Emrs 2012

A B C D E F G H I J K L M N O P Q R S T U V W X Y
E-MRS Spring 2012 - Symposium X

Quantitative Microscopy of Energy Materials
Over the past decade, instrumental innovations and improvements (like the commercialization of
aberration-corrected electron optics) have boosted the capabilities of imaging and analysing at the
nanoscale. Consequently, electron microscopy and related techniques are nowadays widely applied to
characterize the micro and nanostructure of all kinds of materials. Driven by restricted natural
resources, so-called energy materials, i.e., materials used for energy generation, transmission, and
storage are gaining increasing importance. Being mostly operated under conditions that have a strong
influence on their microstructure and properties, microdiagnostics and failure analyses are of high
scientific and industrial relevance. This symposium will focus on the quantification of the microstructure
evolution in such devices, using advanced electron microscopy and other microdiagnostics techniques,
and the relationship between microstructure, properties, and efficiency.
Scope
Microstructure-property relations of complex materials commonly used in energy systems form the basis
of the targeted applications. Being often subjected to harsh conditions upon operation, microstructure
modification and interactions between materials have to be monitored. Based on such microstructure
characterization, a fundamental understanding of processes can be developed, being highly relevant for
technological applications and the optimization of materials properties. Microstructure characterization,
down to the nano scale, did significantly profit from the dramatic improvement of electron-optical
imaging and nano analyses over the past decade. The introduction of aberration correction, improved
detectors, enhanced site-specific preparation routes, as well as the exploitation of 3D techniques, has
lead to truly advanced and quantitative imaging, diffraction, and spectroscopic analyses with electrons.
Electron microscopy has become quantitative, e.g., it has rather become a method to analyse and
measure quantitatively important microstructure parameters and materials properties. Now that these
challenging nano-characterization tools are becoming more and more available in academia and
industry, their application in the various fields of materials science and life science is to be addressed
next. In parallel, complementary methods for micro and nanocharacterization covering different length
scales (such as X-ray and neutron diffraction) as well as surface characterization techniques like AFM,
SEM will be addressed to gain a comprehensive picture of micro-nanostructure evolution. It is the
intention of this symposium to invite contributions, which will show current applications of such
advanced techniques to the microcharacterization of materials for energy. This will help to bridge the
gap between microdiagnostics methodology and practical applications to materials of economic and
ecologic importance. Special emphasis will be put on the influence of microstructure evolution on system
properties, and in particular on the efficiency of energy conversion, transportation, and storage. In this
context, the symposium will cover the following topics:
Microdiagnostics:
Advanced quantitative electron microscopy (EM) methods strategies and applications: EBSD,
scanning-transmission EM for atomically resolved imaging and analytics, emerging in situ techniques
(including environmental TEM and SEM), aberration-corrected EM, potential mapping using electron
tomography, electron holography, nano-beam diffraction, electron nano-spectroscopic techniques for
local bonding and elemental mapping, quantification by multiscale modelling
Methods of physical failure localization: lock-in thermography, scanning acoustic microscopy, X-ray
diagnostics (tomography)
Site-specific sample preparation using innovative ion-beam or laser-based approaches
Quantitative microstructure analysis: grain size, coarsening effect, growth mechanisms, radiation
damages, thin film strains and defects, interfaces
Crystal-phase identification (XRD, neutron diffraction, XAS, etc.)
Energy materials:
Materials for solid-oxide fuel cells including purity issues, ceramic-metal interactions, and metallic
interconnects as well as for polymer electrolyte membranes
Thin film PV cells, organic PV cells, materials for high-efficiency PV systems, back reflectors,
substrates, transparent conductive oxides, packaging, nanowires
Metals and alloys for high temperature utilization, catalysts, thermoelectric materials
Separators & active materials for energy-storage
Degradation: relation between microstructure, ageing and efficiency
Diffusion and interdiffusion: interfaces, doping, and implantation
Phase formation and/or transformation: effect of external parameters on phase transformation, related
to property modifications
Hot topics to be covered by the symposium
Page 1of 4 EMRS - Strasbourg - Spring 12 X - Quantitative Microscopy ....
