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Physics, Mechanics & Astronomy


• Research Paper • August 2011 Vol.54 No.8: 1447–1454
doi: 10.1007/s11433-011-4401-2

Embrittlement and toughening in CGHAZ of ASTM4130 steel


LI LiYing*, WANG Yong*, HAN Tao & LI ChaoWen
College of Mechanical and Electronic Engineering, China University of Petroleum, Dongying 257061, China

Received December 16, 2010; accepted March 17, 2011; published online July 1, 2011

In the present investigation, a thermal welding simulation technique was used to investigate the mechanical properties and mi-
crostructure features of the coarse-grained heat-affected zone (CGHAZ) of ASTM4130 steel. The effect of post welding heat
treatment (PWHT) and welding heat inputs on the toughness of CGHAZ was also analyzed. The results show that CGHAZ has
the lowest toughness, which is only 5.5%–7.1% of the base metal. CGHAZ is mainly composed of dislocation martensite, up-
per and lower bainite, and M-A constituents. But after PWHT, carbides precipitate from non-equilibrium microstructures of
CGHAZ accompanying some retained austenite which transforms into low bainite, thereby enhancing toughness over the base
metal. Therefore, the key microstructure factors affecting fracture toughness are lathlike non-equilibrium microstructure and
lowered supersaturation before and after PWHT respectively. When welding heat input is between 12 kJ/cm and 28 kJ/cm, the
mechanical properties in CGHAZ of ASTM4130 with single-pass welding can satisfy the requirements when PWHT is ap-
plied.

ASTM4130 steel, coarse-grained heat-affected zone, embrittlement, toughening


PACS: 81.20.Vj, 81.30.-t, 81.40.-z, 81.70.-q

The balance of strength and toughness in the weld heat- microstructural and mechanical properties. Therefore, the
affected zone (HAZ) is usually upset due to the effect of aim of the present work is to systematically investigate the
welding thermal cycles. Generally speaking, the coarse- effect of welding heat input and post weld heat treatment
grained HAZ (CGHAZ) possesses the lowest toughness (PWHT) on microstructure and low temperature impact
which controls the failure of welded steel structures. In this toughness in CGHAZ of ASTM4130 steel pipes welded
region, the degraded fracture performance is associated with under quenched and tempered (Q&T) conditions by means
the formation of coarse-grained microstructures, represent- of thermal welding simulation techniques.
ing brittle-hard phases, such as untempered martensite and
martensite-autensite (M-A) constituents [1–3]. As one kind
of Cr-Mo steel, ASTM 4130 steel exhibits high strength-to- 1 Experimental material and procedures
weight ratio and excellent low temperature toughness, and
has been widely used in oil and gas production efforts, such The ASTM4130 steel pipe used in the experiments is
as tubing, tubular components, drilling blowout preventers, 141.3 mm×30 mm, and the measured chemical composi-
etc. However, its weldability is not desirable due to its car- tion is given in Table 1.
bon equivalent CEIIW up to 0.73. In addition, since HAZ is A thermal welding simulation experiment was done us-
generally narrow and discontinuous, a welding thermal ing Gleeble-1500. Square bar specimens (10.5 mm×10.5
simulator is often employed to produce a large volume of mm×80 mm) for the thermal cycle simulation were cut
uniform microstructure, which is suitable for assessment of along the axial direction parallel to the pipe. The specimens
were uniformly heated at 130°C/s to five peak temperatures
*Corresponding author (email: llying3456@163.com; wangyong@upc.edu.cn) (Tp) corresponding to the subcritical HAZ (SCHAZ, 700°C),

© Science China Press and Springer-Verlag Berlin Heidelberg 2011 phys.scichina.com www.springerlink.com
1448 Li L Y, et al. Sci China Phys Mech Astron August (2011) Vol. 54 No. 8

