standard GB/T229-1994. In the three-dimensional HAZ (including coarse grain zone and fine grain zone) are
solid model, the supports are simulated as two fixed baffles. simulated by changing these two parameters. The
The dimension of the model is designed by the actual properties of each region in the welded joint specimen are
standard impact specimen. The shape and size of the shown in Table 1. For the impact rammer, the elastic
impact rammer is modeled by the cutting edge shape of the modulus and Poisson ratio is 400 GPa and 0.3, respectively.
actual pendulum. The total width of the HAZ is 3.5mm, The density is 6.8×106 kg·m-3.
among which the coarse grain zone is 1mm and the fine
Table 1 Properties of welded joint at different parts
grain zone is 1.2mm.
The element meshes near the notch are dense while Region Yield strength ı s /MPa Failure strain H
those far from the notch are sparse. When the notch is
Base metal 560 0.5
located in HAZ, weld metal or base metal, the Coarse grain zone 545 0.45
heterogeneity of HAZ has great influence on the specimen Fine grain zone 550 0.47
impact result. The region near the notch is divided to
simulate each area of the HAZ. The properties of material
far away from the notch are set as those nearby. The impact
When the notch is located at weld metal, HAZ and
toughness is simulated respectively when the notch is
base metal, the fracture situation of impact numerical
located at the three different regions. The impact model
model is shown in Fig 2.
graph for the notch is located at weld metal is shown in
* State key laboratory for mechanical behavior of materials, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Xian Jiaotong University, Xian, China Japan
** Tubular Goods Research center of China National
141
Numerical simulation of impact toughness of welded joints for X80 pipeline steel
(c) The notch located at base

(a) The notch located at weld metal (b) The notch located at HAZ
metal
Fig. 2 Fracture model for different notch locations
When the notch is located at the weld metal, cracks According to the dynamic numerical simulation
initiate at the root of notch and weld metal, and then results and the force/displacement curves under various
propagate through the coarse grain zone. When the notch is conditions, the impact absorbing energy, peak load and the
at the fusion line, the crack develops mainly through the initial cracking power are all counted as Table 2 shows.
coarse grain zone, which accounts for a large proportion of
the fracture path. The specimen broke at the weld metal Table 2 Results statistics for notch located at different parts
finally. When the notch is located in the HAZ, crack also
grows through coarse grain zone. It can be seen that the Weld metal HAZ Base metal
boundary between coarse grain zone and fine grain zone on
the fracture cross section obviously. When the notch is Peak force F/kN 24 23.3 25.1
located at the base metal, the crack completely propagates Impact absorbed energy W/J 289 246 307
through the base metal and the plastic deformation is large
at impact fracture. Initial crack energy W 1 /J 96 83 107
For analyzing the impact toughness of joint specimens,
it is necessary to calculate the absorbed energy during the From the table above, the load required for base
impact process. The impact toughness (absorbed energy) metal fracture is the largest t. The impact absorbed energy
can be obtained from the force/displacement curve as shown of base metal is 307J, which is much higher than 246J for
in Fig. 3. HAZ. That indicates HAZ properties have seriously
declined. The toughness of weld metal near the HAZ has
25000
Gap located at weld metal
declined as well. It is the most difficult for base metal to
Gap located at HAZ initiate cracks so the required initial cracking power is the
20000 Gap located at base metal largest. Therefore, the toughness of base metal is the best

and HAZ is the worst.
Force F/N
15000
10000
4. Conclusion
The LS/DYNA finite element software is used to
5000 simulate the impact testing with a reasonable FEM model.
The numerical results show that the impact toughness is
0 affected by yield strength and failure strain. The impact
0.00 0.01 0.02 0.03 toughness is different when the notch is located at different
displacement S/m regions. The impact toughness is the worst for a notch
located at the HAZ and best in the base metal. It can be
Fig. 3 Three force/displacement curves for notch
used to predict the impact toughness of welded joint and
located at different parts provides a new method to evaluate the properties of joint.
Comparing the curves above it can be seen that the
References
location of the notch has a great influence on the impact [1] Atkinson.C, Eshelby JD.:International Journal of Fracture
energy when the difference of material properties between Mechanics, (1968), pp. 3-8.
HAZ and base metal is large. When the notch is at the base [2] Mott NT. Fracture of metals theoretieal consideration.
metal, the force/ displacement curve is the highest and the Engineering, 165 (1948), pp.16-18.
enclosed area is the biggest. This means the impact
toughness there is the best. When the notch is at the weld
metal, the toughness gets worse and becomes worst when
the notch is in the HAZ. That is because the yield strength
and fracture strain have a certain decline. Besides,
softening phenomena in HAZ causes the impact toughness
to reduce significantly.
142
Numerical analysis of deformation and thermal behavior during

†
ultrasonic Al ribbon bonding
SUZUKI Shinji *, OYAMA Yusuke *, MAEDA Masakatsu **, and TAKAHASHI Yasuo **
KEY WORDS: (Eco electronics packaging) (Ultrasonic bonding) (Numerical simulation) (Ribbon bonding)
(Power electronics assembly)
1. Introduction the heat input per unit volume and unit time is calculated to
In the recent years, thick Al ribbon bonding has been be 4.0x10-9Jm-3s-1. The heat was supplied only to the
applied to the packaging of power devices such as IGBT elements in contact with the bond-interface in proportion to
(Insulated Gate Bipolar Transistor) modules to secure high the volume of each element.
power density and to improve power control. These are Calculation of plastic deformation of Al ribbon was
very important for green innovations. carried out by using a finite element method[5]. The strain-
Al thick wire bonding is used in the power electronics rate-depending large plastic deformation was taken into
packaging. The wire bonding process has been studied account. The tool and the substrate were assumed to be
experimentally [1, 2, 3] and numerically [4, 5]. These rigid bodies. We assumed that the interface between tool
studies are useful to understand the wire bonding and ribbon was fixed but the interface between ribbon and
mechanism, wire deformation and interfacial behavior substrate was able to slip. The material constants of heat
during bonding. The Al ribbon bonding is affected by conduction and plastic deformation were given from
temperature rise of the bond-area and ribbon deformation. literatures[5, 6].
The temperature rise is related with frictional slip behavior
at the bond-interface. In the present study, a simple 3. Experimental procedure
numerical model of the ultrasonic Al ribbon bonding is The ribbon bonding tests are carried out under the
proposed. The heat conduction between the Al ribbon and condition of ultrasonic power 1~4 W, bonding force
tool (substrate) is modeled to visualize the temperature 1~5.0N and frequency 60kHz. The Al ribbon of 1mm wide
change and distribution. The plastic deformation behavior and Si chip (or SiO2 substrate) were used. The bonding
affected by the friction slip is numerically examined. The time (duration of ultrasonic vibration input) was 100 ~
calculated results are verified, based on the experimental 400ms.
results.
2. Numerical modeling and simulation procedure Figure 2 shows the calculated results of heat conduction
Figure 1 shows the mesh pattern of the bonding tool, Al (change of temperature T with time t at positions A ~ G
ribbon, Al electric pad, and Si chip (or SiO2 substrate). The along y axis of Fig. 1. The bottom of chip and the top of
bonding tool is made of WC. The model is two tool are assumed to be cooled at 300K, i.e., Ts = Tt = 300K,
dimensional and the heat flow in the z direction where Ts is the temperature of imaginary elements (meshes)
(perpendicular to the space) is ignored because the length under the bottom of chip and Tt is the temperature of
of substrate in the z direction is 10 times greater than the imaginary elements on the top of tool. The heat input rate
thickness of the substrate (2.4 mm) and the bottom of the into the bond-interface is constant during bonding. As can
substrate is assumed to be cooled at 300K (in contact with be seen in Fig.1, temperature continously increases at time
a large heat sink). Two boundary conditions were given to t > 0 (after ultrasonic power is inputted) and decreases after
the top of the bonding tool; 1) at 300K and 2) J = 0 in the y t >100s (ultrasonic power is turned off). The temperature
direction, where J is the heat flux. The heat conduction curves for the positions A~F are convex up during bonding
behavior was calculated by using a finite differential but that of position G changes from concave to convex.
method, based on the control volume method. The heat This is due to thermal flow in the x direction. It is
generation at the bond-interface is produced by the friction suggested that Al ribbon heats up to 393K.
slip at the bonding interface. The heat generation is Figure 3 shows the temperature distribution map when
affected by ultrasonic power input. For example, if the heat the substrate is silica and Ts = Tt = 300K without heat
input of 4 W is given to the elements in the vicinity of the resistance of the interfaces. The Al ribbon is heated up
bond-interface and the bonding area is 1mm x 100μm, then uniformly as shown in Fig. 4. Because thermal
͊ Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding

* Graduate student, Osaka University, Suita, Japan. Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Center for Advanced Science and Innovation (CASI), Osaka Japan
University, Suita, Japan.
143
Numerical analysis of deformation and thermal behavior during ultrasonic Al ribbon bonding
Fig. 3 Temperature distribution for silica substrate,

Tt = Ts = 300K. The temperature of Al ribbon is
about 530 K because of small thermal conductivity
Fig. 1 Schematic illustration (Mesh pattern of cross of silica.
section) of bonding tool, Al ribbon, Al pad,
and substrate (Si chip or silica).
Fig. 4 Equivalent stress distribution of Al ribbon when

the displacement rate of 1.88x10-2 m/s is applied
to right hand direction of the top of ribbon. The
bonding pressure P = 15MPa, the ultrasonic
vibration amplitude is 50nm at the top side of Al
ribbon. Bond-interface can frictionally slide
( u x §1.76x10-2m/s at the bond-interface).
Fig. 2 Temperature change of representative
distribution were visualized. The main results are as
positions A~G which are denoted in Fig. 1.
follows;
conductivity of silica is smaller (1/102), than that of silicon, (1)Al ribbon heats up to about 373 K, if the ultrasonic
Al ribbon heats up to 532K. The temperature at the power is less than 4W.
bonding interface was measured experimentally. It was (2) Insulating or heating of the bonding tool is effective
about 365~370K during bonding. Actual temperature rise for heating Al ribbon.
is about 100K at the highest. (3) Large stress is not obtained under the free slip
Al ribbon is deformed as the temperature rises. The plastic condition, i.e., the large compression of Al ribbon
deformation with strain rate dependence was simulated by cannot be produced.
the assuming that the Al ribbon is kept at T = 373K, where (4) Large stress is produced under the frictional slip or
T is average temperature of the ribbon. Figure 4 shows the fixed conditions and Al ribbon largely deforms. This is
equivalent stress distribution in the Al ribbon. Fig. 4 is for a softening effect of ultrasonic vibration.
the frictional slip condition. (5) Revolving moment is produced after Al ribbon adheres
As can be seen in Fig. 4, the equivalent stress strikingly to Al Pad.
increases up to be 10 times greater than the bonding
References
pressure. This is an ultrasonic vibration effect. As a result, [1] S. Kitamori, M. Maeda and Y. Takahashi: MATE 2006, Vol.
a large plastic strain rate is produced by ultrasonic 12, JWS, Yokohama, (2006) pp. 345-348.
vibration. After the bond- interface is fixed, a revolving [2] A Shah et al.: J. Applied Physics, Vol. 106 (2009) pp.
moment is produced. The very high shear stress greater 013503-1~8.
than 1700 MPa causes the increase of the equivalent stress. [3] H. Gaul, M. Schneider-Ramelow and H. Reichl: Microsystem
Technol. Vol. 15 (2009) pp.771- 775.
5. Conclusions [4] Y. Ikeda et al. : MATE 2001, Vol. 7, JWS, Yokohama, (2001)
The ultrasonic bonding of Al ribbon is necessary for pp. 5-8.
power electronics packaging technologies. The temperature [5] Y. Takahashi and M. Inoue: J. Electronic
Packaging, ASME, Vol. 124, (2002) pp. 27-36.
rise and plastic deformation during the ultrasonic bonding
[6] Dictionary of physics and chemistry, Vol. 4, Iwanami, Tokyo,
were simulated. The temperature distribution and stress Japan (1992) .
144
Visualization of heat and stress flows in thermodynamic crystals

†
fabricated by laser scanning stereolithography
KIRIHARA Soshu *, UEHARA Yasunori *, TAKINAMI Yohei * and TASAKI Satoko *
KEY WORDS: (Thermodynamic crystal) (Heat and stress flow) (Stereolithography) (CAD/CAM/CAE)
1. Introduction processes, sub-millimeter order three dimensional

Thermodynamic crystals are new artificial materials composite models were formed successfully. After
with periodically percolated morphologies of metals and dewaxing process of alumina dispersed resin precursor at
ceramics to control heat and stress flows intentionally by 600 ºC for 2 hs with heating rate of 1 ºC/min, the samples
using laser scanning stereolithography, freeform sintering were sintered at 1500 ºC for 2hs with the heating rate of 8
and precision casting. Artificial dislocations of point and ºC/min. Subsequently, the polyester resin past mixed with
plane defects were introduced to localize thermal and WKH SXUH FRSSHU SDUWLFOHV RI ȝP LQ GLDPHWHU DW LQ
mechanical energies strongly through the computer aided volume contents were percolated into the inverse ceramic
design, manufacturing and evaluation. The alumina structures. After the resin dewaxing for the infiltrated
structures including air spheres with body centered cubic samples at 800 ºC for 2 hs with the heating rate of 1 ºC/min,
patterns were processed by using the stereolithography [1- the pure copper particles were sintered at 1000 ºC for 2hs
4]. Resin slurries with pure copper particles were infiltrated with the heating rate of 8 ºC/min in an argon atmosphere.
into the formed ceramics objects. After heat treatments, the The relative densities of the sintered samples were
thermodynamic crystals with the metals spheres measured by using Archimedes method. The part accuracy
arrangements in the ceramics matrices could be obtained. of the metal spheres arrangements in the ceramic matrices
These artificial microstructures were observed by using a were measured by using a digital optical microscope
digital optical and scanning electron microscope. Thermal (Keyence, VHX-200) system. And, the microstructures of
and mechanical properties were simulated through a finite the ceramic and metal phases were closely observed by
difference time domain simulation. The directional using the scanning electron microscope (JEOL, JSM-6060).
distributions of the heat and stress flows in the periodically The heat and stress flows were simulated in the crystals by
percolated materials morphologies will be discussed. using a finite difference time domain application (Cybernet
Systems, Ansys).
2. Experimental Procedure
The three dimensional body center cubic structures were
created by the computer aided graphical design application
(Toyota Keram, Think Design) as shown in Fig. 1. The
inverse crystal model of 10×10×10 mm in size included the
air spheres of 4.0 mm in diameter. The lattice spacing for
<100> direction was 4.5 mm. The volume ratio of the
matrix was 26.5 %. The three dimensional ceramics models
were fabricated automatically by using the
stereolithographic machine (D-MEC, SI-C1000). The
designed models were converted into the rapid prototyping
format of the stereo-lithography files and sliced into thin
VHFWLRQV 7KH DOXPLQD SDUWLFOHV RI ȝP LQ DYHUDJH
diameter were dispersed into the photo sensitive acrylic Fig. 1 A computer graphic model of thermodynamic crystal
resin at 70 % in volume contents. The resin paste with the with an inverse body centered cubic lattice. Air spheres are
alumina particles was spread on a glass substrate with 50 closely arranged in a bulk to realize a spatial periodicity.
μm in layer thickness by using a mechanically moved knife
edge. An ultraviolet laser beam of 355 nm in wavelength
DQGȝPLQEHDPVSRWZDVVFDQQHGRQWKHUHVLQVXUIDFH 3. Results and Discussion
WR FUHDWH WZR GLPHQVLRQDO LPDJHV ZLWK ȝP LQ scanning The three dimensional periodic structures composed of
part accuracy. Through the layer by layer stacking the alumina dispersed acrylic resin were processed exactly

Japan
145
Visualization of heat and stress flows in thermodynamic crystals fabricated by laser scanning stereolithography
by using the stereolithography. The spatial resolution in the intermediate layers. The heat and stress flow patterns in the
fabricated body was approximately 0.5 % in size. Figure fabricated thermodynamic crystals were simulated as shown
2(a) shows (100) planes of the sintered body centered cubic in Fig. 3(a) and (b), respectively. The heat flow
structure composed of the micrometer order alumina transmitted effectively from the source plane to the opposite
lattices including the air spheres. Deformation and cracking side along the connected copper spheres of the percolated
were not observed. Linear shrinkage on the horizontal axis metal phases with high thermal conductivities. And, the
was 6.5 % and that on the vertical axis was 7.8 %. It is tensile stresses were distributed periodically into the
possible to obtain the uniform shrinkage by designing an alumina lattices of the distributed ceramics phases with high
appropriate elongated structure in the vertical direction for Young's modulus. Through introductions of point or plane
compensating the gravity effect. The relative density defects in to the perfect periodic structures, the heat and
reached at 98.5 %. Dense alumina microstructure was stress flows can be localized into the specific regions to
formed, and the average grain size was approximately 2 μm. control the thermal and mechanical properties of the
Figure 2-(b) shows the (100) plane in the sintered artificial crystals.
thermodynamic crystal composed of the pure copper
spheres and alumina matrix. Diffraction peaks indicating 4. Conclusions
the formation of copper oxide phases did not appear in X- Three dimensional thermodynamic crystals with body
ray diffraction spectra. Sintering defects of cracks and pores centered cubic structures composed of pure copper spheres
were not observed in the microstructures of the copper arrangements in alumina matrices were fabricated by using
phase. Smooth interfaces between the copper spheres and stereolithography and heat treatment processes. The
alumina matrices were obtained successfully. These periodic arrangements with high part accuracies of dense
material phases were joined continuously without
Fig. 2 A sintered alumina lattice with the inverse body centered cubic structure fabricated by using stereolithography of a
structural joining process (a) and a formed thermodynamic crystal with periodic arrangements of pure copper spheres in an
alumina matrix though powder sintering treatments (b).
Fig. 3 The computer graphic models of simulated heat and stress distributions in the fabricated thermodynamic crystals
with the body centered cubic structure. The graphics (a) and (b) show the heat and stress flows through the connected metal
spheres and the continuous ceramic matrix, respectively.
146
alumina and copper phases were observed and verified by for Advanced Structural and Functional Materials Design)
using a digital optical and scanning electron microscope. from the Ministry of Education, Culture, Sports, Science
The heat and stress distributions in the thermodynamic and Technology (MEXT), Japan.
crystals were simulated and discussed theoretically by finite
difference time domain methods. The heat flow transmitted References
effectively through the connected copper spheres with high [1] C. Kai and L. Fai: Rapid Prototyping, Singapore John Wiley
thermal conductivities, and the tensile stress were and Sons, (1997).
distributed in the alumina matrices periodically with high
[2] A. Pique, A.Holmes and D. Dimos: Materials Research
Young's modulus. Society Symposium Proceedings, (2003), pp.758-764.
5. Acknowledgments [3] S. Kanehira, S. Kirihara and Y. Miyamoto, Journal of the
American Ceramic Society, 88 (2005), pp.461-1464.
This study was supported by Priority Assistance for the
Formation of Worldwide Renowned Centers of Research - [4] S. Kirihara and Y. Miyamoto, The International Journal of
The Global COE Program (Project: Center of Excellence Applied Ceramic Technology, 6 (2009), pp.41-44.
147
Visualizations of microwave emissions through pure copper

photonic crystals†
TAKINAMI Yohei *and KIRIHARA Soshu **
KEY WORDS: (Visualization) (Microwave) (Photonic crystal) (Stereolithography) (Powder sintering process)
1. Introduction application. Figure 1 shows the designed models of the

Photonic crystals with periodic arrangements of metal inverse photonic crystal. The air sphere diameters were
or ceramic media exhibit forbidden bands in optimized as 2.82 to 3.0 mm through the theoretical
electromagnetic wave transmission spectra [1]. These simulations and visualizations of the electromagnetic fields.
artificial crystals have been developed to be applied to The whole crystal was designed as 12 ×12×6 mm in edge
novel electromagnetic wave control devices such as band lengths to include 4×4×2 numbers of the unit cells.
pass filters, telecommunication equipments, and Subsequently, the modified crystal structure with the
waveguides [2]. In this investigation, pure copper photonic compressed lattice spacing for the <100> direction at 70 %
crystals were fabricated successfully in sub-millimeter to in size ratio was designed successfully. Figure 2 shows a
control microwaves by using stereolithography. The pure schematic illustration of the stereolithography system. In
copper has thermal shock resistances and shows nearly the fabrication process, photo sensitive resin paste
perfect reflection properties. Moreover, the modified including pure copper particles was spread on a substrate
photonic crystals with compressed lattice spacing in by a moving blade. An ultraviolet laser was scanned on the
specific direction were designed and fabricated. These resin surface to create cross sectional patterns. Through the
compressed crystals can be expected to realize directional layer by layer process, solid composite objects were formed.
transmissions through anisotropic wave diffractions. To Dense pure copper structures were obtained by successive
confirm directive emissions of microwave intensities, dewaxing and sintering at 800 and 1080 °C in an argon
radiation patterns from a monopole antenna located inside atmosphere to prevent the metal phase oxidations. The
the crystal were visualized by using finite difference time microwave propagations through the fabricated photonic
domain simulation. crystals were measured by a time domain spectroscopy
system. Obtained results were compared with simulated
ones. The microwave radiating patterns from the monopole
antenna located inside the compressed crystal lattice were
visualized to confirm the directive emission by using the
finite element simulation.
Fig. 1 Computer graphics of an inverse sphere structure

with a body centered cubic arrangement.
The photonic crystal structure was designed as an Fig. 2 A schematic illustration of stereolithography
inverse type with the periodic arrangements of air spheres system of a computer aided design and manufacturing.
in a pure copper bulk by using a computer graphic
* Graduate school, Osaka University, Suita, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** JWRI, Osaka University, Suita, Japan Japan
148
Visualizations of microwave emissions through pure copper photonic crystals

The crystal planes of the fabricated photonic crystal
with the inverse body centered cubic arrangements are
shown in Fig. 3. The hollow structures were precisely
shaped without macro fractures or deformations. The
smooth surfaces were obtained successfully through the
layer by layer stacking of the thin cross sections in the
micrometer order processing. Achieved spatial resolution
was 1.0 % approximately. And, copper oxide peaks were
not detected in an X-ray diffraction spectrum. In
transmission spectra through the obtained metal photonic
crystals, the common forbidden region especially called the
perfect band gap was observed from 95 to 110 GHz in
frequency range. The other opaque band was shown under
80 GHz meaning typical cut off effects through the metal
hollows. In the simulated results, the perfect band gap was
observed in the frequency range from 94 to 110 GHz nearly
coinciding with the measured one. And, the measured
microwave transmittances of the pass bands were lower
than the simulated ones. The incident electromagnetic Fig. 4 Electric field distributions of (a) transmission and (b)
waves are considered to be scattered by the fabricated real band gap modes simulated by using a transmission line modeling
method of a finite difference time domain.
surfaces of sintered pure copper. The copper inverse sphere
structures were verified to forbid the propagations of
microwave for all directions. Figure 4 shows the
visualization of the electric field distributions through the
inverse photonic crystal for <100> direction. Bright areas
mean the space with higher electronic intensity, while dark
one indicates lower. At the frequency of the band gap
region, propagating waves from left side were reflected
perfectly. On the other hand, at the frequency of
transmission region, the electric field intensities were
concentrated into air spheres and the high transmittance
properties were exhibited. These phenomena are considered
to be caused through surface plasmon polariton effects. In
the case of electromagnetic wave propagating into the
metal structures, the surface plasmon polariton was excited Fig. 5 A microwave radiation pattern from a monopole
on the metal surface with the periodic gaps. The high antenna embedded into the compressed crystal structure.
transmission properties are attributed to the resonant
coupling of the free space electromagnetic waves vibrations 112 to 130 and 104 to 118 GHz, respectively. In the
with the occurred surface plasmon polariton [3]. Figure 5 selected frequency band from 105 to 110 GHz, the
presents the radiation pattern from the monopole antenna microwaves were permitted and prohibited wave
inside the compressed photonic crystal at the frequency of propagations along the parallel or perpendicular routes for
108 GHz. The forbidden bands for <100> and <010> the compressed direction, respectively. The directional
crystal directions parallel and perpendicular to the lattice wave transmission and energy concentration for the limited
compression axis were exhibited in the frequency ranges of angle area through the modified metal photonic crystal with
the compressed lattice spacing were demonstrated clearly.
4. Conclusion
We succeeded in fabrications of pure copper photonic
crystals with or without compressed lattice spacing by
using stereolithography and a powder sintering process.
Fine metal structures were precisely formed without
delamination and fracture. The obtained photonic crystals
showed perfect band gaps from 95 to 110 GHz in frequency.
The modified crystal with compressed lattice spacing
Fig. 3 Pure copper photonic crystals with the inverse
exhibited directional transmission properties at the
body centered cubic structure fabricated by using the
frequency range from 105 to 110 GHz. Simulated and
stereo-lithography and powder sintering processes.
measured transmission properties of the microwave
propagation through the copper crystals showed good
149
agreements. The compressed metal crystals are considered for Advanced Structural and Functional Materials Design)
to be capable of controlling the emission of high energy from the Ministry of Education, Culture, Sports, Science
microwaves in the near future industrial fields. and Technology (MEXT), Japan.
References
Acknowledgments
[1] E. Yablonovitch: J. Opt. Soc. Am. B, 10, (1993), pp.283.
This study was supported by Priority Assistance for the [2] M. Notomi, A. Shinya, S. Mitsugi, E. Kuramochi and H-Y.
Formation of Worldwide Renowned Centers of Research - Ryu: Optics Express,12 , (2004), pp. 1551-1561
The Global COE Program (Project: Center of Excellence [3] F. Miyamaru and M Hangyo, appl. Phys., 84,(2004), pp. 2742,
150
Visualizations of terahertz frequency amplifications in water cells

†
introduced into alumina diamond photonic crystals
OHTA Noritoshi *, NIKI Toshiki * and KIRIHARA Soshu **
KEY WORDS: (Photonic crystal) (Terahertz waves) (Micro stereolithography) (Transmission line modeling)
(Localized mode)
a unit cell of the diamond photonic crystal, components of

1. Introduction the resonance structures, and the cross sectional image of
Photonic crystals with periodic variations in dielectric the terahertz wave resonator, respectively. The micro glass
constants can exhibit forbidden band in transmission cells including pure water were sandwiched as a plane
spectra of electromagnetic waves to realize total reflections defect between two alumina photonic crystals with the
through Bragg diffraction [1]. Diamond lattice structures diamond lattice. In order to operate this resonator under the
with three-dimensional periodicities can prohibit the wave low loss conditions within the terahertz region, geometric
propagations for all directions in the perfect band gaps. By parameters of the models were calculated and optimized by
introducing artificial defects of air cavities into the periodic using a transmission line modeling simulator (Flomerics,
arrangement, the waves corresponding to the defect sizes Micro-Stripes) of a finite difference time domain method.
can be localized and amplified in the photonic crystals [2]. In the unit cell of the artificial crystals, the lattice constant
Our investigation groups have fabricated successfully the and the aspect ratio of the dielectric lattice were optimized
ceramic photonic crystal with diamond structures composed as 375 ȝP DQG to create the wider band gap in the
of fine ceramic lattices to controlled terahertz waves by terahertz frequencies. The localized frequency is tunable by
using micrometer order stereolithography. In the near future adjusting the defect thickness of the resonator. In this
industries, the terahertz waves can be expected to be investigation, the plane defect was designed as a water cell
applied to various types of novel sensors for detecting RI ȝP LQ WKLFNQHVV FRPSRVHG RI WZR TXDUW] SODWHV RI
harmful substances in human bloods, early stage cancer ȝP DQG DQ DTXHRXV FDYLW\ RI ȝP 7KH UHVRQDQFH
cells in human skins and micro bacteria in vegetables [3]. In qualities can be enhanced by increasing the number of
this study, we designed and fabricated terahertz wave micro diamond structural units in the resonator. However, the
resonators composed of aqueous cavities introduced the transmission level of the localized mode peak becomes
diamond photonic crystals to amplify the sensing signals in lower through the perfect confinement of the
the liquid region. Their wave properties were measured by electromagnetic wave energy into the defect domain. The
spectroscopy and compared with theoretical visualizations diamond lattices composed of two units in the period
of electromagnetic fields. number were optimized in order to detect the sharp
localization peak in the transmission spectrum.
2. Calculations
Figure 1(a), (b) and (c) show schematic illustrations of
Fig. 1 Schematic illustrations of a unit cell of diamond structure (a), components of resonance cells (b), and a terahertz wave
resonator (c). The resonator is composed of two diamond photonic crystals to localize the terahertz waves in an aqueous phase.

* Graduate school, Osaka University, Suita, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** JWRI, Osaka University, Suita, Japan Japan
151
Visualizations of terahertz frequency amplifications in water cells introduced into alumina diamond photonic
crystals
3. Experimental Procedure ceramic sample reached 97.5 %. The integrated terahertz

The diamond lattices were designed exactly by using a wave resonator is shown in Fig. 3-(b). Two diamond lattice
graphic application (Toyota Caelum, Think-Design). Whole components were attached on the quartz glasses, and these
size of the crystal component was 5×5×1 mm consisting of SODWHV ZHUH DUUDQJHG ZLWK ȝP LQ SDUDOOHO LQWHUYDO
10×10×2 unit cells. After slicing operation, these data were Tolerance for the transmission direction of the
transferred into a micro stereolithographic equipment (D- electromagnetic wave converged within 5 ȝP In the
MEC, SI-C 1000) as schematic illustrated in Fig. 2. Photo transmission spectrum through the resonator including
sensitive acrylic resin including alumina particles of 170 distilled water, the localized mode of transmission peak was
nm in average diameter at 40 percent in volume contents observed at 0.410 THz in the band gap. The measured peak
were supplied on a glass substrate with 15 ȝP in layer frequency has good agreement with the simulated result by
thickness by using a mechanical knife edge. And, two the transmission line modeling. The cross sectional profiles
dimensional images of a visible ray were exposed through a of the electric field intensity corresponding to the localized
digital micro mirror device with 2 ȝP in part accuracy. modes were simulated and visualized theoretically as shown
Through the layer by layer stacking under the computer in Fig. 4. Bright and dark areas indicate the high and low
control, the acrylic resin component with the alumina intensities of the electric field, respectively. The incident
particles dispersion was obtained. The composite precursor terahertz waves were resonated and concentrated strongly
was dewaxed at 600 °C for 2 hs and sintered at 1500 °C for through the multiple reflections in the liquid cell between
2 hs in air atmosphere. Subsequently, in order to create a two diffraction lattices with the diamond structures. By
plane defect between two diamond structures, a micro glass replacing the water with ethanol, the localized frequency
cell was also fabricated by the micro stereolithography. The was shifted from 0.410 to 0.430 THz in frequencies due to
quartz plates of 160 ȝPLQWKLFNQHVVZHUHLQVHUWHGLQWRWKH the change of dielectric properties in the liquid area. From
photosensitive acrylic resins during the stacking and these results, the fabricated resonator is considered to be a
exposing. Finally, the micro cell was put between the promising candidate as the novel device to determine the
diamond photonic crystals, and the terahertz wave resonator dissolved components in the aqueous solution.
was integrated successfully by using acrylic resin flames.
These flames were glued together by using the photo
sensitive resin and the light exposure solidification. Water
solutions were infused through catheters connected on the
top side of the micro resonance cell. The transmission
properties of terahertz waves were analyzed by using the
time domain spectroscopy (Advanced Infrared
Spectroscopy, J-spec 2001 spc/ou). The intensity profiles of
electric field in the resonator were simulated and visualized
at the localized frequency by using the transmission line
modeling method.
Fig. 3 The sintered alumina photonic crystal (a), and the

fabricated terahertz wave resonator (b).
Fig. 2 A schematically illustrated micro stereolithography

system of a computer aided manufacturing.

The photonic crystals composed of the acrylic lattices
with the alumina particles dispersion were formed by the
micro stereolithography. The spatial resolution was Fig. 4 A cross sectional distribution profile in electric
approximately 0.5 %. Figure 3(a) shows the alumina field intensities inside of an photonic crystal resonator.
ceramic lattice with the diamond structure formed through
the powder sintering. Cracks or deformations were not
5. Conclusions
observed in the obtained components. Average linear
A terahertz wave resonator of ceramic photonic crystals
shrinkage was 25 %. The lattice constant of the sintered
with diamond structure was fabricated successfully by using
diamond structure ZDV ȝP Relative density of the
micro stereolithography system. Transmission spectra were
152
measured through the resonator including pure water or Acknowledgements

ethanol. Localized modes of sharp transmission peaks were This study was supported by Priority Assistance for the
observed in photonic band gaps. In a distribution profile of Formation of Worldwide Renowned Centers of Research -
electric field intensity simulated by using a transmission The Global COE Program (Project: Center of Excellence
line modeling, the localized modes were formed by the for Advanced Structural and Functional Materials Design)
multiple reflections in the liquid cells between the from the Ministry of Education, Culture, Sports, Science
diffraction lattices. Moreover, the localized mode peak was and Technology (MEXT), Japan.
shifted clearly from higher to lower frequencies through
replacing the pure water with the ethanol. The fabricated References
resonator is considered to be a promising candidate for
novel devices to detect the compositional variations in [1] E. Yablonovitch: Phys. Rev. Lett. 58 (1987), pp.2059-2062.
aqueous phase environments. [2] S. Kirihara and Y. Miyamoto: Int. J. Appl. Ceram. Tech. 6
(2009), pp.41-44.
[3] M. R. Kutteruf, C. M. Brown, L. K. Iwaki, et al.: Chem. Phys.
Lett., 375 (2003), pp.337-343
153
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156
Nonlinear ultrasound and its applications in quality inspection and

damage assessment in metallic materials†
JIN-YEON Kim*, LAURENCE Jacobs* and JIANMIN Qu**
KEY WORDS: (Nonlinear ultrasound) (Fatigue damage) (Nondestructive evaluation)
1. Introduction longitudinal [2], Rayleigh [3], and Lamb [4,5] waves. Each
Recent experimental studies and new physical models of these has its own advantages and unique applications. In
[1] demonstrate the high potential of nonlinear ultrasonics particular, the nonlinear Lamb waves are certainly the best
to quantitatively characterize fatigue and creep damage in candidate for efficiently performing a long range inspection
metals. On the fundamental side, a physics-based model is of plate and shell structures. Due to the dispersive and
needed to establish the relationship between the measured multi-modal characteristics of the Lamb waves, the
higher order harmonic and the parameters that characterizes measurement of the second harmonic wave is more difficult
fatigue damage. Recent advances in metal fatigue research than in the non-dispersive waves. A theoretical analysis on
have enables predicting, with reasonable accuracy, the the conditions to generate a spatially growing higher
cumulative plastic deformation in a structure component harmonic has been performed [6]. In addition, an advanced
during cyclic loading. Thus, a physics-based relationship signal processing technique has been applied to extract the
between the higher order harmonic and the cumulative fundamental and second-harmonic amplitudes of a
plastic strain would allow us to estimate the remaining measured Lamb wave signal.
fatigue life of a component based on the nondestructive The developed techniques have been applied to
nonlinear ultrasonic measurements. characterize damage in materials subject to static load, low
This paper presents our recent experimental and theoretical and high cycle fatigue for various metallic materials.
developments in the nonlinear ultrasonic material For example, Fig. 1 shows results of measured material
characterization technique. The developed experimental nonlinearity for the nickel-base superalloy (IN-100) during
techniques are applied to track fatigue and other plasticity- a low cycle fatigue using both longitudinal and Rayleigh
induced damage in nickel-base and aluminum alloys to waves. The maximum stress level is 105% of the yield
demonstrate the capability of the techniques. The stress, and the fatigue tests are interrupted to perform the
microplasticity-based model that relates the acoustic nonlinear ultrasonic measurements at different numbers of
nonlinearity and the cumulative plastic strain is introduced fatigue cycles. Figure 1 shows a rapid increase in İŰġĩŶűġ
and results are compared with experimental data. to 30%) during the first 40% of fatigue life, which
demonstrates that these nonlinear ultrasonic measurements
2. Experimental results can be used to quantitatively characterize the damage state
We have developed robust experimental techniques to of this material in the early stages of fatigue life. Similar
track the evolution of fatigue damage in several different trend of large increases in the initial stage is observed in the
alloys including the nickel-base superalloy (IN-100) and Lamb wave measurement results. This implies that the
aluminum alloys (AA6061-T6, AA2024-T3, Al1100-H14), dispersive nature of Lamb waves does not alter their
with the acoustic nonlinearity parameter and demonstrated interaction with fatigue damage and that there is a
its effectiveness and robustness by making repeatable fundamental relationship between fatigue damage and
measurements of the material nonlinearity parameter (ĪġŪůġ acoustic nonlinearity, independent of wave type. Figure 2
multiple specimens subjected to static, high- and low-cycle shows the acoustic nonlinearity (versus the plastic strain)
fatigue load. Varying geometries of the structure measured with Lamb waves for Al-1100-H41 specimens
components to be inspected requires the experiment method subjected to low cycle fatigue. Note that Fig. 2 can be
to adapt to the geometrical constraints. This led to important baseline data for lifetime prediction of a
developments of three different techniques that use component subjected to cyclic fatigue loading.

* Georgia Institute of Technology, Atlanta, GA, USA Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Northwestern University, Evanston, IL,USA Japan
157
Nonlinear ultrasound and its applications in quality inspection and damage assessment in metallic materials
Longitudinal wave measurement (Specimen #1) The effects of the microplastcity enter in the coefficient
Normalized acoustic nonlinearity, E/Eunfat

1.6 Longitudinal wave measurement (Specimen #2)
Rayleigh wave measurement (Specimen #1)
Rayleigh wave measurement (Specimen #2)
tensors CIJKL and DIJKLMN and the acoustic nonlinearity
1.5 Best fit of longitudinal wave measurement results parameter can be calculated solving this equation.
1.4 Prediction of the cumulative plastic strain in each grain of a
1.3 polycrystalline metal requires a finite element simulation of
the microplasticity evolution from various types of
1.2
substructural damage. Figure 3 shows the nonlinearity
1.1
parameter predicted with this microplasticity-based model
1.0 for the nickel-base superalloy (IN-100) under the same
0 10 20 30 40 50 60 70 80 90 100 loading condition as in Fig.1. The comparison between Figs.
Fatigue life (%) 1 and 3 shows a very reasonable agreement and this result
Fig. 1 Normalized acoustic nonlinearity parameter as a proves practical usefulness and capability of the present
function of percentage fatigue life for the low-cycle fatigue combined experimental and theoretical framework.
results, measured using longitudinal and Rayleigh waves.
Fig. 2 Normalized acoustic nonlinearity measured using Lamb

waves versus measured plastic strain,. Fig. 3. Normalized acoustic nonlinearity vs. fatigue life of IN100
during low-cycle fatigue, predicted by the microplasticity based
model.
3. Microplasticity-based model
Cantrell [1] proposed a nonlinear elasticity model in
which the evolution of sub-structural organization of 4. Knowledgments
dislocations is taken into account to predict total acoustic The work was supported in part by NSF CMMI-
nonlinearity of a polycrystalline nickel under cyclic load. 0653883, and AFOSR FA9550-08-1-0241.
As an engineering alternative to Cantrell model, we
References
proposed a microplasticity-based model [7]. Instead of [1] J. H. Cantrell, Proc. R. Soc. Lond. A 460, 757-780, 2004.
relating the acoustic nonlinearity parameter directly to the
dislocation substructure, this model exploits the continuum [2] J.-Y. Kim, L.J. Jacobs, J. Qu, and J.W. Littles, J. Acoust. Soc.
manifestation of these dislocations, namely, plastic Am. 120(3), 1266-1273, 2006.
deformation. The advantage of this approach is that plastic [3] J. Herrmann, J.-Y. Kim, L.J. Jacobs, J. Qu, J.W. Littles and M.
strain is a measurable parameter yet quantitatively Savage J. Appl. Phys. 99(12), 124918, 2006.
characterizes the effect of the dislocations and thus the
[4] C. Bermes, J.-Y. Kim, J. Qu, and L.J. Jacobs, Appl. Phys. Lett.
fatigue damage. The theoretical nonlinearity vs. plastic 90(2), 021901, 2007; C. Pruell, J.-Y. Kim, J. Qu, and L.J.
strain relationship can be used with experimental results Jacobs, ibid 91(23), 231911, 2007.
(nonlinearity vs. fatigue life) such as that in Fig 2 for
predicting the remaining useful life of a critical structure [5]C. Pruell, J.-Y. Kim, J. Qu, and L. Jacobs, Smart Mater. Struct.
component. Under this mission, the nonlinear wave 18, 035003, 2009.
equation in an elastic medium with localized microplastic [6] M. Mueller, J.-Y. Kim, J. Qu, and L. Jacobs, in press, J.
deformation is derived Acoust. Soc. Am. 127, 2010.
[7] J.-Y. Kim, J. Qu, L.J. Jacobs, J.W. Littles and M. Savage, J.
w ª1 § § 1 · wuM · wuK º U w 2u I Nondestruct. Eval. 25(2), pp.29-37, 2006.
« ¨ CIJKL J V JLG IK ¨ CJLMN G IK DIJKLMN ¸
i
¸ »
wX J ¬ J © © 2 ¹ wX N ¹ wX L ¼ J wt 2
158
Measurement of fatigue damage parameter by sacrificial test piece

and thermography†
SAKINO Yoshihiro *, SAKAGAMI Takahide ** and YOU-CHUL Kim*
KEY WORDS: (Fatigue damage parameter) (Thermography) (Sacrificial test piece) (Bridge maintenance)
(Crack growth)(Thin steel plate)
1. Introduction
Unit: mm
͆The sacrificial test piece” is used as a specimen Jig-plate
Sacrificial Test Piece
attached to the member of a main structure in order to 㻝㻜㻜㻚㻡
evaluate the damage before the appearance of a crack in a
member of that structure. The sacrificial test piece is 㻝㻞㻝㻜
㻠㻜㻠㻜
designed so that it is damaged earlier than the main 㻡㻜㻝㻟㻡㻣㻜㻝㻟㻡㻡㻜
members under the same loads because of crack and stress
magnification. The damage to the bridge members can be 㻞㻡
estimated by the observation of the sacrificial test piece. If
the fatigue damage parameter can be made clear by the 㻝㻜㻜㻞㻜
behavior of the sacrificial test piece, the maintenance
management of the structure can be determined.
Thin steel plates, which have initial cracks at the 㻠㻠㻜
center, are used as the sacrificial test pieces in this study. Fig. 1 Sacrificial test pieces with jig-plate
When strains are applied to the main member, these are
transmitted from the main member to the thin steel plate
and the crack in the thin steel plate will grow as a result.
Therefore, the monitoring of fatigue damage parameters on
the bridge can be carried out by the observation of the
crack growth in the thin steel plate. If the thin steel plate
can be used as the sacrificial test piece, it seems that fatigue
damage on a bridge can be monitored widely. Because the
thin steel plate is cheap, everyone can obtain it easily [1].
In this paper, a measuring method for the crack length
of the sacrificial test piece from a long distance by self-
reference lock-in thermography is proposed. Applicable
stress ranges and frequency of measurement by the
proposed method are clarified.
Fig. 2 Measurement of crack length in sacrificial test
2. Remote Measurement of Crack Length piece by self-reference lock-in thermography.
by Self-Reference Lock-in Thermography
The sacrificial test piece was attached to four steel jig-
plates by bolts. The shape and the dimensions of the jig- be carried out in a short period. The specimen is attached
plates are shown in Fig. 1. The thickness of the sacrificial on the lower flange of bridge members with high strength
test piece is 0.5 mm, and the thickness of one side edge of vices at the edge of the jig-plates.
the jig-plate is 12mm and other part of the jig-plate is If the crack length of the sacrificial test piece can be
10mm. Using the jig-plates, the strain between the measured from a long distance, the damage in a member of
connected points is concentrated at the sacrificial test piece a bridge can be evaluated more easily and cheaply. We
by the difference in stiffness between the thin plate and the propose a measuring method of the crack length from a
jig-plate. Strain in the sacrificial test piece is concentrated long distance by thermoelastic stress analysis.
more than about 3 times that of the flange by theoretical A self-reference lock-in infrared thermography
calculation. This strain concentration makes the crack technique is newly proposed, in which a reference signal is
growth faster, and the measurement in bridge members can constructed by using the same sequential data on
** Graduate School, Kobe University, Kobe, Japan Japan
159
Measurement of fatigue damage parameter by sacrificial test piece and thermography
Crack Tip
Crack Ti
Fig. 3 Crack tip in sacrificial test piece searched Fig. 4 Crack tip in sacrificial test piece searched
by self-reference lock-in thermography by self-reference lock-in thermography
ǻV=120MPa, 10Hz, Crack length: 20.5mm) ǻV=120MPa, 10Hz, Crack length: 38.0mm)
thermoelastic temperature change. Temperature change in a frequency during measurement were 120MPa-10Hz and
region of interest, such as crack tip, is correlated with that 60MPa-3Hz.
in a remote area, where uniform stress is applied, for Figure 3 and 4 show contours drawings of the relative
reference signal construction. The temperature changes thermoelastic temperature change distribution obtain by the
obtained from the region of interest and remote area are in- self-reference lock-in thermography in the measurement of
phase and have similar waveforms but big differences are 20.5 mm and 38.0 mm. The applicable crack length of the
found in their amplitudes. Consequently if a reference sacrificial test piece is from 20 mm to 40 mm [1]. So Fig. 3
signal could be constructed from the signal obtained from a and 4 show the results of just about the lower and upper
remote area, it is possible to perform correlation processing limits of applicable range. In spite of the crack length, the
without an external reference signal. The lock-in algorithm location of the crack tip can be estimated as the largest
based on the least squares method is employed for signal point of the thermoelastic temperature change.
processing under random loading. It enables us to measure Figure 5 shows the comparison between the crack
the distribution of relative intensity of applied stress under lengths measured by crack gauge and those estimated by
random loading without using any external loading signal the self-reference lock-in thermography. Good agreement
[2]. can be found between the crack length measured by crack
To examine the applicability of self-reference lock-in
Crack Length mesured by Thermography (mm)
thermography to the measurement of the crack length of the 40

sacrificial test piece from long distances, fatigue tests of the 120MPa, 10Hz
sacrificial test pieces were performed and crack length was
60MPa, 3Hz
measured by the proposed method. As shown in Fig. 2, 0.5 35
mm thick steel plate as the sacrificial test piece without jig-
plates was fixed to the 9 mm thickness of a main member.
Backing plates are put between the main member and the 30
thin steel plates and then the thin steel plates and backing
plates are fixed by the high strength vices. Material of the
main member and backing plates are mild steel. In order to 25
propagate the fatigue crack, cyclic load was applied to the
main member using a servo-hydraulic testing machine.
Crack gauges (pitch = 0.5 mm), fixed in the back side 20
of the thin steel plate, were used to measure the length of 20 25 30 35 40
crack. Measurement of the crack length by self-reference
lock-in thermography was performed every 0.5 mm of Crack Length mesured by Crack gauge (mm)
crack growth measured by crack gauge. Distance from the Fig. 5 Comparison between crack lengths
lens to thin steel plate was 2 m. Loading stress range and measured by crack gauge and thermography
160
gauge and those estimated by the self-reference lock-in sacrificial test pieces in the bridge members from long
thermography in all ranges, not only in the case of 120MPa- distance by the self-reference lock-in thermography is
10Hz, but also in the case of 60MPa-3Hz. So it can be said demonstrated.
that the proposed method of self-reference lock-in
thermography can measure the crack length of the Acknowledgments
sacrificial test piece accurately. The authors would like to thank Mr. Nishimura and
Mr. Nakatsuji for their help during the experiments.
3. Conclusions
(1) Even when the frequency is as small as 3Hz, the self- References
reference lock-in thermography can measure the crack [1] Y. Sakino, Y.-C. Kim, and Horikawa, Trans. of JWRI 35(1),
length of the sacrificial test piece accurately in the case 63-70.
[2] T. Sakagami, K. Nishimura and S Kubo, Proc. of SPIE
that the stress range is 60MPa or more.
Vol.5782, 379-387.
(2) The possibility of measurement of crack length in the
161
Role of ambient pressure on splat formation and coating adhesion
strength during thermal spraying process†
KUN Yang*, EBISUNO Yoshinobu *, TANAKA Kazuhiro *, USAMI Takashi *,
FUKUMOTO Masahiro **, YASUI Toshiaki **, and YAMADA Motohiro **
KEY WORDS: (Thermal spraying) (Ambient pressure) (Disk-shaped splat) (Splash splat) (Adhesion strength)
1. Introduction reduction of ambient pressure, the splash fingers always

Thermal spraying is a process that can provide thick connect with the center solidification area (Fig. 1(b)).
coatings over a large area at high deposition rate. As the While the ambient pressure was lowered to 6.7kPa, the
splat is unit cell for the entire coating build–up, it is splat pattern changed from the form with splashing to the
necessary to study in detail the basic process of flattening one without splashing (Fig. 1(c)). The fraction of splash
behavior of the sprayed particles. In this study, the splat increases significantly with increasing the ambient
flattening behavior of the individual thermal sprayed pressure, which agrees with the BET isotherm [1]. This
particle collected under various ambient pressures was indicates that the adsorption/desorption of adsorbed
investigated. The heat transfer of the free-falling droplet gas/condensation plays an important role on the flattening
was conducted to simulate the thermal conduct process behavior of thermal sprayed particles. The microstructure
from molten droplet to substrate. Moreover, properties, in observation on the bottom surfaces of Cu splats were
particular of the adhesion strength of the coatings conducted as shown in Fig. 1(d, e, f). It is clearly
fabricated under the similar ambient pressure as the splats recognized that with the decrease of ambient pressure, the
collection were evaluated. amount of the pores decreased remarkably, while the
solidification structure become more homogeneous.
2. Experimental Procedures Moreover, no substrate melting can be observed from the
Cu powders were thermally sprayed onto mirror cross section view, significant interface exist between splat
polished AISI304 substrate surface by low pressure plasma and substrate at any ambient pressures. However, the gain
spraying (LPPS) at various ambient pressures ranging from size is coarser than that of the splat deposited at low
6.7kPa to 101.3kPa. Splat morphologies in detail were pressure condition, which may be due to the lower thermal
observed using scanning electron microscope (SEM) and conductivity at high pressure condition.
focus ion beam (FIB). ImageJ imaging software was
employed to quantify pore size and distribution on the
bottom surface of the splats. Millimeter-sized molten Cu
droplets were deposited on AISI304 substrate surface by
free falling experiment. The droplet was melted by
radio-frequency heating equipment prior to the falling. The
thermal history of molten droplet was measured at
splat-substrate interface using J-type thermocouple. Thick
coatings were deposited on blasted AISI304 substrate using
controlling ambient pressure. The shear adhesion strength
of the coatings was evaluated by Autography AGS-L.
Moreover, the coating’s cross section microstructure and
elements distribution was evaluated using Energy
Dispersive X-Ray (EDX).
Fig. 1 Splat morphologies of Cu sprayed onto
3. Results and Discussion AISI304 substrate under various ambient pressures
Most splats deposited at the atmospheric pressure The bottom surface analysis was conducted using
performed a typical splash-like shape with a center splat ImageJ imaging software as shown in Fig. 2. Both of the
surrounded by a ring of fragments (Fig. 1(a)). With the area fraction and average size of the nano-pores increase
* Graduate School, Toyohashi University of Technology, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan Japan
** Toyohashi University of Technology, Toyohashi, Japan
162
Role of ambient pressure on splat formation and coating adhesion strength during thermal spraying process
gradually with the increase of ambient pressure. It is

known that water and other substances can be adsorbed on
clean solid surface, the most common condensate is water
from moisture. There has a lack of a true chemical bond
between adsorbed gas molecular and substrate surface,
desorption tends to occur when the ambient pressure
decreases. Because there has no chemical modification and
Fig. 4 Cross-section morphology and adhesion

strength of Cu coating fabricated on AISI304
substrate under various ambient pressures
adhesion strength changed transitionally along with the
ambient pressure reduction, which corresponded well with
the splat shape change with the ambient pressure. Hence,
Fig. 2 Dependence of nano-pores’ average size
the splat shape likely has a strong influence on the coating
and area fraction on ambient pressure
adhesion. The coating and substrate elements distribution
surface topography change occurs when the ambient was evaluated by EDX. Cu couldn’t be found on the
pressure change, desorption is the only possible physical substrate side, also, no substrate composition elements (for
change taking place on the surface. It must be the reason of example, Fe, Cr, Ni) could be observed on the coating
pore characteristic change transitionally along with the fabricated under various ambient pressures, which
reduction of ambient pressure [2]. indicates that there has no significant diffusion and
To clarify the effect of ambient pressure on heat transfer chemical reaction occur at the interface between the
at interface between molten droplet and substrate surface, coating and substrate. Mechanical adhesion is the only
temperature history of free-falling droplet was measured possible adhesion mechanism during the thermal spraying
under the designated pressure conditions. The results of process. In other words, not the adhesion mechanisms
temperature histories and corresponding cooling rates in change, but the individual splat formation behavior under
the splats kept at various ambient pressures are shown in the designated conditions likely affects the adhesion
Fig. 3. All measurements were conducted on non-heated strength.
substrate, and ambient pressure was 101.3kPa, 40.0kPa and
6.7kPa, respectively. According to Fig. 3(b), it is found that 4. Conclusions
cooling rate in the splat increases with decrease of ambient (1) The splat shape from a splash splat to a disk one was
pressure, increasing from 4.4×103 K/s on the substrate recognized by reducing the ambient pressure. This
under atmospheric pressure to 1.1×104 K/s on the substrate transition is likely attributed to the
located at an ambient pressure of 6.7kPa [3]. adsorption/desorption of the adsorbed
gas/condensation.
(2) The conduct condition at splat/substrate interface was
improved by pressure reduction. Therefore, the heat
transfer should be enhanced, followed by the improved
cooling rate, which results in the disk-shaped splat
formation.
(3) The adhesion strength of the coating and splat shape
obtained under various ambient pressures correspond
quite well with each other. The results suggest that the
Fig. 3 Droplet temperature history and cooling coating adhesion change was attributed remarkably to
rate by controlling ambient pressure the individual splat formation behavior.
Figure 4 shows the cross section morphology and shear References

[1] S. Brunauer, P. H. Emmett and E. Teller: J. Am. Chem.
adhesion strength of Cu coating fabricated on blasted
Soc., 60(1938), pp.309–319
substrate under various pressures. Similar typical
multi-layer structures were observed of the coating [2] K. Yang, K. Tomita, M. Fukumoto, M. Yamada and T. Yasui:
fabricated at different ambient pressures, no remarkable J. of Therm. Spray Technol., 18(2009), pp.510-518
differences of contact condition between coating and [3] M. Fukumoto, K. Yang, K. Tanaka, T. Usami, T. Yasui, and M.
substrate could be observed. It is noted that the shear Yamada: J. of Therm. Spray Technol., (in press)
163
Repair heavy-duty generator rotor shaft by electro spark deposition

process†
WANG Ruijun*, WANG Weiping*, Lü Yufen*, TIAN Hehong*
KEY WORDS: (Electro spark deposition) (Generator rotor shaft) (Repair)
1. Introduction
As the basic industry of national economy, power Table 1 ESD Parameters
industry has been the focus of national development. Recent
Frequency
Discharge
Capacity
Weight
two decades, it is the fastest development period and gains
Output
Model
Input
Size
the most achievements [1] [2].
If the generator rotor shaft wear or damage occurs, rotor
running at high speed is hindered and generator output
power decreased, which may result in the units failure [3]. DZ- AC 1.4 40u 40 420 50-
This paper discusses that the repair of worn parts for 1400 220 KVA 60u Kg F 1200
generator rotor shaft at site using DZ 1400 Electro Spark 50 80 HZ
Deposit (ESD) system manufactured by Surface HZ
Engineering Technology Institute of CAAMS with
satisfactory results and successful experiences.
with ground line of ESD, and repair welding on the sample
surface with a thickness of 1mm. After overlaying by ESD,
2. Electric Spark Deposition (ESD)
obtain cross-section of the coating by line cutting method
Electric Spark Deposition Principle
and prepare metallographic sample.
Electric Spark Deposition (ESD) process is to instantly
release in high frequency high-energy from the power Table 2 Chemical composition of the electrodes for sample
supply between electrode and substrate, then produce air
Ni Cr Fe Mo Mn Si Other
ionic passage, inducing micro-zone of high temperature,
high-pressure physic-chemical metallurgical process 70 14 4.5 --- 7.8 0.5 Bar
between high alloy electrode and substrate surface.
Test Analysis
ESD process combines the characteristics of welding,
spraying and other processes with low heat input, good Figure 1 is the cross-section micrograph (u3000) of the
coating. It’s known that:
metallurgical bonding between weld pass and substrate.
1) There isn’t welding defect such as pore, oxide slag
inclusion, crack, etc. in overlay.
ESD Equipment 2) Crystallite of overlay and substrate transition layer is fine,
Power output of ESD (DZ-1400) is 1400W㸪using argon no growing tendency.
for welding, self-consumable anode moves at 4700rps at the 3) The coating structure is very fine small columnar crystal,
worn place of the work piece, induce HF spark discharge, which shows good corrosion and abrasion resistance.
and form dense and homogeneous overlay coating with a Figure 2 is the energy spectrum analysis of Ni, Cr
thickness up to 2mm or more. Substrate temperature elements in the coating. The thickness of heat-affected zone
remains around 60Υduring repair, and the substrate does of ESD is 10ȣm. It demonstrates that a good metallurgical
not distort and undercut. Table 1 is ESD parameters. bonding can be obtained by ESD, also shows that deposit
heat-affected zone is small and welding residual stress can
3. Experiment and Analyses be ignored. The average hardness of coating and heat-
Sample preparation affected zone is very close to the matrix hardness HV220.
According to the common material of rotor shaft,
35CrMoA is selected as the sample substrate material with Result
the size of 25mmu10mmu50mm.Nickel-based high alloy The result of experiments show the metallurgical bond
rod is chosen as electrode material with a specification of between coating and substrate has not welding defect by
I3.2mmu6.0mm, the chemical composition is listed in depositing inconel alloy on substrate 35CrMoA using ESD
Table 2. After pretreatment, connect tightly substrate process. After welding, heat-affected zone is very narrow
* Chinese Academy of Agricultural Mechanization Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Science(CAAMS), China Japan
164
Repair heavy-duty generator rotor shaft by electro spark deposition process
(thickness of coating reaches 1mm, but heat-affected zone Visual check overlay after each layer DERXW ȝP
is only 0.01mm), hardness of coating conform to that of thickness) to see if has welding defects such as oxide㸪if
substrate. The above results meet the requirement of rotor has, use needle file to remove and use brass wire brush to
shaft repair in power plant. clean, then overlay the next layer. When overlay is close to
the desired size, use toolmaker's straight edge to align㸪the
overlay should be more than the final repaired size 50-
ȝP$IWHUWKHFRPSOHWLRQRIRYHUOD\LIWKHUHLVZHOGVSRW
or side missed during inspection can make up welding.
Post-treatment
After the completion of ESD, the bench worker will work
on the dimensional recovery and finishing polish of the
repaired surface of the shaft. The repair standard refers to
the technical specifications of shafts. Fig. 3 is seal section
shaft of generator rotor after repair and finishing,
respectively.
Fig. 1 Cross-section micrograph of the coating㸦u3000㸧
Fig. 2 Heat-affected zone testing

4. Field Repair Fig. 3 Seal section shaft after repairing and finishing,
Pretreatment (a) repairing; (b) finishing.
First, the worn section of shaft is filed. Then oxide and
fatigue layer of the surface to repair is cleaned using
5. Conclusion
sandpaper or flat file. After the iron cutting is cleaned
(1) Between ESD overlay and substrate is metallurgical
using brass wire brush or compressed air, the oil stains of
bond, heat-affected zone is very narrow, and residual
shaft surface are cleaned using acetone solution. stress can be ignored.
(2) Rotor seal section shaft of power plants can be repaired
ESD Equipment Preparation by ESD on the site, and the process is simple. There is a
The removal & mounting and transport of generator rotor little post processing after patching to reduce downtime.
are difficult for its large size and weight of tens of tons, and (3) We have collaborated with several power plants by ESD
repair has to be on the site. DZ-1400 ESD system is repaired seal section shaft of generator rotor with
installed near the location of shaft to repair. AC220V power success and gained great economic and social benefits.
supply and industrial pure argon gas source are properly
connected with quick connector. The argon gas flow rate is References
set at 7L/ min, the electrode should be controlled out of 2- [1] Electric Power Reliability Management CenterˈManual of
3mm to ensure protective effect of argon gas during National Large Units [M]ˈ1998, 4
welding. [2] Prospect of Power Welding Technology [C] ˈ The 60th
Anniversary Academic Report for council of Chinese
Society of Electrical Engineering.
Overlay deposition
[3] Williams A D, Humphries J L. Proceeding of the 15th
Refer to the processes provided by the equipment manual, International Thermal Spray Conference (1998).
welding at the worn part of generator rotor shaft to obtain
silver homogeneous coating, which is the desired effect.
165
Visualization of nugget formation in resistance spot welding of

multi-stackup sheets†
YANSONG Zhang*, JIE Shen**, PC Wang***
KEY WORDS: (Resistance spot welding) (Nugget formation) (Numerical modeling) (Sheet thickness)
1. Introduction Resistance spot welding of multi-stackup steel sheets

With the demand of lightweight vehicle structures, was prepared using a DC current. The welding schedules
resistance spot welding of multi-stackup steel sheets is employed are given in Table 1. The welding time contains
increasingly applied in some complex structures such as three current pulses with 140ms and two cooling pulses
front longitudinal rails, A, B, and C pillars, and the with 20ms.
bulkhead to inner wing. However, due to the difference in The detailed governing equations, boundary conditions
mechanical and physical properties for different sheet grade, and numerical method are given in our previous paper [2].
the contacts of the workpieces and resultant weld current
flow are complex in welding process. As a result of this, Table 1 Welding parameters for stack-up steel sheets
the weld nugget sizes at the faying interfaces become an
issue. Therefore, it is essential to obtain an understanding of Welding parameters Value
the welding process [1]. Electrode force (kN) 5.5
Welding current (kA) 9.5
In this study, a combined thermal-mechanical/thermal-
Squeezing time (ms) 200
electrical incremental model has been developed to Welding time (ms) 460
reasonably predict the nugget formation in resistance spot Hold time (ms) 100
welding process. These calculations would provide
guidance in the selection of welding variables for resistance 3. Results and Discussion
spot welding of multi-stackup assemblies. Before applying the electrical current, an electrode
force is applied to bring the workpieces into intimate
2. Numerical Modeling contact. The electrode-to-sheet and sheet-to-sheet
Figure 1 shows an example of multi-stackup steel deformation influences the weld current density. After
sheets with various sheet gages and material properties. applying the welding current, the temperature of the sheets
Galvanized coated low carbon steel (SAE1004) and high would rise by the generation of the joule heat. Figures 2(a),
strength steel (DP600) was used in this study. A weld 2(b) and 2(c) show the temperature distributions for the
nugget will develop first at the sheet-to-sheet interface, and welding times of 240ms, 360ms and 460ms under an
then in an increasing volume of material about the sheet-to- electrode force of 5.5kN and a welding current of 9.5 kA,
sheet interface. At the completion of weld cycle, the current respectively. Firstly, high temperature has built up at two
is shut off and the hold cycle begins. The water-cooled faying interfaces between the multi-sheets. As the welding
copper electrodes extract a significant quantity of heat from time is increased to240ms, shown in Fig. 2(a), the
the weld area. Because the electrodes are in contact with maximum temperature switched from top-to-middle sheet
sheets, the weld region is effectively quenched. Finally, interface to middle-to-bottom sheet interface due to the
the electrodes are retracted and a completed weld is switch of the high current density and diameter B begins. At
developed. the welding time of 360ms shown in Fig. 2(b), a weld
nugget initiated at the faying interface A. As the welding
time is increased to 460ms, the weld nugget at the two
interfaces grows bigger.
Since the sheet thickness has a significant effect on the
sheet-to-sheet pressure, it would be useful to know how the
sheet thickness affects the nugget size for a fixed electrod
force. To study the effect of sheet thickness combination on
the weld size of multiple stacks of steel sheets, the thickness
of the bottom sheet (DP600) was varied from 0.6 mm to 2.4
Fig. 1 Weld nugget configuration and dimensions for resistance
mm, while the gages of the top and middle sheets
spot welding of multi-stackup steel sheets. (SAE1004) are fixed at 0.6 and 1.8 mm, respectively. Weld
† Received on 30 September 2010 *** China Science Lab, General Motors Research &
* State Key Lab of Mechanical System and Vibration, Development Center, Shanghai, China
Shanghai Jiao Tong University, Shanghai, China Transactions of JWRI is published by Joining and Welding
** Shanghai Key Lab of Digital Autobody Engineering, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Shanghai Jiao Tong University, Shanghai, China Japan
166
Visualization of nugget formation in resistance spot welding of multi-stackup sheets
nugget sizes were modeled and the results are shown in Fig.
3. The diameter B at the faying interface between top and
middle sheet is always greater than the minimum acceptable
weld size, 5 mm. However, there is a significant decrease in
the diameter A at the faying interface between middle and
bottom sheet. It is shown that, when the thickness of the
bottom sheet is 2.4 mm, the weld size at the faying interface
A is less than the minimum required weld size (i.e.4 mm)
[3].
(a) 240ms
(a) Diameter A
(b) 360ms
(b) Diameter B
Fig. 3 Effect of the bottom sheet gage on nugget diameter (a)
Diameter A, and (b) Diameter B.
4. Conclusions
follows:
(1) A finite element model has been developed to predict the weld
(c) 460ms
nugget size for RSW of multiple stacks of steel sheets.
Fig. 2 Temperature field during the welding process for0.6mm (2) The weld nugget on the faying interface of DP600 forms
SAE1004 +1.8mm SAE1004 +1.2mm DP600 under a welding earlier than that on the other interface of SAE1004 in RSW. It
current of 9.5kA. is due to the fact that the greater bulk and contact resistivity of
DP600 would lead to a quicker heat development in the weld
cycle than SAE1004.
167
Acknowledgement References
This research was supported by the General Motors [1] Harlin N., Jones T.B., Parker J.D.:J. of Materials Processing
Collaborative Research Laboratory at Shanghai Jiao Tong Technology (2003), pp. 448–453.
University, the Research Fund of State Key Lab of MSV, [2] Jie Shen, Yansong Zhang, Xinmin Lai and P.C. Wang,
Modeling of Resistance Spot Welding of Multiple Stacks of
China (Grant No. MSV-2010-04) and Project 50905111
Steel Sheets’, Materials & Design, (In Press)
supported by National Natural Science Foundation of China. [3] ANSI/AWS/SAE/D8.9-97. Recommended practices for test
methods for evaluating the resistance spot welding behavior of
automotive sheet steel materials. AWS, 1997
168
Development of wettability evaluation equipment for solder paste

†
using laser displacement method
KOYAMA Shinji *, OYA Issei *, ISAKA Toshihiro *, SHOHJI Ikuo *,

NISHIMURO Masashi **, HIRAMOTO Kiyoshi ** and MIYAMOTO Hironaga ***
KEY WORDS: (solder paste) (wettability) (laser displacement meter) (reflow soldering) (lead-free solder)
(surface mount technology)
1. Introduction (2) The equipment has a system which can take a picture of
Built-in electronic parts are made minute as mobile continuous animation of joints with CCD camera in the
products are miniaturized. Then, surface mount technology reflow process.
by reflow soldering is growing rapidly [1, 2]. Moreover, it (3) The equipment has a system which controls the
is known that the wettability to the electrode of the solder temperature with the halogen heater and a system which
paste is affected worsened by the world trend of Pb free in controls the cooling speed by introducing atmosphere
the solder paste [3, 4]. Therefore, the development of the gas into the chamber.
evaluation technique of the wettability of the solder paste is
a pressing need. However, the evaluation technique of the 3. Results and discussion
wettability of the solder paste has only a wetting balance Figure 2 shows the heat pattern in reflow process used.
method in which the size effect of the electronic parts can The shape of the metal mask and copper land is as shown in
hardly be considered [5-7]. So, the development of Fig. 3. The 1608 chip capacitor was used for electronic
equipment which can evaluate the wettability of the solder parts. The results of measuring the descent behavior of
paste to actual electronic parts at the speed of parts in the electronic parts are shown in Figs. 4-7.
reflow process was attempted with a laser displacement In the case of Sn-3.0Ag-0.5Cu (mass%) solder paste, it
meter in this research. has been understood that electronic parts descend with the
melt of the solder powder as shown in Figs. 4 and 5. In
2. Feature of developed equipment addition, the descent of electronic parts has progressed
As shown in Fig. 1, the equipment developed by this when the molten solder was wetting up to the electrode on
research is chiefly composed of the following three parts. sides of electronic parts. Even if Sn-3.5Ag-8In-0.5Bi
(1) The equipment has the temperature measurement system (mass%) solder paste was used, a similar tendency was
with a thermo-couple and the height measurement observed as shown in Figs. 6 and 7. However, it was
system of electronic parts with a laser displacement understood that Sn-3.0Ag-0.5Cu solder was longer
meter. compared with Sn-3.5Ag-8In-0.5Bi solder for the time to
get to the bottom after electronic parts descended rapidly. It
is thought that this factor depends on the amount of solder
which is wetting up to the electrode on sides of electronic
parts (see Figs. 5 and 7).
Fig. 1 Outline chart of developed equipment. Fig. 2 Diagram of heat pattern in reflow process.
* Graduate School, Gunma University, Kiryu, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Sanyo Seiko Manufacturing Co., Ltd., Hachioji, Japan Japan
*** Yamanashi Pref. Industrial Technol. Center, Kofu, Japan
169
Development of wettability evaluation equipment for solder paste using laser displacement method
Fig. 3 Shape of metal mask (a) and Cu pad (b) used in

this research.
Fig. 6 Relation between descent behavior and reflow

temperature of electronic parts (Sn-3.5Ag-8In-0.5Bi).

temperature of electronic parts (Sn-3.0Ag-0.5Cu).
Fig. 7 CCD camera images which observed joint in

reflow process. The number in figure correspond to those
in Fig. 6.
Table 1 Effect of solder paste composition on descent

behavior.
As a result of the analysis, the descent speed of parts in

Sn-3.5Ag-8In-0.5Bi solder paste was twice compared with
Fig. 5 CCD camera images which observed joint in
reflow process. The numbers in figure correspond to that of Sn-3.0Ag-0.5Cu solder paste although negligible
those in Fig. 4. change was observed in the amount of the descent of parts.
The wettability of the solder paste strongly depends on the
As described above, not only the observation of the electrode type and the solder paste type. Although the
joints in the reflow process but also the analysis of the evaluation of the wettability is difficult, the developed
relation between the processing time and the descent method which measures the descent behavior of the part
amount of electronic parts (descent speed) is possible with could suggest a new evaluation technique for the wettability
developed systems. of the solder paste.
An analytical result of the descent speed and the amount
of the descent is shown in Table 1. Ten examinations were 3. Conclusions
conducted for each solder paste, and the average wetting
curve was obtained. From the average wetting curve, the
follows.
descent speed and the descent amount were investigated.
170
(1) The wettability of the solder paste is appreciated by [3] E. E. M. Noor, N. M. Sharif, C. K. Yew, T. Ariga, A B. Ismail
measurement of the descent speed of electronic parts in and Z. Hussain: J. Alloys and Compounds, 507 (2010),
the reflow process with a laser displacement meter. pp.290-296.
(2) The developed equipment can evaluate the difference of [4] D. Rocak, S. Macek, J. Sitek, M. Hrovat, K. Bukat and Z.
Drozd: Microelectronics Reliab., 47 (2007), pp.986-995.
the wettability of the solder paste which depends on the
[5] J. Kloeser, P. Coskina, R. Aschenbrenner and H. Reichl:
solder paste type. Microelectronics Reliab., 42 (2002), pp.391-398.
[6] K. M. Martorano, M.A. Martorano and S.D. Brandi: J. Mater.
Proces. Technol., 209 (2009), pp.3089-3095.
References
[7] E. Attar and C. Korner: J. Colloid and Inter. Sci., 335 (2009),
[1] B. Noh, J. Choi, J. Yoon and S. Jung: J. Alloys and
pp.84-93.
Compounds, 499 (2010), pp.154-159.
[2] T. Chang, Y. Hsu, M. Hon and M. Wang: J. Alloys and
Compounds, 360 (2003), pp.217-224.
171
Examination of improvement effect of surface modification of Cu

with organic acid on solder paste wettability using a laser
displacement meter†
KOYAMA Shinji *, AOKI Yukinari * and SHOHJI Ikuo *
KEY WORDS: (solder paste) (wettability) (laser displacement meter) (reflow soldering) (lead-free solder)
(modification) (organic acid)
1. Introduction
In surface mount technology, the deterioration of the
wettability to the Cu pad and the electrode of the part of the
solder paste according to the abolition of the use of Pb have
been pointed out [1, 2]. The deterioration of the wettability
influences the reliability of products with solder joints.
Therefore, the improvement of the wettability is a very
important technology in the electronic industry. In this
research, the verification of the effect to the wettability was
attempted by using the surface modification method with an
organic acid from which the effect of decreasing the solid-
state bonding temperature of Sn and Cu was confirmed [3]. Fig. 2 Diagram of heat pattern in reflow process.
The organic acids used in the experiment are formic acid
process used the heat pattern shown in Fig. 2. The
and citric acid. For the comparison, the surface which had
wettability was evaluated by measuring a descent speed of
been processed by the procedure of making to cleanness on
the fragment in reflow process with a laser displacement
the Cu surface used for wettability evaluation method of the
meter.
solder paste (JIS Z3284) was examined.

2. Experimental details
The result of measuring descent behavior and a
The sample used for the evaluation cut a fragment (3x3 temperature of the fragment in the reflow process is shown
mm2) and a substrate (5x5mm2) from the copper sheet of 1 in Figs. 3-6. A black-solid line in the figure is an average
mm in thickness. The surface to be soldered was ground on displacement curve of five examinations. As a result of the
emery paper (#800). The surface modification processing measurement, it has been understood that the fragment
was performed by boiling the Cu surface in organic acid begins descending when the temperature of solder paste
(formic acid or citric acid). The Sn-3.0Ag-0.5Cu (mass%) reaches the melting point, and the descent speed has
solder paste was printed on the substrate by using the metal approached zero with the passage of the processing time.
mask (120 Pm in thickness) shown in Fig. 1. The reflow This descent behavior showed a similar tendency regardless
of the type of surface modification.
However, in the case of the fragment modified by the
formic acid, it has been understood that the fragment
descent speed quickens (refer to Figs. 3 and 5). When citric
acid was used for the modification process, a similar effect
was observed. Therefore, it was suggested that the
wettability of the solder paste was improved by giving the
modification process on the Cu surface with an organic acid.
To clarify the improvement mechanism for the
wettability of the solder paste, the Cu surface modified by
formic acid was analyzed by X-ray diffraction analysis. As
a result, as shown in Fig. 7, Cu(II) formate was formed on
Fig. 1 Shape of metal mask used in this research. the surface layer when the modification process was applied.
* Graduate School, Gunma University, Kiryu, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
172
Examination of improvement effect of surface modification of Cu with organic acid on solder paste
wettability using a laser displacement meter

temperature (as grinding).
Fig. 6 CCD camera images of joints in the reflow
process. The numbers in figure correspond those in Fig.
5.
Fig. 7 X-ray diffraction patterns of surface of copper

modified by formic acid.
In addition, it is known that Cu(II) formate undergoes

an exothermic decomposition reaction at about 413 K, as
Fig. 4 CCD camera images of joints in the reflow shown by following reaction formula, and metallic copper
process. The numbers in the figure correspond to those in is generated [5]:
Fig. 3.
Cu(HCOO) 2 ĺ&X+ 2 + 2CO 2 (4)
Therefore, it is thought that the wettability of the solder

paste has been improved by surface modification process
because Cu(II) formate formed on the Cu surface by
modification process and metallic copper was exposed by
thermal decomposition of Cu(II) formate in the reflow
process. Moreover, it is thought that the wettability of the
solder paste is improved in the case of the citric acid by a
similar improvement mechanism. The result of obtained in
this research is collectively shown in Table 1.
Fig. 5 Relation between descent behavior and reflow Table 1 Effect of surface modification on descent
temperature (modificated by formic acid). behavior.
The generation process of Cu(II) formate is shown in

following reaction formulae [4]:
Cu + 2HCOOH ĺ Cu(HCOO) 2 + H 2 Ĺ (1)

Cu2+&22+ĺCu(HCOO) 2 + H 2 2Ĺ (2)
CuO 2 +&22+ĺCu(HCOO) 2 + H 2 Ĺ2 2 Ĺ (3)
173
The conclusions of this study are summarized as [1] D. Rocak, S. Macek, J. Sitek, M. Hrovat, K. Bukat and Z.
follows. Drozd: Microelectronics Reliab., 47 (2007), pp.986-995.
(1) The difference of the wettability of the solder paste [2] J. Kloeser, P. Coskina, R. Aschenbrenner and H. Reichl:
Microelectronics Reliab., 42 (2002), pp.391-398.
which depends on the surface modification of Cu is
[3] S. Koyama and I. Oya: J. Japan Inst. Metals, 73
revealed by the measurement of the descent speed of a
(2009), pp.809-815.
Cu fragment with a laser displacement meter. [4] S. Poulston, R. P. Holroyd, M. Bowker, S. F. Parker and P. C.
(2) The wettability of the solder paste to the Cu surface is H. Mitchell: Surface Science, 402-404 (1998), pp.599-603.
rapidly improved by a surface modification process [5] M. A. Mohamed, A. K. Galwey and S. A. Halawy:
which uses an organic acid. Thermochimica Acta, 411 (2004), pp.13-20.
174
Effect of welding direction on weld bead formation in high power

†
fiber laser and MAG arc hybrid welding
MURAKAMI Takahiro*, SHIN Min-Hyo*, NAKATA Kazuhiro**
KEY WORDS: (High power fiber laser) (MAG arc) (Hybrid welding) (T-joint fillet weld) (Welding direction)
1. Introduction Table 1 Hybrid welding conditions

For many structural materials, it is required to establish
Laser Defocus Laser Arc Wire Arc torch
high–speed, highly-efficient, and high-quality welding
power distance angle current extension angle
methods. As one of them, attention is being paid to hybrid
welding method which combines laser welding and arc 9kW 㼼0mm 7㼻 200A 15mm 45㼻
welding [1]. In this research, a hybrid welding method
which has a high power fiber laser and a pulsed MAG arc Distance/
Vertical
Angle/
Arc Welding Shield
has been applied to T-joint fillet welding of SS400 steel laser and
offset speed offset
laser and
gas
plate. arc arc
The effect of welding direction, which means laser- 1.0~2.0 CO220%
2mm 1.5mm 1mm 35㼻
m/min +Ar80%
leading or arc-leading, on the weld bead formation has been
revealed by parametric study of hybrid welding conditions Table 1 shows hybrid welding conditions used. Fiber
and direct observation of weld pool behavior by using an diameter was 0.3mm and focal point of the laser beam was
infrared high- speed video camera. fixed on the plate surface. Distance between laser and arc
was fixed to 2mm [2].
(a) Vertical plate Horizontal T-fillet welding of SS400 steel plate with the
Arc dimension of 150mm x 50mm x 12mm in thickness was
cond ucted in T-fillet joint by using 10kW class high
Laser 45㼻 power fiber laser and pulsed MAG arc as shown in Fig. 1
(a) and (b), which shows the schematic illustration of the
setup of a hybrid welding. During welding, the behavior of
Laser angle molten metal flow in the weld pool was observed by using
Vertical offset an infrared high-speed video camera with 2000 frames/s.
After the welding, the welded specimens were cut, polished
1.5mm and etched to reveal the microstructure and weld defect.
Horizontal plate
3. Results and Discussions
(b) In hybrid welding, welding direction which means laser-
Arc leading or arc-leading is one of the important and special
Laser
parameters for hybrid welding. Figure 2 shows the typical
bead appearance and cross-section of 1 pass-1 side fully
Arc-leading 35㼻 Laser-leading
penetrated T-fillet weld beads in each welding direction at
the same welding condition. Comparing two weld beads
large differences were easily observed. In laser-leading, a
smooth weld bead was obtained, while a humping and
Vertical plate 2mm undercut bead with pit and void was observed in the arc-
Horizontal plate leading, which was caused by different types of molten
metal flow. In order to reveal this, the behavior of molten
Fig. 1 Schematics illustration of the setup of a hybrid metal flow in the weld pool was observed. Figures 3 and 4
welding show typical frames of weld pool surface during hybrid
(a) Horizontal view , (b) Vertical view welding in laser-leading and arc-leading, respectively. In
the laser-leading molten metal flew forward to the front end
175
Effect of welding direction on weld bead formation in high power fiber laser and MAG arc hybrid welding
is well known that a humping or undercut weld bead is easy

to form due to elongated shape of weld pool and strong
molten metal flow to rearward in the weld pool, and in
addition the plasma gas flow promotes it [3].
Therefore, in this experiment conducted at the condition
as shown in Fig.1, the welding direction of laser-leading is
obviously better than that of arc-leading.
Laser spot Plasma stream
Plasma stream Laser spot
Fig. 2 Appearance and cross-section of hybrid weld bead of

SS400 at different welding directions
Laser leading Arc leading
Arc torch
Fig. 5 Schematics of molten metal flow in the weld pool
Welding direction
laser-leading and arc-leading conditions
Figure 6 shows the effect of the welding speed of laser-

leading on the weld bead formation. At higher welding
Wire speed than 1.25m/min, solidification cracking was observed
at the middle to lower part of the penetration, and in
Molten pool addition, a lack of fusion at the fusion boundary of
Laser beam horizontal plate was observed at the upper part. At
1.0m/min, however, these weld defects were not observed.
Welding line
Thus, a 1pass-1side fully-penetrated horizontal T-fillet weld
bead can be successfully made by optimizing the hybrid
Fig. 3 Typical frame of weld pool surface during hybrid welding parameters.
welding in laser-leading by high speed camera
Arc torch
Pit Wire
Laser beam
Welding direction
Molten pool
Fig. 4 Typical frame of weld pool surface during hybrid

welding in arc-leading by high speed camera
of the weld pool, and then went rearward along the edge of
the weld pool. On the other hand, molten metal flew
continuously and rapidly rearward to the rear end of the
weld pool in the arc-leading and in addition, opening of a
pit was observed. Figure 5 shows schematics of these
obvious differences in molten metal flow comparing in
laser-leading and arc-leading, which is caused by the strong
plasma gas flow of arc and its flow direction related to the Fig. 6 Appearance and cross-section of hybrid weld bead of
inclination of GMA arc torch. In high speed arc welding, it SS400 with different welding speeds at laser-leading
176
4. Conclusions Acknowledgment
The conclusive remarks are summarized as follows. This study was carried out as a part of research activities
(1) 1 pass-1 side fully-penetrated horizontal T-fillet weld of “Fundamental Studies on Technologies for Steel
bead can be successfully made by optimizing the fiber Materials with Enhanced Strength and Functions” by
laser and pulsed GMA arc hybrid welding parameters. Consortium of JRCM.
(2) Different molten metal flows are observed in laser-
leading and arc-leading, which caused differences in References
appearance and cross-sectional shape of weld bead as [1] M. Kutsuna, Welding Guide Book 6, Development in
well as weld defect formation. Advance Welding Processes, JWS, 2009, I-45 - I-66.
[2] M.H. Shin, K. Nakata, Quarterly Journal of the Japan Welding
(3) Laser-leading in the welding direction is beneficial to
Society, 27, 2009, 80-84(in Japanese).
make a smooth weld bead without weld defect at a [3] Japan Welding Society, Handbook of Welding and Joining,
hybrid welding with horizontal T-fillet joint. Maruzen, 2003, 188-189(in Japanese).
177
Numerical analysis on effects of power source characteristics on arc

†
properties in gas tungsten arc
TSUJIMURA Yoshihiro *, TASHIRO Shinichi * and TANAKA Manabu *
KEY WORDS: (Arc) (Power source characteristic) (Arc length) (Gas tungsten arc) (Numerical analysis)
1. Introduction
Arc properties in Gas Tungsten Arc (GTA) strongly In the numerical models, the tungsten cathode, the arc
depend on welding conditions such as arc current, arc plasma and the water-cooled copper anode are described
length and so on [1-3]. In GTA, the arc current and arc relative to cylindrical coordinates, assuming rotational
voltage are determined by an external characteristic of a symmetry around the arc axis. An arc length varied between
power source and an electrical characteristic of the arc. 2 mm and 7 mm at 10 Hz like Fig. 1. In this model, number
There are two kinds of external characteristics of power of the mesh is constant, however, mesh size changes if arc
sources, namely, Constant Current (CC) and Constant length changes. The arc current is set to be a 150 A for a
Voltage (CV) characteristics. The electrical characteristic CC characteristic. The arc voltage is set to be 11.0 V for a
of the arc depends on the arc length. In this study, CV characteristic. The other approximations, governing
dependences of the arc properties and relationships between equations and boundary conditions are given in detail in our
the current and the voltage on the arc length in GTA previous papers [3-5].
employing power sources with the CC and the CV
characteristics were analyzed. In the experiment and the 4. Results and Discussion
numerical simulation, arc length varies time-dependently. Figure 2 shows dependence of arc voltage on arc length
for the CC characteristic. The experimental result of arc
2. Experimental method voltage is between 11.8 V and 15.0 V and the calculation
In the experiments, the free-burning arcs were generated result is between 8.3 V and 12.7 V. Although the
between a tungsten cathode and a water-cooled copper experimental result of arc voltage is higher than the
anode in argon at atmospheric pressure. A commercial calculation result, both results decrease with decrease of arc
GTA torch was fixed on vibratory equipment, and an arc length. Figure 3 shows dependence of arc current on arc
length varied between 2 mm and 7 mm at 10 Hz. An arc length for the CV characteristic. The experimental result of
current was set to be DC 150 A with a CC characteristic. arc current is between 114 A and 189 V and the calculation
An arc voltage was set to be 13.8 V in order to make an arc result is between 80 A and 351 A. Although there are some
current about 150 A with a CV characteristic. difference between the experimental result and the
calculation result of arc voltage, both results increase with
3. Simulation model decrease of arc length and changed circularly. In the same
arc length, arc current at decreasing pattern is higher than
increasing pattern. This is because the thermal problem that
the temperature of the tungsten cathode changes due to
change of arc current.
Figure 4 shows dependence of arc power on arc length.
In experimental results, arc power is between 1776 W and
2248 W for the CC characteristic and is between 1567 W
and 2615 W for the CV characteristic. In calculation results,
arc power is between 1252 W and 1911 W for the CC
characteristic and is between 881 W and 3869 W for the
CV characteristic. With the same variation of the arc length,
the arc power hardly changes for the CC characteristic,
although the arc power largely changes for the CV
characteristic. Furthermore, the arc power decreases with
decrease of the arc length in case of the CC characteristic
and the arc power increases dramatically with decrease of
Fig. 1 Assumption of time-dependence of arc length at the arc length in case of the CV characteristic.
10Hz
Japan
178
Numerical analysis on effects of power source characteristics on arc properties in gas tungsten arc
ii) Calculation results

Fig. 2 Dependence of arc voltage on arc length for constant
current characteristic. Fig. 4 Dependence of arc power on arc length.
5. Conclusions
(1) Study of dependences of the arc properties and
relationships between the current and the voltage on the
arc length in GTA employing power sources with the
CC and the CV characteristics were experimentally and
numerically analyzed.
(2) It was found that the voltage and power of the arc
decreased with decrease of the arc length in case of the
CC characteristic and the current and the power of the
arc increase dramatically with decrease of the arc length
in case of the CV characteristic.
(3) With variation of the arc length, the arc power hardly
changes for the CC characteristic, although the arc
power largely changes for the CV characteristic.
Fig. 3 Dependence of arc current on arc length for constant References

[1] T. Ouji: Introduction of Welding Processes, First edition
voltage characteristic. (1996), SANPO PUBLICATIONS, INC (in Japanese)
[2] A.B.Murphy, et al: A computational investigation of the
effectiveness of different shielding gas mixtures for arc
welding, J.Phys.D:Appl.Phys.42(2009),115205(14pp)
[3] M. Tanaka, et al: Influence of shielding gas composition on
arc properties in TIG welding, Science and Technology of
Welding & Joining, Volume 13, Number 3, April 2008 , pp.
225-231(7)
[4] M. Tanaka, et al: Predictions of weld pool profiles using
plasma physics, J.Phys.D:Appl.Phys.40(2007),R1-R23 K.
[5] Yamamoto, et al: Metal vapour behaviour in thermal plasma
of gas tungsten arcs during welding, Science and Technology
of Welding & Joining, Volume 13, Number 6, September
2008 , pp. 566-572(7)
i) Experimental results
179
Experimental observation of cleaning action of cathode spots in AC

†
TIG welding of aluminum plates
TASHIRO Shinichi *, SAWATO Hiroshi * and TANAKA Manabu *
KEY WORDS: (AC TIG welding) (Cathode spots) (Aluminum) (Oxide layer)
1. Introduction the aluminum plate was recorded with GX1 at frame rate of
Since it is necessary to remove the the oxide layer on 40,000fps for 1s from the arc ignition. On the other hand,
aluminum for realizing high quality weld joint in arc traces of cathode spots were recorded with HPV-1 at frame
welding of aluminum plates, AC TIG welding is generally rate of 500,000fps for ȝV
employed. In duration of EP (Electrode Positive) in AC
TIG welding, the oxide layer is removed by the cleaning
action of cathode spots. In this study, the cleaning action of
cathode spots on the oxide layer in AC TIG welding of the
aluminum was experimentally observed with a high speed
video camera and the cleaning rates of the oxide layer and
velocities of cathode spots were evaluated.
Fig. 1 shows a schematic illustration of the experimental
setup which consist of a TIG torch, an AC power source
(DAIHEN: DA300P), a water cooled copper electrode, an
aluminum plate as a base metal (A1050, 10mm thickness),
high speed video cameras (SHIMAZU: HPV-1 and NAC:
GX1), a PC for image processing and a data logger
(KEYENCE: NR-200). The tungsten electrode with added
2% La 2 O 3 with the diameter of 3.2mm and the conical
angle of 60 degrees was employed. The electrode gap was
5mm. An arc current was set to be AC 250A (frequency of
70Hz). The length of EP to that of a cycle was 0.3.
Shielding gas was argon and introduced at the flow rate of
15l/min. The wave form of the current was recorded with
the data logger. The cleaning zone of the oxide layer by
Fig. 2 Time variation of cleaning zone.
cathode spots on Fig. 1 Experimental setup.