25/04/2012 http://www.emrs-strasbourg.com/index.php?option=com_content&task=view&id=47...
Following the two-pronged scope, the scientific sessions (including a poster session) will be dedicated to
methodological and microanalysis application subjects.
Topics will include:
Methods of failure analysis: lock-in thermography, scanning acoustic microscopy
Site-specific sample preparation: focused ion beam, laser-based methods
Microstructure imaging and chemical analysis: scanning-transmission electron microscopy
(STEM), in situ electron microscopy, electron tomography, diffraction, e.g. for local strain analyses,
aberration-correction and high-throughput EM, electron-beam techniques to map local bonding and
elemental distributions, chemical analyses (EDXS, EELS, EFTEM)
Solid oxide fuel cells (SOFC): Anode and cathode microstructure evolution, poisoning, pollutant
species, metallic interconnect conductivity, protective layers
Photovoltaic devices: thin film PV cells, organic PV, high efficiency systems, back reflectors,
substrates, transparent conductive oxides, packaging, nanowires
Polymer electrolyte membranes (PEM): water transport, membrane microstructure, charge
transfer, catalysts
Metals and alloys in energy systems: corrosion, creep, mechanical wear, high temperature
utilisation, radiation damage, supported catalysts, thermoelectric materials
Energy storage systems: Storage capacity and stability (during hydrogen absorption and
desorption), separators, active materials, corrosion, passivation
Conference Proceedings
Paper submission is now possible via the JMS Online Manuscript Submission website:
https://www.editorialmanager.com/jmsc/
Please note that this will NOT be A CONFERENCE PROCEEDING IN THE CLASSICAL SENSE!
All submitted papers will be reviewed by the Guest Editors according to USUAL J Mater Sci
standards.
Anything looking like a conference proceedings will be automatically refused.
ONLY FULL ORIGINAL ARCHIVAL PAPERS AND REVIEW PAPERS WILL BE CONSIDERED.
Anything that is not original will be automatically rejected.
Please, complete your submission prior to May 12 and select: Special: Energy Materials &
Thermoelectrics as an article type.
List of invited speakers
Rik Brydson (U Leeds)
Miran Ceh (ISJ Ljubljana)
Rafal E Dunin-Borkowski (FZ Jlich)
Frank Dimroth (Fraunhofer ISE)
Thomas Klassen (HZG)
Laurent Legras (EDF)
David McComb (Imperial)
Paul Midgley (U Cambridge)
Robin Schublin (CRPP-EPFL)
Dries Van Gestel (Imec)
Nestor Zaluzek (ANL)
Stefan Zaefferer (MPI Dsseldorf)
Sponsors:


Symposium organizers
Acha Hessler-Wyser
Centre Interdisciplinaire de Microscopie Electronique
Ecole Polytechnique Fdrale de Lausanne
Bat MXC 134, Station 12
CH-1015 Lausanne, Switzerland
Phone: +41 21 693 4830
Fax: +41 21 693 4401
aicha.hessler@epfl.ch
Thomas Hche
Fraunhofer Institute for Mechanics of Materials IWM
Walter-Hlse-Strae 1, D-06120 Halle, Germany
Phone: +49 345 5589 197
Fax: +49 345 5589 101
Thomas.Hoeche@iwmh.fraunhofer.de
Wolfgang Jger
Institute for Materials Science
Christian-Albrechts-University Kiel
D-24143 Kiel, Germany
Phone: +49 431 880 6177
Fax: +49 431 880 6178
wj@tf.uni-kiel.de
Hugo Bender
Imec
Kapeldreef 75
B-3001 Leuven, Belgium
Phone: +32 16 281304
Fax: +32 16 28 1515
hugo.bender@imec.be

A B C D E F G H I J K L M N O P Q R S T U V W X Y

European Materials Research Society
23 Rue du Loess - BP 20 - 67037 Strasbourg Cedex 02 - France - Phone:+33-(0)3 88 10 63 72 - Fax:+33-(0)3 88 10 62 93 - emrs@emrs-
strasbourg.com
14 May 2012 15 May 2012 16 May 2012
hide a
(close full abstract)
PROGRAM VIEW : 2012 Spring
MY PROGRAM : 2012 Spring
Symposium : X

start at Subject Num.