Table 1 Chemical composition of ASTM4130 steel (wt.%) CGHAZ has the lowest toughness, which is only about
C Si Mn Cr Mo Ni S P Fe
5.5% of the BM. However, hardness shows an opposite
trend compared to impact toughness. At a Tp of 1350°C,
0.32 0.355 0.62 1.15 0.25 0.17 0.004 0.010 balance
hardness is almost two times greater than that of BM.
Data describing the properties of CGHAZ before and af-
ter PWHT are presented in Table 2. The toughness and
the intercritical HAZ (ICHAZ, 800°C), the fine-grained
hardness of CGHAZ as-welded are extremely low and high
HAZ (FGHAZ, 950°C) and the coarse-grained HAZ
respectively, regardless of the welding heat input. However,
(CGHAZ, 1200°C and 1350°C). The specimens were held
the toughness of CGHAZ subjected to PWHT is remarkably
at the Tp value for 2 s. The cooling rates t8/5, as defined by
increased. Moreover, the hardness obviously declines. It can
the thick-plate formula, were 6.4 s, 10.6 s, and 14.9 s for
be noted that PWHT has a significant effect on the proper-
heat inputs corresponding to 12, 20, and 28 kJ/cm, respec-
ties of CGHAZ. In addition, it is interesting to find that the
tively, and the preheat temperature was 200°C.
specimens having high impact toughness and hardness be-
PWHT of specimens undergoing Tp of 1350°C was car-
fore PWHT show the lowest toughness and hardness after
ried out in a box furnace. Heat treatment conformed to JB/T
PWHT.
6046-1992. The temperature of the treatment was 640°C,
and the holding time was 1.5 h. The heating and cooling
rates were 120°C/h and 150°C/h above 300°C, respectively. 2.2 Microstructures
After the simulation test, the simulated CGHAZ speci-
2.2.1 Microstructure of BM
mens were sectioned, polished, and etched by 4% nitric
solution, following Labara [4] and two-step metallographic Figure 2(a) is an optical micrograph of BM. As can be seen,
etching [5]. Their microstructures were observed by an op- BM consists of typical tempered sorbite with ferrite mor-
tical microscope (OM), a scanning electron microscope phology of equiaxed and strip, and the carbides are highly
(SEM), and a transmission electron microscope (TEM). The dispersed on the matrix. Also, TEM analysis shows that BM
prior austenite grain was etched by a saturated picric acid contains a small amount of lower bainite (seen in Figure
solution and observed by the OM. The impact toughnesses 2(b)).
were evaluated by means of a standard V-notch Charpy
2.2.2 Microstructure of CGHAZ before PWHT
specimen of 10 mm×10 mm×55 mm, and the test tempera-
ture was 30°C. Fratography results of the impact speci- The microstructure of ASTM4130 steel has obviously
mens were analyzed by SEM. Hardness was measured un- changed after undergoing the thermal welding cycle of Tp
der the load of 10 kg and 25 g. 1350°C and being etched by a 4% nitric solution, which is
shown in Figure 3. It can be found that CGHAZ has a mi-
crostructure of untempered lath martensite and feathery
2 Results and discussion bainite, regardless of the applied welding heat. Figure 4 is
also a group of optical micrographs of CGHAZ etched by
2.1 Properties Labara which has been widely used for martensite identifi-
cation in dual-phase steels. The matrix is martensite, while
The toughness and hardness of base metal (BM) are 188 J the other is bainite. It can be clearly observed that CGHAZ
and 252.4 HV10, respectively. The relationship of peak consists of a considerable amount of feathery and acicular
temperature with Charpy energy and hardness is shown in bainite, regardless of the applied welding heat. But the dis-
Figure 1. As can be seen, HAZ impact toughness signifi- tribution and size of acicular bainite vary with the increase
cantly decreases with increasing Tp. At Tp of 1350°C, in the welding heat input. When the applied welding heat
(12 kJ/cm) is low, most acicular bainite is relatively slend
and aligned parallel to each other. Some of the acicular
bainite constituent contacts each other at an angle, and its
width slightly increases when the welding heat input further
increases.