Japan
180
Experimental observation of cleaning action of cathode spots in AC TIG welding of aluminum plates
Fig. 3 Distribution of cathode spots.

Figure 2 shows cleaning zone of the oxide layer by
cathode spots in 4 cycles from the arc ignition recorded
with GX1. In EP of the second cycle, although cathode
spots appeared on the oxide layer, cleaning of the oxide
layer didn’t occur. In EP of the third cycle, the oxide layer
in the region near the arc axis was removed by cathode
spots. After that, a large number of cathode spots occurred
on the edge of the cleaning zone and the cleaning zone was
expanded outward due to the cleaning action. From this
observation, it was found that cleaning rate of the oxide
layer was approximately 180cm2/s. A cleaning rate of
10cm2/s was reported in the case of stainless steel cathode
in low pressure [1]. As a reason for the difference, it is
considered that although the thickness of the oxide layer
formed on the aluminum plate was an order of 10nm [2],
that of the stainless steel was an order of ȝP Fig. 4 Traces of cathode spots
Figure 3 shows distribution of cathode spots recorded
with HPV-1. The cathode spots mark as positions 1~8 in
Fig. 3 were traced and their velocities were calculated. The
cathode spots at positions 1~5, positions 6 and 7 and
position 8 were on the weld pool, the oxide layer and the
boundary of the weld pool, respectively.
Figure 4 shows trace of each cathode spot for the same
duration. It was seen that distances of traces of the cathode
spots on the weld pool where the oxide layer was already
removed were larger than those on the oxide layer.
Figure 5 and Table 1 show time variations of cathode
spot velocities and their averaged velocities, respectively. Fig. 5 Time variation of cathode spot velocities
As a result, it was found that cathode spots moved slowly
on the oxide layer and their averaged velocity was an order Table 1 Averaged velocities of cathode spots
of 10m/s. On the other hand, cathode spots near the center
of the weld pool, where the oxide layer had been mostly
removed, moved at high speed and their averaged velocity
reached an order of 100 m/s. Furthermore, the velocity
greatly changed depending on the position of the cathode
spot and exceeded 1 km/s at the maximum.
4. Conclusions moved at high speed and their averaged velocity

Conclusions are summarized as follows. reached an order of 100 m/s.
(1) The cleaning rate of the oxide layer was approximately (4) The velocity greatly changed depending on the position
180cm2/s of the cathode spot and exceeded 1 km/s at the
(2) The cathode spots moved slowly on the oxide layer and maximum.
their averaged velocity was an order of 10m/s. References
(3) The cathode spots near the center of the weld pool, [1] K. Takeda et. al.: Material Transactions, 7 (1997) pp. 636.
where the oxide layer had been mostly removed, [2] M. S. Hunter, P. Fowle: Journal of the Electrochemical
Society 103 (1956) pp. 482.
181
Numerical simulation of heat source properties of pulsed tungsten

inert gas arc†
ITO Kuniyoshi*, TASHIRO Shinichi* and TANAKA Manabu*
KEY WORDS: (Numerical simulation) (Pulsed TIG arc) (Heat source property)
1. Introduction 5DGLDOPRPHQWXPFRQVHUYDWLRQHTXDWLRQ
The heat source properties of TIG arc strongly depend on w Uv r 1 w w wP
(rUv r2 ) ( Uv z v r ) j z BT
wt r wr wz wr
the composition of shielding gas. For example, since the arc
1 w wv w wv wv v
column is constricted due to low electrical conductivity of ( 2 rK r ) (K r K z ) 2K r2
r wr wr wz wz wr r
the helium arc, heat flux onto a base metal in case of helium
TIG arc is higher than that of argon TIG arc. The heat $[LDOPRPHQWXPFRQVHUYDWLRQHTXDWLRQ
source properties can be controlled also by current w Uvz 1 w w wP
( rUvr vz ) ( Uvz2 ) jr BT
waveform. Pulsed TIG welding is suitable for back-bead wt r wr wz wz
welding and thin plate welding, because the heat flux onto w wv 1 w wv wv
(2K z ) (rK r rK z ) Ug
the base metal can be controlled by adjusting peak / base wz wz r wr wz wr
current ratio and frequency. A number of results on (QHUJ\FRQVHUYDWLRQHTXDWLRQ
experimental and theoretical investigations of the heat w Uh 1 w w 1 w rN w h w N wh
(rUvr h) ( Uvz h) ( ) ( )
source properties of DC TIG arc have been reported. wt r wr wz r w r cp w r w z cp w z
However, those of pulsed TIG arc are still not fully jr E r j z E z U
understood because of the complexity of the phenomenon.
&XUUHQWFRQWLQXLW\HTXDWLRQ
In this study, the heat source properties of pulsed TIG arc

1 w
rj r w j z 0
for various shielding gas composition were numerically
analyzed.
r wr wz
2. Simulation Model 2KP̓VODZ
The calculation region for TIG arc consists of a tungsten jr VE r , j z VE z
cathode with diameter of 3.2mm and tip angle of 60 degrees,
arc plasma and a water-cooled copper anode. It is described
in a frame of cylindrical coordinate with axial symmetry
around the arc axis. The electrode gap is set to be 5mm.
Argon (Ar), helium (He) or carbon dioxide (CO 2 ) is
introduced as shielding gas from the upper boundary at the
flow rate of 10 l min-1. For example of physical properties
of each gas, specific heat, thermal conductivity and
electrical conductivity are shown in Fig. 1. Figure 2 shows
current wave form with the peak current of 150A and the
base current of 50A. The frequency is 100Hz and the pulse
width is 5ms. The laminar flow is assumed, and the arc
plasma is considered to be in the local thermodynamic
equilibrium (LTE). The governing equations (1)-(6) are
solved iteratively by the SIMPLEC numerical procedure [1].
The other numerical modeling methods are given in detail
in our previous paper [2].

0DVVFRQWLQXLW\HTXDWLRQ
wU 1 w w
(rUv ) ( Uv ) 0
wt r wr r
wr z
Fig. 1 Physical properties of shielding gas


Japan
182
Numerical simulation of heat source properties of pulsed tungsten inert gas arc
Fig. 2 Current wave form
In the above equations, t is time, h is enthalpy, P is

pressure, v z and v r are the axial and radial velocities, j z and
j r are the axial and radial component of current density, g is
acceleration due to gravity, Nis thermal conductivity, C p is
specific heat, U is density, K ŪŴġŷŪŴŤŰŴŪŵźĭġV is electrical
conductivity, U is radiation emission coefficient, E r and E z
are the radial and axial components of the electric field Fig. 3 Temperature distribution (Ar)
defined by E r =㸫ѨV/Ѩr and E z =㸫ѨV/Ѩz, where V is
electric potential.

Figure 3 shows two-dimensional temperature
distributions at t=30ms,32.5ms,35ms and 37.5ms in the
case of Ar. During the peak current, the heat caused by
Joule heating near the cathode tip was transported toward
the anode by convective flow and was also transported in a
radial direction by thermal conduction. Figure 4 shows
two-dimensional temperature distributions in the case of
CO 2 . In this case, although the heat transport toward the
anode by convective flow was seen, that in the radial
direction due to thermal conduction was smaller than that of
Ar because of influence of large specific heat. As a result,
the radius of the arc column hardly changed during the
calculation. Finally Fig. 5 shows two-dimensional
temperature distributions in the case of He. It was seen that
the temperature distribution changed momentarily
following the change in the arc current due to high thermal Fig. 4 Temperature distribution (CO 2 )
conductivity of He.
4. Conclusions
(1) In the case of Ar, the heat caused by Joule heating near
the cathode tip was transported toward the anode by
convective flow and was also transported in a radial
direction by thermal conduction.
(2) In CO 2 , although the heat transport toward the anode
by convective flow was seen, that in the radial direction
due to thermal conduction was smaller than that of Ar
because of influence of large specific heat.
(3) In the case of He, the temperature distribution changed
momentarily following the change in the arc current
due to high thermal conductivity of He.
References
[1] S.V. Patanker: Numerical heat transfer and fluid flow,
Hemishpere Publishing Corporation (1980).
[2] M. Tanaka, et.al.: Plasma Chem. Plasma Process, 23 (2003),
585-606. Fig. 5 Temperature distribution (He)
183
Numerical analysis of weld pool formation mechanism in TIG

welding in consideration of the influence of emitter material adding
to the tungsten cathode†
ZENIYA Tasuku *. TASHIRO Shinichi *, TANAKA Manabu*, YAMAMOTO Eri **,

YAMAZAKI Kei ** and SUZUKI Keiichi **
KEY WORDS: (Arc) (TIG welding) (Numerical simulation) (Unified model) (Emitter material)
1. Introduction treatment of current attachment on the cathode surface and

Generally, ThO 2 or La 2 O 3 are added to a tungsten heat and mass transfers among the cathode, the arc and the
cathode for prompting electron emission from the cathode weld pool.
and preventing cathode consumption [1]. Tungsten
employed as a cathode emits thermoelectrons enough for 2. Simulation model
providing arc current acting as thermionic cathode near the Figure 2 shows the simulation region. Pure tungsten
melting point of tungsten (3680K). The work function (W) and tungsten with added 2%ThO2 (2%ThO2-W) are
required for electron emission from the cathode surface selected as cathode materials. An arc current is 150A.
depends on the emitter material added to the tungsten Helium is introduced at flow rate of 30L/min as shielding
cathode. Therefore, the emitter material strongly affects gas. The laminar flow is assumed, and the arc plasma is
current characteristics near the cathode. Figure 1 shows a considered to be in the local thermodynamic equilibrium
photograph of the cathodes during TIG welding at 200A in (LTE). The anode material is stainless steel with low sulfur
cases of pure tungsten (W) cathode and tungsten cathode (30ppm). As driving forces of convective flow in the weld
adding 2% ThO 2 (2%ThO 2 -W) [1]. Although the cathode pool, electromagnetic force, Marangoni force, shear force
tip maintains a solid phase in the case of 2%ThO 2 -W and buoyancy force are considered. Figure 3 shows the
cathode, it was melted in case of a pure W cathode. In case assumption of surface tension of weld pool [2]. The
of a W cathode, the cathode temperature increases due to conservation equations of mass, momentum, energy and
decrease in cooling effect by thermionic electron emission current are solved iteratively by the SIMPLEC numerical
because of the large work function. It is considered that the procedure [3]. The other numerical modeling methods are
arc properties change through the redistribution of arc
current due to change of cathode shape. In this study, the
influence of adding 2% ThO 2 to the tungsten cathode as
emitter material on arc properties and weld pool formation
mechanisms in TIG welding were investigated by
employing a numerical simulation model considering
Fig. 1 Appearances of W cathode and W-2% ThO 2 cathode Fig. 2 Simulation region

** Kobe Steel, Ltd., Fujisawa, Japan Japan
184
Numerical analysis of weld pool formation mechanism in TIG welding in consideration of influence of emitter
material adding to tungsten cathode
given in detail in our previous paper [4]. The area of cathode. Although the maximum flow velocity in the
current attachment on the cathode surface was modeled by outward radial direction close to the anode surface was 11.2
the same treatment in Ref [5]. The cathode surface has the m/s in the 2%ThO 2 -W cathode, that decreased to 5.2 m/s in
work function of the emitter material where the surface a 2%ThO 2 -W cathode. For the reason of the difference in
temperature exceeds the melting point of the emitter weld pool shapes, it is considered that because shear force
material. Except for this region, the surface has the work acting on the weld pool surface for 2%ThO 2 -W cathode
function of the tungsten. was larger than that of a W cathode due to higher cathode
jet velocity, the heat transport in the weld pool near the
surface in radial outward direction increased.
Fig. 3 Assumption of surface tension [3]

Fig. 5 Calculation result of temperature for a pure W electrode
Figure 4 and 5 show two-dimensional temperature
distributions in the cathode, the arc and the anode in case of
2%ThO 2 -W and W cathodes, respectively. The maximum
temperatures of the arcs in both cases were 21740 K and
18580 K, respectively. It was found that difference between
the maximum temperatures was approximately 3000K. It
was also found that the maximum velocities of the cathode
jets were 156 m/s for 2%ThO 2 -W cathode and 497 m/s for
W cathode. It was seen that the arc temperature decreased
due to lower current density in the case of a W cathode
because the cathode tip was melted and became spherical in
Fig. 6 Cross section of the welding bead for a 2%ThO 2 -W
shape.
electrode
Figure 6 and 7 show cross section of the welding bead
for both cases. For evaluating validity of the simulation
model, those obtained from experiments were also
presented. It was found that the shape of the weld pool
became shallow and wide in case of 2%ThO 2 -W cathode.
On the other hand, that was deep and narrow in case of a W
Fig. 7 Cross section of the welding bead for pure a W electrode
4. Conclusions
It was found that although the maximum cathode jet
velocity in case of a 2%ThO 2- W cathode was 497 m/s, that
in case of pure W cathode was only 156 m/s because of low
current density caused by the flattened surface of the
melting cathode tip. In case of a 2%ThO 2 -W cathode, the
depth and the width of the weld pool became shallow and
wider than those in case of a pure W cathode. For the
reason of the difference in weld pool shapes, it is
Fig. 4 Calculation result of temperature for a 2%ThO 2 -W considered that because shear force acting on the weld pool
electrode surface for a 2%ThO 2 -W cathode was larger than that of a
185
W cathode due to higher cathode jet velocity, the heat [2] S.V. Patanker: Numerical heat transfer and fluid flow,
transport in the weld pool near the surface in radial outward Hemishpere Publishing Corporation (1980).
direction increased. [3] M. Tanaka, et.al.: Plasma Chem. Plasma Process, 23 (2003),
585-606.
[4] M.J. McNallan and T. Debroy: Metall. Trans. B, 22B (1991),
References
[1] M. Tanaka et al: J. Phys. D: Appl. Phys., 38 (2005), pp. 29-35. pp. 557-560.
[5] M. Tanaka et al: IIW Doc. 212-1091-06.
186
Efficiency comparison between iterative substructure method and

†
commercial software
ZHANG Linjie*, ZHANG Jianxun*, SERIZAWA Hisashi** and MURAKAWA Hidekazu**
KEY WORDS: (Finite element method) (Efficiency) (Iterative substructure method) (ANSYS) (Residual stress)
1. Introduction with acetone before welding. Argon was chosen as

A Welding process can result in undesirable residual shielding gas. Welding of beads-on-plate was performed in
stresses and distortion which is particularly critical for a welding fixture to ensure that a constant focal length was
precision components. Because it is impossible to obtain used.
the experimental data of every situation, computer Then, experimental tests were conducted to collect data
simulations of welding processes are needed in order to of residual stresses on the surface of workpiece. The hole-
predict the impact of different design options on residual drilling method was adopted. Figure 1 shows the positions
stress and deformation. Finite element simulation has at which the hole-drilling method was used to measure the
become a proven and reliable technique for prediction of residual stress.
welding deformations and residual stresses. However, finite Table 1 Chemical compositions of TC4 titanium alloy (wt %)
element simulations are currently only used in applications Al V Fe Si C N H O Ti
5.5~6.8 3.5~4.5 0.3 0.15 0.1 0.05 0.015 0.2 Bal
where safety aspects are very important or when a large
x
economic gain can be achieved [1]. The time and cost
associated with reliable analysis of complex industrial
problems appear to be the main reason contributing to this
practice. Investigators have attempted to develop strategies 3 4
10
0
7
10
6 1
focusing on different dominant factors that influence the
10
8 2 5
efficiency of modeling actual welded structures [2–6].
Noting the fact that the high temperature region which exhibits
strong non-linearity is limited to a very small area compared to
y
the size of the model to be analysed and the remaining part is Fig. 1 The positions at which hole-drilling method was used
mostly linear, an iterative substructure method (ISM) has been
to measure the residual stress.(Unit: mm)
developed to transform welding problem into the combination
of a large linear problem and a small but moving strong
nonlinear region, to improve the speed of computation.[7,8] 3. Numerical Model
In this work, we carried out a comparison of calculation Figure 2 shows the coordinate system and the mesh used
efficiency between an in house finite element (FE) code to predict the quasi-stationary shape of the molten pool.
developed based on the idea of iterative substructure Only half of the specimen is considered as it is symmetrical
method (ISM) and commercial FE software ANSYS. To about the symmetry plane of the weld. It can also be seen
achieve the research purpose, thermal elastic-plastic finite from Fig.2 that a dense mesh is put around the heat source
element analysis of laser welding process of TC4 plate was and the vicinity of top surface and bottom surface, while for
taken as an example and was simulated by ANSYS and an the other regions, a coarse mesh is employed. Eight node
in house developed FE code based on ISM, respectively. In brick element is used in this study and the model contains a
total of 20503 nodes and 16800 elements.
order to make a comparison of residual stress between
experiment and simulation, a hole drilling technique was
used to measure the residual stresses in the weldments.
2. Experiment Procedures
Welding was done with a continuous wave CO 2 laser
which delivers 3KW maximum mean power. The diameter
of the minimum focal spot was 0.4mm. The material used in
this study was TC4 of which the chemical composition is
presented in Table 1. The geometry of the welded plate was
200mm×200mm×2mm. Samples were manually cleaned Fig. 2 Mesh of the plate

* State Key Laboratory for Mechanical Behavior of Materials, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Xi’an Jiaotong University, Xi’an, China Japan
** JWRI, Osaka University, Osaka, Japan
187
Efficiency comparison between iterative substructure method and commercial software

Material Properties 200 ANSYS
The thermal and mechanical properties of TC4 alloy
employed in this study are shown in Fig. 3. 150
CPU time / h
1.2 100

E× 105[MPa]
1.0
C [J/gK] 50
0.8 VY× 103[MPa] ISM
0.6
0
U× 102[g/mm3]
0.4 Fig. 4 A comparison of CPU time between ANSYS and
0.2 ISM.
D× 104[1/K]
O>JmmsK@
0.0 1000
Longitudinal residual stress/Mpa

0 200 400 600 800
Tempreture t/qC Experiment
800 ISM
Fig. 3 Thermal and mechanical properties of TC4 600
ANSYS
400
Boundary Conditions 200

In thermal analysis, the thermal load was applied as a
0
heat generation rate corresponding to a volume of internal
heat generation power progressing along the weld line 0 5 10 15 20
Distance from weld centerline/mm
25 30
during analysis. Convection to the environment from all

exterior faces of the workpiece was considered, while Fig. 5 Results of longitudinal stress
radiation heat loss was neglected. 800
In the structural analysis, the boundary condition is that
Transversal residual stress/MPa

Experiment
points A, B and O (Fig. 2) are constrained in the z direction, 600 ISM
ANSYS
points O is constrained in the x direction, and the plane of 400
symmetry (i.e. x-o-z) is constrained in the y direction.
200
Analysis Procedure 0
Commercial FE software ANSYS and an in house
developed FE code based on ISM were used to solve the 0 5 10 15 20 25 30
model, respectively. To ensure a balanced comparison Distance from weld centerline/mm
between the analysis results for each case, the same analysis Fig.6 Results of transversal stress
procedure was used for both cases.
The problem was treated as a sequentially coupled The experimental result of longitudinal stress at the weld
analysis. First, a thermal analysis was performed to predict center is about 670MPa. The longitudinal stress at the weld
the temperature history of the model. Subsequently, center predicted by ISM and ANSYS are about 800 MPa
temperature results of the thermal analysis were applied as and 920MPa, respectively. In other words, at the central
body loads in a nonlinear transient thermal–mechanical region of the weld, the results predicted by ISM are closer
analysis. The same mesh used in the thermal analysis was to the experimental result than that predicted by ANSYS. In
used for the thermal–mechanical analysis. A volumetric addition, it is noted that when ANSYS is used the
heat source was employed in the thermal analysis. The maximum longitudinal stress appears at the weld center.
continuous welding process was approximated by the When ISM is used, the maximum longitudinal residual
advancing of a volumetric heat source. During welding, the stress arises in the heat affected zone(HAZ), which is
temperature, and consequently the temperature dependent similar to the experimental results. It can also be seen from
material properties, changed very rapidly. Thus, material Fig.6 that ISM predicted a slightly narrower width of the
properties and the stiffness matrix were updated at every tensile stress zone than the experimental result, while
equilibrium iteration. In addition it is assumed that elements ANSYS predicted a tensile stress zone in which the width is
with a temperature higher than 1500 Υ had little appreciably larger than the experimental result.
mechanical effect on the surrounding elements. Furthermore, Fig. 6 represents the distributions of
residual stress on the top surface in the Y-direction, as
4. Results and Discussion measured by hole-drilling method and the finite element
Figure 4 shows a comparison of CPU time between method. As Fig. 7 shows, ISM provided a slightly lower
ANSYS and ISM. As shown in the figure, the computation stress than the experimental results at the centerline of the
speed of ISM is about 13 times faster that that of ANSYS. weld, but are close to the experimental results in the HAZ.
Figure 5 depicts the distributions of longitudinal
residual stress on the top surface as measured by the hole- 5. Conclusions
d r illing metho d and the finite element method. (1) The computation speed of ISM is about 13 times faster
than that of ANSYS;
188
(2) At the central region of weld, the results predicted by [4] L.E. Lindgren, H.A. Haggblad, J.M.J. McDill, A.S. Oddy,
ISM are more accurate than those predicted by ANSYS; Comput. Methods Appl. Mech. Eng. 147 (1997) 401–409.
(3) The tension stress zone predicted by ISM is narrower [5] Y. Ueda, M.G. Yuan, ASME J. Eng. Mater. Technol. 115
than the experimental result, while that predicted by (1994) (1993) 417–423.
ANSYS is wider than the experimental result. [6] A. Bachorski, M.J. Painter, A.J. Smailes, M.A. Wahab, J.
Mater. Process. Technol. 92/93 (1999) 405–409.
References [7] H. Nishikawa, H. Serizawa and H. Murakawa: Sci. Technol.
[1] L.E. Lindgren, J. Thermal Stresses 24 (2001) 305–334. Weld. Join., 2007, 12, (2), 147–152.
[2] J.M.J. McDill, A.S. Oddy, Comput. Struct. 54 (1995) 183– [8] H. Serizawa, S. Itoh, T. Tsuda, H. Nishikawa, M. Shibahara
189. and H. Murakawa: Proc. Int. Conf. on ‘Welding science and
engineering’, Xi’an, China, October 2005, Xi’an Jiaotong
[3] J.M.J. McDill, J.A. Goldak, A.S. Oddy, M.J. Bibby, Comm. University, 240–246.
Appl. Num. Methods 3 (1987) 155–163.
189
Experiment and numerical simulation in temperature distribution

†
and welding distortion in GMA welding
YAMANE Satoshi *, YAMAZAKI Takuya *, KANETA Tomoaki *, NAKAJIMA Toru ** and

YAMAMOTO Hikaru **
KEY WORDS: (Weld pool) (Numerical simulation) (Welding distortion) (Penetration depth) (Thermal
conductivity) (GMA welding) (Temperature distribution of base metal) (Robotic welding)
(CAD)
1. Introduction
Recently, the robotic welding is applied in the need field Welding direction
to save the human costs and to reduce the need for skilled +
㼀㼛㼞㼏㼔
workers. This is important to save the production costs. If
the welding distortion before the welding can be predicted,
the design cost will be saved.
The simulation technologies are developed according to
the development of computers. In many applications, the
numerical simulation is applied to save costs. In the field of
the welding, the numerical simulations were proposed and
- 㻿㼑㼚㼟㼛㼞
applied to the practical field to determine the welding

conditions.
The accuracy of dimensions after welding of the steel Fig. 1 Setting for fundamental experiment
structure becomes an important factor for the product cost.
The dimension becomes inaccurate due to the welding
35
distortion. Therefore, the control of the welding distortion
a
is demanded in the steel structure welding to improve the
200
productivity. For this purpose, the estimation of the amount
160
Bead
of the deformation is needed and its behavior is investigated.

100
In this paper, the numerical model of the heat source was
35
20
proposed for the GMA welding. The fundamental welding 45

experiments in the bead were carried out to improve the 20 145
200 220
accuracy of the numerical model. Its model was based on
the fundamental welding result and the cross section agreed Fig. 2 Clamp position on base metal
with the experimental results. During the welding, the
behavior of the deformation and the temperature Table 1 Parameters in the numerical simulations
distribution was investigated by using a laser sensor and a Specific heat c [J/kg㺃K] 473
thermoelectric couple. Dynamic behavior of the
deformation was investigated during the welding. The 0DVVGHQVLW\ȡ>NJP3] 7850
visualizations of the dynamic behavior of deformation were Thermal conductivity ț>W/m㺃K] 51.5
tried by using the numerical analysis. The behaviors are in
good agreement with the experimental results. The effect of Emission coefficient h [W/ m㸰㺃K] 33.4
the bead shape on the deformation was discussed. Poisson’s ratio 0.33
Coefficient of linear thermal 11.8
2. Fundamental experiment expansion[1/K] ×10-6
Setting of the fundamental experiment is shown in Fig.
1. The dimension of the base metal is 500mm length, current and the welding speed were 28.7 V, 292.6 A and 5
200mm width and 12mm thickness. The fundamental mm/s, respectively. The displacement at the point a in Fig.
experiment was carried out under the conventional welding 2 was measured with a laser displacement meter. The right
condition, i.e., setting of the welding voltage, the welding side of the base metal was restricted by 6 clamps. The
numerical model was introduced by using the welding
* Graduate School, Saitama University, Saitama, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Hitachi Construction Machinery Co., Ltd, Ibaraki, Japan Japan
190
Experiment and numerical simulation in temperature distribution and welding distortion in GMA welding
conditions. in Fig. 4(b). The left side of the base metal without the
clamping was bended.
3. Numerical model of welding
Dimension of the numerical model is the same as the
fundamental experiment. The flow of the weld pool was
neglected. The arc was approximated by the heat input. The
numerical model is induced with the assumption, that the
heat conduction is dominant. The heat input is equal to the
product of the welding voltage V and the welding current I.
The calculation was carried out under the assumption that
40% of the heat input was used for melting of the electrode
wire, i.e., 60% of VI was given to the base metal. Let heat Fig. 3 Heat input to metal surface and weld pool
efficiency to the base metal, K be 0.7. The heat input VI is
8400 J/s. An equation of heat conduction is
wU § w 2U w 2U w 2U ·
Uc N ¨¨ 2 2 2 ¸¸ (1)
wt © wx wy wz ¹
where NU and c are heat conductivity, density and specific
heat, respectively.
The distortion analysis is based on the following partial (a) Temperature distribution. (b) Displacement due to
distortion.
differential equation:
Fig. 4 Simulation result
1 § we we we · 21 Q § wT wT wT ·
2 u , v, w ¨ , , ¸ D¨ , , ¸
1 2Q ¨© wx wy wz ¸¹ 1 2Q ¨© wx wy wz ¸¹ The penetration depth and the displacement were compared
wu , wv , ww between the simulation and the fundamental experiment, as
e Hx Hy Hz, Hx H Hz (2)
wx y wy wz shown in Fig. 5 and 6.
The simulation results of the bead width and the penetration
where QandD are Poisson's ratio and the coefficient of
depth was agreed with the fundamental experimental result.
linear thermal expansion.
In the fundamental experiment, the displacement was
The authors tried to denote the latent heat in the
measured with a laser displacement meter. The behavior of
numerical simulation, i.e, the specific heat is changed
the displacement at the point a on the base metal, as shown
between 1807 K and 1809 K to denote transition
in Fig. 1, is shown in Fig. 6. A good agreement between the
temperature between solid and liquid phase. The parameters
simulation and the experiment was obtained.
were listed on Table 1.
Moreover, the other experiment with other welding
conditions was carried out to confirm the validity of the
4. Boundary conditions in numerical model
numerical simulation. The results of simulation and the
The Newton cooling law was applied on the surface
experiment are shown in Fig. 7 and 8, respectively.
except for that in contact with the carrier.
wU 6. Conclusions
Uc q h(u 293) (3)
wt The numerical model was designed to investigate the
Since the heat capacity of the carrier is very big, the dynamic behavior of the displacement due to the welding
temperature for the surface in contact with the carrier is distortion. In spite of the difference between the numerical
fixed to 293 K corresponding to the atmosphere simulations and the experiments about the temperature
temperature. The heat input to the base metal is divided to behavior on the back side of the base metal, the behavior of
two parts, to be agreement with the penetration of the weld the displacement in simulation due to the welding distortion
pool, as shown in Fig. 3. One is the heat input for the base almost agreed with experiment.
metal. Other one is heat input for the weld pool. If the penetration shape in the numerical simulation is
The heat input is denoted by the following equation: the same as the experiment, the welding distortion can be
predicted.
3Q 3x 2 3z 2
q1 ( x, y, z ) 2
exp( ) (4)
) exp(
ȧr r2 r2
where r is the radius of the heat input to be 6.6 mm.
5. Simulation result
Numerical simulation was carried out by FEM, for
which the software is Mentat 2007. According to the
movement of the heat, the weld pool corresponding to a
gray color is moved and the deposited metal was made, as Fig. 5 Comparison of penetration shape
shown in Fig. 4(a). The displacement is denoted as shown in fundamental experiment
191
Fig.6 Comparison of amounts of transformation in

Fig. 8 Comparison of amounts of transformation.
fundamental experiment.
Fig. 7 Comparison of penetration shape for vilification.
192
Measurement of dynamical variation in two-dimensional

temperature distribution of TIG pulsed-arcs†
SAWATO Hiroshi *, TASHIRO Shinichi *, NAKATA Kazuhiro *, TANAKA Manabu *,

YAMAMOTO Eri **, YAMAZAKI Kei **, and SUZUKI Keiichi **
KEY WORDS: (TIG) (Pulse) (Arc) (Welding) (Spectroscopic Analysis)
1. Introduction to be 50A, 100A, 150A or 200A to compare with

TIG pulsed-arc welding is suitable for back-bead welding, experimental results and simulation results in the literature
thin plate welding and so on, because the heat source to confirm validity of these experimental results. Moreover,
properties can be controlled by the current waveform. The time variation in temperature distribution of the TIG pulsed
heat flux into the base metal is affected mainly by thermal arc was also observed. The peak and base currents were
conduction and electron condensation from the arc. Both 200A and 50A, respectively. The frequency was 50Hz.
factors strongly depend on the temperature distribution and
current path in the arc. In order to clarify the heat source 3. Result and discussion
properties of a TIG pulsed-arc, dynamic variation in two- Figure 2 shows temperature distributions in the radial
dimensional temperature distribution of TIG pulsed-arc was direction below 1mm from cathode tip. The cathode tip
measured through the Fowler-Milne method with a high angle was 45 degrees, arc current was 100A and arc length
speed video camera as a first step of the study. was 5mm. The measured temperature distribution was
compared to the experimental result in the literature [2] to
2. Experimental procedure confirm the validity of our experimental results. It was
A schematic diagram of experimental observation is found that both results were in good agreement and the
shown in Fig.1. In this study, the radiation from the TIG arc validity of our experimental results was confirmed.
on a water cooled copper anode was observed. The Figure 3 shows comparisons of temperature distributions
radiation was diffracted to the specific wavelength of (a) experimental results and (b) simulation results in the
(696.5nm) in the spectroscope and recorded as the two literature [3] at contact tip angle 60 degrees, arc current
dimensional image by the high speed camera (Photron, 150A and arc length 5mm. It is seen that both the maximum
FASTCAM-512PCI). The temperature distribution of the temperatures were approximately 17,500K and both
TIG arc was calculated from the intensity distribution in the temperature contours of 10,000K, 12,500K, 15,000K were
image through the Fowler-Milne method [1]. In this in good agreement.
experiment, we used tungsten cathodes with the conical tip Figure 4 shows the comparison of temperature
angles of 45 degrees and 60 degrees. The shielding gas distributions in cases of conical tip angles of (a) 45degrees
composition was pure argon. The welding currents were set and (b) 60 degrees. The arc current is 100A and the arc
length is 5mm.The both maximum temperature are about
17,500K. It was found that the arc in the case of a conical
tip angle of 45 degrees was more constricted than that of 60
degrees. It seems this indicates the effect of conical tip
angle on maximum arc pressure [4].
Figure 5 shows current waveform for TIG pulsed arc and
Fig. 6 shows time variation of temperature distributions of a
TIG pulsed arc at the times (A) ~ (D) marked in Fig. 5. As
a result, it was found that the arc column was expanded in
the radial direction and the maximum arc temperature was
20,000K during the peak current of 200A. On the other
hand, the width of the arc column decreased especially in
the downstream region of the arc and the maximum arc
temperature fell to 17,500K during the base current of 50A.
Fig.1 Schematic diagram of observation[1]

** Welding Company, Kobe Steel, Ltd., Fujisawa, Japan Japan
193
Measurement of dynamical variation in two-dimensional temperature distribution of TIG pulsed-arcs
Fig.5 Current waveform of TIG pulsed arc
Fig.2 Temperature distributions in radial direction below

1mm from cathode tip
㸦A㸧㸦B㸧
Fig.3 Experimental result (a) and simulation result (b) of 㸦C㸧㸦D㸧
two-dimensional temperature distributions
Fig.6 Time variation of temperature distributions of TIG
T(K) T(K) pulsed arc at the times (A) ~ (D) marked in Fig. 5
25000 25000
22500
20000
22500
20000
4. Conclusions
17500 17500 The dynamic variation in two-dimensional temperature
15000
12500
15000
12500
distribution of a TIG pulsed-arc was measured through the
10000 10000 Fowler-Milne method with a high speed video camera as a
7500
5000
7500
5000
first step of the study. Consequently, it was found that the
arc column was expanded in the radial direction and the
1mm 1mm maximum arc temperature was 20,000K during the peak
current of 200A. On the other hand, the width of the arc
column decreased especially in the downstream region of
the arc and the maximum arc temperature fell to 17,500K
during the base current of 50A.
References
[1] G N Haddad and A J D Farmer: J. Phys. D:Appl. Phys. 17
(1984), 118
䠄a䠅㻌㻌㻌㻌㻌㻌 (b)
㻌
Fig.4 Comparison of temperature distributions between [2] Hiraoka,et : Quarterly journal of the Japan Welding Society,
14 (1996), pp.641-648
cases of conical tip 45°(a) and 60°(b)
[3] M.Ushio, M.Tanaka and J.J.Lowke: IEEE Tran. P. S., 32
(2004), pp. 108~117
[4] Hiraoka et: Effect of electrode geometry on maximum arc
pressure in gas tungsten arc welding. Data of welding society
in Japan.
194
Improvement of bead formation in plasma MIG welding process in

pure argon atmosphere†
KATAYAMA Tsubasa *, TASHIRO Shinichi *, and TANAKA Manabu *,**
KEY WORDS: (Plasma MIG welding) (Bead formation) (Pure argon atmosphere)
1. Introduction
In the plasma MIG welding process, because shielding
gas is ionized in advance by a plasma electrode before
supply, the shape of arc is easily controlled through
electromagnetic force. Therefore the controllability of the
arc is remarkably enhanced compared with that in a
conventional MIG welding process. Because of this
advantage, it can be employed for MIG welding in pure
inert gas atmosphere. Although experimental results on
plasma MIG welding in pure argon atmosphere were
reported, further improvement of the welding process is
required because it is difficult to form a bead stably due to
lack of the wettability [1]. We have developed a new torch
for plasma MIG welding which has a shorter distance Fig. 1 Schematic illustration of Plasma MIG welding
between a contact tip and the top of a nozzle than that of the
conventional torch. In this study, experimental results on Contact tip
welding of steel plates with V groove in pure argon
atmosphere employing the new torch are discussed Plasma Electrode
compared with those for the conventional torch. Plasma nozzle
2. Experimental procedure Shield nozzle

The plasma torch for plasma MIG welding was 10 mm
improved to shorten the distance between a contact tip and
10 mm
the top of a nozzle than that of the conventional torch in
order to increase heat flux to base metal for increasing
wettability in pure argon atmosphere. Figure 1 shows a
schematic illustration of plasma MIG welding and Fig. 2 Fig. 2 Schematic illustration of anew torch
shows a schematic illustration of the new torch. The
distance between a contact tip and the top of a nozzle is
shorter than that of the conventional torch by 5mm. Figure
3 shows configuration of a V groove in the base metal.
Table 1 shows the experimental conditions of plasma MIG
welding. Furthermore, a surface temperature of weld pool
was also measured by a two color pyrometry method Fig. 3 Configuration of V groove
utilizing a measurement system consisting of a high speed
video camera and a spectroscope as shown in Fig. 4.
Table 1 Experimental condition of plasma MIG welding
Fig. 4 Temperature measurement system by two color

pyromety method
** "Fundamental Studies on Technologies for Steel Materials Japan
with Enhanced Strength and Functions" Consortium of
JRCM (The Japan Research and Development Center for
Metals)
195
Improvement of bead formation in plasma MIG welding process in pure argon atmosphere

Figure 5 and 6 show bead appearance and cross section
in the case of conventional torch and new torch,
respectively. It was seen that bead formation was improved
due to high wettability in the case of new torch. On the
other hand, incomplete fusion occurred due to the small
melting volume of the base metal and the bead surface
became convex in the case of the conventional torch. It is Fig. 5 Bead appearance and cross section in case of
considered that melting volume of the base metal increased conventional torch
because of the increased heat flux caused by high averaged
MIG current.
Oxygen content in the base metal was also measured. It
was found that although oxygen content in the case of the
conventional torch was 58.1ppm, that of the new torch
decreased to 41.3ppm. It is considered that the shielding
effect from the surrounding air was enhanced due to Fig. 6 Bead appearance and cross section in case of new
stabilization of the arc in the case of new torch. torch
Furthermore, the surface temperature of the weld pool
was measured by a two color pyrometry method.
Consequently, it was found that the surface temperatures in
both cases were approximately the same, which is the
melting point of the base metal. For this reason, it was
considered that the input powers in both cases were at
nearly the same level. Although the averaged MIG current
increased in the case of the new torch, MIG voltage and
plasma voltage decreased due to the short distance between
a contact tip and the top of a nozzle. In the case of the new Temperture[K]
torch, heat transport in the weld pool was enhanced because

of strong convective flow in the weld pool caused by
increased electromagnetic force. It is considered that this
factor also contributed to high wettability and increase in
the melting volume. Weld pool
As a result, it was found that bead formation in the case
of the new torch was improved preventing increase in heat
input to the base metal.
Fig. 7 Surface temperature distribution of weld pool in
4. Conclusions case of conventional torch
It was found that by utilizing the new torch with shorter
distance between a contact tip and the top of a nozzle
comparing to that of the conventional torch, the bead
formation was improved due to high wettability, because
melting volume of the base metal increased due to increase
in averaged MIG current and heat flux.
Acknowledgement
Part of this study was carried under the research activities
Temperture[K]
of the Consortium, which are financially supported by
NEDO.
References
[1] T. Kozuru et al: Preprints of the national meeting of J.W.S.,
83 (2008) pp.330-331.
Weld pool
Fig. 8 Surface temperature distribution of weld pool in

case of new torch
196
Mechanism of undercut in high speed welding based on moveless

TIG welding†
LU Zhenyang*, HUANG Pengfei*, CHEN Shujun* and LI Yan*
KEY WORDShigh speed welding)( undercut)( surface tension)(temperature gradient)
Sketch map of surface tension

1. Introduction
Undercut is the main form of welding defect with the
increasing of welding speed. In order to improve the Tc
appearance of the weld, the mechanism of undercut needs
to be analyzed. The flow direction of liquid metal in a
welding pool near the periphery is the main factor that
Periphery
decides undercut
The surface tension is the main driving force of liquid
Fig.1 Schematic diagram of motionless arc pool
metal movement in a welding pool, moreover, the
distribution and the direction of surface tension are decided 2. The influencing factors of undercut
by the surface temperature of the liquid metal. If the The experiment was also done with the base metal in
temperature coefficient of surface tension wV / wT 0 , the which the content of S is individually 0.02% ,0.01% and
liquid flow from the center of the welding pool to the 0.004%. The experimental results are shown as Fig.2. For
periphery appears in the surface of the welding pool, so the metal in which the content of surface active element is
undercut can’t occur easily. On the contrary, if wV / wT ! 0 , low, undercut will not appear in the moveless welding.
the flow direction of liquid metal is reversed, so undercut When surface active elements exist in metal (e.g the content
occurs easily. When there is no surface active element in of S is about 0.02-0.04% in steel), undercut occurs in the
moveless TIG spot weld without. Whereas, the results of
the metal, wV / wT 0 . Under the driving force of surface
welding experiment have no undercut with the iron-base
tension, a single circulation flow of liquid metal, which is
metal in which the content of S is very low (e.g S% is less
from welding pool center where the surface temperature is
0.01%).
high and the surface tension is small to welding pool edge
where the surface temperature is low and the surface
tension is large, appears in the welding pool. However,
when there is some surface active element existing in metal,
the temperature Tc in certain places of the welding pool
surface is the right temperature it changes the sign of the
temperature coefficient of surface tension. Based on the
sign of wV / wT , two regions are formed in the welding pool
S=0.02% S=0.01% S=0.004%
surface, so two or more circulation flow will appear in Fig.2 Appearance of weld spot under the same
welding pool, as shown in Fig. 1. When liquid metal flows welding condition
from the center of the welding pool to the periphery, When the energy input is equal, with different welding
undercut doesn’t occurEut when liquid metal flows from current and different welding time, the depth of undercut
periphery to the center of welding pool, undercut is likely to will rise with the increase of welding current and the
appear. decrease of welding time, because the temperature gradient
is large when the high-current is used to weld for a short

* The institute of welding technology, Beijing 8niversity of Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
7echnology, Beijing China. Japan
197
Mechanism of undercut in high speed welding based on moveless TIG welding

Under cut depth Hc/mm

$6 $6 $6 $6 Fig
4 Schematic diagram of flow in welding pool
Heat input distributiong
The filling metal is another factor to effect undercut.
Fig3 Undercut depth of different welding
When other conditions have no change, the depth of
current under the same input energy
undercut will decreases along with the quantity of filling
metal increase, and will disappear finally, as shown in
time, during which the surface tension gradient will
Table 1. This is mainly because the addition of filling metal
increase, which enhances the trend that liquid metal flows
makes trend of flow from periphery to welding pool center
from periphery to welding pool center, so the depth of
lower, which will counteract the effect of liquid metal flow
undercut increases, as shown in Fig. 3.
to inner absolutely, when its quantity reaches a definite
As described in Fig. 4, the molten angle is expressed
value. Therefore, undercut can be restrained.
byȘ. A liquid element near the periphery whose volume,
Table 1 Quantity of filling metal
of which the volume is V㸪is chosen in this article. / R is the Mass of filling Depth of undercut
outflow of liquid metal, and / L is the inflow of liquid metal. metal㸦mg㸧㸦mm㸧
When other conditions are the same, the lower the Șis ,the 0 0.1
higher the Li will be. On one hand, it is because the 30 0.066
distance between / R and / L decreases with the decrease of 70 0.018
Ș, which makes the two reverse liquid flows that, effected 100 0
by the viscous force of liquid and restricted by each other, 150 0
and the liquid canÿt reach the region near the periphery
easily. On the other hand, this is also because the cooling 3. ConclusionV
V
velocity of the welding pool is higher in the condition of To sum up, the existance of surface active elements,
smaller Ș , which makes the columnar crystals grow up temperature gradient, molten angle and filling metal, all of
quickly from periphery to form a mushy region near the those have important effects on undercut. When the content
periphery area , and the flow of / L is blocked. Both of them of a surface active element reaches definite values (e.g the
will cause the deficiency of liquid near the periphery area, content of S is about 0.02-0.04% in steel), undercut will
so the trend of undercut is enhanced. occur. Temperature gradient makes the degree of undercut
It can be seen from the fore analysis, that increasing increase along with its augment. Increasing molten angle
molten angle can decrease the drag of liquid flow near the can restrains undercut efficiently. Adding the quantity of
periphery area efficiently, and can slow down the freezing filling metal can also reduces the degree of undercut.
rate, which is favorable for the metal of welding bottom to
supply the area of periphery. So this has obviously effect to References
[1]Seigo Nishikawa. High Speed Arc Welding, Industrial
restrain undercut.
Robot,1999,26(5)㸸371-376
[2]すṊྐ.: ⁐᥋Ꮫ఍ᚿࠋ1982 ᖺ 30㸦8㸧㸸pp68-74
[3]G.M.Oreper,J.Szekely: Journal of Fluid
Mechanism,1984,147,pp53-79
[4]R.T.C. Choo, J. Szekely. Welding Research Supplement
1992,(3):77-93
[5]R.T. C.Choo, J. Szekely, R.C. :Welding Research Supplement
September 1990:346-361
198
Numerical analysis the influence of arc shape on metal transfer

process†
KADOTA Keiji*, HIRATA Yoshinori **
KEY WORDS: (Metal transfer model) (Arc discharge model) (Unified model) (Fe-vapor) (Electro-magnetic
force) (Shielding gas)
1. Introduction determined by Gaussian distribution.

In GMAW(gas shielded metal arc welding), a metal As shown in Fig. 1, the cells near a droplet surface have
transfer process dominates arc stability and affects weld a boundary between molten drop and arc plasma inside
quality. The quantitative analysis of the metal transfer themselves because a rectangular grid is used in this model.
process is needed to control the process. The boundary is determined by PLIC(piecewise linear
In a metal transfer process, an electro-magnetic force interface calculation)[2] used in the VOF(volume of
strongly acts molten droplets. The action of electro- fluid)[3] method when electrical conduction and heat
magnetic force vary with arc shapes which are not fixed. conduction on the boundary is calculated.
During a metal transfer process, the arc shape is also The other boundary condition is illustrated in Fig. 2.
changing as electrode shape is changing. Moreover, the arc VLiquid
&
n
&
n
shapes are changed by the plasma properties. In GMAW, Liquid
metal vapor evaporates from a weld pool and metal drops, J gas q gas
Tbboundary
and run into arc plasma. The metal vapor makes the arc Liquid Liquid
Liquid o u n d a ry
' J Right qRight

shape contracted because electrical conductivity and
radiation loss increase[1]. Vgas

'
Tgas
In this report, we calculated the time-change of arc
plasma together with a metal transfer process with/out J Bo
Bottom
tto m
qBo
Bottom
tto m
metal vapor. Therefore, the unified model, which consists Vliquid Vgas Tboundary Tgas
of metal transfer model and arc discharge model, was J gas V g l q gas O g
liquid '1 liquid '2
constructed. 1
V g l
Fg V g Fl V l
2. Assumptions and boundary conditions
Metal transfer and arc discharge are assumed as (a) Electrical conduction (b) Thermal conduction
axisymmetric phenomena around the wire axis. The
calculation model is constructed as cylindrical coordinate Fig. 1 Electrical and Thermal conduction
model under following assumptions. inside boundary cell
(1) A wire melting rate equals a wire feed rate. The Calculation domain
boundary between the solid region and the molten 8.0mm 10.0mm 8.0mm
region in electrode wire is fixed. A molten wire is
flowing out from the boundary at a constant rate. In
other words, molten droplets hang down on the Shield gas
boundary and grow at the wire feed rate. Wire(Anode)
(2) The temperature on the surface of the molten
wire is 2500K. In a solid region, the surface dr
temperature is below melting point and dropping dz
with distance from molten region. In addition, the 5.0mm Arc
physical properties of an electrode wire are uniform.
(3) LTE(local thermal equilibrium) approximation
is applied to the arc discharge model. Arc plasma BaseMetal(Cathode)
can be treated as viscous fluid with electro-magnetic
properties under LTE condition. Electrical density (Gaussian)
(4) The polarity is DCEP(direct current electrode
positive). The current density on a cathode surface is Fig. 2 Calculation domain
** Division of Materials and Manufacturing Science, Japan
Graduate School of Engineering, Osaka University, Japan
199
Numerical analysis the influence of arc shape on metal transfer process
Table 1 Welding condition 10%Fe.

Welding current 250A As previously explained, this is caused by the rise of
Shielding Gas 100%Ar electrical conductivity and radiation loss. As the arc
90%Ar+10%Fe contracts, the metal drop in 90%Ar+10%Fe is a little
Gas nozzle I16mm slimmer than that in 100%Ar.
(inside diameter)
Welding wire I1.2mm (mild steel) 4. Conclusions
The conclusions of this paper are described as follows.
3. Result and discussion (1) The interrelated influence between metal transfer and
The time-change of the metal transfer process and the arc discharge is represented by a unified model. The
arc discharge in two types of shielding gas was calculated. arc contracts as the metal drop is growing. The metal
The calculation conditions are described in Table 1. The drop grows slimly as the arc is contracting.
calculation results of the temperature distribution and (2) The addition of 10%Fe into Ar prompts contraction of
current density distribution are shown for 100%Ar in Fig. 3 the arc and makes the metal drop slim.
and for 90%Ar+10%Fe-vapor in Fig. 4.
References
As seen in Fig.3 and Fig.4, the metal transfer mode is
[1] S. Tashiro, M. Tanaka, K. Nakata, T. Iwao, F. Koshiishi, K.
spray transfer at 250A in both gas types. Arc length Suzuki and K. Yamazaki: Plasma properties of helium gas
becomes short and arc shape becomes small as the metal tungsten arc with metal vapour, Sci. Technol. Weld. Joining
drop is growing. The electro-magnetic force near the tip of 12 (2007), pp.202–207
drop becomes stronger because the current density is
increased by contraction of the arc. As a result, the metal [2] Kothe,D.B.,Rider,W.J.,Mosso,S.J.,Brock,J.S. : Volume
tracking of interfaces having surface tension in two and three
drop grows down slimly. Fig. 3 shows that the arc dimensions, AIAA 96-0859,(1996)
temperature in 100%Ar is very high. Arc temperature near
the drop tip is heated over 25000K. On the other hand, the [3] Hirt,C.W., Nichols,B.D.: Volume of Fluid㸦VOF㸧Method
arc temperature is lower in the whole and the arc shape of the Dynamics of Free Boundaries, J. Computational
contracts when the shielding g ggas is Ar gas containing Phy.,Vol.39,No.1, ((1981)pp.201-225
)pp
mm 3000K 27000K 3000K 21000K

mm
8 8
0ms 4ms 8ms 0ms 4ms 9.3ms
27100K 26100K 27500K 19000K 21000K 17000K
0 0
0 5 0 5 0 5 0 5 0 5 0 5
mm mm
(a) Temperature (a) Temperature
mm
5.0108A/m2 mm 5.0108A/m2
5
5
0ms 4ms 8ms 0ms 4ms 9.3ms
8 8 8 8 8 8
2.3x10 3.6x10 7.1x10 2.3x10 4.4x10 3.4x10
2 2 2 2 2 2
A/m A/m A/m A/m A/m A/m
2 2
2
0 2 0 2 0 2 0 2 0 2 0
mm mm
(b) Current density (b) Current density
Fig. 3 The time-change of the arc temperature and current Fig. 4 The time-change of the arc temperature and current
density distribution in 100%Ar density distribution in 90%Ar+10%Fe
200
In-process monitoring and adaptive control for micro welding of

titanium†
NAKAMURA Hiroshi *, KAWAHITO Yousuke ** and KATAYAMA Seiji **
KEY WORDS: (In-Process monitoring) (Adaptive control) (Titanium) (Micro laser welding) (Butt seam welds)
1. Introduction
Micro butt-welding with a pulsed laser has been often
used for sealing batteries in automobile and electronics
industries [1,2]. A gap in such laser welding is one of the
most important manufacturing problems, because the gaps
may cause fatal welding defects such as shallow
penetrations with underfilling or non-bonded joints.
In-process monitoring and adaptive control has been
proposed as one of the useful procedures to stably produce
sound penetration welds without welding defects.
Recently, some articles have been devoted to the researches Fig. 1 Schematic experimental set-up of in-process
of in-process monitoring and advanced adaptive control monitoring and adaptive gap control in micro butt laser
welding
technology in laser welding [3, 4]. The authors [3] have
shown that the heat radiation signal levels increase in gas. The beam was focused into a I 150 Pm spot diameter
proportion to the molten pool diameters and accordingly the as shown in Fig. 1. The laser oscillator has the noteworthy
shear strengths of lap welds in thin A3003 aluminum alloy feature of 50 W maximum average output power, with peak
sheets, and demonstrated that adaptive control on the basis power changeable within 5 kW at intervals of 100 Ps
of the heat radiation signal could stably produce sound according to the external voltage signal. The reflected
welds or on-site repaired welds. light and heat radiation from the laser irradiated area were
In this research, micro butt welding of pure titanium monitored coaxially with the Nd:YAG laser beam. The
was used with a pulsed fundamental Nd:YAG laser beam, in-process monitoring signals were measured by pin photo
and the reflected light and the heat radiation from the laser- diode sensors. High-speed pictures of the molten area
irradiated area were measured as in-process monitoring during laser irradiation were taken at the frame rate of
signals. These in-process monitoring signals were 20,000 frames/s from the angle of 45 degrees under the
evaluated by the correlation with the spot diameter of a illumination light of a 22-mW He-Ne laser. As for
molten pool, the penetration depth or the gap. Moreover, adaptive control, the laser peak power was controlled at
the laser peak power was controlled on the basis of both the 150 Ps intervals during irradiation according to the
reflected light and the heat radiation detecting the gap and reflected light or heat radiation to produce designed-size
the spot diameter of a molten pool in order to suppress spot diameters with suppression of underfilling. The 150
underfilling and small spot diameters for, not only spot Ps-rapid adaptive control loop consists of 100 Ps
welding, but also seam welding with the pulsed laser. monitoring periods and 50 Ps for the estimation of laser
welding conditions on the basis of in-process monitoring
2. Materials and Experimental Procedures signals and the change in the laser peak power.
The material used was commercially available pure
titanium of more than 98 % in purity. The samples were 3 3. Experimental Results and Discussion
mm thick and 1 mm wide as shown in Fig. 1. In-Process Monitoring of Reflected Laser Beam and Heat
Micro butt welding was carried out with the pulsed Radiation
fundamental Nd:YAG laser in 40-L/min Argon shielding An example of typical monitoring results of reflected
201
In-process monitoring and adaptive control for micro welding of titanium
was terminated according to the heat radiation over 1.7 PW

which predicted that the spot size reached the designed size
of 0.6 mm. Figure 4 shows typical surface appearances
and cross sections produced by the adaptive control for the
joints with the gaps of 60 Pm and 106 Pm, and as a
reference the ones on the right were made with
conventional rectangular pulses of 1.6 kW and 2 ms. The
minimum spot width was improved from 0.4 mm to more
than 0.6 mm, and the underfills were also reduced from 0.4
Fig.2 Monitoring results of typical butt welding, showing
mm to 0.15 mm as a result of the adaptive control.
laser pulse shape, reflected light, heat radiation and
high-speed observation images of the spot molten Moreover, the penetration depths were kept constant at all
pool under non-gap conditions the gap sizes.
Furthermore, the adaptive control was applied to the
light, heat radiation and high-speed video pictures during laser seam welding of butt joints with a 100 Pm gap. The
laser spot welding of a butt joint without a gap at 0.4 kW surface appearances and cross sections under the adaptive
power is shown in Fig. 2. The horizontal axis is time, and control or with the conventional rectangle laser pulse are
the vertical axis indicates measured values of laser power demonstrated in Fig. 5. However, the rectangle pulse had 2
and monitoring signals. The pictures show that melting ms pulse duration and 1.6 kW laser peak power. The
started at 0.4 ms and the molten pool expanded gradually minimum bead width increased from 0.4 mm to 0.6 mm and
during the following laser irradiation. According to the the maximum depth of underfills was reduced from 0.32
series of pictures from 5.75 to 5.85 ms, the molten pool mm to 0.16 mm. Therefore, the bead surface appearances
surface oscillated rapidly in 100 Ps short periods. The and underfills were improved greatly in comparison with
molten pool grew continuously during the laser irradiation. those with the conventional rectangle laser pulse.
As for the reflected light, the intensity increased until the Moreover, it was found that the adaptive control was more
molten area was formed at 0.4 ms, and then it became effective with the underfills or the smaller spots in more
almost constant during laser irradiation. On the other early laser shots, because the gap size was reduced by
hand, the intensity of heat radiation increased continuously solidification shrinkages generated in the previous laser
from the start of the laser irradiation. Compared with the welds.
molten pool in the high-speed video pictures, it was found
that the increase in the heat radiation was in proportion to
the growth of the molten pool.
Adaptive control for defect reduction in laser spot and
seam welding of butt joints
In order to produce the designed spots with reduction in
deeply-concaved underfills or smaller spots, the laser peak
power was controlled according to the flow chart as shown
in Fig. 3. The 0.4 kW laser peak was changed to 1.6 kW
on the basis of the reflected light over 80 PW indicating
that a molten pool bridged a gap. The laser irradiation
Fig. 4 Surface appearances and cross sections under adaptive
control for several sizes of gap
Fig. 5 Surface appearances and cross sections under the

Fig. 3 Flow chart of adaptive control for narrow spot and
adaptive control in seam welding with Pulsed YAG
underfilling
laser beam
202
The gap is one of the most important issues to be solved [1] T. Sakurai and Y. Nakagawa, Proc. 62nd Laser Materials
Processing Conf. Osaka, (2003), pp 102-110.
in laser welding of a micro butt joint, because the gap leads [2]H. Fukuda, K. Ito, H. Tmaki, Y. Yamauchi and T. Amazutumi,
to welding defects such as underfilling or a non-bonded SANYO Technical Rev., 28 (1995), pp 112-118.
joint. The experimental studies indicated that the adaptive [3] Y. Kawahito and S. Katayama, J. Laser Applications 17
control of the laser peak power on the basis of in-process (2005), pp.30-37.
[4] C. Begger and F. O. Olsen, J. Laser Applications 15 (2003),
monitoring could reduce the harmful effects due to gaps in pp.19-24.
micro butt laser welding with a pulsed laser beam.
203
Numerical analysis on heat source characteristics of two-electrodes

†
TIG arc
OGINO Yosuke*, HIRATA Yoshinori*, NOMURA Kazufumi*
KEY WORDS: (Arc welding process) (Two-Electrodes TIG Arc) (3D numerical model) (Heat input density)
(Arc pressure) (Total heat input)
1. Introduction are shown in Fig. 1. Each electrode is the same shape;

Various kinds of multi-electrodes welding processes have
been applied to manufacturing fields such as shipbuilding,
automobile and piping. However, their welding z
phenomena are very complex and it is hard to find and Electrode
Gas flowing
select optimum welding condition, because there are many area
particular parameters; electrodes distance, polarity and
current ratio of each electrode, which do not need to be
taken care for conventional single-electrode welding Arc plasma
process. Some work has been done to understand such x
complicated phenomena with experiments [1, 2].
In this research, we picked the two-electrodes TIG arc
process as an example of the multi-electrodes welding
process, and numerically investigated it with a 3D arc
plasma model. In the case of two-electrodes welding y
Base metal
with same polarities, two arc plasmas attract each other. Analysis condition
z Calculation domain
Therefore electrode distance is very important parameter. : 30 x 30 x 20 mm3
We numerically investigated the influence of the electrode (Two-electrodes)
distance on heat source characteristics of arc plasma : 20 x 20 x 15 mm3
focusing on heat input density, arc pressure and total heat (Single-electrode)
Arc length : 3 mm
input into the base metal. Electrodes distance Shielding gas : Ar
4 ~ 14 mm x
2. Numerical Model
Under the LTE (local thermo-dynamical equilibrium) Fig. 1 Schematic image of 3D numerical model of
approximation, the arc plasma can be treated as an two-electrode TIG arc
electromagnetic viscous fluid. Schematic explanations of
the 3D numerical model of TIG arc and analysis condition
z [mm] z [mm]
15 15
10000 K
10000 K
Max. temp. = 13390 K Max. temp. = 16850 K

Max. vel. = 52.7 m/s Max. vel. = 76.0 m/s
300 15000 K Arc voltage = 7.64 V x 300 15000 K Arc voltage = 9.45 V x
-10 0 10 -10 0 10
(a) Electrodes distance 6 mm [mm] (b) Electrodes distance 12 mm [mm]
Fig. 2 Influence of electrodes distance on temperature and velocity field of arc plasma

* Division of Materials and Manufacturing Science, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Graduate School of Engineering, Osaka University, Japan Japan
204
Numerical analysis on heat source characteristics of two-electrodes TIG arc
diameter is 3 mm and vertex angle is 90 degrees, set up

vertically to anode plate. The arc current of 100 A is 8.9 x 107
supplied for each electrode. Numerical analysis on single- Single-electrode TIG (200 A)
electrode arc is also carried out for comparison. In the
Peak of heat input density [W/m2]

5.0 x 107
case of single-electrode, arc current is 200 A. Electrode
distance is defined as distance between both electrodes’ tips.
In this calculation, anode plate is assumed to be not melted 4.0 x 107
nor deformed. TIG torch is stationary. Shielding gas is
Ar and flow from the gas flowing area shown in Fig. 1, 3.0 x 107
which includes space between electrodes.
2.0 x 107
3. Calculation Results
Figure 2 shows temperature distributions of arc plasma
calculated in the case of electrode distances of 6 mm and 12
1.0 x 107 Two-electrodes TIG
mm. It shows the xz surface across the two electrodes tips. (100 A x 2)
In the figures the isothermal line shows a temperature of 0
4 6 8 10 12 14
10,000K and the white arrows show flow vectors. As seen, Electrodes distance [mm]
the arc plasma generated from each electrode is drawn each
other by the electromagnetic force. Arc plasma shapes are Fig. 3 Influence of electrodes distance on peak value of heat
clearly changed as electrode distance is changed. As seen, input density
in the case of short electrodes distance, two arc plasmas are
421
combined as one large arc plasma. Single-electrode TIG (200 A)
Next, the heat source characteristics of the two-electrode
TIG arc were compared with those of single-electrode TIG Peak of arc pressure [Pa] 200
arc. When the arc current of 100 A is supplied to each of
the two-electrodes, the electrode distance is changed. 160
Then, the two-electrode distance decreases and ideally
becomes zero. We regarded it to be 200 A single- 120
electrode TIG arc.
Figure 3 shows the relationship between the electrode 80
distance and the peak value of the heat input density. In
this research, heat input into base metal from TIG arc is
40 Two-electrodes TIG
assumed to be provided by heat conduction and current
carrying electrons. Figure 4 shows the relationship (100 A x 2)
between the electrode distance and the peak value of the arc 0
4 6 8 10 12 14
pressure. These peak values of two-electrode TIG with
various electrode distances are much smaller than those of Electrodes distance [mm]
single-electrode TIG. The figures of Fig. 3 and Fig. 4 Fig. 4 Influence of electrodes distance on peak value of arc
show common characteristic trend clearly. Heat input and pressure
arc pressure of two-electrodes TIG arc significantly
changed depending on electrode distance, and take Single-electrode TIG (200 A)
minimum values at the electrode distance of 7-8 mm. 2000
Figure 5 shows the relationship between the electrodes
distance and the total heat input. As seen, the total heat
Total heat input [W]
input doesn’t change so much even if the electrodes 1600

distance changes. Moreover, there is not so large a
difference among total heat inputs of two-electrode with 1200
various distances and 200 A single-electrode.
In this way, in the two-electrode TIG arc, the heat input 800
density and the arc pressure change significantly, but the
total heat input does not change so much even if the 400
electrode distances changes. These heat source Two-electrodes TIG
characteristics of the two-electrode TIG arc is useful for (100 A x 2)
0
controlling heat input distribution with low arc pressure. 4 6 8 10 12 14
So, these calculation results show the possibility of the
Electrodes distance [mm]
“soft” heat source with high heat input by using the two-
electrode TIG arc. Fig. 5 Influence of electrodes distance on peak value of total
heat input
205
4. Conclusion References
In this work the heat source characteristics of two- [1] T. Ueyama, T. Uezono, T. Era, M. Tanaka, K. Nakata, Science
electrode TIG are numerically investigated with three- and Technology of Welding & Joining, 14, 4, (2009), 305-314
dimensional TIG arc model. Results obtained are [2] X. Leng, G. Zhang, L. Wu, Journal of Physics D: Applied
summarized as follows: Physics, 39, (2006)
(1) In the two-electrode TIG arc, both distributions of heat
input density and arc pressure significantly change
depending on electrode distance.
(2) The total heat input of the two electrode TIG arc does
not change so much even if the electrodes distance
changes.
(3) The two-electrode TIG arc with appropriate electrodes
distance serves as a “soft” heat source with high heat
input.
206
†
Research on discharge of sub-millimeter size process
PARK Mingon *, HIRATA Yoshinori *, NOMURA Kazufumi *
KEY WORDS: (Precise materials processing) (Glow discharge) (Arc discharge) (Glow-arc transition)
1. Introduction 2. Experimental procedure

Arc welding processes have been widely used as the The schematic illustration of the experimental setup is
indispensable joining technologies for various shown in Fig. 1. The electrode (W-2%ThO2) of 1mm
manufacturing fields because of low process cost with high diameter is used and placed inside the torch. The nozzle
efficiency and reliability. Plasma arc welding process, diameter is 0.3mm. The argon gas is used as plasma gas
which is one of the arc welding processes, has been applied for this experiment (0.2~0.5l/min). The current-voltage
to one pass welding with low distortion for sheet and/or waveform was measured by means of an oscilloscope. The
thin thickness plate up to 6 mm. But conventional plasma appearance of plasma discharge was observed using an
arc is not suitable for the precise materials processing of optical microscope set with a high-speed CCD camera. The
sub-millimeter sizes. In conventional plasma arc process, size of melting spot on base metal surface was also
the arc temperature increases with decrease of constricted evaluated by using optical microscope.
nozzle diameter. Then the nozzle is burn out eventually
when the nozzle diameter is less than 1mm. 3. Experimental results and discussion
Therefore, micro sized and/or sub-millimeter sized Figure 2 shows an example of waveforms of current
welding is normally carried out with a laser beam or and voltage of electrical discharge using the new type of
electron beam because it is possible to reduce the beam nozzle with the experimental power source. Nozzle
diameter less than 0.1mm. Recently micro sized discharge diameter and discharge gap was fixed at 0.3mm and 5mm,
process at atmospheric pressure is strongly demanded respectively. The electrode vertex angle was 30 degree.
because in laser beam process and/or electron beam process As seen in Fig. 2, the waveform of voltage was almost
there are several problems such as high cost, big size of constant at 800V, but
processing machine, low energy efficiency, and so on. some instances of high-voltage of around 1100V were
In this research, the possibility of precise materials observed. This phenomenon is considered to occur as
processing by electrical discharge energy at glow region or transition from normal glow to abnormal glow, that is, the
glow-arc transition region, which consists of low electric discharge is in glow-arc transition region. The
temperature plasma, was experimentally investigated using discharge appearance is shown in Fig. 3. It is noted that the
a new type of nozzle which was designed to establish very plasma diameter increased at the area of base metal then
small diameter plasmas and an experimental power source directly under nozzle.
which can supply wide range of voltage.
1600 1000
DCEN Plasma gas : Ar
Pulse 1400 900
Generator
Electrode 䠉 1200
ThO22%-W 1mm dia.
Nozzle diameter : 0.3mm
Arc length : 5mm
800
700
Current(mA)
Basemetal : stainless steel

Voltage(V)
1000 600
800 500
Power 600 400
Oscilloscope 300
CCD camera Microscope supply 400 Voltage
200
200 Current 100
0 0
nozzle
VTR PC 0 2 4 6 8 10 12 14
Base metal Discharge time(ms)
Fig. 2 Current and voltage waveforms of the electrical

TV monitor 䠇 discharge with the experimental torch and power source.
Fig. 1ᴾ Schematic illustration of the experimental setup.
* Graduate School of Eng., Osaka University, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
207
1300 DCEN Plasma gas : Ar gas

ThO22%-W 1mm dia.
Arc length : 4mm
1100
V o lta g e ( V )
Discharge time :8ms
Base metal : Stainless steel
900
700
500
0 100 200 300 400 500
Current (mA)
Fig. 5 Relationship between current and voltage of

the discharge in atmospheric pressure (nozzle
0.5mm diameter: 0.3mm)
Fig. 3 Appearance of Ar DC discharge-plasma Figure 4 indicates the melting spot at a base metal
surface formed with use of the nozzle of diameter of 0.3
constricted by the nozzle of diameter of 0.3 mm.
mm. The size of melting spot was formed with about
ίGap length 5mm, Discharge current 390mA, 0.3mm diameter. The center of melting spot is seen with
Discharge voltage 800Vὸ small dimple shape as seen in Fig. 4. This phenomenon
mainly occurred due to the high-current density at the
center of the melting spot, high arc-pressure, and local
evaporation of melting metal.
Figure 5 shows a relationship between current and
voltage of the discharge at atmospheric pressure. In the
figure average voltage and range of voltage fluctuation are
indicated. The average voltage gradually decreases with
increase of current beyond around 300mA. This is
considered to be arc-glow transition region.
G
4. Conclusion
The possibility of precise materials processing by
electrical discharge energy at glow region or glow-arc
transition region was experimentally investigated using a
new type nozzle which was designed to establish very
small diameter plasmas and an experimental power source
which can supply a wide range of voltage. The results
obtained are summarized as follows:
(1) When discharge current increases, discharge mode
changes from normal glow to abnormal glow, that is,
glow-arc transition region.
0.5mm (2) Sub-millimeter sized melting spots were formed at the
base metal surface using the constricted nozzle of 0.3
mm in diameter.
Fig. 4 Photograph of melting spot at a stainless steel References

plate formed by the nozzle of diameter of 0.3 mm. [1] Y. Hirata: J. Japan High-Temp Soc., 28 (2002), pp.40-44.
ίGap length 4mm, Discharge current 390mA, [2] S. Watanabe, S. Saito, K. takahasi and T. Onzawa: J. Japan
Discharge voltage 800Vὸ Welding Soc., 20 (2002), pp.493-498.
208
Influence of magnet configurations on magnetic controlled TIG arc

†
welding
NOMURA Kazufumi *, OGINO Yosuke *, HAGA Takuya ** and HIRATA Yoshinori *
KEY WORDS: (Magnetic control) (Permanent magnet) (Arc plasma) (Weld penetration) (3D analysis)
1. Introduction
Magnetic field
Arc plasma is affected by external magnetic forces.
From this view point, conventional studies have been Arc plasma
conducted on controlling the arc plasma by magnetic force
N S
for effective welding [1-4]. We focused on the cusp type
of magnetic field, which changes the cross section of the arc
plasma from a circular to an elliptical shape. In the
previous study, the cusp magnetic field suggested by Maruo
et al. was given by solenoid coils [4]. On the other hand,
we made the magnetic field by permanent magnets. Its S N
characteristics are small device size and no other power Electromagnetic
source. We have applied this magnetic control to TIG arc pinch force Magnetic poles
welding and evaluated its performance experimentally and
theoretically. It was confirmed experimentally that the (a) Conventional TIG arc (b) Magnetized TIG arc
permanent magnets installed in the TIG torch can make an
arc plasma with an elliptical shaped cross section. As a Fig. 1 Principle of elliptical arc shape by cusp type
result, bead on plate welding with the magnetized TIG arc magnetic field
provided sound weld beads and the limit of welding speed
without a weld imperfection was expanded [5, 6]. Our
previous results show that arc
shape control by permanent S N
magnets is useful. Tungsten
electrode
2. The Aim of This Study
13 mm
Figure 1 shows the principle
of the elliptical arc shape
generated by the cusp type Arc plasma
magnetic field. A conventional
13 mm
TIG arc plasma is illustrated in N S
Fig. 1 (a). The cross section of Water

the arc plasma is circular. In cooled 2 mm
contrast, the magnetized arc device
plasma by the cusp type magnetic
field, which is composed of four
S N S N
magnetic poles, is shown in Fig. S N
1 (b). The magnetic fields of N S
the arc and the external magnets Arc length Hm Hm

are in the same direction in the
right and left areas, and reversed Base metal
in the top and bottom areas.
Therefore, the field produces (a) Without magnets (b) Type A (c) Type B
alternative electromagnetic pinch
forces, and changes the cross Fig. 2 Experimental condition of magnet configurations

* Graduate School of Engineering Osaka University, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Osaka, Japan Japan
㻌 ** School of Engineering Osaka University, Osaka, Japan
209
Influence of magnet configurations on magnetic controlled TIG arc welding
section of the arc plasma from a circular to an elliptical 5. Conclusions

shape. For example, Fig. 2 (b) is one of actual alignment
In this study, we applied the cusp type magnetic control
of magnets providing a cusp type of magnetic field. In
to TIG arc welding with permanent magnets and
order to provide the cusp type magnetic field, an
investigated the influence of the magnet configurations.
arrangement of magnets’ position like that is required.
We made two types of magnet configuration where the
Therefore, we can consider different configurations of
magnetized direction is different from each other. As a
magnet positions. In this paper, the influence of the
result of magnetic control, narrower bead width, deeper
magnetic field varying with the arrangement of magnets is
penetration, higher aspect ratio of weld penetration and
investigated experimentally.
change of the flow inside the weld penetration were
obtained. However, their effects depend on the magnets
3. Experimental setup
configuration. One type affects the arc plasma much more
We performed TIG arc welding with the cusp type than the molten pool, resulting higher elliptical effect.
magnetic field experimentally. Four permanent magnets Another type has the advantage in controlling the weld
are placed inside the water cooled device to prevent the penetration such as deeper penetration.
magnets from heating as shown in schematic Fig. 2. This
device is inserted into the nozzle of the TIG torch. The
base metal is stainless steel plate. Other experimental References
conditions are tabulated in Table 1. To investigate the [1] K. Ando, J. Nishikawa and N. Yamanouchi: J. Japan Welding
influence of magnet configurations, we made two types of Soc., 37-3 (1968), pp. 249-254.
magnet configurations where the magnetized direction is [2] S. Ukita, T. Masuko, T. Irie and K. Kokubo: Quarterly J.
Japan Welding Soc., 20-4 (2002) pp. 484-492.
different from each other. Furthermore, the distance [3] H. Kobayashi and S. Nakahara: Quarterly J. Japan Welding
between the magnets and the base metal (= Hm) is a factor Soc., 7-3 (1989) pp. 57-63.
that determines the relationship of the magnetic field and [4] Y. Arata and H. Maruo: IIW Doc., IV-53-71 (1971).
the arc plasma. This is also investigated by changing this [5] K. Nomura, K. Morisaki and Y. Hirata: Welding in the World,
value from 5 mm to 3 mm. 53, 7/8 (2009) pp.181-187.
[6] K. Nomura, Y. Ogino and Y. Hirata: Quarterly J. Japan
4. Results and Discussions Welding Soc., 27, 3 (2009) pp. 170-175.
The experimental results are summarized in Fig. 3. Table 1 Experimental conditions

The crater shape comparison shows that the elliptical effect
and the sensitivity to magnets’ positions of type A seem to TIG arc condition Base metal䠖 SUS304
be higher than that of type B. The comparison of weld Welding speed: 0, 10 cm/min
Arc length: 5 mm
penetration under the 10 cm/min bead on plate welding also Current: 150 A Magnets condition
shows differences. Narrower bead width and higher D/W Shielding gas: ArƐPLQ
are obtained due to the magnetic control. In the case of Size: 5x6x2 mm3
Electrode diameter: 3.2 mm Surface magnetic flux: 300 mT
type B, the penetration becomes deeper compared with the Electrode vertex angle: 60 o
conventional arc. This implies that the magnetic control Height (= “Hm” in Fig. 2): 3, 5 mm
also changes the flow inside the weld penetration.
Hm = 5 mm Hm = 3 mm
Weld penetration
Crater Crater Bead appearance
D: depth, W: width [mm]
D = 2.4
magnets
Without
W = 9.9
D/W = 0.24
D = 2.1
Type A
W = 4.2
D/W = 0.49
D = 3.1
Type B
W = 7.1
D/W = 0.43
Stationary arc
(1 sec. after arc ignition) Bead on plate welding (10 cm/min)
Fig. 3 Influence of magnet configurations on TIG arc welding
210
Visualization of EM process by FEM†
YU Chun *,
LU Hao *
KEY WORDS: (Electromigration) (Concentration) (Finite element method) (lead-free solder)
1. Introduction
Electromigration (EM) is a directional mass transporting
phenomenon, which is induced by a high current density. It
is a critical reliability issue in electronic packaging, since
the dimension of the interconnects and solder bumps
continuously decrease, and meantime, the current stressing
increases. Up to date, there are a lot of reports on the
investigation of EM mechanism in the flip chip solder joints
from an experimental view [1,2]. A few works have also Fig. 1 Cross section of solder joint
been performed to study the current density distribution in
the solder bump by employing finite element modeling 3. Results and Discussions
(FEM). However, the concentration distribution of the Figure 2 shows the concentration fields of the Cu and Sn
elements in the solder bump in the EM process is unclear. elements, just under the driving force from chemical
This paper aims at investigating the concentration field in potential. It is seen that the diffusion is uniform.
the solder joints under current stressing. And the model can
be used to predict the EM lifetime of the solder joints.
2. Model
There is a well established function, which describes the
relationship among the atomic flux and different physical (a) (b)
field, it is,
* * * * * Fig. 2 Diffusion under chemical potential. (a) Cu; (b)Sn
J J CH J EM J TH J ST
Figure 3 reflects the cross-sectional views of the current
CD * * 㸦1㸧
( DC ) eZ j density distribution in the solder joints The current density
kT distribution is non-uniform in the XY plane; most current
CQ * D Cȍȍ concentrates on the entry and exit points inside the bump.
T ı H
kT 2
kT The current crowding at the cathode side induces a
According to the second Fick’s law, the concentration maximum current density, which occurs at the entry point
equation for a multi-field EM process is established, near the top Cu line.
wC CD * *
[( DC ) eZ j
wt kT 㸦2㸧
CQ * D Cȍȍ
T ı H
kT 2 kT
*
For simplification, J*TH , and J ST are neglected in this
work. Figure 1 shows the geometry model and mesh for a
Cu/Sn-0.7Cu/Cu joint. 2.85A current was applied.
Fig. 3 Current density

* Materials Science and Engineering School, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Shanghai Jiao Tong University, Shanghai, China Japan
211
Visualization of EM process by FEM
The maximum current density is the cause for the EM 0.65

failure in the solder joints. The electron wind force
generated by current crowding pushes the atoms from the 0.60
cathode side to the anode side. So we can see the different
Concentration (wt%)
0.55
concentration field, as shown in Fig. 4.
0.50 away from the crowding area
0.45
0.40
0.35
0.30
0 20 40 60 80 100
Time (hr)
Fig.4 Diffusion of Cu under current stressing Fig. 6 Concentration change of Sn in cathode IMC
Due to the higher concentration in the solder, the 4. Conclusions

diffusion of Sn determines the formation of voids. Figure 5 (1) A concentration equation was established to visualize
shows the concentration change of Sn under the electrical the EM process;
field. Basically, the Sn concentration change reflects two (2) Atoms flow from the cathode crowding zone to the
information, namely, where the EM-voids and where the anode crowding zone under current stressing, which
crush happen, and the voids grow up with aging time. It is results in void formation at the cathode crowding
agreement with the Ref.[3]. zone.
Also, we found that the concentration change is different (3) Atom diffusion is different according to the site from
according to the distance away from the crowding zone, as the crowding zone.
shown in Fig. 6 where near the crowding zone, the current
stressing dominates the diffusion, and at the site far away
References
from the crowding zone, where chemical potential
determines the diffusion. [1] K N Chiang, C C Lee, C C LEE: Applied Physics Letters,
88(2006), 072102.
[2] D Yang, Y C Chan, K N Tu: Applied Physics Letters,
93(2008) , 041907.
[3] T Y Lee, K N Tu, S M Kuo: Journal of Applied Physics,
89(2001), pp.3189-3194.
Fig. 5 Concentration change of Sn under electrical and

temperature fields. 100, 300, 700, and 1000 hrs
212
Numerical simulation of fusion zone shape of lotus-type porous

†
metals produced by laser welding
TSUMURA Takuya *, NAKAJIMA Hideo ** and NAKATA Kazuhiro *
KEY WORDS: (Lotus-type porous metal) (Laser welding) (Anisotropy) (Thermal diffusivity)
ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ (Laser absorption coefficient)
1. Introduction
Lotus- and Gasar- type porous metals had been
developed by Boiko et al. [1, 2] and Nakajima et al. [3-5]
and these were expected as innovative engineering
materials because the directional pore yields various unique
properties [6]. Laser weldability of the lotus-type porous
copper [7], iron [8] and magnesium [9] was investigated,
and the effect of pore direction on laser fusion zone shape
of the magnesium [10-12] and the copper [11,12] by using
the results of 3D FEM analysis of temperature distribution
during welding were demonstrated. These have pointed out
that the relation between direction of the pores and the laser
irradiated direction appreciably influence weld formation.
In the present paper, we performed 3D FEM analysis of Fig. 1 Schematic views of the lotus-type porous metals
temperature distribution during laser welding for the lotus- showing combinations of pore direction, applied
type porous iron and compared the fusion zone shape with heat source direction, and welding direction.
those cross sections obtained by experiments [8]. We also
estimated the anisotropy of thermal diffusivity inherent in
the lotus-type porous metals, and the anisotropy of the laser
absorption coefficient caused by the phenomenon of
multiple reflections of laser on the wall of pores.
2. Experimental procedure and results

Table 1 shows properties of the lotus-type porous
metals used; They are Lotus copper [4-6, 7, 13, 14], Lotus
magnesium [6, 9, 15-17], and Lotus iron [8, 18]. These
metals exhibited different thermal conductivity along and Fig. 2 Bead appearance and cross section of Lotus iron
normal to the directional pores [14]. In order to welds; laser power of 1.0 kW, laser spot diameter
demonstrate the effect of this characteristic on the welding of 1.0 mm, and welding speed of 1 m·min-1 [8].
phenomena, three different combinations of relationships - Laser welding was conducted using an Nd:YAG laser
pore direction, applied heat source direction, and welding unit. Laser beam irradiated the specimen surface with spot
direction- were considered as shown in Fig. 1. diameter of 0.45 - 1.0 mm at irradiate
Table 1 Properties of the lotus-type porous metals and laser irradiate conditions. angles of 10-32q as shown in Table 1.
Argon with a flow rate of 25-30 l·min-1
was used during welding. Cross sections
of the welded samples were observed
with a digital microscopy.
Figure 2 shows bead appearance
and cross section of the Lotus iron [8].
Fusion zone shape and penetration depth
of the weld bead has little difference for
three combinations.