Advanced microscopy: 3D and in situ : Thomas Hche
09:00 Quantitative Electron Tomography
Authors : Paul Midgley
Affiliations : University of Cambridge, Department of Materials Science and
Metallurgy, Cambridge, U.K.
Resume : The challenge to find new materials to help solve the worlds
growing energy problems is one of the most important we face. To meet
that challenge, electron microscopy can play a key role in elucidating the
property-microstructure relationships of these often complex materials.
Electron tomography allows the microstructure of such materials to be
studied in three dimensions and at a high spatial resolution revealing key
information that can otherwise be obscured. Over recent years, electron
tomography has developed into a powerful tool for materials science and
with the implementation of novel imaging modes has enabled not just
morphology to be seen in 3D but also composition, electrostatic potentials
and defects. Alongside such hardware and technique development, there
has been a rapid development of novel visualization software and
reconstruction algorithms. Importantly, as many of these materials are
beam sensitive, much of the software progress has been aimed at achieving
reconstructions with minimal artefacts from limited data sets (and thus
limited electron dose). In this presentation, I will show a number of
examples related to energy materials that illustrate the quantitative nature
of electron tomography and how high fidelity reconstructions are possible
from very few images. Recent progress in atomic resolution tomography will
also be discussed.
1 1
add to my program
09:30 Nanometric Defects in Metals in Transmission Electron Microscopy
Authors : Robin Schaeublin (1), Brigitte Dcamps (2)
Affiliations : (1) Ecole Polytechnique Fdrale de Lausanne (EPFL), Centre de
Recherches en Physique des Plasmas, Association Euratom-Confdration Suisse,
5232 Villigen PSI, Switzerland; (2) Centre de Spectromtrie Nuclaire et de
Spectromtrie de Masse (CSNSM), CNRS-IN2P3-Univ. Paris-Sud 11, UMR 8609, Bt.
108, 91405 Orsay, France
Resume : Conventional transmission electron microscopy including in situ
deformation experiments is revisited in order to refine methods for the
identification of nanometric defects in metals and their interaction with
dislocations. Nanometric crystal defects play an important role as they
influence, generally in a detrimental way, physical properties and in
particular mechanical properties of metals designed for aggressive
environments such as high irradiation fields or high heat loads. For instance,
radiation induced damage in metals strongly degrades mechanical
properties, rendering the material stronger but brittle. Indeed, these defects
are obstacles to mobile dislocations, vector of plasticity. It is thus critical to
fully characterize them, ideally with transmission electron microscopy. The
difficulty in using TEM to identify the nature and size of such defects resides
in their small size, close to the resolution of CTEM. TEM image simulations
are deployed to explore limits and possible ways to improve on spatial
resolution and contrast on e.g. dislocation loops or stacking fault tetrahedra.
Examples of in situ straining experiments of Cu and Fe showing the
1 2
Page 1of 9 EMRS - Strasbourg
25/04/2012 http://www.emrs-strasbourg.com/index.php?option=com_abstract&task=view&id=17...
interaction of mobile dislocations with nanometric defects are given. Results
obtained in Fe are compared to molecular dynamics simulation. Besides, it
appears that some image formation mechanisms, using diffraction contrast,
are still unclear. We present here the case of energy filtered images of
threading dislocations that exhibit a top bottom asymetry with increasing
energy loss, and also three dimensional defects in pure Fe and Fe(Cr) that
exhibit anomalous contrast behaviour in weak beam dark field under g
condition while it is normal under bright field condition.