Table 2 Properties of CGHAZ before and after PWHT

Welding heat input (kJ·cm1) 12 20 28


as-welded 13.40 10.32 10.34
Charpy energy (J)
PWHT 183.67 193.67 207.67
as-welded 547.6 489.4 435.8
Hardness (HV10)
Figure 1 Relationship of peak temperature with Charpy energy. PWHT 222.7 240.9 234
Li L Y, et al. Sci China Phys Mech Astron August (2011) Vol. 54 No. 8 1449

Figure 2 Microstructure of BM. (a) Optical micrograph; (b) TEM.

The area fraction and microhardness of the microstruc-


ture resulting from Figure 4 are shown in Table 3. It can be
found that the hardness of the matrix is higher than that of
the microstructure with morphology of feather and acicular.
Therefore, it is confirmed that the matrix is martensite and
the other is bainite. Meanwhile, the area fraction of marten-
site (bainite) decreases (increases) with increasing applied
heat, for heat inputs of 12, 20, and 28 kJ/cm. This is consis-
tent with the theoretical inference that much of the micro-
structure which transformes at high temperature is obtained
since the cooling rate decreases with increasing applied Figure 3 Optical micrographs of CGHAZ as-welded etched by a 4%
heat. nitric solution. (a) 12 kJ/cm; (b) 20 kJ/cm; (c) 28 kJ/cm.
Figure 5 illustrates that the prior austenite grain of
CGHAZ is coarsened regardless of the amount of welding welding heat has no effect on the prior austenite grain size
heat applied. Calculation from GB/T 6394-2002 shows that when it increases from 12 kJ/cm to 20 kJ/cm, but when it
the average intercepts are approximately 116.19, 115.19 and increases from 20 kJ/cm to 28 kJ/cm, the prior austenite
126.39 m corresponding to welding heat inputs of 12, 20 grain size slightly increases.
and 28 kJ/cm, respectively. It is evident that the applied Taking CGHAZ with welding heat input 20 kJ/cm, as is
typically used, the fine microstructure was further investi-
gated by TEM, as shown in Figure 6. It can be found that
Table 3 Area fraction and microhardness of the microstructure
CGHAZ as-welded also contains a small amount of
Welding heat Area fraction (%) Microhardness (HV0.025) high-carbon martensite with twinned morphology charac-
input (kJ·cm1) Bainite Martensite Bainite Martensite teristic (Figure 6(a)). Figure 6(b) shows that low bainite
12 54.8 45.2 300.7 417.8 contains stacking fault substructure, which differs from
20 68.5 31.5 381.5 421.5 what is usually observed. In addition, martensite-austenite
28 76.2 23.8 322.2 376.3
(M-A) constituents (Figure 6(c)) and granular bainite
1450 Li L Y, et al. Sci China Phys Mech Astron August (2011) Vol. 54 No. 8

Figure 4 (Color online) Optical micrographs of CGHAZ as-welded Figure 5 Prior austenite grain of CGHAZ. (a) 12 kJ/cm; (b) 20 kJ/cm; (c)
etched by Labara. (a) 12 kJ/cm; (b) 20 kJ/cm; (c) 28 kJ/cm. 28 kJ/cm.

(Figure 6(d)) appear in CGHAZ. Figure 7 depicts the mor- carbon diffuses outside into austenite, and it will further
phology of M-A constituents which take on a black color. It transform to M-A constituents when it is cooled.
was etched by two different steps of the etching procedure.
It is found that there is a considerable amount of M-A con- 2.2.3 Microstructure of CGHAZ after PWHT
stituents in CGHAZ of ASTM4130 steel compared with that Optical micrographs of CGHAZ after PWHT are shown in
of other low carbon alloy steels. The reason is that Figure 8. Martensite and other non-equilibrium microstruc-
ASTM4130 steel has a relatively high carbon content in tures are decomposed to tempered martensite and fine car-
austenite under the same welding condition, which is bene- bides, regardless of the welding heat input. It can be seen
ficial to the formation of M-A constituents. On the other that the prior austenite grain boundaries are still visible, in
hand, once the bainite phase transformation occurs, retained particular the change of grain size is not apparent and the
austenite with a high carbon content usually exists because strip characteristic is still obvious. This means that the tem-
the formation process of bainite is also the process in which pering resistance of ASTM4130 steel is high, which is
Li L Y, et al. Sci China Phys Mech Astron August (2011) Vol. 54 No. 8 1451