** ISIR, Osaka University, Ibaraki, Japan Japan
213
Numerical simulation of fusion zone shape of lotus-type porous metals produced by laser welding
3. Numerical simulation and discussions determined as shown in Table 1. There is very little
3D FEM calculations of temperature distribution of the difference between E and E ' .
Lotus iron were performed using ABAQUS with user-
defined subroutines. The Lotus iron is modeled as an
equivalent orthotropic material. Equivalent density, 4. Conclusions
equivalent specific heat, and thermal conductivity along and The conclusions of this study are summarized as follows.
normal to the directional pores with temperature (1) Fusion zone shape of the weld bead has little difference
dependencies are described by the pore volume content for three combinations. Calculated shapes and the
ratio H and the property of non-porous iron (AISI1006) experimental ones were similar.
[20]. (2) The difference between the equivalent thermal
Fusion shape of the weld metal is estimated by the cross diffusivity along and normal to the directional pores is
section of maximum temperature exceeding the melting small for the Lotus iron.
(3) The little difference of laser absorption coefficient E
and E ' for the Lotus iron.
Acknowledgment
This research was supported as part of the entrusted
project “development of lightweight high stiffness structural
materials and evaluation technology” for the “advanced
Fig. 3 Maximum temperature distributions of Lotus iron in machining system development project” in the fiscal year
the cross section at half of the welding (x) direction; 2005 consigned by NEDO. The authors gratefully
absorbable laser power of 0.522 kW, laser spot appreciate this support.
diameter of 1.0 mm, and welding speed of 1 m·min-1.
point at half of the x direction. Figure 3 shows maximum References
temperature distributions of the Lotus iron. The absorbable [1] L.V. Boiko et al.: Sov. Powder Metal. Met. Ceram., 30
laser power is assumed to 0.522 kW as the most similar (1991), pp. 78-81.
results between the experimental fusion depth and the [2] L.V. Boiko: Mater. Sci., 36 (2000), pp. 506-512.
calculated ones for the Combination 2 A A . Fusion [3] S.K. Hyun et al.: Proc. Int. Conf. Solid-Solid Phase
Transformations ’99 (JIMIC-3), (1999), pp. 341-344.
zone shape has little difference, and the calculated shapes [4] H. Nakajima et al.: Coloids Surfaces A, 179 (2001),
and the experimental ones were similar. pp. 209-214.
The reason is considered as follows; Equivalent thermal [5] S.K. Hyun et al.: Mater. Sci. Eng. A, 299 (2001),pp.241-248.
diffusivity along and normal to the directional pores are [6] H. Nakajima: Prog. Mater. Sci., 52 (2007), pp. 1091-1173.
described as follows: [7] T. Murakami et al.: Mater. Sci.Eng.A,357(2003),pp.134-140.
[8] H. Yanagino et al.: Mater. Trans., 47 (2006), pp. 2254-2258.
D eq// D n , D eqA 1 H D n
1
(1).
[9] T. Murakami et al.: Mater. Sci.Eng.A,456(2007),pp.278-285.
Table 2 shows the equivalent thermal diffusivity for the [10] T. Tsumura et al.: Mater. Sci. Forum, 502 (2005), pp. 499-
used metals. The difference between these values is small 504.
for the Lotus iron. [11] T. Tsumura et al.: Mater. Trans., 47 (2007), pp. 2248-2253.
Anisotropy of the laser absorption coefficient caused by [12] T. Tsumura et al.: Soild State Phenomena, 127 (2007),
the phenomenon of multiple reflections of laser on the wall pp. 307-312.
[13] S.K. Hyun et al.: Mater. Sci. Eng. A, 340 (2003), pp. 258-
of open pores is also considered; Number of multiple
264.
reflections n is described by: [14] T. Ogushi et al.: J. Appl. Phys., 95 (2004), pp. 5843-5847.
n int t tan T / d (2). [15] T. Ikeda et al.: J. Jpn. Foundry Eng. Soc. 74 (2002),
Here, t is sample thickness, T is laser irradiated angle, pp. 812-816 (in Japanese).
[16] T. Ikeda et al.: J. Jpn. Inst. Light Met. 54 (2004), pp. 388-
d is average pore diameter. Equivalent heat input along
393 (in Japanese).
and normal to the directional pores are described as [17] Z.K. Xie et al.: Jpn. J. Appl. Phys. 43 (2004), pp. 7315-
follows: 7319.
Q Ain = E Q, Q in// = [(1-H )E + (1-(1-E )n )H ]Q=E ' Q (3). [18] M. Tane et al.: Acta Mater. 52 (2004), pp. 5195-5201.
[19] E.A. Brandes: Smithells Metal Reference Book, 6th ed.,
Therefore, laser absorption coefficient E and E ' are Butterworths, London, (1983), p. 17-7.
[20] M.R. Frewin et al.: Welding Research
Table 2 Estimated thermal properties of material used at room temperature. Supplement, (1999), pp. 15s-22s.
[21] Japan Society of Thermophysical
Properties Ed.: Thermophysical
Properties Handbook, Yokendo LTD,
Tokyo, (1990), p. 23 (in Japanese).
214
Numerical simulate on the coupled arc and pool for GTAW using a
†
unified mathematical model
LEI Yongping*, SHI Yaowu*, LIN Jian *, LU Zhenyang **, XIAO RONGSHI*** and
MURAKAWA Hidekazu****
KEY WORDS: (Numerical simulation ) (Unified mathematical model) (Coupled arc and pool ) (Boundary-
fitted coordinate system ) (GTA) (Welding)
1. Introduction "clear" interface characteristics, and is different from the

It is well known that in tungsten arc (GTA) welding whole model with a "fuzzy" interface.
process, the formation of weld is accompanying the The detailed governing equations, auxiliary formulas,
interaction between the weld arc and pool. The arc heat boundary conditions and numerical method are given in the
melts the work-piece and forms a pool. Once the molten paper [3].
pool begin to form, several important physical chemistry This model is also can be used for the situation of a water
phenomena, such as depression of weld pool surface, cooled cupper work-piece. In that cases the arc physical
radiation and convection heat loss from the free surface, phenomena can be study deeply.
will simultaneously take place at the pool surface. These cathode (-)
phenomena turn back again to influence the arc thermo-
self induced E D
fluids phenomena. Therefore, the weld arc and pool electromegnitic F
filed radiative and convection
essentially compose of an integrated system. But in the losses
most of numerical simulation models, the weld arc and pool G
are deal with as an independent model, or the weld pool
surface is assumed as flat [1], or specified weld pool shapes heat flux current
flux
were used [2]. Su
a
ten rface sm rce
In this paper, a unified mathematical model for a sio
n Plag fo I r
H dra C
stationary Gas Tungsten Arc (GTA) welding was developed. Lorentz bouyancy force
The model was composed of two sub-models describing the force
weldpool
heat transfer and fluid flow in weld arc and pool conduction
z
respectively. anode (+)
A B
2. Numerical Solution Strategy

As we know, the welding arc and pool constitute a whole radiative and convection
system, but they have different physical characteristics. losses
Therefore, this system can be divided into two sub-systems Fig.1 Schematic diagram of stationary GTA welding with
which connected by a variable common interface. The computational regions and driving forces
unified computational model is schematically illustrated in
Fig. 1 in which the different driving forces, the coordinate
system and computational regions of welding arc and weld The material used for calculation was AISI 304 stainless
pool are shown. The two set of governing equations and steel. The shielding gas used for calculation was pure argon
auxiliary formulas, controlling the welding arc and pool and the thermo-physical properties of the argon plasma at
respectively, were solved separately by a finite difference atmospheric pressure are obtained from Murphy [6]. The
method. In the calculation, the interface profile between
calculation conditions are 5mm arc length and 60rcathode
welding arc and pool is updated dynamically in a small time
step until it satisfied the convergence criterions, and then vertex degree, 200A welding current, 14V welding voltage,
the calculating regions for the two sub-models are re- 3.2mm the cathode diameter, 10.0 L/mm-1 shielding gas
meshed. A boundary-fitted coordinate system was adopted flux.
to precisely describe the cathode shape and weld-pool free- Figure 2 shows a set of typically calculated results. The
surface profile as well as the unknown molten shape of arc temperature fields, the fluid flow in the weld pool and
work-piece during welding. This calculation method has a the weld pool shapes at different welding time. It can be
* School of MSE, Beijng University of Technology, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** School of MS&AET, Beijng University of Technology, Japan
China
*** LERI, Beijng University of Technology, China
**** JWRI, Osaka University, Japan
215
Numerical simulation of the coupled arc and pool for GTAW using a unified mathematical model
temp temp
2 20000 2 20000
19000 19000
18000 18000
4 17000 4 17000
16000 16000
15000 15000
6 14000 6 14000
13000 13000
12000 12000
z /mm
z /mm
8 11000
8 11000
10 10
12 12
L = 5 mm
14 t = 0.5 s 14 L = 5 mm
t = 1.0 s
16 16
-10 -8 -6 -4 -2 0 2 4 6 -10 -8 -6 -4 -2 0 2 4 6
r /mm r /mm
(a) heating time is 0.5 second (b) heating time is 1.0 second
temp temp
2 20000 2 20000
19000 19000
18000 18000
4 17000 4 17000
16000 16000
15000 15000
6 14000 6 14000
13000 13000
12000
z /mm
12000
z /mm
8 11000 8 11000
10 10
12 12
14 L = 5 mm 14 L = 5 mm
t = 1.5 s t = 2.0 s
16 16
-10 -8 -6 -4 -2 0 2 4 6 -10 -8 -6 -4 -2 0 2 4 6
r /mm r /mm
(c) heating time is 1.5 second (d) heating time is 2.0 second
Fig.2 Weld arc temperature distribution and weld pool shape and size under different heating time
(a) 100% Ar shielding atmospheres (b) 75%Ar25%O shielding atmospheres

Fig3 Temperature fields in two kind of shielding atmospheres.
seen that the volume of the weld pool is increasing with the
welding time extending, but the change of arc temperature 4. Conclusions
distribution is slight. (1) The developed model is suitable to describe the
Figure 3 shows the temperature fields in two kind of behavior of the integrated welding arc and pool system.
shielding atmospheres. It can be see that the highest (2) The two-way interaction of the arc and pool
temperature decrease and the high temperature area is subsystems can be calculated by the two sub-model
contracted into the arc center. with “clear” interfaces.
216
(3) The influence of weld pool deformation on the arc supplying the thermo-physical properties of the argon
temperature fields is very small when the welding plasma.
current is 200A.
References
Acknowledgment [1] Lowke J.J., Proceedings of International Symposium on
This work was supported by the Beijing Nature Science Theoretical Prediction In Joining and welding, Editor
Foundation under grant No.3102002 which is gratefully M.Ushio, JWRI, Osaka University, 1996, 1-9
acknowledged. The author also thanks Prof Murphy A.B, [2] Choo R.T.C., Szekely J., Westhoff R.C., Metall. Trans.
CSIRO Division of applied physics, Australia, for his B ,1992, 23B: 357-369
[3] Lei Y.P., Gu X.D., Shi Y.W. and Murakawa H., Acta
Metallurgica Sinica (Chinese), 2001, No.5, 537-542.
217
Prediction of 475°C embrittlement in stainless steel welds using

†
phase field model
SAIDA Kazuyoshi * and NISHIMOTO Kazutoshi *
KEY WORDS: (475°C embrittlement) (Austenitic stainless steel) (Spinodal decomposition) (Phase field model)
(Prediction of hardening) (Computer simulation) (Solidification mode)
1. Introduction
It has been widely recognised that ferritic stainless
steels with more than 20mass%Cr are embrittled by
exposure to temperature of 673-823 K known as “475°C
embrittlement”. This embrittlement is generally
attributed to the separation of an originally single phase
to one containing an iron-rich bcc phase (D) and a
chromium-rich bcc phase (D’) caused by spinodal
decomposition. On the other hand, the chemical
compositions of the austenitic stainless steel weld metals
have been designed to contain the 3-10vol% ferritic
phase in order to reduce the hot cracking susceptibility.
The objective of the present study is to validate the
possibility of spinodal decomposition in the austenitic
stainless steel weld metal. The effect of alloying
elements in a ferritic phase, which is influenced by the
solidification mode, on the behaviour of spinodal Fig. 1 Comparison of microstructure in weld metal
between SUS316L-1 and SUS316L-2
decomposition was investigated by the computer
simulation based on the phase filed model for ternary Table 2 Analysed compositions of G-ferrite (at%)
alloy system.
2. Materials and Experimental Procedures

Austenitic stainless steels used in the present study
are three kinds of type 316L stainless steels with the
slightly different chemical compositions within a
standard. The chemical compositions of steels used were axes of the cells or dendrites, its solidification mode
shown in Table 1. In order to obtain the weld metal of being determined as FA mode. A ferritic phase is located
type 316L stainless steels, GTA melt-run welding was at cellular dendritic substructure boundaries in the type
conducted. 316L-2 weld metal, its solidification mode being
determined as AF mode. Table 2 shows the measured
Table 1 Chemical compositions of steels used (mass%) chemical compositions of a ferritic phase in the weld
metals with FA mode (type 316L-1) and AF mode (type
316L-2). Nevertheless the content of Cr in the base
metal of type 316L-1 stainless steel is higher than that of
type 316L-2, and the contents of Ni and Mo are
comparable in each base metal, the contents of Cr, Mo
3. Microstructural Analysis of Weld Metals
and Ni in a ferritic phase with AF mode are higher than
Figure 1 shows the SEM microstructures of the melt-
those with FA mode. It follows that alloying elements of
run weld metals of type 316L-1 and type 316L-2
Cr, Ni and Mo are relatively enriched in a ferritic phase
stainless steels. In case of the type316L-1 weld metal, a
with AF mode compared with that with FA mode.
vermicular or lathy ferritic phase is located mainly at the
* Dept. of Materials & Manufacturing Science,.Graduate Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
School of Eng., Osaka University, Osaka, Japan Japan
218
Prediction of 475°C embrittlement in stainless steel welds using phase field model
4. Computer Simulation of Spinodal Decomposition (D) and Cr-rich (D’) phases with the progress of ageing.
Phase Field Model of Spinodal Decomposition for Ternary In the initial stage of spinodal decomposition, Mo is
Alloys distributed along with Fe in the D phase. Then, the
The evaluation equations governing spinodal bifurcation of Mo peaks along peak tops of Cr
decomposition in the A-B-C ternary system are concentration occurs with the progress of phase
expressed as:
GG sys GG sys
decomposition. Then, Cr-rich D’ phase grows and
wc 2
wt
= L 22
Gc 2
+L 23
Gc 3
coarsens as well as slightly modulating along <100>
(1) direction with the lapse of ageing time. Mo is finally
wc 3 GG sys GG sys
wt
= L 32
Gc 2
+L 33
Gc 3
redistributed to the interface between D and D’ phases,
and surrounds Cr-rich D’ phase.
where c i is the local composition of the component i at The effects of Cr and Ni contents in Fe-Cr-Ni ternary
spatial position r (r represents a vector) and time t in the alloy on the beginning time for spinodal decomposition
microstructure. The subscript numbers i = 1, 2 and 3 were investigated. Figure 3 shows the predicted contour
refer to elements A, B and C, respectively. G sys is the of the beginning time for spinodal decomposition as the
total free energy of the microstructure, which is function of Cr and Ni compositions. The beginning time
expressed by the sum of the Gibbs energy density, the for spinodal decomposition shortens with increasing Cr
density of the composition gradient energy and the
density of the elastic strain energy. L ij is the Onsager
coefficient.
In the present study, it is assumed that the change in
hardness due to spinodal decomposition and/or 475°C
embrittlement is followed by the precipitation hardening
theory (cut-through model) proposed by Mott-Nabarro.
Effect of Alloy Composition on Spinodal Decomposition

The microstructure evolution in Fe-Cr-Mo ternary
alloy was calculated. Figure 2 shows the two-
dimensional profiles of Fe, Cr and Mo concentrations
perpendicular to the direction [001] of D phase during
isothermal spinodal decomposition at 723 K. The
original single phase is phase-decomposed into Fe-rich
Fig. 3 Contour of beginning time for spinodal

decomposition in Fe-Cr-Ni ternary alloy
composition, while it much lengthens contrarily with

increasing Ni composition. Furthermore, it takes
extremely long time to spinodal-decompose with the
chemical compositions of the alloy approaching the
spinodal line. The result is that spinodal decomposition
would be delayed in approx. half or one order of time
when Ni composition is varied in 1at%.
Prediction of Hardening due to Spinodal Decomposition

The hardening behaviour of a ferritic phase due to
spinodal decomposition was predicted. Figure 4 shows the
predicted Martens’ hardness increment 'HM of a ferritic
phase with different solidification modes during spinodal
decomposition process. The hardness of a ferritic phase
with FA mode begins to increase at the holding time approx.
5 Gs, while that with AF mode begins to increase at the
holding time as long as approx. 150 Gs. It follows that the
hardening and/or 475°C embrittlement due to spinodal
decomposition of a ferritic phase with FA mode would take
place more rapidly compared with AF mode, and that the
maximum hardness increment attained with a ferritic phase
with AF mode is slightly higher than that with FA mode.
Fig. 2 Time evolution of spinodal decomposition
calculated for Fe-40at%Cr-5at%Mo alloy
219
5. Conclusions
(1) The original single phase was phase-decomposed into
Fe-rich and Cr-rich phases with the progress of ageing.
The beginning time for spinodal decomposition
shortened with increasing Cr composition, while it
much lengthened contrarily with increasing Ni
composition.
(2) The predicted hardness of a ferritic phase with FA mode
began to increase as the holding time approx. 5 Gs,
while that with AF mode began to increase at the
holding time as long as approx. 150 Gs.
Fig. 4 Prediction of hardening in ferritic phase with

different solidification modes due to spinodal
decomposition at 561K
220
Metallurgical mechanism of ductility-dip cracking in multipass

†
welds of alloy 690
OKAUCHI Hironori *, NOMOTO Yuki *, OGIWARA Hiroyuki *, SAIDA Kazuyoshi * and

NISHIMOTO Kazutoshi *
KEY WORDS: (Alloy 690) (Multipass weld metal) (Microcracking susceptibility) (Impurity elements)
ᴾ ᴾ ᴾ ᴾ (Grain boundary segregation) (Molecular orbital calculation) (Cracking mechanism)
1. Introduction
A Ni-base superalloy, alloy 690 is highly susceptible
to ductility-dip cracking, and the primary cause of
ductility-dip cracking in the reheated weld metal of alloy
690 is likely to be the reduction of hot ductility
attributable to grain boundary segregation of impurity
elements such as P and S [1]. The objective of the
present study is to clarify the cause of the increased
ductility-dip cracking susceptibility with an increase in
the P and S contents based on a grain boundary
segregation analysis and a molecular orbital analysis of Fig. 1 Relation between (P+1.2S) in weld metal and
ductility-dip temperature range, DTR
the binding strength of the grain boundary.
2. Materials and Experimental Procedures compositional parameter of (P+1.2S) and the DTR for
The base metal used is a commercial alloy 690. all weld metals. According to the multipass weld
Several kinds of commercial filler metals (FM1-FM3), cracking test results, the critical DTR where microcracks
lab-melting filler metals (FF1-FF5) and extra high-purity didn’t occur during multipass welding could be
filler metal (EHP) were employed for comparison. The estimated as approx. 200K. It follows that the amount of
chemical compositions of base metal and filler metals (P+1.2S) in the weld metal should be limited to 30ppm
used are shown in Table 1. The ductility-dip cracking in order to prevent ductility-dip cracking in the multipass
susceptibility in the reheated weld metal was evaluated weld metal.
by the spot-Varestraint test.
4. Grain Boundary Segregation of P and S
Table 1 Chemical compositions of steels used (mass%)
Numerical Model of Grain Boundary Segregation
The numerical model of microsegregation involves
segregation during the solidification stage and
segregation/ desegregation during the cooling/reheating
stage following solidification in welding under the initial
3. Effects of P and S on Ductility-Dip Cracking

The relationship between (P+1.2S) content in the
weld metals and the DTR evaluated is shown in Fig. 1.
Open and filled symbols indicate crack-free and
Fig. 2 Schematic illustration of analysis model of
cracking in the multipass weld cracking test, respectively. microsegregation during multipass welding
There is a good linear relationship between the
* Dept. of Materials & Manufacturing Science, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Graduate School of Eng., Osaka University, Osaka, Japan Japan
221
Metallurgical mechanism of ductility-dip cracking in multipass welds of alloy 690
increased again at lower temperatures and were

saturated at constant values below about 1000 K. In the
reheating process, the P and S concentrations at the
grain boundary slightly increased during the cooling
stage in the reheating process, and afterwards changed
cyclically with each thermal cycle. The grain boundary
concentration of S during multipass welding was
relatively higher than that of P even when their initial
contents were identical. Furthermore, the P and S
Fig. 3 Calculated P and S concentrations at grain concentrations at the grain boundary slightly increased
boundary during multipass welding with an increase in the number of thermal cycles
employed. This fact suggests that grain boundary
condition of an inhomogeneous distribution formed by segregation of S as well as P would be promoted by the
solidification segregation. The solidification segregation multiple thermal cycles occurring during multipass
behaviours of P and S were calculated for pseudo-binary welding.
systems of (Ni-30%Cr-10%Fe)-P and -S. The
cosegregation effect of P with S was considered in the 5. Grain Boundary Embrittlement due to P and S
equilibrium grain boundary segregation using pseudo- Analysed by Molecular Orbital Method
ternary systems of (Ni-30%Cr-10%Fe)-P-S. The The binding strength of the grain boundary was
distribution of solutes during solidification was numerically analysed by a molecular orbital analysis
determined by the non-equilibrium solidification (DV-;ĮPHWKRG). Figure 4 schematically illustrates the
segregation theory, and that in the solid phase during FOXVWHU PRGHO XVHG LQ WKH SUHVHQW FRPSXWDWLRQ WKH Ȉ
cooling/reheating processes was calculated by the coincidence boundary of Ni consisting of 67 atoms. One
equilibrium cosegregation theory. The one-dimensional or two Ni atoms on the grain boundary were replaced by
diffusion model in a regular triangle assuming that the P or S atoms to simulate grain boundary segregation.
morphology of dendrite is basically a hexagonal prism, The binding strength of the grain boundary was
as shown in Fig. 2. evaluated from the bond order between intergranular and
Grain Boundary Segregation Behaviour of P and S intragranular Ni atoms in the near neighbourhood of P
A computer simulation was carried out with the peak and S atoms. The calculated bond orders of Ni atom at
temperatures in the 2nd and 3rd cycles being 1200 K. the grain boundary for different segregation situations
Figure 3 shows the relation between the elapsed time in are shown in Fig. 5. Ni 67 indicates the non-segregated
multiple welding thermal cycles and the calculated P and situation, Ni 66 X 1 and Ni 65 X 2 , Ni 65 X 1 Y 1 (X, Y=P, S)
S concentrations at the grain boundary. In this figure, the indicate the segregated situations where one and two
calculated P and S concentrations without considering intergranular Ni atoms were replaced by an X and/or Y
the cosegregation effect (i.e., “independent segrega- atom, respectively. When P and S were segregated at the
tion”) are also depicted. The P and S concentrations at grain boundaries, the bond orders of the Ni atoms were
the grain boundary allowing for cosegregation were reduced compared to the non-segregated situation, and it
slightly reduced compared with those in independent decreased with an increase in the number of segregated
segregation because of the competitive effect between P P and S atoms. The bond orders of the Ni atoms when S
and S. However, similar changes can be seen in the was segregated to the grain boundary were lower than
grain boundary concentrations for both situations. those for P segregation. However, the fact that the
Namely, in the solidification process, the P and S calculated bond order of Ni atom in Ni 65 P 1 S 1 ranked
concentrations in the liquid phase increased with the between Ni 65 P 2 and Ni 65 S 2 prevented the confirmation
progress of solidification, and were rapidly reduced to of any discernible effect of cosegregation of P with S in
their equilibrium concentrations (desegregation) when the present analysis.
the weld metal was cooled down. However, they
Fig.4 Schematic illustration of cluster model used Fig.5 Calculated bond order between Ni atoms for
(molecular orbital analysis by DV-XD method) different grain boundary segregation scenarios
222
7. Conclusions
6. Mechanism of Ductility-Dip Cracking in Multipass (1) A numerical analysis of the segregation behaviours of P
Weld and S revealed that these elements were cosegregated at the
A grain boundary segregation analysis revealed that grain boundary during multipass welding. P and S
P and S (especially S) were segregated to the grain concentrations at the grain boundary slightly increased with
boundary in the weld metal during multipass welding. A an increase in the number of thermal cycles applied.
molecular orbital analysis suggests a possibility that (2) A molecular orbital analysis suggested a possibility that
grain boundary segregation of P and S leads to grain grain boundary segregation of P and S led to grain
boundary embrittlement. It follows that the ductility-dip boundary embrittlement.
cracking in the reheated weld metal of alloy 690 would
References
be dominantly caused by the embrittlement of grain [1] K.Nishimoto, K.Saida, H.Okauchi and K.Ohta : Sci. and
boundaries resulting from the imbalance between Technol. of Welding and Joining, 11-4 (2006), p.462-470.
intergranular strength and intragranular strength at high
temperature attributable to grain boundary segregation
of impurity elements such as P and S.
223
Interfacial reaction between Sn-3.0Ag-0.5Cu solder / Co-P plating

†
and Ni-Co-P plating
DAITO Tomoya *, NISHIKAWA Hiroshi **, TAKEMOTO Tadashi **,

MATSUNAMI Takashi ***
KEY WORDS: (Lead-free solder) (Intermetallic compound) (Reaction layer) (Under bump metallurgy)
(Co-P plating) (Ni-Co-P plating)
1. Introduction the center of the substrate and activated flux (0.01 ml) was
In response to health and safety concerns, lead-free dropped on the solder. The test specimen was put into a
soldering has become a popular technology in electronics radiation furnace in a nitrogen atmosphere and heated
packaging. Compared with the lead-containing solders, Sn- according to the temperature rise profile shown in Fig. 2.
3.0mass%Ag-0.5mass%Cu (SAC, all mass% unless The reflow peak temperature was 513 K with the sample
specified otherwise) solder widely used in Japan has a above 490 K for 115 s. After soldering, the spreading area
relatively low impact reliability owing to the solder alloy of the solder on the UBM was measured by using the
hardness that induces a high stress concentration at the optical microscope (OM). Three tests were conducted to
interface. In general, there is a correlation between the obtain an average value for each specimen. Then,
impact reliability and the morphology and thickness of the specimens were cut and the cross-section of the specimens
reaction layer formed at the solder/under bump metallurgy was polished to observe the interface between the solder
(UBM) interface. The most common UBM is electroless and UBM. The reaction layer at the interface was observed
Ni-P plating over copper pad. Electroless Ni-P acts as a by scanning electron microscope (SEM).
diffusion barrier layer between the copper and the solder.
However, due to nickel diffusion, P-rich layers form at the 3. Result and discussion
interface between the solder and electroless Ni-P. Solder A spreading test was carried out to examine the
joint failure is related to the growth of these layers and to wettability of solders on UBMs and to clarify the interfacial
their brittleness and affects the mechanical reliability of reaction between the solder and UBMs after soldering. The
joints. Recently, a new composition of UBM is proposed as wettability of solder was experimentally assessed by
diffusion barrier1-4). For instance, Magagnin et al. reported measuring the spreading area of solders on the UBMs.
that electroless Co–P strongly limits interdiffusion and
intermetallic compounds formation as compared with the
electroless Ni–P with Sn-Ag-Cu alloy. Furthermore, in the
Co-P samples, P-rich layers did not form at the interface4).
It is important to investigate the relationship between
morphology of reaction layer and UBM. This study aims to
clarify the effect of Co-P and Ni-Co-P on the morphology
of reaction layer formed at the solder/UBM interface.
2. Experimental
SAC solder (0.3 g) was used in this study. Electroless
Co-P(Au) (3.1 Pm) and electroless Ni-Co-P(Au) (5.2 Pm)
finished Cu plates on FR-4 PCBs (25.0×25.0×1.6 mm)
were prepared as UBM. Electroless Ni-P(Au) (5.0 Pm)
substrate was also used as a reference substrate. These
substrates were plated with gold to avoid oxidation of the
cobalt and nickel surface.
The experimental procedure is shown in Fig. 1. The Fig. 1 Experimental procedure of this study.
substrate was immersed in 4% HCl solution for 120 s and
then rinsed with deionized water. Then, solder was put on
*** Okuno Chemical Industries Co., Ltd., Osaka, Japan
224
Interfacial reaction between Sn-3.0Ag-0.5Cu solder / Co-P plating and Ni-Co-P plating
Fig. 4 Effect of UBMs composition on spreading area.
Fig. 2 Temperature profile in reflow soldering.

Figure 3 shows the appearance of a typical spreading
test specimen after soldering. It is clear that the spreading
area of solder on electroless Co-P was greater than that on
electroless Ni-Co-P and Ni-P. Figure 4 shows the results of
spreading area measurements for SAC solder on the three
types of UBMs. The spreading area of the solder on the
electroless Co-P was larger than that of the solder on the
electroless Ni-Co-P and Ni-P. This results show that the
electroless Co-P had better wetting characteristics than the
electroless Ni-Co-P and Ni-P.
Then, the morphology of the reaction layer at the
interface was observed by SEM. Figure 5 shows the SEM
image of the reaction layer at the interface between SAC
solder and UBMs after soldering. It is clear from Fig. 5 that
the morphology of the reaction layers at the interface Fig. 5 SEM images of reaction layer at the interface
changes depending on the UBMs. While the layer-like IMC between SAC solder and UBMs after soldering.
with 1.6 Pm in average thickness was formed at solder/Ni-P a) electroless Co-P, b) electroless Ni-Co-P, c) electroless
interface, in the electroless Co-P sample, the thin Ni-P
continuous layer attached to electroless Co-P layer and the
fine needle-like IMC in contact with the solder was 4. Conclusion
observed at the solder/Co-P interface. In the electroless Ni- This study aims to clarify the effect of electroless Co-P
Co-P sample, the thin continuous layer attached to and Ni-Co-P on the morphology of the reaction layer
electroless Ni-Co-P layer and the large needle-like IMC formed at the solder/UBM interface.㻌 The results obtained
with more than 10 Pm thickness in contact with the solder are summarized as follows.
was observed.
(1) The spreading area of the solder on the electroless Co-
P was larger than that of the solder on the electroless
Ni-Co-P and Ni-P. These results show that the
electroless Co-P had better wetting characteristics than
the electroless Ni-Co-P and Ni-P.
(2) While a layer-like IMC was formed at the solder/Ni-P
interface, fine and large needle-like IMCs were formed
at the solder/Co-P and solder/Ni-Co-P interface,
respectively.
References
[1] Chwan-Ying Lee et al., Thin Solid Films, 239, (1994), pp.93-
98.
[2] Yi-Hsiang Chao et al., Metallurgical and Materials
Transactions A, 39, (2008), pp.477-489.
[3] Takashi Yamamoto et al., Materials Transactions, 46, (2005),
Fig. 3 Appearance of typical spreading test specimen after pp.2406-2412.
[4] L. Magagnin et al., Electrochimica Acta, 50, (2005), pp.4621-
soldering. a) electroless Co-P, b) electroless Ni-Co- 4625.
P, c) electroless Ni-P
225
Formation of reaction layers at anodically-bonded metallc

†
glass/silicate glass interfaces
TAKAHASHI Makoto *, WATATANI Yuuki **, IKEUCHI Kenji *, KIMURA Hisamichi ***
and INOUE Akihisa ***
KEY WORDS: (Anodic bonding) (Metallic glass) (Silicate glass) (Joinability) (Microstructure)
1. Introduction microscopy (TEM).

Anodic bonding is a method for bonding conductive
materials to silicate glass containing alkali ions by applying 2. Experimental
a D.C. voltage of 100-1000 V between them with the Experimental materials are zirconium-based metallic
conductive material side anodic. With adequate heating glass (Zr 55 Cu 30 Al 10 Ni 5 ) and silicate glass, soda-
thermal diffusion of alkali ions in silicate glass is activated. aluminosilicate glass Matsunami 801 and soda-potassia
Under the influence of the electric field induced by the glass Matsunami 7622. Linear expansion coefficients of the
applied voltage, these ions drift toward the cathode side, metallic glass , 801 glass, and 7622 glass are ~10x10-6 /
and an alkali ion depletion layer forms in the silicate glass K 6) , 10.7x10-6 / K and 12x10-6 / K 7), respectively.
near the joint surface. This layer has a strong negative Crystallization temperature of the metallic glass is ~750
charge because of the presence of non-bridging oxygen K 8). Metallic glass was provided as plates 2 mm thick and
anions that lose their bonds with the alkali ions. A Coulomb 25 mm square. One side of each plate was finished flat and
force acting between this negative charge and the positive glossy by mechanical grinding and buffing. After that these
charge appearing at the surface of the anode conductor plates were cut into pieces 10 mm square. Buffed sides of
brings the silicate glass and the conductor into intimate these pieces were used as faying surfaces. The silicate glass
contact, and a permanent bond is achieved by the oxidation was provided as disks of 1 mm in thickness and 25 mm in
of the surface of the conductor by oxygen derived from the diameter. Both sides of the disks were finished by
alkali ion depletion layer in the silicate glass 1). Anodic mechanical grinding and polishing.
bonding achieves direct bonding of conductor to silicate The procedure of anodic bonding was as follows.
glass without intermediates such as solder or adhesive, and The silicate glass piece was placed on the negative
it is workable at a temperature low enough not to cause electrode plate. The surface of the silicate glass piece
softening of the silicate glass 2). These features make anodic contacting the electrode plate was painted with a carbon
bonding a powerful method for precise bonding of conductive coating (Aquadag: colloidal graphite) in order
conductors to silicate glass. Anodic bonding is commonly to obtain a uniform electric potential at the surface. The
used in sealing of silicon micro devicesύfor example, metallic glass piece was placed on the silicate glass piece
sensors for pressure or acceleration. with the faying surface down, and connected with the
Bulk metallic glasses (BMG) have many attractive positive electrode. These specimens were heated to a
features, such as high strength, low Young’s modulus, and predetermined bonding temperature (T b ) by surrounding
high corrosion resistance 3, 4). And they have excellent graphite heaters in an pure argon atmosphere of 0.12 MPa.
compatibility with microfabrication because of their Bonding temperatures adopted for 801 glass joints were
isotropic nature 5). These features make BMGs promising 483 K, 523 K, and 563 K, and those for 7622 glass joints
materials for microsensors or micromachines. It is desirable were 523 K, 564 K, and 603 K. After the temperature of
to establish anodic bonding of metallic glass in order to specimens settled, a bonding voltage of 500 V was applied
realize micro devices made of metallic glass. In this study, to the specimens for a predetermined bonding time (t b ) with
anodic bonding of zirconium-based metallic glass to two the metallic glass side anodic. The electric current that
different kinds of silicate glass, soda-aluminosilicate glass passed through the specimens (i b ) was monitored during the
Matsunami 801 and soda-potassia glass Matsunami 7622 application of the voltage. After the voltage application,
was tried with various bonding temperatures and voltage specimens were cooled slowly in the bonding apparatus.
application times. These silicate glass materials have In order to evaluate the progress of bonding, the
thermal expansion coefficients near to that of the used appearances of joint interfaces of the obtained joints were
metallic glass. Joint interfaces in the obtained joints were examined visually through the silicate glass. Microstructure
examined by appearance and the microstructure around the around the joint interfaces wasᴾ investigated closely by
joint interface was observed by transmission electron TEM. Thin foil specimens for TEM were cut from the
** Graduate School, Osaka University, Osaka, Japan Japan
*** Institute of Materials Research, Tohoku University
226
Formation of reaction layers at anodically-bonded metallc glass/silicate glass interfaces
5 mm 5 mm
tb = 150 s tb = 300 s tb = 600 s tb = 150 s tb = 300 s tb = 600 s tb = 1200 s

Partially contact full contact full contact Partially contact full contact Partially contact Separated
(a) Zr-based metallic glass / 801 glass joint, Tb = 523 K (b) Zr-based metallic glass / 7622 glass joint, Tb = 563 K
Fig. 1 Appearances of the metallic glass / silicate glass anodically-bonded interface.
anodically-bonded joint across the bond interface with the anodic bonding. At a higher temperature drift of alkali ions
focused ion-beam (FIB) system. The FIB system used was in silicate glass with voltage application is enhanced more
Hitachi FB-2000A, and TEM observation was performed strongly, and buildup of the alkali ion depletion layer and
by JEOL JEM-2010 operating at an accelerating voltage of consequently the bonding process become quicker. On the
200 kV. other hand, anodic bonding of metallic glass to 7622 glass
showed a peculiar progress (Fig. 1(b)). At T b = 563 K, the
3. Results and Discussions 7622 glass joints once achieved intimate contact of almost
In Fig. 1 are shown the appearances of the metallic all the joint interface with the voltage application for 300 s.
glass silicate glass anodically-bonded interfaces. The 801 But the joint interfaces were separated again with longer
joints shown in Fig. 1 were bonded at 563 K, and the 7622 voltage application. At a higher T b of 603 K, all the
joints were bonded at 563 K. In the joint interfaces, the metallic glass / 7622 glass joint interfaces remained
areas in which intimate contact of the metallic glass to the separated with the voltage application from 75 s to 300 s.
silicate glass showed a little dark tone, and the areas in Microstructures around the joint interfaces in a 801
which metallic glass was separated from the silicate glass glass joint anodically-bonded at 563 K with voltage
showed bright tone with Newton fringes. (In the 7622 glass application for 300 s and a 7622 joint bonded at 523 K with
joint of t b = 1200 s all the joint interface was separated. voltage application for 4800 s were observed by TEM. In
The appearance was oberved without 7622 silicate glass.) Fig. 2 is shown the microstructure of the joint interface in
As is shown in Fig. 1(a), in 801 glass joints the ratio of the the 801 joint. Reaction products formed two layers at the
intimate contacting area increased with the voltage joint interface. One is a crystalline layer ~70 nm thick
application time, and progress of the bonding became faster contacting the metallic glass, and another is an amorphous
at higher bonding temperatures. This is a usual tendency in layer ~20 nm thick contacting the silicate glass. Chemical
analysis by energy dispersion X-ray Spectroscopy (EDS)
(a) Metallic glass (b) showed existence of high-concentrations of oxygen in these
layers. Therefore, these reaction layers were thought to be
of oxide formed by reaction of elements from the metallic
0 glass with oxygen from the silicate glass in anodic bonding.
And Cu concentration in the amorphous oxide layer was
Reaction
801 silicate glass very low. The microstructure around the joint interface in
layers
the 7622 joint is shown in Fig. 3. Reaction products were

200 nm
found at the joint interface also. But the reaction layer in
the 7622 joint formed a single layer ~40 nm thick. This
Fig. 2 Microstructure around the metallic glass / 801 layer contained some crystals, but mainly formed of
silicate glass anodically-bonded joint interface. amorphous. EDS analysis showed high oxygen
Bright-field image (a), and SAD pattern taken from the concentration and low Cu concentration in the reaction
area indicated by the circle in the image a (b). layer.
Results from TEM observation suggest that the peculiar
(a) (b) progress of metallic glass / 7622 glass is concerned with the
Metallic glass formation of Cu-poor amorphous oxide layer at the joint
interface.
0
References
Reaction
[1] G. Wallis and D. I .Pomerantz: Field Assisted Glass-Metal

7622 silicate glass
layer
Sealing, J. Appl. Phys., 40(1969), 3946-3949

200 nm [2] K. Hiller, R. Hahn, C. Kaufmann, S. Kurth, K. Kehr, T.
Gessner, W. Doetzel, M. Wiemer and I. Schubert: Low
Fig. 3 Microstructure around the metallic glass / 7622 Temperature Approaches for Fabrication of High Frequency
Microscanners, Proceedings of SPIE - The International
silicate glass anodically-bonded joint interface.
Society for Optical Engineering, 58-66 (1999), 3878
Bright-field image (a), and SAD pattern taken from the
area indicated by the circle in the image a (b).
227
[3] Z. Zhang, V. Keppens and P. K. Liaw, Y. Yokoyama and A. pp. 1-6.

Inoue: Elastic properties of Zr-based bulk metallic glasses [6] T. Terajima, K. Nakata, K. Hisamichi and A. Inoue:
studied by resonant ultrasound spectroscopy, Journal of Development of W-Reinforced Zr-based Metallic Glass,
Materials Research, 22(2007), pp. 364-367 Materials Transactions, JIM, 50(2009), pp. 1322-1325.
[4] S. Pang, T. Zhang, H. Kimura, K. Asami and A. Inoue: [7] “Denshi Buhin, Kougaku Buhinyou Glass”, Matsunami Glass
Corrosion behavior of Zr-(Nb-)Al-Ni-Cu glassy alloys, Ind. Ltd. (Products catalog)
Materials Transactions, JIM, 41(2000), pp. 1490-1494. [8] H. Kato, T. Hirano, A. Matsuo, Y. Kawamura and A. Inoue:
[5] P. Sharma, N. Kaushik, H. Kimura, Y. Saotome and A. Inoue: High strength and good ductility of Zr 55 Al 10 Ni 5 Cu 30 bulk
Nano-fabrication with metallic glass – an exotic material for glass containing ZRC particles, Scripta Materialia, 43(2000),
nano-electromechanical systems, Nanotechnology, 18(2007), pp. 503-507.
228
The dissymmetry of friction stir welding joints and variable

polarity plasma arc welding joints study†
CHEN Shujun*, WANG Long*, YU Yang*
KEY WORDS: (FSW) (VPPAW) (nano-indentation experiment) (Half-leaf”zone), (dissymmetry)
1. Introduction
Recently, because of aluminum’s light weight, it has 3. Results
been considered an energy-saving structural material in At first Keller reagent is used to corrode the specimens,
advanced applications. In addition, aluminum is an easily second the specimens are washed by the 4% of the nitrate
saved resource because it can be recycled, and thus can be acid, at last, the specimens are observed by optical
expected to be an environmental friendly metallic material. microscope. FSW joint can be divided into the following
One such application would be its use in automobiles, several zones(see Fig. 1) : A: ḛ Half-leafḜ zone, B:zone
which would facilitate transportationύ numerous similar above WNZ, C:TMAZ, D:WNZ, E:boundary of AS,
examples could be cited in support of employing aluminum F:boundary of RS, G:HAZ, H:Base metal.
as a structural material[1]. In addition, because aluminum
has large thermal conductivity, large specific heat, quick
thermal conductivity and large linear expansion coefficient,
it easy to form an air hole during the welding[2]. So, welding
Aluminum welding is a difficult problem. Two kinds of
mature approach are Friction Stir Welding(FSW) and
Variable Polarity Plasma Arc Welding(VPPAW).
Therefore, it is important to compare the microstructure and Fig. 1 Macro Map of FSW joint
micro-hardness of the Friction stir welding joints and
Variable polarity plasma arc welding joints. The regions are observed under the microscope. And
Therefore, the friction stir welding and the variable the regions show different characteristics, and asymmetry
polarity plasma welding are compared, and the study is features of the FSW joints
based on differences of the microstructure and mechanical
properties of these two methods. A nano-indentation
experiment is used to test the hardness in some narrow and
small zones, such as the ḛHalf-leafḜzone . The nano-
indentation method is flexible and accurate and provides a
powerful tool to test the hardness of weld joints. It is the
basic work for the hybrid welding has laid a solid
ίaὸḛHalf-leafḜzone corroded ίbὸḛHalf-leafḜ zone corroded
foundation. by Kellar acid by aqua regia
Fig. 2 microstructure of ḛHalf-leafḜzone
2. Experimental procedures
Specimens of the FSW and VPPAW joints are Figure 2(a) shows the ḛHalf-leafḜzone, the zone is
obtained from 6mm 2219 aluminum alloy plate. By using under strong pressure. ḛ Half-leaf Ḝ zone can be shown
an optical microscope, the microstructure of welding joint clearly by use of aqua regia, and this area can be corroded
is observed. The procedures are sampling, polishing,
easier than other zone(see. Fig. 2(b)).
corrosion and observation. The cross sections of
metallographic specimens are polished, etched with
Keller’s reagent (1 ml hydrochloric acid,1.5 ml nitric acid,
PO K\GURÀXRULF DFLG DQG PO ZDWHU DQG washed by
4% of the nitrate acid. At last specimens are observed by
optical microscopy. WhDW’s more, aqua regia is used. By
using SEM, microstructure is very clearly seen. After these ίaὸḛHalf-leafḜzone ίbὸbound ofḛHalf-leafḜzone ίcὸnear theḛHalf-leafḜ
experiments, a Nano-indentation test is done. All the tests zone(TMAZ)
were conducted on a Nano Indenter G200. Fig. 3ᴾ result of ḛHalf-leafḜzone by Scanning electron
microscopy
* Beijing University of Technology, China Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
229
The dissymmetry of friction stir welding joints and variable polarity plasma arc welding joints study
Scanning electron microscope tests are done on

ḛHalf-leafḜzone, ș-phase grown up and gathered together
from ḛ Half-leaf Ḝ zone to TMAZ by observing. 2219
aluminum alloy used in solid solution strengthening. With
WKH SUHFLSLWDWLRQ RI ș-phase, the effect of solid solution
strengthening can be weak. So the hardness of TMAZ is
lower than ḛHalf-leafḜzone. See, Fig. 3.
According to the microstructure observed by optical ίeὸ100X weld
microscope, the indentation experiments are arranged. Test Fig. 7 microstructure of keyhole-mode welding joint
points of Nano-indentation test for the FSW joints as shown
in Fig. 4. Figure 7(a-d) are shown HL and HAZ by Metallo-
graphic microscope at 40 times. It is worth noting that
keyhole-mode welding joint is asymmetric. The grains in
two HAZ grow up differently. The grains in left HAZ(see
Figure 7(a)) grow up obviously. But Figure 7(d) shows that
right grains don’t change obviously after thermal cycling,
and these grains still retains the rolling direction of the base
Fig. 4 distribution of Nano-indentation test point on material. Dissymmetric microstructure is decided by
FSW joint dissymmetric heat input in this area. Because VPPAW uses
vertical position, and it has strong power of arc, so the heat
The hardness of ḛHalf-leafḜzone has been greatly input is dissymmetric.
improved and increased the 21.5% of hardness. This is the Test points of Nano-indentation test for the VPPAW
severely corroded area which is used aqua regia. The grains joints as shown in Fig. 8.
of ḛHalf-leafḜzone are slightly larger than the grains of
WNZ, and less than the surrounding. The smaller grains are
brought about the higher hardness.
The microstructure of VPPAW joint, which is used
2219 aluminum alloy as base material and 2319 aluminum ίaὸkeyhole ίbὸmelting-keyhole
alloy as filling material, is observed. VPPAW joint can be Fig. 8 distribution of nano-indentation test point on
divided into the following several zones (see Fig. 5); VPPAW joint
A:weld, B:HAZ, C:FL, D:BM. There are two methods for
forming VPPAW joints: keyhole-mode variable polarity
plasma arc welding (see Fig. 5) and melting-keyhole
variable polarity plasma arc welding (see Fig. 6).

Fig. 9 result of nano-indentation Fig. 10 result of nano-
test on melting-keyhole VPPAW indentation test on keyhole
joint VPPAW joint

Fig. 5 keyhole-mode VPPAW Fig. 6 melting- keyhole
As shown in Fig. 9, reasonable welding process makes
joint VPPAW joint
the performance of VPPA obvious symmetry. Hardness of
weld is slightly lower than the base metal. Weld nugget has
a part of dendrites, rather than completely composed of
equiaxed grains. There are satisfactory aluminum welded
joints, but not all VPPAW processes can achieve
satisfactory results. For VPPAW includes keyhole VPPAW
and melting-keyhole VPPAW. The peak hardness is found
ίaὸFL ίbὸHAZ in HL, so the property of the weld is asymmetry in the
whole joint (see Fig. 10). It has not only relationship with
the high mobility of melt metal, because keyhole VPPAW
uses large energy, but also VPPAW is generally vertical
position welding.
4. Conclusions
In this paper, two welding methods which are FSW
ίcὸHL ίdὸHAZ and VPPAW are used to weld 2219 aluminum alloy. Finally
both the FSW and VPPAW will appear non-symmetrical
welded joints, such non-symmetry is reflected in the
microstructure morphology and performance.
230
(1)In the FSW joints, defects in onion rings, the VPPAW, VPPAW joint can be adjusted to symmetry and
different of forward side and backward side microstructure results of satisfactory welding. Not only symmetrical
and ḛHalf-leafḜzone have made FSW joints have a strong microstructure is obtained, but also good properties of
dissymmetry. The dissymmetry in welded joints is brought welded joints are obtained by using the right filling material.
about the dissymmetry in joint performance. The
dissymmetry in FSW joint can not be suppressed due to the References
nature of the mixing head and the process of FSW, it is [1] Tomotake Hirata ,Taizo Oguri, et al. Materials Science and
Engineering A456 (2007) 344–349
difficult to over come.
[2] Huang Wangfu. Aluminum and aluminum alloy welding
(2)The problems about dissymmetry are also present guide.Chang Sha: Hunan Science and Technology Press,2004
in the VPPAW joint. However by changing the form of
231
Industrial application of welding temperature field and distortion

visualization using FEA†
,
THATER Raphael*, PERRET William**, SCHWENK Christopher* **, ALBER Uwe ***
,
and RETHMEIER Michael* **
KEY WORDS: (Numerical welding simulation) (Temperature field) (Distortion) (Industrial application) (Auto-
motive assembly)
1. Introduction to the AUDI-Space-Frame (ASF®) (Fig. 1) of the prede-

The non-uniform heat input during the welding process cessor of the current AUDI A8 and consists of a cross-
leads to problematic permanent deformations of welded member (1600 mm x 180 mm x 80 mm) and four inserts all
parts. The control of these welding distortions is, with the made of AlMgSi alloy. Two MIG welds were applied per
absence of the knowledge of the fundamental mechanisms insert, giving a total of eight welds. The entire weld seam
responsible for these deformations, an extremely time and length is approximately 500 mm.
cost consuming iterative “trial-and-error” optimization For the case study, measurements of transient tempera-
process. The visualization of the involved physical pheno- ture cycles and distortion fields have been done. The tem-
mena, like temperature and distortions, is an indispensable perature cycles have been obtained with thermocouples and
tool to clearly identify these mechanisms in order to adapt the transient 3D distortion field has been measured with an
the welding parameters and clamping conditions target- optical 3D analysis system, ARAMIS. The evaluable mea-
oriented. Both experimental and virtual methods exist to surement field of this optical analysis was restricted by the
obtain these physical data, however the possibilities to experimental set-up like clamping devices, robot arm and
visualize them with experimental methods are laborious, limitations of the measurement equipment to a quarter of
expensive and limited in their application. Welding simula- the assembly.
tion using finite element analysis (FEA) offers many bene- The execution of the experiments with the measurement
fits and has a great potential to reduce the experimental equipment, e.g. CCD cameras and spot lights, is not possi-
effort. Nevertheless, the industrial application of welding ble in a real production line. Hence, the experiments were
simulation is not yet established widely because of reserva- executed at the Federal Institute for Materials Research and
tions regarding the computation costs and the resulting Testing (BAM), Berlin. For this purpose a clamping fixture
accuracy for instance. equivalent to the real clamping device was designed. A
In this paper, the results of a case study for a welding more detailed description about the experimental set-up is
simulation with an industrial background are presented. A given in [1].
welded assembly from the automotive industry has been
investigated with numerical and experimental methods. A 3. Numerical set-up
comparison between both methods demonstrates the poten- The simulation results presented in this paper have been
tials of welding simulation in terms of visualization. Fur- done with the commercial welding simulation software
thermore, the numerical results reveal the possibilities of SYSWELD™ 2009 on a fast desktop PC (Intel Core i7
current resources regarding calculation time and result 950@3 GHz and 12 GB RAM) with a Linux operating
accuracy of an industrial applied welding simulation. system. The mechanical calculation time for the investi-
gated 150.000 nodes large FE-model is approximately 15 h,
2. Welded assembly and experimental set-up so the simulations can be done overnight, which is a rea-
The welded assembly investigated in this work belongs sonable time frame.
Assumptions and simplifications according to the cur-
rent state of the art were assumed to run the simulations. A
key assumption is the reduction of the complex real physi-
cal welding phenomena to a phenomenological heat source
model. The parameters of this heat source have to be cali-
brated iteratively by an adjustment of the numerical calcu-
lated temperature field to match the measurements of the
Fig. 1 Investigated assembly and its position in the A8 thermocouples and cross sections. In this study, a moving
AUDI-Space-Frame (ASF®). volumetric heat source with a double ellipsoidal distribution
† Received on November 1, 2010 Transactions of JWRI is published by Joining and Welding
* Fraunhofer IPK, Berlin, Germany Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** BAM, Federal Institute for Materials Research and Testing, Japan
Berlin, Germany
*** AUDI AG, Neckarsulm, Germany
232
Industrial application of welding temperature field and distortion visualization using FEA
proposed by Goldak [2] has been used to describe the MIG- fied. The welding simulation therefore offers significant
welding process. After calibration of this phenomenological benefits in terms of visualization in comparison to experi-
heat source, the simulated temperature distribution is in best mental methods. Nevertheless, an advantage of the experi-
agreement with experimental data. mental observation is the direct measurement of the real
The necessary temperature dependent material proper- component behavior. The result quality of a welding simu-
ties of an AlMgSi alloy were taken from [3]. Softening lation, however, is highly dependent on the accuracy of the
effects occurring in the heat affect zone of a T6 tempered calibrated temperature field and the chosen assumptions
aluminum alloy are taken into account using the micro- and simplifications.
structure model developed by Leblond [4]. The parameters The result accuracy of this study is illustrated in Fig. 3
of this model were calibrated against hardness measure- as a comparison of the numerical and experimental tran-
ments across a weld seam of the actual alloy. sient distortion behavior at point A. Qualitatively, the cha-
The calibrated temperature distribution is used as an racteristics of the welding distortions are well reproduced
input for the subsequent mechanical calculation, which by the simulation. Quantitatively, the calculated distortion
determines the distortions according to the calculated tem- is approximately 60 % higher than the measured one. Con-
peratures. The mechanical boundary conditions were ap- sidering the simplifications and assumptions of the simula-
plied to the experiments equivalent places and removed at tion model the result accuracy is reasonable.
equivalent times. Orthotropic elastic constraints were used
to reproduce the clamping conditions. It should be noted
that, in contrast to the production, in this study the assem-
bly was not fully unclamped. One side of the crossmember
was clamped over the entire measurement period to sup-
press rigid body motions and thus enable the direct compar-
ison of experimental and numerical results at defined refer-
ence points.

The calculated distortions according to the calibrated
temperature field are shown in Fig. 2 as a contour plot of
the entire assembly with a magnification factor of 25. In
addition to the shown distortions many further physical data
can be visualized flexible at the surface or in the inside of
the investigated part for each recorded time step by a cali-
brated welding simulation without any problems or restric-
tions.
Fig. 3 Comparison of calculated and measured transient
distortions at Point A.
5. Conclusions
As shown in the previous section the increasing compu-
tational power enables us to run a 3D nonlinear transient
welding simulation for a large industrial geometry in a time
frame that allows a widely industrial application of welding
simulation. In this case, the calculation could be done over-
night on a desktop PC.
Fig. 2 Simulated distortion distribution (magnification fac- Finally the results of this study show that the calculation
tor: 25). of complex and large industrial parts with good result accu-
racy and a reasonable calculation time is possible. Welding
In contrast to that, the experimental visualization of simulation, therefore, has a great potential with its strengths
many of these physical data is very complex, restricted or in visualization and the specific examination of parameter
even impossible. Clamping devices, welding robots and the influences to reduce experimental effort within a target-
welding process itself limit an observation during the weld- oriented distortion optimization in industrial environments.
ing process to small sections. An experimental visualization However, additional research is needed with respect to the
of the entire assembly is usually possible only for un- time-to-solution (e.g. automatic heat source adjustment and
clamped conditions before and after the joining process. meshing) and the user-friendliness of the software in order
Furthermore, the numerical approach offers, in contrast to become even better suited to industrial requirements.
to experiments, the opportunity to examine the influences
of individual parameters by an uncoupled parameter varia- The conclusions of this study are summarized as follows.
tion, so that the fundamental mechanisms responsible for (1) A welded assembly from the automotive industry has
the deformations of welded parts can be clearly identi- been investigated with experimental and numerical
233
methods. References
(2) The results of the simulations show that current re- [1] W. Perret, R. Thater, U. Alber, C. Schwenk, M. Rethmeier:
sources allow an industrial applied welding simulation Case study for welding simulation in the automotive industry,
with good result accuracy and reasonable calculation IIW-Doc. SC-Auto-37-10 (2010).
times. [2] J. Goldak, A. Chakravarti, und M. Bibby: A new finite element
model for welding heat sources, Metallurgical Transactions B
(3) Compared to experimental methods the flexibility of
15B (1984), pp.299-305.
welding simulation offers great advantages in terms of [3] SYSWELD™ 2009: Material Database, ESI Group.
visualization. Many physical data can be visualized [4] J. B. Leblond and J. Devaux: A new kinetic model for
without any problems and restrictions. anisothermal metallurgical transformations in steels including
effect of austenite grain size, Acta Metallurgica 32 (1984), pp.
137-146.
234
Prospective design of weld joint between first and side walls in

the test blanket module for ITER†
NAKAMURA Shinichiro*, SERIZAWA Hisashi**, TANIGAWA Hiroyasu***,

MURAKAWA Hidekazu**
KEY WORDS: (Welding residual stress) (Electron beam welding) (Hot isostatic pressing) (Finite element
method) (Cooling channel) (Test blanket module)
1. Introduction The welding conditions were basically decided from the

Recently, in the collaboration with seven members, the experiment and other two parameters (heat source model
international thermonuclear experimental reactor (ITER) and thermal efficiency), which cannot be directly
has been constructed at Cadarache in France as the world’s determined in the experiment, were assumed according to
largest experimental fusion facility [1]. In current design of our previous studies [3]. Namely, the homogeneous heat
the Japanese test blanket module for ITER, the water source model, whose shape was T-type, was employed and
cooling channels have to be installed in the first and side the thermal efficiency was set to 0.7. Figure 1 shows the
walls and these walls are planned to be joined by electron welding residual stress distribution parallel to the weld line
beam (EB) welding. at a cross sectional plane in the middle of the weld line, and
The size of cooling channels is 8 mm square while the the stress beside the cooling channels is also plotted as
thickness of first wall is 25 mm in current design, and such shown in Fig. 2. From these figures, it was found that large
first wall is planned to be fabricated by using hot isostatic tensile residual stress over 500 MPa was generated on the
pressing (HIP) method [2]. On the other hand, the cooling surface of the cooling channels when the distance from
channels are planned to be located near the EB welding and weld line to cooling channels was 10 mm. On the other
it is considered that the EB welding would affect the hand, the residual stress was changed to be compressive
deformation of cooling channels and the residual stress at when that was 16 mm. So, in order to reduce the risk of
the surface of cooling channels. Sometimes, there might be SCC, it is desirable for the location of weld line to be more
a risk of stress corrosion cracking (SCC) at the surface of than 16 mm apart from the surface of cooling channels.
cooling channels because of the tensile residual stress on
the surface. Case 1 (10mm) Case 2 (12mm)
So, in this research, for the purpose of decreasing the z -10 0 (weld line) -12 0 (weld line)
risk of SCC, the modification of the current design based on x x
45
the welding residual stress was studied by using thermal
elastic–plastic finite element method (FEM). Also, the
prospective design proposed by the above research was
examined by comparison between current and prospective [MPa]
designs.
2. Analyses by Simplified Models 0

It is desirable to reduce the size of cooling channels for
controlling the risk of SCC, but this cannot be realistic Case 3 (14mm) Case 4 (16mm)
z -14 0 (weld line) -16 0 (weld line)
concerning the effect of cooling. On the other hand, a x x
position of EB weld joint between the first and side walls 45
seems to be slightly movable because the first wall is
planned to be fabricated by HIP method. So, in this
research, the modification of the current design was studied
by focusing on the distance from weld line to cooling
channels in the first wall. Then four simplified FEM models
were employed for the analysis of EB welding. The size of 0
plates was 200l x 400w x 45t (mm), and the distance from
weld line to cooling channels were varied from 10 to 16mm. Fig. 1 Residual stress distributions parallel to weld line
at cross sectional plane of middle of weld line.
* Graduate School, Osaka University, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** JWRI, Osaka University, Japan Japan
*** Japan Atomic Energy Agency, Japan
235
Prospective design of weld joint between first and side walls in test blanket module for ITER
45
1490mm
40 FEM modeling Side wall
35
200mm
Side wall
30 Weld
First wall
422mm
x direction First wall
z [mm]
25
Case1 y Weld line
20 Case2 (180mm) 200mm
Case3 z 232mm 116mm
15
Case4
10
5 Weld Line Bucking

0
21.5mm
-400 -300 -200 -100 0 100 200 300 400 500 600 700
12mm
Residual Stress along Y-direction [MPa]
25mm
25mm
Fig. 2 Residual stress distributions parallel to weld line 10mm 16mm
beside cooling channels.
(Current Design) (Prospective Design)
3. Evaluation of Prospective Design Fig. 3 Schematic illustration of box structure for TBM and
Figure 3 shows a schematic illustration of the box FEM models with current and prospective design.
structure for Japanese TBM and FEM models for numerical
analysis. As shown in this figure, a partial model was Case-1 Case-2
x
employed for this evaluation because of the limitation of
Weld line
computer resources. This figure also shows the FEM model z y
with current and prospective designs obtained from the
above studies. In prospective design, the width of backing
16mm
was modified without changing the thickness of first wall. 10mm
In the order to evaluate the residual stress in the prospective
design, the thermal elastic-plastic analyses were conducted
in two cases, which were Case-1 (current design) and Case- Fig. 4 Plastic strain distributions parallel to weld line
2 (prospective design), respectively. at cross sectional plane of middle of weld line.
In the elastic-plastic analyses, the mechanical boundary
[MPa] Case-1 Case-2
conditions were set as follows.
1) Displacement along y-direction was fixed at the x
Weld line
cutting planes of the first and side walls
perpendicular to the welding direction z y
2) Displacement along z-direction was fixed at the
other cutting plane of the first wall
16mm
10mm
3) Displacement along x-direction was fixed at the

other cutting plane of the side wall
The plastic strain distributions parallel to the weld line
at center cross section were shown in Fig. 4. It can be found Fig. 5 Residual stress distributions parallel to weld line
that the compressive plastic strain on the surface of cooling at cross sectional plane of middle of weld line.
channels in Case 2 was much smaller than that in Case 1.
Also, it was revealed that the distribution near the weld line 4. Conclusions
became uniform by setting the weld line 16 mm away from In order to reduce the risk of stress corrosion cracking
the cooling channels. in the test blanket module for ITER, the modification of
Figure 5 shows the welding residual stress distributions current designs was studied focusing on the location of the
parallel to the weld line at center cross section. From this weld line by thermal elastic-plastic finite element analysis.
figure, it was found that the residual stress on the surface of Also, the prospective design was examined by using a
cooling channels in Case 2 was smaller than that in Case 1. partial FEM model of a box structure composed of the first
However, tensile residual stress more than 200 MPa was and side walls.
generated beside channels in Case 2. Thus, it is necessary to (1) The change of distance between weld line and cooling
conduct post weld heat treatment (PWHT) for decreasing channels from 10 to 16 mm would decrease the welding
the residual stress around channels. As for the appropriate residual stress on the surface of channels and this
condition of PWHT, it is revealed that the prospective decrement might lead to the reduction of risk for SCC.
design would be more suitable than the current design since (2) Residual stress on the surface of channels in the
the plastic strain beside channels was small and its prospective design was smaller than that in current
distribution would be uniform as shown in Fig. 4. design, while tensile residual stress more than 200 MPa
was generated. Thus, there is a need to conduct PWHT
to reduce the residual stress, and the prospective design
would be suitable for PWHT because the plastic strain
236
around cooling channels was small and its distribution M.A. Sokolov, R.E. Stoller and S.J. Zinkle: Fusion
was more uniform than that in current design. Engineering and Design, 83, (2008), pp.1471-1476.
[2] T. Hirose, M. Enoeda, H. Ogiwara, H. Tanigawa and M.
References Akiba: Fusion Engineering and Design, 83, (2008), pp.1176–
[1] H. Tanigawa, T. Hirose, K. Shiba, R. Kasada, E. Wakai, H. 1180.
Serizawa, Y. Kawahito, S. Jitsukawa, A. Kimura, Y. Kohno, A. [3] H. Serizawa, S. Nakamura, M. Tanaka, Y. Kawahito, H.
Kohyama, S. Katayama, H. Mori, K. Nishimoto, R.L. Klueh, Tanigawa and S. Katayama: Journal of Nuclear Materials, to
be published (2011).
237
Preliminary numerical research of microstructural fracture

behavior in metal by using interface element†
TOMIYAMA Seigo*, SERIZAWA Hisashi**, HAJIMA Tsuyoshi**and

MURAKAWA Hidekazu*
KEY WORDS: (Interface element) (Grain orientation) (Grain boundary) (Finite element method)
(Stress concentration)
1. Introduction Two dimensional ideal microstructure of steel was

Recently, super high strength steel has been developed created by using Voronoi tessellations and Fig.1 shows
by controlling its microstructure precisely and this steel has finite element model based on this microstructure. This
been widely used in various fields. Although there have model contains 30 grains, whose orientations are varied.
been various experimental studies about fracture behavior In order to demonstrate the interfacial deformation, the
of the high strength steel, its microstructural deformations interface elements were arranged along the grain
have not been revealed because only the deformation of boundaries.
grain has been modeled in the conventional finite element
method. The authors have developed the interface Interface element
element in order to model the interfacial deformation such Essentially, the interface element is the distributed
as crack opening, crack propagation and interfacial sliding nonlinear spring existing between surfaces forming the
[1]. In this research, the interface element was employed interface or the potential crack surfaces. The interaction
for modeling the deformation of grain boundary and the between surfaces is characterized by a potential function
microstructural fracture behavior was examined by using that involves the surface energy J, the shape parameter N
the finite element method with the interface element. and the scale parameter r 0 . In order to describe both the
Namely, the anisotropic deformation of grain due to grain opening and sliding deformations at the grain boundary, the
orientation was modeled by the ordinary finite element and combined potential function was employed in this research
the opening and slipping at grain boundary was [1]. The opening and shear stresses to the displacement G
demonstrated by the interface element where the effect of could be described as the following equations, and these
grain orientation on the mechanical property at the grain relationships are shown in Fig. 2.
boundary was taken into account as the preliminary
4JN °§ r0 · ½°
N 1 2 N 1
numerical examination. By using two dimensional § r0 ·
V ¨
®¨ ¸
¸ ¨
¨ ¸
¸ ¾ (1)
microstructure obtained through Voronoi tessellations, the r0 °̄© r0 G ¹ © r0 G ¹ °¿
influence of grain orientation on the microstructural
fracture behavior was investigated 4 AJN °§ r ·
N 1
§ r ·
2 N 1
½°
W ®¨¨ ¸¸ ¨¨ 0 ¸¸
0
¾ (2)
r0 °̄© r G ¹ © r0 G ¹ °¿
2. Analysis Method 0
Model for analysis
Fig. 1 Finite element model for analysis. Fig. 2 Opening and shear stresses related to displacement.
** JWRI, Osaka University, Japan Japan
238
Preliminary numerical research of microstructural fracture behavior in metal by using
interface element
Table 1 Stiffness of hexagonal crystal for a-Fe.
The parameters involving the above equations were

determined for demonstrating D-Fe fracture behavior.
Namely, the surface energy J and the shape parameter N
were assumed to 2.0 N/mm and 4, respectively. The scale (a) Isotropic model (b) Anisotropic model
parameter r 0 is the property related to maximum bonding Fig. 5 von Mises stress distributions
and sliding stresses (V max and W max ), and was determined
according to the misorientation angle between neighbor Anisotropy at grain boundary
grains as described in the following section. Also, the Generally, the intergranular fracture is caused by crack
interaction parameter A which indicates the ratio V to W is opening and slipping at grain boundaries. The interface
included in Eq. (2). element can demonstrate such deformations by employing
the interaction parameter A in Eq. (2). In the case with a
Anisotropy in grain low value of parameter A, the interfacial slipping easily
The properties of each grain in metal materials have occurs in comparison with the crack opening at the
anisotropy due to the direction of grain growth. In order interface. The parameter A was varied as 1.0, 0.25 and
to demonstrate the microstructural deformation precisely, 0.01 in order to examine the influence of difference
the anisotropy has to be taken into account and was between opening and shear strength on the microstructural
assumed by changing the elastic moduli of each directions fracture behavior.
(E 11 , E 22 and G 12 ). The material studied in this research The grain boundary can be regarded as disorder of
was D-Fe which has hexagonal crystal lattice, and target atoms between neighbor grains. So, it can be assumed that
plane was assumed to (110) plane which contains only tilt the fracture strength at grain boundary would be related to
boundaries not twist boundaries. Table 1 shows the the boundary energy, which could be determined by the
stiffness of hexagonal crystal for D-Fe [2], and the elastic atomic disorder at the boundary. There have been many
moduli in anisotropic grain were determined according to researches about the symmetric tilt boundary, and various
the direction of the target plane. Namely, the moduli of boundary energies in different plane were studied by using
each direction in (110) plane (E 11 , E 22 and G 12 ) were the molecular dynamic method. Tanaka et al. examined
assumed to 125.0, 210.5 and 66.20 GPa, respectively. <110> boundary energy of molybdenum and revealed that
the square of fracture strength V bd would be linearly
proportional to the grain boundary energy J bd [3]. Since
the boundary energy of D-Fe was reported as shown in Fig.
3 [4], the authors assumed that the boundary fracture stress
of D-Fe would follow the relation to misorientation as
shown in Fig. 4.

As a preliminary analysis, the influence of anisotropy in
grain on fracture behavior of the model shown in Fig. 1 was
examined by assuming only the elastic deformation in grain
and the anisotropy at grain boundary. Fig. 5(a) and (b)
show the typical results of isotropic and anisotropic grains
Fig. 3 Relationship between boundary fracture stress and in applying 0.624 % strain, respectively. The interaction
misorientation angle. parameter in Eq. (2) A was assumed as 0.25, which means
that the shear sliding stress W is half of the bonding stress V.
In the isotropic model, the significant difference among
Interpolated
curve grains was not obtained and the stress distribution was
almost homogeneous. So, the position of crack
propagation was determined by the distribution of boundary
fracture stress at the grain assumed. On the other hand,
the stress distribution of the anisotropic model was
heterogeneous and stresses among grains were very
different. This difference was considered to affect the
crack propagation process. In addition, the analyses for
studying the influence of interaction parameter A and
anisotropy at grain boundary were conducted.
Fig. 4 Relationship between boundary fracture stress and
misorientation angle.
239
4. Conclusion References
In order to demonstrate the microstructural fracture [1] H. Serizawa et. al: Trans. of JWRI, 33, 2, (2004), pp.181-185.
behavior in metal, the finite element method with an [2] N. Igata: Strength of Materials, Tokyo, BAIFUKAN Co., Ltd,
interface element was developed. The anisotropy in grain (1983), pp.11 (in Japanese).
[3] T. Tanaka et. al: Bulletin of the Japan Institute of Metals
and that at grain boundary were modeled by the ordinary Materia Japan, 58, 4, (1994), pp.382-389 (in Japanese).
finite element and the interface element, respectively. By [4] H. Nakashima et. Al: TETSU-TO-HAGANE, 86, 5, (2000),
using this method, the influence of anisotropy in grain and pp.357-362 (in Japanese).
at grain boundary on the microstructural fracture behavior
were examined successfully.
240
Thermoreversible colloidal gelation for direct-assembly of

†
nanoparticles
KONDO Akira *, ANDATSU Masahiro *, ABE Hiroya * and NAITO Makio *
KEY WORDS: (Direct ink writing) (Colloidal gel) (Viscoelastic) (Nanoparticles)
1. Introduction appeared by physical cross-linking of the triblock

Direct ink writing (DIW) techniques offer the ability to copolymer due to temperature-induced hydrophobic
produce ceramic components on-demand with complex interactions.
structures. These techniques can be attractive routes for
advanced ceramics, sensors, composites, tissue engineering 2. Experimental
scaffolds and photonic materials[1],[2]. Several approaches (Material)
such as robocasting [3],[4], fused deposition [2],[5], and Alumina powder (TM-DAR,Taimei Kagaku, Japan) was
micropen writing [6] have been introduced and have used for the model particles. The specific surface area of
demonstrated solid freeforming of 2D and 3D colloidal the powder, measured by nitrogen adsorption, was
structures via a layer-by-layer deposition of particle based approximately 13m2/g yielding an equivalent spherical
inks. In each approach, ink is continuously extruded diameter of 120nm. A poly(acrylic acid)(PAA) type
through a micro-nozzle to create a filamentary element. dispersant (CELNA D305, Chukyo-yushi, Japan) was used.
Nanoparticle suspensions for filament-based direct A high affinity of PAA on oxide surfaces can promote the
writing techniques must satisfy two important criteria [4]. colloidal stabilization of oxide particles in aqueous system.
First, they should exhibit a well-controlled viscoelastic Poly(propylene oxide) - poly(ethylene oxide) (PEO-PPO-
response, i.e., they flow through the deposition nozzle and PEO) triblock copolymers (Lutrol F127, MW~12,000,
then set immediately to facilitate shape retention of the BASF, Germany) as a gelling agent. Deionized water was
deposited features. Secondly, they should contain a high used as solvent.
volume fraction of powder to minimize drying-induced (Preperation of colloidal ink)
shrinkage after assembly is complete, i.e., the particle The solid volume fraction of alumina in the aqueous
network must be able to resist compressive stresses arising suspension was set at 15vol%. The amount of PAA added
from capillary tension. The developed nanoparticle ink was was 1.0mass% of the solid. The suspension was milled in a
an aqueous colloidal gel comprised of poly(acrylic laboratory scale ball mill for 24h using alumina milling
acid)(PAA)-coated BaTiO 3 nanoparticles, whose media. Then, F127 was mixed and dissolved under cooling
interactions were carefully modulated by changing ionic below 10°C. The total amount of F127 added was 29mass%
strength through the addition of monovalent or divalent salt of the solid.
species [7]. However, there is a large risk that the rapid (Rheological Measurements)
gelation induced by change of salt concentration or pH may The rheological measurements of the colloidal inks
result in large inhomogeneities in the dense suspension. were conducted using a rheology meter (HAAKE
In this study, we have newly developed Rheostress RS600, Thermo fisher scientific Inc., USA). As
thermoreversible viscoelastic slurries which may provide sensor attachments, cone-plate type sensors with 20 and
homogeneous gel state for DIW. Its thermoreversible 35mm diameters were employed. To avoid undesired
property increases reliability on the preparation of influence from different mechanical histories, samples were
homogenous gel and allows easy operation on the processes homogenized by shearing at an identical rate of 20s-1 for
of DIW including ink charge and nozzle cleaning. The 10s and left standing for an additional 10s prior to
slurry of ceramic nanoparticles was prepared with addition measurement. Flow curves were automatically recorded via
of poly(ethylene oxide) - poly(propylene oxide) - a built-in program. The measurements were performed with
poly(ethylene oxide) (PEO-PPO-PEO) triblock copolymers the following input conditions: the shear rate increased
[8],[9] and then applied for DIW. The PEO-PPO-PEO logarithmically from 0.1s-1 to 100s-1, over the time period of
aqueous solution with enough concentration shows nearly 2min. The measurement temperatures were 5 and 30°C.
Newtonian behavior (sol state) at cooled temperatures (Direct Ink Writing)
(5°C) and thickened (gel state) at room temperature (25°C) A robocasting system with a micro-pen was employed.
or above 25-70°C. These states were reversible with the The colloidal ink was housed in a syringe and warmed at
temperature change. The reversible sol-gel transition can be 30°C to induce sol-gel transition. And then the resultant
Japan
241
Thermoreversible colloidal gelation for direct-assembly of nanoparticles
colloidal gel pushed out as a filament through a tapered direct writing technique. We used the PEO-PPO-PEO block
QR]]OH GLDPHWHU ' ȝP E\ D SQHXPDWLF V\VWHP 7KH co-polymer as a gelation agent. Using the present colloidal
filament was deposited on a plate or deposited layers while gel, the 3D wood-pile structure of alumina nanoparticles
the position of the nozzle was moving with a CAD system was directly formed.
control. The deposition was carried out in air, and the plate
for deposition was warmed at 60°C. The deposited colloidal
gel was dried with keeping the assembled shape.
The CAD program was designed to form the 3D-woodpile ȝP (a)
structures. The width between lattices was set 500ȝm.
(Sintering)
After drying, the assembled specimen was burned to
ȝP
remove polymers at 500°C for 5h and then sintered at
1450°C for 2h.
ȝP
3. Result and discussion
Figure 1 shows shear stress as a function of shear rate
for the prepared colloidal ink at 5 and 30°C. Viscosity of the
colloidal ink drastically increased with increase of
temperature. The shear stress at the low shear rate (0.1s-1)
(b)
was about 100Pa (at 30°C). It was applicable for the DIW.
Actually, the 3D wood-pile structure was successfully
formed without any defects.
104
103 30Υ
102
Shear stress (Pa)
ȝP
101
100 (c)
10-1
10-2 5Υ
10-3
10-1 100 101 102
ȝP
Shear rate (s-1)
Fig. 1 Shear stress as a function of shear rate for Fig. 2 Photographs of the assembled wood-pile structure
the prepared colloidal inks after sintering at 1450°C
(a) optical microscope (b),(c) SEM
Figure 2 shows the photographs of the specimen
assembled by the DIW. Fig.2(a) was taken by optical References
microscope. Fig.2(b) and Fig.2(c) were taken by scanning [1] J.A.Lewis and J.E.Smay, J.Stuecker, J.Cesarano : J. Am.
electron microscope (SEM). The wood-pile structure was Ceram. Soc., 89(2006), pp.3599-3609.
formed according to the CAD program. The filament which [2] M.Allahverdi, S.C.Danforth, M.Jafari and A.Safari : J. Euro.
was pushed out through the nozzle (diameter, D=1ȝP Ceram. Soc., 21(2001) , pp.1485-1490.
swelled a little because of release from the pressure at the [3] J.Cesarano, R.Segalman and P.Calvet : Ceram. Ind., (1998),
nozzle. After sintering, the diameter of the sintered filament pp.94-102.
was 125ȝP. The width between the lattices of the sintered [4] J.E.Smay, J.Cesarano and J.A.Lewis : Langmuir, 18(2002) ,
pp.5429-5437.
specimen was about 380ȝP. The shrinkage with the
[5] G.M.Lous, I.A.Cornejo, T.F.MacNulty, A.Safari and
sintering was about 20%. S.C.Danforth : J. Am. Ceram. Soc., 83, (2000), pp.124-128.
[6] S.L.Morissette, J.A.Lewis, P.G.Clem, J.Cesarano and
4. Conclusions D.B.Dimos : J. Am. Ceram. Soc., 84 (2001), pp.2462-2468.
In this study, we have newly developed [7] Qi Li and J.A.Lewis : Ad. Mater. , 15(2003),pp.1639-1643.
thermoreversible viscoelastic slurries which may provide
homogeneous colloidal gel states of nanoparticles for a
242
†
YAMANAKA Shinya*, ABE Hiroya*, NAITO Makio*, UESHIMA Yuya**, NOMA Junichi**
KEY WORDS: (Magnetorheological effect) (Magnetorheological suspensions) (Dynamic rheology)

(Modification) (Oleic acid)
1. Introduction surface of oxide particles [5], fabrication of MR fluid using

Current magnetorheological (MR) fluids are non- oleic acid has not been reported because oleic acid and
colloidal dispersions of micron-sized magnetic particles in a silicone oil are mutually-immiscible. In this work, we have
carrier liquid such as silicone oil. Under an applied investigated the influences of oleic acid as a surface-active
magnetic field, MR fluids alter their rheological properties, substance on the dispersibility into oil phase and the MR
rapidly and reversibly. Such magnetic-field tunable response.
rheological behavior of MR fluids is the base in many smart
actuation systems [1]. The MR fluids stability against 2. Method
aggregation and settling of micron-sized magnetic particles Crystalline Fe nanoparticles which used a magnetizable
is an intrinsic hindrance for many practical applications. matrix were fabricated via an arc-plasma method [6]. The
Several studies based on interfacial chemistry have been nanoparticles had a spherical shape with about 100 nm in
done to improve this problem. Surface modification of size and were covered with 2 nm thin oxide layer as shown
magnetic particles with surfactants or polymers is a in Fig. 1.
common sense approach that prevents aggregation by MR fluids were prepared as follows. The Fe
means of steric repulsion. In order to avoid particle settling, nanoparticles were coated with oleic acid (Kanto Chemical,
however, a thickening carrier liquid using additive (fumed Japan) by means of planetary centrifugal mixer (AR-100,
silica [2] or organoclay [3], for instance) is required. Nano- THINKY, Japan) during 10 min. Then, either non-modified
sized magnetic particles are capable of homogeneous or the modified Fe nanoparticles were mixed with silicone
dispersion into the oil phase without aggregation and settling. oil (KF96-50cs, Shin-Etsu Chemical, Japan) using the
Hydrophilic oxide magnetic particles are difficult to planetary centrifugal mixer for 10 min. Additive amount of
disperse into conventional silicone oils due to a poor oleic acid was 0–11 wt%. The solid concentration of MR
interaction of the oil with particle surfaces. A colloidal fluids was set to 1–15 vol%.
dispersion system should be then developed. Generally, MR responses of the fluids were measured at 293 K
principle phenomena in developing colloidal dispersion using a parallel-plate rheometer (RheoStress600, HAAKE,
system are dissolving additives in liquid, adsorption of Germany) attached to the electro-magnetic system (MR-
additives on particles and wetting of the particles by liquid 100N, EKO Instruments, Japan). The diameter of the plates
[4]. Liquid must dissolve additives so that they become was 20 mm and the gap distance was fixed at 0.5 mm.
uniformly distributed and have wettability with the liquid. Magnetic flux was applied perpendicular to the direction of
Although oleic acid (C 18 H 34 O 2 ) can be adsorbed on the the shear flow from 0 to 0.3 T.
Fe3O4 (~2nm) 3. Results and Discussion

Influence in the dispersibility on MR effects was firstly
investigated by using the non-modified and modified Fe
nanoparticles. Additive amount of oleic acid was 3.0 wt%.
Figure 2 shows shear stress versus shear rate relationship
with and without internal magnetic flux for 15 vol% MR
fluids.
With respect to the surface-modified nanoparticles, the
shear stress of the dispersions increased with strengthening
magnetic fields. Additionally, the MR fluid behaves as a
Bingham fluid which is generally monitored in micron-
sized MR fluids. The yield stress at 0.3 T of the applied
magnetic field was ca. 5.9 kPa, indicating significant turn-
10 nm
up ratio (=1150, refers to the difference between off-state
Fig. 1 TEM image of a Fe nanoparticle apparent viscosity and on-state yield stress) of the modified
** Kurimoto, LTD., Suminoe-ku, Japan Japan
**** Industrial Science, RIWM, Osaka, Japan
243
Above 5 vol% of solid volume fraction, the relative

0.3T viscosity increased, dramatically. Surface distance between
nanoparticles for 5 vol% MR fluid calculated from the
0.1T Woodcock equation [7] is ca. 100 nm. Actually, the
distance basically agrees with interaction distance of a
hydrophobic attraction force [8].
It is commonly believed that there is an optimal amount
0T of added dispersant. That is, incomplete coverage or
excessive addition of dispersant leads to particles
aggregation. Figure 4 demonstrates the effect of additive
amounts of oleic acid on off-state apparent viscosity. The
fluid showed the lowest viscosity with the 3.0 wt% addition.
4. Conclusions
We have found that the adequate addition of oleic acid
into silicone oil including the magnetic nanoparticles
dramatically reduced their apparent viscosity and was a key
to develop
colloidal
dispersion
system.
Additionally,
the
Fig. 2 Shear stress versus shear rate relationship with and resulting fluid clearly demonstrated a large MR effect.
without magnetic flux for 15 vol% MR fluids
Fig. 4 Off-state apparent viscosity of MR fluids with

Fig. 3 Relative viscosity as a function of solid volume various amount of oleic acid
fraction without internal magnetic field
References
nanoparticles dispersions. It should be noted that oleic acid [1] J. D. Carson, M. R. Jolly: Mechatronics, 10 (2000), pp.555-
569.
is effective to control dispersibility of the nanoparticles into
[2] S. T. Lim, M. S. Cho, I. B. Jang, H. J. Choi: J. Magn. Magn.
the silicone oil. Hence, resulting MR fluids clearly verifies Mater., 282 (2004), pp.170-173.
a large MR effect. [3] M. T. López-López, A. Gomez-Ramirez, J. D. G. Duran, F.
In contrast, a slight turn-up ratio (=82) was observed for Gonzalez-Caballero: Langmuir, 24 (2008), pp.7076-7084.
the non-modified nanoparticles fluid. The shear stress of the [4] J. S. Reed: Principles of Ceramics Processing, Wiley and
non-modified based fluid at the off-state field is ten times Sons, New York, (1995)
larger than that of the modified dispersions. This result [5] S. Sun, H. Zeng, D. B. Robinson, S. Raoux, P. M. Rice, S. X.
indicates that the non-modified nanoparticles formed Wang, G. Li: J. Am. Chem. Soc., 126 (2004), pp.273-279
aggregates in the oil phase spontaneously due to [6] J. Noma, H. Abe, T. Kikuchi, J. Furusho, M. Naito: J. Magn.
entropically unfavorable interaction between the oil and the Magn. Mater., 322 (2010), pp.1868-1871.
nanoparticles. Obviously, the most illustrative expositions [7] L. V. Woodcock, Proc. of a workshop, Nov. (1985) pp.11-13.
[8] N. Ishida, M. Sakamoto, M. Miyahara, K. Higashitani:
of the interparticle attraction between nanoparticles are Langmuir, 13 (2000), pp.5681-5687.
volume fraction dependency of relative viscosity in Fig. 3.
244
Molecular dynamics analysis of fcc nanowire under torsional loading†
OGAWA Takaki *, ** and NAKATANI Akihiro***
KEY WORDS: (Molecular dynamics) (Atomic simulation) (FCC crystal)
1. Introduction deformation from the similar concept to cohesive law of

The macroscopic mechanical properties of interplanar tensile deformation.
polycrystalline materials strongly depend on their
microscopic structure. For example, grain refinement by 2. Model and Simulation Method
some severe plastic deformation can improve the tensile We consider the torsional deformation of a
strength of industrial pure aluminum from 80 to single-crystal Cu nanowire having a circular cross section,
350MPa[1]. The knowledge obtained by the study of the as shown in Fig. 1. Here, the length and radius of specimen
mechanism of deformation from a microscopic point of is 7.514 nm and 3.615 nm, respectively. The torsion axis is
view can be useful for the fundamental principles of the along the crystal orientation 111!. The crystal comprises
material design. Even if the crystallographic structure is 36 atomic layers along the z-axis, for a total of 26,076
initially perfect, lattice defects such as the dislocation, atoms. We adopt the twisted periodic boundary condition
stacking fault, etc. which occur after the plastic [4] along the z-axis with dimension L z of the unit cell. ș
deformation contribute the mechanical properties for denotes the twist angle per unit length, ȭ denotes the
inelastic behavior. Therefore the evaluation of an ideal twist angle for the specimen, and their relation is ș = ȭ
strength of a single crystal including evolution of defect /L z .
structure is meaningful as the first step. The interaction between the Cu atoms is analyzed using
Nguyen and Ortiz presented two different approaches for the embedded-atom method of Mishin et al. [5], which can
coarse-graining interplanar potentials and determining the be used to accurately determine the stacking-fault energy.
corresponding macroscopic cohesive laws on the basis of The time step is set to 2 ps, and the simulation period is up
energy relaxation and renormalization group [2]. They to 350 ps. First, we set atoms with a random initial velocity
show that a universal asymptotic form of macroscopic and calculate the time required under no load to reach a
cohesive law can be derived from the analysis of cohesive condition of equilibrium. Subsequently, the torsional
behavior of a large, but finite, number of interatomic deformation is determined under repeated cycles
planes. In our previous study, we analysed fcc Cu and Al comprising a small torsion ǻș = 6.25 × 10.4 rad/nm
nanowires under torsional loading using molecular followed by relaxation for 0.5 ps. On average, there exist a
dynamics and investigated systematically the influence of proportional relation between the energy relaxation time
the stacking-fault energy on defect structures in and the twist angle per unit length. Temperature is
nanowires[3]. In this study, we conduct a detailed
investigation into the localization of deformation and
derive a constitutive relation of interplanar tosional
Fig. 1 Schematic of specimen. Fig. 2 Time vs torsion angle.
† Received on 30 September 2010 Proceedings of the Visual-JW2010 organized by JWRI, Osaka

* JSOL Corporation, Osaka, Japan University.
** Graduate School, OSAKA University, Suita, Osaka, Japan
*** OSAKA University, Suita, Osaka, Japan
245
Molecular dynamics analysis of fcc nanowire under torsional loading
(a) 20 ps (b) 40 ps (c) 60 ps (d) 80 ps

Fig. 3 Atomic arrangement of quarter Cu nanowire under 111! torsion
maintained at a constant 300 K by the velocity scaling face-centered-cubic (fcc), local hexagonal-close-packed
method. (hcp) or the other. In this specimen, it is the hcp atomic
structure that makes up the stacking faults. These hcp
3. Results and Discussion atoms are named as stacking-faults atoms and represented
atomic layer of the specimen with respect to time. The in red. Other atoms are named as other defects and
atomic layers are sequentially numbered along the z-axis. represented in blue. Fcc atoms are represented in gray.
The rotation angle is evenly distributed until approximately Elastic deformation occurs at 20 ps. The external force
30 ps. Then they are divided into two. causes equal strain along the twist axis. At 40 ps, multiple
Next, Fig. 3 shows the atomic configuration of a quarter stacking faults are observed, and at 60 ps, the deformations
of the Cu specimen at 20–80 ps. In order to analyze the are found to be concentrated in some of the stacking faults.
defect structure, common neighbor analysis (CNA) is used These concentrations give rise to localization of defect
to classify the structure of the Cu atoms into local structures. Finally, at 80 ps, the defect structures are almost
fully localized. The other stacking faults recover from their
deformations. As a result, we conclude that the given load
induces only localized defect structures.
Next, Fig. 4 and 5 show the change in the potential
energy per unit length, along the z-axis. It shows plots for
the entire system and for sets of three adjacent atomic
layers. Figure 4 shows the change in the potential energy
with time. Up to approximately 30 ps, the potential energy
increases quadratically with time. That is, the potential
energy increase quadratically with the macroscopic torsion,
and all atomic layers of the crystalstructure exhibitelastic
deformation. Then, up to approximately 120 ps, the 34–36
atomic layers show an increase in their twist angle, but the
other atomic layers show none. Hence, we can confirm that
macroscopically, the nanowire exhibits plastic
Fig. 4 Potential energy vs time. deformation; however, from the microscopic point of view,
the stacking fault elastic recovery is going. Next, Fig. 5
shows the relative twist angle for each set of three adjacent
atomic layers. The twist angle of the atomic interplane is
UHSUHVHQWHG E\ į UDGQP 7KH UHODWLRQ EHWZHHQ WKH WZLVW
angle and the potential energy for atomic layers is obtained.
As a result, we are able to define the microscopic
interplanar potentials.
4. Conclusions
We analyze fcc Cu nanowires under torsional loading
using molecular dynamics analysis. We investigate the
mechanism of localization by observing the potential
energy of each atomic layer and its twist angle in detail.
We obtain the following findings through this study:
(1) We demonstrate that macroscopic plastic deformation
Fig. 5 Potential energy vs torsion angle. occurred in the nanowires, but that from the microscopic
246
point of view, the stacking fault elastic recovery is going. [3] T. Ogawa and A. Nakatani: International Symposium on
(2) We obtain the relation between the twist angle and the
Structures under Earthquake, Impact, and Blast Loading 2008
potential energy for each of the atomic layers. That helps
us define the microscopic interplanar potentials. (IB2008), (2008), pp. 47-52.
[4] A. Nakatani, T. Shimokawa, R. Matsumoto and H. Kitagawa:

References
[1] N. Tsuji, Y. Ito, Y. Saito and Y Minamino: Scripta Materialia, Solid Mechanics and Its Applications, 115 (2004), pp.
47 (2002), pp. 893-899. 365-380.
[2] O. Nguyen and M. Ortiz: Journal of the Mechanics and [5] Y. Mishin, M. J. Mehl, D. A. Papaconstantopoulos, A. F.
Physics of Solids, 50 (2002), pp. 1727-1741. Voter and J. D. Kress: Phys. Rev. B 63 (2001), p. 224106.
247
Visualization of mechanical properties in alumina dental crowns

†
fabricated by using laser scanning stereolithography
TASAKI Satoko *, KIRIHARA Soshu * and SOHMURA Taiji **
KEY WORDS: (Dental crown) (Alumina) (Stereolithography) (Flexural strength) (Sintering behavior)
1. Introduction stereolithography. Figure 1 shows schematic illustrations of

Ceramic dental crowns to cover human teeth or dental the fabrication system. Three dimensional model data was
implants are investigated and developed actively in world- converted into the stereolithography file format, and sliced
wide medical industries in order to realize advantages of into a series of two dimensional data with uniform thickness.
aesthetic sensuousness and to avoid serious risks for These files were transferred into the process equipment
metallic allergies. In this investigation, the dental crown (D-MEC, SCS-300P). Slurry material was prepared through
models of acrylic resins including ceramic particles were mixing photo sensitive acryl resin and alumina powder
fabricated by using laser scanning stereolithography of a (Showa Denko, AL-170) at 60 to 70 volume %. The mixed
computer aided design and manufacturing. Graphic data of paste was spread on a flat substrate and smoothed. An ultra
the crowns were obtained through a computer tomography violet laser beam of 355 nm in wave length was scanned
scanning. Dense objects of alumina ceramics as biomedical over the deposited layer to create cross sectional planes.
components were fabricated successfully through powder After these layer stacking processes, solid components were
sintering processes [1,2]. Moreover, the formed crowns fabricated. These precursors were de-waxed at 600 to
were coated by dental glasses to improve aesthetic and 800 oC for 2 hs and sintered at 1400 to 1600 oC for 2 hs in
mechanical properties. the air atmospere. The sintered ceramic components were
coated with La 2 O 3 -B 2 O 3 -Al 2 O 3 -SiO 2 glass (Zahnfabrik,
In-Ceram-Alumina) for the dental use and heated at
1100 oC for 2 hs. The ceramic microstructures were
observed by using a scanning electron microscope. And the
flexural strengths of plate specimens were measured by
using a three point bending test machine.