add to my program
10:00 Coffee break
10:30 NiO reduction studied by environmental transmission electron microscopy
Authors : Q. Jeangros (1), T.W. Hansen (2), J.B. Wagner (2), C.D. Damsgaard (2),
R.E. Dunin-Borkowski (3), C. Hbert (1), J. Van Herle (4), A. Hessler-Wyser (1)
Affiliations : (1) Interdisciplinary Centre for Electron Microscopy, EPFL, CH-1015
Lausanne, Switzerland; (2) Center for Electron Nanoscopy, Technical University of
Denmark, DK-2800 Lyngby, Denmark; (3) Ernst Ruska-Centre, Jlich Research
Centre, D-52425 Jlich, Germany; (4) Laboratory for Industrial Energy Systems,
EPFL, CH-1015 Lausanne, Switzerland
Resume : Nickel oxide reduction and subsequent Ni behavior under H2
atmosphere is of practical importance in the field of solid oxide fuel cells
(SOFC) as it determines the structure of the anode electron conductor
during operation. Despite extensive coverage in literature, some
discrepancies remain, notably regarding NiO reduction kinetics and
structural evolution. In situ reduction of an industrial NiO powder from JT
Baker is performed under 1.3 mbar of H2 (2 mlN/min) in a differentially
pumped FEI Titan 80-300 environmental transmission electron microscope
(ETEM). Images, diffraction patterns and electron energy loss spectra
(EELS) are acquired at different temperatures to monitor the structural and
chemical evolution of the system. High-resolution ETEM is also performed
during similar experiments. EELS analysis illustrates that reduction first
proceeds quickly at temperatures below 400C up to a reduced fraction of
about 0.6, until the reaction is slowed down by water created upon
reduction. Ni nucleation on NiO is observed to be either epitaxial in thin
areas or randomly oriented in thicker regions. The growth of Ni crystallites
creates pores within NiO grains to accommodate the volume shrinkage
associated with reduction. Densification is then observed at temperatures
higher than 550C: pores created at lower temperatures disappear and Ni
grains coarsen. This reorganization of Ni is detrimental to both the
connectivity of the Ni catalyst and to the redox stability of the SOFC.
1 3
add to my program
10:45 Resolving deformation in carbon nanotubes in contact with metal islands at
the atomic level
Authors : X. Ke, S. Turner, S. Bals, C. Bittencourt, G. Van Tendeloo
Affiliations : EMAT, University of Antwerp, Belgium
Resume : The high contact resistance between the carbon nanotubes
(CNTs) and metal leads is one main concern in integration of CNTs into
devices. The diameters of the CNTs, the quality of the CNTs and different
contact materials are all considered to influence the contact. Therefore, we
focus on the study of the interface between CNTs and various contact
materials from structural point of view. CNTs deposited with Au, Pd, Rh and
Ti are studied by aberration-corrected high resolution transmission electron
microscopy (AC-HRTEM). Au, Pd and Rh form discreet nanoparticles on multi
-walled CNTs, whereas Ti forms continuous film wetting completely the
CNTs. More interestingly, 3D electron tomography of the structure has found
out that the graphitic layers in direct contact with Au nanoparticles are
deformed to a certain degree. The deformation degree depends not only on
the contact metal, but also on the diameters of CNTs. Examples will be given
for different metals and different size CNTs. By using AC-HRTEM at 80kv in
order to reduce knock-on damage to the CNTs, the deformation of the
graphitic layers can be investigated at atomic resolution. The displacement
of the carbon atoms from their perfect position can be further quantified and
related to the strain which is believed to be induced by the contact to metal.
AC-STEM-EELS is performed in deformed CNT layers to look for the
differences in electronic states. The study may help optimizing the system
forming CNT-metal contacts for devices.
1 4
add to my program
Electron Backscatter Diffraction, Atomic Force Microscopy, X-ray Absorption
Spectroscopy, X-ray Diffraction : Hugo Bender
11:00 Quantitative characterization of deformation and transformation
microstructures of advanced steels using electron diffraction techniques in
the SEM
Authors : S. Zaefferer, N.N. Elhami, C. Tasan, P. Konijnenberg, F. Ram
Affiliations : Max-Planck-Institute for Iron Research, Department of Microstructure
Physics, 40237 Duesseldorf, Germany
Resume : The scanning electron microscope offers powerful diffraction
techniques which allow the quantitative characterization of defects of
crystalline materials. These techniques are electron backscatter diffraction
(EBSD), electron channelling contrast imaging (ECCI) and Kossel diffraction.