Figure 6 TEM images of CGHAZ. (a) High carbon martensite; (b) low bainite; (c) M-A constituent; (d) granular bainite.

cementite; the alloying elements forming carbide will dif-


fuse into cementite to form alloy cementite, such as
(Fe,Cr)3C, (Fe,Mo)3C, or further transform to metastable
and special stable carbides. In this case, the alloy cementite
M3C is found to exist in CGHAZ. It can effectively prevent
aggregation and growth of carbides since its chemical bond
energy is higher than that of Fe3C. At the same time, recov-
ery and recrystallization of the ferrite is suppressed due to
the difficulty of carbon atom diffusion, hence, most of the
original remains in a strip shape. In addition, M-A con-
stituents are not clearly found after PWHT (Figure 9).
For detailed microstructure analysis, CGHAZ with a
welding heat input of 20 kJ/cm after the PWHT was ob-
Figure 7 Morphology of M-A constituents before PWHT. served by TEM. From Figure 10(a), it can be found that the
temper is not sufficient since stacking fault substructure still
exists. It can also be found that dislocation density de-
closely related to the added alloying elements Cr and Mo. In creases, contrasting with that before PWHT, and Fe3N par-
fact, the PWHT process is the process in which recovery ticles are confirmed to precipitate along the lath boundaries
and recrystallization of ferrite, as well as aggregation and and inside laths of low bainite. As can be seen in Figure
growth of carbides, occur based on the disappearance and 10(b), retained austenite transformed to low bainite, which
recombination of dislocation [6]. On one hand, carbon at- is located among the prior laths since Fe4N is found to be
oms in the non-equilibrium microstructure primarily pre- located in the ferrite needle. The existence of Fe3N and
cipitate in the carbon segregation area, such as grain and Fe4N may be induced by the incomplete excretion of nitro-
lath boundaries, and then gradually transform into cementite, gen during the steelmaking process. In addition, it is noted
so that the prior austenite boundaries are evident compared that part of the CGHAZ microstructure has been trans-
with those before the PWHT. On the other hand, alloying formed to tempered sorbite (Figure 10(c)). However, no
elements will be redistributed between the  matrix and M-A constituent is found by TEM.
1452 Li L Y, et al. Sci China Phys Mech Astron August (2011) Vol. 54 No. 8

Figure 9 Morphology of M-A constituents after PWHT.