The stereolithographic composite model and the
sintered alumina crown are shown in Fig. 2. Macroscopic
damage and deformations are not observed. Cross sectional
micro-structures of sintered bodies and glass infiltrate
samples are shown in Fig. 3. The large cracks propagate
parallel to the stacked layers formed in the
stereolithographic processes. Through the glass infiltrate
treatments, these cracks become inconspicuous. The
maximum flexural strength is achieved 587±91 MPa by
sintering at 1500 oC and glass infiltration. This mechanical
property is acceptable level for dental crown use.
Fig. 1 Schematic illustrations of data processing and laser Subsequently, we considered sintering behaviour at each
scanning in stereolithography technique of a computer temperature for the non-keeping times. Figure 4 shows the
aided design and manufacturing (CAD/CAM) procedure. ceramic microstructures at each heating temperature. The
sintered sample at 1300 oC shows the powder-like
2. Experimental Procedure microstructure. Comparing with this, by the sintering at
ᴾ ᴾ The dental crown models and flexural test specimens of 1400 to 1500 oC, the neck growths between the particles
4.5×22×1.0 mm in dimensions were fabricated by using were considered to be started.
†ᴾ Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding

*ᴾ JWRI, Osaka University, Ibaraki, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
**ᴾ Graduate School of Dentistry, Osaka University, Osaka, Japan Japan
248
Visualization of mechanical properties in alumina dental crowns fabricated by using laser scanning
stereolithography
Fig. 4 The ceramic microstructures of the sintered

alumina. The composite precursors formed by the
stereolithography were de-waxed and sintered at 1300 to
1700 oC without time keeping for the necking growth
observations.
Fig. 2 Dental crown models of green bodies composed of
4. Conclusion
acrylic resin with alumina particles formed by the stereo-
lithography and sintered ceramic components. Three dimensional alumina components of dental
crowns and mechanical test plates were fabricated
successfully by using stereolithography. Flexural strength of
glass infiltrated sample is achieved about 600 MPa as an
acceptable level for dental crown use. Subsequently,
sintering behaviours of the alumina components were
investigated, and the obtained results will serve as a guide
to material designs.
5. Acknowledgments
This study was supported by Priority Assistance for the
Formation of Worldwide Renowned Centers of Research -
The Global COE Program (Project: Center of Excellence
for Advanced Structural and Functional Materials Design)
from the Ministry of Education, Culture, Sports, Science
and Technology (MEXT), Japan.
References
[1] M. Suwa, S. Kirihara and T. Sohmura: Ceramic Transactions,
219 (2009), pp. 331-336.
[2] M. Suwa, S. Kirihara and T. Sohmura: Proceedings of the
34th International Conference on Advanced Ceramics and
Composites, 31, 8(2009), pp.239-245.
Fig. 3 Cross sectional ceramic microstructures of alumina
flexural test samples with or without glass infiltrations. The
plate specimens were formed by stereolithography and heat
treatment processes. FS and RD mean the flexural strength
and relative density, respectively.
249
Combinatorial analysis of plasma-polymer interactions for

†
formation of inorganic-soft materials hybrid structure
, , ,
TAKENAKA Kosuke * ****, CHO Ken * ****, SETSUHARA Yuichi * ****,
, , ,
SHIRATANI Masaharu ** ****, SEKINE Makoto *** **** and HORI Masaru *** ****
KEY WORDS: (Plasma) (Polymer) (Combinatorial analysis) (Soft material) (Flexible electronics)
1. Introduction The working gas of argon-oxygen mixture was supplied to

For fabrication of the future nano device using soft the discharge chamber through a gas inlet located at the top
flange. The argon-oxygen mixture plasma was generated
materials including next-generation ULSIs, MEMS, NEMS
at a total pressure of 2.6 Pa and RF power of 88 - 350 W
and bio-chips [1], plasma processes have played important
with an oxygen partial pressure of 20% in the total pressure.
roles as base technologies. It has become of key Ion-saturation current profiles along the substrate were
importance to develop process technologies with nano- measured with a cylindrical Langmuir probe at 5 mm above
sized structure control, which are required to be performed the substrate holder. Poly(ethylene terephthalate) (PET)
via plasma processing technologies. However, it is greatly films with a thickness of 100 Pm were exposed to argon-
anticipated that optimal process conditions can be attained oxygen mixture plasmas on an electrically grounded
at a pinpoint window of the process conditions, in which substrate holder with and without water-cooling. In this
device structures and/or organic-inorganic interface should investigation, five samples were located at substrate
be controlled with a precision of nanometer size either via positions x = 40, 80, 120, 150, and 220 mm. Etching
top-down or bottom-up process. depth of the PC and PET films via plasma exposure was
In order to overcome these constraints involved in next- measured with stylus surface profiler. Surface roughness
generation plasma nano fabrication technologies, it is of of the PC and PET films was observed with atomic force
great significance to establish "Plasma Nano Science", in microscopy AFM). Chemical bonding states of the nano
which the process results are essentially characterized by surface layer of polymers exposed to plasmas were
the basic elements of processes rather than the conventional analyzed using x-ray photoelectron spectroscopy (XPS).
process parameters involved in the apparatus. For the
breakthrough of the next-generation plasma nano Top view
technologies, we have developed a plasma-process analyzer Substrate holder
300
based on the combinatorial methods, in which a variety of
process results can be efficiently analyzed via inclination of
process parameters (ion flux, radical flux) along the Langmuir probe
substrate. In this paper, combinatorial analysis of plasma-
200
70
polymer interactions has been carried out in terms of

Antenna
etching characteristics and chemical bonding states of
polymers to show efficiency and effectiveness for basic data
acquisition.
Side view
2. Experimental
Figure 1 shows the plasma reactor for sustaining
100
Antenna
plasmas with density gradient via localized power
180
200
deposition of RF power through inductive coupling with a 40

LIA module. The LIA module consisted of a U-shaped Langmuir probe
copper tube covered with a quartz tube, which allow low-
voltage and high-density plasma production [2]. The LIA
Substrate holder
with 70 mm width and 100 mm length was located at x =
260 mm on a top flange of the chamber with a horizontal x (mm)
length (in the direction of density inclination) of 300 mm 0 300
and a width of 200 mm. The LIA was coupled to an RF Fig. 1 Schematic diagram of combinatorial plasma process
power generator at 13.56 MHz via a matching network. chamber.
** Dpt. of Electronics, Kyushu University, Fukuoka, Japan Japan
*** PLANT, Nagoya University, Nagoya, Japan
**** JST, CREST
250
Combinatorial analysis of plasma-polymer interactions for formation of inorganic-soft materials
hybrid structure
(b)
(a)
Fig. 2 Typical AFM images of polymers with

ith and
d without
ith t argon-
oxygen mixture plasma exposure.
3 0.6
2.5 C-O/C-C
Intensity ratio
0.5
Ra (nm)
C-O/C-C
2 0.4
1.5 0.3 raw
1 0.2 88W
0.5 175W
0.1
0 350W
350
0
O=C-O/C-C
Intensity ratio
RSm (nm)
300 0.5
O=C-O/C-C
250 0.4
200 raw
150 0.3
88W
100 175W 0.2
50 350W 0.1
0
10
-2
10
-1 0
10 0
10-2 10-1 100
Iis (mA) x Time (min) Iis (mA) x T (min)
Fig. 3 Variation of surface roughness Ra and average Fig. 4 Variation in deconvoluted peak-area ratio of IC-O/IC-C
peak interval RSm of polymers on the product of and IO=C-O/IC-C as a function of the product of (ion
(ion saturation current Iis) x (plasma exposure saturation current Iis) x (plasma exposure time T) as a
time T) as a measure of the ion dose. measure of the ion dose onto the PET surface.
The XPS analyses were performed in AXIS-165x PET films and the PET surface located at x = 220 mm (I is =
spectrometer (SHIMADZU corp., JAPAN) with non- 0.43 mA) which was exposed to argon-oxygen plasma for 1
monochromatized MgKa radiation (photon energy of min. After exposure to the argon-oxygen plasma, the PET
1253.6 eV). surface showed enhancement in surface roughness (R a ) and
suppression of average peak interval (R Sm ) as can be seen in
3. Results and discussion AFM images. Figure 3 shows dependence of the surface
In order to investigate characteristics of argon/oxygen roughness (R a ) evaluated from the AFM images on ion
mixture plasmas, plasma parameters were measured for saturation current x exposure time corresponding to ion
argon/oxygen mixture plasmas. Considerable gradients of dose. The R a of the PET surface after plasma exposure
plasma density were obtained by localized power slightly increased with increasing ion dose, while the R Sm
deposition profiles (not shown here). Based on the results considerably decreased with increasing ion dose.
in terms of ion-saturation current density, analysis of Thr deconvoluted peak-area ratio of the C-O bond to
plasma-polymer interactions has been carried out in terms the C-C bond (I C-O /I C-C ) and O=C-O bond to the C-C bond
of etching characteristics and chemical bonding states. (I O=C-O /I C-C ) are evaluated and are summarized in Fig. 4 as
In order to examine the influence of plasma exposure a function of the product of the ion saturation current I is and
time on morphological change of polymers, the plasma- the plasma exposure time T as a measure of the ion dose
exposed surface was imaged with AFM. Figure 2(a) and onto the samples from the typical XPS C1s spectra of PET
(b) shows typical AFM images of the original surface of the films. These results indicate that the increase of the peak-
251
area ratio I C-O /I C-C is considered to be due to C-O bond ion dose. The XPS results showed almost linear
formation either via the side-band scission of the O=C-O dependence with increasing ion dose. The data points
bond and/or via the incorporation of oxygen radicals and/or obtained from three independent batches of experiments
ions through chemical reactions on the surface. with 5 samples showed universal relations, indicating
efficiency of the combinatorial method for effective basic
4. Conclusions data acquisition.
Combinatorial analysis of plasma-polymer interactions
with combinatorial plasma-process analyzer has been References
carried out in terms of etching characteristics and chemical [1] International technology roadmap for semiconductors, 2007
bonding state of polymers. Surface roughness of the edition, Executive summary.
polymer slightly increased with increasing ion dose, while [2] Y. Setsuhara, T. Shoji, A. Ebe, S, Baba, N. Yamamoto, K.
the average peak interval considerably decreased with Takahashi, K. Ono, and S. Miyake, Surf. Coat. Technol.,
174-175 (2003), pp. 33-39.
252
†

KUSUMOTO Kazuomi *, SUN Hao * and ISHIKAWASatoshi *
KEY WORDS: (Plasma arc) (Drilling) (Hole formation) (Dross) (Molten metal)
1. Introduction
Recent thermal processes for drilling, such as laser
drilling and plasma arc drilling, are challenging the
traditional drilling methods. Laser drilling has high speed
and high precision for thin plates of almost all materials,
while plasma arc drilling has high speed and a high material
removal rate for thick plates of almost all metals.
The mechanisms of thermal drilling differ from those of
traditional drilling methods. Laser drilling as a
representative thermal process has been widely investigated.
Melt ejection during laser drilling of metals has been
observed and analyzed by high-speed photography,
showing a significant mechanism of material removal [1]. Fig. 1 Experimental setup.
When melt ejection occurs, spatter or dross readily forms at
the entrance and exit sides of the hole. The characteristics 3. Results and discussion
of spatter formation and its prevention have been Hole formation in plasma arc drilling is dependent on
investigated in detail [2, 3]. Furthermore, phenomena the removal of molten metal. Observations were carried out
accompanying hole formation, such as the flow velocity of at the upside and downside positions of the hole.
molten material and heat flow models, have also been Representative photographs are shown in Fig. 2. The
discussed [4, 5]. observation results show that the quantity of residual
The geometrical characteristics and drilling molten metal around the entrance hole increases with the
performance of the plasma arc drilling method were passage of processing time before the penetration time of
investigated in our previous studies [6, 7]. However, the 0.7 s. Subsequently, the quantity of residual molten metal
mechanism of hole formation during plasma arc drilling has remains almost unchanged and its temperature falls with the
not yet been fully elucidated. We therefore used a high- passage of processing time, as shown by the brightness of
speed video camera to observe and analyze the process of the white region. The process of ejection at the exit side
drilling under different conditions. The results obtained differs from that at the entrance side. Initially, the molten
confirm the mechanisms of the hole formation process, metal inside the hole is entirely blown away in the form of a
ejection of molten metal, and dross formation. cloud without residue immediately after penetration occurs.
This is because of the large internal pressure of the hole.
2. Experimental procedure Then, with the increase in the exit hole diameter, the
The setup for our plasma arc drilling experiments internal pressure decreases, leading to a reduction in the
consisted of a power supply device, gas supply device,
water-cooled tool, work-piece fixture, and time control
switch, as shown in Fig. 1. A high-speed video camera was
employed to observe the process of plasma arc drilling from
different positions (upside, horizontal, and downside). The
photographic conditions of the camera were fixed at a
frame rate of 2000 f/s and a shutter speed of 1/272,000 s. A
number of observational experiments were conducted by
varying the arc current (100, 120, 140 A) and torch height
(6, 8, 10 mm). Sequences of photographs with the passage
of time were obtained to analyze the drilling process.
Fig. 2 Ejection of molten metal at an arc current of

140 A and torch height of 6 mm.

* Graduate School of Engineering, Gunma University, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
253
ejection of molten metal. As a consequence, molten metal Fig. 5 shows the representative appearances of a hole
begins to remain at some specific positions around the exit with dross and after dross removal at both the entrance and
side.In order to clearly observe the evolution of hole exit sides. Circular dross was formed around the entrance
formation, we conducted a series of drilling experiments at hole, while partial dross was produced around the exit hole.
the end surface. Representative photographs, which reveal Although the amount of residual dross at the entrance side
the processes of metal melting and hole formation, are is greater than that at the exit side, it is relatively easy to
shown in Fig. 3. The situation of metal removal and the remove. Comparing the appearances of both the entrance
development of the hole shape with the passage of and exit sides after the dross is removed, it can be seen that
processing time can be clearly observed. The hole shape the entrance side is cleaner while some indelible dross still
changes from a blind taper hole to a taper hole, then a remains at the exit side. This can be explained by the
cylinder hole, and finally a reverse taper hole. When the mechanism of ejection of the molten metal. As a
drilling processes under different conditions are compared, consequence of prolonged continuous processing, residual
the evolution of the hole is seen to be faster at the larger arc hot molten metal constantly remains around the exit side
current and lower torch height. Based on the above until the drilling is completed. The work-piece is partly
observations, the mechanisms of hole formation and melted and fuses with the residual molten metal. The
ejection of molten metal are simulated in Fig. 4. The combination makes dross removal difficult. At the entrance
plasma ejected from the nozzle heats the work-piece to side, however, the work-piece is not fused with the residual
melting point or boiling point. The molten metal is ejected molten metal, with the result that the dross and the work-
from the entrance side by the high-pressure gas (a). piece are readily separated.
However, because of its viscosity, the molten metal is not
entirely blown away and some remains around the entrance
side of the hole before penetration occurs (b). After
penetration, almost all of the molten metal is ejected from
the exit side (c), and the quantity of molten metal at the
entrance side thus remains unchanged. With the passage of
processing time, the exit hole diameter continues to enlarge
(d), with a cylinder hole (e) and then a reverse taper hole (f)
being formed. Meanwhile, some of the molten metal
remains around the exit hole.
Fig. 5 Appearance with dross and after dross removal of a

hole produced at an arc current of 140 A, torch height of
6 mm, and processing time of 2.7 s.
In addition to the above findings, a peculiar

phenomenon observed inside the hole is a discharge from
the plasma arc, in which an anode spot moves on the hole
inwall at super-high speed. A representative anode spot is
shown in Fig. 6. The discharge contributes to local thermal
input in the metal removal process. Moreover, the electric
attraction assists in removing part of the molten metal
accumulated around the exit side.
Fig. 3 Observations of hole formation on the end surface.
Fig. 6 Representative anode spot.
4. Conclusion
Fig. 4 Mechanisms of hole formation and ejection of The process of hole formation during plasma arc
molten metal. drilling was observed using a high-speed video camera. The
254
evolution of the hole from a blind taper hole to a taper hole, [2] D. K. Y. Low, L. Li, A. G. Corfe: J. Mater. Process. Tech.,
cylinder hole, and reverse taper hole was clearly observed 118 (2001), pp. 179-186.
under different conditions. The mechanisms of hole [3] D. K. Y. Low, L. Li, P. J. Byrd: J. Mater. Process. Tech., 139
formation with the passage of processing time and ejection (2003), pp. 71-76.
[4] C. F. Cheng, Y. C. Tsui, T. W. Clyne: Acta Metall. Mater. 46
of molten metal at the entrance and exit sides were clarified
(1998), p. 4273.
by analysis of the process phenomena. An understanding of [5] A. Luft, U. Franz, A. Emsermann, J. Kaspar: Appl. Phys. A,
these mechanisms will be useful to improve hole quality 63 (1996), p. 93.
and reduce dross around the hole. [6] K. Kusumoto, H. Sun: Nat’l. Meeting of JWS, 82 (2008-4), pp.
114-115.
References [7] H. Sun, K. Kusumoto: Nat’l. Meeting of JWS, 83 (2008-9), pp.
[1] K. T. Voisey, S. S. Kudesia, W. S. O. Rodden, D. P. Hand, J. 74-75.
D. C. Jones, T. W. Clyne: Mater Sci Eng, A356 (2003), pp.
414-424.
255
†
Prediction of ion engine lifetime
NAKANO Masakatsu *
KEY WORDS: (Prediction) (Numerical simulation) (Lifetime) (Grid erosion) (Sputtering) (Ion engine)
1. Introduction Since grid erosion occurs very slowly, taking several

Ion engines are a form of electric propulsion used for tens of thousands of hours to become life-threatening to ion
spacecraft that generate thrust by accelerating ions. engine operation, simulation of grid erosion is essential for
Although ion engines can generate very high specific cost-effective design and development of ion engines. In
impulses, they produce much lower thrusts than this study, numerical simulations are performed to assess
conventional chemical rockets. Consequently, ion engines grid lifetime.
have to be operated for a very long time to achieve the
velocity changes required by a particular mission. 2. Physical and numerical models
In June 2010, the Hayabusa spacecraft returned to Earth Figure 2 shows the computational domain and its
after completing a seven-year mission. The ion engines on boundaries. The symmetry of the grid hole distribution
the Hayabusa spacecraft (P10 ion engines) had been permits the computational domain size to be reduced to
operated for more than 40,000 hours in space. Prior to the 1/12 of a grid hole. The simulation employs the finite
element method and the domain is covered with a mesh of
flight, the P10 ion engines had been subjected to a series of
eight-node hexahedral elements.
18,000 h ground-based lifetime tests.
The electrostatic potential in the computational domain
These lifetime tests represent a major hurdle to using
can be calculated using Poisson’s equation. The ion density
ion engines in the future because they are prohibitively
term of Poisson’s equation is obtained from the beam
time consuming and expensive. If lifetime tests are required
current, the velocity, and the stay times of the ion beams
after making minor improvements to an ion engine, it will
passing through the elements. The electron density is
be practically impossible to modify and improve ion
evaluated using the Boltzmann relation based on the
engines. To increase the use of ion engines, it is thus
potential difference from the local plasma. Grid voltages
essential to both shorten the lifetime verification process
are specified at the boundaries that represent the screen,
and lengthen the lifetimes of ion engines.
accel and decel grid surfaces. The plasma potential is
Particles (ions and neutrals) produced by charge-
applied for the inlet boundary and the zero Neumann
exchange and elastic collisions in ion engines can be
boundary condition is specified for other boundaries.
directed toward the accel and/or decel grid with very high
Poisson’s equation is discretized using the normal finite
energies, which can cause grid erosion (see Fig. 1). End of
element method and the resulting simultaneous equations
life is reached when either the holes in the accel grid
are solved iteratively by the incomplete Cholesky conjugate
become so large that ion extraction is greatly affected by
gradient method.
electron backstreaming or structural failure occurs in the
Ion beams are injected from the upstream boundary.
grid. Grid erosion is unavoidable and it is the principle life-
The inlet velocities of the ions are determined to satisfy the
limiting factor in ion engines.
Bohm sheath criterion. Each ion beam trajectory is
Screen grid Accel grid Decel grid calculated from the equations of motion for electrostatic
particles.
C The amounts of sputtering particles generated by
Discharge
plasma Xe+
Charge-exchange Xe Neutralizing
and/or Elastic Collisions C plasma
C Xe+
Xe+
C
Ion sheath Xenon ion
Xe+
XeXenon neutral
C Grid material
Fig. 1 Grid erosion mechanism in ion engines. Fig. 2 Computational region.

* Tokyo Metropolitan College of Industrial Technology, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Tokyo, Japan Japan
256
BOL After 20,000 h

Fig. 3 (a) Grid surfaces and erosion intensities in the high beam BOL After 20,000 h
current region for I a = -350 V.
Fig. 5 (a) Grid surfaces and erosion intensities in the low beam
current region for I a = -350 V.
Potential distribution Ion beam trajectories
Fig. 3 (b) Potential distribution and ion beam trajectories in the

high beam current region for I a = -350 V.
50 Downstream view Diagonal view.

Mimimum pontetial on axis [V]
0
Fig. 5 (b) Decel grid after 20,000 h of operation for I a = -350 V.
-50 accumulated operating time reaches the specified value. A
detailed description of the simulation is given in Ref. 1.
-100
-300 [V]
-150
-350 [V] Parametric calculations for the P20 ion engine grid were
-200 -400 [V] performed by varying the accel grid voltage. Calculations
-450 [V] were performed for high and low ion beam currents and a
-250 fixed total acceleration voltage. Detailed grid and operation
0 10000 20000 30000 40000 parameters are given in Ref. 2.
Operation time [hrs] Figure 3(a) shows the grid surfaces and erosion
Fig. 4 Minimum potential on axis. intensities for grid holes in the high ion beam current
region at the beginning of life (BOL) and after 20,000 h of
charge-exchange and elastic collisions are evaluated from operation. The downstream edge of the accel grid hole is
the ion beam current, collision cross section, and local severely eroded, which may lead to electron backstreaming.
neutral density. Neutral densities are obtained prior to Fig. 3(b) represents the potential distribution and ion beam
performing the potential and beam trajectory calculations trajectories. From the figure, the downstream edge erosion
using the free molecular flow approximation. Sputtering of of the accel grid is explained by the impact of cross-over
the grid material is incorporated using experimental data in ions.
the form of tables of values for incident energies and Figure 4 shows the variation of the minimum
incident angles. Since redeposition of the sputtered grid electrostatic potential on axis as a function of the
materials is a very complex process that involves accumulated operating time for I a = -300 to 450V. If
interactions between the incident sputtered particles and the electron backstreaming is assumed to occur when the
grid surface atoms, it is modeled by a simplified approach minimum axial potential exceeds -T e [V] (T e : electron
using a sticking factor, in which the redeposition flux is temperature), the lifetimes are predicted to be about 14,000
given by the product of the incoming sputtered particles h for I a = -300 V, 32,000 h for I a = -350 V, and over
and the sticking factor.
40,000 h for I a = -400 and -450 V.
The grid surface profile is updated from the rate of
Figure 5 shows the grid surfaces at the BOL and at
change of the grid surface obtained by the sputtering and
after 20,000 h of operation for grid holes in the low ion
redeposition calculations. This update is repeated until the
beam current region. Since ion beams tend to diverge at
257
lower beam currents, the inner surfaces of the accel and (2) Two major failure modes (electron backstreaming and
decel grids are significantly eroded and the decel grid is structural failure) of the P20 ion engine were
close to structural failure due to six-point star-shaped successfully analyzed.
erosion. (3) Using numerical simulations accelerates the lifetime
Based on these simulations, it is concluded that the end verification process by two orders of magnitude or more.
of life of the grid holes in the high beam current region is
caused by electron backstreaming, whereas the end of life Acknowledgement
of the grid holes in the low beam current region is caused This study was performed under a corporative research
by structural failure of the decel grid in the P20 grid system. program with JAXA. The author thanks Prof. Nishiyama
The total calculation time was about one week using a for providing the P20 ion engine data.
PC (Intel Core i7 965), which is two orders of magnitude
smaller than actual lifetime tests. References
[1] M. Nakano: Vacuum 83 (2008), pp. 82-85.
4. Conclusions [2] K. Nishiyama, Y. Toyoda, S. Hosoda, Y. Shimizu, and H.
The following conclusions were obtained: Kuninaka: Journal of Plasma and Fusion Research SERIES, 8
(2009), pp.1590-1594.
(1) Numerical simulations can be employed to determine
the lifetimes of ion engines.
258
Materials joining technologies and interface science for integration

†
of novel structured metallic and inorganic materials
SETSUHARA Yuichi *, NAKATA Kazuhiro *
KEY WORDS: (Materials Joining and Welding) (Laser processes) (Plasma processes) (Friction stir welding)
(Nanoparticles)
1. Research Activities of JWRI, Osaka University 3. Research Division of Materials Joining Mechanism
Since the foundation originally as “Welding Research This division has devoted research activities for
Laboratory” in 1969 at Osaka University, the Joining and investigation of the physical and chemical properties of
Welding Research Institute (JWRI) has devoted research high performance joints and composites produced by
activities to better understanding of fundamental welding and joining, and the control of the joint
mechanisms involved in joining and welding science and microstructure by highly-controlled material processing.
development of industrial technologies in wide scales of The results of these investigations have been applied to
structures ranging from huge constructions including the designing and development of optimum materials for
nuclear power plants, ships and tall buildings to micro and joining and welding. Investigation is also made of the
nano-scales including microelectronic devices and modification of the joint microstructure by well-controlled
nanoparticles, as key technologies for manufacturing materials processing using laser and thermal energies.
functional structures.
With a variety of high-energy-density beams (arc 4. Research Division of Functional Assessment
discharge, lasers and electron beams) as well as other types The structures studied in this division are not only
of heat source including frictional heat, JWRI has carried large-size welded structures including ships, bridges, and
out investigations on welding and joining, creation of nuclear reactors, but also microelectronic and nano
advanced materials and composites, highly functional structures, which have specific structures and functions, and
surface modifications, and development of novel frontier structures used in space and in the deep sea. The
technologies including space welding. researches progress under the balance between social
Since the restructuring of the JWRI in 1996, the JWRI usefulness and the conservaton of environment and
has consisted of three divisions (the research division of resources.
Materials Processing System, the research division of
Materials Joining Mechanism, and the research division of 5. Smart Processing Research Center
Functional Assessment) and the Smart Processing Research The Smart Processing Research Center was established
Center. in 2003 by consolidating two centers, i.e., the Research
Center for Ultra High Energy Density Heat Source, and the
2. Research Division of Materials Processing System Research Center for Materials Recycling and Integration, to
This division is oriented to provide scientific bases for develop advanced processes for nano and micro-structured
generation, conversion, transfer of processing energy materials, thereby contributing to the establishment of next
sources and interaction with materials for well-controlled
multi-functional processes and development of high-quality
energy sources suitable for various materials processing.
In particular, the division has made great contributions
to development of various advanced materials processing
systems with concentrated and dispersed energy sources,
which are expected to have wide application fields in the
future. Major emphasis is placed on the developments of
advanced monitoring and estimating techniques for material
processing and the systematization of the functional
materials processing technology through interpretation of
phenomena relating to the high energy involved in the
processing.
Fig. 1. Cooperation of the six Research Institutes.

Japan
259
Materials joining technologies and interface science for integration of novel structured metallic and inorganic
materials
generation manufacturing that can encourage industries to 7. Global Collaborative Research Center for Computational
minimize any negative impact on the environment. Welding Science (CCWS)
To establish the advanced science and technology in the The JWRI proposed the concept of computational
global research field of welding and joining processes, welding science as early as the 1970’s. It is one of the
JWRI is making continuous and significant efforts to obtain world pioneers in this field and has organized an
instructive and informative R&D results by intelligent international symposium on “Theoretical Prediction in
innovation. Joining and Welding” in 1996. In further development of
computational welding science, JWRI conducted a project
6. Development Base of Advanced Materials on “Development of Highly Efficient and Reliable Welding
Development and Integration of Novel Structured Technology” which has been supported by the New Energy
Metallic and Inorganic Materials and Industrial Technology Development Organization
The project, Development Base of Advanced Materials (NEDO). One of the main objectives of this project is to
Development and Integration of Novel Structured Metallic establish a framework of the computational welding science
and Inorganic Materials (Fig. 1), started in 2010 as inter- which covers the entire aspects of welding, i.e. Welding
university cooperative research project (Joining and Process, Welding Metallurgy and Welding Mechanics. This
Welding Research Institute, Osaka Univ., Institute for framework has been further developed to meet various
Materials Research, Tohoku Univ., Materials and demands from the industry.
Structures Laboratory, Tokyo Institute of Tech., Eco Topia
Science Institute, Nagoya Univ., Institute for Nanoscience 8. Research Activities for the Project “Advanced
and Nanotechnology, Waseda Univ., Institute of Materials Development and Integration of Novel
Biomaterials and Bioengineering, Tokyo Medical and Structured Metallic and Inorganic Materials”
Dental Univ.). This development base promotes the joint In the present project, research and development
research for development of new functional materials by activities are underway in the following fields of
integration of novel structured metallic and inorganic investigations; 1) Development of Materials for
materials for applications in the specific fields including Environment and Energy System, 2) Development of
environment&energy, electronics, and biomedical materials Electronics Materials, 3) Development of Bio-Medical
through the inter-university cooperative researches. Materials, 4) Development of Novel Structured Advanced
Materials and Integration Technologies.
Fig. 2. Nano-particle based technologies.
Fig. 3. Soldering technologies. Fig. 4. Friction stir welding of bulk metallic glasses.
260
In the research field for Environment and Energy technologies. For the development of Bio-Medical
System, JWRI is to contribute to develop Environment Materials, JWRI is to make approaches via nano-particle
and Energy Systems with metallic glasses and advanced technologies and bio-ceramics coating with advanced
ceramics via nano-assembly technologies (nano-particles, surface modification technologies.
slurry and casting, Fig. 2), micro-assembly technologies, Furthermore, in the field of Development of Novel
dissimilar materials joining technologies based on laser Structured Advanced Materials and Integration
welding and nano-surface modification with advanced Technologies, a variety of research activities are to be
plasma processing. carried out for the establishment of scientific and
For development of Electronics Materials, the JWRI is technological bases of joining of metallic glasses and
to contribute to develop device fabrication technologies via advanced ceramics materials. (Fig. 4)
soldering technologies (Fig. 3) and plasma processing
261
Cooperative researches in Tohoku University†
FUKUHARA Mikio*
KEY WORDS: (Cooperative research) (6 Universities) (Environment and energy materials) (Electronic
materials) (Bio- and medical materials) (Tohoku university’s activities)
1. Introduction specialized fields, as a leader of the practical use

We started a new project, “Advanced Materials acceleration group. The organization table is presented at
Development and Integration of Novel Structured Metallic Table 1.ᴾ ᴾ ᴾ ᴾ ᴾ
and Inorganic Materials” from April of 2010 to March of
2015, under cooperative researches by six-leading ᴾ Table 1 Organization table for project activity in IMR of
universities which stand for materials research in Japan. Tohoku University
Before this project, we have successfully run the previous Project Group Name group leader content
project, “Research and Development Project on Advanced Environment and Prof. Dr. fuel cells and
Metallic Glasses, Inorganic Materials and Joining energy materials W.Zhang catalytic
Technology” for five years [1-5]. According to its results,
we focus on three priority research fields of environment materials
and energy, electronics, and bio- and medical materials in Electronic materials Prof. Dr. M. development of
the current project. Nagoya University, Waseda Fukuhara glassy alloy
University and Tokyo Medical and Dental University electronics
(TMDU) were respectively nominated as powerful
universities.ᴾ The summary figure is schematically shown in Bio- and medical Prof. Dr. G. development of
Fig.1. materials Xie bio- and medical
We have published a large number of academic papers materials
and made application for patents under three university’s
cooperation. We have also conducted personal exchanges Practical use Prof. Dr. X. application of
during 5 years. acceleration Wang three fields
2. Project activity of Tohoku University

Our project members of the Institute for Materials 3. Future schedule of the project
Research (IMR) in Tohoku University have been We have plans to have academic activities per year as
researching in collaboration with members of Osaka follows:
University, Tokyo Institute of Technology (TIT), Nagoya 1. International Conference: Visual JW2010, Nov.2010,
University, Waseda University and Tokyo Medical and Osaka
Dental University(TMDU). 2. Opening Conference: March 10, 2011, Tokyo, Tokyo.
Prof. Dr. Zhang’s group has studied glassy alloys as 3. Field Meetings of three fields: 3-4 times/year
constituent materials for fuel cells and catalytic materials in 4. The Steering Committee: Tokyo.
cooperation with EcoTopia Science Institute (ESI) of 5. Research Report of Cooperative Project: the end of
Nagoya University. March, 2011.
Prof. Dr. Fukuhara’s group has devoted itself to the
development of glassy alloy electronics (single electron References
transistors) which were the initiative of the Institute for [1] Research Report of Cooperative Project,1, Tohoku University
(2006).
Nanoscience and Nanotechnology (INN) of Waseda
[2] Research Report of Cooperative Project,2, Tohoku University
University. (2007).
Prof. Dr. Xie group’s members have engaged in glassy [3] Research Report of Cooperative Project, 3, Tohoku University
alloy development as main materials for bio- and medical (2008).
materials which are under the conduct of Institute of [4] Research Report of Cooperative Project, 4, Tohoku University
Biomaterials and Bioengineering (IBB) of Tokyo Medical (2009).
and Dental University. [5] Research Report of Cooperative Project, 5, Tohoku University
Prof. Dr.Wang has organized application of these (2010).

*ᴾ IMR, Tohoku University, Sendai, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
262
Cooperative researches in Tohoku University
Advanced Materials Development and Integration of Novel

Strucctured
ctur Metallic and Inorganic Materials Project
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Fig.1 The summary figure of the 2nd project, “Advanced Materialsᴾ Development
and Integration of Novel Structured Metallicᴾ and Inorganic Materials” derived
from the 1st projectᴾ “Research and Development Project on Advanced Metallicᴾ
Glasses, Inorganic Materials and Joining Technology”.
263
Approach for the project on advanced materials development and

integration of novel structured metallic and inorganic materials by
materials and structures laboratory of Tokyo Institute of
†
Technology
OKADA Kiyoshi *
KEY WORDS: (Advanced inorganic materials) (Novel structures) (Environment) (Energy) (Electronics)
(Biomaterials)(MSL) (Tokyo Tech)
1. Introduction 2. Organization for the AMDINSMIM project in the

The Materials and Structures Laboratory (MSL) of MSL
Tokyo Institute of Technology is one of the nationwide The number of members joined in the last project was
collaborative research institutes in Japan covering the fields about 25, involving most of the academic members in the
of inorganic materials and building materials since 1996 [1]. MSL. We especially encouraged the young members in the
The MSL performed the special collaborative project on MSL to challenge new research topics considered from
Metallic Glass-Inorganic Materials Joining Technology their fresh ideas.
Development (MGIMJTD) with two other nationwide In the present project, we selected only 17 members
collaborative research institutes, the Institute for Materials based on their applied proposals because the budget size for
Research (IMR) of Tohoku University and the Joining and the MSL was greatly decreased. The project organization in
Welding Research Institute (JWRI) of Osaka University the MSL is shown in Fig. 1. We have a steering committee
from 2005 to 2009 [2]. Based on a lot of fruitful results for this project chaired by the director of the MSL. This
obtained by this special project, the MSL, IMR and JWRI committee receives the activity reports from the project
agreed to progress the project to the second stage for group and gives advise to the group. The project group has
realizing the outcomes of the first project by making a new one project leader and two sub-leaders to organize the
group with three institutes specialized in the environment, project. The leader is Professor F.Wakai and sub-leaders
Eco Topia Science Institute (ETSI) of Nagoya University, are Professors T.Kamiya and N.Matsushita. The 17 project
nanotechnology, Institute for Nanoscience and members are divided into the above mentioned four
Nanotechnology (INN) of Waseda University, and bio- research fields, i.e. three members in the environment and
medical materials, Institute of Biomaterials and energy materials, four members in the electronics materials,
Bioengineering (IBB) of Tokyo Medical Dental University five members in the bio and medical materials and five
from 2010. members in the novel structured materials. We selected a
A new special project, Advanced Materials head in each research field to effectively progress their
Development and Integration of Novel Structured Metallic research topics and organize their fields.
and Inorganic Materials (AMDINSMIM) is strongly
Project group
focused to four research fields, i.e. (1) environment and Leader: F.Wakai
Report
Steering Committee
energy materials, (2) electronics materials, (3) bio and Advise Chair: K.Okada
Sub-Leader: T.Kamiya & N.Matsushita
medical materials and (4) novel structured materials. Many
topics will be performed by collaborative works with some
Environment & Electronics Bio & Medical Novel Structured
member institutes in the AMDINSMIN project. Thus, MSL Energy Materials Materials Materials (5) Materials (5)
will have strong contact especially with the ETSI in the first (3) (4)
Associate Prof. Prof. F.Wakai
research field, with the INN in the second research field, Prof. K.Okada Prof. T.Kamiya N.Matsushita Associate Prof.
Prof. J.Tanaka T.Akatsu
with the IBB and IMR in the third research field and with Associate Prof. Associate Prof.
Associate Prof. Associate Prof.
K.Hayashi T.Taniyama
the JWRI in the fourth research field. Asistant Prof. Associate Prof. T.Ikoma H.Kawaji
The organization of the project group in the MSL and K.Katsumata Y.Matsumoto Associate Prof.
T.Susaki
Associate Prof.
T.Atou
research topics planned for this AMDINSMIN project are Associate Prof.
Assistant Prof. Assistant Prof.
T.Sasagawa
briefly introduced in this presentation. T.Yoshioka Y.Shinoda
Fig. 1 Line-up for the project in the MSL.

* MSL, Tokyo Institute of Technology, Yokohama, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
264
Approach for the project on advanced materials development and integration of novel structured metallic and
inorganic materials by materials and structures laboratory of Tokyo Institute of Technology
3. Research topics in the MSL institutes are very important to enhance our research works
The main topics planned in this special project at the toward the goal.
MSL are listed in Table 1.
Environment and energy materials: Since the main topics in References
this field are focused on the materials related to fuel cells [1]E.Yasuda (eds): Ceramics and Building Materials, Yokohama,
organized by the ETSI, we will investigate a material for Materials and Structures Laboratory, (2004).
separators using metallic glasses [3]. On the topics related [2] A.Inoue (eds): Research Result Report of Metallic Glasses,
Sendai, Tohoku University, (2010).
to the environment, a collaborative work on oxidation
[3] K.Katsumata, T.Wada, A.Inoue, M.Sakai, A.Nakajima,
catalyst using mayenite type compounds [4] will be A.Fujishima, N.Matsushita and K.Okada: Abstracts
performed with the ETSI. Book STAC-4, Yokohama, (2010), pp.
Electronics materials: Main part of the work in this field [4]J.Li, K.Hayashi, M.Hirano and H.Hosono: Solid State Ionics,
is preparation and evaluation of photonic, electronic and/or 180 (2009), pp. 1113-1117.
spintronic devices with some novel nanostructures by [5]T.Kamiya, K.Nomura and H.Hosono: Phys. Status Sol. A, 206
combinations of inorganic materials, semiconductors and/or (2009), pp. 860-867.
metals [5-8]. Since these devices consist of multi-thin film [6]T.Taniyama, K.Akasaka and M.Itoh: J. Appl. Phys., 105
nanotextures, strong collaboration with the INN group is (2009), pp. 07D901-1-3.
[7]R.Takahashi, M.Katayama, O.Dahl, J.K.Grepstad,
essentially important.
Y.Matsumoto and T.Tybell: Appl. Phys. Lett., 94 (2009), pp.
Bio and medical materials: Preparation and biomedical 232901.
evaluation of Ti based bulk metallic glasses (BMGs) having [8]I.M.Vishik, E.A.Nowadnick, W.S.Lee, Z.X.Shen, B.Moritz,
nanostructured bioactive surfaces is the main topic and this T.P.Devereaux, K.Tanaka and T.Sasagawa: Nature Phys., 5
will be performed by collaborative team of the MSL, IMR, (2009), pp. 718.
IBB and JWRI. The MSL will mainly take a part of [9]N.Sugiyama, H.Xu, T.Onoki, Y.Hoshikawa, T.Watanabe,
preparation of nanostructured bioactive surfaces on the Ti- N.Matsushita, X.Wang, F.X.Qin, M.Fukuhara, M. Tsukamoto,
BMGs using hydrothermal and/or electro-hydrothermal N.Abe, Y.Komizo, A.Inoue and M. Yoshimura: Acta
techniques [9,10]. Evaluation of bioactivity of oxide thin Biomater., 5 (2009), pp. 1367-1373.
films controlling their atomic precisions [11] is a new [10] T.Onoki, T.Higashi, X.Wang, S.Zhu, N.Sugiyama, Y.
Hoshikawa, M.Akao, N.Matsushita, A.Nakahira, E. Yasuda,
challenging work in this field. M.Yoshimura and A.Inoue: Mater. Trans., 50 (2009), pp.
Novel structured materials: Relatively wide topics are 1308-1312.
proposed in this field but main topics will be focused on [11]T.Susaki, S.Kumada, T.Katase, K.Matsuzaki, M. Miyakawa
control of interfaces for developing novel structured and H.Hosono: Appl. Phys. Exp., 2 (2009), pp. 091403.
materials [12-14]. The topics related to joining of different [12]Y.Shinoda, Y.Yanagisawa, T.Akatsu, F.Wakai and H.Fujii:
materials will be performed collaboratively with the JWRI. Mater. Trans., 50 (2009), pp. 1250-1254.
[13]N.Kawai, T.Atoh, K.G.Nakamura, K.Kondo, S.Ito, K. Yubuta
4. Conclusions and M.Kikuchi: J. Appl. Phys., 106 (2009), pp. 23525.
In the present project, clear outcomes developed to [14]T.Yoshida, Y.Moriya, T.Tojo, H.Kawaji, T.Atake and
Y.Kuroiwa: J. Therm. Anal. Calor., 95 (2009), pp. 675-683.
actual materials contributing to our society are strongly
requested. Strong collaborations with the six member
Table 1 The research topics of the project in the MSL
Field Name Title of the topics

K.Okada Surface treatment of metallic glasses and its property change for fuel cell applications
Environment and
K.Hayashi Catalytic properties of mayenite type Sr12Al14O33 (S12A7)
Energy Materials
K.Katsumata Environmentally benign optical materials by novel nanostructures
T.Kamiya Inorganic material/metal/semiconductor novel structures for photonic and electronic devices
PLD synthesis of metallic glass/oxide novel structures and its new function as environmental
Y.Matsumoto
Electronics catalysts
Materials Control of magnetic anisotropy in ferromagnetic metal/ferroelectrics/semiconductor hetero-
T.Taniyama
structures for spintronic devices
T.Sasagawa Impacts of anisotropic lattice deformations on the electronic functions at the heterointerfaces
N.Matsushita
J.Tanaka Ti based bulk metallic glasses having nanostructured bioactive surfaces and its applications
Bio and Medical
T.Ikoma for artificial dental roots
Materials
T.Yoshioka
T.Susaki Medical application of oxide thin films with atomic precision
F.Wakai Joining process technology of interfaces between different phases
T.Akatsu Superior ceramic coatings on a metal substrate through plasma electrolytic oxidation
Novel Structured
Y.Shinoda Development of creep resistant titanium carbide cermets
Materials
H.Kawaji Relaxization mechanisms of metallic glasses and development of high functional materials
T.Atou Shock-assisted joining between metallic glasses and ceramics
265
Synthesis and properties of hybrid-type polymer membranes for

†
fuel cells
YOGO Toshinobu *
KEY WORDS: (Fuel Cell) (Hybrid) (Membrane) (Proton Conductivity)
1. Introduction copolymerization reaction followed by sol-gel reaction.

Fuel cell technology has been considered a promising Each styryl-substituted alkoxysilane (DMMSMS(M) or
alternative source for future energy. Growing attention has MDMSMS(D)) was copolymerized with EPA in various
been focused on proton exchange membrane fuel cells monomer ratios using a radical initiator (AIBN). The
(PEFCs) for mobile, stationary and portable electrical samples were labeled with their monomer feed ratios such
devices because of their high energy efficiency and clean as DMMSMS(M) (or MDMSMS(D))/EPA = x/y. The
exhaust. Perfluorosulfonic polymers including Nafion ratio of x/y = 1/2, 1/4, 1/6 were investigated in this study.
have many attractive properties including good mechanical
strength, good chemical stability and high proton 3. Properties of Hybrid Membranes
conductivity, and they are widely used in commercial ᴾ Figure 1 shows the DTA-TG curves obtained for
applications. However, the perfluorosulfonic membranes DMMSMS(M)/EPA(=1/2) and MDMSMS(D)/EPA(=1/2)
have several drawbacks such as complex water management, hybrid membranes with a solid line and a dashed line,
CO poisoning of Pt anode catalysts and high cost. An respectively. Both TG curves for DMMSMS(M)/EPA and
increase in PEFCs operation temperature would allow for MDMSMS(D)/EPA hybrid exhibit first weight losses up to
increased reaction kinetics of the fuel cell, lower around 100ºC. This weight loss is attributed to the loss of
consumption of the platinum catalyst, and a decrease in the absorbed water molecules. The second step ranging from
size of the heat management system. Thus, proton- 100ºC to 300ºC shows a gradual weight loss attributed to
conducting materials of high conductivity at the the loss of chemically bound water. Above 200ºC, water
intermediate temperature range from 100 to 200 ÛC are generated from the condensation of -P(O)(OH) 2 groups isᴾ
required. also lost from the hybrid. The decomposition of
ᴾ ᴾ ᴾ This paper describes the synthesis and characterization membranes starts above 280ºC. The exothermic peaks are
of silica-based inorganic/organic hybrid membranes with also observed with rapid weight losses for both membranes.
chemically bound phosphonic acid. The structure, thermal 120
stability and proton conductivities of hybrid membranes
were analyzed. The H 2 /O 2 fuel cell performances of (a)
membrane–electrodes assemblies (MEAs) were also studied.ᴾ 100
Exo.
(b)
2. Synthesis of Hybrid Membranes 80
Starting compounds for membranes are styryl-
Weight / %
substituted alkoxysilanes and a derivative of acrylic

DTA
phosphonic acid (EPA). The styryl-substituted 60

alkoxysilanes used in this study contain organosilyl groups
of –Si(CH 3 )(OCH 3 ) 2 and –Si(CH 3 ) 2 (OCH 3 ), which are 40
called difunctional (MDMSMS(D)) and monofunctional
Endo.
DMMSMS(M), respectively. The Si-OCH 3 group

undergoes acidic hydrolysis affording a Si-O-Si linkage. 20
Therefore, the structure of the hybrid membrane can be
controlled by the number of alkoxy groups. On the other 0
hand, a derivative of acrylic phosphonic acid used in this 0 100 200 300 400 500
study has an acrylic ester group and a phosphonic acid
Temperature / ºC
group. The acrylic ester group allowsᴾ copolymerization
with other polymerizable groups and the phosphonic acid Fig. 1 DTA-TG curves of hybrid membranes:
group is expected to contribute to proton conduction. (a) DMMSMS(M)/EPA=1/2 and
Hybrid membranes were prepared through (b) MDMSMS(D)/EPA=1/2.
* EcoTopia Sci. Inst., Nagoya University, Nagoya, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
266
Synthesis and properties of hybrid-type polymer membranes for fuel cells
The results confirm that the hybrid membranes possess and Si-O linkage were successfully synthesized via the
sufficient thermal stability up to 200ºC. It is worth noting copolymerization and sol-gel reaction. A phosphonic acid
that the exothermic peak temperatures vary according to the group was immobilized to polymer chain by radical
functionality of the membrane. The DTA curve for polymerization of styryl-substituted alkoxysilane and a
DMMSMS(M)/EPA=1/2 membrane exhibits a peak at derivative of acrylic phosphonic acid (EPA) via a stable C-
328ºC, whereas the curve for MDMSMS(D)/EPA=1/2 P bond. The membranes exhibited good thermal stability,
membrane shows a peak at 348ºC. MDMSMS(D)/EPA which depended on the degree of inorganic chain in the
hybrid membrane has a linear siloxane linkage and a higher hybrid membrane. The proton conductivity depended on
thermal stability than that of DMMSMS(M)/EPA above the temperature and relative humidity. The membranes
280ºC. This result reveals that siloxane chain formed in synthesized from monomethoxysilane derivative were
the membrane improves the thermal stability of the hybrid found to show higher conductivities than those from the
membrane. dimethoxysilane derivative. The membrane exhibited
Figure 2 shows the proton conductivities under good conductivities up to 140ºC at various humidities.
different relative humidities for the hybrid membranes of The hybrid membranes immobilizing phosphonic acid
DMMSMS(M)/EPA=1/6 and MDMSMS(D)/EPA=1/6. The groups have a potential for a PEFC application operated at
conductivities of Nafion 112 measured under the same intermediate temperatures.
humidified conditions are also shown in Fig. 2. Obviously,
R
the conductivity strongly depended on the relative humidity Temperature / C
and decreased with decreasing relative humidity. The -1140130120 100 80 60 40
proton conduction for hydrated membranes generally 10
occurs via a proton hopping mechanism (Grotthuss
mechanism) and a diffusion mechanism (vehicle (a)
mechanism) [1]. It should be noted that the activation -2
10
energy of the proton conduction is dependent on the relative
-1
Conductivity / S cm
humidity and increases with decreasing the relative (b)
humidity. The activation energies for
DMMSMS(M)/EPA=1/6 and MDMSMS(D)/EPA=1/6 -3
10
membranes are 0.14 and 0.26 eV at fully hydrated state,
0.40 and 0.48 eV at about 65 %RH and 0.75 and 1.05 eV at
about 20 %RH, respectively. At the fully hydrated state, (c)
-4
the activation energy for proton conduction in the hybrid 10
membrane is comparable to that of Nafion [2]. This result (d)
suggests that water molecules absorbed in the membrane (e)
contribute to the proton conduction like usual water- -5
(f)
cooperative proton conductive membranes by both 10
Grotthuss and vehicle mechanisms in the fully hydrated 2.5 2.6 2.7 2.8 2.9 3.0 3.1 3.3
-1
state. The increase in activation energy with decreasing 103(1/T) / K
relative humidity is reported for Nafion [2]. Similarly, the Fig. 2 Temperature dependencies of proton conductivities
increase in activation energy for the current membrane for the hybrid membranes of
derives from the decrease in water content used for proton DMMSMS(M)/EPA=1/6 (solid symbols) and
conduction. The conductivities of hybrid membranes were MDMSMS(D)/EPA=1/6 (open symbols) under
considerably low compared to that of Nafion 112 in the different relative humidities: (a) and (b) 100 %RH,
range from 40 to 120ºC (Fig. 2). However, the (c) and (d) from 63.5 to 67.7 %RH humidified with
conductivity of Naffion 112 drastically decreased above NaCl solution, (e) and (f) from 19.3to 20.8 %RH,
120ºC. In contrast, the conductivity of hybrid membranes humidified with MgCl 2 solution.The conductivities
increases with temperature up to 140ºC under any of Nafion 112 are also plotted for comparison; (+)
humidified conditions. Also, no decrease in conductivity humidified with NaCl solution, (×) humidified with
by water evaporation was observed up to 140ºC even at low MgCl 2 solution.
humidified conditions. The results indicate that the
membrane is superior in water retention to Nafion above References
120ºC. [1] W.H.J. Hogarth, J.C.D. da Costa, G.Q. Lu: J. Power Sources,
142 (2005), pp.223-237.
4. Conclusions [2] Z. Siroma, R. Kakitsubo, N. Fujiwara, T. Ioroi, S. Yamazaki,
Proton conducting hybrid membranes consisting of K. Yasuda: J. Power Sources, 189 (2009), pp.994-998.
organic polymer chains containing phosphonic acid groups
267
Evolution of laser welding to dissimilar materials joining†
KATAYAMA Seiji * and KAWAHITO Yousuke *
KEY WORDS: (Laser Welding) (Dissimilar materials joining) (Steel) (Aluminum alloy) (Plastic) (TEM image)
1. Introduction produce a strong dissimilar metal joint. The LAMP

Metals and plastics have been used in several industrial joining was created by optimization of diode laser (LD)
applications such as automobiles, electronic devices and joining parameters such as laser power or welding speed
aircrafts. The features of metals include high strength, depending on each kind of material. The metallic
high toughness, high heat conductivity and high heat materials used were low carbon steel and aluminium alloy
resistance. For example, low carbon steel is typical for because this combination was expected to be utilized more
automobile parts, for its easiness of press working in extensively in transportation means. PET was used as
addition to the above properties. Moreover, aluminium plastic material because it could produce strong joints with
alloy has a good resistance to corrosion and is lightweight, various metallic materials and some joint parts could resist
so it would be utilized more and more for weight saving of heat cycle tests according to the previous research [2].
transport machines. On the other hand, plastics are Thus it was thought that PET was one of the best plastics
characterized by lightweight, high corrosion resistance and suited to dissimilar metal joining. The strengths of LAMP
excellent formability. Polyethylene terephthalate (PET) is joints were measured by tensile shear testing. The best
known as a typical engineering plastic and commercially welding conditions were obtained for PET and low carbon
available bottles. steel as well as PET and aluminium-alloy, and dissimilar
Recently it has been reported that the LAMP joining metals joining was implemented separately under these
between metals and engineering plastics could produce conditions to evaluate the joint strengths.
sufficiently strong joints, which possessed tensile shear
loads of more than 3000 N with samples of 30 mm width as 2. Experimental Results and Discussion
shown in Fig. 1 [1]. The LAMP joining is characterized by Dissimilar metal welding was exploited with the
the formation of small bubbles in the plastic just near the procedures as illustrated in Fig. 2. The first step of
interface, and it was interpreted that the bubbles enabled the dissimilar welding was the LAMP joining between PET and
melted plastic to join to the metal surface by the generation low carbon steel by plastic side irradiation, and the second
of their high pressures. Plastics and metals were tightly step of joining was performed between A5052 and PET by
bonded in nanometer sizes, which suggested the strong metal side irradiation, under the respective desirable
physical bonding and a possibility of chemical bonding. welding conditions. The dissimilar metal joint through a
In this research, LAMP joining method was applied to plastic plate could be fabricated. The tensile shear load
achieved 5000 N. This was because the stress on the
plastic was compressive in the tensile shear test, so the joint
strength was improved in comparison with the base plastic
elongation of 3000 N. In addition, the joint part had no
Fig. 2 Schematic experimental set-up of LAMP joining for

Fig. 1 LAMP joints before and after tensile shear test. dissimilar metal welding.

Japan
268
Evolution of laser welding to dissimilar materials joining
weld bead on both surfaces of A5052 and low carbon steel, that the carbon steel and the plastic are tightly bonded at the
and showed good appearances as shown in Fig. 3. atomic or molecular size level.
On the other hand, as for the boundary between A5052
and PET in the obtained joint, the observation image is
shown in Fig. 5. The bright upper part is PET and the
dark lower area is A5052 aluminum alloy. The TEM
image also demonstrates that the aluminum alloy and the
plastic are tightly bonded at the atomic or molecular size
level, which was similar to the above-mentioned LAMP
joints. Moreover, it was found that the oxide film was
composed mostly of aluminum and magnesium by energy
dispersive X-ray spectroscopy (EDS) analysis as indicted in
Fig. 6. A carbon peak was measured in the EDS analysis,
which means that the oxide film of A5052 and the polymer
molecule of PET are close on the atomic or molecular size
level.
㻝㻜㻜㻸㻳㻟㻜㻜㻞㻟㻌㻧㻌㻞㻟㻚㻟㻤㻜㻌㼚㼙
Fig. 3 Surface appearances of dissimilar metal welds produced 㻥㻜

by LAMP joining with both-side irradiations.
㻤㻜㻭㼘
Concerning the boundary between carbon steel and 㻣㻜
PET in the obtained joint, the observation image is shown
in Fig. 4. The bright upper part is PET polymer and 㻢㻜
㻯
the dark lower area is Fe. The TEM image demonstrates
㻯㼛㼡㼚㼠㼟
㻡㻜
㻻
㻠㻜
㻹㼓
㻟㻜
㻹㼛
㻞㻜
㻹㼛
㻝㻜
㻜
㻜㻚㻜㻜㻝㻚㻜㻜㻞㻚㻜㻜㻟㻚㻜㻜㻠㻚㻜㻜㻡㻚㻜㻜㻢㻚㻜㻜㻣㻚㻜㻜㻤㻚㻜㻜㻥㻚㻜㻜㻝㻜㻚㻜㻜
㼗㼑㼂
Fig. 6 EDS analysis of dissimilar metal weld with LAMP joint.

3. Conclusions
LAMP joining made dissimilar metals joining possible
without formation of brittle intermetallic compounds
between them and without dissimilar metal corrosion or
bimetal corrosion by sandwiching a plastic plate. The
dissimilar metals joint with a plastic plate could be
Fig. 4 TEM image of boundary between carbon steel and
PET in dissimilar metal weld. fabricated and the joint shear load reached to 5000N, which
was high. Then both A5052 sheet and low carbon steel
sheet were deformed and elongated due to the formation of
strong joints.
Acknowledgments
This work was conducted as part of the Industrial
Technology Research Grant Program “Development of
high-quality direct laser joining of metal and plastic by
laser adaptive control” supported by New Energy and
Industrial Technology Development Organization (NEDO).
The authors would like to acknowledge whom it may
concern.
References
[1] S. Katayama and Y. Kawahito, Scripta Materialia, 59-12
(2008), pp.1247- 1250.
[2] S.Katayama; Y. Kawahito; A. Tange; S. Kubota, Online Proc.
Fig. 5 TEM image of boundary between aluminum alloy and of LAMP 2006, Kyoto, (2006) #06-7.
PET in dissimilar metal weld.
269
†
YAMASHITA Kimihiro *
KEY WORDS: (Vector materials) (Poling) (Electret) (Biomaterials) (Hydroxyapatite)
1. Introduction In a biological condition surrounded with water, typical

Recently, we have proved that hydroxyapatite (HA) electrolytic substance, local electrostatic influence is
bioceramics and 45S5-type bioglasses (BG) are excellent sometimes desirable. Living bodies consist of lots of ionic
electrets with an outstanding chemical and biological groups including proteins and cells. In such systems, the
effects [2-7]. These electrets can be prepared by electrical application of external fields is limited because of side
polarization. Conventionally polarization has been effects. Polarized HA and BG have recently been proved
applied mainly to ferroelectric or piezoelectric ceramics, in as the members of vector materials.
which spontaneous dipoles are predominantly arranged in a The word “vector” is commonly used in mathematics and
dc field of polarization. In our study of bioceramics and biology. The terminology of vector is originally defined
bioglasses, polarization has been proved to take place due as a noun; (1)(a) a quantity that has magnitude, direction,
to ionic displacement to a rather long range, where ion and sense, (b) a course or compass direction especially of
vacancies play important roles. Due to the electrical an airplane, or (2) an organism that transmits a pathogen.
treatment, surfaces are electrically charged, depending on The word is also to guide (as an airplane, its pilot, or a
the direction of applied dc field. Based on the finding of missile) in flight by means of a radioed vector. According
remarkable effects of polarized electrets, vector effects [1] to the usage, we define vector, vector materials, and vector
are employed as a concept exceeding bioactivity. effects for materials science as: Vector is to manipulate the
This report will firstly present the concept of vector constituents of a living body and environmental system
effects, and then show the electroceramic properties of HA such as non-alive substances of ions, proteins sugars, and
and BG with interesting electrical properties. Their alive cells and bacteria, tissues and organs by biocompatible
biological effects will also be demonstrated in the or eco materials themselves. A vector material is a
solidification phenomena in a simulated body fluid (SBF). material which has an ability to vector. A vector effect is
an effect which a vector material brings forth.
2. Concept and Definition of Vector Effects and Ceramic magnets and electrets are therefore typical
Materials vector materials after the definition. A radioactive
Under certain circumstance where a force is desired to material is another candidate of vector material because
act on a targeted spot in a quasi-closed system such as they can individually irradiate a force on its surrounding.
human body, an external magnetic, sonic or electric field is As mentioned below, radioactive ceramics incorporated in
usually applied to the whole system. The application of an glass beads have been applied in medical applications for
external field, however, needs a continuous power supply as cancer therapy. These materials are classified as
well as working electrodes, and to make matters worse it radioactive vector ceramics. Non-polarized 45S5-type
actually arouses some secondary competitive reactions such bioglass and E-tricalcium phosphate are comparatively
as dissociation of water molecules. For such situation, dissolved in a body and release chemical constituents or
independently workable substances such as magnets are artificial chemicals, resulting in good bone conductivity.
expected to have great benefits, because they can bring These materials fall to chemicovector materials. Scaffolds
effects only to a given local spot. Such materials are are a kind of biovector materials which can activate
expected to have useful effects in some applications of surrounding cells at a desired spot through biological
environmental devices as well as biomedical ones. substances incorporated in themselves.
Contrasting with magnets, materials with electrostatic Such effects are expected to bring about using various
working forces have been called electrets. Electrets also kinds of energies stored in a solid, and these materials are
have isolated working forces, however, they have not yet assigned to vector materials. The family of vectors
been acknowledged, still less practically employed. Some ceramicsmay be classified on the basis of the mechanisms
physical shortage of electrostatic force such as the effective to drive the effects. Vector ceramics are divided into two
range of influence in comparison with magnetic force might categories according to the velocity of irradiated force to
be attributed to the above situation, however, it is also penetrate through bio-interface; the lines of magnetic and
pointed out that an important application of electrets has electric forces or E-ray instantly traverse the interfacial
not yet been invented. zone, while released ions by dissolution gradually diffuse
ᴾ ᴾ *ᴾ Tokyo Medical and Dental University, Tokyo, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
270
from a surface to the zone. A combination of several bioactovity.

vector effects may amplify an effect. A variety of Wet-chemically synthesized HA powders were
functional materials are under development for other vector uniaxially pressed into pellets with a thickness=1mm and a
materials such as mechanovector or optovector materials. diameter=1cm, then sintered at 1523K for 2h under a water
vapor stream. The densities of the sintered pellets were
3. Electrical Properties of Hydroxyapatite Ceramics 95% of the theoretical value. The HA structures of
In addition to the unparalleled bioactivity, HA has specimens were confirmed using crushed powders of the
important and interesting properties as an electroceramic. sintered specimens by X-ray diffraction (XRD) and infrared
These biomedical and electrical properties of HA are (IR) analyses.
largely attributed to its stable lattice hydroxide ions, Polarization of HA was carried out with dc 1kVcm-1 at
surrounded with calcium ions in the crystal structure. 573K using Pt plates as electrodes. As vector effects were
Prior to the present study, the dielectric measurements were dependent upon the electric signs of surface charges, the
carried out for understanding of the bioactive polarized surfaces were named as N- and P-surfaces.
characteristics of HA. Non-polarized surface was designated as 0-surface for
As a result, HA ceramics were proved to exhibit reference. To confirm polarization and evaluate the stored
dielectric characteristics below ca. 800K. At higher charges in HA, a thermally stimulated current technique
temperatures, HA ceramics show an unusual phenomenon was employed, in which thermally dissipated current was
of time dependent conductivity. The measured impedance measured at temperatures of room temperature to 1073K.
of HA specimen changed with time over a wide range Although slow crystallization took place dispersedly
between 107 and 104Scm-1. The time-dependent- on non-polarized HA, large crystals of 1-4Pm in diameter
conductivity was strongly dependent upon the water of covered the N-surface of polarized HA after an immersion
sintering ambience; the aging was characteristic of HA in 1.5SBF for only 12h. Higher field strength gave rise to
sintered under a steam stream, while HA sintered in air did faster crystal growth; sizable agglomerated crystals of
not show aging behavior. Then, it was considered that the 10mm in diameter were observed in some spots on
electrical properties of HA can depend upon the polarized HA under 1kVcm-1. The accelerated crystal
constituents of water molecules such as H+, OH-, O2-. It growth mentioned above was observed on the N-surface,
was demonstrated from a concentration cell measurement of whereas no crystal growth ever took place on the P-surface
the electromotive force generated using a hydrogen even after 3-day immersion in 1.5SBF. Although the
concentration cell of HA ceramic that the mass transport polarization at 573K was effective for the acceleration of
takes place due to the migration of protons in HA. The crystal growth, we also identified the acceleration effect by
recent studies by the thermally stimulated current method the polarization at 473K. The crystal growth was
showed that HA ceramics were polarizable at a temperature dependent upon the dc field strength, temperature and time
higher than the monoclinic-to-hexagonal phase transition for polarization.
temperature (500K). In the early stage of the study, we Some experiments confirmed 1h-polarization enough
assumed polarization might be due to the reorientation of for the optimum acceleration of crystal growth; under this
the lattice OH- ions along the c-axis. However, the condition the surfaces of HA were already coated with thick
assumption was inappropriate, because the relaxation was bone-like layers within 6-12h. Under an optimum
observed to take place only due to polarization conditions. polarization condition (actually 1.5SBF), the growth rate
Relaxation or depolarization occurs only when the strain was estimated as 6Pm/day, almost 3 times of the result
induced by electric stress is thermally released. A obtained by the biomimetic method (1.7Pm/day). The
measured thermally stimulated depolarized current (TSDC) growth rate was increased to 10Pm/day, as large as several
confirmed that HA is polarized like ferro- or piezo-electric times of that of non-polarized HA . At the early stage of
ceramics. Using the I-T curve, we can evaluate the stored the crystal growth, the grown crystals were spherical and
energy in HA. their sizes were dependent on the field strength and time for
BG is also a good ionic conductor with a conductivity polarization. The polarization is therefore considered to
of the order of 10-4Scm-1and an activation energy of 0.6eV. effect the nucleation as well as the crystal growth.
As BG contains a considerable amount of sodium ions in
the silica networks, the charge carriers are considered as 5. Conclusion
Na+. BG is polarized between 350 and 800K. The The electroceramic properties of biomedical materials
TSDC curves gave the stored energies of 50-200 mCcm-2. have recently gained an increasing attention for nano-
Based on the results, BG is regarded as a good electret. interface engineering, in which polarized bioceramics and
bioglasses are centered. Based on the excellent biological
4. Vector effect of polarized hydroxyapatite ceramics performance of the polarized biomedical materials, the new
and bioglasses in SBF concept of vector materials has been developed for nano-
Taking the polarizability into account, we conducted a interface engineering.
study of the vector effect on the crystal growth on HA
ceramics. We observed the remarkable phenomenon on References
crystal growth. Here it should be noticed that bone-like [1] K. Yamashita and S. Nakamura: J. Ceram. Soc. Jpn., 113
crystal growth in SBF is proposed by Kokubo and his (2005), pp.1-9.
colleagues as pre-examination of bioactovity, or in vitro
271
[2] K. Yamashita, N. Oikawa and T. Umegaki: Chem. Mater., 8 [5] M. Ueshima, S. Nakamura, M. Ohgaki and K. Yamashita:
(1996), pp.2697-2700. Solid State Ionics, 151 (2002), pp.29-34.
[3] M. Ohgaki, S. Nakamura, T. Okura and K. Yamashita: J. [6] Y. Toyama, M. Ohgaki, S. Nakamura, K. Katayama and K.
Ceram. Soc. Jpn., 108 (2000), pp.1037-1040. Yamashita: Solid State Ionics, 151 (2002), pp.159-163.
[4] H. Takeda, Y. Seki, S. Nakamura and K. Yamashita: J. Mater. [7] A. Obata, S. Nakamura, Y. Moriyoshi and K. Yamashita: J.
Chem., 12 (2002), pp.2490-2495. Biomed. Mater. Res., 67A (2003), pp.413-420.
272
Preparation of metal nano particles using electrochemical

†
deposition
Pt nano patterned electrodes
SAITO Mikiko *, MIZUNO Jun * and HOMMA Takayuki *
KEY WORDS: (Metal nano-particles) (UV-NIL ) (Electrochemical deposition)
1. Introduction
Table 1 Bath composition for Pt
Metal nano-particles have been known to possess electrodeposition.
various properties which cannot be obtained in the bulk
Chemicals Concentration ᴾ ᴾ ᴾ ᴾ
phase and are expected to be applied to various fields such
as electronics and biotechnology, etc [1-4]. The nano H 2 (PtCl 6 ) · 6H 2 O ᴾ 10 g dm-3
particles are prepared through physical or chemical
approaches. The chemical method has advantages for PEG (M. W. 200- ᴾ 0-100 mM
fabricating the nano particles with precisely controlled nano 20000)
structure. Among the chemical methods, an electrochemical
process is utilized in which the nano particles are prepared Figure 1 shows the UV-NIL process for the nano-
by reduction at a cathode substrate [5]. In this case, the patterning of the cathode surface patterns. First, UV resin is
metal occasionally forms dendritic like growth, which spin-coated on a Si substrate with a seed layer (1). A
results in non-uniformity of the particles. In order to solve stamper with nano patterns is pressed to the substrate and
this problem, in this study, we attempt to optimize the UV light is irradiated from above (2, 3, 4). Then, the
surface nanostructure of the cathode. In order to prevent stamper is removed from the sample (5). Subsequently, the
coagulation of the metal particles and achieve numerous residual films at the hole are removed using O 2 RIE (6).
nucleation, we applied the nano-dot-patterning to the This substrate with a nano-patterned surface is used as a
electrode surface using Pt electrodeposition and UV-NIL cathode electrode(7). Figure 2 shows the schematic
processes[6]. Furthermore, we investigated the Pt illustration of the Pt electrodeposition. A Pt film is
deposition conditions, mainly focusing upon the effect of deposited on the Si substrate with nano patterns using a
rotating disk electrode system. The 100 nm thick Pt films
additive such as polyethylene glycol(PEG) in order to
were deposited using HZ-5000 rotating electrode system
obtain high surface activity.
(HOKUTO DENKO) with a SCE as reference electrode.
2. Experimental
A Ni and a Ti seed layers were deposited onto Si(111)
wafer using sputtering. The thickness of the Ni and the Ti
layers were 100 nm and 10 nm, respectively. The substrates
with the seed layers were cleaned with 14 wt% HCl
aqueous solution for 20 s followed by rinsing with ultra
pure water, then in order to generate uniform nucleation the
specimens were immersed into a 0.2 mM Pd aqueous
solution for 300 s followed by rinsing with ultra pure water.
After these pretreatments, the Pt was electrodeposited using
the bath shown in Table 1. The surface morphology was
observed using scanning electron microscopy with field
emission source (FE-SEM, S-4800, Hitachi) and atomic
force microscopy (AFM, Dimension 3100, Veeco
Instruments). The composition was analyzed using a glow
Fig. 1 UV-NIL process.
discharge optical emission spectrometer (GDOES, JY-
5000RF, HORIBA).

* Waseda University,Tokyo,Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
273
Preparation of metal nano particles using electrochemical deposition
Pt nano patterned electrodes
(a) Sputtered Pt film (b) Electrodeposited Pt

Ra: 0.595 nm film deposited without
additives
Ra:㻌 2.40 nm 200㻌 nm
(c) Electrodeposited Pt (d) Electrodeposited Pt film

film deposited with deposited with PEG20000, 10
PEG6000, 10 mM mM
Ra: 3.59 nm Ra: 2.34 nm
Fig. 4 AFM images of Pt films.
Figure 5 shows the representative results in 0.5 M

aqueous sulfuric acid solution. The observed current
Fig. 2 Schematic illustration of the electrodeposition. density of the electrodeposited Pt film was larger than that
of the sputtered film. The film deposited from the bath
containing PEG exhibited the highest current density among
3. Results and Discussion the examined films. These results correspond to those
Figure 3 shows the cathodic polarization curves of the related to the surface morphology described above. Namely,
bathᴾ for the Pt electrodeposition. The results for the bath it was suggested that the Pt films with larger surface area or
with and without additives are shown. As is seen in the
0
figure, the cathodic current was suppressed by adding PEG
to the bath. It was confirmed that the PEG acts as inhibitor.
-0.1
Also, the cathodic current decreases with an increase in the
Current Density / A cm -2
molecular weight (M. W.) of the PEG. These results for the
-0.2
behavior of PEG showed the same trends to those observed
Electrodeposited Pt film
for Cu electrodeposition for via-filling [7]. deposited without additives
-0.3
Figure 4 shows representative AFM images of the Electrodeposited Pt film
electrodeposited Pt films. As a reference, the image for deposited with PEG6000, 10
-0.4 mM
sputtered Pt film is also shown. From the results, it is Sputtered Pt film
confirmed that the electrodeposited Pt films have rougher
-0.5
surface than that of the sputtered film. Moreover, the -1.8 -1.6 -1.4 -1.2 -1 -0.8 -0.6 -0.4 -0.2 0
roughness became larger by the addition of PEG to the bath.
On the other hand, as is seen in Fig. 4, when the PEG with Potential / V vs. SCE
larger M. W. such as 20000, is applied, the surface Fig. 5 Cathodic polarization measurement of the Pt films in
becomes smoother. 0.5 M aqueous sulfuric acid.
0.02
0
Current Density / Acm -2
-0.02
-0.04
-0.06
No additive
-0.08
PEG6000, 10 mM 200 nm 200 nm
-0.1
PEG20000, 10 mM ᴾ (a) Pt nano patterned (b) Cu nano-particles formed
-0.12
on the Pt nano patterned
-2 -1 0
Potential / V䚷䡒䡏. SCE
Fig. 6 SEM images for electrodeposited Pt nano patterned
Fig. 3 Cathodic polarization measurement of the bathᴾ for electrode using UV-NIL(a) and Cu nano-particles formed
the Pt electrodeposition. on the Pt nano patterned(b).
274
examined samples. The Pt films, which exhibited the

larger surface roughness possess larger cathode current highest current density, were adapted to fabricate nano-
flow. patterned electrode with 400 nm pith periodic structure
In order to confirm the effectiveness of the Pt nano- using UV-NIL. It was revealed that Cu nano particles were
patterned electrodes, Cu nano particles were performed prepared using Pt nano-dot-patterned electrode.
with the electrolyte containing Cu-Acetate using the Pt
nano-patterned electrodes. Figure 6 shows representative References
SEM images of the surface of nano patterned Pt electrode [1] A. Pietrikova and E. Kapusanska: Kovove Materialy, 29
with 400 nm pith periodic structure and Cu nano particles (1991), p.262.
[2] K. Mizugaki, K. Wada, K. Sakurada, T. Shintate, J. Yamada,
formed on the Pt nano electrode [8]. It was confirmed that T. Mikoshiba, N. Uehara and M. Yajima: J. Jan. Inst.
the Pt nano-patterned electrodes revealed the ability for Electronics Packaging, 9 (2007), p.546.
preparing Cu nano particles. [3] T. Osaka, J. Sasano, M. Matsunaga and H. Iida: J. Surf. Fin.
Soc. of Jpn., 59 (2008), p.355.
4. Conclusions [4] S. Motokawa, M. Mohamedi, T. Momma, S. Shoji and T.
Electrodeposited Pt nano-patterned electrodes for the Osaka: Electrochemistry, 73 (2005), p.346.
formation of nano particles were investigated. In order to [5] N. Toshima: J. Surf. Fin. Soc. Jpn., 59 (2008), p.708.
achieve higher activity, the deposition conditions of Pt were [6] M. Fukuhara, J. Mizuno, M. Saito, T. Homma and S. Shoji:
optimized using additives such as PEG. The surface activity Transactions on Electrical and Electronic Engineering IEEJ
Trans, 2 (2007), p.307.
of the Pt films was affected by the size of molecular weight
[7] K. Kondo, K. Hayashi, Z. Tanaka and N. Yamakawa: J. Jpn.
of PEG. It was considered that the Pt films, which have Inst. Electronics Packaging, 3 (2000), p.7.
large surface area, exhibited high surface activity among the [8] M Saito, J. Mizuno, H. Nishikubo, H. Fujiwara and T.
Homma: ECS Trans., 16 (2009), pp131-136.
275
Fabrication and thermoelectric properties of eco-friendly silicides

†
for thermoelectric power generation using waste heat
ITOH Takashi *
KEY WORDS: (Eco-friendly) (Higher manganese silicide) (Magnesium silicide) (Synthesis) (Mechanical
grinding) (Pulse discharge sintering) (Liquid-solid phase reaction) (Thermoelectric properties)
1. Introduction stoichiometry of Mg66-yAlySi33.3, and mixed in an argon

Development of alternative energy sources like the atmosphere. The powder mixtures with different amounts of
recycled energy sources is required for resolution of energy Al (y=0, 0.05, 0.10, 0.15, and 0.20 at.%) were prepared.
security and environmental problems. Thermoelectric The powder mixture was put into an alumina crucible, and
power generation (TEG) is a prospective means using the Mg66-yAlySi34 compound was synthesized from the mixture
waste heat discharged from many kinds of energy systems, through the LSPR process at 953 K for 1 h in an argon
and it is expected to contribute to the resolution of these atmosphere using an infrared lamp heating furnace. The
issues. The low-cost thermoelectric materials are required synthesized powder was consolidated by PDS at 1003 K for
for the practical use of TEG and the materials with low- 30 min under the pressure of 60 MPa. Influences of Al
environmental load are preferred. P-type higher manganese dopant on the lattice parameter and the thermoelectric
silicide (HMS) [1-3] and n-type dimagnesium silicide properties were investigated.
(Mg2Si) [4-6] are candidates for low-cost and eco-friendly
thermoelectric materials. In this research, the HMS 3. Results and Discussion
compounds were synthesized and consolidated by pulse The fabricated MnSix (x=1.73, 1.80, 1.84 and 1.90)
discharge sintering (PDS) combined with mechanical samples had the relative density of 93, 92, 91 and 92 %,
grinding (MG). Influence of Si content on the respectively. In the x-ray diffraction (XRD) analysis, HMS
microstructure and the thermoelectric properties were phase and MnSi phase were detected in the MnSi1.73 and
investigated. The Mg2Si compounds were synthesized by MnSi1.8 samples. The relative diffraction intensity of MnSi
liquid-solid phase reaction (LSPR), and consolidated by phase of the MnSi1.73 sample was larger than that of the
PDS. Influences of Al dopant on the lattice parameter and MnSi1.8 sample. On the other hand, only HMS phase was
the thermoelectric properties were also investigated. detected in the MnSi1.84 and MnSi1.9 samples. Figure 1
shows the scanning electron microscope (SEM) images of
2. Experimental Procedures the samples. In the MnSi1.73 and MnSi1.8 samples, MnSi
For fabricating HMS compounds, pure Mn powder phase coexisted with HMS phase, and in the MnSi1.84 and
(purity >99.9 %, particle size <75 Pm) and Si powder MnSi1.9 samples, free Si particles were dispersed in the
HMS matrix. The microstructures were changed with Si
(>99.9 %, <75 Pm) were used as the raw powders. Each of
content.
Mn and Si powders were mechanically ground using
(a) (b)
planetary ball milling equipment at 400 rpm for 3 h. The MnSi
ground Mn and Si powders, passing through a sieve of 44
Pm opening, were individually collected. The sieved Mn
and Si powders were weighed with non-stoichiometry of MnSi
MnSix (x=1.73, 1.80, 1.84 and 1.90), and mixed by using a
rotary blender at 60 rpm for 1 h. The HMS compounds 500Pm 500Pm
were synthesized from the powder mixtures and
(c) (d)
simultaneously consolidated by PDS at 1173K for 15 min Si
Si
under 60 MPa in a vacuum atmosphere. Influences of Si
content on the microstructure and the thermoelectric
properties were investigated.
For fabricating Al-doped Mg2Si compounds, Mg
powder (> 99.9 %, < 180 Pm), Si powder (> 99.9 %, < 75 500Pm 500Pm
Pm) and Al powder (> 99.9 %, 106-180 Pm) were used as Fig. 1 SEM images of four MnSix samples; (a) x=1.73, (b) x=1.8,
the raw powders. The powders were weighed with non- (c) x=1.84, and (d) x=1.9.
ᴾ ᴾ ᴾ † Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding

* EcoTopia Science Institute, Nagoya University, Nagoya, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan Japan
276
Fabrication and thermoelectric properties of eco-friendly silicides for thermoelectric power generation using waste
heat
1.0 The relative density of all Mg66-yAlySi34 samples

x=1.73 obtained by LSPR-PDS was more than 95%. In the XRD
x=1.80 analysis, only Mg2Si phase was detected in all samples. It
0.8 x=1.84 indicates that Mg66-yAlySi34 compounds were successfully
x=1.90 synthesized regardless of Al content. It is also found out
0.6 that the diffraction peak positions shift slightly toward the
larger diffraction angle with an increase of Al content,
ZT
ZT
indicating that the lattice parameter of Mg66-yAlySi34

0.4 becomes smaller with increase of Al content. The relation
between the Al content and the lattice parameter estimated
Sample (x=1.73) from the XRD data is shown in Fig. 3. It linearly decreases
0.2 with increasing Al content, obeying the Vegard’s law. This
prepared by MA-PDS [3]
result supports the view that Al atoms successfully
0.0 substituted into a part of Mg sites in Mg2Si and the lattice
300 400 500 600 700 800 900 1000 1100 parameter decreased with substituting Al atoms having
Temperature (K) smaller atomic radius than Mg atoms.
The electrical resistivities of the Mg66-yAlySi34 samples
Fig. 2 Temperature dependence of the dimensionless figure (y=0.15 and 0.20 at.%) were one sixth or less than that of
of merit, ZT of four MnSix samples (x=1.73, 1.8, the non-doped sample (y=0 at.%) all over the temperature
1.84 and 1.9) and of MnSi1.73 sample prepared by range. The absolute value of the Seebeck coefficient was
MA-PDS [3]. remarkably decreased by Al doping, but the Seebeck
coefficients of the Mg66-yAlySi34 samples (y=0.15 and 0.20
The optimum Si content that makes a nearly single HMS
at.%) were varied similarly with temperature. The thermal
phase will exist between x=1.8 and 1.84.
conductivities of all samples increased with increase of Al
The electric resistivity of MnSix samples increased with
content all over the temperature range. The temperature
increase of Si content. This would be caused by the amount
dependences of the dimensionless figure of merit, ZT are
of MnSi phase having a lower electrical resistivity than
shown in Fig. 4. The maximum ZT was 0.27 at 789 K for
HMS phase and by the amount of free Si having a larger
the non-doped sample, 0.61 at 883 K for the 0.15 at.%Al-
electrical resistivity than HMS phase. The maximum
doped one, and 0.47 at 833 K for the 0.20 at.%Al-doped
Seebeck coefficient was achieved in the MnSi1.84 sample
one, respectively. The 0.15 at.%Al-doped sample had the
having a small amount of free Si, because both MnSi phase
best thermoelectric performance.
and free Si have lower Seebeck coefficients than the HMS
phase. All of the MnSix samples had similar levels of 0.7
thermal conductivity. From these thermoelectric properties, x= 0.20
the dimensionless figure of merit, ZT was calculated. 0.6 x= 0.15
Figure 2 shows the temperature dependences of ZT for the x= 0
four MnSix samples together with the result of the MnSi1.73 0.5
sample prepared by PDS combined with mechanical
alloying (MA) [3]. In the MnSi1.84 sample, the best 0.4
ZT
thermoelectric performance was obtained and the maximum

ZT of 0.83 was achieved at 818K. 0.3
6.355 0.2
0.1
6.350
Lattice parameter (Å)
0.0
300 400 500 600 700 800 900
6.345
Temperature (K)
6.340 Fig. 4 Temperature dependence of the dimensionless figure

of merit, ZT of three Mg66-xAlxSi34 samples (x=0,
0.15 and 0.20).
6.335
4. Conclusions
6.330 The MnSix compounds were synthesized by MG-PDS.
0.05 0
0.10 0.15 0.20 The MnSi phase or free Si existed in the matrix of HMS
Al content (at.%) depending on Si content. The maximum ZT of 0.83 was
Fig. 3 Relation between Al content and lattice parameter of achieved at 818K by optimizing Si content (x=1.84) in
Mg66-yAlySi34 samples. MnSix. The Mg66-yAlySi34 compounds were synthesized by
LSPR, and consolidated by PDS. The Al atoms were
277
substituted into parts of Mg sites in Mg2Si. The maximum Metastable and Nanocrystalline Materials, 8 (2000), pp.918-
ZT of 0.61 was achieved at 883K by optimizing Al content 923.
(y=0.15 at.%) in Mg2Si. [3] T. Itoh and M. Yamada: J. Electronic Materials, 38 (2009),
pp.925-929.
References [4] M. Riffel and J. Schilz: Proc. 16th Int. Conf. on
[1] S. Okada, T. Shishido, M. Ogawa, F. Matsukawa, Y. Thermoelectrics, Dresden, IEEE, (1997), p.283.
Ishizawa,K. Nakajima, T. Fukuda and T. Sundstrand: J. Cryst. [5]T. Kajikawa, K. Shida, M. Ohmori and T. Hirai: Proc. 16th Int.
Growth, 229 (2001), pp.532-536. Conf. on Thermoelectrics, Dresden, IEEE, (1997), p.275.
[2] M. Umemoto, Z.G. Liu, R. Omatsuzawa and K. Tsuchiya: J. [6] J. Tani and H. Kido: Intermetallics, 15 (2007), pp.1202-1207.
278
Fabrication of zirconium oxide solid electrolytes with ordered

†
porous structures by using micro stereolithography
KIRIHARA Soshu * and TASAKI Satoko *
KEY WORDS: (Solid electrolytes) (Zirconium oxide) (Ordered porous structures) (Micro stereolithography)
1. Introduction crystal lattice model of 3×3×0.37 mm in size included the

Zirconium oxide solid electrolytes with ordered porous arranged rods of I100×150 mm in dimension. The volume
structures were successfully fabricated by using novel ratio of the lattice was 33.3 %. The real ceramic lattice
micro stereolithography with computer aided design and model was fabricated automatically by using the
manufacture processes. Micrometer order zirconia ceramic stereolithographic machine (D-MEC, SI-C1000). Figure 2
lattices with coordination number 4 were propagated shows a schematic illustration of the fabrication system.
spatially to realize high porosities from 60 to 80 percent. In The designed model was converted into a rapid prototyping
these fabrication processes, nanometer sized zirconia format of the stereolithography files and sliced into thin
particles were dispersed in photo sensitive resins to obtain sections. The zirconia particles of 100 nm in average
thixotropic slurries. The paste was spread on a glass diameter were dispersed into photo sensitive acrylic liquid
substrate by using a mechanic at knife edge movement, and resin at 30 % in volume content. The mixed slurry was
an ultra violet micro pattern was exposed on the surface to squeezed on a working stage from a dispenser nozzle. This
create a cross sectional solid layer. After the layer stacking material paste was spread uniformly by a moving knife edge.
processes [1-3], a micrometer order structure of the resin The layer thickness was controlled to 5 μm. An ultra violet
and ceramic composite was obtained. The formed layer of 405 nm in wavelength was exposed on the resin
composite precursor was dewaxed and sintered at high surface according to the computer aided operations. Two
temperatures in an air atmosphere, and the fine ceramic dimensional solid patterns were obtained by light induced
lattices with high density were created. photo polymerization. The high resolutions in these micro
patterns had been achieved by using a digital micro mirror
device. In this optical device, square aluminum mirrors of
14 ȝP LQ HGJH OHQJWK ZHUH closely assembled with
1024×768 in number. Each micro mirror can be tilted
independently, and cross sectional patterns were
dynamically exposed through the objective lens as bitmap
LPDJHVRIȝPLQVSDFHUHVROXWLRQ$IWHUthe stacking and
joining these layers through photo solidifications, the
Fig. 1 A computer graphic model of a solid electrolytes

with ordered porous structure. A ceramic lattice distributes
in air space to create periodic arrangements of opened paths.
The zirconia lattice model with the coordination Fig. 2 A schematically illustrated micro stereolithography ᴾ
number 4 was created by the computer graphic application system. Acrylic resin lattices including zirconia nano-sized ᴾ
(Toyota Keram, Think Design) as shown in Fig. 1. The particles were processed through solidified layers stacking.
*ᴾ JWRI, Osaka University, Ibaraki, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
279
Fabrication of zirconium oxide solid electrolytes with ordered porous structures by using micro stereolithography
periodic arrangements of micro dielectric tablets were

btained. After the dewaxing process of the zirconia
dispersed resin precursor at 600 ºC for 2 hs with a heating
rate of 1 ºC/min, the sample was sintered at 1500 ºC for 2hs
with a heating rate of 8 ºC/min. Relative densities of these
sintered samples were measured by using the Archimedes
method. Part accuracy of the ceramic lattice arrangement in
the metal matrix was measured by using the digital optical
microscope (Keyence, VHX-200). And, microstructures of
ceramic phases were closely observed by using the scanning
electron microscope (JEOL, JSM-6060).