EBSD has become a popular method to obtain microstructural images and
local texture of materials with a spatial resolution of 50 to 100 nm. New
analysis methods for EBSD patterns and orientation data allow deeper
insight into materials: The measurement of orientation gradients enables the
quantitative description of the density of geometrically necessary
dislocations (GND), the detailed evaluation of diffraction band profiles gives
access to the total dislocation density, in-situ deformation experiments allow
understanding of interaction of boundaries and dislocations. 3-dimensional
EBSD based on serial sectioning enables the detailed description of the
crystallography of grain boundaries. The ECCI technique makes it possible to
observe dislocations and stacking faults directly with a similar (but weaker)
contrast as in dark field TEM but on bulk samples. This allows, for example,
characterization of slip systems, quantification of dislocation and nanotwin
densities and observation of dislocation evolution during deformation
experiments. The smallest features observable with this technique are in the
order of 10 to 20 nm.
2 1
add to my program
11:30 Intermetallic growth in Al-Fe system studied by time resolved X-ray
tomography combined with FIB/SEM/TEM
Authors : Guillaume Pasche, Acha Hessler-Wyser, Robin Schublin, Ccile Hbert
Affiliations : Centre Interdisciplinaire de Microscopie Electronique, Ecole
Polytechnique Fdrale de Lausanne, CH-1015 Lausanne, Switzerland
Resume : The formation of Fe-Al intermetallics is known as taking an
important part in the wear process of steel tools used for aluminium
injection moulding. Rapid formation of intermetallic phases with high
brittleness coupled to different mechanical movements and thermal cycling
lead to a precocious wear of a specific part of the tool called shot sleeve.
Studying their formation gives precious information how to limit intermetallic
growth and subsequently the shot sleeve wear. A liquid metal immersion
facility (LMIF) is used for diffusion couple investigation. Scanning electron
microscopy (SEM) techniques are used to assess kinetics and morphology in
intermetallics growth process. A quantitative method shows that the growth
of the two principal intermetallic phases (Fe4Al13 and Fe2Al5) is dictated by
species diffusion. A tongue-like structure of the Fe2Al5 is observed and
transition layer of the FeAl phase around the tongue is identified for the first
time in the Fe-Al system at 973 K through electron back scattered diffraction
(EBSD), 3D Focused Ion Beam tomography (3D FIB) and Transmission
Electron Microscopy (TEM). Further investigation through in situ X-Ray
tomography gives a more complete understanding of growth/dissolution
competition of the intermetallic compounds in providing a continuous
observation of the interface during the reaction.
2 2
add to my program
11:45 Nanoscale electrical characterization of polymer/carbon nanotubes blends
for organic photovoltaic applications
Authors : Simon Desbief (1), Olivier Douhret (1), Nomie Hergu (2), Mathieu
Surin (1), Philippe Dubois (2), Roberto Lazzaroni (1), Philippe Leclre (1)
Affiliations : (1) Laboratory for Chemistry for Novel Materials; (2) Laboratory of
Polymeric and Composite Materials Center of Innovation and Research in Materials
and Polymers (CIRMAP), University of Mons, UMONS / Materia Nova, Place du Parc
20, 7000 Mons, Belgium
Resume : In the growing field of molecular electronics, devices containing
carbon nanotubes (CNTs) are extensively studied. In this context, the
2 3
control of the morphological properties, and the understanding of the
electrical properties at the nanometer scale are essential. The use of the
AFM (Atomic Force Microscopy) permits to have access to the local
morphological properties. Besides this technique, the recently introduced
Peak-Force TUNA (PFTUNA) constitutes a powerful imaging mode allying the
advantages of the Tapping Mode AFM (spatial resolution below 10 nm) and
of C-AFM (current sensitivity of 100 fA). In this work, we characterize
morphological and electrical properties of blends made of CNT and a p-type
semiconducting polymer, the regio-regular poly-3-hexylthiophene (P3HT),
deposited on a glass substrate patterned with ITO (Indium Tin Oxide). The
P3HT is a very good candidate for the fabrication of organic photovoltaic
devices thanks to its good carrier mobility and its absorption spectra. The
CNTs present good conduction properties, and their size is ideal for building
conduction paths in organic devices. The combination of C-AFM and PFTUNA
provides valuable information on the electrical properties of the hybrids,
showing a high resolution contrast attributed to the local properties of the
conjugated materials and therefore contributes to a better understanding of
the links between the morphological properties and the global electrical
performances of the devices.