3 Discussion

3.1 Brittle analysis

The foregoing results show that CGHAZ toughness dra-


matically decreases when the peak temperature is 1350°C,
regardless of whether the welding heat input is applied. This
is in good agreement with conclusions drawn from studies
of most high strength low alloy (HSLA) steels. In this case,
the ASTM4130 steel CGHAZ embrittlement might be de-
scribed by the following:
(1) The prior austenite grain is coarse. The average in-
tercept of CGHAZ austenite is about 115–126 m (Figure
5). Different from normal heat treatments, the heated tem-
perature CGHAZ experienced during fusion welding is up
to 1350°C, and austenite grain grows with thermal inertia
due to the welding feature of rapid heating and cooling. On
the other hand, there is not enough time for carbides to melt
completely in austenite, thereby leading to the loss of pin-
ning in prior austenite grain boundary migration. So, the
prior austenite grain becomes coarse, and accordingly, the
toughness decreases significantly according to the Hall-
Petch formula.
Figure 8 Optical micrographs of CGHAZ after PWHT, etched by 4% (2) The presence of non-equilibrium microstructure.
nitric solution. (a) 12 kJ/cm; (b) 20 kJ/cm; (c) 28 kJ/cm. CGHAZ possesses microstructure of untempered lath mart-
ensite, as well as feathery, acicular and butterfly bainite
(Figures 3–4). In fact, the microstructure feature of CGHAZ
2.2.4 Fractograph characterization is strongly dependent on the thermal cycle experienced dur-
ing welding and chemical composition of ASTM4130 steel.
Typical fracture modes observed in Charpy specimens of
Firstly, when CGHAZ is heated to 1350°C, the prior
CGHAZ before and after PWHT are shown in Figures 11(a)
austenite grain becomes coarse, thereby increasing the bain-
and (b). It is clear that the CGHAZ fractured surface is en-
ite transformation temperature (Bs) [7]. Secondly, the added
tirely dominated by the quasi-cleavage mode before PWHT.
alloying elements, namely Cr and Mo, can effectively post-
However, it is transformed into a ductile dimpled fracture
pone the formation of ferrite and pearlite. However, their
after PWHT. This means that impact toughness is signifi- influence on the bainite transformation is negligible. Finally,
cantly improved due to the tempering effect of PWHT. the high carbon content in ASTM4130 steel improves the
Semiquantitative energy dispersive spectroscopy (EDS) stability of austenite, thus the CCT curve moves rightwards.
analysis revealed that three main elements (Ca, Cr and Mn) Therefore, the bainite transformation zone is expanded, and
were present in the process, in addition to iron. a large amount of bainite and martensite is formed from the
Li L Y, et al. Sci China Phys Mech Astron August (2011) Vol. 54 No. 8 1453

in this case its existence does not endow CGHAZ with the
balance of high strength and excellent toughness. The rea-
son is that low bainite contains stacking fault substructure
(Figure 6(b)). This stacking fault corresponds to a film hav-
ing a closely-packed hexagonal structure being inserted into
a body-centered cubic structure, which can prevent plastic
deformation continuity of ferrite, thereby resulting in dislo-
cation pile-up, stress concentration, and microcrack forma-
tion. In addition, M-A constituents play a significant role in
hydrogen and stress concentration. Microcracks are always
generated and propagate along their boundaries. Hence, the
presence of non-equilibrium microstructure is responsible
for the CGHAZ toughness degradation.

3.2 Effect of PWHT on CGHAZ toughness

After PWHT, although the microstructure of CGHAZ has a


distinct lath form, the CGHAZ toughness of ASTM4130
steel is remarkably improved over that of the BM, and
hardness obviously declines (Table 2). This demonstrates
that PWHT plays a significant role in the improvement of
CGHAZ toughness. During the PWHT process, fine car-
bides precipitate from non-equilibrium microstructure, but
do not become coarse due to high tempering resistance.
Some big Ca-Cr-Mn particles are also found to be located in
CGHAZ (Figure 11(b)). At the relatively low impact stress
levels, the big Ca-Cr-Mn particles preferentially separate

Figure 10 TEM images of CGHAZ after PWHT. (a) Tempered bainite;


(b) freshly formed bainite; (c) tempered sorbite.

large prior austenite grain size.


The decrease in CGHAZ toughness is closely related to
its microstructure. Firstly, the carbides, which are located
among upper bainite laths, provide the initiating sites and
propagating channel of the crack [8]. Secondly, martensite
is a kind of supersaturated carbon solid solution, and has a
large lattice distortion and high hardness. Moreover, it is
difficult to generate the associated self-tempering effect
since the austenite-martensite transition temperature Ms is
low. Thirdly, although lower bainite has excellent me-
chanical properties according to the conventional viewpoint, Figure 11 Fractographs of CGHAZ. (a) Before; (b) after PWHT.
1454 Li L Y, et al. Sci China Phys Mech Astron August (2011) Vol. 54 No. 8