The stereolithographic models of the acryl lattice
pattern with the zirconia nano particles were successfully
fabricated. The spatial resolution was measured as 0.5 % in Fig. 3 The nanometer sized particles of the zirconium oxide
size. The nanometer sized zirconia particles were dispersed ceramics dispersing in the acrylic resin lattices fabricated by
uniformly in the acrylic resin matrix as shown in Fig. 3. using the micro stereolithography process.
Through the heat treatments of the precursors, the
micrometer order zirconia lattices including the air gaps
were formed exactly as shown in Fig. 4. By the optical and
scanning microscopic observations, the deformation and
cracking were not observed. Linear shrinkages for the
horizontal and vertical axis were different at 2 %
approximately. Uniform shrinkage will be obtained through
the optimizations in the model design considering the
gravity effect. The relative density reached 98.5 %. Dense
zirconia microstructure was formed, and the average grain
size was approximately 2 μm.
4. Conclusions
We have fabricated three dimensional solid electrolytes
of zirconia lattices successfully by using stereolithography.
These ceramic lattices with coordination number 4 could
Fig. 4 The sintered zirconium oxide lattices with the ordered
realize ordered porous structures. The fabricated ceramic
porous structures. The lattice coordination number is 4. The
structures with high porosities and wide surface areas are
opened air paths were arranged periodically.
expected to be applied to novel electrodes in solid fuel cells.
References
[1] C. Kai and L. Fai: Rapid Prototyping, Singapore John Wiley
5. Acknowledgments and Sons, (1997).
This study was supported by Priority Assistance for the [2] A. Pique, A. Holmes and D. Dimos: Materials Research
Formation of Worldwide Renowned Centers of Research - Society Symposium Proceedings, (2003), pp.758-764.
The Global COE Program (Project: Center of Excellence [3] S. Kanehira, S. Kirihara and Y. Miyamoto, Journal of the
for Advanced Structural and Functional Materials Design) American Ceramic Society, 88 (2005), pp.461-1464.
[4] S. Kirihara and Y. Miyamoto, The International Journal of
from the Ministry of Education, Culture, Sports, Science
Applied Ceramic Technology, 6 (2009), pp.41-44.
and Technology (MEXT), Japan.
280
Application to catalyst of mayenite consisting of ubiquitous

†
elements
SUZUKI Kenzi *
KEY WORDS: (Environmental material) (Mayenite) (Ubiquitous elements) (Oxygen radical)
1. Introduction stoichiometric ratios, grinding without water, calcining at

The effective utilization of the tar discharged from ÛC in air environment for 4 hours, using a temperature
gasification of biomass is required. By the steam reforming LQFUHDVH UDWH ÛC/min, lastly crushing and sieving to 212-
reaction of the tar using a Ni catalyst, it is possible to 425ȝP. The commercial-like Ni/Al 2 O 3 (5wt%) was
produce synthesis gas such as H 2 and CO. One of the prepared by an impregnation method.
problems of this reaction is the degradation of the catalytic
activity by the coking. Mayenite, Ca 12 Al 14 O 33 , is the 2) Catalyst performance examination
material which occludes oxygen radicals in the structure, Toluene was selected as the biomass tar model
and it is known to have the function of an oxidation catalyst compound. Experiments were carried out at atmospheric
[1]. In addition, the composition of the mayenite consists of pressure in a fixed-bed reactor. All the catalysts were
only ubiquitous elements. In this study, the coking initially activated under the reduced gas mixture (<5% H 2
protective effect by using mayenite for a catalyst support of GLOXWHG E\ $U IRU KRXUV DW ÛC, then tested at the
the Ni catalyst is presented. given operation parameters. Two conditions of toluene
concentration around 2000 and 4000ppm were studied.
2. Experimental
Catalysts preparation 3. Results and discussion
Mayenite (Ca 12 Al 14 O 33 ) was prepared by solid mixing Figure 1 showed Raman spectra of Mayenite and
of Ca(OH) 2 and Al(OH) 3 in stoichiometric ratio, grinding Ni/Mayenite before reaction. The Raman band at 1090cm-1
DQGFDOFLQDWLRQDWÛC for 4 hours in an air environment, was O 2 - species, and an additional band assignable to the
followed by crushing and sieving to obtain particle sizes O 2 2- species appeared at 880cm-1.
between 212-425ȝP. Ni/Mayenite (Ni = 1, 3, 5wt%) was Experiments of steam reforming for toluene were
prepared by mixing Mayenite with NiO in different carried out on Mayenite and Ni/Mayenite with a
temperature range of 550-ÛC for a S/C ratio of 1.9 and
O2- 100 100

O22-
Toluene conversion (%)
80 80
Toluene Conversion(%)
60 60
Intensity(a.u.)
Ni/Mayenite
40 40
Ni/Mayenite(5%)
20 20 Ni/Mayenite(3%)
Ni/Mayenite(1%)
Mayenite
0 0
550 600 650 700 750 800 850
Mayenite 550 600 650Temperature(
700 0750 800 850
C)
Temperature (䁸C)
900 1000 1100
-1
Raman Shift(cm )
Ÿ1L0D\HQLWHƔ1L0D\HQLWH
Ŷ1L0D\HQLWHż0D\HQLWH
Fig. 1 Raman spectra of Mayenite and Ni/Mayenite Fig. 2 Toluene conversion vs. Reaction temperature for
before reaction. Mayenite and Ni/Mayenite.
Japan Japan
281
Application to catalyst of mayenite consisting of ubiquitous elements
Conversion, Yield, Selectivity (%)

space velocity of 6000h-1 DWÛC. No catalyst deactivation 100 100
was observed after 24 hours of time on stream. Toluene
conversion on different catalysts is shown in Fig. 2. From 80 80
Fig. 2, Ni/Mayenite exhibited excellent performance. For

all Ni/Mayenite catalysts, the toluene conversion reached 60 60
nearly 100% at the temperature 80ÛC, even though the

40 40
concentration of Ni metal was only 1%. Results were
compared to that obtained with Mayenite alone. The latter 20 20
VKRZHG DOPRVW QR DFWLYLW\ XQWLO ÛC, moderate
DWÛC) and weaker activity than with Ni/Mayenite 0 0
(5wt FDWDO\VW DW ÛC. And also for Mayenite, 00 20
20 40
40 60
60
additionally to CO, CO 2 and H 2 , significant selectivity TimeTime(h)
(h)
toward benzene (22% at 8ÛC) was observed, but for
䕔:Conversion (Ni/Mayenite), 䕿:Conversion(Ni/Al2O3),
Ni/Mayenite, almost no benzene was observed.
䖃:H2 yield, 䕦:CO selectivity, 䕰:CO2 selectivity
The detailed UHVXOWVREWDLQHGDWÛC are presented in
Toluene concn. = 4000ppm
Fig. 3. H 2 and CO 2 yields increased but CO yield
decreased when the S/C ratio increased. These gas yield Fig. 4 Toluene conversion, H2 yield, CO and CO2
evolutions with the S/C ratio can be explained by the selectivity vs. Time.
reactions involved in toluene steam reforming (C 7 H 8 +
WROXHQH UHIRUPLQJ IRU PRUH WKDQ KRXUV DW ÛC, more
7H 2 O ĺ 7CO + 11H 2 , C 7 H 8 + 14H 2 O ĺ 7CO 2 + 18H 2 ).
stable than that of traditional Ni/Al 2 O 3 .
The water-gas shift reaction (CO + H 2 O ĺ CO 2 + H 2 )
The observed promotion of catalysts such as dolomite,
produced more H 2 and CO 2 at higher values of S/C ratios,
olivine by loading Ni metal for hydrocarbon reforming was
so the increase in the CO selectivity at the same time less
justified, but also easily devitalized because of carbon
H 2 and CO 2 yield could be explained, as a high steam
formation on the nickel metal surface [2, 3]. However, no
partial pressure made the water gas equilibrium shift toward
obvious decrease of activation was observed for our
hydrogen formation. However, the partial pressure of the
catalyst based on the above results. At least three possible
organic compound in the gas stream will be lower due to
reasons to account for such unexpected observation may be
the dilution as the S/C ratio rises. All of these will affect the
considered. The first possibility is that the excess S/C ratio
apparent kinetic constant.
can prevent or reduce the formation of coke on the catalyst,
From the above results, Ni/Mayenite (5wt%) exhibited
especially the ratio above 1.2 [4], but the long-time
excellent steam reforming activities above 600ÛC. To
evaluation of our experiments was carried out on the
confirm the practical applicability of this promising
smaller S/C (1.15). A second possibility is that the
industrial catalyst, long-term durability tests were
formation of coke deposits on the surface of Mayenite not
FRQGXFWHG DW WKH FRQGLWLRQ RI ÛC, space velocity of
nickel metal. In some cases, most of the formation of coke
6000h-1 DWÛC and inlet toluene concentration of 4000ppm,
deposited on the supported surface, but only a small amount
S/C is 1.15. The results are shown in Fig. 4, which
on the activity component surface [5]. The quantitative
illustrates that Ni/Mayenite maintains more than 98% of
analysis of coke amount on the after reaction catalyst
performed with the TG analyzer. The sample of 50-70mg
80 80
100 was heated from 30 to 1000ÛC with a heating rate of
H2 yield, CO, CO2 selectivity
100
10ÛC/min in air. The weight loss due to the combustion of
Toluene conversion (%)
70 70
H2 yield, CO, CO2 selectity
80 deposited carbon less than 0.1% was observed, which

Toluene conversion(%)
80
60 60 indicated nearly no carbon deposition on Ni/Mayenite.

60 60 Tolene Conversion For the third possibility is the “free” oxygen in the
H2 yield
CO selectivity
50 50 special structure of Mayenite, which was attributed to the
40 40 CO2 selectivity presence of hydroxide, peroxide and superoxide radicals in
40 40
the cages. So the super oxide radicals in the cages will
20 20 transfer to nickel sites to gasify the surface carbon on nickel
30 30
1.5 2.0 2.5 3.0 3.5 metal to CO, which is the reasonable explanation for the
1.5 2.0 2.5
S/C ratio 3.0 3.5 excellent performance of Ni/Mayenite [5].
S/C ratio
‫ە‬: Toluene conversion, ‫ڦ‬: H2 yield, 4. Conclusion

The newly synthesized nickel mayenite catalysts
‫ڦ‬: CO selectivity, ‫ڸ‬: CO2 selectivity
(Ni/Ca 12 Al 14 O 33 ) is developed and studied. It was observed
that Ni/Ca 12 Al 14 O 33 showed excellent sustainability against
Fig. 3 The influence of S/C on toluene conversion coke formation due to the “free oxygen” in the catalysts.
and products composition for Ni/Mayenite (5%).
282
Acknowledgement [2] J. Corella, J.M. Toledo and R. Padilla: Energy Fuels, 18

The author thanks Prof. C. Li, Institute of Process (2004), pp.713-720.
Engineering, CAS, China, for his useful comments. [3] J.N. Kuhn and Z.K. Zhao: Appl. Catal., A, 341 (2008), pp.43-
49.
References [4] T.J. Wang, J. Chang and P.M. Lv: Energy Fuels, 19 (2005),
[1] For example, T. Kamiya and H. Hosono: Semicond. Sci. pp.22-27.
Technol., 20 (2005), S92-S102. [5] L. Palacios, A. Cabeza, S. Bruque, S. G. Granda and M.A.G.
Aranda: Inorg. Chem., 47 (2008), pp.2661-2667.
283
Arrangement of Pd nanoparticles on SDS-functionalized

†
single-walled carbon nanotubes
TAN Zhenquan *, ABE Hiroya *, NAITO Makio * and OHARA Satoshi *
KEY WORDS: (Carbon Nanotubes) (Pd Nanoparticles) (Arrangement) (SDS) (Supramolecular Self-assembly)
1. Introduction in Scheme 1. SWCNTs (5mg, 0.05 wt %) in aqueous

Carbon nanotubes (CNTs) have many unique physical, solution (10 ml, containing 0.5 wt % SDS) were mixed for
electrical, mechanical and chemical properties and 8 hours assisted by ball-milling as previously described [3,
represent one of the most extensively studied 4]. The SWCNTs were essentially bundles with an average
nanostructured materials because of their potential diameter 50 nm. The bundles of SWCNTs were separated
applications in many fields. Surface functionalization and into individual nanotubes and/or small bundles, and
hybridization of CNTs currently attracts significant research dispersed in an SDS aqueous solution by ultrasonic
interest because CNTs are ideal templates for the treatment. SDS molecules were adsorbed onto the surfaces
decoration of functional nanoparticles. Among these of SWCNTs to form half-cylindrical supramolecular self-
research branches, one of the most attractive topics is to assembly oriented perpendicular to the CNT axis. A 2 ml
construct designed and controllable heterogeneous aqueous solution of palladium chloride (20 mM) was added
nanostructures on one-dimensional CNTs with sub ten to the SDS-functionalized SWCNTs solution. Since SDS is
nanometers diameter. Polymers and many organic an anionic surfactant, Pd (II) cations were selectively
molecules seem to be candidates for this objective because absorbed onto the walls of SWCNTs along the helix of the
they are reported to form ordered self-assembly half-cylinders of SDS due to the electrostatic interaction
nanostructures on CNTs, which provide suitable between Pd (II) cation and the anionic groups of sulfate in
combination sites to arrange metal nanoparticles or SDS molecules. The mixed solution was then irradiated for
quantum dots on CNTs by the specific bonding interactions 60 min by a UV lamp (O = 254 nm). Consequently, Pd
between the nanoparticles and the terminal groups of nanoparticles were site-selectively reduced by a
organic molecules.[1] Surfactant-functionalized CNTs are photoreduction reaction and formed ordered nanostructures
now also considered as another approach to control the on the surface of SWCNTs which used the supramolecular
designed heterogeneous nanostructures on one-dimensional self-assembly of SDS as a soft patterning template. The
CNTs. Surfactants have been widely studied because of the resulting nanostructures were characterized by scanning
advantages of dispersing CNTs in water and changing the electron microscopy (SEM, SU-70, Hitachi, Japan) and
surface physical properties of CNTs. SDS is one of the well transmission electron microscopy (TEM, JEM-2100F,
known surfactants to disperse and functionalize CNTs in JEOL).
water. It is also reported that SDS forms a supramolecular
self-assembly with half-cylinder structure on the surface of
CNTs.[2] The nanostructural pattern of SDS-functionalized
CNTs represents an ideal template to construct designed
one-dimensional heterogeneous nanostructures on the
surface of CNTs. In this study, we report site-selective
deposition and patterning of Pd nanoparticles on SWCNTs
by utilizing the supramolecular self-assembly of SDS acting
as a soft template. Since Pd nanoparticles have great
applications in fuel cell, high-performance catalyst and
hydrogen storage, it is of many scientific interests to
construct ordered one-dimensional Pd nanostructures on
SWCNTs.
2. Experiment Scheme 1. A schematic approach for the arrangement of Pd

The experimental approach for the site-selective nanoparticles on the SDS-functionalized SWCNTs.
synthesis of Pd nanoparticles templated by supramolecular
self-assembly of SDS-functionalized SWCNTs is described
Japan
284
Arrangement of Pd nanoparticles on SDS-functionalized single-walled carbon nanotubes
3. Results and Discussions of SDS-functionalized SWCNTs. It is clearly observed that

Figure 1 shows the SEM image of pristine SWCNTs (A) Pd nanoparticles formed ordered nanostructures that Pd
and TEM images of SDS-functionalized SWCNTs (B, C). nanoparticles arranged on the surface of SWCNTs (Fig.
The pristine SWCNTs are almost ca. 50 nm bundles and 2A). These nanostructures are very similar to those using
twisted together due to the van der Waals interaction (Fig. copolymers as a soft template.[1] Since SDS, the soft
1A). After dispersing in SDS aqueous solution, the large template, formed a periodic supramolecular self-assembly
bundles of pristine SWCNTs were effectively separated on SWCNTs, the deposited Pd nanonparticles also formed
into small bundle and/or individual SWCNTs (Fig. 1B). ordered periodic nanostructures on the surface of SWCNTs.
Figure 1C shows a high-resolution TEM photograph of Such periodic nanostructures were clearly observed by
SDS-functionalized SWCNTs. We can clearly observe the high-resolution TEM (Fig. 2B). The Pd nanoparticles have
ordered supramolecular self-assembly of SDS half- a size of 2.5 ± 0.5 nm. The inter-nanoparticle distance was
cylinders wrapped on the surface of SWCNTs. The ordered 4.5 ± 0.5 nm along the orientation parallel to the tube axis.
nanostructures of SDS with varying tilt angles can be This value is the same to the lateral striations of SDS half-
clearly observed in this photograph. The tilt angles of cylinders that were shown in Fig. 1C. This observation
helices depend on the diameter of the CNTs.[2] The lateral indicates that the Pd nanoparticles were selectively
striations of SDS supramolecular self-assembly were 4.5 ± deposited onto the SDS-functionalized SWCNTs along the
0.5 nm. This value is agrees well with the previous half-cylinders of SDS supramolecular self-assemblies
research.[2] The supramolecular self-assembly of SDS half- wrapped around the SWCNTs. Figure 2C shows a high
cylinders provide a soft template to deposit and arrange resolution image of Pd nanoparticles forming ordered
metal nanoparticles on the surface of SWCNTs to construct nanostructures wrapped around the SWCNTs. The
ordered heterogeneous nanostructures. nanostructures have a right helix twist with a tilt angle of -
24° relative to the tube axis. In our experiment, we
observed that the ordered nanostructures of Pd
nanoparticles have various helices and tilt angles wrapped
around SWCNTs. It indicates that the tilt angle of Pd
nanostructures depends on the various helices of SDS
supramolecular self-assembly on the surface of SWCNTs.
Figure 2D shows a dark field STEM image of Pd
nanoparticles wrapped around SWCNTs. The ordered
nanostructures of Pd nanoparticles arranged on SWCNTs
were also clearly confirmed by the STEM observation.
Fig. 1. TEM images of (A) pristine SWCNTs and (B,C) The crystalline structures of Pd nanoparticles were also
fine dispersed SDS-functionalized SWCNTs. confirmed by powder X-ray diffraction (XRD)
measurement. There sharp diffraction peaks were clearly
The photo-reduction reaction of palladium chloride in the observed in the XRD profile, which were assigned to (111),
suspension of SDS-functionalized SWCNTs was (200) and (220) planes of Pd nanoparticles.
characterized by the UV-Vis absorption spectroscopy. The In this study, we found that increasing the concentration
palladium chloride aqueous solution shows a clear of the palladium chloride aqueous solution resulted in a
absorption at 420 nm, which originates from the d-d significantly higher density of site-selectively deposited Pd
electron transition of Pd (II) ions. After irradiation by UV nanoparticles. The average size of Pd nanoparticles slightly
light, The absorption band of Pd (II) ions at 420 nm increased to 3.2 ± 0.5 nm. In the case of high coverage, it is
disappeared completely when Pd nanoparticles were found that the disordered Pd nanoparticles increased when
reduced and deposited on SWCNTs. This suggests the larger numbers of Pd nanoparticles deposit onto the SDS
complete reduction of Pd (II) ions and deposition of Pd functionalized SWCNTs. This may due to the deposition
nanoparticles onto the surface of SWCNTs. rate of Pd nanoparticles being higher than the equilibrium
rate of Pd absorbed to SDS molecules on the surface of
SWCNTs.
4. Conclusions
In summary, we report a route to site-selectively deposit
and arrange Pd nanopaticles on the surface of SDS-
functionalized SWCNTs. SDS formed supramolecular self-
assembly wrapped around SWCNTs. The terminal
functional group of SDS provided the combination site to
immobilize Pd nanoparticles. Pd nanoparticles are arranged
Fig. 2. TEM images of Pd nanoparticles selectively on the surface of SWCNTs and form ordered periodic
deposited on the SDS-functionalized SWCNTs. nanostructures. By control of the concentration of Pd (II)
ions, it also allows high density deposition of Pd
Figure 2 shows the high-resolution TEM images of nanoparticles on SWCNTs. This is very important for the
resulting nanostructures of Pd nanoparticles on the surface potential applications of these kinds of heterogeneous
285
nanostructures. This approach is easily applied to a variety References

of metal nanoparticles and/or quantum dots. It represents a [1] B. Li, L. Li, B. Wang, C. Y. Li: Nat. Nanotechnol., 4 (2009),
potential and simple chemical route to arrange pp.358-362.
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Mioskowski: Science, 300 (2003), pp.775-778.
ordered heterogeneous nanostructures on CNTs by utilizing
[3] Z. Tan, H. Xu, H. Abe, M. Naito, S. Ohara: J. Nanosci.
organic molecules as soft templates. Nanotechnol., 10 (2010), pp.3978-3982.
[4] Z. Tan, H. Abe, M. Naito, S. Ohara: Chem. Comm., 46 (2010),
pp.34363-4365.
286
†
NORIMATSU Wataru * and KUSUNOKI Michiko *
KEY WORDS: (Graphene) (Carbon nanotube) (Silicon carbide) (Transmission electron microscopy)
1. Introduction removed, and then the remaining carbon atoms form

Graphene, a one-atom-thick carbon material, has graphene layers or a nanotube film. In this study, we
attracted extensive research due to its novel structure and present crystallographic features of carbon-nanotube and
electronic properties, and to its extremely high carrier graphene layers formed epitaxially on the surface of
mobility for semiconducting devices [1]. Carbon- silicon-carbide, which were revealed by high-resolution
nanotubes (CNT) can be obtained by folding graphene transmission electron microscopy (HRTEM).
layer(s) into a cylinder, which is famous for its outstanding
electrical, thermal, and mechanical properties [2]. These 2. Experimental procedure
novel nano-structured carbon materials can be fabricated Graphene-on-SiC and CNT-on-SiC samples were
by the SiC thermal decomposition method [3-8]. Using prepared by annealing the 6H-SiC single crystal at 1450 ºC
this method, carbon-nanotube and graphene are selectively in a vacuum of 1.0×10-4 Torr. Detailed sample preparation
formed on SiC just by heating the silicon carbide substrate procedure was described in our previous papers. The
in vacuum. In a vacuum furnace, silicon atoms are crystallographic features of graphene and CNT on SiC
Fig. 1 (a) Bi-layer graphene formed on the Si-terminated SiC surface.

(b) Carbon-nanotube film on the C-terminated SiC surface.

Japan Japan
287
were examined by observation using JEM-2010-type and is suggested that after the Si removal, on the Si-face,
EM-002B-type transmission electron microscopes. Thin carbon atoms make bonds parallel to the surface indicating
specimens for observation were made by an Ar-ion the formation of a two dimensional graphene structure,
thinning method. while on the C-face they make bonds perpendicular to the
surface, resulting in CNT formation.
Fundamentally, graphene layers were formed on Si- 4. Conclusions
terminated SiC (0001) surfaces [3-5], while CNTs were on Nano-carbon structures formed on the SiC surfaces
C-terminated (000-1) surfaces [6-8]. Figure 1 shows the were presented, and were investigated by HRTEM
HRTEM images of (a) graphene layers on SiC (0001) and observations. On the Si-terminated face of SiC,
(b) carbon-nanotube film on SiC (000-1). In Fig. 1(a), homogeneous graphene layers were obtained. Whereas
bi-layer graphene is observed as a dark line contrast. on the C-terminated face, highly-dense and well-aligned
Graphene layers are formed covering the whole terrace of CNTs were produced.
the SiC surface. In addition, similar line contrast can be
seen in the interface between graphene and SiC, which is References
denoted by a dashed line. Carbon atoms in this layer have [1] K.S. Novoselov, A.K. Geim, S.V. Morozov, D. Jiang, Y.
strong covalent bonds with silicon atoms beneath, and this Zhang, S.V. Dubonos, I.V. Grigorieva and A. A. Firsov: Science,
layer is called a buffer layer, which doesn’t have the 306 (2004), p.666.
[2] S. Iijima: Nature, 354 (1991), p.56.
electronic features of graphene. Elevating annealing [3] W. Norimatsu and M. Kusunoki: Chem. Phys. Lett., 468
temperature increases the number of graphene layers. (2009), p.52.
On the other hand, carbon nanotubes are formed on C- [4] W. Norimatsu and M. Kusunoki: Physica E, 42 (2010), 691.
terminated SiC as shown in Fig. 1(b). Characteristic [5] W. Norimatsu and M. Kusunoki: Phys. Rev. B, 81 (2010),
features of these carbon nanotubes are that almost all the p.161410.
well-aligned nanotubes are of zigzag-type and formed [6] M. Kusunoki, T. Suzuki, K. Kaneko and M. Ito: Phil. Mag.
perpendicularly to the SiC surface, and that the density of Lett., 79 (1999), p.153.
the nanotubes is extremely high. The thickness of the [7] M. Kusunoki, T. Suzuki, T. Hirayama, N. Shibata and K.
carbon nanotube film can be controlled by annealing Kaneko: Appl. Phys. Lett., 77 (2000), p.531.
[8] M. Kusunoki, T. Suzuki, T. Hirayama, N. Shibata and K.
temperature and time.
Kaneko: Chem. Phys. Lett., 366 (2002), p.458.
Common features of graphene and CNTs on SiC are [9] Z. Wang, S. Irle, G. Zheng, M. Kusunoki and K. Morokuma:
their homogeneity and their strong bonding with the J. Phys. Chem. C, 111 (2007), p.35.
substrate. These features and the selectivity of graphene
or CNTs are based on the crystal structure of SiC [9]. It
288
Room-temperature Coulomb oscillation of Ni-Nb-Zr-H glassy alloys

with nanoscale size clusters†
M. Fukuhara*, H.Yoshida* and A.Inoue**
KEY WORDS: (Room temperature) (Coulomb oscillation) (Glassy alloys) (Nanoscale ) (Clusters) (Hydrogen)
(First-principles density functional calculation)
1. Introduction Since the glassy alloy can be considered a self-organized

Glassy alloys are peculiar metallic alloys that lack the assembly of low-capacitance, multiple-junction
long-range cyclic order of crystalline alloys, on the configuration, i.e., a huge assembly of 0.5-nm-sized
nanoscale. Therefore, glassy alloys, which are considered quantum dots, we can expect room-temperature three-
to be macroscopic materials with a mesoscopic system of terminal transistor.
nanostructures, are candidate materials for future
nanoelectronic devices. Following the theoretical 2. Experimental
pioneering work of Ben-Jacob and Grefen [1] and the The rotating wheel method under an argon atmosphere
subsequent discovery of the Coulomb blockade effect by was used for the preparation from argon arc-melted ingots
quantum-dot tunneling at low temperature, [2] a number of of amorphous ((Ni 0.6 Nb 0.4 ) 1-x Zr x ) 1-y H y alloy ribbons of 1-
studies have reported achievement of room-temperature mm width and 20-ȝm thickness. Hydrogen charging was
oscillation. [3] carried out electrolytically in 0.5 M H 2 SO 4 and 1.4 g/L
Recently, Fukuhara et al. [4, 5] have observed the thiourea (H 2 NCSNH 2 ) at room temperature and current
electric current-induced voltage oscillation in densities of 30 A/m2. [4, 5, 7]
((Ni 0.6 Nb 0.4 ) 0.7 Zr 0.3 ) 1-y H y JODVV\DOOR\\DW The specific electrical resistances of hydrogenated
temperature below 240 K, and ((Ni 0.6 Nb 0.4 ) 1-x Zr x ) 1-y D y specimens were measured by the four-probe method. [4-7]
[ DQG\48) alloys [6] at The I-V curve for the four-probe method was measured
room temperature. We propose the tunneling of individual from 0 mA to 100 mA with a constant current step of ±0.1
protons that are charging and discharging the capacitance of mA at room temperature, using a Semiconductor
Zr-H(D)-Ƒ-H(D)-Zr atomic bond arrays among the Zr(Nb)- Characterization System 4200 (Keithley Instruments Inc.).
tetrahedral sites, where b is the vacancy barrier, termed the Electrical resistance measurements of onset
free volume, in the glassy alloys. Furthermore, the superconductivity were determined by the temperature
frequency of the (Ni 0.36 Nb 0.24 ) 90.1 Zr 9.9 glassy alloy dependence of the DC current four-probe method at a
decreased remarkably with increasing capacitance (C) and cooling rate of 1 K/min from 323 K to 4.2 K in He of
resistance (R) in the dc/ac circuit at room temperature.[7] ambient pressure under a magnet in the High Field
This resembles discharging behavior in which a constant Laboratory (IMR, Tohoku University).
voltage-discharge tube with a parallel condenser and high The optional atom configuration and the adiabatic
resistance causes block oscillation, which is derived from potential energy curve of the icosahedral cluster that
the charging and discharging of the capacitance. Thus the consisted of Ni-Nb-Zr-H were calculated by the first-
glassy alloy could be regarded as a dc/ac converting device principles density functional calculations using the Vienna
with a large number of nanoscopic capacitors.[7] Indeed, ab initio simulation package.[8] The nuclei and core
the hydrogenated glassy alloy is characterized by an electrons are described by the projector augmented plane-
assembly (free volume) of such vacancies (0.7-3 at%), wave method and the wave functions are expanded in a
which are distributed homogeneously among the plane wave basis set with a cutoff energy of 293.2 eV.
icosahedral clusters. The hydrogen atoms of Ni-Nb-Zr
glassy alloys settle stably into four-coordination sites that 3. Results
are surrounded tetrahedrally by four Zr (Nb) atoms, from The dc electrical resistances of the
analysis results of the XAFS spectra using synchrotron (Ni 0.36 Nb 0.24 Zr 0.40 ) 90 H 10 glassy alloy were measured in the
radiation photons at SPring-8.[8] Thus we propose the current region from 1 nA to 100 mA during cooling and
icosahedral Zr-centered Zr 5 Ni 5 Nb 3 cluster (~0.55 nm), as a heating runs at a temperature region between 300 and 7 K.
possible model for the main cluster of the glassy alloy.[9] The maximum amplitude of the Coulomb oscillation

* IMR, Tohoku University, Sendai, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Tohoku University, Sendai,, Japan Japan
289
Room-temperature Coulomb oscillation of Ni-Nb-Zr-H glassy alloys with nanoscale size clusters
LQFUHDVHV DV WKH FXUUHQW GHFUHDVHV GRZQ WR ȝ$ DQG WKHQ Nb are nonmagnetic elements. In the atomic configuration
decreases in the lower current region from 100 to 1nA, of Ni 5 Zr 5 Nb 3 cluster, five Ni atoms are separately
indicating an occurrence of the optimum current for coordinated against Zr and Nb atoms.[8]
quantum dot tunnelling between the icosahedral Zr 5 Ni 5 Nb 3
cluster islands.
When we apply a magnetic field to the specimen from 0 References
to 15 T at 100 and 200 K in parallel and normal directions, [1] E.Ben-Jacob and Y.Grefen: Phys.Lett., 108A(1985), pp. 289.
we observed the voltage oscillation from around 6 T and 9 [2] M.A.Kastner, P.F.Kwasnick and J.C.Licini: Phys. Rev. B36
T at 100 K and 200 K, respectively. The amplitude of (1987), pp.8051.
vibration increases with increasing of magnetic field up to [3] For an example, H.W.Ch.Postma, T. Teepen , Z.Yao and M.
15 T except for a parallel magnetic field above ~12 T at Grifoni and C.Dekker: Science, 293 (2001), pp.76.
200 K. Here we should be noted that the chemical potential [4] M.Fukuhara, A.Kawashima, S.Yamaura and A.Inoue:
of the conduction electrons in the ferromagnetic island is Appl.Phys.Lett. 90 (2007), pp.20311.
affected by magnetic field. This is similar to variation in [5] M.Fukuhara, S.Yamaura and A.Inoue: J.Phys: Conf. Ser., 114
electrostatic potential caused by gate voltage in field (2009), pp.012086.
electrostatic transistor (FET). By analogy, we infer that [6] M.Fukuhara and A.Inoue: Europhy.Lett., 83 (2008), pp. 36002.
application of magnetic field induces Coulomb oscillation [7] M.Fukuhara and A.Inoue: J.Appl.Phys., 105 (2009), pp.
derived from noticeable variation in the chemical potential 063715.
of an isolated ferromagnet (island) in ferromagnetic fields. [8] M.Fukuhara, N.Fujima,H.Oji, A. Inoue and S.Emura: J.Alloy
In this study, the ferromagnetic metal responsible for the Comp., 497 (2010), pp.182.
magneto- Coulomb oscillation is Ni alone, because Zr and
290
†
Superconductivity of Ni 0.324 Nb 0.216 Zr 0.36 H 0.1 glassy alloys
YOSHIDA Hajime *, FUKUHARA Mikio *, INOUE Akihisa *
KEY WORDS: (Glassy alloys) (Superconductor) (Meissner effect) (Hydrogen charging) (Nanoclusters)
1. Introduction mA at cooling and heating rates of 1 K/s from 373 K to 5.5

Glassy alloys are peculiar metallic alloys in that they K in He of ambient pressure (Top Loading Refrigerated
lack the long-range cyclic order of crystalline alloys, on the Cryostat; JECC Torisha Co.). The distance between the two
nanoscale [1, 2]. Therefore, glassy alloys, which are voltage electrodes was 20 mm. Electrical resistance
considered to be macroscopic materials with a mesoscopic measurements of superconductivity below 4 K were
system of nanostructures, are candidate materials for future determined by the temperature dependence of the DC
nanoelectronic devices. Indeed, the electronic char- current four-probe method at a cooling rate of 1 K/min
acteristics of (Ni 0.36 Nb 0.24 Zr 0.40 ) 100-y H y \ from 323 K to 1.4 K in He of ambient pressure under a
amorphous alloys are characterized by semi- superior- and magnetic in High Field Laboratory (IMR, Tohoku
superconductor and Coulomb oscillation, as hydrogen University).
increases [3]. In the present work, we focus on
superconductivity in the glassy alloys with nanoclusters, as
a function of hydrogen.
Superconductivity of amorphous phases has been
observed in many materials, such as, amorphous binary
MoSi[4] and NbGe[5] films, and amorphous ternary
Mo 80 P 10 B 10 [6] and Hf 55 Nb 30 Si 15 [7] ribbons. These
are transition metal-metalloid-type alloys. On the other
hand, superconductivity of binary and ternary metal-metal-
type amorphous alloys, such as Zr 64 Ni 36 [8] and
Cu 40 Nb 30 Ti 30 [9], has also reported. However, the critical
temperature for these alloys are not high, except for
Cu 40 Nb 30 Hf 30 [9]. In the reference [3], we have reported an
effect that the amount of hydrogen content gave to the Fig. 1 Temperature dependence of electrical resistance
superconductivity characteristic in terms of electromagnetic for Ni-Nb-Zr-H glassy alloy.
interaction under strong magnetic field. As far as we know,
3. Experimental Results
there are no previous reports on this subject for glassy
We show the temperature dependence of electrical
alloys with hydrogen, and also no distinct interpretation for
resistance for Ni-Nb-Zr-H in Fig. 1. In a cooling run from
superconductivity of glassy alloys.
300 K the value of resistance increases with decreasing
temperature like for a semiconductor.
2. Experimental Procedure The current induced Coulomb oscillations are observed near 250
The rotating wheel method under an argon atmosphere K in heating run. The total variation of the resistance is not
was used for the preparation from argon arc-melted ingots ODUJHDQGWKHUHVLVWLYLW\LVRIWKHRUGHURI-cm. We
of amorphous Ni 36 Nb 24 Zr 40 alloy ribbons of about 1-mm observed two jumping up steps around 50 K. When
width and 30-μm in thickness. Hydrogen charging was temperature decreases still more, the resistance curve
carried out electrolytically in 0.5 M H 2 SO 4 and 1.4 g /L begins to drop abruptly from 10 K. The heating run from 6
thiourea (H 2 NCSNH 2 ) at room temperature and at the K almost follows on the cooling run’s trace except
current densities of 30 A/m2. The amounts of hydrogen resistance variation near 250 K, i.e., the current induced
absorbed in the specimens were measured by the inert gas Coulomb oscillation. Figure 2 shows the resistance
carrier melting-thermal conductivity method. The structure dropping behavior in the low temperature area. The
of the (Ni 0.36 Nb 0.24 Zr 0.40 ) 100-y H y \) glassy alloys decrease from 10 K to 3 K is about 13 % and the following
was identified by X-ray diffraction with Cu KĮ radiation at abrupt variation was observed below 3 K. The resistance-
grazing incident mode. The specific electrical resistance of zero temperature was found to be 2.1 K. This curve shows a
hydrogenated specimens was measured by the four-probe behavior as if there are two kind of transition, as shown in
method DC and AC Current Source 6221, Nano Voltmeter the figure. We measured the temperature dependence of
2182A; (Keithley Instruments Inc.) with a DC current of ±1 magnetization underᴾ 50 Oe in order to compare with the
† Received on November 1, 2010 Transactions of JWRI is published by Joining and Welding

ᴾ ** JWRI, Osaka University, Osaka, Japan Japan
291
Superconductivity of Ni0.324Nb0.216Zr0.36H0.1 glassy alloys
ᴾᴾ resistance measurements.ᴾ A temperature variation of the

magnetization at 50 Oe and the magnetization loop at 2 K
and 5 K areᴾ shown in Fig. 3(a), (b) and (c), respectively.
The magnetization at higher temperature than 10 K shows a
small positive value due to Pauli paramagnetism. However,
in a lesser temperature range than 10 K, the magnetization
reveals a negative value and shows two steps of stages.
Taking the temperature dependence of electrical resistance
and magnetization into consideration, there are two peculiar
regions, 2.1 K <T< 10 K and T < 2.1 K, for
superconductivity. Magnetic loop at 2 K shows a
complicated aspect in comparison with one at 5 K. In other
words, the behavior of low temperature shows the aspect of
the loop with plural superconducting phases. We measured
the magnetoresistance effect at 4.2 K in Fig. 4. The
measured curve shows a small abnormal peak at 4 T and
Fig. 2 Resistance variation in low temperature area. then saturates, while the nonhydrogenized sample does not
show the irregular peaks. A similar peak was also observed
in a temperature dependent resistance curve.
Fig. 4 Magnetoresistance effect at 4.2 K.

4. Conclusions
We measured temperature- and magnetic field
dependences of superconductivity for
(Ni 0.36 Nb 0.24 Zr 0.40 ) 100-y H y glassy alloys in the temperature
region from 300 K to 2 K and in the magnetic field from 0
T to 10 T. There are possibilities that the specimens have
two kind of superconductive phase with transition
temperatures of 2.1 K and 10 K. The latter phases showed
an irregular peak at 4T.
References
[1] G.J. Fan and H. J. Fecht: J. Chem. Phys., 116 (2002), pp.5002.
[2] A.R. Yavari: Nature, 439 (2006), pp.405.
[3] M. Fukuhara, H. Yoshida, K. Koyama, A.Inoue and Y.miura:
J. Nanosci. Nanotechnol., vol.10 No.8 (2010).
[4] A.W. Smith, T.W. Clinton, C.C. Tsui and C. J. Lobb: Phys.
Rev. B, 49 (1994), pp.12927.
ᴾ [5] N. Kokubo, J. Aarts and P.H. Kes: Phys. Rev. B, 64 (2001),
pp.014507.
[6] W.L. Johnson, S.J. Poon, J. Durand and P. Duwez: Phys. Rev.
B, 18 (1978), pp.206.
[7]A. Inoue, Y. Takahashi, C. Suryanarayana and T. Masumoto: J.
Mater. Sci., 17 (1982), pp.1753.
[8] A. K. Bhatnagar, R. Pan and D.G. Naugle: Phys. Rev. B, 39
(1989) pp.12460
Fig. 3 (a) Magnetization vs. temperature [9] A. Inoue, C. Suryanarayana and T. Masumoto: J. Mater. Sci.,
curve under 50 Oe, (b) Magnetization loop 16 (1981), pp.1391.
at 2 K.
292
Enhancement of solderability of Cu 60 Zr 30 Ti 10 bulk metallic glass by

dealloying in hydrofluoric acid solution†
NAOI Takehiro *, NISHIKAWA Hiroshi *, TAKEMOTO Tadashi *, ABE Hiroya *,

FUKUHRA Mikio ** and INOUE Akihisa **
KEY WORDS: (Bulk metallic glass) (Dealloying) (Laser soldering) (Lead-free solder)
1. Introduction
Despite the good mechanical, chemical [1] and
magnetic [2] properties of bulk metallic glasses (BMGs),
the serious issue during the joint of BMG is the
recrystallization of the glassy phase at high temperatures. In
order to extend the engineering application of BMG it is
necessary to establish appropriate joint processes of
BMG/BMG and BMG/crystalline metal [3-4]. The lead-free
soldering process is a low temperature joining process and
therefore it can be performed below the crystallization
temperature of BMGs. However, many kinds of BMGs Fig. 1 Cross section of sample after HF treatment
such as Zr 55 Cu 30 Ni 5 Al 10 and Cu 60 Zr 30 Ti 10 exhibit no
wetting of lead-free solder on the surface of BMGs because In the reflow process, a Sn-3.0 mass%Ag-0.5 mass%Cu
of Zr- and Ti-oxide on their surface [5]. In previous (SAC) solder ball with a diameter of 1 mm was set on the
research, we found that selective leaching of Zr and Ti HF treated Cu 60 Zr 30 Ti 10 sample with RMA flux. Then, the
occurred upon immersing Cu 60 Zr 30 Ti 10 into HF solution, sample was put into a radiation furnace in a N 2 atmosphere
which resulted in the formation of a Cu rich layer [6]. and heated according to the temperature rise profile shown
The objective of this study is to evaluate wettability of in Fig. 2.
solder on the surface of HF treated Cu 60 Zr 30 Ti 10 in order to
make better joints between Cu 60 Zr 30 Ti 10 and lead-free
solder.
2. Experimental
Cu 60 Zr 30 Ti 10 BMG ribbon was cut into 20 mm ᶣ 20
mm ᶣ 70 ȝm strips and polished by SiC paper with 2000-
grit. The surface treatment was performed by immersing in
0.5 mol/L HF solution for 13 s at room temperature.ᴾ The
formation of Cu phase was confirmed with the amorphous
pattern by X-ray diffraction (XRD) as in the previous
study [6]. The porous layer with the thickness of about 500
nm was observed from scanning electron microscopy
(SEM) image as shown in Fig. 1. Fig. 2 Thermal profile of the reflow process.
Table 1 Some characteristics and preheating process of solder pastes used for laser soldering.

* Joining and Welding Research Institute, Osaka Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
University,Osaka, Japan Japan
** Institute for Materials Research, Tohoku University,
ᴾ Sendai, Japan
293
Enhancement of solderability of Cu60Zr30Ti10 bulk metallic glass by dealloying in hydrofluoric acid solution
Table 2 Wetting behavior of solder pastes.
In the laser soldering process, the wetting behavior of

lead-free solder on the sample was summarized in Table 2.
In the case of SAC there is a serious effect of laser power
on the wetting behavior of the solder. A good wetting
behavior of solder paste at only 12 W and 13 W was
observed. On the other hand, SB solder paste showed good
wetting at higher and lower laser power than SAC. This is
due to the differences in melting temperature of solder paste
and dissolution rate of Cu into molten solder. As shown in
Table 1, the melting temperature of SAC is 490 K and SB
is 412 K. So, at 11 W, SAC showed insufficient wetting
behavior because of inadequate melting time, although SB
showed good wetting at the same laser power. Additionally,
Fig. 3 The top surface of the soldered sample. SB exhibited no dewetting from 16 W to 18 W, which
showed dewetting in the case of SAC because of too long
reaction time with Cu surface. This is because it could be
estimated from Sn-Bi-Cu and Sn-Ag-Cu ternary alloy phase
diagrams that dissolution rate of Cu into SB is slower than
that into SAC. Therefore SB showed no dewetting at high
laser power.
Figure 3 is the top view of solder pastes after the laser
heating at 13 W. The spread area of SB is larger than that
of SAC despite the same laser power. In the case of SAC,
the diameter of spread area is about 1.2 mm equal to the
diameter of laser irradiation area, and SB spread with the
diameter of about 2 mm, which is larger than the laser
irradiation area. This would appear that SB solder melted
not only in the laser irradiated area but also in the heat
Fig. 4 SEM image of IMC layer at the SAC/Cu affected zone because of the low eutectic temperature of SB.
layer interface after laser process In fact, the wetting behavior of SB solder is better than
SAC.
Figure 4 shows the SEM image of a cross section at the
In the laser process, two kinds of solder pastes were joint interface between HF treated Cu 60 Zr 30 Ti 10 / SAC
prepared as shown in Table 1. Solder pastes were applied solder paste. The intermetallic compound layer with the
with 50 ȝm thickness on the HF treated Cu 60 Zr 30 Ti 10 . After thickness of about 400 nm was formed at the interface. This
preheating, the laser irradiation was performed. The laser means that the porous Cu layer properly reacted with SAC
irradiation time was 0.01 s and the laser power range from solder by the laser heating.
8 to 20 W at 1 W interval. The top surface of the soldered
sample was observed by optical microscope (OM) and the 4. Conclusion
cross sections of joint interfaces were observed by SEM. HF treatment and laser soldering was carried out to
react with Cu 60 Zr 30 Ti 10 BMG and lead-free solder. The
3. Results & Discussion main results were summarized as follows
ᴾ ᴾ The wetting behavior of lead-free solder on the HF (1) In the reflow process, the HF treated Cu 60 Zr 30 Ti 10
treated sample was evaluated by the spread area of the sample showed complete dewetting due to the
solder on the sample. In the reflow process, during the early dissolution of the thin Cu-rich layer into the molten
stage of the process, the molten solder seemed to spread on solder.
the sample surface, and then the sample showed complete (2) The laser process with 0.01 s irradiation time offered
dewetting during the heating due to dissolution of the thin good wettability of SAC and SB solder pastes. At the
Cu-rich layer into the molten solder. interface, an IMC layer was observed. The wetting
behavior of SB is better than SAC because SB solder
294
paste showed good wetting at broader laser power [2] A.Makino, T.Bitoh, A.Kojima, A.Inoue, T.Matsumoto.: J. of
ranges than SAC paste. The spread area of SB is larger ᴾ ᴾ Magnetism and Magnetic Mater., 215-216 (2000) , pp.288-292.
than that of SAC. This is attributed to the lower melting [3] Y.Kawamura: Mater. Sci. and Eng. A, 375-377 (2004),
temperature and slower Cu dissolution rate of SB. pp.112-119.
[4] Y.Kawamura, Y.Ohno: Scripta Mater., 45 (2001), pp.127-132.
In this study, the possibility to enhance the solderability of
[5] H.Nishikawa, K.WongPiromsarn, H.Abe, T.Takemoto,
Cu 60 Zr 30 Ti 10 by selective leaching in HF solution and laser ᴾ ᴾ M.Fukuhara, A.Inoue: Mater. Sci. and Eng. B, 148 (2008),
soldering was found. pp.124-127.
[6] H.Abe, K.Sato, H.Nishikawa, T.Takemoto, M.Fukuhara,
Reference A.Inoue: Mater. Trans., 50 (2009), pp.1255-1258.
[1]ᴾ A. Inoue: Materials Science and Engineering A, 267 (1999), ᴾ
ᴾ ᴾ pp.171-183.
295
Local structures of amorphous (Ni 0.6 Nb 0.4 ) 100-x Zr x (x=30, 35, 40)
†
alloys by XAFS
MATSUURA Makoto *, KONNO Kazuya **, FUKUHARA Mikio *, FUJIMA Nobuhisa ***
and INOUE Akihisa ****
KEY WORDS: (XAFS) (Local structure) (Amorphous) (Metallic glass) (NiNbZr) (Icosahedral cluster)
1. Introduction the Zr and Nb K-edges and Si(111) for the Ni K-edge. The
A wide composition range of amorphous-forming ability higher harmonics of the incident X-ray were reduced by
has been reported in the ternary Ni-Nb-Zr alloy system by two Rh-coated mirrors. The XAFS data were analyzed
Kimura et al. [1]. Because Zr and Nb have high hydrogen using coded program Athena.
permeability, amorphous Ni-Nb-Zr alloys have been studied
to develop superior hydrogen permeation materials. Atomic 3. Results and discussion
structure of the amorphous Ni-Nb-Zr(-H) alloys has been Figure 1 shows the results of the XAFS oscillations ᷒
studied Yamaura et al [2]. and Sakurai et al [3] by XRD (k) weighted by k3 of the Ni-Kedges for the amorphous
and XAFS, respectively, in which the local structural (Ni 0.6 Nb 0.4 ) 100-x Zr x (x=30, 35 and 40) alloys. Figure 2
change by hydrogen absorption was the main issue. shows the results of the Fourier transform |F(r)| of k3Ὁ᷒(k)
Recently amorphous (Ni 0.6 Nb 0.4 ) 100-x Zr x (x=30 and 40) of the Ni K-edge for amorphous (Ni 0.6 Nb 0.4 ) 100-x Zr x (x=30,
alloys attracted much attention from a quiet different 35 and 40) alloys. The k-range in the Fourier transform is
viewpoint. Fukuhara et al. found strange behavior of the 2<k<12(Ḩ-1). The Fourier transforms of the Nb and Zr K-
electrical conductivity for the amorphous (Ni 0.6 Nb 0.4 ) 100- edges are shown in Fig. 3 and 4, respectively with the same
x Zr x H y (x= 30, 40 and y= 9 - 11) alloys such as the k-range as for the Ni K-edge.
Coulomb oscillation [4]. Oji et al. measured XAFS spectra The characteristic features of the XAFS results are that
for the amorphous (Ni 0.6 Nb 0.4 ) 100-x Zr x (x=30, 40) alloys the |F(r)| curves of the three elements do not change
and their hydrogenated (Ni 0.6 Nb 0.4 ) 100-x Zr x H y (x=30, 40 continuously with Zr concentration but change sharply from
and y=9 and 11) ones [5]. They achieved curve fitting x=30 to 35. This indicates that the local structures of the
analysis for the XAFS results of the Nb and Zr K-edges, amorphous (Ni 0.6 Nb 0.4 ) 100-x Zr x alloys of x<35 are different
(not for the Ni K-edge) and estimated lattice parameters for from those of x>35. The second feature of the XAFS results
these amorphous alloys and their hydrogenated one. is that the first peak of the |F(r)| for the Ni K-edge clearly
In order to elucidate the structural origin of the strange splits into two while those for the Nb and Zr ones show a
electrical behaviors for these hydrogenated amorphous single peak.
alloys, it is necessary to obtain more detail structure Considering atomic radii of the constituent elements, i.
information; concentration dependence of the local e. r Ni =1.24, r Nb =1.47 and r Zr =1.60 ( in Å ), the nearest
structures of the x=30, 35 and 40 for (Ni 0.6 Nb 0.4 ) 100-x Zr x neighbor peak of the |F(r)| for the Ni K-edge consists of Ni-
amorphous alloys and fitting analysis for the Ni K-edge
䢳䢲
XAFS data as well as the Nb and Zr K-edges. In the present (Ni0.6Nb0.4)100-xZrx
Ni K-edge
work XAFS measurements for the (Ni 0.6 Nb 0.4 ) 100-x Zr x 䢺
x=40
(x=30, 35 and 40) alloys were carried out and the results
were compared with the first principle calculation based on 䢸
the icosahedral cluster model.

䣭䢬䪼䢪䣭䢫
䢶
x=35
䢵
2. Experiments 䢴
x=30
Ribbon samples were prepared by a melt-quenching
䢲
technique using a single-roller apparatus. XAFS
measurements of the Ni, Nb and Zr K-edges were made at 䢯䢴
20K in a transmission mode at beam line BL14B2 of the 䢳䢴䢵䢶䢷䢸䢹䢺䢻䢳䢲䢳䢳䢳䢴䢳䢵䢳䢶

large scale synchrotron radiation facility, SPring-8, in 䢯䢳
䣭䢪䱛䢫
Hyogo, Japan. The incident X-ray was monochromatized Fig.1 ;$)6 RVFLOODWLRQ ȤN 㺃 k3 of the Ni K-edge for
by a Si double crystal monochromator: Si(311) plane for amorphous (Ni0.6Nb0.4)100-xZrx (x=30, 35 and 40) alloys at 20K.
† Received on 30 September 2010 ****ᴾ Tohoku University,2-1-1 Katahira, Aoba,Sendai 980-8577
* Institute for Materials Research, Tohoku University, Japan
2-1-1 Katahira, Aoba, Sendai 980-8577, Japan Transactions of JWRI is published by Joining and Welding
** National College of Technology-Sendai, 48 Nodayama, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Shiote-Aza, Natori 981-1239, Japan Japan
*** Faculty of Engineering,Shizuoka University,Hamamatsu
432-8561, Japan
296
Local structures of amorphous (Ni0.6Nb0.4)100-xZrx(x=30, 35, 40) alloys by XAFS
䢺䢵䢰䢷
Ni K-edge (Ni0.6Nb0.4)100-xZrx (Ni0.6Nb0.4)100-xZrx

Nb K-edge
䢵䢰䢲
䢴䢰䢷
䢢䣺䢿䢵䢲
䢢䣺䢿䢵䢷
䣾䣈䢪䣴䢫䣾䢢䣱䣨䢢䣭䢬䢢ȮN
䢸
䢴䢰䢲
䢢䣺䢿䢶䢲
䢵
䢳䢰䢷
x=40
䣾䣈䢪䣴䢫䣾䢢䣨䣱䣴䢢䣭䢬ȮN
䢳䢰䢲
䢵
䢶
䢲䢰䢷
䢲䢰䢲
x=35 䢲䢰䢷䢳䢰䢲䢳䢰䢷䢴䢰䢲䢴䢰䢷䢵䢰䢲䢵䢰䢷䢶䢰䢲
䣴䢪ύ
䢴
Fig.3 Fourier transform of the Nb K-edge of k3㺃
ȤN IRU the amorphous (Ni0.6Nb0.4)100-xZrx
x=30 (x=30, 35 and 40) alloys at 20K.
䢲
䢲䢰䢷䢳䢰䢲䢳䢰䢷䢴䢰䢲䢴䢰䢷䢵䢰䢲䢵䢰䢷䢶䢰䢲
䣴䢪ύ 䢷
Fig.2 Fourier transform of the Ni K-edge of k3㺃ȤN (Ni0.6Nb0.4)100-xZrx
Zr K-edge
for the amorphous (Ni0.6Nb0.4)100-xZrx (x=30, 35 and 䢶
40) alloys at 20K. x = 30

x = 35
䣾䣈䢪䣴䢫䣾䢢䣱䣨䢢䣭䢬ȮN
Ni correlations and the second one Ni-Nb and Ni-Zr ones. 䢵 x = 40
䢵
This can be proved by the fact that the intensity of the first
shoulder in the |F(r)| decreases with increase in Zr 䢴
concentration. On the contrary, the intensity of the second

䢳
one increases with Zr as shown in Fig. 1. A broad single
peak of |F(r)| for the Nb and Zr K-edges may consist of
䢲
mainly Nb-Ni and Zr-Ni correlations and a small number 䢲䢰䢷䢳䢰䢲䢳䢰䢷䢴䢰䢲
䣴䢪ύ
䢴䢰䢷䢵䢰䢲䢵䢰䢷䢶䢰䢲
of Nb-Nb(Zr) and Zr-Zr(Nb) ones. One of the authors, N.

Fujima, calculated electronic states of the icosahedral Fig.4 Fourier transform of the Zr K-edge of k3㺃
Ni 5 Nb 3 Zr 5 clusters and optimized structures by using the ȤN IRU the amorphous (Ni0.6Nb0.4)100-xZrx
first principles calculation. The results of the calculation (x=30, 35 and 40) alloys at 20K.
suggest that Ni-centered icosahedral clusters are most stable
among three types of a centered atom (Ni, Nb and Zr). References
There are two types of energetically stable icosahedrons, i.e. [1]H. Kimura, A. Inoue, S. Yamaura, K. Sasamori, M. Nishida, Y.
distorted one(d-icosa) and isotropic one(i-icosa). The d- Shimpo and H. Okouchi: Mater. Trans., 44 (2003), pp.1167-
icosa exhibits similar atomic configuration as the 1171.
NiZr(C33) and NiZr 2 (C16) crystalline compounds. Fourier [2] S. Yamaura, M. Sakurai, M. Hasegawa, K. Wakoh. Y. Shimpo,
transforms |F(r)|’s are calculated for the two Ni-centered M. Nishida, H. Kimura, E. Matsubara and A. Inoue: Acta
icosahedral clusters, d-icosa and i-icosa, using the coded Mater., 53 (2005), pp.3703-3711.
program Artemis. |F(r)| result of the Ni K-edge for i-icosa [3] M. Sakurai, S. Yamaura, K. Wakoh, E. Matsubara and A.
Inoue: J. Metastable and Nanocrys., 24-25 (2005), pp.551-554.
shows a single broad peak while d-icosa shows a tendency [4] M. Fukuhara and A. Inoue: J. Appl. Phys., 105 (2009),
of splitting. Though further elaborated works are necessary, pp.63715-63719.
a distorted icosahedron with a similar local structure as Ni- [5] H. Oji, K. Handa, J. Ide, T. Honma, S. Yamaura, A. Inoue, N.
Zr compounds is a favorable structural model for the Umesaki, S. Emura and M. Fukuhara: J. Appl. Phys., 105
(Ni 0.6 Nb 0.4 ) 65 Zr 35 amorphous alloy. (2009), pp.113527-113533.
297
Effects of photon irradiation in UV and VUV regions during

†
plasma processing of organic materials
CHO Ken *,****, TAKENAKA Kosuke *,****, SETSUHARA Yuichi *,****, SHIRATANI
Masaharu **,****, SEKINE Makoto ***,**** and HORI Masaru ***,****
KEY WORDS: (Inductively-coupled plasma), (Low-inductance antenna), (Low-damage process), (Hard x-ray
photoelectron spectroscopy)
1. Introduction
Next-generation devices including flexible displays, generator at 13.56 MHz via a matching network. Each LIA
thin-film photovoltaic cells and advanced ULSIs (low-k unit was connected in parallel to the matching network. The
interlayer and EUV lithography) are expected to occus in LIA unit consists of a U-shaped antenna conductor, which
combination with polymer materials [1,2]. For successful was fully covered with dielectric tubing for complete
development of these devices, therefore, it is of great isolation from the plasma [4]. The chamber had a 500 mm
significance to control polymer surface and/or interface inner diameter and a 200 mm height, which was connected
with functional layers in terms of chemical and physical to a diffusion chamber with a 500 mm inner diameter and a
structures. In order to satisfy these requirements, it is 400 mm height. The Ar-O 2 mixture plasma was sustained at
necessary to use plasma processes, because plasma has an oxygen partial pressure (R p ) of 20% at a total pressure of
high-reactivity due to ions and radicals. However, bond- 2.6 Pa at an RF power of 1 kW. Optical emission spectra in
dissociation energies of polymer materials for thermal UV and VUV regions were measured with a VUV
decomposition are less than that of inorganic materials (3.4 monochrometer mounted on the sidewall of the chamber.
eV for the O-C(=O) bond, 3.6 eV for the C-CH 3 bond and For evaluating the interactions of the polymer surface
8.4 eV for C=O bond). Thus, it is considered that ions, with UV and VUV photons from the plasmas, PET films
radicals, photons and electrons from plasma may (thickness 100 Pm) were exposed to photons from the Ar-
give significant degradation in chemical bonding structures O 2 mixture plasmas by covering the PET samples with a
of soft materials beneath the surface and/or the MgF 2 window. Here it is noted that thickness of the MgF 2
inorganic/organic interface. Therefore, it is necessary to window is 2 mm. The MgF 2 window is transparent in
understand plasma-polymer interactions for development of UV+VUV regions (wavelength longer than 115 nm).
low-damage and low-temperature plasma processes. Therefore, it is possible to evaluate the effects of photo-
As one of the effective plasma sources for these irradiation by comparing results of the sample with a
processes, inductivity-coupled plasma sources have been plasma exposed sample [5].
developed with multiple low-inductance antenna (LIA)
modules, which allowed low-voltage operation of high-
density ICPs [3]. In terms of interactions of radiations from
plasmas with organic materials surface, radiations in
vacuum ultraviolet (VUV) and ultraviolet (UV) are
significant in that the photon energies are higher than the
bond dissociation energies. In this study, interactions of
optical emissions from Ar-O 2 mixture plasmas with
polymer surfaces have been investigated on the basis of
surface morphological changes and non-destructive depth
analyses of chemical bonding states in the nano-surface
layer of polyethyleneterephthalate (PET) films via hard x-
ray photoelectron spectroscopy (HXPES).
2. Experimental
A schematic diagram of the process chamber is shown
in Fig. 1. The LIA units were mounted on the top flange of Fig. 1 Schematic diagram of the discharge chamber.
the discharge chamber and were coupled to a RF power
* JWRI, Osaka Univ., Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Dpt. of Electronics, Kyushu Univ., Fukuoka, Japan Japan
*** PLANT, Nagoya Univ., Nagoya, Japan
**** JST, CREST
298
Effects of photon irradiation in UV and VUV regions during plasma processing of organic materials
(a) Raw (b) Plasma (c) UV+VUV

Rq = 1.0 nm Rq = 5.6 nm Rq = 0.9
nm
Fig. 2 Typical AFM images of the PET surface; (a) before and (b) after direct exposure to the plasma,
(c) after irradiation with the UV+VUV photons from the plasma.
For investigation of surface morphological changes, the The HXPES and XPS C1s spectra for PET films
sample surface was observed with an atomic force without and with direct exposure to the Ar-O 2 mixture
microscope (AFM). The depth analysis of chemical plasma and irradiations with photons from the Ar-O 2
bonding states was carried out by hard x-ray photoelectron mixture plasma are shown in Fig. 3. The HXPES spectra
spectroscopy (HXPES) and conventional x-ray showed insignificant change of the O=C–O bond and the
photoelectron spectroscopy (XPS). The HXPES analysis C–O bond after the plasma exposure and the UV+VUV
was performed with x-rays from a synchrotron at a photon photo-irradiation. Whereas, in the XPS spectra, the samples
energy of 7940 eV at the national synchrotron radiation exposed to the Ar-O 2 mixture plasma and the UV+VUV
facility (SPring-8) of the Japan Synchrotron Radiation photons clearly exhibit significant increase in the oxygen
Institute [6]. The inelastic mean free path (IMFP) of 7940 functionalities (the O=C–O bond and the C–O bond). In
eV electrons in polymers is approximately 18 nm [7]. particular, substantial increase is found for the C=O bond,
Therefore, the probing depth of HXPES is about 50 nm for which is not observed in the spectrum of raw PET film.
analysis of polymers The XPS analysis was performed with The UV+VUV photo-irradiation from the Ar-O 2
non-monochromatized Mg KD radiation (photon energy of mixture plasmas resulted in insignificant change of the bond
1253.6 eV). structures in deeper regions up to about 50 nm from the
surface. However, in regions up to about 10 nm from the
3. Results surface, the UV+VUV photo-irradiation resulted in increase
Figure 2 shows typical AFM images of the PET surface of the oxygen functionalities.
(a) before and (b) after direct exposure to the plasma, (c)
after irradiation with the UV+VUV photons from the 4. Summary
plasma (with MgF 2 window). Surface roughness R q (root- Interactions of UV+ VUV photons from Ar-O 2 mixture
mean-square) of the raw PET film (Fig. 2(a)) was 1.0 nm. plasmas with polymer surfaces were investigated using
After the direct exposure to the Ar+O 2 mixture plasma for AFM, HXPES and conventional XPS analyses. The AFM
1052 seconds, the roughness increased to 5.6 nm (Fig. 2 images indicated that the surface morphological change of
(b)). Whereas, the roughness was almost constant (R q = 0.9 PET films due to Ar-O 2 mixture plasma exposure is not
nm) even after exposure to UV+VUV photons from the caused by only UV+VUV photons from the plasma. The
plasma for 1052 seconds as shown in Fig. 2(c). These HXPES analysis suggested that the effects of UV+VUV
results suggest that the surface morphological change of photons from the Ar-O 2 mixture plasmas on the chemical
PET films due to the Ar-O 2 mixture plasma exposure is not bonding states of polymer are insignificant in deeper
caused by only UV+VUV photons from the plasma. regions up to about 50 nm from the surface. The XPS
analysis shows that the formation of oxygen functionalities
HXPES, TOA = 80deg
after UV+VUV photo-irradiation is localized in the vicinity
XPS
of the surface regions as shallow as 10 nm. These results
O=C-O (288.6eV)
C=O (287.4eV)
C-O (286.1eV)
O=C-O (288.6eV)
C=O (287.4eV)
C-O (286.1eV)
C-C (284.6eV)
C-C (284.6eV)
˭ය˭ (291.2eV)
˭ය˭ (291.2eV)
C1s C1s
indicated that the UV and VUV photo-irradiation caused

photodecomposition of the chemical bonds to create free
Intensity (arb. units)
radicals, which were terminated and/or chemically reacted

with oxygen and/or OH species in the vicinity of the sample
surface; oxygen molecules and radicals during plasma
(c) UV+VUV
(b) plasma
(c) UV+VUV
(b) plasma
exposure and/or oxygen molecules and moisture after
(a) raw (a) raw
taking the PET samples out of the plasma reactor to the
296 292 288 284 280
Binding energy (eV)
292 288 284 280
Binding energy (eV) ambient air.
Fig. 3 HXPES and XPS C1s spectra for PET films; Acknowledgement
(a) before and (b) after direct exposure to the plasma, This work was partly supported by The Global COE
(c) after irradiation with the UV+VUV photons from the Program "Center of Excellence for Advanced Structural
plasma. and Functional Materials Design" through the Ministry of
299
Education, Culture Sports, Science and Technology [3] Y. Setsuhara, T. Shoji, A. Ebe, S, Baba, N. Yamamoto, K.
(MEXT), Japan, and by a Grant-in-Aid for Young Takahashi, K. Ono and S. Miyake, Surf. Coat. Technol. 174 -
Scientists (B) from the Japan Society for the Promotion of 175 (2003) 33.
Science (Research Project Number: 21760587). [4] Y. Setsuhara, K. Takenaka, A. Ebe and K. Nishisaka, Plasma
Process. Polym. 4 (2007) S628.
References [5] S. Uchida, S. Takashima, M. Hori, M. Fukasawa, K.
[1] M.-C. Choi, Y. Kim and C.-S. Ha, Prog. Polym. Sci. 33 Ohshima, K. Nagahata, and T. Tatsumi, J. Appl. Phys. 103,
(2008) 581. 073303 (2008)
[2] K. L. Chopra, P.D. Paulson and V. Dutta, Prog. Photovolt: [6] K. Kobayashi, Nucl. Instrum. Meth. Phys. Res. A 601 (2009)
Res. Appl. 12 (2004) 69. 32.
[7] S. Tanuma, C.J. Powell and D.R. Penn, Surf. Interface. Anal.
21 (1994) 165.
300
†
D. H. Yoon*, D. Wakui*, T. Sekiguchi* and S. Shoji*
KEY WORDS: (Sampling), (Horizontal pneumatic valve), (PDMS), (Droplet)
1. Introduction resistance initially. However, flow resistances of channels

Micro/nano liter sampling technologies are in high between parallel walls are changed by controlled
demand for a wide range of applications in areas such as deformation amounts from one side or both sides. As a
clinical diagnosis and biomedical/chemical researches. To result, it is possible to control the flow resistance of each
control the sample flow in integrated micro fluidic systems, channel and to sort only single droplets to a specific
electrokinetic methods [1], hydrodynamics [2], and chamber (Fig. 2).
mechanical valves are used. Among them, pneumatic
flexible valves of horizontal type and vertical type have
been widely used because of their simple structure and
good controllability [3, 4].However, issues are remain to be
solved for the complicated stacking process of the vertical
type and insufficient multiple control of the horizontal type.
We propose a novel type of the multiple droplet sampling
system realizing minimum numbers of active horizontal
microvalves.
2. Principle
Figure 1 shows a working principle of single droplet
sampling by horizontal valves and flexible parallel walls.
PMDS walls on both sides of the micro channel are
Fig. 2 The principle of multi modes droplet sampling.
deformed by controlled air pressure. The deformation,
especially, overshot deformation of valves makes a
sequential deflection of the flexible walls inside the channel.
Each fluidic channel is designed to have the same flow
resistance initially. However, flow resistances of channels

between parallel walls are changed by controlled
deformation amount from one side or both sides. As the
result, it is possible to control the flow resistance of each
channel and to sort only single droplet to a specific
chamber (Fig. 2).
Fig. 3 Design of total system and detailed size of multi
(a) Construction of multi mode sorting part modes sorting part.
3. Design and Fabrication

The whole system consists of a droplet generation part,
pneumatic valve lines, a deformable part, sampling
chambers, and a drain channel. Figure 3 shows the
designed total system and detailed sizes of deformable parts.
:LGWK RI IOXLGLF FKDQQHO LV DERXW ȝP WKLFNQHVV RI WKH
SDUDOOHO ZDOOV LV DERXW ȝP DQG WKH KHLJKW RI DOO
VWUXFWXUHV LV DERXW ȝP Positions of the moving walls
(b) Images of deformed walls by pneumatic pressure and pneumatic valves were optimized by calculations to
Fig. 1 The concept of droplet sorting by pneumatic obtain maximum deflection of the parallel walls. Also, the
valves and moving flexible walls. drain channel width was GHVLJQHG DV ȝP WR GUDLQ the
* Major in Nanoscience and Nanoengineering, Waseda Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
University, JAPAN Japan
301
main stream out of the device under initial condition. remaining issues. It is expected that integration of an
Designed structures were formed from PDMS using a SU-8 automatic pressure control system will be a solution of
mold. It is bonded to the PDMS coated glass substrate after these problems. Some specific structures which can realize
plasma pretreatment. The fabrication results by single step independent control of droplet generation from sampling
SU-8 patterning and PDMS replication are shown in Fig. 4. are considered.
In order to realize flexible PDMS structures, resin and
curing agent were mixed in a 15:1 ratio. For fluidic
experiments, syringe (1750CX, HAMILTON) and syringe
pump (KDS210, kdScientific) were used. The air pressure
was controlled by pressure regulator (2657 pneumatic
pressure standard, YOKOGAWA).
Also, a CCD camera (JK-TU53H, TOSHIBA) and a data
processing computer were utilized for visualization and
storage of the droplet sampling processes.
(a) 0 sec (b) 1 sec
(c) 1.5 sec (d) 2 sec

Fig. 5 Captured images of single droplet sampling with
time sequence (Mode 1).
Fig. 4 Fabrication results of the sampling device.
4. Experimental Results and Discussion

In the droplet generation part, 4ȝPGLDPHWHUDTXHRXV
droplets were generated. As shown in Fig. 5, generated
droplets initially flow into the drain channel, because the
flow resistance of the drain channel was designed as three
times higher than that of the parallel sampling channel (a).
According to deformation by pneumatic pressure, the flow
resistance of the drain channel increases and a target
droplet flows into the sampling channel (b).Simultaneously,
selection of sampling chamber is performed with the
multiple channel selection principle described in Fig.2. As a
result, the target droplet is delivered to one objective micro
chamber (c). By pressure release, droplet sampling finished,
and the main stream is restored to the drain channel (d).
Fig. 6 Captured images of droplets placed at entrance to
The other delivery behaviors under different pressure
their objective chamber and pressure conditions.
conditions are shown in Fig. 6. It is demonstrated that five
different modes droplet are sorted by combination of
5. Conclusions
applied pneumatic pressures from 0 kPa to 250 kPa.
Proposed multiple sampling was successfully
Furthermore, the pneumatic line for drain and sampling
demonstrated. The valves and flexible moving walls were
channel is connected to each other for simple control. As a
operated precisely and one droplet sampling from
result, the walls of the drain channel are deformed in
continuous droplet phase flow was also realized. The total
proportion to the pressure at different sampling modes. The
flow sampling system was fabricated by single step PDMS
adequate combination of PDMS pneumatic deformations
molding and bonding. We improve the structure of the total
enables multi droplet sorting. The multi mode sorting and
flow system to realize stable particles and bio molecules
manually controlled single droplet sampling was performed
sampling.
within about 1 second. This device can be used effectively
for sampling of biological cells and biomolecules. Slow References
switching speed compared to the electric methods and [1] A.Y. Fu, H.P. Chou, C. Spence, F. H. Arnold and S. R.
instability of droplet generation during sampling are the Quake: Anal. Chem., 74 (2002), pp.2451.
302
[2] T. Arakawa, Y. Shirasaki, T. Izumi, T. Aoki, H. Sugino, T.

Funatsu and S. Shoji: Meas. Sci. Technol., 17 (2006), pp.3141.
[3] K. Kawai, Y. Shibata, M. Kanai and S. Shoji: ȝ7$6
(2008), pp.683.
[4] K. Iwai and S. Takeuchi: MEMS2009, 1 (2009), pp.371.
303
Development of a novel integrated iontophoresis electrode

†
consisting of metallic and drug-loaded layers
T. Yoshioka*, N. Saito*, T. Ikoma*, N. Ohashi**, H. Haida***, S. Ando***, R. Wakita***,

H. Fukayama***, M. Umino****, and J. Tanaka*
KEY WORDS: (Metal) (Gel) (Integration) (Iontophoresis) (Local anesthesia)
1. Introduction of the IR beam was set to be 60° from the surface normal.
Iontophoresis is a drug delivery method that can be used
to enhance the movement of ionic compounds or non- 3. Results and Discussion
charged drug molecules by the application of external Figure 1 shows the FT-IR spectra of the Al electrodes
electric fields. Iontophoresis can transport ionic substance subjected to the electrochemical deposition process of
across skin or membranes into the body. Although alginic acid under the current density of 1 mA/cm2 for 120 s,
iontophoresis needs a drug-loaded electrode, a metal 300 s, and 600 s. The characteristic peaks at 1420 cm-1 and
electrode is unable to adsorb a large amount of drugs. Thus, 1600 cm-1 were assigned to dissociated carboxyl groups (–
the electrode that conjugates drug-absorbable gels is COO-) of alginate, which corresponded to the symmetric
desired for sustainable administration. Alginic acid and and asymmetric C=O stretching vibration. The result
chitosan have been widely studied as drug delivery carriers. indicated that the electrochemical process successfully
Sodium alginate or chitosan form gels around electrodes by deposited the alginate on the electrodes. The deposited
the pH change of the solution that was generated by mass on the electrodes was increased with an increase of
electrolysis of water. In this study, we investigated the the applied times. The band at 1740 cm-1 was assigned to
interface stability of the gels formed on a metal electrode by C=O stretching vibration of the undissociated carboxyl
applying direct currents in the solutions in order to develop groups (–COOH). It was already described that alginic acid
a novel iontophoresis electrode. gels were formed around anode electrodes due to
electrochemical decomposition of water [1]. According to
2. Materials and Methods the literature, the related reactions at the anode were
Al electrodes were cut into 2.5 x 1 x 0.01 cm pieces. expressed as follows;
The electrodes were ultrasonically washed three times with
acetone for 10 min, and then dried under nitrogen gas flow. H 2 2ĺ++ + 1/2O 2 + 2e- (1)
The cleaning procedure was completed by 10 min
UV/ozone irradiation (ProCleaner 110, BioForce Application of an electric field caused a pH decrease at the
Nanosciences, Inc., USA). The electrochemical deposition anode. In the aqueous solution, sodium alginate was
cell was a two-electrode system, which consisted of a dissociated to sodium ions and alginate molecules, and then
cylindrical polystyrene cell and ᴾ metal electrodes. The the alginate molecules were protonated around the anode.
deposition was obtained on Al electrodes that were set as
anodes for alginic acid and as cathodes for chitosan. The Pt Na-$OJĺ$OJ- + Na+ (2)
electrode was used as a counter electrode. The distance Alg- + H+ ĺ+-Alg (3)
between two electrodes was 10 mm. Twenty mL of 0.5%
sodium alginate aqueous solution or 0.2% chitosan solution where the symbols Na-Alg and H-Alg denote sodium
was poured into the cylindrical polystyrene cell. The alginate and alginic acid, which are strong and weak
surface area of the electrodes exposed to the solution was electrolytes, respectively. The formed H-Alg turned to gels
adjusted to be 4 cm2. The electrochemical deposition was via hydrogen bonding between –COOH of H-Alg, which
conducted under application of a DC electric field with was confirmed in the FT-IR spectra shown in Fig. 1. Thus,
current densities of 1.0-5.0 mA/cm2 for up to 3600 s at the alginic acid layers were deposited through the proton-
room temperature. The electrodes were dried at 37°C for 24 mediated gelation. The intensity of the peaks for –COOH at
h. The surface of the electrodes was characterized by FT-IR. 1740 cm-1 was increased with an increase of the applied
All measurements were performed using FT-IR times. This result indicated that the prolonged application
spectrometer, model FT/IR-4100 (JASCO, Japan) equipped leads to an increase of the hydrogen bonding in the layers in
with PR-5101 system (JASCO, Japan). The incident angle addition to an increase of the deposited amount.
* Tokyo Institute of Technology, Tokyo, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** National Institute for Materials Science, Tsukuba, Japan Japan
*** Tokyo Medical and Dental University, Tokyo, Japan
**** TTI ellebeau, Inc., Tokyo, Japan
304
Development of a novel integrated iontophoresis electrode consisting of metallic and drug-loaded layers
Figure 2 shows the FT-IR spectra of the Al electrodes

subjected to the electrochemical deposition process of
chitosan under the current density of 5 mA/cm2 for 600 s,
1200 s, and 3600 s. The characteristic peaks at 1645 cm-1
and 1570 cm-1 were assigned to amide I and amide II of
chitosan, respectively. Chitosan was also shown to deposit
on the Al electrodes. The deposited mass of chitosan on Al
was lower than that of alginic acid irrespective of longer
applied time. It is suggested that the cathodic reactions
were expressed as followed;
2H 2 O + 2e- ĺ H 2 + 2OH- (4)

Ch-NH 3 + + OH- ĺ Ch-NH 2 + H 2 O (5)
where the symbols Ch-NH 3 + and Ch-NH 2 denote

protonated and deprotonated chitosan, respectively. At the
cathode, electrochemical decomposition of water resulted in
an increase of pH as expressed in eq. (4).ᴾ Then, the
chitosan molecules lost their charge and formed insoluble
deposits on the Al surface.
The results indicated that alginic acid and chitosan gels
successfully deposited on the Al electrodes. However, their
chemical stability was different. The alginic acid gels on Al
Fig. 1 FT-IR spectra of the Al electrodes subjected to the electro-
chemical deposition process of alginic acid.
did not exfoliate in ionic solution, while the chitosan gels
easily exfoliated. It has been reported that there are a
number of –OH groups on the metal surface, and the groups
existed mainly as –OH 2 + at lower pH than an isoelectric
point and as –O- at higher pH [2]. Since the electrochemical
deposition of alginic acid occurred at acidic pH, the ionic
interaction between –OH 2 + on the surface and –COO- of the
alginic acid could be exist. On the other hand, the chitosan
gels deposited at a basic pH did not involve in ionic
interaction between chitosan molecule and the Al surface.
4. Conclusion
Drug-absorbable gels of alginic acid or chitosan were
successfully deposited on the Al electrodes.
References
[1] F. Yokoyama et al.: Eur. Polym. J., 34 (1998), pp.229-234.
[2] G. A. Parks: Chem. Rev., 65 (1965), pp. 177-198.
Fig. 2 FT-IR spectra of the Al electrodes subjected to the electro-

chemical deposition process of chitosan.
305
†
NAGAI Akiko*, YAMASHITA Kimihiro*, MURAYAMA Sayaka**,

MATSUSHITA Nobuhiro**, OKADA Kiyoshi**, ABE Nobuyuki***,
TSUKAMOTO Masahiro ***, SON Kunsu ****, WANG Xinmin ****, XIE Guoqiang ****
and INOUE Akihisa *****
KEY WORDS: (Metallic glass) (Femtosecond laser) (Hydrothermal-electrochemical treatment) (Osteoblast) (Cell
attachment assay) (Yinculin expression)
1. Introduction kHz, respectively. The laser beam was focused onto the Ti-
Metallic glass has many attractive properties as a based BMG (Ti 40 Zr 10 Cu 36 Pd 14 ) surface by a lens with a
biomaterial, such as high strength, high elastic limit, low 100 mm focal length. The Gaussian laser beam had a
Young’s modulus and high corrosion resistance. Surface GLDPHWHURIȝPDWWKH/e2 intensity points) on the Ti-
modifications of the metallic materials have been tried due based BMG surface. Ti-based BMG’s surface was
to insufficiency of biocompatibility. One of the techniques irradiated with the femtosecond laser at the average laser
is a combination of femtosecond laser and hydrothermal- fluence of 0.15 and 1.0 J/cm2, respectively. The laser beam
electrochemical treatment (Ref. 1,2). The modified surfaces was scanned on the Ti-based BMG’s surface in the area of
are expected to obtain bioactive property since apatite 5 x 5 mm2 using the XY stage. Then, laser scanning speed
forming ability in the simulated body fluid has been was 1 mm/sec and hatching distance was 20 μm.
demonstrated. To evaluate biocompatibility in vitro, the
objective study was to examine cellular behavior c) Hydrothermal-electrochemical (H-E) treatment
responding to the surface modified metallic glass. The After femtosecond laser irradiated, Ti-based BMG was
attachment, spread, and adhesion of osteoblasts on the subjected to H-E treatment at 90 °C for 120 hours in 5
materials are investigated. mol/L NaOH solutions to attain the surface bioactivity. The
cylindrical Ti-based BMG (Ti 40 Zr 10 Cu 36 Pd 14 ) specimen, 5
2. Materials and Methods mm in diameter was used as the working electrode facing
1. Fabrication of surface modified Ti-based bulk metallic the circular surface to the counter electrode of platinum
glass sheet, 10×50×0.5 mm3. The constant dc voltage of 1.4V
a) Ti-based (Ti 40 Zr 10 Cu 36 Pd 14 ) bulk metallic glass (BMG) was applied between these electrodes keeping their
samples distance at 4 cm during H-E treatment.
The Ti 40 Zr 10 Cu 36 Pd 14 alloy ingots (compositions are
given in nominal atomic percentages) were prepared by arc 2. Cell culture and evaluations of biological responses
melting mixtures of pure Ti, Zr, Cu, and Pd metals (>99.9 a) Cell culture
mass%) in a high purity argon atmosphere purified using Zr Osteoblast-like MG63 cells were seeded directly onto
getter. Bulk cylindrical rods with a diameter of 5 mm were the Ti-based BMG’s surface irradiated with the
prepared by melting of the master ingots followed by tilt femtosecond laser at the average laser fluence of 0.15 and
casting into copper molds. 1.0 J/cm2 and subjected H-E treatment (designated 0.15
The disc samples with 5 mm in diameter and 2 mm in and 1.0 J/cm2 surface, respectively).
height were cut out from the rods, then polished. The
glassy structure of as-prepared samples was examined by b) Cell attachment assay and morphology analysis
X-ray diffractometry in reflection with monochromatic Cu The attachment of cells were fixed and stained with
KĮ radiation. The thermal stability was examined by fluorescent dye, rhodamine phalloidin and DAPI, and
differential scanning calorimetry (DSC) under an argon analyzed using a microscopic image-based observation.
atmosphere at a heating rate of 0.67 K/s.
c) Vinculin expression analysis
b) Femtosecond (Ti:sapphire) laser The expression and localization of focal adhesion
A femtosecond (Ti:sapphire) laser was employed in this protein, vinculin, were analyzed using a microscopic
experiment. The wavelength, pulse duration and repetition image-based observation and densitometry.
rate of the femtosecond laser were 775 nm, 150 fs and 1
* IBB, Tokyo Medical and Dental University, Tokyo, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** MSL, Tokyo Institute of Technology, Tokyo, Japan Japan
*** JWRI, Osaka University, Osaka, Japan
**** IMR, Tohoku University, Miyagi, Japan
***** Tohoku University, Miyagi, Japan
306

The number of osteoblasts attached to the two surfaces
after 3h of incubation was not significantly different (Fig.
1).
Fig. 3 Representative microscopic images of cells stained

with anti-vinculin (green) and DAPI (blue) on (A) 0.15 and
(B) 1.0 J/cm2 surface.
Fig. 1 Representative microscopic images of cells stained 4. Conclusions

with DAPI for nuclei (blue) on (A) 0.15 and (B) 1.0 J/cm2 This study addressed the initial cell-material interaction
surface. occurring on a surface-modified BMG. The conclusions of
this study are summarized as follows.
Microscopic images of cells stained with rhodamine (1) The number of osteoblasts attached to both surfaces is
phalloidin showed that the cells were larger on the 1.0 nearly equal. The spread and adhesion of osteoblasts
J/cm2 surface than on the 0.15 J/cm2 surface where a was enhanced on 1.0 J/cm2 surface compared to 0.15
majority of cells were rounded (Fig. 2). J/cm2 surface, which was supported by the increased
The expression of vinculin was observed in cells both expression of focal adhesion protein, vinculin.
on 0.15 and 1.0 J/cm2 surfaces. However, the localization (2) The interactions between cells and the surface-modified
of vinculin at the tip of stretching cytoplasmic projections BMG at an early stage may indicate the potential as
was seen appearently on 1.0 J/cm2 surface compared to future biomaterials.
0.15 J/cm2 surface (Fig. 3).
Acknowledgement
The work was financially supported by Research and
Development Project on Advanced Materials Development
and Integration of Novel Structured Metallic and Inorganic
Materials from the Ministry of Education, Sports, Culture,
Science and Technology, Japan.
References
Fig. 2 Representative microscopic images of cells stained [1] M. Fukuhara, X. Wang and A. Inoue: Appl. Phys. lett., 91
with rhodamine phalloidin for actin filaments (red) and (2007), p.171908.
DAPI (blue on (A) 0.15 and (B) 1.0 J/cm2 surface. [2] M. Yoshimura, T. Onoki, M. Fukuhara, X. Wang, K. Nakata
and T. Kuroda: Mater. Sci. Engineer. B, 148 (2008), pp.2-6.
307
Joining of ceramic nanocrystals and bio-molecules towards bio-

†
medical applications
OHARA Satoshi *, SATO Kazuyoshi **, TAN Zhenquan *, UMETSU Mitsuo ***
KEY WORDS: (Zirconia) (Nanocrystals) (DNA) (Arrangement) (Coulomb interactions)
1. Introduction 50 Pmol/L) with a HCl solution was prepared to maintain a

Oxide nanoparticles, as the basic building blocks for constant pH value of 3.0. Then 900 PL ZrO 2 solution
nanostructure, make the further miniaturization of structures (concentration 50 Pmol/L) was added to the 900 PL
and devices possible [1]. How to assemble nanoparticles on solution of 0.5 Pmol/L bp O-DNA to make a 1800 PL
nanoscale has generated considerable interest in recent compound solution of 0.25 Pmol/L bp O-DNA.
years [2-10]. Deoxyribonucleic acid (DNA) plays an
important role in assembling nanoparticles on the nanoscale 3. Results and Discussion
because of its stable physicochemical property, linear and Figure 1(a) and (b) shows a photograph and particle
semi-rigid molecular structure [11]. The role of DNA in size distribution of the obtained transparent ZrO 2 colloidal
assembling metal nanoparticles has been reported [12-19], solution. The ZrO 2 nanoparticle surface contains numerous
but the role of DNA in assembling oxide nanoparticles has positive charges at a pH value of 3 because the isoelectric
not been reported as yet. The aim of this paper is to study point of ZrO 2 ceramic is around 5-6, and due to the electric
how Zirconia (ZrO 2 ) nanoparticles assemble with the aid of repulsion force in water, each ZrO 2 nanoparticle is assumed
DNA. The ZrO 2 nanocrystals are important for Bio-medical to be dispersed separately. The average diameter of the
applications such as bioactive coatings on bone implants. ZrO 2 nanoparticle is about 5 nm, and has a very narrow
particle distribution (Fig. 1(b)). Fig. 1(c) shows a TEM
2. Experimental picture of the ZrO 2 nanoparticles. Although the primary
The ZrO 2 ceramic nanoparticles, which were ZrO 2 nanoparticles on the TEM grid aggregate after drying
synthesized by a hydrothermal reaction, were in a colloidal the colloidal solution, the primary nanoparticles are about 3
solution. Aqueous solution of ZrOCl 2 ·8H 2 O was nm, which is consistent with that measured by DLS. Hence,
neutralized by K 2 CO 3 solution. Then the solution was it is concluded that the ZrO 2 nanoparticles can be dispersed
hydrothermally treated at 150 ºC for 1 hour in the Teflon perfectly in water under this low pH condition.
lined stainless steel vessel. The detailed hydrothermal Figure 2 shows the TEM picture of the mixed solution
synthesis is described in a previously reported paper [20]. of ZrO 2 nanoparticles and O-DNA, and indicates that a
After the reaction, undesirable K+ and Cl- were removed by network is formed as the ZrO 2 nanoparticles are assembled
an ultrafiltration and 5 M of HCl was added to the product on the DNA strands. In contrast, without DNA, the ZrO 2
for dispersion of the nanoparticles in water. The particle nanoparticles are aggregated randomly on the TEM grid
size distribution of the obtained ZrO 2 nanoparticle colloidal (Fig. 1(c)). However, the ZrO 2 nanoparticles are arranged
solution was measured by the dynamic light scattering in the presence of O-DNA. This arrangement is likely due to
(DLS) method, whereas transmission electron microscopy the Coulomb interactions between the negatively charged
(TEM) was used to observe the ZrO 2 nanoparticles and DNA and positively charged ZrO 2 nanoparticles.
their assembled nanostructures.
The ZrO 2 nanoparticles were assembled by O-DNA as 4. Conclusion
follows. O-DNA, which was 48502 base-pairs (bp) long, The study suggests the DNA plays an important role in
was purchased from TaKaRa Biotechnology (Dalian) Co., the assembling of ZrO 2 nanoparticles, it provides a
Ltd. The original concentration was 0.3 Pg/PL, and the template for the arraying of nanoparticles. We believe that
equivalent base pair concentration was 450 Pmol/L. The this assembly of metal oxide nanoparticles by DNA will
buffer was 10 mmol Tris-HCl-1mmol EDTA, pH=8.0, yield novel hybrid nano-biomaterials with synergetic
A260/A280=1.8-2.0. The O-DNA solution (450 Pmol/L bp properties and functions.
concentration) was diluted to a 1 Pmol/L bp concentration
by adding a 0.0025 mol/L HCl solution to maintain the pH
of O-DNA near 3.0. A 900 PL ZrO 2 solution (concentration

** Graduate School, Gunma University, Kiryu, Japan Japan
*** Graduate School, Tohoku University, Sendai, Japan
308
Joining of ceramic nanocrystals and bio-molecules towards bio-medical applications
(a)
(b) 10 nm
Fig. 2 TEM image of a zirconia nanoparticle assembly by
O-DNA.
[3]H. Nakao, H. Shiigi, Y. Yamamoto, S. Tokonami, T. Nagaoka ,

S. Sugiyama and T. Ohtani: Nano lett., 3 (2003), pp.1391-
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309
†
Cu-based metallic glass surfacemodified with Cu for soldering
Productions and applications of Cu clad metallic glass
TERAJIMA Takeshi *, KIMURA Hisamichi ** and INOUE Akihisa ***
KEY WORDS: (Cu-based metallic glass) (Clad material) (Soldering) (Wettability) (Quench) (passive oxide
film) (Surface modification)
1. Introduction soldering enables us to join metallic glass with dissimilar

It is necessary to develop joining techniques for materials such as crystalline alloys, and surface-metalized
metallic glasses because they are required to build in to ceramics.
manufactured products. One of the serious problems with However, a serious problem in soldering metallic glass is
welding metallic glass is crystallization in the molten zone. poor wettability. Although Pd-based metallic glass exhibits
If the cooling rate from the liquidus temperature to the glass a good wettability to Pb free solder, Zr-Cu based metallic
transition temperature is slower than the critical value, glasses doesn't wet at all because of a strong and
metallic glass rapidly transforms into intermetallic homogeneous passive oxide film, which mainly consists of
compounds. Formation of the intermetallic compounds is ZrO x , and protects the surface. Some attempts have already
not preferred because most of them are brittle and of low been reported to remove the passive oxide film. A. Imai et
weld strength compared. Recently, there have been some al. removed the surface oxide film of the Cu 60 Zr 30 Ti 10
attempts to join pieces of Zr-based metallic glass using metallic glass by Ar ion beam, and then deposited Ag thin
electron beam welding, explosive welding, pulse current layer on it in an ultra high vacuum environment [9]. The
welding, friction welding [1-3], laser welding [4-7] and Ag-deposited Cu 60 Zr 30 Ti 10 surface showed a resistivity to
ultrasonic bonding [8].However, weldability is strictly the reoxidation in air, and also good wettability to Sn-Ag-
limited by the specimen size, the glass forming ability and Cu solder. S. Tamura et al. studied wetting behavior of Zr-
the heat source. based metallic glass in a Sn-Cu-Ni solder bath by ultrasonic
Soldering is one of candidate techniques for joining cavitation in air [10]. They found that the surface
metallic glass. Soldering can be processed approximately morphology of the metallic glass was roughed when
below 600K, which is far below the transition temperatures cavitation bubbles collapsed on the surface, and this
of metallic glasses. The low processing temperature doesn't phenomenon promoted the wetting between the metallic
induce a structural relaxation of atomic order and thus glass and the solder. The application of ultrasonic
enables joining without any crystallization. Furthermore, cavitation is useful for the immediate removal of passive
Fig. 1 Production of Cu thin film cladding bulk Fig. 2 Cross-section image of Cu-cladding bulk
metallic glass (BMG). metallic glass Cu36Zr48Al8Ag8.
** IMR, Tohoku University, Sendai, Japan Japan
*** Tohoku University, Sendai, Japan
310
Cu-based metallic glass surfacemodified with Cu for soldering Productions and applications of Cu clad metallic glass
oxide film on the metallic glass. However, the removable phase identification was conducted by micro-focused X-ray
area was limited around the ultrasonic-transducer. diffraction (XRD) analysis using Co KD radiation. The
In this paper, we report a development of Cu thin film microstructure of the interface between Cu thin film and
clad Cu-based metallic glass Cu 36 Zr 48 Al 8 Ag 8 for the aim of metallic glass was observed with an optical microscope
improving solder wetting. By cladding Cu thin film over the (OM), a scanning electron microscope (SEM), and a
transmission electron microscope (TEM). The Surface
oxide layer was analyzed by auger electron spectroscopy
(AES). Solder wettability was evaluated by dipping Sn-
3Ag-0.5Cu solder on the Cu thin film clad metallic glass at
553K for 60 s.