add to my program
12:00 Characterization of Electrical Surface Properties by Electrostatic Force
Microscopy: Modeling Resolution and Sensitivity
Authors : Markus Ratzke, Jrgen Reif
Affiliations : Lehrstuhl fr Experimentalphysik II, BTU Cottbus, IHP/BTU JointLab,
Konrad-Wachsmann-Allee 1, 03046 Cottbus, Germany
Resume : Today's highly integrated semiconductor technology requires a
mapping of surface properties with resolution in the nanometer range, with
particular emphasis on electrical features such as surface potential and near
-surface capacitance, these parameters giving access to the material's
electronic properties. For photovoltaic applications, local recombination
activities are of interest. To obtain such information, non-destructive
experimental methods are of particular advantage, which do not require
complicated, invasive sample preparation, thus allowing investigations of
pristine surfaces. Non-contact scanning probe techniques, generally, provide
a tool for such investigations. "Scanning Kelvin Probe Microscopy" and
"Scanning Capacitance Microscopy" have been demonstrated to be very well
suited for a QUALITATIVE estimate of surface electronic structure. However,
for a QUANTITATIVE assessment, fundamental aspects of these experiments
have to be clarified. Most important hereby will be the specific knowledge of
the relation between quantity of interest and measured signal, determined
by an appropriate transfer function. We will derive such a transfer function,
based on both numerical simulations and analytical modeling. We estimate
the resolution and sensitivity of the experimental techniques, thus
addressing potential ways for a reliable quantitative signal recovery. Our
quasi analytical models allow, indeed, a simple deconvolution of the raw
data, making Electrostatic Force Microscopy an even more useful tool.
2 4
add to my program
12:15 Lunch
Fuel Cells : Acha Hessler-Wyser
14:15 Effect of interfaces on the ionic conductivity of SOFC materials
Authors : David W. McComb
Affiliations : Dept of Materials Science and Engineering, The Ohio State University,
Columbus, OH, 43210, U.S.A.
Resume : The search for new strategies to enhance the oxide ionic
conductivity in oxide materials is an active field of research. Such materials
are needed for application in a new generation of more efficient and durable
solid state electrochemical devices such as reduced-temperature Solid Oxide
Fuel Cells (SOFCs). There have been numerous reports in the literature of
significantly enhanced ionic conductivity in multilayer heterostructures
formed from ionic conductors and insulators. There have also been a
number of reports suggesting that these enhancements are due to electronic
rather than ionic conductivity. In this invited contribution I will discuss
recent results obtained in collaboration with colleagues in Spain, the UK and
3 1
the USA from three different multilayer structures. Using scanning
transmission electron microscopy (STEM) combined with electron energy-
loss spectroscopy (EELS) and energy-dispersive X-ray (EDX) analysis we
have probed the structure, composition and bonding with high spatial
resolution in order to relate the interfacial structure and chemistry to the
observed conductivity.