from the matrix and form large microvoids. Fine carbides of a welding simulation technique. Some main conclusions
experience a similar process with increasing impact stress, are summarized as follows:
except that the associated microvoids are smaller than those (1) The impact toughness in CGHAZ of ASTM4130
of their counterparts. Then small and large microvoids fur- steel is only 5.5%–7.1% that of the base metal, which
ther grow and eventually contact each other. As can be seen makes CGHAZ become the local brittle zone in single-pass
in Figure 11(b), small microvoids are located among the welding.
large ones, which consumes more energy during the fracture (2) CGHAZ toughness degradation of ASTM4130 steel
process. Additionally, PWHT can relax residual stresses, is primarily due to the presence of non-equilibrium micro-
which is also beneficial to increasing toughness. structure, particularly feathery, acicular, and butterfly bain-
ite and M-A constituents. In addition, the coarse grain size
3.3 Effect of heat input on CGHAZ toughness also results in the deterioration of toughness.
(3) The 650°C/1.5 h PWHT restores CGHAZ toughness
When applied welding heat values are 12 and 20 kJ/cm, of ASTM4130 steel in single-pass welding, showing that
prior austenite grain size is almost the same, but it slightly PWHT is required. This improvement resulted from the
increases when welding heat input increases to 28 kJ/cm. decomposition of non-equilibrium microstructure and relief
However, the total CGHAZ toughness of the input welding of residual stresses.
heat of 20 kJ/cm is as high as that of the input welding heat (4) For single-pass welding of ASTM4130 steel, the ef-
of 28 kJ/cm, and slightly lower than that of the input weld- fect of applied welding heat increasing from 12 kJ/cm to 28
ing heat of 12 kJ/cm. Analysis suggests that the factor con- kJ/cm on CGHAZ toughness is negligible regardless of
trolling CGHAZ impact toughness is the resultant micro- whether PWHT is applied or not. After PWHT, the associ-
structure rather than the prior austenite grain size. As can be ated mechanical properties of CGHAZ can all satisfy the
seen in Table 3 and Figure 4, the area faction of upper and requirements. When the welding efficiency is taken into
lower bainite and the ferrite lath width increase with the account, a larger welding heat input is preferred.
increase in welding heat input. It can be inferred from Ta-
bles 2 and 3 that the area fraction of bainite dramatically
affects the impact toughness, and the impact toughness de- 1 Zhang L P, Davis C L, Strangwood M. Effect of TiN particles and
microstructure on fracture toughness in simulated heat-affected zones
clines to the limit where the bainite fraction increases to of a structural steel. Metall Mater Trans A, 1999, 30(8): 2089–2096
about 70% (welding heat input 20 kJ/cm). After PWHT, the 2 Gao H L, Dong Y H, Hendricks R W. Microstructure transformation
specimens with high welding heat input having low tough- and brittlement of a ultra-low carbon QT steel during double welding
ness before PWHT later have high toughness after PWHT. thermal cycle. Acta Metall Sin, 2001, 37(1): 34–38
3 Bonnevie E, Ferrière G, Ikhlef A, et al. Morphological aspects of
Also, impact toughness slightly increases with the increase martensite-austenite constituents in intercritical and coarse grain heat
in welding heat input. The reason might be that the super- affected zones of structural steels. Mater Sci Eng A, 2004, 385(1-2):
saturation of bainite is lower than that of martensite, so 352–358
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carbon atoms undergoing the same PWHT process diffuse
impact toughness of CGHAZ of ultra-low carbon copper-bearing
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toughness of CGHAZ is not very obvious regardless of 5 Alé R M, Rebello J M A, Charlier J. A Metallographic technique for
whether PWHT is applied or not. detecting martensite-austenite constituents in the weld heat-affected
zone of a micro-alloyed steel. Mater Charact, 1996, 37(2-3): 89–93
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