Cu thin film with thickness of 2 Pm was successfully
welded to amorphous Cu 36 Zr 48 Al 8 Ag 8 . The cross-section
image is shown in Fig. 2. From microstructure analysis, it
was found that reaction layer such as Cu 5 Zr and Cu 10 Zr 7
was formed at the interface between Cu and
Cu 36 Zr 48 Al 8 Ag 8 . AES results show that the formation of a
surface oxide layer was suppressed by the cladding Cu thin
film.
Wettability of Sn-3Ag-0.5Cu solder on (a) monolithic
metallic glass and (b) Cu cladding metallic glass are shown
Fig. 3 Wettability of Sn-3Ag-0.5Cu solder on (a) in Fig. 3. Solder was not wet on monolithic metallic glass at
monolithic metallic glass and (b) Cu cladding all, however, was wet on Cu thin film clad metallic glass.
metallic glass. The improvement of the solder wetting originated from
interception of the oxide film formation.
Cu-based metallic glass surface, the formation of passive
surface oxide film was intercepted. Microstructure at the 4. Conclusions
Cu/Cu 36 Zr 48 Al 8 Ag 8 interface and the solder wettability Amorphous Cu 36 Zr 48 Al 8 Ag 8 was successfully clad by
were discussed. Cu thin film. Solder wetting was drastically improved by
cladding Cu thin film because formation of a native oxide
2. Experimental film was intercepted by the Cu layer.
A pre-alloy of Cu 36 Zr 48 Al 8 Ag 8 (in atom%) was
prepared by arc-melting a mixture of pure Cu (99.99%), Zr References
[1] Y. Kawamura, T. Shoji, and Y. Ohno, J. Non-cryst. Solids,
(99.99%), Al (99.99%) and Ag (99.999%) metals in an
317 (2003), pp.152-157.
oxygen-gettered argon atmosphere. Figure 1 shows [2] Y. Kawamura and Y. Ohno, Scr. Mater., 45 (2001), pp.279-
schematic illustration of the procedure to produce Cu thin 285.
film clad Cu-based metallic glass. A rectangular hollow [3] Y. Kawamura and Y. Ohno, Scr. Mater., 45 (2001), pp.127-
with dimension of H25xW25xD2mm was machined on the 132.
side of a Cu mold. The rectangular hollow was covered [4] J. Kim, D. Lee, S. Shin, and C. Lee, Mater. Sci. and Eng. A,
with a tungsten thin plate with thickness of 100 Pm, on A434 (2006), pp.194-201.
which Cu thin film with thickness of 2 Pm was adhered. [5] B. Li, Z. Y. Li, J. G. Xiong, L. Xing, D. Wang, and Y. Li, J.
Alloys Comp., 413 (2006), pp.118-121.
The pre-alloy (Cu 36 Zr 48 Al 8 Ag 8 ) was melted in a quartz [6] Y. Kawahito, Y. Niwa, T. Terajima and S. Katayama, Mater.
glass nozzle at 1473 K by induction heating, and then the Trans., 51 (2010), pp.1433-1436.
melt was cast into the gap of the hollow. Just after casting, [7] Y. Kawahito, T. Terajima, H. Kimura, T. Kuroda, K. Nakata,
the Cu thin film was semi-molten by a residual heat of the S. Katayama and A. Inoue, Mater. Sci. and Eng. B, B148
melt and was welded to it. Then the melt and Cu thin film (2008), pp.105-109.
were quenched together by the Cu mold. As a result of the [8] M. Maeda, Y. Takahashi, M. Fukuhara, X. Wang, A. Inoue,
process, Cu thin film was clad on a surface of Mater. Sci. and Eng. B, B148 (2008), pp.141-144.
Cu 36 Zr 48 Al 8 Ag 8 metallic glass.. [9] A. Imai, M. Katayama, S. Maruyama, H. Nishikawa, T.
The thermal stability associated with the glass transition wada, H. kimura, M. Fukuhara, T. Takemoto, A. inoue and
Y. Matsumoto,J. Mater. Res., 24 (2009), pp.2931-2934.
and crystallization was analyzed using a differential
[10] S. Tamura, Y. Tsunekawa, M. Okumiya and M. Hatakeyama,
scanning calorimeter (DSC) at a heating rate of 20K/s. The J. Mater Proc. Technol. 206 (2008), pp.322-327.
311
Shock-assisted joining between metallic glass and ceramics†
ATOU Toshiyuki *, MUKOGAWA Shintaro **, KIMURA Hisamichi ***, ITO Shun ***
and KIKUCHI Masae ****
KEY WORDS: (Metallic glass) (Ceramics) (Joining) (Shock wave) (High pressure) (High temperature)
(Short duration)
1. Introduction 3. Results and Discussion

Metallic glasses have many specific features in In the sample recovered from 24 GPa, consolidated
mechanical and corrosion resistance. If metallic glasses crystalline SiO 2 (quartz) 50-200 ȣm in thick was adherent
could be joined with ceramics, the application field could to the surface of metallic glass, as shown in SEM image
be widely spread by combining the merits of each material, (Fig. 2). Almost all the area of the surface was covered by
i.e. biomaterials, electronics, and so on. However, quartz. Textures in which melted metal seems to flow into
formation of well joined interface between a metallic glass the SiO 2 layer were observed, revealing complicated
and a ceramic is difficult due to the different nature of microstructure in the interface. Figure 3 shows EPMA
chemical bonding in these two materials, as well as the mapping of the interface. Metallic elements infiltrated into
metastable state of metallic glasses. the SiO 2 layer with 20-30 ȣm in depth, but no apparent
Intense shock waves can generate very high pressure deviation from the chemical composition of the metallic
and temperature in a short period of time about 1 ᷈s in glass was observed. Furthermore, microtexture observed by
condensed matters. Because of the impulsive nature of TEM showed metallic glass joined amorphous SiO 2 with
shock conditions, joining between ceramics and metastable only partial crystallization of metallic glass (Fig. 4).
metallic glass might be realized without crystallization of
metallic glass. Under such extreme conditions, unusual
redox reactions have been reported between metals (Zr, Nb)
and ceramic ((SiO 2 ) under shock compression [1,2]. We
have expected that joining between metallic glass and
ceramics can be achieved by shock-loading with chemical
reactions to enhance the firm joining. As a model case, we
tried shock-assisted joining between Zr 55 Al 10 Ni 5 Cu 30
metallic glass and quartz (SiO 2 ) using gun method, and the
interface between metallic glass and silica was examined by
SEM, TEM, and EPMA measurements.
2. Experimental
Shock-loading experiments were performed using a
two-stage light gas gun at Tokyo Institute of Technology up
to 2.1 km/s (Fig. 1(a)). 3-mm-thick and 21-mm –diameter
Cu flyer plates were used. Flyer velocity was measured
using a magneto-flyer method, and the pressures in the
recovery capsule were determined by an impedance match
method [3]. Fig. 1(b) shows a shock recovery system used
for recovery experiment. Zr 55 Al 10 Ni 5 Cu 30 metallic glass
was formed into disk 14-mm in diameter and 1-mm in
thickness and then encased in an iron recovery capsule with
quartz (SiO 2 ) powder in 1-mm thick. Porosity of quartz
powder was estimated to be about 50 %. The recovery
capsule was placed within a steel recovery fixture [4].
Recovered specimens were examined using SEM, TEM, Fig. 1 (a) Two-stage light gas gun installed at Tokyo
and EPMA measurements to investigate the microstructures Tech (b) Shock recovery system used for shock
in the interface between metallic glass and SiO 2 . assisted joining experiments (see text).
* MSL, Tokyo Tech., Yokohama, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** IGSSE, Tokyo Tech.,, Yokohama, Japan Japan
*** IMR, Tohoku Univ., Sendai, Japan
**** Kansei Center, Tohoku Fukushi Univ., Sendai, Japan
312
Shock-assisted joining between metallic glass and ceramics
6L2 =UEDVHGEXONPHHWDOOLF
JODVV
wP
Fig. 2 SEM photograph of interface of metallic glass Fig. 4 TEM photograph of interface of metallic glass and
and SiO2 shock-loaded to 24 GPa. amorphous SiO2 shock-loaded to 28 GPa.
=U &X glass surface covered with transparent SiO 2 amorphous of

30-200 ȣ m thick. This surface of the metallic glass
exhibited black color, suggestive of a chemical reaction at
the interface. Under higher shock pressure, different
adhesion mechanisms with accompanying chemical changes
might be occurring. Detailed analysis of the interface is
next step of this study.
4. Conclusions
(1) Joining between metallic glass and ceramic was tried
using impulsive shock-loading to Zr 55 Al 10 Ni 5 Cu 30
1L 6L metallic glass and quartz (SiO 2 ) system.
(2) We have confirmed that metallic glass could be covered
with thin layer of SiO 2 .
(3) Microtexture observation suggested that adhesion
mechanism might be different against applied shock
pressure.
References
[1] M. Kikuchi, Y. Syono, K. Fukuoka, K. Hiraga: J. Mat. Sci.
Lett., 6 (1987), pp.97-99.
wP
[2] R. Murao, M. Kikuchi, K. Fukuoka, E. Aoyagi, T. Atou, Y.
Syono: J. Mat. Res., 14 (1999), pp.3169-3174.
Fig. 3 Mapping by EPMA of interface of glass and SiO2 [3] T. Goto, Y. Syono: Materials science of the Earth’s Interior
shock-loaded to 24 GPa. (Ed: I. Sunagawa), Terra, Tokyo (1984), pp.605.
[4] T. Hongo, T. Atou, S. Ito, K. Yubuta, M. Kikuchi, K. G.
These results suggest that the joining of this interface might Nakamura, S. Itoh, K. Kusaba, K. Fukuoka, and K. Kondo:
be due to physical (mechanical) adhesion, as distinct from Phys. Rev, B76 (2007), pp.104114.
the chemical reaction between metallic glass and quartz, as
observed in the previous shock experiments [1, 2]. On the
other hand, recovered sample from 48 GPa showed metallic
313
Development of plasma MIG brazing process of advanced

materials†
TASHIRO Shinichi *, KATAYAMA Tsubasa * and TANAKA Manabu *
KEY WORDS: (Plasma MIG) (Brazing) (Advanced materials)
1. Proposal of plasma MIG brazing process

Figure 1 and 2 show schematic illustrations of
experimental setup for the plasma MIG welding process [1]
and conventional MIG welding process, respectively. In
plasma MIG welding processes, because shielding gas is
ionized in advance by a plasma electrode before supply, the
shape of arc is easily controlled and stabilized through
electromagnetic force as shown in Fig. 3. Therefore the
controllability and stability of the arc are remarkably
enhanced compared with those in a conventional MIG
welding process as shown in Fig. 4. Because of this
advantage, it can be employed for MIG welding in pure
inert gas atmosphere. In this study, we will develop a
brazing process of advanced materials employing the
plasma MIG. It is expected that because of low energy
density of the plasma produced by the plasma electrode, the
base metal is heated uniformly over the wide range and Fig. 2 Schematic illustration of experimental setup for
melting of that is prevented and, consequently, high conventional MIG process.
wettability of filler metal is achieved. Furthermore, the
cleaning action of cathode spots for oxide layer on the base
metal contributes to produce high quality weld joints.
Fig. 3 Schematic illustration of metal transfer in case of

plasma MIG process.
Fig. 1 Schematic illustration of experimental setup for

plasma MIG process.

Japan
314
Development of plasma MIG brazing process of advanced materials
References
[1] T. Kozuru et al: Preprints of the national meeting of J.W.S.,
83 (2008) pp.330-331.
Fig. 4 Schematic illustration of metal transfer in case of

conventional MIG process.
315
Developments of hybrid in-situ observation system to study the

†
microstructural change of metallic alloys
TERASAKI Hidenori * and KOMIZO Yu-ichi *
KEY WORDS: (Steel) (Phase transformation) (Time-Resolved X-ray Diffraction) (Martensite) (LSCM)
1. Introduction on the 46XU beamline at SPring-8 in Hyogo, Japan. The

Rapid heating and cooling is one of the characteristics infrared furnace was set on the theta axis of a goniometer
of welding conditions. The metallic alloys under such situated within the hatch of the beamline. In this system, the
thermal conditions show non-equilibrium behavior of phase head of a laser scanning confocal microscope (LSCM) was
transformation (PT). The non-equilibrium behavior of PT also set by fitting the theta axis, as shown in the photograph.
results in unexpected microstructures at room temperature. The focus point of the LSCM is on the surface of the
Then understanding such a behavior is essential for observed sample, which is set in the furnace. A two-
controling the microstructure of a weld accurately. dimensional pixel detector (Pilatus2M) was placed. The
A typical instance of non-equilibrium PT was presented incident beam, an ultra bright X-ray, was introduced into
by Vitek et al in the case of solidification process of the furnace and the diffractions were recorded by the pixel
stainless steel [1]. When the cooling rate increased, the detector with high time resolution. Simultaneously, the
solidification path was changed from delta-ferrite region to microstructural changes were observed through the LSCM
austenite region. Then the quantity of delta-ferrite at room in situ. The specimens, 5 mm in diameter and 1 mm thick,
temperature was unexpected in the case of rapid cooling. In were placed in a boron-nitride (BN) crucible in which the
that case, the solidification path was estimated from the X-ray absorption is quite small. The crucible was held by a
quantity of the delta-ferrite at room temperature. On the platinum holder, which was inserted in the furnace. The
other hand, Babu et al [2] has directly confirmed that the temperature was measured by a thermocouple incorporated
primary phase of solidification depended on the cooling into the crucible holder. The specimens were placed at the
rate by using a time-resolved X-ray diffraction (TRXRD) focal point of a halogen lamp. The temperature controller,
technique. The primary phase of Fe-C-Al-Mn steel changed which was connected to a personal computer (PC), the
from delta-phase to austenite phase for rapid cooling
conditions. This work shows that the in-situ observation
technique is useful to trace the PT under the rapid
cooling/heating conditions. The TRXRD technique gives
valuable information about PT, such as phase identification
and element partitioning during phase transformation. On
the other hand, the optical microscope technique is suitable
for getting the information about the microstructural
morphology and origin of microstructure growing.
Especially, laser scanning cofocal microscopy (LSCM)
system is appropriate for tracing of PT under the thermal
cycle designed [3]. The system consists of LSCM and an
infrared furnace. The infrared furnace possesses good
response of temperature.
In order to use all the features a described above, our
r e se a r c h gr o up has b e e n d e velo p ing a hyb r id TRX
RD/LSCM system to trace the PT [4]. In the present work,
the detail of the hybrid system is described. Furthermore,
the application of the hybrid TRXRD/LSCM system to
trace the PT of metallic alloys, such as steel alloy is
described.
2. Hybrid TRXRD/LSCM system Fig. 1 Hybrid TRXRD/LSCM system at the 46XU

Figure 1(a) shows a photograph of the experimental setup beamline of SPring8.
Japan
316
Developments of hybrid in-situ observation system to study the microstructural change of metallic alloys
thermocouple and the halogen lamp in the furnace were

placed outside the beamline hatch. When the thermal cycles
that simulate welding were programmed on the PC, the
profiles were sent to the temperature controller, which
reproduced the desired thermal cycles by switching the
halogen lamp on and off, based on the measured
temperature. Both the maximum heating and cooling rates
of the system were 37 K/s. The LSCM head enables in situ
observations of microstructural changes at 30 frames/s at
high temperatures. A CCD camera was connected to the
PC located outside the hatch and the images were stored at
a rate of 30 frames/s. The control program could trigger the
temperature controller, the X-ray shutter, the x-y-z stages
on theta axis, goniometer-axis control and the exposure of
the pixel detector.
Before the measurements, the specimen position was
adjusted in the manner explained in the following section.
Then, the theta axis was tilted to a fixed angle (5° in the
present study). The temperature controller was then
triggered at a set time, and the exposure of the detector was
activated with the time resolution of 0.2 s. TRXRD data
and LSCM images under the desired thermal cycles were
obtained simultaneously.
The undulator beam was monochromatized by the double
Si crystal, and a 30 keV of X-ray energy was used. The X-
ray was introduced into the hatch through a mirror; The X-
ray beam was shaped by the slit; the dimensions of the
beam were 0.5 mm × 0.5 mm. Before the measurements, the
position of the sample surface was adjusted. By controlling
the z-stage, the sample surface is forced to be in the middle
of the beam height. The theta axis was then rotated by 5°.
The camera length was 468.79 mm. The detector
dimensions were 1475 pixels (one pixel has an area of
0.172 mm2) × 1679 SL[HOV LQ WKH ș GLUHFWLRQ The PT of
low temperature transformation steel (LTT) was analyzed in
Fig. 2 Snap shots of PT of LTT under the cooling
the present work. Fig. 1(b) shows thermal cycle applied and
cycle.
the circle on the temperature profile means the X-ray
exposure point.

Figure 2 shows snapshots of LSCM images of PT of
LTT material under the cooling cycle. The austenite was
super-cooled until 300 Centigrade as shown in Fig. 2(a).
The austenite had large driving force of PT and changed the
transformation mechanism from diffusive to displacive
since diffusion is impossible at low temperature. As shown
in Fig. 2(b), the clear contrast appeared in the LSCM
images. The contrast increase as temperature decreased as
shown in Fig. 2(c). The clear contrast corresponds to Fig. 3 d-spacing, intensity, time and temperature diagram.
surface relief of martesitic microstructure. Finally, the
martensitic transformation stopped as shown in Fig. 2(d).
described in reference [5]. The mark on the temperature
The displace transformation discretely occurred along the
profile corresponds to that in Fig. 2. The 5 diffraction peaks
decreasing of temperature. As shown in this instance, the
of austenite transformed to diffraction peaks of martensite.
contrast of image included many information about the
The change was compatible to results in LSCM images. For
mechanism of PT.
instance, the analyzing the d-spacing change during PT
Figure 3 shows d-spacing, intensity, time and
gives the information about element partitioning during PT
temperature diagram during PT of LTT. The figure shows
[5, 6]. Then it could be said that the developed hybrid
reflections of J111, D’110, J200, D’200, J220, D’211, J311, system enable in-situ observation of PT of metallic alloys in
J222 and D’220 starting from the right. The diffraction data real and reciprocal lattice space.
were analyzed using the method and programming
317
4. Conclusions [2] S.S. Babu, J.W. Elmer, J.M. Vitek, S.A. David: Acta Mater,
The detailed configuration of the hybrid TRXRD/LSCM 50 (2002), pp. 4763-4781.
system was explained. The phase transformation behavior [3] H. Yin, T. Emi, H. Shibata: Acta Mater, 47 (1999), pp. 1523-
of low-temperature transformation steel was traced by using 1535.
[4]Y. Komizo and H. Terasaki: Sci. and Tech. Weld.
the system and it was shown that the hybrid system enable
Joining,(2010)doi:10.1179/136217110X12785889549822.
in-situ observation of phase trasnformation of metallic [5] S.S. Babu, E.D. Specht, S.A. David, E. Karapetrova, P.
alloys in real and reciprocal lattice space. Zschack, M. Peet, H.K.D.H. Bhadeshia: Metall Mater Trans A,
36A (2005), pp. 3281-3289.
References [6] H. Terasaki and Y. Komizo: Scripta Mater., 64 (2011) pp. 29-
[1] J. M. Vitek, A. Dasgupta and S. A. David: Metall. Mater. 32.
Trans. A, 14 (1983), pp. 1833-1841.
318
Measurement of fracture behavior of Zr-based metallic glass by

†
thermography
SAKINO Yoshihiro *, IZUMI Yui **, KURODA Toshio *, SAKAGAMI Takahide ***
and KIM You-Chul *
KEY WORDS: (Zr-based metallic glass) (High speed tensile test) (Thermography) (Fracture) (Spark)
ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ (Hot oxide particle) (Liquid droplet)
1. Introduction observe the sparking phenomenon of the metallic glass at

Since metallic glass is an amorphous solid, it offers fracture, the infrared (IR) thermograph was used. An
approximately three times the strength of crystalline infrared thermograph camera (Titanium 530L, Cedip) was
materials and it breaks without plastic deformation in used for thermograph detection; the sensor was made of
tensile tests1). Therefore, it is considered that enormous mercury cadmium telluride (MCT) with 7.6– ȝP
adiabatic deformation will occur. Molten particles or wavelength and 25-mK temperature resolution. A 128×128-
liquefied fractures are often observed after tensile tests on pixel area (4×4 cm) was measured at 700 Hz by an IR
metallic glass. Recently, Wang et al. conducted fatigue tests thermograph camera. A thin submicron graphite coating
on Zr-based metallic glass and reported the occurrence of was provided to reduce the heat reflection on the
sparking at fatigue fracture, which was photographed using measurement sample surface. After fracture, amorphous
an IR thermograph camera[1]. In the present study, the structures and crystallization of Zr 48 Cu 36 Al 8 Ag 8 metallic
high-speed tensile tests were performed on Zr-based glass specimens were analyzed using SEM observation of
metallic glass at various strain rates from low to high speed the fracture surface and XRD analysis.
using a high-speed tensile test unit of the dynamic structural
testing system. The sparking phenomenon at tensile fracture 3. Sparking Phenomenon
was photographed using a IR thermograph camera. We also The sparking phenomenon was observed in all
elucidated a mechanism generating the sparking Zr 48 Cu 36 Al 8 Ag 8 and Zr 55 Cu 30 Al 10 Ni 5 metallic glass
phenomenon by examining fracture surfaces and using specimens regardless of strain rate.
material science methods such as X-ray analysis[2]. Figure 2 shows IR thermograph camera photographs of
high-speed tensile fracture of Zr 48 Cu 36 Al 8 Ag 8 metallic
2. Experimental glass at 10 mm/s crosshead speed. It was detected at 1/700
Zr-based metallic glasses of Zr 48 Cu 36 Al 8 Ag 8 and second per frame. While fracture has not yet started in (a),
Zr 55 Cu 30 Al 10 Ni 5 were prepared at Tohoku University by the fracture section is indicated in red by the sparks in (b),
casting. Figure 1 shows a photograph of a tensile test and rough flying particles are seen at the moment of
specimen. The specimen was smooth and rod-shaped. The fracture. Particles are also seen in (c) and (d). This
specimen geometries were 5 mm in diameter, 30 mm in indicates that the fracture occurred instantaneously and that
gauge length and 60 mm in overall length. The amorphous the oxide particles or liquid droplets appear as particles.
nature of the structure was confirmed by halo pattern Although this can only be seen as a momentary spark when
detection through X-ray diffraction (XRD). observed visually, it could be detected with an IR
The tensile crosshead speed was varied from 0.001 to thermograph camera.
1200 mm/s. The strain rate ranged from 1.7×10-5 s-1 to Figure 3 shows IR thermograph camera photographs of
2.3×101 s-1. The test temperature was room temperature. To high-speed tensile fracture of Zr 55 Cu 30 Al 10 Ni 5 metallic
glass at 1200 mm/s crosshead speed. While fracture has not
yet started in (a), the fracture section is indicated in red.
5 Unit: mm Particles are seen in (c) ᴾ and (d) as same as
Zr 48 Cu 36 Al 8 Ag 8 , but the size of particles is very small, and
they are few in number compared to those for
30 Zr 48 Cu 36 Al 8 Ag 8 metallic glass.
As discussed above, it is considered that the particles are
60
flying and these are observed as sparks at the moment of
Fig. 1 Photograph of specimen. fracture of Zr-based metallic glass. However the number
and size of particles are different for compositions of Zr-
** Graduate School, Osaka University, Suta, Japan Japan
*** Graduate School, Kobe University, Kobe, Japan
319
Measurement of fracture behavior of Zr-based metallic glass by thermograpy
(a) 1/700 s (b) 2/700 s (a) 1/700 s (b) 2/700 s
(c) 3/700 s (d) 4/700 s (c) 3/700 s (d) 4/700 s

Fig. 2 Moment of fracturing of Zr48Cu36Al8Ag8 Fig. 3 Moment of fracturing of Zr55Cu30Al10Ni5
metallic glass (Crosshead speed 10 mm/s). metallic glass (Crosshead speed 1200 mm/s.)
based metallic glass. and the fracture surface was heated to high temperatures,
The mechanism generating this sparking phenomenon which caused oxidation.
has been suggested as follows: (1) thermal insulation From these observations, the flying particles, that are
phenomenon, (2) spattering of hot oxide particles, (3) observed as the sparks, are hot oxide particles and liquid
spattering of liquid droplets, (4) process of vanishing or droplets.
elimination of excess electrons specific to metallic glass,
and so on. This sparking phenomenon seems to be unique 4. Conclusions
to amorphous metallic glass. The conclusions of this study are summarized as follows.
Considering that the flying particles are also attached to (1) The sparking phenomenon was also observed in
the fracture surface, we examined the fracture surface using Zr 48 Cu 36 Al 8 Ag 8 and Zr 55 Cu 30 Al 10 Ni 5 metallic glass
SEM observation and XRD analysis. Figure 4 (a) and (b) specimens regardless of strain rate at the moment of
shows the fracture surface of Zr 48 Cu 36 Al 8 Ag 8 metallic fracture. However the amount of sparks are different,
glass in the tensile test at a low and high strain rate.
Regardless of the strain rate, smooth dimples (A) and
smooth areas (B) are observed, in addition to the rough
dimple fractures normally observed that indicate ductile
fracture. The smooth dimples (A) are regarded as attached
marks of flying particles due to sparking. These indicate
that the hot oxide particles collided with the fracture surface
and become attached. The smooth areas (B) are regarded as
melting and solidification cracking. This indicates that it
was heated to the melting temperature of metallic glass,
which is 900°C or higher, by thermal insulation change, etc.,
during the tensile fracture of the metallic glass, causing it to
melt, and then generate high-temperature cracks during
cooling. The large localized deformation and the remelting
feature are believed to be due to the high strength, large
elastic energy and low melting temperature of the alloy,
which are common characteristics of bulk metallic glass.
As for the results of XRD analysis, most of the fractures
had a halo pattern indicating an amorphous structure.
However, a peak for ZrO 2 oxide film or oxide particles or a
crystallization peak for substances such as ZrNi 2 were
observed in some parts along with the halo patterns. Thus,
some of the fracture particles become attached to the
fracture surface as flying particles at the moment of fracture Fig. 4 Fracture surfaces of tensile test. (a) Crosshead
speed 0.001 mm/s. (b) Crosshead speed 1200 mm/s.
320
depending on the components of Zr-based metallic glass. with the experiment. This work was supported by Grant-in-
Aid for Cooperative Research Project of Nationwide Joint-
(2) It is revealed by SEM observation and XRD analysis of
Use Research Institute on Development Base of Joining
the fracture surface that the flying particles of hot oxide
Technology for New Metallic Glasses and Inorganic
particles and liquid droplets are observed as sparks at
Materials from The Ministry of Education, Culture, Sports,
the moment of fracture. Although this can only be seen
Science and Technology, Japan.
as a momentary spark when observed visually, it could
be detected with an IR thermograph camera. References
[1] G.Y. Wang, P.K. Liaw, W.H. Peter, B. Yang, Y. Yokoyama,
Acknowledgements M.L. Benson, B.A. Green, M.J. Kirkham, S.A. White, T.A.
The authors sincerely thank Professor Inoue and Saleh, R.L. McDaniels, R.V. Steward, R.A. Buchanan, C.T.
Associate Professor Kimura, Tohoku University for Liu and C.R. Brooks: Intermetallics, 12 (2004), pp.885-892.
supplying the samples for this study.ᴾ The authors also [2] Y. Sakino, T. Kuroda, A Kobayashi and Y.-C. Kim: Frontier
thank Technical Specialist Mr. Nakatsuji, for his assistance of Applied Plasma Techmology, 2(3), pp.102-106.
321
Development of amorphous boron carbon oxynitride film for

†
transmission electron microscope with environmental-cell system
MATSUTANI Takaomi *, TSUTSUI Hidenori * and KAWAKAKI Tadahiro **
KEY WORDS: (Plasma chemical vapor deposition) (Amorphous boron carbon oxynitride) (Diaphragm)
(Environmental cell) (Transmission electron microscope)
1. Introduction chamber to isolate the vacuum around the TEM from the
It is an unquestionable fact that bulk gold is chemically reaction gas atmosphere around the specimen by means of a
inert. Recently however, it was reported that gold particles diaphragm [3]. The diaphragm is the most important part of
of less than 10 nm in diameter exhibit unique catalytic the E-cell TEM system because it not only maintains the
properties [1]. The level of catalytic activity is particularly pressure difference between the vacuum and the reaction
high in the oxidation of carbon monoxide (CO) and similar gas but also transmits the electron beam. Amorphous
substances when the particles are bound tightly to specific carbon thin films have so far been used as the diaphragm to
metal oxides, such as TiO 2 [2]. To determine the reaction allow observation of the oxidation of CO using the gold
mechanism of this gold nanoparticle catalyst, which is nanoparticle catalyst. The carbon thin film (thickness 8 nm)
unclear, requires investigation of the gold nanoparticle has advantages such as high hardness, no electron
surface and interface atomic structures. Transmission diffraction contrast and low electron scattering. However,
electron microscopy (TEM) is useful for analyzing extended observation is not possible as the film suffers
structures at the atomic level, but as specimens are normally damage from the electron beam and the oxygen in the E-
placed under a strong vacuum, it is difficult to examine cell. The diaphragm must consist of a light element,
directly the relationship between the observed structures chemically inert, of high hardness, and amorphous. The
and catalytic behavior, which requires instead observation development of a diaphragm is therefore a pressing need.
of the catalyst under reaction gas conditions. The present paper turns attention to the use of boron
The environmental-cell (E-cell) TEM system developed carbon oxynitride films in the diaphragm of the E-cell TEM.
by Ueda et al. includes a specimen holder with a small The films for the diaphragm were prepared using plasma
enhanced chemical vapor deposition (p-CVD) with
TAC film Cu grid for precursor of trimethyl borate (B(OCH 3 ) 3 : TMB) and
Environmental cell mixture gases of nitrogen (N 2 ) and argon (Ar). This
method has the advantage of greater film step coverage than
other coating methods. The prepared films on a Cu mesh
(1) (2) (3) for a specimen holder of TEM were characterized by
Slide glass scanning electron microscopy (SEM) and X-ray
photoelectron spectroscopy (XPS).
(4) (5)
Deposited film Etching Figure 1 shows the procedure for diaphragm formation.
First, a triacetyl cellulose (TAC) film was formed on a slide
Fig.1 Procedure for diaphragm formation. glass. The TAC film peeled off from slide glass was put on
a Cu mesh (diameter I 3.5 mm, thickness 1 mm, hole
Chamber
diameter I 100 Pm). A boron carbon oxynitride film was
Source gas deposited on it by p-CVD. Finally, the TAC film was
and carrier gas etched with acetone.
Figure 2 shows a schematic diagram of p-CVD method
experimental equipment. The gas canister and the chamber
were connected with stainless pipes. The source gas and
carrier gas were adjusted using a flow meter between
chamber and gas canisters. The electrodes were isolated
Fig. 2 Schematic diagram of p-CVD method. with glass. The inter electrode distance was 13 mm.
The boron carbon oxynitride films were deposited on
* Kinki University, Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Nagoya University, Nagoya, Japan Japan
322
Development of amorphous boron carbon oxynitride film for transmission electron microscope with environmental-
cell system
B-N
Intensity (arb. u.) B 1s B-C
(a) TMB
(b) TMB + N2
(c) TMB + N2 + Ar
B-O
(c)
(b)
(a)
220 210 200 190 180 170

Binding Energy (eV) Fig. 4 SEM photographs of boron carbon oxinitride
film applied to holes of Cu mesh; before (a) and after
C-B deposition (b).
C 1s
and N 2 (300 ml/min). Sample (c) was deposited with Ar gas
Intensity (arb. u.)
C-C (100 ml/min.) added to the gas flow for sample (b). In the B
(a) TMB 1s spectrum of sample (a), main peak was 189.6 eV
(b) TMB + N2
corresponding to B-C bonding and the spectrum did not
(c) TMB + N2 + Ar
C-N
include a peak at 192-193 eV corresponding to B-O
bonding [5, 6]. The C 1s spectrum of sample (a) included
(a) peaks at 288.5 eV and 283 eV corresponding to C-O and C-
(b)
B bonding, respectively. The atomic ratio of sample (a) was
(c)
about B:C = 1:2. TMB is composed of the chemical
305 300 295 290 285 280 bonding of B-(O-CH 3 ) 3 and the atomic ratio of TMB is
B:C = 1:3. It is therefore thought that oxygen desorption in
Binding energy (eV) the TMB gas was promoted by the generation of TMB
plasma and that film with B-C bonding was deposited by
N 1s
C-N
B-N
recombination of B-C or displacement of TMB.
In the B 1s spectrum of sample (b), main peak was
Intensity (arb. u.)
190.2 eV corresponding to B-N bonding and the spectrum

(a) TMB
also had a shoulder corresponding to B-O bonding (192-
(b) TMB + N2
(c) TMB + N2 + Ar
193 eV) and B-C bonding [7]. In the N 1s spectrum of
sample (b), main peak was at 398.5 eV corresponding to B-
N bonding and there was also a shoulder corresponding to
(c)
(b)
C-N bonding (399 eV). Although the deposited film was
(a) nitrided by incorporation of N 2 gas in TMB, TMB
decomposition of TMB was less than in sample (a) because
415 410 405 400 395 390 of the inclusion of B-O bonding in sample (b). The atomic
Binding energy (eV) ratio in sample (b) was B:C = 1:0.48 indicating a lower
carbon content than sample (a). It is thought that
Fig. 3 XPS spectra of B 1s, C 1s and N 1s for decomposition of O-CH 3 bonding to a level lower than the
boron carbon oxynitride films deposited on Cu bonding energy of B-O in TMB was mainly promoted. In
substrate under various gas conditions. the B 1s spectrum of sample (c), the main peak was the
Cu mesh and Cu substrate by p-CVD. TMB and N 2 were same as in sample (b) but the spectrum did not include a
used as source gases and Ar as carrier gas. The gas flow peak for B-O bonding. In the C 1s and N 1s spectra of
rate of TMB, N 2 and Ar ranged from 5 to 50 ml/min., 50 to sample (c), C-N bonding and the atomic ratio of nitrogen
500 ml/min., and 0 to 450 ml/min., respectively. A direct were higher than in sample (b). This suggests that inclusion
current (D.C.) power supply was used to generate plasma of Ar in the source gas enhances the dissociation of TMB
with voltage 250 V. The pressure at deposition was 5-20 Pa. and the reaction of boron, carbon, and nitrogen.
Figure 4 is a SEM photograph of the boron carbon
3. Results and discussion oxynitride film applied to the holes of Cu mesh. Photograph
Boron carbon oxynitride films deposited by p-CVD with (a) is before deposition on the Cu mesh and the photograph
source gases of TMB and N 2 were investigated by XPS. It (b) after deposition. A film was formed on the holes of Cu
is well known that including nitrogen in films made of mesh. There is no contrast variation, indicating that the film
boron-carbon produces high hardness [4]. Figure 3 shows was extremely smooth.
XPS spectra of B 1s (upper), C 1s (middle) and N 1s
(lower) for deposited films. Sample (a) as a control was 4. Conclusions
deposited at a TMB gas flow rate of 50 ml/min. Sample (b) For use as a diaphragm in the environmental cell, boron
was deposited under mixed gas flow of TMB (50 ml/min) carbon oxynitride films were prepared on Cu mesh by
323
plasma enhanced CVD with TMB and were characterized [2] M. Haruta: Catalysis Today, 36 (1997), pp.153.
by XPS. The films were composed of B-C, B-N and C-N [3] K. Ueda et al.: Sufrace and Interface Analysis, 40 (2008),
bonding and inclusion of Ar in the source gas enhanced the pp.1725.
dissociation of TMB and the reaction of boron, carbon and [4] Z. F. Zhou et al. : Surface & Coatings Technology, 128-129
(2000), pp.334.
nitrogen. The boron carbon oxynitride films were
[5] M.A Mannan et al.: American Journal of Applied Science, 5
successfully applied to a Cu mesh with holes of I 100 Pm. (2007), pp.736.
[6] M.C. Polo, E. Martinez, J.Esteve, J.L. Andujar: Diamond and
References Related Materials, 7 (1998), pp.376.
[1]M. Haruta: Journal of the Surface Science Society of Japan, 26, [7] Pi-Chuen Tsai: Surface & Coatings Technology, 201 (2007),
No. 10 (2005), pp.578 (in Japanese). pp.5108.
324
Properties of metallic glass coatings sprayed by gas tunnel type

†
plasma spraying
KOBAYASHI Akira *, KURODA Toshio *, KIMURA Hisamichi **, and INOUE Akihisa ***
KEY WORDS: (Metallic glass) (Gas tunnel plasma spraying) (Ni-based metallic glass coating) (Microstructure)
ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ (Scanning electron microscope (SEM)) (X- ray diffractmeter (XRD))
1. Introduction conditions shown in Table 1. The plasma torch was

Metallic glass is one of the most attractive advanced operated at power levels up to P = 20kW and the arc
materials because it has excellent physical and chemical current was changed I = 100-350 A. The plasma jet was
functions such as high strength and corrosion resistance [1]. generated with the aid of argon working gas supplied at Q =
Therefore many researchers have engaged in various 200 l/m. The torch was maintained at a spray distance of
developmental research works. However, as the metallic L = 40 mm from the substrate surface. The powder feed rate
glass material is expensive, the application for small size was about 7 g/min. The stainless steel substrate was
parts has been carried out only in some industrial fields. In traversed at N =16 times during the spraying time of t =24 s.
order to widen the industrial application fields, a composite
material is preferred for the cost performance. In the L
coating processes of metallic glass with the conventional
deposition techniques such as plasma sputtering, there is a
problem of the difficulty of obtaining thick coatings
because of their low deposition rate. Thermal spraying is
one of advantageous methods to produce metallic glass
composites for easy operation.
The gas tunnel plasma spraying is the besk technology
for high quality ceramic coatings [2-4]and synthesizing new Coating
functional materials [5], because the plasma jet has a high-
speed and a high-energy density under a controlled Plasma jet Substrate
Powder
operating condition [5]. By gas tunnel plasma spraying,
metallic glass coatings can be formed on stainless steel
substrates by using Fe-based or Zr-based metallic glass Fig. 1 Gas tunnel type plasma spraying used in this
powder [7,8]. The proper conditions for high quality study. (L=spraying distance).
metallic glass coatings have been clarified from those
experimental results. Microstructure of the Ni-based metallic glass coatings
In this study, a Ni-based metallic glass coating was also was observed by using a scanning electron microscope
formed by the gas tunnel plasma spraying, and the (SEM). The surface morphology of the feedstock powder
microstructures and surface morphology of the different and the metallic glass coating cross-section was also
metallic glass coatings were observed by using a scanning examined by a scanning electron microscope.
electron microscope (SEM). Those results were compared
to Fe-based and Zr-based metallic glass coatings. Table 1 Spraying conditions.
Arc current 100-350A
2. Experimental Voltage 40-50V
Ni-based metallic glass powder (Ni 60 Nb 20 Zr 20 ) was Spraying distance 40 mm
used in this study. This powder was atmospherically plasma Working gas flow rate (Ar) 200 l/min
sprayed (APS) on a flat 304 stainless-steel substrate by a Powder feed gas flow 10 l/min
gas tunnel type plasma spraying torch as shown in Fig. 1.
rate(Ar)
Ni-based metallic glass powder was externally fed into the
plasma flame from the exit of gas divertor nozzle, in order Powder feed rate 7 g/min
to melt the metallic glass powder effectively. Traverse number 16 times
Experiments were carried out under the spraying Spraying time 24 s
** Welding Company, Rokko Steel, Ltd., Kobe, Japan Japan
*** Tohoku University, Sendai,, Japan
325
Properties of metallic glass coatings sprayed by gas tunnel type plasma spraying
The phase constituents of metallic glass coating were amorphous phase (Phase center is about 42 degree) was
identified by using a X-ray diffractmeter (XRD) system observed in this pattern. But the XRD pattern has some
with CuKDradiation source at voltage of 40 kV and current crystalline peaks corresponding to some other compounds
of 40 mA. Obtained results were also discussed and of Ni, Nb, Zr, etc. shown in Fig. 3. Ni crystalline peak was
compared to Fe-based and Zr-based metallic glass coatings. recognized as shown in this figure. This means that the
Vickers microhardness measurement was made on the powder was not a perfectly amorphous phase and it
coating cross section by using a load of 100g. Indentation contains some metal or oxidation phase.
parameters were set as 20s loading time. These crystalline peaks near 40 degree were suppressed
Regarding the Ni-based metal glass powder used in this and disappeared on the metallic glass coating at 300A. The
study, the size of powder was 10-25Pm, and it was broad amorphous phase was clearly observed in the pattern
spherical type. (Average diameter is 18Pm.ὸ which is shown in Fig. 3(a). There were some new peaks
related to Ni, Nb, Zr, etc. at different diffraction angles of
the XRD pattern. Two crystalline peaks near 30degree and
3. Results 50degree were recognized as the peaks from Zr oxide phase.
Microstructure of the metallic glass coating When the metallic glass powder is injected into the plasma
Figure 2 shows the SEM micrographs of the cross- jet, particles under high temperature conditions are heated
section of Ni-based metallic glass coatings sprayed at and may be simultaneously decomposed. So, there is the
different plasma spraying current of I=100A and I=300A, large possibility of the crystalline peaks, and peaks of
at L=40mm.
There are some large pores in the Ni-based metallic
glass coating at a low current of 100A in Fig.ᴾ 2(a). The 㻟㻡㻜
coating thickness increased with increase in the plasma
㻟㻜㻜
current and it was more than 200 ȝm at 300A which is
shown in Fig.ᴾ 2(b). In this case, the coating was much 㻞㻡㻜
denser on the cross section of surface side and it was rather
㻞㻜㻜
lower porosity than that at 100A as shown in Fig. 3(a). The
ᙉᗘ㼇㼍㻚㼡㼉
bonding condition between the coating and the substrate 㻝㻡㻜

seemed good.
㻝㻜㻜
㻡㻜
㻜
20
㻞㻜 30
㻟㻜 40
㻠㻜 50
㻡㻜 60
㻢㻜 70
㻣㻜 80
㻤㻜
Diffraction angle, 2ș (degree)
ᅇᢡゅ㻞䃗㼇ᗘ㼉
Coating
ίa) Coating at 300A
SUS304
(a) 100A
㻣㻜㻜
(b) 300A
㻢㻜㻜
(a.u.)
ᙉᗘ䠄㼍㻚㼡䠅 (a.u.)
㻡㻜㻜
Intensity
Intensity
㻠㻜㻜
Coating 㻟㻜㻜
㻞㻜㻜
㻝㻜㻜
SUS304
㻜
㻞㻜㻟㻜㻠㻜㻡㻜㻢㻜㻣㻜㻤㻜
20 30 40 50 60 70 80
ᅇᢡゅ㻞䃗
Fig. 2 SEM micrographs of the cross-section of the Ni Diffraction angle, 2ș (degree)
based metallic glass coating sprayed at 100A and
300A, on the 16 times traversed substrate. ίb) Powder
Crystallie structure of the metallic glass coating
The XRD pattern from the surface of the metallic glass Fig. 3 XRD patterns of the Ni-based metallic glass coating
coating at 300A which is shown in Fig. 2(b) is shown in Fig. sprayed on stainless-steel substrate (a) and Ni-based
3(a). For comparison, the XRD pattern of Ni-based metallic metallic glass powder (b).
glass powder used is shown in Fig. 3(b). The broad
326
other oxidized materials, but there were no peaks from Ni, References
Nb, Zr detected in this XRD pattern. [1] A. Inoue, B.L. Shen and H.M. Kimura: J. Metastable
Nanocrys. Mater., 20-21 (2004), pp.3-12.
[2] Y. Arata, A. Kobayashi and Y.Habara: J. Appl. Phys., 62-12,
4. Conclusions (1987), pp.4884-4889.
The Ni based metallic glass sprayed coating in thickness [3] A. Kobayashi: Surface and Coating Technology, 90 (1990),
of more than 200 ȝm with Hv 100 = 700, was obtained at pp.197-202.
300A by gas tunnel type plasma spraying. The coating [4] A. Kobayashi, T. Kitamura: Vacuum, 59 (2000), pp.194-202.
thickness depends on the spraying parameters. Ni-based [5] A. Kobayashi: Weld.International, 4 (1990), pp.276-282.
metallic glass particles had some decomposition of [6] Y. Arata and A. Kobayashi: J. Appl. Phys., 59 (1986),
amorphous phase and/or oxidation (ZrO 2 ) during pp.3038-3044.
[7] A. Kobayashi, S. Yano, H. Kimura and A. Inoue: Surface
deposition at high plasma current above 350A.
and Coating Technology, 202 (2008), pp.2513-2518.
[8] A. Kobayashi, S. Yano, H. Kimura and A. Inoue: Frontier of
Applied Plasma Technology, 1 (2008), pp.47-50.
327
Inter-granular cracking of a splat of zirconia coating fabricated by

†
plasma spraying technique
FUJIMOTO Koji *, EL-SHEIKHY Refat ** and KOBAYASHI Akira ***
KEY WORDS: (Zirconia) (TBC) (Inter-granular fracture) (Columnar grain) (Crack) (Crack propagation)
㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 (Fracture) (Stress intensity factor) (Energy release rate) (Gas tunnel type plasma spraying)
1. Introduction 1) Two dimensional model with homogeneous and

The zirconia coating is useful for the thermal barrier isotropic material is assumed.
coating (TBC). But this ceramic coating has a problem such 2) Cracks can be propagating only along the grain
as cracking in the inside of coating as well as delamination. boundaries and each end of the cracks is on a triple
Therefore to investigate the mechanism of the cracking and point of the grains.
fracture is one of the most important issues for the 3) Equi-biaxial tension is applied to the model as the
development of high performance TBC. Previously, thermal stress.
zirconia coating was fabricated over the surface of the
substrate of stainless steel by gas tunnel type plasma
spraying system and the crack running in a splat of the
coating was observed using a SEM (scanning electron
microscope) [1-3]. As a result, it has been shown that crack
propagation occurs with many kinks and bifurcations along
columnar grain boundaries of zirconia and that regular
zigzag crack patterns are sometimes observed. Furthermore,
based on simplified assumptions, stress intensity factors of
inter-granular cracks with kinks in a splat were calculated
and the crack propagation was also simulated in order to
reveal the process of cracking and fracture [3]. In this
report, previous studies by the authors are summarized and
further numerical simulation of crack propagation in a splat
of zirconia coating is conducted with a new postulation ȝP
regarding the energy release rate.
Fig. 1 Honeycomb-like microstructure of a splat
2. Experimental
of zirconia coating.
Kobayashi has developed the gas tunnel type plasma
spraying system [4], [5]. Figure 1 shows an example of the
SEM photographs of a splat of zirconia coating fabricated ȝP
on the substrate of stainless steel using the spraying system
[2], [3]. From this figure, it can be seen that the splat
consists of honeycomb-like crystal grains.
El-Sheikhy and Kobayashi observed inter-granular
cracks running along the boundaries of the columnar
honeycomb-like grains of the splat as shown in Fig. 2 and
found that some parts of the cracks are running with regular
zigzag pattern like Fig. 3 [1], [3]. These cracks are
anticipated to be extending due to the thermal stress
induced by cooling from high temperature during spraying
to the room temperature.
3. Numerical Simulation of Crack Propagation

The authors have analyzed inter-granular crack paths in Fig. 2 Inter-granular crack propagation along the
the honeycomb-like grains model shown in Fig. 4 [3]. In honeycomb-like columnar grain boundaries
this analysis, the following assumptions are made. observed in a splat of zirconia coating.
* School of Engineering, The University of Tokyo, Tokyo, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan Japan
** Faculty of Engineering, King Saud University, Riyadh,
Kingdom of Saudi Arabia
*** JWRI, Osaka University, Ibaraki, Japan
328
Inter-granular cracking of a splat of zirconia coating fabricated by plasma spraying technique
Crack tip
Crack tip
ȝP Fig. 5 Direction of inter-granular crack propagation in the

model shown in Fig. 4. The red line and the blue arrows
Fig. 3 Regular zigzag crack propagation observed show the crack and the directions of crack propagation,
in a splat of zirconia coating. respectively.
V V
B C
A D (1) (3)
(2)
V V (4) (5)
V V
(6) (7)
(8) (9)
(10)
V
Fig. 4 Model of a splat of zirconia coating with V
honeycomb-like crystal grains under
equi-biaxial tension. Fig. 6 An example of numerically simulated crack path in
a splat of zirconia coating. The red line ABCD is the
assumed initial crack and the crack is spreading
in the order of (1), (2), (3), ···.
4) The size of the model is sufficiently large comparing
with the cracks.
5) According to the maximum tangential stress criterion energy release rates of four directions are calculated using
[6], the crack is running in the direction T íZKHQ the method proposed by Nuismer [7]. An example of
K II > 0 and T = +60° when K II < 0, where K II is the numerically simulated crack paths is shown in Fig. 6 in
mode II stress intensity factor. (Regarding the detail, which the red line ABCD indicates the assumed initial
refer to [3].) crack and the blue lines are the predicted crack paths. The
Here, instead of the above assumption 5), the following crack is simulated to be propagating in the order of (1), (2),
postulation is adopted. (3), ··· without the branch (2) extending any more. Some
6) Crack propagation occurs by the length a to the other numerical simulations suggested that a crack is
direction in which the energy release rate is the largest extending only at one of its tips showing regular zigzag
among four directions shown in Fig. 5, where a is the pattern, and at another crack tip, it extends only in one
side length of the hexagon of the crystal grain. The branch or never extends.
crack does not extend in multiple directions
simultaneously. 4. Conclusions
The stress intensity factors at the tips of the inter-granular Based on the inter-granular crack propagation observed
crack are calculated by the method shown in [3] and the in a splat of the zirconia coating fabricated by the plasma
329
spraying technique, numerical simulations of crack [2] R. El-Sheikhy and A. Kobayashi: Transactions of JWRI,
propagation were conducted using a simplified model of Osaka University, 37-1 (2008), pp.69-72.
honeycomb-like crystal grains based on the energy release [3] A. Kobayashi, R. El-Sheikhy and K. Fujimoto: Appl. Plasma
rate. As a result, the regular zigzag crack propagation has Sci., 17-2 (2009), pp.117-124 (in Japanese).
[4] Y. Arata, A. Kobayashi and Y. Habara: Journal of High
been simulated.
Temperature Society, 13-3 (1987), pp.116-124 (in Japanese).
This work was performed under the Cooperative Research
[5] A. Kobayashi, Y. Habara and Y. Arata: Journal of High
Program of Joining and Welding Research Institute, Osaka
Temperature Society, 18-2 (1992), pp.25-32 (in Japanese).
University, Japan.
[6] F. Erdogan and G. C. Sih: Journal of Basic Eng., 85 (1963),
pp.519-527.
References [7] R. J. Nuismer: International Journal of Fracture, 11 (1975),
[1] R. El-Sheikhy and A. Kobayashi: Transactions of JWRI, pp.245-250.
Osaka University, 36-2 (2007), pp.87-94.
330
Tungsten coatings on reduced-activation ferritic/martensitic steel

†
by plasma spray technique
Thermal behavior of Tungsten coatings
TOKUNAGA Kazutoshi *, KOBAYASHI Akira **, ARAKI Kuniaki *, FUJIWARA Tadashi *,

MIYAMOTO Yoshio *, NAKAMURA Kazuo *, KURUMADA Akira ***,
TOKITANI Masayuki ****, MASUZAKI Suguru ****, EZATO Koichiro *****,
SUZUKI Satoshi *****, ENOEDA Mikio ***** and AKIBA Masato *****
KEY WORDS: (Plasma spray) (Tungsten) (Ferritic/martensitic steel) (Coating) (Thermal property) (Heat flux
test) (Fusion device) (First wall) (Divertor) (High heat flux)
1. Introduction block with a cooling tube of inside diameter of 7mmIHeat

Tungsten is potential candidate for an armor of the first load tests were performed on an active cooling test stand
wall and the divertor plate of the fusion reactor because of (ACT) of NIFS and an electron beam irradiation test
its low erosion yield and good thermal properties. The simulator at the Research Institute for Applied Mechanics
disadvantages of tungsten are its heavy weight and the (RIAM) at Kyushu University. In the case of ACT
brittleness below DBTT. In the case of the fusion experiments, a uniform electron beam was irradiated on the
demonstration reactor (DEMO), neutron damage will be a tungsten surface through a beam limiter with an aperture of
critical issue. Structure materials of the first wall/blanket 20mm×20 mm. Beam duration during ramp-up, plateau and
and the cooling channels of the divertor will be made by ramp-down were 20, 40 and 0 s, respectively. Heat flux was
low activation materials. Tungsten coated reduced changed from 1 to 3.4 MW/m2. Thermal fatigue tests were
activation materials could be convenient for the first also carried out for up to 100 cycles at a heat flux of 3.2
wall/blanket because the thickness of tungsten on the first MW/m2. Surface temperature of the tile is measured by an
wall/blanket is designed at about 2῍3 mm and the coating optical pyrometer. Temperatures of F82H (T1) and OFHC
technique can be used for this[1]. (T2) at interfaces of the brazed area were also measured
In the present work, tungsten coating on reduced- with thermocouples. The heat flux tests have been carried
activation ferritic/martensitic steel (RAF/M) F82H substrate out under the condition that the water flow velocity,
(F82H: Fe-8Cr-2W), which is a leading structural material pressure and temperature were 18.0 m/s, 0.7 MPa and 20 oC,
candidate for DEMO [2], by Atmospheric Plasma Spraying respectively.
(APS), Vacuum Plasma Sprayin (VPS) and Gas Tunnel
Type Plasma Spraying (GTP) ᴾ were prepared. Surface 3. Results
morphology of the deposited W and adhesion property Figure 1 shows the APS-W coated F82H brazed on
between the substrate and the coatings have been OFHC with cooling tube. There is no damage after the
investigated using SEM/EDS. In addition, heat flux tests brazing of the OFHC block with the cooling tube.
and thermal fatigue tests using an electron beam have been
also carried out.
2. Experimental
W coated material has been produced by APS and VPS
to evaluate thermal behavior of APS-W and VPS-W. The
substrate material is reduced-activation ferritic/martensitic
steel (RAF/M) F82H (Fe-8Cr-2W) [2]. Size of the substrate
material was 20 mm x 20 mm x 2.6 mmt. A thickness of W
is 1mm. Temperatures of the substrates during the APS
and VPS were 150 oC and 600 oC, respectively. In addition,
mock-ups were made by brazing the tiles (VPS-W/F82H,
APS-W/F82H) on oxygen free high purity copper (OFHC) Fig. 1 Photograph of APS-W/F82H/OFHC mock-up
† Received on 30 September 2010 ***** JAEA, Ibaraki, Japan
* RIAM, Kyushu University, Fukuoka, Japan Transactions of JWRI is published by Joining and Welding
** JWRI, Osaka University, Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
*** College of Engineering, Ibaraki University, Ibaraki, Japan Japan
**** NIFS, Gifu, Japan
331
Tungsten coatings on reduced-activation ferritic/martensitic steel by plasma spray technique
Thermal behavior of Tungsten coatings
Figure 2 and 3 show heat flux dependence of plateau strongly dependent on the fabrication process. Therefore,
temperatures measured at the surface, T1 and T2 for VPS- we estimated the thermal conductivity of the present case as
W/F82H/OFHC and APS-W/F82H/OFHC, respectively. It follows. The heat flux q through a material layer at steady
can be seen that the temperatures increased continuously state for plane geometries is given by
with increasing heat flux. Surface temperature of the VPS-
W/F82H/OFHC is always lower than that of the APS-
'T
W/F82H/OFHC; for example, the surface temperatures are q k
about 700 oC and 1200 oC at the heat flux of 3.4 MW/m2, 'x
respectively. In the case of steady state, temperature
increase is inversely proportional to the thermal where 'x is the thickness of material layer of PS-W and
conductivity. The thermal conductivity of plasma spray W F82H, 'T the temperature difference corresponding to
depends strongly on its texture structure and residual
porosity. Cross sectional observation of the APS-W showed the 'x and k thermal conductivity [6]. Estimated thermal
that pores partially existed between W particles. This is one conductivities of APS-W/F82H is 10 W/mk, which is about
of the reasons for the high temperature increase of the W 5.6 % of normal W and 37 % of F82H at RT. On the other
surface of APS-W. hand, estimated thermal conductivities of VPS-W/F82H is
77 W/mk, which is about 43 % of normal W and 285 %
㻝㻠㻜㻜
㻌
of F82H. It is considered that the thermal conductive of
㻝㻞㻜㻜
㼂㻼㻿㻙㼃㻛㻲㻤㻞㻴㻛㻻㻲㻴㻯
㻌㻿㼡㼞㼒㼍㼏㼑
VPS-W/F82H is good enough taking into account thermal
conductivity of F82H.
㼀㼑㼙㼜㼑㼞㼍㼠㼡㼞㼑㻌㻔㼛㻯㻕
㻌㼀㻝
㻝㻜㻜㻜㻌㼀㻞
The thermal fatigue test up to 100 cycles (3.2 MW/m2,
㻤㻜㻜
40 s ON:40 s OFF) for APS-W/F82H/OFHC and VPS-
㻌
㻢㻜㻜
W/F82H/OFHC showed that temperatures of surface, T1
㻠㻜㻜 and T2 did not change. The surface morphology also did
㻞㻜㻜 not change. In addition, no cracks and exfoliation were
㻜 observed. These results indicate that no failure occurred at
㻜㻚㻜㻜㻚㻡㻝㻚㻜㻝㻚㻡㻞㻚㻜㻞㻚㻡㻟㻚㻜㻟㻚㻡㻠㻚㻜
㻴㼑㼍㼠㻌㻲㼘㼡㼤㻌㻔㻹㼃㻛㼙㻞㻕 the interface or in the W coating during cyclic heat load.
Fig. 2 Thermal response of VPS-W /F82H/OFHC 4. Conclusions
㻌 Two types of plasma spray tungsten coatings on
㻝㻠㻜㻜
㻭㻼㻿㻙㼃㻛㻲㻤㻞㻴㻛㻻㻲㻴㻯 ferritic/martensitic steel F82H made by vacuum plasma
㻝㻞㻜㻜
㻌㻿㼡㼞㼒㼍㼏㼑 spray technique (VPS) and atmospheric plasma spray
technique (APS) have been examined to evaluate their
㼀㼑㼙㼜㼑㼞㼍㼠㼡㼞㼑㻌㻔㼛㻯㻕
㻌㼀㻝
㻝㻜㻜㻜㻌㼀㻞
㻤㻜㻜 possibility as a plasma-facing armor in the fusion device.

Thermal response test and thermal fatigue tests indicate a
㻌
㻢㻜㻜
㻠㻜㻜 high potential of this coating as plasma-facing armor under

㻞㻜㻜
thermal loading.
㻜
㻜㻚㻜㻜㻚㻡㻝㻚㻜㻝㻚㻡㻞㻚㻜㻞㻚㻡㻟㻚㻜㻟㻚㻡㻠㻚㻜 References
㻴㼑㼍㼠㻌㼒㼘㼡㼤㻌㻔㻹㼃㻛㼙㻞㻕 [1]S. Suzuki, Y. Ueda, K. Tokunaga, K. Sato and M. Akiba:
Fig.3 Thermal response of APS-W /F82H/OFHC Fusion Sci. Technol., 44(1) (2003), pp.41-48.
[2] K. Shiba, M. Enoeda, S. Jitsukawa: J. Nucl. Mater. 329-333
As shown in Figs. 2 and 3, the surface temperatureᴾ of (2004), pp.243-247.
APS-W coated mock-ups is always higher than that of VPS- [3] I. Smid, M. Akiba, G. Vieider, L. Plo¨ chl: J. Nucl. Mater,
W coated mock-ups. This degradation in heat transfer must 258–263 (1998), pp.160.
be caused by low thermal conductivity of the APS-W layer [4] B. Riccardi, A. Pizzuto, L. Bertamini, M. Diotalevi, G.
and/or interface of APS-W and F82H. The thermal Vieider: Proc. 17th IEEE:NPSS Symposium on Fusion
conductivity of plasma spray W (PSW) depends strongly on Engineering, SOFE 97, San Diego, CA, 1997.
[5] R.A. Neiser, R.D. Watson, G.R. Smolik, K.J. Hollis: Proc.
its texture structure and residual porosity. It was reported
1993 National Thermal Spray Conference, NTSC’93,
that thermal conductivity of APS-W and VPS-W is about Annaheim, CA, 1993.
20 and 60% of pure W, respectively [3–5] but it also [6] J. Linke, H. Bolt, Thermal Stability, in: W.O. Hofer, J. Roth
(Eds.), Physical Processes of the Interaction of Fusion Plasmas
with Solids, Academic Press, New York, 1996.
332
†
Plasma plume length determined from light intensity
KOIKE Kazuo *, ONO Norifumi * and KOBAYASHI Akira **
KEY WORDS: (Plasma jet) (Image analysis) (Light intensity) (Gas tunnel type plasma spraying) (Thermal
barrier coatings) (Atmospheric pressure)
1. Introduction
Thermal Barrier Coatings (TBCs) have been
synthesized with plasma aided techniques such as the
thermal plasma spraying method[1-4]. In plasma sprayed
TBCs, flow and thermal characteristics of spraying plasma
affect the performance of TBC materials. Therefore, it is
important to obtain a better understanding of the behavior
of arc plasma during synthesizing the materials.
From this view point, light intensity analysis was
conducted to consider the behavior of the plasma flow in
the preparation of TBC materials by plasma spraying
techniques. The effects of powder feed rate on plasma
plume length were mainly examined in the present study.
The spraying plasma was observed with a digital single-lens
reflex camera. Contours of light intensity in the plasma are
visually determined from RAW image files of the camera
with the software for analyzing the RAW format. Simple
consideration of thermal characteristics was done on the
basis of the obtained results. Fig.1 Image of plasma jet and contour plot of light
intensity (I =300A, without powder).
Plasma jet was generated under atmospheric pressure by was set to certain values that were practically used for the
using a gas tunnel type plasma spraying torch [5]. Working experimental studies of plasma sprayed coatings in the case
gas is argon, with a flow rate set to 200 l/min. Powders for of each powder. These were 200A, 300A and 400A in the
TBCs were fed into the plasma plume with carrier gas. case of TiO 2 and HA and 200A and 300A in the case of
Argon was also used as the carrier. The flow rate was ZrO 2 and Al 2 O 3 . The behavior of spraying plasma was
specified to about 5 l/min. In this study, TiO 2 (titanium observed under the same conditions of shutter speed and
dioxide), ZrO 2 (Zirconium dioxide) and Al 2 O 3 (Aluminum exposure time with a digital single-lens reflex camera
oxide) were employed as injected powders. In addition to (Nikon D2x, 12.4Mpixels) through the viewing window
them, HA(hydroxyapatite) was also examined. Feed rate of that can observe the plasma jet flowing out from the torch
each powder is shown in Table 1. The plasma arc current I exit. RAW data format, which records data directly from
the image sensor of the camera and has precise information
Table 1 Feed rate of each powder.
on the light intensity, was employed as image format.
Digital data on light intensity in the plasma are determined
Feed rate (g/min) from the RAW image files with the software for analyzing
Powder
Case 1 Case 2 Case 3 Case 4 Case 5 the RAW format [6]. Digital data on light intensity were
averaged over 10 RAW data sets as illustrated in upper
TiO2 0 <5 ~10 ~15 photograph of Fig. 1. Lower figure of Fig. 1 indicates
HA 0 <5 ~10 ~15 contour plot of light intensity in the domain bounded by the
rectangle-shaped solid line in the upper image. Since the
ZrO2 0 ~5 ~7 ~10 ~15 image sensor of the camera has a Bayer filter, whose pattern
Al2O3 0 ~5 ~7 ~10 ~15 consists of red, blue and two green filters, data on red, blue
and green can be captured. Averaged light intensity
*ᴾ Department of Mechanical Engineering and Intelligent Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Systems, Tohoku Gakuin University, Tagajo, Japan Japan
**ᴾ JWRI, Osaka University, Osaka, Japan
333
Plasma plume length determined from light intensity
between two green filters was mainly used in the present Figure 3 indicates variation of the length 'x with feed
analysis. The length 'x between the torch exit and the rate of powder in the case of ZrO 2 and Al 2 O 3 . Plasma arc
boundary of specified threshold intensity was determined current I was set to 200A and 300A in these cases. 'x is
from the light intensity contours. normalized with respect to ('x) 300A,NP that stands for 'x in
the case of plasma torch current I of 300A without powder.
3. Results and Discussion The results of ZrO 2 and Al 2 O 3 are indicated by squares and
Figure 2 shows variation of the length 'x with feed rate circles, respectively. 'x shows a tendency to shorten due to
of powder in the case of TiO 2 and HA. 'x is normalized the injection of powders in both cases. It also decreases
with respect to ('x) 400A,NP that denotes 'x for a plasma with increases in powder feed rate. These results are
torch current I of 400A without powder. In the case of HA thought to be caused by the somewhat high rate of energy
represented by circles, 'x shows a tendency to decrease by given to powders since plasma arc current is relatively low.
the injection of powder for I =200A and 300A. The In the present experiment, different results were obtained
influence of powder addition on the plume length is not according to the kinds of feeding powders. Therefore, it is
obvious for I =400A. It is thought that the effect of powder necessary to consider not only powder properties but also
injection on the plasma plume becomes less due to higher properties of feeding powders for plasma as working fluid.
input to the plasma generation. On the other hand, the
length is not influenced much by feeding of TiO 2 powder as 4. Conclusions
denoted by squares. This is partly because the flow rate of To obtain a better understanding of the behavior of arc
the plasma jet increases due to the addition of carrier gas. plasma in the preparation of TBC materials by the plasma
Moreover, there does not appear to be a clear effect of spraying techniques, light intensity analysis was conducted
powder feed rate on the length. by utilizing RAW image files. The results obtained here are
summarized as follows.
(1) Different results of the influence of powder injection on
plasma plume length were obtained according to kinds
of injected powders.
(2) The plasma plume length is not obviously affected by
powder injection in the case of higher plasma arc
current.
(3) The plume length shows a tendency to decrease with
increases in feeding rate of ZrO 2 and Al 2 O 3 powders in
the case of relatively lower plasma torch current.
5. Acknowledgement
The authors would like to thank Dr. Yugeswaran
Subramanium for his help in operation of the experiment.
This work was performed under the Cooperative Research
Program of Institute for Joining and Welding Research
Institute, Osaka University.
Fig. 3 Variation of length 'x with powder feed rate References

[1] A. Kobayashi: Surf. and Coat. Technol., 90 (1990), pp.197-
for ZrO2 and Al2O3. 202.
[2] A. Kobayashi, T. Kitamura: Vacuum, 59-1 (2000), pp.194-
202.
[3] G. Shanmugavelayutham, S. Yano and A. Kobayashi: Adv. in
Appl. Plasma Sci., 5 (2005), pp.259-264.
[4] J-L. Zhang and A. Kobayashi: Adv. in Appl. Plasma Sci., 6
(2007), pp.113-116.
[5] A. Kobayashi: J. High Temp. Soc. 11 (1985), pp.124-131.
[6] K. Koike and N. Ono: Adv. in Appl. Plasma Sci., 6 (2007),
pp.33-36.
Fig. 2 Variation of length 'x with powder feed rate

for TiO2 and HA.
334
Titanium oxide film deposition by vortex air thermal plasma

†
assisted spray pyrolysis deposition
ANDO Yasutaka * and KOBAYASHI Akira **
KEY WORDS: (Titanium oxide) (Photo-catalysis) (Thermal plasma) (Thermal spray) (CVD) (Dye sensitized
solar cell)
1. Introduction After titanium oxide films deposition, investigations

Spray pyrolysis deposition (SPD) is a rapid film were made of the microstructure of the film by X-ray
deposition process. Various functional material films, such diffraction (CuKD, 40 kV, 100 mA). Besides, in order to
as SnO 2 [1], YSZ [2], CuInSe 2 [3] and so on, have been confirm photo-catalytic property of the film, methylene-
successfully deposited so far. Especially, in the case of blue droplet test and its decoloration test using UV
oxide film deposition, film deposition can be carried out in irradiation equipment (Fig. 2) were carried out.
open air. Therefore, SPD is hoped to be a low cost
deposition process for functional material films. However, Anode Substrate
since film was deposited by chemical reaction of non- Cathode
activated precursors on the substrate, substrate should be

heated over 773 K in the case of conventional SPD. So, it Micro 㸫
was very difficult to apply this process to low melting point tube
materials such as plastics. pump +
Plasma jet
In this study, in order to develop a low temperature film
deposition process using spray pyrolysis deposition, as a
basic study, titanium oxide film deposition by vortex air
thermal plasma assisted spray pyrolysis deposition was DC
carried out. Feed
-stock power
Air
In this study, two types of SPD equipments, which were a) Straight plasma jet type
straight plasma jet assisted SPD equipment and vortex
plasma jet assisted SPD equipment, were used. These SPD Substrate
equipments consisted of plasma torch, DC power supplying Coating
Plasma jet
system, micro tube pump (feedstock supplying system) and Cathode Anode
working gas supplying system as shown in Fig. 1. Table 1
shows deposition conditions. The plasma torch has water 㸫
cooled electrodes. The anode is made from copper, has
feedstock feeding port at the head and has a constrictor
which is 6 mm in diameter. A cylindrical cathode made +
Airbrush
from tungsten has a diameter of 5 mm. Air was used as
working gas. Mass flow rate of the gas was fixed at 50
l/min. As the feedstock for titanium oxide film deposition, Micro
tube
ethanol diluted titanium tetra iso butoxide (Ti(OC 4 H 9 ) 4 ) DC pump Feed
Air
was used. Substrates were 15mm x 15mm x 1mmt 304 power -stock
stainless steel plates with #400 sand paper polished surface.
The spray distance (the distance between the nozzle outlet b) Vortex plasma jet type
of the plasma torch and the surface of the substrate) was
fixed at 100 mm. The deposition time was 7 min. The Fig. 1 Schematic diagrams of the SPD equipments.
discharge power was 10A/ 100V. In the case of vortex
plasma jet assisted SPD equipment, a commercial airbrush
was used as feedstock spraying equipment.
* Ashikaga Institute of Technology, Tochigi, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** JWRI, Welding University, Osaka, Japan Japan
335
Titanium oxide film deposition by vortex air thermal plasma assisted spray pyrolysis deposition
Table 1. Film deposition conditions . on the condition of 100 mm in deposition distance.

Therefore, amorphous titanium oxide film was deposited.
Air working gas flow rate 50 l/min. However, by post heat (723 K, 30 min.), the amorphous
film could be changed into anatase dominant film. Besides,
Discharge Power 10A/ 100V
it was confirmed that the anatase film has photo catalytic
Deposition distance 100 mm properties according to the methylene-blue decoloration test.
Deposition time 7 min
C2H5OH diluted
Feedstock
TTIB* solution
Feedstock feed rate 200 ml /h
Subatrate 304 stainless steel
*TTIB: Titanium tetra iso butoxide
UV light Darkroom
Fig. 3 Appearance of the TiO2 film deposited substrate.

10mm
Methylene blue droplet Substrate

Fig. 2 Equipment for methylene-blue decoloration test.

Film deposition by straight plasma jet assisted SPD
Since thermal plasma has steep axial and radial profiles,
deposition distance is one of the most important operation
conditions affecting the film structure and component.
Figure 3 and 4 show the appearance and XRD pattern of Fig. 4 XRD pattern of the TiO2 film deposited substrate.
the sample deposited on the condition of 100mm in
deposition distance. The deposition temperature was
approximately 673 K. As for the appearance of the sample,
gray color film with coarse surface was deposited. As the
reason why the film became coarse, it was thought that the
partially vaporized and activated feedstock was fed to the
substrate surface because the feedstock was fed to the
plasma jet as droplets due to its surface tension of the
feedstock. However, in the XRD pattern, diffraction peaks
indicate TiO 2 . Especially, anatase which is known as
excellent photo catalytic material was dominant in the
deposited titanium oxide film. As photo-catalytic property a) 0 hr b) 4 hr
detection methods, wettability testing and methylene-blue
decoloration testing are relatively easy methods. Figure 5 Fig. 5ᴾ Results of metylene blue decoloration testing in the
shows appearances of the sample before and after case of TiO2 film deposited substrate
methylene-blue decoloration test. The films were
hydrophilic and it was observed that the methylene-blue 4. Conclusions
droplet was slightly decolored after only 4 hour UV In order to develop a high rate and low cost functional
irradiation. oxide film deposition process, deposition of titanium oxide
film by two types of SPDs using air working gas was
Film deposition by vortex plasma jet assisted SPD carried out. Consequently, anatase dominant gray color film
In the case of vortex plasma jet assisted SPD, since the could be obtained and it was confirmed that the anatase
substrate could not be heated by plasma jet directly, the films had photo-catalytic properties by the methylene-blue
substrate temperature during deposition was under 623 K droplet test and its decoloration test. From these results, this
336
technique was found to have high potential for high rate and References
low cost functional oxide film deposition. [1] T. Nagamoto, M. Endo, O. Omoto: Jpn. J. Appl. Phys. 18, 6
(1979), pp.1103-1109.
[2] H. Ishizawa: Am. Ceram. Soc. Bull. 65 (1986), pp.1399-1402.
[3] S. Shirakata, H. Kubo, C. Hamaguchi, S. Isomura: Jpn. J.
Appl. Phys. Pt. 2, Letters 36, 10B (1997), L1394-L1396.
337
Investigations on frequency shift probes for monitoring of electron

conditions in nano-materials processing plasmas†
NAKAMURA Keiji * and SUGAI Hideo *
KEY WORDS: (Electron density) (Electron temperature) (Frequency shift probe) (Plasma monitoring) (Sheath
effect) (Sheath width) (Resonance frequency)
1. Introduction for the slit width of 1 mm, 5 mm or 8 mm in the present

In advanced materials processing for manufacturing LSI FDTD simulation.
devices, improvement of accuracy and repeatability has Since the sheath is formed around the probe head
been required to achieve high performance process. In homogeneously, a vacuum thin layer was considered as the
general, temporal variation of plasma components is sheath in the whole surface of the probe in the model. The
believed to be one of reasons for the problems, so it is resonance frequency was examined as a function of a
important to understand the phenomena in the plasma and thickness of the vacuum layer.
to develop technologies for accurate plasma control. As one
of solutions, we have developed a frequency shift probe as 3. Results and Discussions
a novel in-situ plasma monitoring technology. The probe Figure 2 shows dependence of a resonance frequency
enables us to measure an electron density from variation of of the probe head on the sheath width as a parameter of the
the resonance frequency of the probe head caused by the slit width for the electron density of 3x1010 cm-3. The
plasma, and the density measurement is possible under resonance frequency shown in Fig. 2 was normalized by
minimum disturbance to the plasma. Furthermore, the probe
is applicable to reactive plasmas such as fluorocarbon
plasmas since the deposited polymer has little effect on the
resonance frequency. Sheath
Recently, the frequency shift probe has been studied
Slit
from a viewpoint of fundamental measuring characteristics
and miniaturization of the probe size[1, 2]. When the
resonance frequency of the probe varies from f 0 (GHz) to f r Probe
(GHz) by producing the plasma with the electron density of Plasma
n e , (1010 cm-3), the value of n e is given by
ne ( f r2 f 02 ) / 0.81 Fig. 1 Model of frequency shift probe
However influences of the sheath formed around the probe 1.2

have not been considered in the studies. In this work, sheath Slit 1mm
effects on the frequency shift probe are investigated based
Normalized Resonanc
on finite difference time domain (FDTD) simulation, and it 1.1 Slit 5mm
Frequency [-]
is examined how much influences on the measured density Slit 8mm

the sheath have[2]. Furthermore, the frequency shift probe 1.0
is tried for measurements of electron temperature using the
sheath effects. 0.9
2. Model of Frequency Shift Probe

0.8
The frequency shift probe was modeled as shown in 0.0 0.2 0.4 0.6 0.8 1.0
Fig. 1: a 3 cm x 4 cm rectangular probe head with a
Sheath Width d [mm]
thickness of 0.2 mm is immersed into a 10 cm x 10 cm x 10
cm cubic plasma, and has a semi-circular slit. Frequency-
swept microwave voltage is applied to the end of the slit, Fig. 2 Variation of resonance frequency with sheath width
and a resonance frequency of the probe head was calculated as a parameter of slit width

* Graduate School of Engineering, Chubu University, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
338
Investigations on frequency shift probes for monitoring of electron conditions in nano-materials processing plasmas
that for the sheath width of 0 mm. The resonance frequency

decreased as the sheath width increased since effective
permittivity of the media around the probe head decreased.
Such a decrease of the resonance frequency was observed
regardless of the slit width, however its dependence on the
sheath width was affected by the slit width, and it became
significant as the slit width decreased. Actually, when the 1-
mm-thick sheath was formed around the probe, the
resonance frequency varied by ~3 % at most for the slit
width as large as 8 mm, but by ~13 % for the slit width of 1
mm. The sheath width is proportional to Debye length, so
the resonance frequency shown in Fig. 2 is given as a
function of electron density and electron temperature.
Since the resonance frequency of the frequency shift
probe is a function of electron density n e and electron
temperature T e , resonance frequencies obtained in two Fig. 3 ne-Te characteristic curves for different frequency
frequency shift probes with different sheath dependence shift probes
give unique solutions of ne and T e .
For example, assume that production of plasma induced
shift of resonance frequency from 1.78 GHz to 2.8 GHz for
the probe of 1 mm in a slit width and from 1.62 GHz to 2.9
GHz for that of 5 mm in a slit width. A relationship
between n e and Te to satisfy the measured resonance 㻢
frequency can be calculated from the FDTD simulation, and
it is shown in Fig. 3 as a n e -Te characteristic curve for 㻡
㻲㼞㼑㼝㼡㼑㼚㼏㼥㻌㼟㼔㼕㼒㼠㻌㼜㼞㼛㼎㼑
each probe. A crossing of the two curves represents a
㻱㼘㼑㼏㼠㼞㼛㼚㻌㼀㼑㼙㼜㼑㼞㼍㼠㼡㼞㼑㻌㻌㼇㼑㼂㼉
solution of 7.5x1010 cm-3 in n e and 4.8 eV in T e .

㻠
According to the above procedure, the electron temperature
of an inductively-coupled plasma (ICP) was measured and
compared with a conventional Langmuire probe. The ICP 㻟
㻸㼍㼚㼓㼙㼡㼕㼞㻌㼜㼞㼛㼎㼑
was produced with 13.56 MHz RF power up to 400 W at an
argon pressure of 3 mTorr. Two frequency shift probes 㻞
whose slit widths were 1 mm and 5 mm gave measured
electron temperatures as constant as 3.1 ~ 4.8 eV, which 㻝
was comparable to 4 eV obtained by the Langmuir probe.
These results suggest that measurements of electron 㻜
temperature is available with the frequency shift probe. 㻜㻝㻜㻜㻞㻜㻜㻟㻜㻜㻠㻜㻜㻡㻜㻜
㻰㼕㼟㼏㼔㼍㼞㼓㼑㻌㻼㼛㼣㼑㼞㻌㻌㼇㼃㼉
4. Conclusions
Recently, the frequency shift probe has been studied Fig. 4 Comparison of electron temperature between
from a viewpoint of fundamental measuring characteristics frequency shift probe and Langmuir probe
and miniaturization of the probe size. However influences
of sheath formed around the probe have not been
considered in these studies. In this work, sheath effects on
the frequency shift probe are investigated based on finite
difference time domain (FDTD) simulation, and it is
examined how much influence on the measured density the References
sheath has. As a result, the resonance frequency decreased [1] S. Yajima, K. Nakamura and H. Sugai; 27th Int. Symp. Dry
as the sheath width increased since effective permittivity of Process (DPS2005) (Nov. 2005, Korea) 5-36.
[2] H. Kim, K. Nakamura and H. Sugai; 28th Int. Symp. Dry
the media around the probe head decreased. Furthermore
Process (DPS2006) (Nov. 2006, Japan) 7-11, pp. 55-56.
such a characteristic enabled us to measure electron density
as well as electron temperature.
339
Dissimilar laser brazing of single crystal diamond and tungsten

†
carbide
SECHI Yoshihisa *,** and NAKATA Kazuhiro ***
KEY WORDS: (Laser brazing) (Single crystal diamond) (Tungsten carbide)
1. Introduction ceramic brazing and its thickness was 0.1mm.

The brazing technology is commonly used for the A braze sheet was sandwiched with a diamond block
bonding of ceramic to metals [1-3]. Although, there are from top side and a tungsten carbide plate from bottom side
some problems such as joint defects that due to thermal in a vacuum chamber as shown in Fig. 1. The topside of the
stress in the joint field and material deterioration by heating specimen was covered with a transparent quartz glass plate,
in these dissimilar joints [4]. which also served to fix the specimen. This chamber was
Diamond has various functional characteristics. evacuated to less than 10-1 Pa after samples had been
Especially single crystal diamond has a good wear loaded, and substitution of the atmospheric pressure with
resistivity and thermal conductivity. Besides, tungsten 99.999% Ar gas was done after the evacuation. This
carbide - cobalt alloy made by powder metallurgy has low evacuation and substitution cycle was done at least three
thermal expansion coefficient and high rigidity good for a times before brazing. During brazing, Ar gas continued to
counter structural material to ceramics. flow, with a flow rate of about 5L/min.
Among brazing processes, laser brazing [3] has good The generated YAG and LD lasers were radiated
characteristics for dissimilar joining because of the through the transparent quartz glass plate to the topside of
possibility of short heating times and small heating areas, the WC-Co. Scanning of laser was done on the WC-Co
and suppression of damage to the base materials without around the single crystal diamond block. Laser brazing
furnace in comparison with conventional furnace brazing. condition is summarized in Table 1. Scanning speed of
This method is suitable for brazing of diamond, which has a laser was determined in order to heat the specimen
tendency to graphitization at high temperature. So, this efficiently in a circle around it.
study describes dissimilar laser brazing of single crystal
Table 1 Laser brazing condition.
diamond and tungsten carbide using Ag-Cu-Ti alloy braze.
Pulsed YAG Average Output (kW) 0.134
Pulsed YAG wave length (nm) 1064
2. Experimental method
CW LD Output (kW) 0.02
Commercially available WC-Co alloy classified as ISO
CW LD wave length (nm) 808
K10 grade and artificial single crystal diamond were used Pulse frequency (Hz) 100
in this work, whose sizes were 10mm × 10mm × 2mm and (1st run) 0.6
4mm × 4mm × 2mm, respectively. The crystal plane (100) (2nd run) 1.0
Scanning speed
of the single crystal diamond was used as the interface. (mm/s) (3rd run) 1.0
70.26mass%Ag-28.06mass%Cu-1.68mass%Ti alloy braze (4th run) 1.0
sheet included Ti as major active ingredient for direct Laser beam diameter (mm) 0.5
Glass fiber 5º Cross sectional observations and elemental analyses of

Beam head the interface were performed using an electron probe micro-
analyzer. Interfacial observation and estimation of interface
Transparent area were performed using a scanning acoustic microscope.
quartz Single Shear strength was calculated from maximum load divided
glass plate crystal Laser beam
diamond by interface area estimated from scanning acoustic
Braze microscopy.
Tungsten
carbide 3. Results and discussions
Laser radiation area
Figure 2 shows a cross sectional SEM observation of a
Specimen stage Thermo couple single crystal diamond / Ag-Cu-Ti braze / WC-Co interface
with low magnification. The interface between single
Fig. 1 Schematic illustration of laser brazing. crystal diamond and Ag-Cu-Ti braze is smooth and no
* Kagoshima Prefectural Institute of Industrial Technology, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Kagoshima, Japan Japan
** Graduate School of Engineering, Osaka University, Osaka,
Japan
*** JWRI, Osaka University, Osaka, Japan
340
Dissimilar laser brazing of single crystal diamond and tungsten carbide
99.9 2
Single crystal diamond 1
Failure probability (%)

-0
-1
lnln(1-F)-1
Ag-Cu-Ti Braze 10 -2
-3
1 -4
WC-Co -5
ȝP m = 2.624 -6
0.1
ı0 =130.4MPa -7
Fig.2 Cross section of a single crystal ȝ 03D -8
diamond / braze / WC - Co interface. 0.01 -9
1 10 100 1000
Shear stress (MPa)
a) SEM Image b) Ag c) C Fig. 5 The Weibull distributions of shear strength test.
Single crystal
diamond distribution of Ti was located at the interface. The
distribution of Cu is similar to that of Ti, but its peak
Ag-Cu-Ti shifted to the braze side and the concentration of Cu in the
Braze braze away from the interface was high. This shows the
ȝP existence of interface layers of C-Ti and Cu-Ti. These
d) Cu e) Ti f) Line analyses results strongly suggest the formation of reacted layers like
Min Max TiC and Cu-Ti like Cu 3 Ti at the interfaces of single crystal
&ĺ diamond / Ag-Cu-Ti braze, respectively [5, 6].
Non-destructive test by scanning acoustic microscopy
ĸ7L
was done to evaluate how the melted braze filler spread at
the interface between single crystal diamond and WC-Co
ĸ&X plate. Figure 4 (a) shows appearance of the specimen and
(b) shows the image of scanning acoustic microscopy at the
Fig. 3 Map analysis of a single crystal diamond / interface of the single crystal diamond / Ag-Cu-Ti braze /
braze interface. WC-Co. The black area in the center of (b) is Ag-Cu-Ti
braze which was melted at the joint interface and partly
a) b) spread out on the interface onto the WC-Co plate. There
were no big voids in the black area where melted braze
existed at the joint interface. So the wettability of these
Single crystal
Ag-Cu-Ti Braze braze fillers and single crystal diamond or WC-Co seemed
diamond
to be good.
Figure 5 shows the Weibull distribution of shear
strength test of single crystal diamond / Ag-Cu-Ti braze.
2mm
WC-Co WC-Co In the case of all tests, fracture occurred at the single crystal
diamond side of the specimen. Average shear strength was
Fig. 4 a) Appearance of specimen and b) interfacial 115.9MPa. This suggests that the fracture occurred at the
observation using scanning acoustic microscopy. base material of single crystal diamond and that the
interface of brazing joint has the strength enough to connect
voids were observed. Also the interface between WC-Co single crystal diamond and WC-Co.
and Ag-Cu-Ti braze is smooth.
Figure 3 shows the result of map analysis of a single 4. Conclusions
crystal diamond / Ag-Cu-Ti braze interface. Figure 3(a) The conclusive remarks of this study are summarized as
shows enlargement of the single crystal diamond / Ag - Cu - follows.
Ti braze interface in Fig. 2. Figure 3(b) shows the (1) At the interface of single crystal diamond / Ag-Cu-Ti
distribution of Ag near the interface in the same area of Fig. braze, a concentration of Ti and C was observed. It was
3(a). Fig. 3(c), (d) and (e) show the distributions of C, Cu presumed that the reacted phase existed at the interface
and Ti, respectively. From these distributions of elements, between single crystal diamond and braze.
the concentration of Ti near the interface was observed and (2) No large voids or cracks in the braze area existed from
its thickness was about 2ȝm. non-destructive observation of the interface using
Figure 3(f) shows line analyses of C, Ti and Cu in the scanning acoustic microscopy.
same area of (b) to (e). The distribution of C is decreased (3) Fracture occurred at single crystal diamond side of each
sharply at the interface. Meanwhile, the peak of the specimen after a shear strength test. This suggests that
341
the shear strength indicates the bulk strength of single References

crystal diamond and this brazing joint has strength [1] Y. Nakao, K. Nishimoto and K. Saida: Trans. of Japan
enough to connect single crystal diamond and WC-Co. Welding Soc., 20 (1989), pp.66-76.
[2] M. Nicholas, D. Mortimer, L. Jones and R. Crispin: J. Mat.
Sci., 25 (1990), pp.2679-2689.
Acknowledgements [3] Y. Sechi, T. Tsumura and K. Nakata: Mat. and Des., 31
This work was supported by Joint Research system at (2010), pp.2071-2077.
the Joining and Welding Research Institute, Osaka [4] W. Wlosinski: Fueg. Keram. Gla. Met., (1985), pp.22-36.
University. [5] A.Palavra, A. Fernandes, F. Costa, R. Silva, C. Serra, L.
Rocha: Dia. and Rel. Mat., 10 (2001), pp.775-780.
[6] Y. Sechi, A. Takezaki, T. Matsumoto, T. Tsumura and K.
Nakata: Mat. Trans., 50 (2009), pp.1294-1299.
342
Joining mechanism between aluminum and polypropylene resin

†
using insert materials by laser irradiation
HINO Makoto *, MITOOKA Yutaka *and KATAYAMA Saiji **
KEY WORDS: (Laser joining) (Different material) (Insert material) (Diode laser) (Aluminum) (Plastics)
ᴾ (Elastomer)
1. Introduction
Table 1 Chemical treatments for 1050P aluminum
Metals and plastics have been widely used in industrial substrate after mirror buffing.
application such as automobiles, aircraft and electronic Alkaline dipping Acid dipping Second alkaline dipping
devices [1]. Joining a metal and a plastic is necessary and
important from a manufacturing viewpoint. Such joining is (Na2CO3(20kg/m3 )+
Na2SiO3(10kg/m3 ) Alkaline dipping Acid dipping
generally performed using adhesive bonds or mechanical
tools, such as bolts and rivets. These joining processes have (325K-30s)
problems in terms of environmental restriction on the Ļ Ļ 䊼
Washing Washing Washing
emission of volatile organic compounds, the difficulties of
䊼䊼
mass production, and high production costs. Therefore, Nitric acid (60%) Alkaline dipping
another process strongly needs to be developed for joining 䊼䊼
a metal and a plastic. Washing Washing
In this study, on laser joining between a 1050P
aluminum sheet and a polypropylene resin sheet with a
newly developed insert sheet, the effects of the 1050P
aluminum sheet having its surface shape and chemical state Table 2 Experimental conditions of laser joining.
changed due to a surface treatment such as alkaline dipping Wavelength 808nm
or acid dipping on the joining properties were examined in Focusing distance 100mm
order to clarify the joining mechanism. Spot diameter ȝP
Defocusing distance 12mm
2. Experimental Exposure mode CW
A 1050P aluminum sheet (1050P) (50×25×1tmm) and a Exposure angle 80° for the joining material
polypropylene sheet (PP) (50×25×2tmm) were used as the
Laser power 200 W
joining materials. Chemical treatments shown in Table 1
Joining Speed 5 mm/s
were done for a mirror surface by buffing in order to clarify
the effect of the chemical state of the 1050P surface on the
joining strength. After the chemical treatment, surface
shape measurement and XPS analysis were conducted on
each treated surface in order to examine the chemical state.
The styrene block copolymer (SBC) thermoplastic
elastomer fabricated into a sheet 50 ȝP in thickness was
used as the insert material, and polarity was given by a
carboxyl group or an amine group for these insert materials
in order to improve the joining ability with 1050P.
The insert sheet was placed between the joining materials,
as illustrated schematically in Fig.1, and laser joining was
conducted under the condition shown in Table 2.
After laser irradiation, joining strength was measured by
the shearing test.

Table 3 shows the surface roughness (Ra) and the Fig. 1 Schematic drawing of experimental set-up of laser
surface area (I Surf Area) of the specimens with chemical joining.
ᴾ †ᴾ Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding
*ᴾ Industrial Technology Research Institute of Okayama Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Prefecture, Okayama, Japan Japan
**ᴾ JWRI, Osaka University, Osaka, Japan
343
Joining mechanism between aluminum and polypropylene resin using insert materials by laser irradiation
treatment shown in Table 1 for the 1050P with mirror showing a similar tendency of the shear strength between
buffing. The surface roughness increased with each the -NH 2 group and the -COOH group as shown in Fig.3
chemical treatment, and the surface then became rougher, demonstrate that the hydrogen bond should be generated
however, there was no significant difference in the surface between the hydroxyl groups on the aluminum surface and
roughness and the surface area with each chemical the -NH 2 group or -COOH group of the given insert
treatment. Therefore, an aluminum surface is etched in the materials. By the way, it was not possible to join 1050P and
first alkali treatment, but that surface is hardly etched in the PP, because no reaction was generated between aluminum
next chemical treatment such as the acid treatment or the and the insert materials on using the insert materials without
second alkali treatment. Thus, in spite of the same alkali a denaturant. These results strongly support the above-
treatment for the buffing or acid treatment, the etching mentioned hydrogen bond between the 1050P and the PP.
effect is remarkably different. This result demonstrates that Table 3 Surface roughness (Ra) and surface area (I Surf
the state of the oxide film which is formed after the buffing area) for various chemical treatments of mirror buffed
or acid treatment is different. No Alkaline Acid Second alkaline
Table 4 shows the shear strength of the specimen after reatment dipping dipping dipping
each chemical treatment. The shear strength with the first 6XUIDFHURXJKQHVV5DȝP 0.063 0.219 0.214 0.207
alkali treatment was improved in comparison with that of Surface area (mm2 ) 0.016 1.548 1.540 1.540
the buffing of a surface that was not treated. The shear
Table 4 Shear strength with various chemical treatments
strength with the next acid treatment then improved further
of 1050P aluminum substrate.
than that with the first alkali treatment. However, the shear
strength with the second alkali treatment was lowered No Alkaline Acid Second alkaline
further than that of the buffed specimen. In spite of the fact treatment dipping dipping dipping
that there was little difference in the surface shape with Shear strength (N) 936.7 1023.0 1122.3 847.7
each chemical treatment based on the results shown in
Table 3, the shear strength after each chemical treatment
was different. These results indicate that the chemical state
of the surface aside from the surface shape seems to affect
the joining strength in this process.
Figure 2 shows the XPS Al 3p1/2 narrow spectra at the
surface with buffing and for each treated surface. The peaks
of the metal and the oxidation state were present for all
specimens, the proportion of the peak of the metal state and
oxide state changing with each treatment. This result
suggests that the chemical state at the outermost surface
varies with each chemical treatment.
In this study, the reactivity between the metal and the
insert material allows improvement by giving the insert
material polarity with a carboxyl group. Because the change
in the chemical state of the aluminum surface by chemical
treatment such as alkali or acid significantly affects the
reactivity with the insert materials, acid-base interaction [2]
is suspected to be responsible for the adhesion model Fig. 2 XPS Al3p1/2 narrow spectra of aluminum
between the 1050P and the insert materials. Degeneration substrates after various chemical treatments.
of the insert material was produced by the -NH 2 group
which was the basic functional group in contrast with the -
COOH group, and similar laser welding was then carried
out; the shear strength was measured in order to clarify the
acid-base interaction. The results of shear strength are
shown in Fig. 3. In comparison with the shear strength of
the insert materials denatured by a -COOH group or an -
NH 2 group, because the shear strength after acid treatment
is the highest though the absolute value is different, the
shear strength due to each treatment tended to be similar.
This result indicates that another joining mechanism exists
in addition to the acid-base interaction.
In general, the adhesive bonds for metals having
organic functional groups such as an OH radical, an -NH 2
group, a -COOH group in the molecule are firmly fixed on Fig. 3 Shear strength with various chemical treatments of
the metal surface by means of the interaction force based on 1050P aluminum substrate.
the hydrogen bond between the hydroxyl groups on metal (a) No treatment, (b) Alkaline dipping,
surface and the organic functional groups [2]. The results (c) Acid dipping, (d) Second alkaline dipping
344
4. Conclusions group at the outermost surface depended on the oxidation

The conclusions of this study are summarized as follows. state which seemed to affect the hydrogen bond, and the
The joining strength changed with a chemical treatment shear strength then changed.
such as acid or alkaline dipping of the aluminum surface,
and this tendency was similar for the insert materials References
denatured by a -COOH group or an -NH 2 group. Therefore, [1] F.Matsuda et al., Data Book for Welding and Joining
a hydrogen bond is a controlling factor in the joining of Technologies, Tokyo ,Tech Information S.C. Co., (2008).
[2] T.Ogawa: Sechaku handbook, 4th, (Ed. by The Adhesion Soc.
aluminum and the insert materials compared to the acid-
of Jpn.,Nikkankogyo-shinbunsya, 2007) pp.836-840.
base interaction. At that time, the state of the hydroxyl
345
Modeling of temperature distribution with metal vapour in pulsed

TIG including influence of radiative absorption†
IWAO Toru *, MORI Yusuke *, SAKAI Tadashi *, TAKI Hiroyuki *, SHIMOKURA Takuya *,
TASHIRO Shinichi **, TANAKA Manabu ** and YUMOTO Motoshige *
KEY WORDS: (Numerical calculation) (Radiation) (Self-absorption) (TIG) (Arc) (Metal vapor) (Welding)
1. Introduction Therefore, a self-consistent modelling approach is required.

Most reports to date have addressed the case of a Tungsten is used for the cathode and stainless steel for
constant arc current. However, pulsed arc currents are the anode. The iron vapour is generated from the molten
widely used in high-speed welding, and in general to region of the anode. The spacing between the electrodes is
control the heat input and droplet transfer in arc welding. In 5 mm, the shielding gas is argon, the gas flow rate is 10 slm,
the case of TIG welding, in which the electrode rod does and the pressure is 0.1 MPa. The following assumptions are
not melt and no droplet transfer occurs, pulsed currents are made: 1) local thermodynamic equilibrium, 2) laminar flow,
used to control the heat input to the arc and weld pool, and 3) incompressible fluid, 4) only the anode is melted, and 5)
to facilitate high-speed welding. There are few if any cases the surface of the welding pool remains flat. The model
in which the time variation of the metal vapour distribution allows the temperature, fluid flow and distribution of
has been discussed for pulsed TIG welding. It is important electromagnetic properties in the electrodes and the arc to
to understand the time dependence of the metal vapour be calculated simultaneously.
distribution, since the mixing of metal vapour with the The pulsed current waveform is used in the calculation
shielding gas affects fundamental properties such as the arc as follows. The peak current is 150 A, the base current is 50
temperature and the radiative emission. Furthermore, A, the duty ratio is 0.5, the transient time of the current is
because the self-absorption of the radiation strongly 0.2 ms, and the frequency is 100 Hz. The characters denote
influences the arc temperature and the heat transfer to the the following: A, the time of transition to base current; B,
weld pool [1]-[4], it is necessary to take into account the the time immediately before the transition from the base
self-absorption of the arc radiation. current to the peak current; C, the time of transition to peak
In this paper, the time dependence of the distribution of current; and D, the time immediately before the transition
temperature with vapour from the anode is analyzed using from the peak current to the base current. The distribution
an electromagnetohydrodynamic simulation that includes of temperature at each time is calculated self-consistently.
the influence of self-absorption of radiation. Iron is the In the present calculation model, the electrode and the
main component of stainless steel, which is often welded arc are combined into one system and simultaneously
using TIG welding. Using plasma thermophysical data that analyzed. The transfer of energy between the arc and the
take into account the iron vapour concentration, the effects electrode is obtained from the equation below and added as
to the temperature distribution are investigated, with the a localized source term in the equation for conservation of
influence of self-absorption included. energy.
The iron vapour concentration on the surface of the
2. Method of Calculation anode is determined by the saturation vapour pressure and
Electromagnetohydrodynamic simulations of arcs are the ambient pressure. The saturation vapour pressure is
performed using a two-dimensional cylindrical coordinate determined by the temperature at the surface of the welding
system. However, it is difficult to treat radiative transfer in pool. The concentration distribution is obtained by solving
the cylindrical coordinate system, because the circular grid the conservation equation of the iron vapour, using the iron
does not conform to the linear propagation paths of light. vapour concentration on the anode surface as a boundary
To solve this problem, a three-dimensional Cartesian condition. Changes in the fundamental characteristics of the
coordinate system is introduced to calculate the radiation arc caused by mixing of iron vapour are studied taking into
power distribution while considering self-absorption. A account the influence of the iron vapour concentration on
two-dimensional axisymmetric cylindrical coordinate the thermophysical properties.
system is used for all other aspects of the The transfer of radiation to and from a control volume
electromagnetohydrodynamic model. It is also important to is calculated using two different methods. In the simple
note that the iron vapour concentration, the arc temperature self- absorption model, the calculation domain is the same
and the radiative properties of the arc all affect each other. cylindrical coordinate system used for the
* Tokyo City University, Tokyo, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
346
Modeling of temperature distribution with metal vapour in pulsed TIG including influence of radiative absorption
Fig. 1 Temperature distribution Fig. 2 Radiation distribution
electromagnetohydrodynamic model. Absorption is which the base current is constant. The concentration near
calculated only within the control volume in which the anode is low. At the time of the base-to-peak current
emission occurs, and depends only on the temperature and transition, the increase in the downward convective flow in
the radial dimension of the control volume (the absorption the arc, driven by the magnetic pinch force, causes the iron
length). In the full self-absorption model case, the vapour to be transported in the direction of the anode. This
calculation domain is divided into a three-dimensional continues during the period in which the peak current is
Cartesian grid. Incident radiation entering a control volume constant.
from all three adjacent control volumes is considered. The When self-absorption is considered, its effects are
flux of incident radiation from each direction is normalized expected to be more pronounced in the low-temperature
to the area of the interface relative to the control volume’s region than in the high-temperature region. Therefore, the
total surface area. With each passage through the control absorption is greatest at locations where a large amount of
volume, the incident radiation intensity decreases because metal vapour is present at low temperatures. This
of self-absorption and increases according to the influence corresponds to the regions in the periphery of the arc near
of the radiative emission from within the control volume. the anode, and it is therefore these regions whose
temperature is increased. The temperature gradient is also
3. Temperature Distribution with Changing Current important; a high gradient favours localized absorption,
Including Influence of Self-absorption since low-temperature absorbing regions are closer to high-
Figure 1 and 2 show the distribution of the arc temperature emitting regions.
temperature and radiation, for the simple model that takes
account of one control volume and directions, and full self- 4. Conclusions
absorption model that takes account of all three adjacent A time-dependent electromagnetohydrodynamic
control volumes and directions. simulation of pulsed TIG arc welding was performed, with
The results show that the iron vapour diffuses upwards the electrodes and arc included in the computational
toward the cathode at the time of the peak-to-base current domain. The distribution of temperature with vapour
transition. Furthermore, it diffuses during the period in generated from the anode was calculated, using
347
thermophysical properties that take into account the iron References

vapour concentration. The influence of self-absorption of [1] A. Essoltani, P. Proulx, M. L. Boulos and A. Gleizes:
radiation was calculated using a Cartesian grid, allowing Volumetric emission of argon plasmas in the presence of vapors
radiation from all three adjacent control volumes and of Fe, Si, and Al, 14 (1994), pp.437-450.
[2] Gonzalez J J, Gleizes A, Proulx P and Boulos M:
directions to be taken into account. Arc temperature Mathematical modeling of a free-burning arc in the presence of
distribution was calculated self-consistently. metal vapor J. Appl. Phys. 74 (1993), pp.3065–3070.
[3] Haidar J: The dynamic effects of metal vapour in gas metal arc
Acknowledgement welding J. Phys. D: Appl. Phys. 43 (2010) pp.165204.
The authors wish to thank Dr Tony Murphy, Mr Yuki [4] Schnick M, Füssel U, Hertel M, Spille-Kohoff A and Murphy
Shibuya, Mr Masakazu Kojima and Mr Masahiro Kimura A B, Metal vapour causes a central minimum in arc temperature
for their fruitful discussions. in gas–metal arc welding through increased radiative emission J.
Phys. D: Appl. Phys. 43 (1994), pp. 022001.
348
†
Development of pure Ar–MIG welding
NAKAMURA Terumi *, HIRAOKA Kazuo ** and TANAKA Manabu **
KEY WORDS: (MIG arc welding) (Pure Ar) (Shielding gas) (Column of liquid metal) (Wire melting
behavior)(Coaxial hybrid solid wire) (Instability) (Simulation)
1. Introduction
Coaxial hybrid solid (CHS) wires have been developed temperature, specific heat and thermal conductivity. We
to carry out stable MIG welding in pure Ar shielding gas [1, discuss the influence of material properties on wire melting
2]. The characteristics of weld metal are improved using behavior using a wire melting model of CHS wire [4] and
MIG welding in pure Ar shielding gas (Ar-MIG welding) develop the design guide for CHS wire.
because the amount of oxygen in weld metal, which Fig.1
deteriorates the characteristics of weld metal, decreases [3]. 2. Wire melting behavior of CHS wire
However, the Ar-MIG welding is not used because of arc In order to investigate the influence of the material
instability. If we use a conventional solid wire, a column of properties on wire melting behavior, the simulation is
liquid metal (CLM) occurs at the wire tip (Fig. 1). This carried out [4]. First, we investigate the effect of melting
CLM makes the Ar-MIG welding unstable. In order to temperature. We changed the melting temperature at the
stabilize the Ar-MIG welding, shortening of the CLM is inner part. The wire tip shape and temperature distribution
indispensable. are shown in Fig. 3. The result of Inconel-Steel CHS wire
To shorten the CLM, the CHS wires (Fig. 2) have been is shown in Fig. 3(b). The melting temperature at the inner
developed [1, 2]. The composition of the inner part and the part is set higher than the melting temperature of Inconel
outer part are selected so that the amount of melting at the (Fig. 3(a)). The wire tip shows the convex shape. The CLM
inner part may increase more than that of melting at the is made easily because the inner part becomes long. The
outer part. Instead of generating the CLM, a big droplet melting temperature at the inner part is set lower than the
was then obtained (Fig. 2). As a result, stable Ar-MIG melting temperature of Inconel (Fig. 3(c)). The CLM is not
welding was achieved. made because the wire tip shows the concave shape. It is
The melting behavior depends on physical properties of effective to use the low melting temperature materials at
inner materials and outer materials, such as melting the inner part to shorten the CLM.
Fig.3Distance from contact tip L (mm)
㻯㻸㻹 C
㻭㼞㼏
0.6
0.4 +RRS6WHHO (a) (K)
0.2
,QQHU70 .
0.0 1700
0.2 13 15 16 17 18
14
0.4
+RRS6WHHO
0.6
0.6
0.4 +RRS6WHHO
Fig. 1 Welding behavior of Ar-MIG welding using 0.2
(b)
Inconel (TM =1627K)
conventional solid wire. 0.0
0.2 8 9 10 11 12 13
1000
0.4 +RRS6WHHO
㻵㼚㼚㼑㼞㻌㻔㻵㼚㼏㼛㼚㼑㼘㻕 0.6
0.6
0.4 +RRS6WHHO (c)
㻰㼞㼛㼜㼘㼑㼠 0.2 5
0.0
,QQHU70 .
㻜㻚㻢㻌㼙㼙
0.2 6 7 8 9 10 11
㻝㻚㻞㻌㼙㼙
0.4
+RRS6WHHO 300
0.6
Fig. 3 Effect of the melting temperature at the inner part

on the wire melting behavior (I = 280 A).
㻻㼡㼠㼑㼞㻌㼔㼛㼛㼜㻌㻔㻿㼠㼑㼑㼘㻕 Next, we show the effect of the specific heat. We
Fig. 2 Cross-section of CHS wire and welding behavior changed the specific heat at the inner part. Figure 4 shows
of Ar-MIG welding. the results. The result of Inconel-Steel CHS wire is shown
* National Institute for Materials Science, Tsukuba, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
349
Development of pure Ar–MIG welding
Distance from contact tip LC (mm) Table 1 Design guide of CHS wire.
0.6
0.4 +RRS6WHHO (a) Melting Thermal
(K) Specific heat
0.2
0.0
Inner (CInconel X2)
㻌㻌 1700 temperature conductivity
0.2 15 16 17 18
0.4
+RRS6WHHO Inner part Low Small Large
0.6
0.6 Outer part High Large Small

0.4 +RRS6WHHO 㻌 (b)
0.2 Inconel (CInconel )
0.0 1000 Temperature T (Co) Temperature T (Co)
0.2 8 9 10 11 12 13
1400 0 500 1000 1500 0 500 1000 1500
0.4
+RRS6WHHO 㻌 400
Thermal conductivity O (W䡡m/K)

Specific heat C (J/kg/K)
0.6 1200
0.6 300
Cu
0.4 +RRS6WHHO 㻌 (c) 1000
0.2
Inner (CInconel /2) 800
Steel
FeFe
0.0 200 Cu
㻌
㻌
0.2 5 6 7 8 9 10 Ti
0.4
+RRS6WHHO 㻌 300
600
Ti Fe
Steel
0.6 400
Cu
Cu 100
Fe
Ti
Fig. 4 Effect of the specific heat at the inner part on the 200
0
Ti
500 1000 1500 2000 500 1000 1500 2000
wire melting behavior (I =280 A). Temperature T (K) Temperature T (K)
Distance from contact tip LC (mm) (a) Specific heat (b) Thermal conductivity
0.6
800 Fig. 6 Material properties of Cu, Steel and Ti.
0.4 +RRS6WHHO K (a) (K)
0.2
0.0
Inner (䃚Inconel X2)
㻌 1700 which are satisfied with design guide. Three materials (Cu,
0.2 8 9 10 11 12 13 Steel and Ti) are used. The melting temperature of Cu,
0.4
+RRS6WHHO 800
K
Steel and Ti are 1356 K, 1773 K and 1958 K, respectively.
0.6
0.6
+RRS6WHHO 800
(b)
Specific heat and thermal conductivity are shown in Fig. 6.
0.4 K 㻌
0.2
Inconel (䃚Inconel )
To shorten the CLM, we selected the Cu for the inner part
0.0
0.2 8 9 10 11 12 13
1000 materials because of following reasons. (i) Melting
0.4
0.6
+RRS6WHHO 800
K 㻌 temperature is low, (ii) Specific heat is small, (iii) Thermal
0.6
800
conductivity is large. The outer part is Ti or Steel. The
+RRS6WHHO 㻌
0.4
0.2
K (c) melting temperatures of both materials are higher than that
Inner (䃚Inconel /2)
0.0 of Cu. The specific heat of steel is larger than that of Ti.
0.2 8 9 10 11 12
0.4
+RRS6WHHO K 㻌 300 Thermal conductivities of both materials are almost same
800
0.6
level. The effect of specific heat is larger than that of
Fig. 5 Effect of the thermal conductivity at the inner part thermal conductivity. Therefore, we select steel for the
on the wire melting behavior (I = 280 A). outer part.
in Fig. 4(b). The specific heat at the inner part was set to In order to investigate wire melting behavior, the
twice the specific heat of Inconel (Fig. 4(a)). The wire tip simulation was carried out. The result is shown in Fig. 7.
shows the convex shape. The CLM is made easily because The wire tip showed concave shape. So a long CLM was
the inner part becomes long. In contrast, the specific heat at not made in this Cu-Steel CHS wire.
the inner part was set in half of the specific heat of Inconel Fig.7
(Fig. 4(c)). The CLM is not made because the wire tip Distance from contact tip Lc (mm)
shows the trapezoidal shape. It is effective to use the small 㻜㻚㻢 (K)
specific heat materials at the inner part to shorten the CLM. 㻜㻚㻠㻿㼠㼑㼑㼘
1700
Last, we show the effect of thermal conductivity. We 㻜㻚㻞
㻯㼡
changed the thermal conductivity at the inner part. Figure 5 㻜㻚㻜
1000
㻜㻚㻞㻞㻝㻞㻞㻞㻟
shows the results. The result of Inconel-Steel CHS wire is
㻜㻚㻠
shown in Fig. 5(b). The thermal conductivity at the inner 㻜㻚㻢
㻿㼠㼑㼑㼘
300
part was set to twice the thermal conductivity of Inconel
(Fig. 5(a)). The thermal conductivity at the inner part was Fig. 7 Simulation of Cu-Steel CHS wire (I = 280 A).
set in half of the thermal conductivity of Inconel (Fig. 5
(c)).The tip shape shown in Fig. 5(a) is round. However,
the tip of shape shown in Fig. 5(c) is sharp, and the CLM is Steel
made easily because the inner part becomes long. The

Cu
influence of thermal conductivity is not large, compared to
the melting temperature and thermal conductivity. 1.0mm
3. Design guide to develop the CHS wire

In order to shorten the CLM in Ar-MIG welding, we (a) Welding behavior (b) Longitudinal section of wire
must select appropriate materials for the inner part and the Fig. 8 Welding result of Cu-Steel CHS wire (I =291 A).
outer part. Then, we propose the design guide shown in
Table 1. To develop a new CHS wire, we choose materials
350
We made Cu-Steel CHS wire to confirm the design melting temperature and thermal conductivity.
guide of the CHS wire. The welding behavior is shown in (3)The design guide for CHS wire is developed, and we
Fig. 8(a). The CLM did not occur and stable welding was demonstrate the effectiveness of design guide by the
possible. Fig. 8(b) shows longitudinal section of wire after simulation and the Ar-MIG welding.
the welding. The amount of melting at center the part was
large. References
Fig. 8 [1] T. Nakamura and K. Hiraoka: IIW Doc.212-1080-05, (2005).
4. Conclusions [2] T. Nakamura, K. Hiraoka and S. Zenitani: Science Technology
(1)The melting temperature and the specific heat have a Welding and Joining, 2008, 13 (1), 25-32.
[3] S. Zenitani, T. Nakamura and K. Hiraoka: Quarterly Journal of
large influence on the wire tip shape, the wire melting the JWS, 2007, 25, (1), 187-195.
rate and generation of CLM [4] T. Nakamura and K. Hiraoka: Welding in the Word, 2009, 53,
(2)The thermal conductivity has an influence on the wire 7/8, R158-R165.
tip shape, but the influence is small, compared to the
351
Newly developed novel transparent conductor of Mg(OH)2-C

compounds†
KUJI Toshiro*
KEY WORDS: (Mg-hydroxide) (Optical transparent) (Electric conductivity) (Sputtering deposition)

(Mg-C composite)
1. Introduction turned in front of the target at 60 rpm. The targets of

Kondoh’s group has recently reported very interesting magnesium and carbon disks were placed on each cathode
results on transparent Mg-C compounds [1]. The structure with the magnetron. Both of the disk shaped targets were a
of compounds was identified to be amorphous. The diameter of 3 inch., and purity was 99 %.The electric power
elemental composition was controlled by magnesium densities applied to each cathode where the film is >90%
content in films. Colored glassy films were obtained. for the visible light (380-780 nm), which is excellent even
Our research group has studied on synthesizing Mg compared with practical ITO(Indium Tin Oxide).Closely
based alloys by Mechanical Alloying (MA) and their controlled from 23 to 26 kW/m2 and from 73 to 100 kW/m2,
properties, i.e., hydrogen solubility in the non-equilibrium respectively.
and/or meta-stable phases [2,3]. From our series of works,
it has been demonstrated that even immiscible elemental
Figure 1 shows an appearance of as-sputtered Mg80-
couples could be alloyed by accumulating the excess
C20 black film and the film after exposing in air for an
mechanical energy created during the MA process. Mg-C
appropriate period. We can see excellent and clear
couple is the case , according to equilibrium phase diagram
transparency after exposing in the air at 298K and 80% of
[4,5].
humidity. We can see clearly our university logo placed
In this study, we will propose a newly developed
behind the Mg(OH) 2 -C film and glass substrate (Fig. 1(b) ).
compound composed of elements of Mg-C-O-H with the
potential high transparency and electro conductivity. In
order to obtain the transparency without loosing electro
conductivity, the material was synthesized by two steps
including alloying of Mg-C by magnetron co-sputtering and
post- reaction of the film with moisture in the air. It was
found that the compound has a Brucite type hexagonal (a) (b)
structure of Mg(OH) 2 -C.
Fig. 1 Appearance of (a) as-sputtered, (b) after post-
From our literature survey, it was concluded that
reaction.
transparent conductive materials are metal oxides without
exception. In this paper, the transparent and electro
Diffraction pattern of as -sputtered Mg-C film includes
conductive properties of non-oxide material, Mg(OH) 2 -C
peaks from some unidentified peaks. As-sputtered Mg-C
will be demonstrated.
film showed a diffraction pattern which was not identified
2. Experimental with peaks from either C or Mg. Unfortunately the phase
The film samples were made on glass substrates using from these limited peaks could not be identified. However,
an RF-sputtering apparatus made in ANELVA, SPC-350. It can be concluded that a Mg-C new phase was formed
The depositions of Mg-C thin films were performed at although the crystal symmetry was not be identified [11].
temperature of from 297 to 320 K in a pressure of 0.5 Pa The XRD diffraction peaks from the transparent film were
during the Ar process gas. The substrate used for well fitted to those from Mg(OH) 2 , but the lattice was
experiment was made in Corning #7059 with size of 25 mm slightly elongated along the hexagonal c-axis due to the
square. The substrates were set on the holder, and it was existence of C atoms in the Mg(OH)2 lattice [6], There are

* Department of applied chemistry, Tokai university Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
352
Newly developed novel transparent conductor of Mg(OH)2-C compounds
However, Rietveld’s analysis of XRD pattern indicated that

this is not the case, On the other hand, In the case that a half
of H atoms are hypothetically replaced by C atoms, XRD
peak pattern should be fitted well, implying that C was not
segregated in the boundary of Mg(OH) 2 grains and formed
Mg(OH) 2 -C compound as shown in Fig. 2. This was
confirmed from EPMA elemental mapping for Mg ,O and C.
Any segregation of C in the film morphology during the
process of black Mg-C film to transparent Mg(OH) 2 -C did
not occur.
Figure 3 shows the optical transmittance of the film
with wavelength. It can be seen that the optical
Fig. 2 Lattice image of Mg(OH) 2 .
transmittance of the film is >80% for the visible light (380-
780 nm), which is excellent even compared with practical
㻌
100 ITO.
The electric resistance of the transparent films shown in
80 Fig.4. The resistance of MgC black film increased with
loosing the color gradually with time after exposing it in the
Transmittance ( % )
60 Mg(OH0.87C0.13)2
air [6]. Then the variation in resistance somewhat fat with
Mg(OH0.67C0.33)2 time when the film became almost transparent, although
C
㻌
40 increasing still exists with time. The resistivity is strong

dependent upon the C composition in the film as shown in
20
Fig. 4. The Electric resistivity of the transparent film was
order of the 10-2 ȍFP )RU SUDFWLFDO XVHV ZH QHHG RQH
0
order lower value of resistivity of the film, which is 10-3
400 600 800 1000 ȍFP ZKLFK LV LPSRUWDQW SUHVHQW ZRUN PDGH HIIRUW LQ RXU
Wavelength, O ( nm ) group because of opening wide applications for our
Mg(OH) 2 -C film.
Fig. 3 Transmittance spectra of the films.
4. Conclusions
㻌 In this work, New Mg-C crystalline phase was
successively prepared by co-sputtering of Mg and C. The
Mg(OH0.87C0.13)2 Mg-C black film became transparent with time after air
100
exposing for an appropriate time. This transparency
Resistivity, ( : cm )
behavior was yielded by the reaction of Mg-C with

10-1 moisture in the air. Consequently, C atoms were distributed
in the Mg(OH) 2 crystal grain. i.e., Mg(OH) 2 -C. This film
㻌
Mg(OH0.67C0.33)2 had excellent optical transmittance for the visible light and
10-2 again excellent low electric resistance of the order of 10-
2
ȍFP,QFRQFOXVLRQZHKDYHVXFFHVVLYHO\GHYHORSHGa new
transparent conductor of Mg(OH) 2 -C except metal oxides.
10-3
0 1k 2k 3k 4k 5k
Time, T ( sec ) References
[1] K. Kondoh, T. Serikawa, K. Kawabata, and T. Yamaguchi,
Scriprta Materialia 57, 489 (2007).
Fig. 4 Resistivity of the samples. [2] T. Nobuki and T. Kuji, J. Adv. Sci. 19 (2007) 11-15.
possible two types of C atoms in the in the Mg(OH) 2 -C [3] M. Abe, and T. Kuji, J. Alloys Comp. 446–447 (2007) 200-
203.
lattice, i.e., substitution or interstitial type. As mentioned [4] T. Honjo, T. Nobuki, M. Chiba and T.Kuji, J. Japan Inst.
above, there are many interstitial sites large enough for C Metals 72 (2008) 780-784.
atoms to stay in the lattice of Mg(OH) 2 . However, if [5] Legkaya T.N., SOVIET JOURNAL OF SUPERHARD
electrically neutral C atoms stay in interstitial sites. MATERIALS 12 (1990) 1-5.
[6] T. Kuji, T. Honjo, M. Chiba, T. Nobuki and J.-C. Crivello, e-J.
Mg(OH) 2 -C should not be semi-conductor. We first Surf. Sci. Nanotech. 6 (2008) 15-16.
hypothesized the case that neutral C atoms stay in (0,0,1/2).
353
Phase transformation at interface using femtosecond laser

†
irradiation
KANEHIRA Shingo*, NISHIMURA Masakazu**, MIURA Kiyotaka**,
and HIRAO Kazuyuki**
KEY WORDS : (Femtosecond laser) (Thin film) (Interface) (Phase transformation)
1. Introduction prepared using a radio-frequency (rf) sputtering method

Interfaces in solids indicate very small areas with (ULVAC RFS-200). Fe (99.9%, Kojundo Chemistry) and
nanometer scales such as grain boundaries between internal Si (99.999%, Kojundo Chemistry) powders with a mole
solids, and they usually decide or dominate the mechanical, ratio of 1 : 2 were mixed using an alumina mortar for 30
thermal, and optical properties of the bulk material. minutes. Next, the mixture was compacted to use as a
Recently, high-resolution TEM provides much information target for the rf sputtering. A non-dope silicon (100) single
about interfaces and reveals the mechanism of additives, crystal or fused silica substrate with the dimensions of
mainly rare-earth elements, for an improvement of strength. 10u10u1 mm3 was mounted parallel to the target at a
The development of controlling the interface is one of the distance of 30 mm, and the thin amorphous Fe-Si film was
crucial subjects in material processing. deposited on each substrate under the following
The femtosecond laser has been widely used in material conditions : the RF power was 100W, the sputtering gas
processing because of its ability to suppress thermal was 100% Ar, and the sputtering pressure was 30mTorr at
damages and to form refractive index changes near the room temperature. The thickness of the prepared film was
focal point. It is possible to fabricate and modify various evaluated using a surface roughness meter (KLA Tencor,
nanostructures inside transparent materials using P-15).
multiphoton absorption at the focus due to the extremely A regeneratively amplified mode-locked Ti:sapphire
high-intensity of the laser pulses. It has previously been laser operating at a wavelength of 800nm (RegA 9000,
reported that refractive index changes at the focus inside Coherent), with a 120fs pulse width, 200 ࠥ 250kHz
glass was approximately 10-4 to 10-3, depending on the repetition rate was used as a light source in this experiment.
laser irradiation condition. We have been developing laser The fabricated Fe-Si thin film sample was fixed on an
processing to form sub-micro holes [1] and for defect x-y-z stepping motor stage and the laser beam with a
control [2] using the laser. To utilize the increase of diameter of ~3mm was focused on the film in air through a
temperature and pressure in a very short time enables us to 10u objective lens with a numerical aperture of 0.3. We
reform the ion distribution inside the glass. [3] confirmed that oxidation did not occur in the laser
Here, we tried to control the phase transformation of irradiation in air from XRD analysis. The pulse energy at
Fe-Si thin film or interfaces between the film and a the sample location was precisely controlled using a
substrate using femtosecond laser irradiation. [4] In neutral density filter between 0.25 and 1.5 PJ. The sample
addition, silicon deposition at the interface was also was scanned at different speeds (250-600Pm/sec) along a
demonstrated using the photo reaction between Al thin film horizontal direction, perpendicular to the incident laser
beam, and the scanning process was repeated many times
and a glass substrate with the assistance of the laser pulses.
The composition and the surface of the reacted area were to form a square photomodified area with the dimensions
evaluated using SEM, TEM, XRD, and confocal Raman of 10u10 mm2 in order to carry out the various analysis
spectroscopy. described below. The chemical composition of the
photomodified area was analyzed using X-ray diffraction
2. Experimental procedure (XRD) under CuKa radiation (Rigaku RINT2500) in order
Fe-Si amorphous thin film with a thickness >2Pm was to verify the phase transformation in the film. The
* Society-Academia Collaboration for innovation, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
Kyoto University, Kyoto, Japan
** Department of Material Chemistry, Graduate School of
Engineering, Kyoto, Kyoto University
354
Phase transformation at interface using femtosecond laser irradiation
microstructure of the photomodified surface area was crystalline Fe x Si y compounds formed by the laser
observed using a scanning electron microscope (SEM : irradiation. In the phase diagram of a Fe-Si binary system,
Hitachi S2600N). The atomic distribution at the stoichiometric E-FeSi 2 is composed of 68at.% Fe and
photomodified area was also analyzed using electron probe 32at.% Si. The E-FeSi 2 phase easily transforms into D
micro analysis (EPMA, JEOL, JSM-8000). FeSi 2 and Ȝ-FeSi phases by heat treatment at over 1255K.
We confirmed that our amorphous thin film transformed
3. Results and discussions into E-FeSi 2 phase by heat treatment at 1123K for 6 hours,
Figure 1 shows SEM and the mixture of D- FeSi 2 andȜ-FeSi at 1373K. In Fig.
photographs of the 2(a), no peaks corresponding to the E-FeSi 2 phase existed,
surface of Fe–Si thin film presumably due to the decomposition of E-FeSi 2 during the
before (a) and after (b) excess laser exposure.
the femtosecond laser Fig. 2(b) shows XRD patterns of the Fe-Si thin film
irradiation with a pulse before (i) and after the laser irradiation with different
energy of 1.5PJ. The scanning speeds of (ii)250Pm/sec., (iii)450Pm/sec., and
Fe-Si compound has a (iv)600Pm/sec., respectively. The pulse energy of the laser
Fig.1. SEM photos of Fe-Si
thin film before (a) and after band gap of ~ 0.85eV beam was set to 1.5PJ in all cases. When the scanning
(b) the laser irradiation. and high optical speed was set to 250Pm/sec., both the D-FeSi 2 andȜ-FeSi
absorption, therefore, the phases were observed at the photomodified area.
film would sufficiently absorb the incident laser beam. However, when the scanning speed increased to above
When the laser pulses were focused on the film, the focal 450Pm/sec., their peak intensity decreased and the E-FeSi 2
spot of the laser beam was illuminated, and a dispersion of phase appeared instead. The fast laser scanning at above
white particles less than 600Pm/sec. could form almost the single E-FeSi 2
~3Pm in diameter was polycrystalline phase. Therefore, the phase transformation
observed around the strongly depends on the scanning speed and pulse energy
scanning area as in the Fe-Si system.
indicated in this photo. The initial temperature at the focus is important for the
Figure 2(a) indicates ultrafast crystallization using the laser pulses. The scanning
XRD patterns of the speed is one of the important parameters in the
Fe-Si thin film crystallization of Fe-Si thin films to control cooling or
(i)as-deposited, and after heating rate around the focus. In general, when the
the laser exposure with a femtosecond laser beam is focused inside solids, not only
different pulse energy of the generation of shock wave but also heat accumulation
(ii) 0.25PJ, (iii) 0.75PJ, occurs around the focal point, resulting in the formation of
and (iv)1.5PJ, ion diffusion or refractive index change with a circular
respectively.The scanning shape after the laser irradiation. The effect depends on the
speed of the sample was temperature cooling rate: if the cooling rate is low, the
set to 250Pm/sec. The effect tends to occur around the focal area. We have
exposed area was calculated the cooling rate near the focal point in the case
apparently crystallized of the laser irradiation on FeSi 2 thin film by solving the
and two phases ascribed thermal diffusion equation. The rate is calculated to ~1012
to D-FeSi 2 and Ȝ-FeSi K/s, which is much faster than that of the commercial glass
phases were identified in sample (~ 108 K/s), due to its large thermal diffusivity (D th:
the XRD spectra. In FeSi = 0.65) rather than that of glass sample (D th:glass =
-6
addition, the crystallinity 0.46u10 ). Therefore, we can estimate that the focal
Fig. 2. (a)XRD patterns of the
of these phases temperature increases dramatically and relaxes to room
Fe-Si thin film after the laser
irradiation with different pulse improved as the pulse temperature before the next pulse arrives. The phase
energy;(i)as-deposited, energy of the laser transformation completed in a very short time before the
(ii)0.25PJ, (iii)0.75PJ, and pulses increased, heat accumulated.
(iv)1.5PJ, respectively. (b) XRD
patterns of the film after the laser especially in the case of
4. Conclusion
irradiation at different scanning 1.5PJ. The white
speeds;(i)as-deposited, Phase transformation in amorphous Fe-Si film was
particles shown in Fig.
(ii)250Pm/sec., (iii)450Pm/sec., demonstrated using femtosecond laser irradiation. The
and (iv)600Pm/sec., respectively. 1(b) were due to the
formation of D-FeSi 2 , E-FeSi 2 andȜ-FeSi depended on
355
the focal energy from the laser : the moderate irradiation 5. References
[1] S. Kanehira, J. Si, J. Qiu, K. Fujita, and K. Hirao, Nano Lett.,
tends to form the E-FeSi 2 phase. To control the photon
5(2005), 1591.
energy will open up the various photo-reactions at the [2] S. Kanehira, K. Miura, K. Fujita, K. Hirao, J. Si, N. Shibata,
interface. and Y. Ikuhara, Appl. Phys. Lett., 90(2007), 163110.
[3] S. Kanehira, K. Miura, and K. Hirao, Appl. Phys. Lett., 93
(2008), 023112.
[4] S. Kanehira, M. Eida, M. Sakakura, Y. Shimotsuma, K. Miura,
and K. Hirao, Appl. Phys. A (in printing, 2010).
356
Laser Micro-machinability of electric field-assisted ion-exchanged

†
glass
MATSUSAKA Souta*, TSUKAMOTO Masahiro**, ABE Nobuyuki**

and WATANABE Takehiro*
KEY WORDS: (Ion-exchange) (Borosilicate glass) (Metal nanoclusters) (UV nanosecond laser)
ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ (Micro-machining)
1. Introduction profiles of processed holes were examined by scanning

Glass materials are so brittle and transparent that laser electron microscope (SEM, JEOL, JSM-840A) and
micro-machining of these materials has various difficulties confocal laser scanning microscope (Keyence, VK-8500),
in processing quality. Therefore, some studies on the respectively.
development of laser-machinable glass have been carried
out [1-5]. Typical laser-machinable glass was prepared by 3. Results and Discussion
ion-exchange process in molten salt bath which contained Figure 1 shows the change in penetration depth of
silver [1,2,4,5] or copper ions [4]. However, the copper ions with exchange time. For the purpose of
conventional method was only applicable to glass materials comparison, in this figure, the penetration depth of silver
containing large amount of alkali ions such as lime-sodium ions in borosilicate glass prepared in molten salt bath of
glass, because the process was driven by the substitution 1.0%AgNO 3 -NaNO 3 at 623 K is also shown (sample E).
between alkali and metal ions at the glass surface. As shown in Fig. 1, the penetration depth of sample D was
In this report, a fabrication method of laser-machinable approximately three times larger than that of sample E,
glass by electric field-assisted ion-exchange (FAIE) is although the ionic diffusion coefficient of copper in glass
proposed. In FAIE process, metal ions are supplied from was smaller than that of silver [6]. Between sample D and E,
metal foil or film placed on the glass surface by applied DC in addition, the cross-sectional profiles of ions were so
voltage. Because the process is electrostatically driven, different, as shown in Fig. 2. In sample D, copper ions were
more rapid and deeper metal penetration will be available. uniformly distributed over the exchanged area, in contrast
Here, the laser-machinability of copper-containing to silver ions in sample E. In the literature [5], it was shown
borosilicate glass by FAIE process was experimentally that the laser ablation rate (removed depth per laser shot) of
investigated. silver-sodium ion-exchanged glass gradually decreased with
the dilution of silver ion concentration. Therefore, it was
2. Experimental expected that glasses prepared by FAIE kept constant
Borosilicate glass slide (Schott, BOROFLOAT, 25 mm ablation rates over exchanged areas.
x 25 mm x 1.1 mm) and pure copper foil (> 99.9 %, 20 mm Figure 3(a)-(e) show SEM micrographs of laser-ablated
x 20 mm x 10 Pm) were used in the experiment. These were square-holes on un-exchanged (sample R) and ion-
placed between two copper electrodes in a high vacuum exchanged (sample D) glasses, when the laser power was
chamber (< 10-3 Pa). After the evacuation and temperature 5.0 J/cm2. The cross-sectional profiles of these holes are
elevation, DC voltage was applied with copper foil as shown in Fig. 3(f). As shown in Fig. 3(a), many micro-pits
anode. The ion-exchange conditions are shown in Table 1. Table 1 Ion-exchange
The cross-sectional distributions of copper ions were di i
measured by electron probe micro-analyzer (EPMAJEOL, Sample Applied voltage (V) Temperature (K) Time (ks)
JXA8900).
A 1.8
The laser micro-machining system consisted of a fourth
B 3.6
harmonic Nd:YAG laser oscillator (Continuum, Surelite I- 100 623
C 10.8
20) and PC-controlled translation stage. Pulse duration of
D 21.6
the laser beam was 6 ns. All samples were irradiated on the
front surfaces through the stainless steel mask (100 Pm x R Un-exchanged borosilicate glass
100 Pm) by a defocused laser beam. The shapes and
* Graduate School, Chiba University, Chiba, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
357
Laser Micro-machinability of electric field-assisted ion-exchanged glass
Glass surface
Cu (a) Sample D
Intensity (arb. unit)

(b) Sample E
Ag
0 20 40
Fig. 1 Change in penetration depth of copper ions with ion- Penetration depth (Pm)
exchange time. Sample E was prepared by
conventional ion-exchange method in molten salt Fig. 2 Comparison of ion distribution profiles in glasses
bath of 1.0%AgNO3-NaNO3 at 623 K. prepared by (a) FAIE (sample D) and (b)
conventional ion-exchange (sample E).
(a) 10 shot on as-received glass (b) 20 shot on as-received glass (c) 80 shot on Cu-doped glass
1' 2' 3'

1 3
2
(d) 100 shot on Cu-doped glass (e) 120 shot on Cu-doped glass (f) 1 1'
2 2'
3 3'
4' 5' 22.2 Pm
4 4'
4 5 27.4 Pm
5 5'
59.4 Pm
50 Pm
50 Pm
Fig. 3 SEM photographs of laser-ablated square holes formed on as-received and Cu-doped glasses. (a) 10 shot and (b) 20 shot
irradiation of as-received glass; (c) 80 shot, (d) 100 shot and (e) 120 shot irradiation of Cu-doped glass. The cross-sectional
profiles of (a–e) are shown in (f). The laser power was 5.0 J/cm2.
were observed at the processed surface after 10 pulses ripple patterns formed by diffracted laser light were
irradiation on sample R. And the processed hole was observed at hole bottoms. These results suggested that the
seriously damaged even by 20 pulses irradiation (Fig. 3(b)). input energy was effectively absorbed in copper-containing
Many large (-50 Pm) chippings occurred at ablated edges, region and rapid ablation of surface layers occurred.
and irregular-shaped and porous structures appeared at the However, the flat bottom face was drastically damaged by
hole bottom. Although the formation mechanism of these 120 pulses irradiation, as shown in Fig. 3(e). Although the
structures was still unknown, it was assumed that micro-pits sharp ablated edge was maintained, the irregular-shaped
formed by multiple laser irradiation played absorption and porus structure, which was very similar to that observed
centers of laser beams and accelerated the generation of on sample R, appeared at hole bottom. As shown in Fig. 3
larger chippings. On the other hand, such defects or (f), the removed depth by 100 pulses irradiation was 27.4
structures were not observed in 80 and 100 pulses irradiated Pm and this value was close to the penetration depth of
holes on sample D (Fig. 3(c) and (d)). Both of these holes copper ions in sample D (see Fig. 1). It was assumed,
had extremely flat hole bottoms, sharp ablated edges and therefore, that the laser machinability degraded at 120
small heat affected zones around the holes, although faint pulses irradiation because the hole bottom reached a non-
358
copper-containing region. In addition, the ablation rates was necessary for the high-accuracy fabrication of micro-
calculated from hole depths by 80, 100 pulses irradiations components. Numerical prediction of ion behavior will be a
were 0.278 (0 - 80) and 0.260 Pm/pulse (80 - 100 pulses). prospective method for this purpose. The effects of other
These values indicated that the copper-containing region metal ions in glasses on optical characteristics and laser-
formed by FAIE had constant ablation rate over exchanged machinabilities will be presented in our future work.
area.
References
4. Conclusions [1] K. Tsunetomo, T. Koyama: Opt. Let., 22 (1997) 411.
[2] T. Koyama, K. Tsunetomo, Jpn. J. Appl. Phys., 36 (1997)
In this report, an improvement method of laser-
L244.
machinability of borosilicate glass by electric field-assisted [3] M. Shojiya, H. Koyo, K. Tsunetomo, Proc. SPIE, 5063 (2003)
solid-state ion-exchange was proposed. Experimental 124.
results showed that the ion-exchanged copper-containing [4] M. Rosenbluh, I. Antonov, D. Ianets, Y. Kaganovskii, A. A.
region had the excellent laser machinability. However, the Lipovskii, Opt. Mater., 24 (2003) 401.
processing quality suddenly deteriorated when the removed [5] S. Matsusaka, T. Watanabe, J. Mat. Proc. Tech., 202 (2008)
depth exceeded the penetration depth of copper ions. 514.
Therefore, well-designed and controlled ion distribution [6] R. Oven, J. Appl. Phys., 101, (2008) 113113.
359
Dynamic mechanical behavior of Sn-Ag-Cu lead-free solders by

†
tensile test under high strain rate
YASUDA Kiyokazu *, SAKINO Yoshihiro **, SHOHJI Ikuo *** , TAKEMOTO Tadashi **
KEY WORDS: (Lead-free solder) (Tensile test) (Strain rate sensitivity) (High strain rate) (Sn-Ag-Cu)
(Ductility) (Rupture) (Stress-strain curve) (Tensile strength) (Yielding point)
1. Introduction maximum cross head speed: 1200mm/s, stroke: 500mm).

The high acceleration vibration or the impact shock During tensile loading the deformation of a test rod was
environment of various electronic components inevitably observed by the dynamic analysis system equipped with
causes the exposure to high strain rates and the severe high speed CCD camera (Keyence VW-6000). The
deformation of micro interconnects. Most lead-free mechanical parameters such as the tensile strength and the
solders are harder compared to the conventional Sn-Pb break elongation were evaluated. The UTS (ultimate tensile
eutectic solder and have lower elongation properties. For strength) and the rupture elongation were compared with
this reason, it has been pointed out that the drop impact those of the normal tensile test results (1.610-3 s-1). The
resistance of mobile devices deteriorates. Nevertheless, few fracture surfaces were observed by an optical microscope.
cases were studied in detail for high-speed impact
deformation of the solder [1]. Considering the future 3. Results and Discussion
situation that more electronics would be used under high Typical fracture surfaces of Sn-Ag-Cu lead-free solder
acceleration shock conditions, and that the type and amount alloys by optical microscope observation are shown in Fig.
of automotive electronics would increase, knowing exactly 1. In these photographs Sn-Ag-Cu lead-free solder alloys
the tensile behavior of lead-free solder at high-speed impact revealed ductile failures of cup and cone rupture in any
can be used for analyzing the impact corruption of lead-free
solder joints. It is expected that useful information for the
design of long life lead-free solder joints against destructive
impact can be obtained.
In this study, therefore, for several lead-free solders,
high strain rate tensile tests were carried out over three
orders of magnitude faster than the rate of the tensile test in
the former study [2][3], in particular, including additional
low silver content solder (Sn-1Ag-0.7Cu) which has been
frequently used recently due to its cost advantages. We
aimed to clarify the differences from traditional tensile
6Q$J&X 6Q$J&X
behavior and the deformation characteristics of lead-free
solder.
2. Experimental
From the fundamental physical point of view, the
mechanical properties of Sn-Ag-Cu solders (Ag content 1.0
- 4.0 vol %, Cu content 0.5-1.0 vol %) were investigated
using a high speed universal tensile test machine in the high
strain rate range (1.610-3s-1 1.6101 s-1). Cylindrical
test rods (diameter: 10mm, gauge length: 50mm) were
provided for the tensile tests according to the testing
method described in JIS Z 3198-2 adopted so far for the 6Q$J&X 6Q$J&X
normal tensile test [4]. For Sn-Ag-Cu based lead-free solder
alloys, mechanical properties were evaluated by a uniaxial Fig. 1 Macroscopic fracture observation of lead-free
tensile test method by using the ultra-dynamic structural solder after high-strain-rate tensile test (specimen
testing system (maximum dynamic load: 1,200 kN, diameter: 10mm, strain rate: 1.6ᶣ101 s-1).

* Graduate School, Nagoya University, Nagoya, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
*** Graduate School, Gunma University, Kiryu, Japan
360
Dynamic mechanical behavior of Sn-Ag-Cu lead-free solders by tensile test under high strain rate
Load (kN) shape, though the cross-sectional area of breakage tends to

1000 increase. As for the hypereutectic alloy of Sn-4Ag-0.9Cu,
the fracture area was larger than those of the former eutectic
alloys, the macroscopic shape of the breakage showed the
800 peripheral cleavage. On the other hand, the hypoeutectic
alloy of Sn-1Ag-0.7Cu was intermediately ductile. The the
fracture area had almost 45 degree angles to the tensile
600
direction.
ᴾ ᴾ Figure 2 shows the typical load – elongation curve of
400 the eutectic alloy Sn-3Ag-0.5Cu in the case of the high
strain rate (strain rate: 1.6ᶣ101 s-1). Since the strain rate
200 is so high, even the ductile eutectic alloy exhibited a linear
(elastic) region before the yielding point which was not
observed under the low strain rate due to the creep
0 phenomena.
Figure 3 shows the tensile strength and fracture
elongation of high-strain-rate tensile testing of Sn-Ag-Cu
20 30 40 50 60 lead-free solders. The top line of the horizontal axis
Elongation (mm) indicates the strain rate for each alloy composition. Tensile
strength increased more than twice as compared to the
Fig. 2 Load – elongation curve of Sn-3Ag-0.5Cu standard static tensile tests (strain rate: 1.6ᶣ10-3 s-1) in all
under the high strain rate (strain rate: 1.6ᶣ101 s-1). alloy compositions. As for the fracture elongation, on the
contrary, the strain rate dependence was obscure regardless
of the alloy composition.
4. Conclusions
Tensile tests under high strain rates of 1.6ᶣ100 s-1to 1.6
ᶣ 101 s-1 were performed for the evaluation of the
mechanical properties of several kinds of Sn-Ag-Cu lead-
free solders. All Sn-Ag-Cu alloys showed ductile fractures.
Eutectic composition revealed the highest strength under
the high strain rate conditions. The tensile strength
increased by 200-300 % compared to the value of the static
tensile conditions at a typical strain rate of 1.6ᶣ10-3 s-1. It
was found that the load-elongation curve of each lead-free
solder exhibited a clear elastic deformation under the
highest strain rate of 1.6ᶣ101 s-1. The rupture elongation
did not show any clear dependence on the strain rate.
Acknowledgements
This study was originally started as a research project on
the testing of the mechanical properties of lead-free solders
in the Solder and Smart Joining Division of the Japan
Welding Engineering Society. The authors are grateful for
the support of the concerned division members.
References
Fig. 3 Tensile strength and elongation of lead-free [1] K. Kaminishi: Proc. 9th Symp. on Microjoining and Assembly
solder in high-speed tensile testing Technology in Electronics (2003) , pp.253-256.
[2] I. Shohji, T. Osawa, T. Matsuki, Y. Kariya, K. Yasuda, and T.
composition. Among those, for Sn-3Ag-0.5Cu known as the
Takemoto: Mater. Trans., 49 (2008), pp.1175-1179.
most commonly-used eutectic lead-free solder, the extent of [3] K. Yasuda, I. Shohji, and T. Takemoto: Mater. Science forum,
the necking was remarkable. The area of the fracture part 580-582 (2008), pp.221-224.
was very small. Similarly, another nearly eutectic lead free [4] T. Takemoto: Proc. 6th Electronic Packaging Technology
solder, Sn-3.5Ag-0.7Cu exhibited the sharp cup-and-cone (2005), pp.8-12
361
Oxide nanosheets and their assemblies for new ceramic joining and
†
smart processing
OSADA Minoru *,** and SASAKI Takayoshi *,**
KEY WORDS: (Oxide nanosheet) (Colloidal suspension) (Layer-by-layer assembly) (Ceramic joining)
(Smart process)
1. Introduction The formation of unilamellar nanosheets was confirmed

Two-dimensional (2D) nanosheets obtained via by direct observation with atomic force microscopy (AFM)
exfoliation of layered compounds have attracted intensive and transmission electron microscopy (TEM). Figure 2
research in recent years [1]. These 2D nanosheets, which depicts an AFM image for Ti0.91O2 nanosheet. This image
possess nanoscale dimensions only in thickness and have clearly reveals a sheet-like morphology, which is inherent
infinite length in the plane, are emerging as important new to the host layer in the parent compound. The thickness is
nanomaterials due to their unique properties. Research in ~1 nm, which is comparable to the crystallographic
such exotic 2D systems recently intensified as a result of thickness of the host layer in the corresponding parent
emerging progress in graphene (carbon nanosheet) [2] and compounds. This supports the formation of unilamellar
novel functionalities in transition-metal-oxide nanosheets nanosheets. Such an exfoliation process is quite general: the
[1]. In particular, oxide nanosheets are exceptionally rich in exfoliation of the other layered host compounds proceeds in
both structural diversity and electronic properties, with a similar fashion.
potential application in areas ranging from catalysis to
electronics. Now, by using of the exfoliation approach, it is
possible to investigate dozens of different 2D oxide
nanosheets in search of new phenomena and applications.
Here, we present the current status of research on oxide
nanosheets. Particular focus is placed on recent progress
that has been made in the synthesis, characterization and
Fig. 2 AFM image for Ti0.91O2 nanosheet on a Si substrate.
properties of oxide nanosheets, highlighting new ceramic
joining and smart processing for electronic applications.
3. Ceramic joining and smart processing using
2. Synthesis of functional nanosheets nanosheets
A variety of oxide nanosheets (such as Ti1-GO2, MnO2 One of the most important and attractive aspects of the
and perovskites) were synthesized by delaminating exfoliated nanosheets is that various nanostructures can be
appropriate layered precursors (Cs0.7Ti1.825Ƒ0.175O4, fabricated using them as 2D building blocks (Fig. 3) [1].
K0.45MnO2 and KCa2Nb3O10) into their molecular single Oxide nanosheets have an extremely high 2D anisotropy of
sheets (Fig. 1) [1]. the crystallites. In addition, these nanosheets are obtained
as negatively charged crystallites that are dispersed in a
colloidal suspension. These aspects make the nanosheets a
suitable building block for new ceramic joining technology
and smart processing of nanostructured films and advanced
nanodevices.
Fig. 3 Schematic illustration of ceramic joining and smart

Fig. 1 Structures of oxide nanosheets.
processing using nanosheets.

* International Center for Materials Nanoarchitectonics, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
National Institute for Materials Science, Tsukuba, Japan Japan
** CREST, JST, Tokyo, Japan
362
Oxide nanosheets and their assemblies for new ceramic joining and smart processing
One of the highlights is the fabrication of 4. Applicatioins to nanoelectronics

nanocomposite films of organic polymer/nanosheet LbL assembly of various nanosheets allows us to tailor
materials that exhibit useful properties. The electrostatic superlattices or heterostructures by tuning the number of
layer-by-layer (LbL) self-assembly via sequential nanosheets and their stacking sequences (Fig. 3) [6].
adsorption [3] and Langmuir-Blodgett (LB) procedure [4] Sophisticated functionalities or nanodevices may be
are effective for this purpose. Sequential LbL assembly, designed with LbL assemblies through the selection of
often called “molecular beaker epitaxy”, is one of the most nanosheets and combining materials, and precise control
powerful methods of fabricating nanostructured multilayer over their arrangement at the molecular scale. We utilized
films with precisely controlled composition, thickness and oxide nanosheets as a building block in a solution-based
architecture on a nanometer scale. Figure 4 depicts an bottom-up assembly, and successfully developed various
example of a multilayer film of perovskite nanosheets on a functional nanofilms such as high-k dielectrics [7-9], field
SrRuO3 substrate. This TEM image clearly reveals a effect transisters [1], ferromagnetic semiconductors [10,11],
stacking structure corresponding to the LbL assembly of magneto-optical films [6,12,13], resistance switching
nanosheets. memories [14], etc.
References
[1] M. Osada and T. Sasaki: J. Mater. Chem. 19, (2009), pp.
2503-2511.
[2] A. K. Geim and K. S. Novoselov: Nature Mater., 6, (2007), pp.
183-191.
[3] T. Sasaki, Y. Ebina, T. Tanaka, M. Harada, M. Watanabe and
G. Decher: Chem. Mater., 13, (2001), pp. 4661-4667.
[4] K. Akatsuka, M. Haga, Y. Ebina, M. Osada, K. Fukuda, T.
Sasaki: ACS Nano, 3, (2009), pp. 1097-1106.
[5] T. Shibata, K. Fukuda, Y. Ebina, T. Kogure and T. Sasaki:
Adv. Mater., 20, (2006), pp. 231-235.
[6] M. Osada, Y. Ebina, K. Takada, and T. Sasaki: Adv. Mater.,
18, (2006), pp. 295-299.
[7] M. Osada, Y. Ebina, H. Funakubo, S. Yokoyama, T. Kiguchi,
K. Takada and T. Sasaki: Adv. Mater., 18, (2006), pp. 1023-
1026.
[8] B-W. Li, M. Osada, T. C. Ozawa, R. Ma, K. Akatsuka, Y.
Fig. 4 Cross-sectional high-resolution TEM image of a 5-
Ebina, H. Funakubo, S. Ueda, K. Kobayashi and T. Sasaki: Jpn.
layer (7.5 nm thick) Ca2Nb3O10 film on a SrRuO3 substrate. J. Appl. Phys., 48, (2009), pp. 09KA15-1-5.
[9] M. Osada, K. Akatsuka, Y. Ebina, K. Ono, H. Funakubo, K.
A clear benefit of these LbL approaches is the interface Takada and T. Sasaki: ACS Nano, 4, (2010), pp.5225-5232.
engineering, which appears to be a key step in the design of [10] M. Osada, Y. Ebina, K. Fukuda, K. Ono, K. Takada, K.
film properties. Physical methods such as vapor deposition Yamaura, E. Takayama-Muromachi and T. Sasaki: Phys. Rev.
and laser ablation are currently the main methods of B, 73, (2006), pp. 153301-1-4.
fabricating oxide films. These techniques, however, usually [11] X-P. Dong, M. Osada, H. Ueda, Y. Ebina, Y. Kotani, K. Ono,
require a complex and difficult deposition process S. Ueda, K. Kobayashi, K. Takada and T. Sasaki: Chem.
involving high-temperature postannealing (>600°C), which Mater., 21, (2009), pp. 4366-4373.
can cause degradation in the film-substrate interface arising [12] M. Osada, M. Itose, Y. Ebina, K. Ono, S. Ueda, K.
Kobayashi and T. Sasaki:Appl. Phys. Lett., 92, (2008), pp.
from both nonstoichiometry and thermal stress. The
253110-1-3.
bottom-up fabrication using oxide nanosheets provides new [13] Z. Liu, R. Ma, M. Osada, N. Iyi, Y. Ebina, K. Takada and T.
opportunities for room-temperature fabrication of oxide Sasaki:J. Am. Chem. Soc., 128, (2006), pp. 4872-4880.
thin films, while eliminating integration problems [14] R. Ma, M. Osada, L. Hu, and T. Sasaki:Chem. Mater., 22,
encountered in current film-growth techniques. Such LbL (2010), in press.
assembly is also expected to have great potential for
advances in new ceramic joining technology.
363
Evaluation of magnetite and related iron compounds in the teeth of

†
chiton using X-ray and electron analyses
NUMAKO Chiya *, SATO Kazuyoshi **, ABE Hiroya and OHARA Satoshi ***
KEY WORDS: (Biogenic magnetite) (Radular teeth) (Chiton) (EPMA) (XRD) (XAFS) (Syncrotron radiation)
1. Introduction same as the organic framework. The color of posterior

Chitons are well known to have special strong radular edges turned into black with magnetite and the anterior
teeth accumulating 䢢 iron oxides, especially magnetite surface colored with gray abruptly at the 4th teeth low,
(Fe 3 O 4 ), and calcium phosphates as major components. which is starting point of the third maturation stage.
In the case of Japanese chiton Acanthopleura japonica, Abundance of the magnetite increased until 60th teeth and
about 80 pairs of the iron teeth (ca. 400 x 200 x 500 mm3) was kept until final stage on the radula. Other mineral
located on the radula with their maturation sequence which components appeared in the later maturation stages as
can be divided into five stages from their color variation. follows; small amount of goethite D-FeOOH) and
The teeth are colorless in the first stage, turn into reddish- lepidocrocite (J-FeOOH) were stored at the anterior surface
brown, gray, red, and black. The magnetite has been of the tooth at fourth stage with red color, and large amount
investigated in the previous studies, however, the formation of calcium phosphate partially crystallized into
mechanism of the magnetite in the maturation process of hydroxyapatite (Ca 10 (PO4) 6 (OH) 2 ) intruded and filled into
the teeth of chiton has not yet been elucidated. In this the anterior part of the tooth in final maturation stage.
study X-ray analyses, XRD and XAFS, and EM The composition and mechanical properties of the
observation were applied to the radular teeth of chiton to posterior and anterior part were indicated by EPMA and
elucidate the variations of mineral components, mechanical SEM observation. The major elemental components of
properties, and structure in their maturation process on the posterior and anterior part were Fe and (Ca + P)
radula. respectively. Their border was very clear and no cross-
boundary transfer of element could be observed.
[1]
[3] Structural features of both parts were not different and any
FP
Acanthopleura japonica
Photos. [1] Japanese chiton, Acanthopleura japonica,

[2] a radular teeth of the chiton (ca.20mm length),
[3] an optical microscopic image of teeth of
chiton
2. Result and Discussion

In the first stage of maturation, there was no mineral
component in the teeth but they are constructed with an
organic framework of chitin. A posterior edges of the
tooth, which is the main place for feeding were filled with Fig and Photos (a) Two dimensional Elemental Mapping for a
reddish-brown material containing iron (III) in the second tooth of chiton in the final maturation stage, (b)(c) SEM image of
stage, in about three teeth low. Their crystality were, secondary electron and reflected electron for the tooth, (d) SEM
however, too low to be detected by ordinary XRD image for a junction zone between iron accumulated area (upper)
measurements and hardness of the teeth were also low as and calcium phosphate area (lower), (e) blade crack to the tooth.
* Tokushima University, Tokushima, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
** Gunma University, Gunma, Japan Japan
*** JWR Institute, Osaka University, Osaka, Japan
364
Evaluation of magnetite and related iron compounds in the teeth of chiton using X-ray and electron analyses
special material for junction of these parts could not be strength of the teeth supported with other mineral
observed even with high resolution SEM. In addition, components where they act a roll as shock absorber.
they were highly integrated mechanically so that a knife Affinity of iron and calcium phosphate parts also would
crack runs in the tooth without exfoliation of these two work to make a extreme strong structure for the tooth
parts. mechanically. Then, mechanical property of the teeth is
From these observations, it could be considered that much higher than those of other marine creatures at
the hardness of the teeth is due to the magnetite, the intertidal zone.
365
Characterication and control of nanoparticle dispersion behavior

†
for smart processing in liquid phase
KAMIYA Hidehiro *, IIJIMA Motoyuki *, TAKENOUCHI Shun *, IINUMA Chihiro *

and NAITO Makio **
KEY WORDS: (Nanoparticle) (Aggregation) (Surface treatment) (Dispersion) (Bead milling) (hybrid material)
ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ ᴾ (Organic solvent) (Smart materials) (Powder Technology) (Colloid probe AFM)
1. Introduction If a hydrophobic surface was produced on particles, TiO 2

Nanoparticles have already become an indispensable nanoparticles were precipitate from suspension. In this
and smart material for many fields of industries because of paper, we investigated mixed silane coupling agents
their unique size dependent properties such as electrical, method5) by using two kinds of agent such as APTMS,
magnetic, mechanical, optical and chemical properties, NH 2 -(CH 2 ) 3 Si(OCH 3 ) 3 , (molecular weight : 179.3g/mol,
which largely differ from those of their bulk materials1, 2). minimum covered surface area : 436䟝/g), and DTMS,
Since nanoparticles have different surface structures and CH 3 (CH 2 ) 9 Si(OCH 3 ) 3 (molecular weight : 179.3g/mol ,
surface interactions compared to the sub-micron sized minimum covered surface area : 436䟝/g). The separated
particles, nanoparticles have an extremely high tendency particles were dried and re-dispersed in various organic
for adhesion and aggregation. Thus, it is quite important to solvents. The relationship between surface molecular
develop techniques to control the dispersion/aggregation structure and dispersion behavior in organic solvent was
phenomena of nano particles to apply them in functional discussed by the measurement results of aggregate size
materials and products.ᴾ In this paper, we focused on the distribution. The aggregation behavior in the organic
post-synthesis surface modification process for the solvent was determined by a dynamic laser scattering
dispersion of nanoparticles in various organic solvents by method, and surface structure was characterized by FT-IR.
using surface chemical reaction of silane coupling agents. The amount of surface modified silane coupling agent was
In order to redisperse this aggregated dry powder into determined by TG-DTA and CHN analyzer after washing
solvents near to their primary particle size, the mechanical of free silane coupling agent.
milling method using small beads has recently been
developed3). The aggregate of dry carbon black Dispersion of carbon black suspension by agitation milling
nanopartiucles was applied to re-disperse into liquid media used small beads of 30 Pm in diameter and simultaneous
by the simultaneous processing of surface modification and processing of surface modification
the bead milling. Carbon black particles (specific surface area : 225 m2/g)
was dispersed into N-metyl-2-pyrrolidone, NMP, with
2. Experimental procedure maleic acid anhydride, for which surface area based
Surface chemical modification of TiO 2 nanoparticles in concentration was fixed at 17.0Pmol/m2. The aggregates in
aqueous suspension and dispersion behavior in organic suspension were dispersed by an agitation bead mill. The
solvent effects of agitation milling time on aggregate size
Recently, aqueous colloidal suspensions with well distribution were determined by laser scattering method.
dispersed various kind of inorganic nano particles, such as After milling, surface treated carbon black was washed and
silica, TiO 2 and ZrO 2 , have been marketed by different dried. Finally, surface modified carbon black particles were
companies. Since the surfaces of nanoparticles in reacted with NaOH in aqueous solution or epoxy and tetra-
suspension have a high electric charge and the double layer butyl-ammoniun-bromide, TBAB, toluene solution at 363
is formed on surface, nanoparticles were dispersed up to K for 24 h. After drying of each surface treated carbon
primary particles without aggregation in aqueous media. black particles, the amount of surface reacted molecules
From commercial TiO 2 aqueous suspension, the surface were determined by TG-DTA, and dispersion behavior of
modification process for dispersion of nano particles in each treated particle was observed in water with pH
organic solvents is shown in Fig. 14). Two kinds of silane adjusted at 11 and toluene.
coupling agents with different molecular structures and
methanol were reacted on the surface of TiO 2 in suspension.
ᴾ ᴾ ᴾ †ᴾ Received on 30 September 2010 Transactions of JWRI is published by Joining and Welding

ᴾ ᴾ ᴾ *ᴾ Tokyo University of Agriculture and Technology, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
**ᴾ Joining and Welding Research Institute, Osaka University, ᴾ Japan
Japan
366
Characterication and control of nanoparticle dispersion behavior for smart processing in the liquid phase
㽢 Non-dispersible in any organic solvents
Fig. 1 Preparing process of surface modified TiO 2 particles

Dispersion behavior of surface treated TiO 2 nano particle
with different silane coupling agents in various organic
solvents
Surface molecular structure of TiO 2 nanoparticles was
characterized by FT-IR and the functional group of each
coupling agent was confirmed. By using the surface
treatment process as shown in Fig. 1, it is possible to
modify and produce hydrophobic chain on TiO 2 Fig. 2 Dispersion behavior of surface treated TiO 2
nanoparticles. The dispersion behavior of surface modified nanoparticles with different amounts of reacted silane
particles with different conditions was observed in different coupling agent in various organic solvents
organic solvents. Based on the observation and aggregate
size distribution determined by dynamic laser scattering
method, an example of the dispersion map was shown in
Fig. 2. This figure shows the dispersion behavior of TiO 2
nanoparticles with different reacted amounts of APTMS
and DTMS, in various organic solvents. The amount of
reacted silane coupling agent was controlled by the additive
content of each silane coupling agent and determined by
CHN analysis. If a transparent suspension was obtained and
the mean aggregate size was smaller than 100 nm, we
decided that the surface modified particle was dispersible in
each organic solvent. The optimum surface modified
amount of each silane coupling agent in various organic
solvents was determined by using this map. Fig. 3 Effect of milling time on aggregate size distribution
in aqueous suspension
Dispersion of carbon black suspension by agitation
milling used small beads of 30 Pm in diameter and
simultaneous processing of surface modification
The effect of milling time on size distribution is shown
in Fig. 3. The minimum aggregate size was observed at 2 hr
milling time. The longer milling time caused an increase in
the aggregate size.
The dispersion behavior of carbon black nanoparticles
with different surface modification conditions in water (pH
= 11) and toluene was observed and shown in Fig. 4. If a
hydrophilic functional group was produced on carbon black,
carbon was able to disperse in water. When an epoxy group
was produced on the carbon surface, carbon black was able
to disperse in water and toluene. The multiple surface Fig. 4 Dispersion behavior of surface treated carbon black
treatment of carbon was useful for the dispersion in polar particles with different conditions in water and toluene
and non-polar solvents.
367
4. Conclusions [2] A. P. Alivisatos, Science, 271 (1996), pp.933-937

Dispersion behavior of TiO 2 and carbon black [3] M. Inkyo, T. Tahara, T. Iwaki, F. Iskandar, C. J. Hogan Jr., K.
nanoparticles was able to be controlled by the surface Okuyama, J. Colloid and Interface Sci., 304 (2006), pp.535-
modification and physical bead milling method in organic 540
[4] M. Iijima, M. Kobayakawa, M. Yamazaki and H. Kamiya, J.
solvent and water.
Am. Chem. Soc., 131(2009), pp. 16342-16343
[5] M. Iijima, M. Kobayakawa, H. Kamiya, J. Colloid Interface
References Sci., 337(2009), pp.
[1] J. L. Marignier, J. Belloni, M. O. Delcourt, J. P. Chevalier,
Nature, 317 (1985) pp. 344-345.
368
†
MATSUBARA Toshio *, TERASAKI Hidenori **, OTSUKA Hiroyuki **

and KOMIZO Yu-ichi **
KEY WORDS: (Digital signal analysis) (Arc voltage) (Welding current) (In-process-monitoring)
(Gas shield arc welding)
1. Introduction pitched at an equal distance is turning circles into ellipses.

Nowadays, demands for the welding process reliability Consequently, MD of point A is small and point B is large.
and on-line welding quality controllability and prediction For this study, how large the compared values of MD are is
are higher than ever before. For this reason, it has become an indicator of whether a welding fault has occurred, with a
more and more important to develop efficient methods for large distance indicating a fault.
evaluating welding quality. Advances in sensor and Figure 3 shows distributions of MD calculated from
computer-related techniques have allowed a wide range of Fig.1(a) and (b). According to quality control, the threshold
computer-based sensing techniques to be brought to use in is commonly set to μᶠ3᷎(μ:mean,᷎:standard deviation).
monitoring welding quality, including the behavior of the That is to say, if results are within the range of μᶠ3᷎, the
arc column, the molten pool and droplet transfer [1-6]. results are good. If not, the results are bad. MD values are
Additionally, traditional nondestructive testing methods are always greater than zero. In this study, MD locating at the
also currently widely used for the credible examination of range from zero to μ+3᷎of the reference MD (the dotted
weld beads. However, methods such as those mentioned line shown in Fig. 3) are defined as “good”. Conversely,
above have the disadvantage of high cost, low efficiency data beyond the range are considered ḛbad”. Consequently,
and cannot be used for in-situ detection. MD on the left-hand side of the line is good, and on the
The present paper deals with the development of a real- right-hand side is bad. It is clear, then, that welding quality
time monitoring equipment to evaluate welding quality in can be quantified as per the formula shown below,
gas shielded arc welding by electrical sensing. Welding Quality (%) = (n/N)* 100
current and arc voltage acquired easily from the welding Where n is the number of data on the left-hand side of the
process. And the hardware used for the proposed system is dotted line, and N is the total number of the data obtained
relatively simple, which should contribute to increasing the in one second. (As described below, in this study, the total
efficiency and decreasing costs. A novel algorithm is number of data accumulated in one second is about 4000.)
presented to analyze data with methods of signal processing
and computer statistics in real time. On the basis of this
algorithm, a new piece of equipment is developed.
2. A developed algorithm
Example scatter plots of transformed data calculated
from blocks of 0.5 second sampled voltage and current data,
as shown in Fig. 1. The data shown in Fig.1 are obtained by
normalizing the reference data. It can be seen that the data
from a reference weld Fig.1(a) are located near the center.
However, the distributions of data shown in Fig.1(b)
deviate from the point of origin and incline to the right.
The analysis method of the proposed system is based on
Mahalanobis distance (MD). The calculation of MD is
described in the field of statistics. To elucidate MD, a
conceptual diagram of MD is shown in Fig. 2. Points A and
Fig. 1 Example scatter plots of transformed data
B are located on the same circle and the Euclidean
calculated from blocks of 0.5 second sampled
distances of two points are equal. However, point B is far
voltage and current data (a) reference and
from the data distribution. Therefore, the shape of the data
(b) comparison.
is considered; this is where MD shows superiority to the
Euclidean distance. With this concept, a set of points
* Tokushima Prefectural Industrial Technology Center, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
369
According to the theory above, a new piece of equipment test weld. Considering arc voltage and welding current are
has been developed. The developed system has the unstable after the welding start, the reference was selected
capability to detect and quantify welding quality in real 4.5 to 5 second data. The sampling rate was about 4000.
time. Quality was calculated every 0.5 second from 5.5 second
after start.
The change of the average voltage is not confirmed, but
the welding quality changes on the butt line. This developed
algorithm is considered to be of benefit for the fault that is
difficult to detect by monitoring only average voltage.
B A
Fig. 2 Conceptual diagram of Mahalanobis distance.
Fig. 4 Test arrangement with weld diagonally crossing

the butt line.
Fig. 3 Distributions of Mahalanobis distance calculated

from Fig.1 (a) and (b).

In order to verify the usefulness and application of the
developed algorithm, TIG welding experiment was
performed. The welding conditions are given in Table Fig. 5 The weld average voltage and quality for
1.The welding torch was fixed on a fixture, which made the test weld.
torch stationary. The specimen was fixed on a trolley
controlled by a speed controller that was able to change the 4. Conclusions
welding speed artificially. In this case, the stability of This study investigated the application of a newly
welding was guaranteed. The test weld was made developed piece of equipment for gas shield arc welding
diagonally across the butt line as shown in Fig. 4. fault detection. MD was used to intuitively quantify and
Figure 5 shows the average voltage and quality for the qualify welding quality in real time. The method had been
developed to be of practical for real time computation and
Table 1 TIG welding conditions
to be applicable to quality monitoring and fault detection in
Specimen dimensions (SUS304) 0mm×200mm×3mm
an industrial production environment.
The proposed algorithm employed the concepts of MD to
Welding current 100A
describe a good quality welding to be used as a reference
Welding speed 5mm/sec
with which to control other welding. First, a reference was
Arc length 2mm
defined; frRP WKLV 0' PHDQ DQG VWDQGDUG GHYLDWLRQ ı
Cathode angle 60°
values were calculated. Then, values of MD obtained from
Shielding gas flow rate(Ar) 0.25L/sec the reference welding current and arc voltage data. And
Back shielding gas flow rate (Ar) 0.125L/sec values located LQ WKH UDQJH IURP ]HUR WR ı RI WKH
370
reference MD were regarded as good. Last, the number of References

values of MD obtained from comparison welds found to [1] S. Patrizia, B. Dario de: NDT&E International, 35 (2002),
belong to the reference set was calculated, in order to pp.37-43.
quantify welding quality. [2] Johannes Ruisz, Jurgen Biber, Mario Loipetsberger: Int J Adv
Manuf Techno, 133 (2007), pp.952-960.
TIG welding experiment was conducted by welding [3] Y.W. Wang, P.S. Zhao: International Journal of Pressure
diagonally crossing the butt line in order to verify the Vessels and Piping, 79 (2001), pp.43-47.
sensitivity and feasibility of the algorithm. The results [4] M. Mi, B. Miller, A. Kita, I.C. Ume: Mechatronics, 12 (2002),
demonstrated that this algorithm was capable of quantifying pp.1259-1269.
and qualifying the welding faults. [5] G. Ladislav, G. Janez, P. Ivan, M.S. Janez: International
Journal of Machine Tools &Manufacture, 44 (2004), pp.555-561.
[6] Kamal Pal, Sandip Bhattacharya, Surjya K. Pal: Journal of
Material Processing Technology 210 (2010), pp.1397-1410.
371
Image measurement of welding distortion of pipe joint in two-phase

†
flow separator
ITOH Shinsuke *, SHIBAHARA Masakazu ** and MOCHIZUKI Masahito *
KEY WORDS: (Welding distortion) (Image measurement) (3D measurement) (Stereo imaging technique)
(Iterative substructure method) (Thermal elastic plastic analysis)
1. Introduction dimentional measurement method by stereo imaging using

The two-phase flow separator is connected to more than two digital cameras is applied to measure the welding
300 pipes, which are attached by fillet welds. Although the deformation. Furthermore, the measured results are
welding causes deformation, it is quite difficult to correct compared with simulated results by Iterative Substructure
this deformation to the shroud head to which the two-phase Method (ISM) for 3-dimentional thermal elastic plastic FE
flow separator is attached because the shroud head material analysis.
is very thick—more than 50 mm. Thus, it is necessary to
clarify the mechanism of welding deformation so that it can 2. Three dimensional measurement based on stereo
be quantitatively predicted and controlled. image processing and experiments
The objective of this paper is to investigate the influence of In this study, a measurement system using the stereo
factors such as the inclination angle of the base plate, to imaging technique based on the digital image correlation
which the pipes are connected, on welding deformation. In method is applied. This technique can eliminate the
this study, the fillet welding experiments of pipe are abovementioned errors by the out-of-plane displacement
performed with changing the angle of joint plane and a 3- effect and both in-plane and out-of-plane deformation can
(a) Photo taken by left cameraᴾ ᴾ (b) Photo taken by right camera
Fig. 1 Photographs of specimen whose angle of joint plane is 30 degree.
[mm]
(a) Image before weld (b) 1st layer (c) 2nd layer (d) 3rd layer
Fig. 2 Distribution of axial displacement measured by 3D measurement
based on stereo imaging technique.
** Graduate School of Engineering, Osaka Prefecture Japan
University, Japan
372
Image measurement of welding distortion of pipe joint in two-phase flow separator

r
r
Translation of pipe (mm)

r

Axial shrinkage (mm)
r

VW
OD\HU
r
r
QG UG r
VW QG UG
OD\HU OD\HU OD\HU
r OD\HU OD\HU

7LPHVHF
7LPHVHF
(a) Axial shrinkage (b) Translation of pipe
Fig. 3 Influence of inclination angle of joint plane on welding distortion.
(a) 1st layer (b) 2nd layer (c) 3rd layer

Fig. 4 Distribution of axial shrinkage simulated by Iterative substructure method.
be measured simultaneously with high accuracy. indicates that the influence of the inclination angle on the
To study the influence of the inclination angle of the joint welding deformation in axial shrinkage is small. On the
plane on the welding deformation, four specimens with other hand, the deformation in inclined direction becomes
different inclination angles of welding plane, namely 0o, large when the inclination angle of the weld plane becomes
10o, 20o and 30o are used. The diameter and thickness of large.
pipe are 168.3mm and 3.4mm respectively. The thin base
plate is 400x400x29 mm. Stainless steel SUS304 is used in 3. Thermal elastic plastic FE analysis using Iterative
both pipe and thick plate. The total welding passes and Substructure Method (ISM)
layers are ten and three. The first and second layers have The same models as the experimental specimens are
four quarter circular passes, respectively. The third pass has used for the FE analyses. After the thermal conductive
two half circular passes. Measurement is carried out before analysis using a moving heat source, the Iterative
welding, after each welding pass and after cooling by taking substructure method (ISM) as high-speed 3-dimensional
photographs by two digital cameras as shown in Fig. 1. thermal elastic plastic FE analysis developed by the authors
Additionally, the specimens are sprayed to collate easier. is performed.
Figure 2 shows the axial displacement distribution of 0o Figure 4 show the result of the welding deformation in
model when the each layer is welded. It is seen that the the axial direction in case of the 0o model. From this figure,
axial shrinkage becomes larger when the layer increases. it is found that the axial shrinkage becomes larger when the
Furthermore, in the axial direction, the pipe is mainly layers increase. This tendency is the same as that of the
deformed and the deformation of the thick plate is very experiment. The influence of the inclination angle of joint
small. In this measurement, it is difficult to use the imaging plane on the welding deformation in inclined direction is
technique where the inclination angle to the camera is large also the same as the experimental result.
or where the spray is not carried out such as the welding
line. In these cases, the results are ignored.
The influences of the inclination angle of the welding 4. Conclusions
plane on the axial and inclined direction are summarized in The three-dimensional displacement measurement
Fig. 3. The displacements of the top of the pipe when the system based on the stereo imaging technique is applied to
welding of each layer is finished are plotted. This figure the welding deformation problem of weld joint model of
373
two phase flow separator and serial computation are the stereo imaging technique based on the digital image
performed by Iterative substructure method as high-speed correlation method and the displacements in axial and
thermal elastic plastic FE analysis. The following inclined direction can be calculated.
conclusions are drawn. (2) When the inclination angle of the welding joint becomes
(1) It is confirmed that the welding deformation distribution lager, welding deformation in inclined direction
of pipe can be measured by measurement system using becomes larger.
374
Microstructure of Cr3Si coatings on austenitic stainless steel by

†
spark plasma sintering
NISHIMOTO Akio *, MIYATA Atsuhiro ** and AKAMATSU Katsuya *
KEY WORDS: (Austenitic stainless steel) (Coatings) (Hot hardness) (Intermetallic compound) (Reaction layer)
(Silicide) (Spark plasma sintering) (Surface modification) (Wear resistance)
1. Introduction Microhardness measurement was carried out using a

The system requirements of high temperature materials Vickers microhardness tester under 0.98 N loads. 22
become ever more severe, material that has both excellent indentations were performed on each sample, and 20 points
oxidation resistance and corrosion resistance is demanded. average value except both maximum and minimum values
Surface modification is one of the effective ways. In surface was used for hardness. Wear testing was carried out at room
modification processes, there are many coating processes, temperature with a pin-on-disk tribometer. The conditions
such as thermal spraying, nitriding and cementation.[1][2] To for wear testing were a running distance up to 300 m, wear
protect the substrate against severe environments, the load of 5 N, rotating speed of 0.047 m/s, wear radius of 3
surface layer is required to be thick and well joined with the mm, and diameter of 6 mm alumina ball used as counter
substrate.[3] In this background, recently, works on the material. Hot hardness test was performed to evaluate the
application of spark plasma sintering (SPS) or pulsed high temperature property of the obtained coating layer.
electric current sintering (PECS) to the joining or surface Table 1 Chemical composition of SUS310S (mass%).
modification process have been reported, though much & 6L 0Q 3 1L &U )H
attention has been paid to this process as a fabrication
method for new functional graded materials and composite %DO
materials. This process enables one to sinter these materials
at lower temperatures and in shorter times than
conventional sintering techniques.[4] 3. Results and Discussion
ᴾ In this investigation, Cr-Si intermetallic compound Figure 1 shows X-ray diffraction (XRD) patterns of Cr-
layers were coated on an austenitic stainless steel SUS310S Si coating layer. XRD studies revealed that the coating
substrate by the SPS process to improve its wear and heat layer treated for 10.8 ks at 1173-1323 K consisted of Cr3Si,
resistances and the resulting properties of the obtained Cr5Si3, and unreacted Cr, and the coating layer treated at
coatings were investigated. 1073-1123 K consisted Cr3Si, Cr5Si3, and unreacted Cr and
Si.
2. Experimental Procedure Figure 2 shows the relationship between hardness and
Cr (99.5 %) and Si (98 %) with average particle sizes of density of Cr-Si coating layer treated for 10.8 ks at 1073-
45 Pm and 150 Pm, respectively were used as starting
&U
powders and were mixed at a molar ratio of 76:24. An &U6L
austenitic stainless steel, SUS310S (I19ᶣ5 mm), was used &U6L
6L
as a substrate. Substrate surfaces were ground with 1.0 Pm
.NV
alumina powders and were degreased by washing in acetone
,QWHQVLW\DUELWDUDU\ XQLW
just before coating. The coating was carried out with a

spark plasma sintering (SPS) apparatus. SUS310S substrate
.NV
and a powder mixture of Cr and Si were loaded into a
graphite die. Sinter-coating was carried out at 1073-1323 K
for 0.6-10.8 ks at a coating pressure of 60 MPa in a vaccum .NV
of 4u10-3 Pa.
The microstructure of the Cr-Si coating layer and the .NV
interface between the Cr-Si coating layer and SUS310S
substrate was observed with optical microscopy (OM) and
scanning electron microscopy (SEM). The surface layer 2T GHJUHH
was also examined by X-ray diffraction (XRD). Fig. 1 X-ray diffraction pattern of Cr-Si coating layer.
* Department of Chemistry and Materials Engineering, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Kansai University, Suita, Japan Japan
** Graduate School, Kansai University, Suita, Japan
375
Microstructure of Cr3Si coatings on austenitic stainless steel by spark plasma sintering

6866 +9

+DUGQHVV+91 1
'HQVLW\ˮ NJ P

:HDUORVVPP

+DUGQHVV

'HQVLW\

&RDWLQJWHPSHUDWXUH 7 . Fig. 4 Wear loss of Cr-Si coating layer
the and SUS310S substrate.
Fig. 2 Relationship between hardness and density
of Cr-Si coating layer treated for 10.8 ks at 1073-
1323 K by the SPS process.
50 .
7KLFNHQHVV RIUHDFWLRQOD\HUPP
1000
40 +DUGQHVV+91 1 500
.
30
100
20 50
٨Cr-Si coating layer
٤SUS310S
10
10
400 600 800 1000 1200
7HPSHUDWXUH7 .
0
0 20 40 60 80 100 120
+ROGLQJWLPHWV Fig. 5 Hot hardness test of Cr-Si coating
layer and SUS310S.
Fig. 3 Effect of holding time on the thickness
of reaction layer in samples coated at 1273 K. higher hardness than SUS310S substrate, even at high
temperature in both Cr-Si coating layr and SUS310S
1323 K by the SPS process. As the coating temperature substrate was observed, as shown in Fig. 5. Transition
increased, the densification was developed and the hardness temperatures of Cr-Si coating layer and SUS310S substrate
of these coating layers also increased up to 1150 HV. were 873 K and 723 K, respectively. These results indicate
Also, a reaction layer with the thickness of 40 Pm and that the hardness of 700 HV relatively up to 873 K.
the hardness of 700 HV was formed between the coatings Therefore, it was concluded that the Cr-Si coating layer
and the substrate in the sample treated for 10.8 ks at 1273 K. could be applied to some parts that require wear resistance
Figure 3 shows the relationship between the thickness at high temperature.
of the reaction layer and holding time. The growth of the
reaction layer showed a parabolic relation against holding 4. Conclusions
time. Cr-Si intermetallic compound layers were coated on
Figure 4 shows the wear loss of Cr-Si coating layer and SUS310S substrate by the SPS process to improve its wear
SUS310S substrate. The SUS310S substrate had poor wear and heat resistance. The conclusions of this investigation
resistance. In comparison, Cr-Si coating layer showsᴾ are summarized as follows.
considerably less wear. This confirmed that the wear (1) XRD studies revealed that the coating layer treated for
property of SUS310S was improved by the SPS process. ᴾ 10.8 ks at 1173-1323 K consisted of Cr3Si, Cr5Si3, and
Figure 5 shows a hot hardness result tested at unreacted Cr and coatings treated at 1073-1123 K
temperatures ranging from room temperature to 1073 K for consisted of Cr3Si, Cr5Si3, and unreacted Cr and Si.
Cr-Si coating layer and SUS310S substrate. Cr-Si coating (2) The hardness of the coating layer showed 1150 HV at
layer showed higher hardness than SUS310S substrate, the maximum.
even at high temperature. A gradual decrease in hardness up (3) The reaction layer with a thickness of 40 Pm and a
to a transition temperature, followed by a rapid drop above hardness of 700 HV was formed between the coatings
376
and the substrate in the sample treated for 10.8 ks at References

1273 K. [1] A. Nishimoto, A. Tokuda and K. Akamatsu: Mater. Trans., 50
(4) Results of pin-on-disk wear tests and hot hardness tests (2009), pp.1169-1173.
show that the wear and high-temperature properties of [2] A. Nishimoto, K. Akamatsu and R. Wada: J. Jpn. Soc. Heat
Treat. 49 (Spec. lss.) (2009), pp.385-387.
SUS310S wear improved by the SPS process.
[3] T. Matsubara, T. Shibutani, K. Uenishi and K.F. Kobayashi:
Intermetallics 8 (2000), pp.815-822.
[4] A. Nishimoto and K. Akamatsu: Plasma Process. Polym., 6
(2009), pp.S941-S943.
377
Modification of thermally sprayed cemented carbide layer by

†
friction stir processing
MORISADA Yoshiaki *, FUJII Hidetoshi **, MIZUNO Tadashi ***, ABE Genryu ***,
NAGAOKA Toru * and FUKUSUMI Masao *
KEY WORDS: (Friction stir processing) (Thermal spray) (Cemented carbide) (Tool steel) (Hardness)
1. Introduction without a probe. A constant tool rotating rate of 600 rpm

Applicable fields of cemented carbide are wide and they was used and the constant travel speed was 50 mm/min. A
are used as the base metals for cutting tools, dies, molds, tool tilt angle of 3°was used.
etc. However, W, Co, and Ni, which are the main Transverse sections of the as-sprayed and the FSPed
compositional elements of the cemented carbide, are rare samples were mounted and then mechanically polished. The
and expensive. The amount of these elements should be microstructure of the cemented carbide layer was observed
reduced for resource savings and cost reduction. by SEM (JEOL JSM-6460LA). The distribution of the
Additionally, the shape and the size of the sintered nanometer-sized defects and the microstructure of the
cemented carbide are limited because of the equipment metallic binder were evaluated by TEM (JEOL JEM-
used for sintering. Therefore, a coating technique to form 4000EX) at the accelerating voltage of 400 kV. The
the sound cemented carbide layer with its original specimens for the TEM observations were prepared by FIB
mechanical properties is desired. (Hitachi High-Technologies Corporation, FB-2000A). The
Although thermally sprayed coatings can produce the microhardness was measured using a micro-vickers
cemented carbide layer on a substrate, the as-sprayed hardness tester (Akashi HM-124) with a load of 300 g.
cemented carbide layer contains many defects and its
hardness is much lower than that of the sintered cemented 3. Results and Discussion
carbide [1, 2]. The weak adherence between the cemented Figure 1 shows the microstructural change of the WC-
carbide layer and the substrate is also a serious problem for CrC-Ni layer following FSP. The porosities in the WC-
many applications. In the past decade, laser heating CrC-Ni layer disappeared due to the FSP. Additionally, the
treatment of the thermally sprayed layer has been studied to WC particles were densely packed. It is considered that the
increase its mechanical properties [3]. However, the plastic flow of the Ni binder induced by the FSP led to the
hardness shows a non-uniform distribution in the depth rearrangement of the WC particles. The Cr 3 C 2 particles
direction of the cemented carbide layer and it is still lower were fragmented and deformed by the tool and were
than that of the sintered cemented carbide. In this study, the dispersed in the matrix. TEM images of the FSPed
modification of a thermally sprayed cemented carbide layer cemented carbide layers showed that the microstructure of
by the FSP is investigated in order to improve the the metallic binder was refined on a nanometer scale by the
mechanical properties and enhance their applicable fields. FSP. The grain size of Ni and Co was refined to 㹼200 nm
by the FSP as shown in Fig. 2. It is considered that they
2. Experimental Procedure were recrystallized by the severe plastic deformation during
Commercially available WC-20mass%CrC-7mass%Ni the FSP.
powder (mean diameter: 40ȣm, Sumitomo Metal Mining The microhardness horizontal profiles for the as-sprayed
Co., Ltd.) and WC-12mass㸣Co powder (mean diameter: and the FSPed cemented carbide layer are shown in Fig. 3.
7KH PLFURKDUGQHVV DW ȝP IURP WKH VXUIDFH ZDV
40ȣm, Sumitomo Metal Mining Co., Ltd.) were sprayed
measured for the horizontal profile. The average
on an SKD61 substrate (17 mm175 mm230 mm) by microhardness of the as-sprayed WC-CrC-Ni layer was
JP5000 HVOF thermal spraying equipment (Eutectic of about 1200 HV which was similar to that of the thermally
Japan, Ltd.). The carrier gas, gun speed, and fuel were Ar, 3 sprayed WC-CrC-Ni layer reported by other researchers [4].
mm/min, and coal oil, respectively. The thickness of the The microhardness of the FSPed zone reached 㹼2000 HV.
WKHUPDOO\VSUD\HGFHPHQWHGFDUELGHOD\HUZDVDERXWȝP The microhardness of the WC-Co layer was also increased
The thermally sprayed cemented carbide layer was by the FSP from about 1200 to 2000 HV.
modified by the FSP. The FSP tool made of sintered WC- Generally, the hardness of the cemented carbide was
&R FHPHQWHG FDUELGH KDG D FROXPQDU VKDSH ĳ PP increased by the reduction of the metallic binder content
* Osaka Municipal Technical Research Institute, Osaka, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan Japan
** JWRI, Osaka University, Osaka, Japan
*** AMC Corporation, Osaka, Japan
378
Modification of thermally sprayed cemented carbide layer by friction stir processing
and close to that of the monolithic WC. The obtained microhardness. The improvement of the mechanical
microhardness of 2000 HV was nearly the same value as properties of the cemented carbide has been studied by the
that of the sintered WC. It should be mentioned that the decrease in the grain size of the WC particles [5]. For
microhardness of the FSPed zone was higher than that of example, the spark plasma sintered WC-Co with the WC
the sintered cemented carbide with the same chemical particles of 㹼100 nm and the hot pressed WC-Co with the
composition. It is difficult to explain such a large increase WC particles of 169 nm had values of 1887 and 2084 HV,
in the microhardness by only the elimination of the defects respectively [6, 7]. On the other hand, there was no
in the as-sprayed layer. It is considered that the grain effective process to refine the microstructure of the metallic
refinement of the Ni and Co binder and the rearrangement binder in the cemented carbide. Although the grain of the
of the WC particles assisted in the change of the metallic materials could be refined by the recrystallization
As-sprayed WC-CrC-Ni layer FSPed WC-CrC-Ni layer process, it was difficult for the cemented carbides because
of their high deformation resistance. In this study, the
Cr3C 2 plastic flow was successfully induced to the thermally
sprayed cemented carbide layer using the rotating tool made
SEM image
Porosity of WC-Co.
2500
䕦: as-sprayed WC-CrC-Ni layer
WC
䖃: FSPed WC-CrC-Ni layer
䕧: as-sprayed WC-Co layer
䕿: FSPed WC-Co layer
2000
Microhardness / Hv
TEM image
1500
1000
Fig. 1 Microstructural change of the WC-CrC-Ni layer
by the FSP.
500
㻙㻤㻙㻢㻙㻠㻙㻞㻜㻞㻠㻢㻤
Distance from the process centerline / mm

Fig. 3 Microhardness horizontal profiles of the cross-
section of the as-sprayed and the FSPed cemented
carbide layer.
4. Conclusions
The thermally sprayed cemented carbide layer was
successfully modified by the FSP. The obtained results are
summarized as follows.
(1) The cemented carbide layer can be stirred by the
rotating tool made of WC-Co. The defects in the
cemented carbide layer disappear and the WC
particles are closely packed after the FSP.
(2) The Ni binder, the Cr 3 C 2 particles in the WC-CrC-Ni
layer, and the Co binder are refined by the FSP.
(3) The FSPed cemented carbide layer has an extremely
high microhardness of 㹼2000 HV which is higher
than that of the sintered cemented carbide with the
same composition.
References
[1] H.S. Ni, X.H. Liu, X.C. Chang, W.L. Hou, W. Liu, and J.Q.
Wang, J. Alloys Compd. 467 (2009) 163.
[2] T.Y. Cho, J.H. Yoon, K.S. Kim, K.O. Song, Y.K. Joo, W.
Fang, and S.H. Zhang, Surf. Coat. Technol. 202 (2008) 5556.
[3] D. Triantafyllidis, L. Li, and F.H. Stott, Surf. Coat. Technol.
201 (2006) 3163.
Fig. 2 TEM images of the as-sprayed and the FSPed [4]S.H. Zhang, T.Y. Cho, J.H. Yoon, M.X. Li, P.W. Shum, and
cemented carbide layers. S.C. Kwon, Mater. Sci. Eng. B 162 (2009) 127.
379
[5] Z.Z. Fang, X. Wang, T. Ryu, K.S. Hwang, and H.Y. Sohn, Int. [7] C.G. Lin, E. Kny, G.S. Yuan, and B. Djuricic, J. Alloys
J. Refract. Metals and Hard Mater. 27 (2009) 288. Compd. 383 (2004) 98
[6] L.H. Zhu, Q.W. Huang, and H.F. Zhao, J. Mater. Sci. Lett. 22
(2003) 1631.
380
Ultimate strength of aluminum alloy plates in compression

†
considering joining locations
OKURA Ichiro *
KEY WORDS: (Aluminum alloy) (Ultimate strength) (FSW) (MIG welding) (Joining location) (FEM)
1. Introduction For the joints,

The ultimate strength of aluminum alloy plates in § § V ·
nj
V
compression is investigated considering joining locations
¨
¨H E
0.002¨ ¸
¨ V j 0.2 ¸
V d V j 0.2 ࠉ
by the elastic-plastic large deflection analysis with FEM. ¨ © ¹ (2)
The aluminum alloys dealt with in this research are heat-
¨V
© V j 0.2 V ! V j 0.2 ࠉ
treated A6061-T6 and non-heat-treated A5083-O. The where V and H are the stress and strain, respectively,
softening of material and the residual stress caused by FSW V 0.2 and V j 0.2 the 0.2 % proof stresses for the parent
and MIG welding are introduced in the analysis. It is shown
that the joining locations and the width of plate have a great material and the joints, respectively, E the Young’s
influence on the ultimate strength in A6061-T6 alloy plates. modulus (= 70 GPa), and n and n j the parameters for
stain hardening for the parent material and the joints,
2. Joining Locations respectively. The values for V 0.2 , V j 0.2 , n and n j are
The joining locations are different between MIG
welding and FSW. As shown in Fig. 1, for the columns of I- listed in Table 1 [1].
shaped section in compression, in MIG welding, both the
edges of a web are joined to flanges by fillet welding, but in Table 1 Values for 0.2 % proof stresses and parameters
FSW, the edges of the extrusions of T-shaped section are for strain hardening
connected in the middle of a web by butt joining. Parent Joints
material MIG FSW
Alloys
25 ı0.2 n ıj0.2 nj ıj0.2 nj
(MPa) (MPa) (MPa)
50 A6061-T6 245 29.1 108 5.3 108 10
A5083-O 127 5.3 127 5.3 127 5.3
25
(a) MIG welding (b) FSW The distributions of the residual stress are given in Fig.
2 [1]. For the edge-joined plate, the tensile residual stress of
Fig. 1 Joining locations
V rt V j 0.2 is created in the region of 25 mm from each
3. FEM Analysis edge, and the compressive one of V rc 50V j 0.2 / b 50
The ultimate strength of the edge- and middle-joined
plates in compression is investigated by the elastic-plastic in the inside. Here b is the width of the plate in mm. On
large deflection analysis with FEM. The analyzed model is the other hand, for the middle-joined plate, the tensile
a square plate which is simply supported around the edges.
25
In A6061-T6 alloy, the strength at the joint is reduced to
b-50
the half of that of the parent material. The softening region 2
is 25 mm on each side of the center of the joint, as shown
by the shaped parts in Fig. 1 [1]. b-50 50
The relationship between stress and strain is given by
the following [1]: b-50
For the parent material, 2
25
§ V § V ·
n
Ȫrc Ȫrt
¨H Ȫrc Ȫrt
¨
0.002¨¨ ¸
¸ V d V 0.2 ࠉ

¨
E © V 0.2 ¹ (1) (a) Edge-joined plate (b) Middle-joined plate
¨V
© V 0.2 V ! V 0.2 ࠉ

Fig. 2 Distributions of residual stress

* Dept of Civil Engineering, Osaka University, Osaka, Japan Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
381
Ultimate strength of aluminum alloy plates in compression considering joining locations
residual stress of V rt V j 0.2 is created in the region of 50 5. Ultimate Strength of A5083-O Alloy Plates
mm in the middle, and the compressive one of The relation between V u V p 0.2 and R p for the
V rc 50V j 0.2 / b 50 in the rest of the plate. A5083-O alloy plates is shown in Fig. 5. Here,
For the initial deflection of the plate, the following V p 0.2 V 0.2 . In this analysis, the residual stress is taken
equation is assumed, which is the same as the buckling into account. The influence of the width of plate on the
shape: ultimate strength is small for both the edge- and middle-
w0 b / 150 sin Sx / a sin Sy / b ᴾ (3) joined plates.
where a is the length of the plate in the direction of the ıu/ıp0.2
1.0
compression. b=200mm
0.8
4. Ultimate Strength of A6061-T6 Alloy Plates
The relation between V u V p 0.2 and R p for the 0.6
Residual stress
A6061-T6 alloy plates is shown in Fig. 3, in which the 0.4
residual stress is not introduced. V u is the ultimate 0.2
No residual stress
strength in terms of the mean compressive stress. V p 0.2

Euler's buckling curve
0.0
and R p are defined as follows: 0.0 0.5 1.0 1.5 2.0
Rp
V p 0.2 ^(b 50) / b`V 0.2 50 b V j 0.2 (4)
ıu/ıp0.2
(a) Edge-joined plate
1.0
1 12(1 P 2 ) V p 0.2
Rp E (5) b=200mm
S 4 E 0.8
where b is in mm, P the Poisson’s ratio, E ( b t ) the 0.6
width-to-thickness ratio, and t the plate thickness. Residual stress
0.4
As shown in Fig. 3(a), in the edge-joined plate,
No residual stress
V u V p 0.2 decreases as the width is smaller. On the other 0.2
hand, as shown in Fig. 3(b), in the middle-joined plate, 0.0
V u V p 0.2 is almost the same in the different width of plate. 0.0 0.5 1.0 1.5 2.0
Rp
The relation between V u V p 0.2 and R p considering the (b) Middle-joined plate
residual stress is shown in Fig. 4. The influence of the Fig. 4 Influence of residual stress
residual stress on the ultimate strength is small for both the
edge- and middle-joined plates. ıu/ıp0.2
1.0
ıu/ıp0.2
1.0
0.8
0.8
0.6
Non-joined plate
0.6
Non-joined plate 0.4 =200mm
0.4 b=200mm b
b =300mm =500mm
0.2 b
0.2 b =500mm Euler's buckling curve
0.0
0.0
0.0 0.5 1.0 1.5 2.0 0.0 0.5 1.0 1.5 2.0
Rp Rp
(a) Edge-joined plate ıu/ıp0.2
(a) Edge-joined plate
ıu/ıp0.2
1.0
1.0
0.8 0.8
0.6 0.6 b
Non-joined plate Non-joined plate
b
0.4 b=200mm 0.4 =200mm
b=500mm =500mm
0.2 0.2
0.0
0.0
0.0 0.5 1.0 1.5 2.0
Rp 0.0 0.5 1.0 1.5 2.0
Rp
(b) Middle-joined plate (b) Middle-joined plate
Fig. 3 Influence of joining locations Fig. 5 Influence of plate width
382
References
[1] I. Okura, T. Nagao, T. Ishikawa, N. Hagisawa and S. Osumi: J.
of Structural and Earthquake Engineering, JSCE, 64 (2008),
pp.789-805.
383
Development of analytical method for welding mechanics using

†
idealized explicit FEM
SHIBAHARA Masakazu * and IKUSHIMA Kazuki *
KEY WORDS: (Numerical analysis) (Nonlinear analysis) (Thermal Elastic Plastic analysis) (Dynamic Explicit
FEM) (Transient stress) (Transient deformation)
1. Introduction In this research, the temperature increment is

Dynamic explicit FEM has been used to analyze automatically divided into tens of time steps which depend
dynamic problems such as impact problems. This method is on temperature load rate. After loading the temperature
discretized for each node and does not need a global increment, Eq. (2) is solved to compute the displacement
stiffness matrix. It does not use much computer memory until the whole system reaches the static equilibrium state.
because it solves only scalar equations. Therefore, unlike In this method, the dynamic effect becomes quite small.
implicit FEM, dynamic explicit FEM can analyze large- This means that plastic strain is not largely influenced by
scale structural problems. However, in dynamic explicit the dynamic effect and the residual displacement and stress
FEM, the time increment at a single time step is determined for each step have almost the same accuracy as the static
by the Courant condition, which means the time increment implicit FEM.
depends on the stress propagation velocity and the smallest >M @û`t >C @û`t ³ >B@T ^V `dV ^F `t (1)
element size of the model. Therefore, the Courant condition
requires a tremendous number of time steps and much § 1
¨ 2 >M @
1
>C @·¸û`t 't
computing time for long-time phenomena such as welding. © 't 2't ¹
In this study, a new dynamic explicit FEM based
analytical method is proposed. This method permits large ^F `t ³ >B @T ^V `dV (2)
time increments for solving welding problems. The
proposed method neglects the mass and damping effects

2
>M @û`t ¨§ 1 2 >M @ 1 >C @·¸û`t 't
and treats the welding phenomena as quasi-static. This 't 2
© 't 2't ¹
means that the static equilibrium condition of the model is
satisfied at each load step in the proposed method. 3. Verification of Proposed Method
The proposed Idealized Explicit FEM is presented in
this paper. It is compared with static implicit FEM by The time history of stress V y for points a, b, and c is
analyses of bead-on-plate welding. The results show the shown in Fig. 1. In Fig. 1, symbols , and show
proposed method has almost the same accuracy as that with 400.0
static implicit FEM. The computing time and memory
utilization of the proposed method are also discussed. a b c
200.0 a b c
Idealized Explicit FEM
2. Development of Idealized Explicit FEM
Stress (MPa)
Static Implicit FEM

As described in the previous section “Dynamic Explicit
0.0 torch
FEM”, Eq. (2) is solved to calculate displacement. B A’
120.0 mm
40 division
However, in long-time phenomenon problems such as

䞉䞉䞉
welding, the computational steps become enormous because a A
-200.0
of the limitation of the very short time increment. This
b
z B’
c 60.0 mm
y
limitation is due to the Courant condition, which is related 30 division
䞉䞉䞉
x 20.0 mm
to the stress wave propagation velocity and time increment. -400.0
10 division
The Courant condition requires the distance traveled by 0.0 10.0 20.0 30.0 40.0 50.0
stress wave in a time increment to be less than the minimum Time history (sec)
element size . In this study, the authors propose a method to
Fig. 1 Time history of stress ı x
overcome this limitation.
* Graduate School, Osaka Prefecture University, Osaka, Research Institute, Osaka University, Ibaraki, Osaka 567-0047,
Japan
Japan
384
Development of analytical method for welding mechanics using idealized explicit FEM
the transient stress computed by the Idealized Explicit FEM 0.16

and symbols , and show that computed by the
Angular Distortion SA (mm)

0.14 SA = Angular distortion
static implicit FEM. Compressive stress is presented before
the welding torch is passed. After that, the stress becomes 0.12
SA
zero due to melting. Finally, tensile residual stress develops A’
0.10
after cooling. It is verified that the transient stress V y
computed by the Idealized Explicit FEM and that by the 0.08
static implicit FEM are almost the same.
0.06
400.0 Vx Vy 0.04
Idealized Explicit FEM
300.0 0.02 A Idealized Explicit FEM
Static Implicit FEM
Static Implicit FEM
0.00
200.0 A’
Stress (MPa)
0.0 10.0 20.0 30.0 40.0 50.0 60.0

100.0 Vy A Coordinate in y-direction (mm)
0.0 Fig. 3 Comparison of angular distortion between Idealized

Explicit FEM and static implicit FEM
-100.0
A
Vx A’ 1000000 Idealized Explicit FEM
-200.0 Static Implicit FEM
0.0 10.0 20.0 30.0 40.0 50.0 60.0 800000
Computing time (s)
Coordinate in y-direction (mm)

600000
Fig. 2 Comparison of residual stress between Idealized Explicit
FEM and static implicit FEM on top of transverse cross
section 400000
1
Figure 2 shows the distribution of residual stress in x- 12
direction V x on the A-A’ cross section. From Fig. 2, it is 200000
verified that the residual stress distribution of the Idealized
Explicit FEM quantitatively agrees well with that of the
0
static implicit FEM. 0 60000 120000 180000 240000 300000
Angular distortion is shown in Fig. 3. From the figure, it Degree of freedom
is verified that the results of the Idealized Explicit FEM and
the static implicit FEM show almost the same accuracy. Fig. 4 Comparison of computing time between Idealized
Explicit FEM and static implicit FEM
4. Computing time
rectangles shows that of the Idealized Explicit FEM. From
Comparisons of the computing time and memory the figure, the computing time of the static implicit FEM
consumption between the Idealized Explicit FEM and the increases proportional to the square of the number of nodes.
static implicit FEM are discussed here by using different In contrast, the computing time of the Idealized Explicit
models. The static implicit FEM requires a very long time FEM increases linearly. Especially, in the 243243-dof
for computing. Then, the computing time is measured for model, the computing of the Idealized Explicit FEM is
only 0.5-second phenomena after the welding starts to almost 12 times faster than that of the static implicit FEM.
evaluate welding-specific local plasticity and melting. The
number of nodes of the analysis models is 13981, 27511, 5. Conclusions
41041, 54351 or 81081. The degree of freedom of the
model is 41,943, 82533, 123123, 163053 or 243243. The In this research, the authors developed a new numerical
welding condition and boundary condition are the same as method for welding analysis, named Idealized Explicit
those in the previous section. Specifications of the FEM, which is based on the dynamic explicit FEM. The
computer used in this comparison are as follows: CPU is proposed method is compared to the static implicit FEM in
Xeon 2.53 GHz, memory size is 32 GB, operating system is the application of bead-on-plate welding. The following
Windows XP Professional x64 edition. The static implicit results are obtained:
FEM uses a skyline solver. (1) It is demonstrated that Idealized Explicit FEM is
Figure 4 shows the relation between the computing time capable of analyzing the long duration problem such as
and the number of nodes. The solid triangles shows the cooling process of welding that Dynamic Explicit FEM
computing time of the static implicit FEM and the open has difficulty in analyzing.
385
(2) Using the model of bead-on-plate welding, the Idealized Explicit FEM and the static implicit FEM show almost
the same accuracy for transient stress, residual stress implicit FEM in the analysis of large-scale welding
and residual deformation. problem whose dof is 243243.
(3) By comparing the computing time, it is verified that the
Idealized Explicit FEM is 12 times faster than the static
386
CONTRIBUTIONS TO OTHER ORGANIZATIONS
(July 2010 ~ December 2010)
[Physics, Processes, Instruments & Measurements] T. IWAO, Y. MORI, M. OKUBO, T. SAKAI, S. TASHIRO,
M. TANAKA and M. YUMOTO
M. TANAKA, Y. TSUJIMURA, K. NAKATA, E. YAMAMOTO, Modelling of Metal Vapour in Pulsed TIG Including
K. YAMAZAKI and K. SUZUKI Influence of Self-Absorption
Dynamic Behavior of Metal Vapor in Arc Plasma J. Phys. D., Vol. 43 (2010), 434010.
during TIG Welding
63rd Annual Assembly of Int. Inst. Welding (IIW), S. TASHIRO, T. ZENIYA, K. YAMAMOTO, M. TANAKA,
(2010), IIW Doc. 212-1169-10. K. NAKATA, A. B. MURPHY, E. YAMAMOTO,
K. YAMAZAKI and K. SUZUKI
Y. TSUJIMURA and M. TANAKA Numerical Analysis of Fume Formation Mechanism in
A Numerical Model of GMA Welding from Arc Welding
Engineering View J. Phys. D., Vol. 43 (2010), 434012.
63rd Annual Assembly of Int. Inst. Welding (IIW),
(2010), IIW Doc. 212-1170-10. S. TASHIRO, T. ZENIYA, K. YAMAMOTO, M. TANAKA,
K. NAKATA, A. B. MURPHY, E. YAMAMOTO,
Y. TSUJIMURA, K. YAMAMOTO and M. TANAKA K. YAMAZAKI and K. SUZUKI
A Simulation Model of a Short Arc Lamp Numerical Analysis of Fume Formation Mechanism in
Ceram. Trans., Vol. 219 (2010), pp. 195-201. TIG Welding
Q. J. Jpn. Weld. Soc., Vol. 28, No. 4 (2010),
J. J. LOWKE, M. TANAKA and A. B. MURPHY pp. 369-375 (in Japanese).
Metal Vapour in MIG Arcs Can Cause (1) Minima in
Central Arc Temperatures and (2) Increased Arc S. TASHIRO, M. TANAKA and A. B. MURPHY
Voltages Numerical Analysis of Non-Equilibrium Plasma
Welding in the World, Vol. 54, No. 9/10 (2010), Property in Anode Boundary Layer of Argon Gas
pp. 292-297. Tungsten Arc
Surf. Coat. Technol., Vol. 205 (2010), pp. s115-s119.
M. TANAKA, K. YAMAMOTO, S. TASHIRO, K. NAKATA,
E. YAMAMOTO, K. YAMAZAKI, K. SUZUKI, A. B. MURPHY C. S. MOON, K. TAKEDA, M. SEKINE, Y. SETSUHARA,
and J. J. LOWKE M. SHIRATANI and M. HORI
Time-dependent Calculations of Molten Pool Surface Loss Probabilities of H and N Radicals on
Formation and Thermal Plasma with Metal Vapour in Different Materials in Afterglow Plasmas Employing
Gas Tungsten Arc Welding H2 and N2 Mixture Gases
J. Phys. D., Vol. 43 (2010), 434009. J. Appl. Phys., Vol. 107 (2010), pp. 103310-1
-103310-7.
A. B. MURPHY, M. TANAKA, K. YAMAMOTO, S. TASHIRO,
J. J. LOWKE and K. OSTRIKOV C. S. MOON, S. TAKASHIMA, K. TAKEDA, M. SEKINE,
Modelling of Arc Welding: The Importance of Y. SETSUHARA, M. SHIRATANI and M. HORI
Including the Arc Plasma in the Computational Etching Characteristics of Organic Low-K Films
Domain Interpreted by Internal Parameters Employing a
Vacuum, Vol. 85 (2010), pp. 579-584. Combinatorial Plasma Process in an Inductively
Coupled H-2/N-2 Plasma
M. MIYATA, S. TASHIRO and M. TANAKA J. Appl. Phys., Vol. 107 (2010), pp. 113310-1
Numerical Analysis of Plasma Keyhole Welding of an -113310-8.
Aluminum Thin Plate
Ceram. Trans., Vol. 219 (2010), pp. 189-194. Y. SETSUHARA, K. CHO, K. TAKENAKA, M. SHIRATANI,
M. SEKINE and M. HORI
S. TASHIRO, M. MIYATA, M. TANAKA, K. SHIN and Advanced Research and Development for Plasma
K. TAKAHASHI Processing of Polymers with Combinatorial
Numerical Analysis of Basic Property of Keyhole Plasma-Process Analyzer
Welding with Plasma Arc Thin Solid Films, Vol. 518 (2010), pp. 6320-6324.
Trans. Mater. Res. Soc. Jpn., Vol. 35, No. 3 (2010),
pp. 589-592.
387
Y. SETSUHARA, K. CHO, M. SHIRATANI, M. SEKINE and K. H. SONG and K. NAKATA
M. HORI Microstructural and Mechanical Properties of
X-Ray Photoelectron Spectroscopy Analysis of Friction-Stir-Welded and Post-Heat-Treated Inconel
Plasma–polymer Interactions for Development of 718 Alloy
Low-Damage Plasma Processing of Soft Materials J. Alloy. Compd., Vol. 505 (2010), pp. 144-150.
Thin Solid Films, Vol. 518 (2010), pp. 6492-6495.
J. LIAO, N. YAMAMOTO, H. LIU and K. NAKATA
Y. SETSUHARA, K. CHO, K. TAKENAKA, M. SHIRATANI, Microstructure at Friction Stir Lap Joint Interface of
M. SEKINE and M. HORI Pure Titanium and Steel
Low-damage Plasma Processing of Polymers for Mater. Lett., Vol. 64 (2010), pp. 2317-2320.
Development of Organic-Inorganic Flexible Devices
Surf. Coat. Technol., Vol. 205 (2010), pp. S355-S359. M. EGAWA, N. UEDA, K. NAKATA, M. TSUJIKAWA and
M. TANAKA
K. S. SHIN, Y. S. CHOI, I. S. CHOI, Y. SETSUHARA and Effect of Additive Alloying Element on Plasma
J. G. HAN Nitriding and Carburizing Behavior for Austenitic
Nano-crystalline Silicon Thin Films Grown by the Stainless Steels
Inductively Coupled Plasma Assisted CFUBM at Low Surf. Coat. Technol., Vol. 205 (2010), pp. s246-s251.
Temperature
Surf. Coat. Technol., Vol. 205 (2010), pp. S227-S230. M. AONUMA and K. NAKATA
Effect of Calcium on Intermetallic Compound Layer at
Y. SETSUHARA and M. HASHIDA Interface of Calcium Added Magnesium-Aluminium
Photon-induced Phonon Excitation Process as Alloy and Titanium Joint by Friction Stir Welding
Low-Temperature Nonequillibrium Nano-Surface Mater. Sci. Eng. B, Vol. 173 (2010), pp. 135-138.
Modification of Silicon
Surf. Coat. Technol., Vol. 205 (2010), pp. 1826-1829. H. LIU, K. NAKATA, N. YAMAMOTO and J. LIAO
Grain Orientation and Texture Evolution in Pure
K. TAKENAKA, Y. SETSUHARA, K. CHO, M. SHIRATANI, Titanium Lap Joint Produced by Friction Stir Welding
M. SEKINE and M. HORI Mater. Trans., Vol. 51, No. 11 (2010), pp. 2063-2068.
Combinatorial Analysis of Plasma-Surface Interactions
of Polyethyleneterephthalate with X-ray Photoelectron I. SEKI, H. KIMURA, K. NAKATA and A. INOUE
Spectroscopy Influence of Precipitation Behavior of Different
Jpn. J. Appl. Phys., Vol. 49 (2010), pp. 08JA02-1 Crystalline Phases for Embrittlement Behavior of
-08JA02-4. Several Zr-Based Metallic Glasses
Mater. Trans., Vol. 51, No. 11 (2010), pp. 2033-2038.
K. CHO, K. TAKENAKA, Y. SETSUHARA, M. SHIRATANI,
M. SEKINE, M. HORI, E. IKENAGA, H. KONDO, E. ASHIDA, X. ZHANG, S. TARASAWA and S. KATAYAMA
O. NAKATSUKA and S. ZAIMA Bead Formation and Stability in Low-Speed Welding
Hard X-Ray Photoelectron Spectroscopy Analysis for of Stainless Steel with High-Power Fiber Laser
Organic-Inorganic Hybrid Materials Formation J. Jpn. Laser Processing Soc., Vol. 16, No. 3 (2010),
Ceram. Trans., Vol. 219 (2010), pp. 183-188. pp. 165-170 (in Japanese).
K. TAKENAKA, K. CHO, Y. SETSUHARA, M. SHIRATANI, S. KATAYAMA, Y. KAWAHITO and M. MIZUTANI

M. SEKINE and M. HORI Visualization of Melt Flows, Plume or Arc Behavior
Development of a Combinatorial Plasma Process During TIG, Laser or Laser-Arc Hybrid Welding
Analyzer for Advanced R&D of Next Generation IIW Joint Workshop of Commission IV, VII and
Nanodevice Fabrications SG212, Vol. 2010, No. 212-1172-10, XII-1996-10,
Ceram. Trans., Vol. 219 (2010), pp. 279-284. IV-1035-10 (2010), pp. 1-17.
K. TAKENAKA, Y. NAKAJIMA, Y. SETSUHARA, H. ABE and S. KATAYAMA, T. ONISHI, M. MIZUTANI and

K. NOGI Y. KAWAHITO
Plasma-Enhanced Nanoparticles-Beam Deposition for High-Power Laser Butt Welding of High-Strength
High-Rate Formation of Nanocomposite Films Steel Thick-Plate
Ceram. Trans., Vol. 219 (2010), pp. 293-297. IIW Commission IV, Vol. 2010, No. IV-1031-10
(2010), pp. 1-7.
388
M. MIZUTANI and S. KATAYAMA Y. KAWAHITO, Y. NIWA, T. TERAJIMA and S. KATAYAMA
Effect of Plume and Induced Hot Air above Specimen Laser Direct Joining of Glassy Metal Zr55Al10Ni5Cu30
on Laser Beam Refraction during Laser Welding to Engineering Plastic Polyethylene Terephthalate
IIW Commission IV, Vol. 2010, No. IV-1032-10 Mater. Trans., Vol. 51, No. 8 (2010), pp. 1433-1436.
(2010), pp. 1-11.
Y. ABE, M. MIZUTANI, Y. KAWAHITO and S. KATAYAMA
S. KATAYAMA Deep Penetration Welding with High Power Laser
Monitoring Apparatus and In-Process Control under Vacuum
Manufacturing by Laser, Practical Lecture Text for Proc. 29th Int. Congress on Applications of Lasers &
Chief Researchers and Engineers (2010), Electro-Optics (ICALEO 2010), (2010), pp.
pp. 5-65-5-89 (in Japanese). 648-653.
S. KATAYAMA, Y. KAWAHITO and M. MIZUTANI Y. KAWAHITO, Y. ABE, M. MIZUTANI and S. KATAYAMA

Elucidation of Laser Welding Phenomena and Factors High-Power and High-Brightness Laser Welding under
Affecting Weld Penetration and Welding Defects Low Vacuum
Physics Procedia, Vol. 5, Part 2 (2010), pp. 9-17. Proc. 74th Laser Materials Processing Conf., Vol. 74
(2010), pp. 19-23 (in Japanese).
S. KATAYAMA, Y. KAWAHITO and M. MIZUTANI
Laser Welding and Hybrid Welding of Aluminium H. SERIZAWA, I. SHIBAHARA, S. RASHED, H. MURAKAWA
Alloys and S. KUMAI
Proc. 12th Int. Conf. on Aluminium Alloys, (2010), Effect of Various Factors on Interface Formation in
pp. 908-914. Magnetic Pressure Seam Welding
Ceramic Engineering and Science Proc., Vol. 31,
S. KATAYAMA, K.-W. JUNG and Y. KAWAHITO No. 8 (2010), pp. 175-182.
High Power Laser Cutting of CFRP, and Laser Direct
Joining of CFRP to Metal A. KITAJIMA, M. TSUKAMOTO and J. AKEDO
Proc. 29th Int. Congress on Applications of Lasers & Hydroxyapatite Film Coated on Poly-L-Lactic Acid by
Electro-Optics (ICALEO 2010), (2010), pp. Aerosol Deposition Method
333-338. J. Ceram. Soc. Jpn., Vol. 118, No. 6 (2010),
pp. 417-420.
J.-B. WANG, H. NISHIMURA, S. KATAYAMA and
M. MIZUTANI M. TSUKAMOTO, H. NAKANO and N. ABE
Welding of Aluminum Alloy by Using Filler-Added Formation of Hydroxyapatite/titania Composite Film
Laser-Arc Hybrid Welding Process with Two Aerosol Beams
J. Light Metal Welding and Construction, Vol. 48, J. High Temperature Soc., Vol. 36, No. 4 (2010),
No. 11 (2010), pp. 12-22 (in Japanese). pp. 196-199.
P. VONDROUS, S. KATAYAMA and J. DUNOVSKY N. MATSUSHITA, N. SUGIYAMA, S. MARUYAMA, R. ITO,

Specifics of Laser Welding of Ductile Iron, Cr-Mo K. KATSUMATA, M. YOSHIMURA, M. TSUKAMOTO,
Steel and Their Dissimilar Butt Joints X. WANG, T. WADA, A. INOUE and K. OKADA
Proc. 74th Laser Materials Processing Conf., Vol. 74 Formation on Bone-Like Hydroxyapatite on
(2010), pp. 89-98. Surface-Modified Bulk Metallic Glass Using a
Hydrothermal-Electrochemical Method
S. KATAYAMA Ceram. Trans., Vol. 219 (2010), pp. 23-28.
Advances in Laser Materials Processing (Book)
Published by Woodhead Publishing Limited, (2010), M. TSUKAMOTO, T. SHINONAGA, N. MATSUSHITA,
pp. 181-210. X. WANG, T. WADA and N. ABE
Microstructure Formation on a Titanium-Based Bulk
Y. KAWAHITO and S. KATAYAMA Metallic Glass Plate by Femtosecond Laser Irradiation
In-process Monitoring and Adaptive Control during Ceram. Trans., Vol. 219 (2010), pp. 49-54.
Pulsed or CW Laser Welding
IIW Joint Workshop of Commission IV, VII and
SG212, Vol. 2010, No. 212-1173-10, XII- 1997-10,
IV-1036-10 (2010), pp. 1-16.
389
H. HONDA, M. TSUKAMOTO, N. ABE, T. SHINONAGA and A. KONDO, H. ABE, M. NAITO, Y. OKUNI, M. MIURA and
M. FUJITA N. ISU
Microstructures Formed on Stainless Steel by Novel Recycling Process of Waste FRP from
Femtosecond Laser Irradiation Advanced Materials
Ceram. Trans., Vol. 219 (2010), pp. 299-303. Ceram. Trans., Vol. 219 (2010), pp. 229-235.
T. NOMURA, M. TSUKAMOTO, N. ABE, M. TAKAHASHI and J. GUO, H. XU, S. WANG, S. ZHANG, H. ABE, X. WANG,
M. FUJITA Y. ZHAO and M. NAITO
Photoconductive Properties of Titanium Dioxide Film Eudragit Polymer Encapsulated Hydroxyapatite
by Femtosecond Laser Irradiation Microspheres as a Carrier for the Sustained Release of
Proc. 29th Int. Congress on Applications of Lasers & Small Molecular Drugs
Electro-Optics, (2010). Ceram. Trans., Vol. 219 (2010), pp. 265-272.
T. SHINONAGA, M. TSUKAMOTO, S. MARUYAMA, A. KONDO, H. ABE, N. ISU, M. MIURA, A. MORI,

N. MATSUSHITA, T. WADA, X. WANG, H. HONDA, T. OHMURA and M. NAITO
S. MOTOKOSHI and M. FUJITA Development of Light Weight Materials with Low
Variation of Topography on the Ti-Based Bulk Thermal Conductivity by Making Use of Waste FRP
Metallic Glass after Femtosecond Laser Irradiation J. Soc. Powder Technol. Jpn., Vol. 47, No. 11 (2010),
Proc. 29th Int. Congress on Applications of Lasers & pp. 768-772 (in Japanese).
Electro-Optics, (2010).
Z. TAN, H. ABE, M. NAITO and S. OHARA
M. TSUKAMOTO, N. ABE, J. MORIMOTO and J. AKEDO A Facile Method to Fabricate Palladium Nanoparticles
Periodic Microstructures Formation on Plastic Plate by Arrangement on Single-Walled Carbon Nanotubes
Aerosol Beam Irradiation J. Flux Growth, Vol. 5, No. 2 (2010), pp. 55-58.
J. High Temperature Soc., Vol. 36, No. 6 (2010),
pp. 300-302. Y. TSUJIMURA, H. TERASAKI, S. TASHIRO and M. TANAKA
Number Density Distributions of Metal Vapor in
M. NAITO, M. OKUMIYA, H. ABE, A. KONDO and Helium Gas Tungsten Arcs
C. C. HUANG Trans. Mater. Res. Soc. Jpn., Vol. 35, No. 3 (2010),
Powder Processing Issues for High Quality Advanced pp. 593-596.
Ceramics
KONA Powder and Particle J., No. 28 (2010), Y. SECHI, A. TAKEZAKI, T. MATSUMOTO, T. TSUMURA and
pp. 143-152. K. NAKATA
Composition Dependence of Titanium in
K. EWSUK, M. NAITO, T. KAKESHITA, S. KIRIHARA, Silver-Copper-Titanium Alloy Braze on Dissimilar
K. UEMATSU and H. ABE Laser Brazing of Boron Nitride Ceramics and
Characterization and Control of Interfaces for High Cemented Carbide
Quality Advanced Materials III (Book) J. JAPAN Inst. Metals, Vol. 74, No. 10 (2010),
Published by WILEY, (2010), pp. 265-402. pp. 643-649 (in Japanese).
M. NAITO, K. KANAMURA, H. MUNAKATA and H. MAKINO J. PURIC and A. KOBAYASHI

Advanced Powder Technology for Battery Novel Plasma Generating Systems for Advanced
Development (Book) Materials Processing
Published by The Nikkan Kogyo Shimbun, Ltd., Vacuum, Vol. 85 (2010), pp. 555-562.
(2010) (in Japanese).
Y. ANDO and A. KOBAYASHI
T. OHMURA, Y. ITO, I. ABE, H. ABE and M. NAITO Rapid Deposition of Titanium Oxide Film by
Fibrous Composite Powder Compacts for Thermal Atmospheric Thermal Plasma CVD Using Vortex Air
Insulation at High Temperature Plasma
Ceram. Trans., Vol. 219 (2010), pp. 123-128. Appl. Plasma Sci., Vol. 18, No. 2 (2010), in press
(in Japanese).
390
[Materials, Metallurgy & Weldability] S. LI, H. IMAI, H. ATSUMI and K. KONDOH
Phase Transformation and Precipitation Hardening
M. TAKAHASHI Behavior of Cr and Fe in BS40CrFeSn Alloy
Anodic Bonding - Its Principle and Potential for J. Mater. Sci., Vol. 45 (2010), pp. 5669-5675.
Application to Various Materials
NEW GLASS, Vol. 25, No. 3 (2010), pp. 7-12 S. LI, H. IMAI, H. ATSUMI and K. KONDOH
(in Japanese). Contribution of Ti Addition to Characteristics of
Extruded Cu40Zn Brass Alloy Prepared by Powder
M. WAHBA, S. KATAYAMA, T. KURODA and H. KIMURA Metallurgy
Laser Welding of Zn55Cu30Al10N5 Bulk Metallic Glass Mater. Des., Vol. 32 (2010), pp. 192-197.
Ceram. Trans., Vol. 219 (2010), pp. 73-79.
K. KONDOH, K. KANEKO and T. AKITA
S. KATAYAMA and M. MIZUTANI Advanced Powder Metallurgy Metals by Metal
Formation and Prevention of Porosity in Laser Working
Welding and Hybrid Welding Steel Res. Int., Vol. 81, No. 9 (2010), pp. 1283-1287.
Proc. 50 Years Memorial Symp. for Foundation of
Welding Metallurgy Research Committee of Japan H. IMAI, K. KONDOH, S. LI, H. ATSUMI, Y. KOSAKA and
Welding Society, -Advance and Innovation in study A. KOJIMA
of Welding Metallurgy-, (2010), pp. 24-27 Effect of Bismuth Addition on Machinability and
(in Japanese). Mechanical Properties of Lead-free Brass via Powder
Metallurgy Process
S. KATAYAMA Steel Res. Int., Vol. 81, No. 9 (2010), pp. 1296-1299.
Laser Joining of Metal and Plastic
Industrial Laser Solutions for Manufacturing, (2010), S. LI, H. IMAI, H. ATSUMI and K. KONDOH
pp. 15-16. Effects of Ti Addition on Microstructure and
Mechanical Properties of Extruded Cu40Zn-2.2Bi
S. KATAYAMA and T. OGAWA Brass by Powder Metallurgy
Laser Weldability and Aging Characteristics of Welds Steel Res. Int., Vol. 81, No. 9 (2010), pp. 1312-1315.
-Laser Weldability of Commercially Available A7N01
Alloy(1)- T. THRERUJIRAPAPONG, K. KONDOH, H. IMAI, J. UMEDA
J. Light Metal Welding and Construction, Vol. 48, and B. FUGETSU
No. 12 (2010), pp. 5-16 (in Japanese). Hot Extrusion of Pure Titanium Reinforced with
Carbon Nanotubes
M. WAHBA, M. MIZUTANI, Y. KAWAHITO and Steel Res. Int., Vol. 81, No. 9 (2010), pp. 1320-1323.
S. KATAYAMA
High-Brightness Disk Laser Welding of Magnesium S. LI, H. IMAI, H. ATSUMI and K. KONDOH
Alloys Precipitation Hardening Response of Ti Addition on
Proc. 29th Int. Congress on Applications of Lasers & BS40 Brass by Powder Metallurgy
Electro-Optics (ICALEO 2010), (2010), pp. CD Proc. World PM2010: Int. Powder Metallurgy
429-435. Congress & Exhibition, (2010), CD-ROM.
Y. KAWAHITO and S. KATAYAMA T. THRERUJIRAPAPONG, K. KONDOH, H. IMAI, J. UMEDA

Characteristics of LAMP Joining Structures for Several and B. FUGETSU
Materials Advantages of a Wet Process for the Production of Ti
Proc. 29th Int. Congress on Applications of Lasers & Matrix Composite Reinforced with Carbon Nano
Electro-Optics (ICALEO 2010), (2010), pp. Materials by Powder Metallurgy Route
1469-1473. CD Proc. World PM2010: Int. Powder Metallurgy
Congress & Exhibition, (2010), CD-ROM.
N. NAKANISHI, H. IMAI, K. KONDOH and H. FUJII
Wettability of Ti by Molten Mg-Al Alloy N. NAKANISHI, H. IMAI and K. KONDOH
J. High Temperature Soc., Vol. 36, No. 4 (2010), Wettability Evaluation of Pure Ti by Molten Mg Alloy
pp. 192-195 (in Japanese). Droplet for Materials Design of P/M Mg Composite
Alloy Reinforced with Ti Particles
CD Proc. World PM2010: Int. Powder Metallurgy
Congress & Exhibition, (2010), CD-ROM.
391
K. KONDOH, R. TAKEI, H. FUKUDA, J. UMEDA and H. IMAI T. MIYAZAWA, Y. IWAMOTO, T. MARUKO and H. FUJII
SKPFM Quantitative Evaluation of Initial Galvanic Development of Ir Based Tool for Friction Stir
Corrosion Phenomenon of Magnesium Alloys Welding of High Temperature Materials
Proc. Materials Science & Technology (MS&T) Q. J. Jpn. Weld. Soc., Vol. 28, No. 2 (2010),
2010, (2010), pp. 745-752. pp. 203-207 (in Japanese).
T. JONES, K. KONDOH and B. PLACZANKIS Y. D. CHUNG, H. FUJII, R. UEJI and N. TSUJI

The Development of Superior Magnesium Alloy Friction Stir Welding of High Carbon Steel with
AMX602 Using a Novel Rapid Solidification Process Excellent Toughness and Ductility
for Structural Applications Scr. Mater., Vol. 63 (2010), pp. 223-226.
Proc. Materials Science & Technology (MS&T)
2010, (2010), pp. 2008-2019. Y. F. SUN, N. TSUJI, H. FUJII and F. S. LI
Cu/Zr Nanoscaled Multi-Stacks Fabricated by
K. KONDOH, T. THRERUJIRAPAPONG and J. UMEDA Accumulative Roll Bonding
Carbon Nanotube Reinforced Pure Titanium Powder J. Alloy. Compd., Vol. 504 (2010), pp. 443-447.
Composite Materials by Using Zwitterionic Surfactant
Solution H. FUJII
Proc. Materials Science & Technology (MS&T) Friction Stir Welding and Processing of Ferrous Alloys
2010, (2010), pp. 2233-2238. Papers for 50th Anniversary Symp. of Welding
Metallurgy of Japan Welding Society, (2010), pp.
H. ATSUMI, H. IMAI, S. LI, Y. KOSAKA, A. KOJIMA and 73-76 (in Japanese).
K. KONDOH
Microstrucutre and Mechanical Properties of High Y. F. SUN and H. FUJII
Strength Brass Alloy with Some Elements Investigation of the Welding Parameter Dependent
Trans. Jpn. Soc. Mech. Eng. -Part A, Vol. 76, Microstructure and Mechanical Properties of Friction
No. 771 (2010), pp. 1501-1508 (in Japanese). Stir Welded Pure Copper
Mater. Sci. Eng. A., Vol. 527 (2010), pp. 6879-6886.
H. FUKUDA, J. A. SZPUNAR, K. KONDOH and R. CHROMIK
The Influence of Carbon Nanotubes on the Corrosion K. IMAGAWA, H. FUJII, Y. YAMAGUCHI and S. KIGUCHI
Behaviour of AZ31B Magnesium Alloy Surface Hardening of Ferritic Spheroidal Graphite Cast
Corrosion Sci., Vol. 52 (2010), pp. 3917-3923. Iron by Friction Stir Processing
J. Jpn. Foundry Soc., Vol. 82, No. 11 (2010),
K. KONDOH pp. 674-679 (in Japanese).
Handbook of Powder and Powder Metallurgy (Book)
Published by Uchida Rokakuho Publishing Co., Z. TAN, H. CHIHARA, C. KOIKE, H. ABE, K. KANEKO,
Ltd., , (2010) (in Japanese). K. SATO and S. OHARA
Interstellar Analogues from Defective Carbon
J. UMEDA, M. KAWAKAMI, K. KONDOH, E.-S. A. HAMADA Nanostructures Account for Interstellar Extinction
and H. IMAI Astron. J., Vol. 140 (2010), pp. 1456-1461.
Microstructural and Mechanical Properties of Titanium
Particulate Reinforced Magnesium Composite S. KIRIHARA, Y. UEHARA and Y. TAKINAMI
Materials Fabrication of Thermodynamic Crystals by Structural
Mater. Chem. Phys., Vol. 123 (2010), pp. 649-657. Joining
Proc. 34th Int. Conf. Advanced Ceramics and
A. ELSAYED, H. IMAI, J. UMEDA and K. KONDOH Composites, Vol. 31, No. 8 (2010), pp. 169-174.
Microstructure and Mechanical Properties of Hot
Extruded ZK61 Alloy Produced by Rapid M. SUWA, S. KIRIHARA and T. SOHMURA
Solidification Powder Metallurgy Fabrication of Alumina Dental Crown Model with
Steel Res. Int., Vol. 81, No. 9 (2010), pp. 1304-1307. Biomimetic Structure by Using Stereolithography
Proc. 34th Int. Conf. Advanced Ceramics and
J. UMEDA and K. KONDOH Composites, Vol. 31, No. 8 (2010), pp. 239-245.
High-purification of Amorphous Silica Originated
from Rice Husks by Combination of Polysaccharide
Hydrolysis and Metallic Impurities Removal
Ind. Crop. Prod., Vol. 32 (2010), pp. 539-544.
392
Y. TAKINAMI and S. KIRIHARA S. KIRIHARA, N. OHTA, T. NIKIL and M. KANEKO
Fabrication of Microwave Structures through Terahertz Wave Properties of Alumina Photonic
Dielectric Materials Percolation into Metal Patterns Crystals
J. Functionally Graded Mater., Vol. 20 (2010), Ceram. Trans., Vol. 216 (2010), pp. 121-127.
pp. 31-36 (in Japanese).
S. KIRIHARA, T. NIKIL and M. KANEKO
C. MAEDA, M. SUWA and S. KIRIHARA Terahertz Wave Harmonization in Geometrically
Fabrication of Artificial Bone Models with Graded Patterned Dielectric Ceramics Through Spatially
Porous Scaffold Structures Composed of Structural Joining
Hydroxyapatite Ceramics by Using Stereolithography Ceram. Trans., Vol. 216 (2010), pp. 113-119.
J. Functionally Graded Mater., Vol. 20 (2010),
pp. 37-40 (in Japanese). M. SUWA, S. KIRIHARA and T. SOHMURA
Freeform Fabrication and Structural Controls of
M. SHAHIEN, M. RADWAN, S. KIRIHARA, Y. MIYAMOTO Alumina Dental-Crown Models by Using
and T. SAKURAI Stereolithography
Combustion Synthesis of Single-Phase Ǻ-Sialons Ceram. Trans., Vol. 218 (2010), pp. 213-220.
(z=2-4)
J. Eur. Ceram. Soc., Vol. 30, No. 9 (2010), S. KIRIHARA, N. KOMORI and N. OHTA
pp. 1925-1930. Smart Processing for Ceramics Structure Tectonics:
Fabrication of Dielectric Micro Patterns for Artificial
N. OHTA, T. NIKI and S. KIRIHARA Photosynthesis in Terahertz Wave Regions by Using
Terahertz Wave Concentrations into Micro Reactors Stereolithography
Including Water Solvents Introduced into Alumina Adv. Sci. Technol., Vol. 63 (2010), pp. 141-146.
Photonic Crystals with Diamond Structures
J. Functionally Graded Mater., Vol. 20 (2010), Y. KOMIZO
pp. 13-18 (in Japanese). Welding Metallurgy I-2 Metallurgy for Welding of
Steel Materials
S. KIRIHARA, D. SANO, T. NIKI, N. OHTA and Textbook for summer school of welding engineering,
Y. TAKINAMI (2010), pp. 89-106 (in Japanese).
Fabrication of Micro Photonic Crystals for Handling of
Terahertz Electromagnetic Waves T. KANNENGIESSER, S. S. BABU, Y. KOMIZO and
Proc. Nanotech Conf. & Expo 2010, Vol. 2 (2010), A. J. RAMIREZ
pp. 223-226. In-situ Studies with Photons, Neutrons and Electrons
Scattering (Book)
S. KIRIHARA, N. KOMORI, M. NAKANO, N. OHTA and Published by Springer, (2010).
T. NIKI
Terahertz Wave Properties of Micro Patterned Titania D. ZHANG, H. TERASAKI and Y. KOMIZO
and Metallic Glass Particles in Hexagonal Tablet In Situ Observation of Phase Transformations in
Fabricated Using Microstereolithography Fe-0.08C Alloy
Ceram. Trans., Vol. 219 (2010), pp. 61-66. Ceram. Trans., Vol. 219 (2010), pp. 397-402.
M. SUWA, S. KIRIHARA and T. SOUMURA T. YAMADA, H. TERASAKI and Y. KOMIZO

Fabrication of Alumina Dental Crowns Using Mechanism of Acicular Ferrite Formation in Low
Stereolithography Carbon Steel Ti-B Weld Metals with Different Oxygen
Ceram. Trans., Vol. 219 (2010), pp. 331-336. Levels
Tetsu-to-Hagane, Vol. 96, No. 10 (2010),
T. NIKI and S. KIRIHARA pp. 608-613 (in Japanese).
Fabrication of Alumina Diamond Photonic Crystals
with Twinned Interfaced to Develop Terahertz Wave S. ZHANG, H. TERASAKI and Y. KOMIZO
Resonators In-situ Observation of Martensite Transformation and
Ceram. Trans., Vol. 219 (2010), pp. 325-330. Retained Austenite in Supermartensitic Stainless Steel
Tetsu-to-Hagane, Vol. 96, No. 12 (2010),
393
H. TERASAKI T. TAKAHASHI, S. KOMATSU, H. NISHIKAWA and
In-situ Studies with Photons, Neutrons and Electrons T. TAKEMOTO
Scattering (Book) High-Temperature Resistant Intermetallic Compound
Published by Springer, (2010). Joints for Si Chips and Cu Substrates
J. Electron. Mater., Vol. 39, No. 10 (2010),
T. DAITO, H. NISHIKAWA, T. TAKEMOTO and pp. 2274-2280.
T. MATSUNAMI
Impact Test of Sn-3.0Ag-0.5Cu (-xCo) Solder with W. CHEN, Y. MIYAMOTO, T. MATSUMOTO and T. TOJO
Co-P Plating Spark Plasma Sintering of Carbon Particles Coated
Proc. Int. Conf. on Electronics Packaging 2010 with Al2O3 Ceramic
(ICEP 2010), (2010), pp. 796-799. Ceram. Trans., Vol. 219 (2010), pp. 285-291.
H. NISHIKAWA, K. WONGPIROMSARN, H. ABE, W. CHEN, Y. MIYAMOTO, T. MATSUMOTO and T. TOJO

T. TAKEMOTO, M. KUBO, Y. SANAGAWA, T. SAKAI, Preparation of AlN Ceramic Bonded Carbon by
M. FUKUHARA and A. INOUE Gelcasting and Spark Plasma Sintering
Low Temperature Bonding of Bulk Metallic Glass Carbon, Vol. 48 (2010), pp. 3399-3404.
Using an Ultrasonic Process
Ceram. Trans., Vol. 219 (2010), pp. 29-35. M. NAKAMURA, Y. MIYAMOTO, T. MATSUMOTO and
T. TOJO
H. NISHIKAWA, F. GAO, A. KOMATSU and T. TAKEMOTO Fabrication and Densification of SiC Coated Carbon
Grain Morphology and Mechanical Property of Microparticles
Intermetallic Compound at Interface between Co Ceram. Trans., Vol. 219 (2010), pp. 305-310.
Added Solder and Cu
J. JRICu, Vol. 49, No. 1 (2010), pp. 121-124 D. HUANG, Y. MIYAMOTO, T. MATSUMOTO, T. TOJO,
(in Japanese). T. FAN, J. DING, Q. GUO and D. ZHANG
Fabrication of Nano-TiO2 Coated Morphgenetic
L.-N. HO, T.-F. WU, H. NISHIKAWA and T. TAKEMOTO Carbon and Its Photocatalytic Performance
Electrical Properties of Pre-Alloyed Cu-P Containing Ceram. Trans., Vol. 219 (2010), pp. 385-390.
Electrically Conductive Adhesive
J. Adhes., Vol. 86 (2010), pp. 805-813. M. NAKAMURA, Y. MIYAMOTO and T. TOJO
Development of Novel SiC/CBC (Ceramic Bonded
T. TAKAHASHI, S. KOMATSU, H. NISHIKAWA and Carbon) with 3D Micro-network Structure
T. TAKEMOTO J. Jpn. Soc. Powder Powder Metal., Vol. 57, No. 11
Improvement of High-Temperature Performance of (2010), pp. 711-715 (in Japanese).
Zn-Sn Solder Joint
J. Electron. Mater., Vol. 39, No. 8 (2010), Y. MIYAMOTO, M. NAKAMURA, W. CHEN and T. TOJO
pp. 1241-1247. Development of New Composites; Ceramic Bonded
Carbon
H. NISHIKAWA J. Functionally Graded Mater., Vol. 24 (2010),
Conductive Filler for Technical Advantages of pp. 88-93 (in Japanese).
Conductive Adhessives
J. Jpn. Weld. Soc., Vol. 79, No. 6 (2010), Y. MIYAMOTO
pp. 550-555 (in Japanese). Handbook of Powder and Powder Metallurgy (Book)
Published by Uchida Rokakuho Publishing Co., Ltd., ,
H. NISHIKAWA, S. MIKAMI, K. MIYAKE, A. AOKI and (2010) (in Japanese).
T. TAKEMOTO
Effects of Silver Coating Covered with Copper Filler H. WATANABE, M. SHIMODA, N. HIDAKA and I. SHOHJI
on Electrical Resistivity of Electrically Conductive Effect of Ni and Ag on Interfacial Reaction and
Adhesives Microstructure of Sn-Ag-Cu-Ni-Ge Solder Alloy
Mater. Trans., Vol. 51, No. 10 (2010), pp. 1785-1789. Proc. 8th Int. Conf. on Fracture and Strength of
Solids, (2010), Paper ID A064.
394
A. KOBAYASHI, T. KURODA, H. KIMURA and A. INOUE K. TOKUNAGA, N. TSUKUDA, N. YOSHIDA, Y. YAHIRO,
Microstructure and Properties of a Ni-Based Metallic M. MITSUHARA, H. NAKASHIMA, A. KOBAYASHI,
Glass Coating Produced by Gas Tunnel Type Plasma K. EZATO, S. SUZUKI and M. AKIBA
Spraying Tungsten Coatings on Reduced-Activation
Ceram. Trans., Vol. 219 (2010), pp. 37-42. Ferritic/Martensitic Steel by Plasma Spray Technique
Appl. Plasma Sci., Vol. 18, No. 2 (2010), in press
A. KOBAYASHI, T. KURODA, H. KIMURA and A. INOUE (in Japanese).
Microstructure and Properties of Zr-Based Metallic
Glass Coatings by Gas Tunnel Type Plasma Spraying
Appl. Plasma Sci., Vol. 18, No. 1 (2010), pp. 43-50 [Mechanics, Strength & Structural Design]
(in Japanese).
A. MAEKAWA, K. NAKACHO, N. MA and R. SATO
T. KURODA, A. KOBAYASHI and K. IKEUCHI Residual Stresses Measurement of Large-Bore
Microstructure and Toughness for Resistance Butt Stainless Steel Pipe with Butt-Welded Joint by
Welding of Super Duplex Stainless Steel Inherent Strain Method
Appl. Plasma Sci., Vol. 18, No. 1 (2010), pp. 57-63 Proc. 2010 Annual Meeting of JSME/MMD, (2010),
(in Japanese). pp. 1260-1262 (in Japanese).
M. F. MORKS and A. KOBAYASHI H. SERIZAWA, S. NAKAMURA, H. TANIGAWA, T. HIROSE,

Plasma Spraying of Zirconia-Titania-Silica Composite M. ENOEDA and H. MURAKAWA
Coating for Implant Application Measurement and Numerical Analysis of Welding
Front. Appl. Plasma Technol., Vol. 3, No. 2 (2010), Residual Stress in Box Structure Employed for Breeder
pp. 113-116. Blanket System of ITER
A. KOBAYASHI, T. KURODA, H. KIMURA and A. INOUE (2010), IIW Doc. X-1671-10.
Microstructure of Metallic Glass Coatings Sprayed by
Gas Tunnel Type Plasma Spraying S. NAKAMURA, H. SERIZAWA, H. TANIGAWA and
III Conferencia Internacional de Soldadure y Union H. MURAKAWA
de Materiales ICWJM 2010, (2010), CD. Influence of Cooling Channel in First and Side Walls
on Welding Residual Stress of Test Blanket Module for
H. WAKI, T. KITAMURA and A. KOBAYASHI ITER
High Temperature Fatigue of Free-Standing 63rd Annual Assembly of Int. Inst. Welding (IIW),
CoNiCrAlY Sprayed Coatings (2010), IIW Doc. X-1672-10.
Proc. 12th Int. Conf. on Plasma Surface Engineering,
(2010), HP, OR2607. Y.-C. KIM, J.-Y. LEE and K. INOSE
Determination of Dominant Factors in High Accuracy
A. KOBAYASHI, T. KURODA, H. KIMURA and A. INOUE Prediction of Welding Distortion
Effect of Spraying Condition on Property of Zr-based Welding in the World, Vol. 54, No. 7/8 (2010),
Metallic Glass Coating by Gas Tunnel Type Plasma pp. R234-R240.
Spraying
Mater. Sci. Eng. B, Vol. 173 (2010), pp. 122-125. Y.-C. KIM, M. HIROHATA, Y. HAGEYAMA and K. INOSE
Distortion and Residual Stress Generated by Laser
A. KOBAYASHI, T. KURODA, H. KIMURA and A. INOUE Beam Welding of High Strength Stee;
Mechanical Properties and Microstructure of Plasma Q. J. Jpn. Weld. Soc., Vol. 28, No. 3 (2010),
Sprayed Ni-Based Metallic Glass Coating pp. 281-287 (in Japanese).
New Trend in Appl. Plasma Sci. Technol., Vol. 1282
(2010), pp. 33-38. H.-S. BANG, H.-S. BANG, Y.-C. KIM and S.-M. JOO
Analysis of Residual Stress on AH32 Butt Joint by
A. KOBAYASHI, Y. ANDO, K. KUROKAWA and Hybrid CO2 Laser-GMA Welding
T. HEJWOWSKI Computational Mater. Sci., Vol. 49 (2010),
Microstructure and Thermal Behaviour of Plasma pp. 217-221.
Sprayed Zirconia/Alumina Composite Coating
J. Nanosci. Nanotechnol., Vol. 11 (2010), in press.
395
Y. AGANO, S. FUJIHIRA, S.-H. LEE and Y.-C. KIM Y.-C. KIM, M. HIROHATA and K. INOSE
Experimental Study on Repair Welding under Static Effects of Phase Transformation on Distortion and
and Cyclic Loads Residual Stress Generated by LBW on High Strength
Proc. Int. Conf. on Bridge Maintenance, Safety and Steel
Management, Life-Cycle Optimization, CD-ROM 63rd Annual Assembly of Int. Inst. Welding (IIW),
(2010), pp. 2998-3004. (2010), IIW Doc. XV-1353-10, IIW Doc.
IV-1033-10.
M. HIROHATA and Y.-C. KIM
Identification of Factor Determining Strength under Y. SAKINO, T. KURODA, A. KOBAYASHI and Y.-C. KIM
Compressive Loads of Steel Members Corrected by Fracture Behavior of Zr48Cu36Al8Ag8 and
Heating/Pressing Zr55Cu30Al10Ni5 Bulk Metallic Glasses in High Speed
Int. J. Steel Structures, Vol. 10, No. 3 (2010), Tensile Test
pp. 245-251. Front. Appl. Plasma Technol., Vol. 3, No. 2 (2010),
pp. 102-106.
J.-Y. LEE, K. INOSE and Y.-C. KIM
Verification of Validity and Generality of Dominant Y. SAKINO, T. KURODA and Y.-C. KIM
Factors in High Accuracy Prediction of Welding Tensile Mechanical Behavior of Zr-based Bulk
Distortion Metallic Glass in High-speed Tensile Tests
Welding in the World, Vol. 54, No. 9/10 (2010), Ceram. Trans., Vol. 219 (2010), pp. 43-47.
pp. R279-R285.
Y. SAKINO and Y.-C. KIM
D.-H. PARK, M. HIROHATA and Y.-C. KIM Effect of Welded Condition on Charpy Absorbed
Effects of 3-D Welding Residual Stress on Energy of Heat Affected Zones in Low Toughness
Elastic-plastic Behavior of Steel Structural Member Steel
J. Constructional Steel, Vol. 18 (2010), pp. 151-158 Steel Constr. Eng., Vol. 17, No. 67 (2010),
(in Japanese). pp. 43-52.
Y. AGANO, S.-H. LEE, S. FUJIHIRA and Y.-C. KIM Y. SAKINO, S. TAKAHASHI and Y.-C. KIM
Effects of Static Loads on Weldability Effects of Strain Rate on Tensile Strength of Steel
—Repair/Reinforcement by Welding for Steel Bridges Specimens of HAZs with Stress Concentrations
in Service— Q. J. Jpn. Weld. Soc., Vol. 28, No. 3 (2010),
Q. J. Jpn. Weld. Soc., Vol. 28, No. 4 (2010), pp. 328-337 (in Japanese).
Y. SAKINO, K. YOSHIKAWA, Y. SANO and Y.-C. KIM
Y. AGANO, S.-H. LEE, S. FUJIHIRA and Y.-C. KIM Residual Stress of High Strength Steel and Its Welds
Verification of Weldability under Cyclic Loads Generated by Laser Peening
—Repair/Reinforcement by Welding for Steel Bridges J. Constructional Steel, Vol. 18 (2010), pp. 493-498
in Service— (in Japanese).
Q. J. Jpn. Weld. Soc., Vol. 28, No. 4 (2010),
pp. 436-442 (in Japanese). Y. SAKINO and Y.-C. KIM
Effect of Multilayered Thermal Cycle on Charpy
D.-H. PARK, M. HIROHATA, S. TAMAGAWA and Y.-C. KIM Absorbed Energy in Heart Affected Zone
Introducing/Reproducing of Welding Distortion and J. Constructional Steel, Vol. 18 (2010), pp. 253-258
Residual Stress in Analysis for Elastic-Plastic (in Japanese).
Behaviors of Steel Plates under Compressive Loads
Int. J. Steel Structures, Vol. 10, No. 4 (2010), T. TERAJIMA, F. TAKEUCHI, K. NAKATA, S. ADACHI,
pp. 349-357. K. NAKASHIMA and T. IGARASHI
Composite Coating Containing WC/12Co Cermet and
D.-C. PARK, M. HIROHATA and Y.-C KIM Fe-based Metallic Glass Deposited by High-Velocity
Consideration for Welding Imperfection in Oxygen Fuel Spraying
Elastic-plastic Large Deformation Analysis J. Alloy. Compd., Vol. 504 (2010), pp. S288-S291.
(2010), IIW Doc. XV-1352-10.
396
[General Welding]
S. KATAYAMA
Laser Welding of Dissimilar Materials
Rev. Laser Eng., Vol. 38, No. 8 (2010), pp. 594-602
(in Japanese).
T. TERAJIMA, K. NAKATA, H. KIMURA and A. INOUE

Laser Butt Welding of The Mg-Based Metallic Glass
Ceram. Trans., Vol. 219 (2010), pp. 55-60.
397
Editorial Members
Chairman ···································· NAITO Makio
TANAKA Manabu
KATAYAMA Seiji
KIM You-Chul
FUJII Hidetoshi
ABE Hiroya
Published by
Joining and Welding Research Institute,
Osaka University
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Telephone (06) 6877-5111
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Published in December 2010
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ISSN 0387-4508

JOINING AND WELDING RESEARCH INSTITUTE

JOINING AND WELDING RESEARCH INSTITUTE

Three-dimensional computational modelling of MIG welding

Three-dimensional simulation of a flow in an arc weld pool by SPH method

A Study on the macro-micro physical properties in pulsed arc plasma

Evaporation phenomena of magnesium during pulsed-MIG arc welding of aluminum alloy

Study on defect in the intersection of VPPA and FSW

Simulations of weld pool dynamics and theis visualization

Development of a high-efficiency / high-quality hot-wire laser fillet welding process

Innovation of laser direct joining between metal and plastic

Optimising residual stress measurements through the use of measurement simulation

Residual stress generated by LBW on HT780

Comparison on several kinds of T-E-P FEM software for welding

Finite element simulation of multi-pass welding process with rezoning technique

Prediction and measurement of welding distortion of thin shell structure

Investigation on ductility dip cracking susceptibility of filler metal 82 in welding

Microstructure and mechanical properties of overlaying specimens in GMAW hybrid

Development of simulation system JWELD for assemble deformation of welded structures

In-situ observation of phase transformation during laser welding processes

Numerical simulation on type IV cracking of ASME P92 steel at high temperature

Numerical simulation of austenite retention in triplex stainless steel weld metals

Visualizations of microwave emissions through pure copper photonic crystals

Weld process management using data visualization

Repair heavy-duty generator rotor shaft by electro spark deposition process

Visualization of nugget formation in resistance spot welding of multi-stackup sheets

Efficiency comparison between iterative substructure method and commercial software

Measurement of dynamical variation in two-dimensional temperature distribution of TIG pulsed-arcs

Mechanism of undercut in high speed welding based on moveless TIG welding

Numerical analysis the influence of arc shape on metal transfer process

In-process monitoring and adaptive control for micro welding of titanium

Numerical analysis on heat source characteristics of two-electrodes TIG arc

Influence of magnet configurations on magnetic controlled TIG arc welding

Visualization of EM process by FEM

Metallurgical mechanism of ductility-dip cracking in multipass welds of alloy 690

Formation of reaction layers at anodically-bonded metallc glass/silicate glass interfaces

Thermoreversible colloidal gelation for direct-assembly of nanoparticles

Dispersion control of magnetic nanoparticles for functional fluids

Molecular dynamics analysis of fcc nanowire under torsional loading

Observation of hole formation process in plasma arc drilling

Cooperative researches in Tohoku University

Synthesis and properties of hybrid-type polymer membranes for fuel cells

Evolution of laser welding to dissimilar materials joining

Introduction to vector materials science and bioengineering

Preparation of metal nano particles using electrochemical deposition

Application to catalyst of mayenite consisting of ubiquitous elements

Arrangement of Pd nanoparticles on SDS-functionalized single-walled carbon nanotubes

Nano-carbon structures on silicon carbide

Superconductivity of Ni0.324Nb0.216Zr0.36H0.1 glassy alloys

Local structures of amorphous (Ni0.6Nb0.4)100-xZrx(x=30, 35, 40) alloys by XAFS

Single layer PDMS flexible parallel wall microvalvets

Responses of osteoblast to surface modified bulk metallic glass

Joining of ceramic nanocrystals and bio-molecules towards bio-medical applications

Cu-based metallic glass surfacemodified with Cu for soldering

Shock-assisted joining between metallic glass and ceramics

Development of plasma MIG brazing process of advanced materials

Measurement of fracture behavior of Zr-based metallic glass by thermography

Inter-granular cracking of a splat of zirconia coating fabricated by plasma spraying technique

Tungsten coatings on reduced-activation ferritic/martensitic steel by plasma spray technique

Behavior of arc plasma for thermal barrier coating preparation

Dissimilar laser brazing of single crystal diamond and tungsten carbide

Control of wire melting behavior using coaxial hybrid solid wire

Newly developed novel transparent conductor of Mg(OH)2-C compounds

TAKASE Kazuyuki, MURAMATSU Toshiharu, SHOBU Takahisa

CHO Dae-Won,NA Suck-Joo, CHO Min-Hyun and LEEJong-Sub

SHIGETA Masaya, ITO Masumi, IZAWA Seiichiro* and FUKUNISHI Yu*

† Received on 30 September 2010. 㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌㻌 Transactions of JWRI is published by Joining and Welding

LIU Zuming, WANG Xiaojie, WU Chuan Song*

WANG Jing-Bo, NISHIMURA Hitoshi, KATAYAMA Seiji and MIZUTANI Masami