add to my program
14:45 Relating nanostructures of yttria-stabilized-zirconia thin films to their
proton conductivity
Authors : Julia Martynczuk(1), Meike V. F. Schlupp(1), Barbara Scherrer(1), Dieter
Stender(2), Ren Tlke(1), Anna Evans(1), Michel Prestat(1), Ludwig J. Gauckler(1)
Affiliations : (1) Nonmetallic Inorganic Materials, Department of Materials, ETH
Zurich, CH-8093 Zurich, Switzerland (2) General Energy Research Department, Paul
Scherrer Institute, CH-5232 Villigen-PSI, Switzerland
Resume : Zirconia-based thin films are potential electrolyte membranes in
micro-solid oxide fuel cells [1]. Below 400C, the electrical conductivity of
some yttria-stabilized-zirconia (YSZ) thin films deviates from the well-known
oxygen ion conductivity and an enhanced conductivity at room temperature
as high as normally at 400C can be observed. In this study, we investigate
the reason for this behavior using advanced electron microscopy with atomic
resolution for the evolution of the different nanostructures of the YSZ films
depending on the deposition technique and conditions. Films made by spray
pyrolysis, aerosol-assisted chemical-vapor deposition and pulsed laser
deposition [2-4] were investigated resulting in either porous thin films with
equiaxed grains or dense films with columnar nanostructures. Cross-
sectional views of the thin films were prepared by site-specific sample
preparation using a focused ion beam technique. Scanning transmission
electron microscopy (STEM), aberration-corrected EM, chemical analyses
(EDXS), and nano-beam diffraction were used to gain a comprehensive
picture of the nanostructure evolution. The rather high electrical conductivity
at low temperatures is attributed to proton conduction of chemisorbed and
physisorbed water in open porosity of the thin films. 1. A. Evans et al., J.
Power Sources (2009). 2. B. Scherrer et al., Adv. Funct. Mater. (2011). 3.
M. V. F. Schlupp et al., J. Power Sources (2011). 4. S. Heiroth et al., J. Eur.
Ceram. Soc. (2010).
3 2
add to my program
15:00 Microstructure influence on ohmic resistance and transport properties of
porous SOFC electrodes and electrolysis diaphragms
Authors : Lorenz Holzer (1) Thomas Hocker (1) Lukas Keller (1) Daniel Wiedenmann
(2) Bernard Grobety (2) Boris Iwanschitz (3) Michel Prestat (4) Beat Munch (5)
Affiliations : (1) ZHAW, Zurich University of Applied Sciences, Winterthur,
Switzerland; (2) Uni Fribourg, Geoscience Department, Fribourg, Switzerland; (3)
Hexis SA, Winterthur, Switzerland; (4) ETH Zurich, Institute for nonmetallic inorganic
materials NIM, Zurich, Switzerland; (5) EMPA Materials Science and Technology,
Duebendorf, Switzerland
Resume : High resolution tomography in combination with dedicated image
modelling techniques allow for a better understanding which morphological
features are actually dominating the transport properties of porous and
composite materials (e.g. conductivity). Investigations are undertaken in
SOFC electrodes (Ni-YSZ and Ni-CGO anodes, LSC cathodes) and in porous
diaphragms of electrolysis cells. A new method is presented which enables
to describe quantitatively the effect of bottle necks (i.e. constrictivity). Data
is presented which indicates that constrictivity has a higher impact on the
macroscipic transport properties than the geometric tortuosity. Using
measured constrictivity, tortuosity and phase volume fractions, the transport
properties (i.e. conductivity) can be predicted based on the parameters
which are entirely extracted from tomography. In this way quantitative
microscopy can be used directly for the determination of macroscopic
materials properties.
3 3
add to my program
15:15 Opportunities and Limits of SEM/EDS Analyses for Polymer Electrolyte Fuel
Cells
Authors : H. Echsler, C. Korte, D. Stolten
Affiliations : Forschungszentrum Jlich GmbH, IEK-3, D-52425 Jlich, Germany
Resume : Besides various other factors, Polymer Electrolyte Fuel Cells rely
on the ion conductivity in both the membrane and the gas diffusion
electrodes (GDE), respectively. Especially in the latter case the micro- or
even nanostructure of the component or the amount and the distribution of
3 4
the ion conducting polymer, in most cases Nafion, is of special interest for
the properties and performance of the cell. Within the last decade great
progress has been achieved in the field of SEM / EDX analyses with regard
to maximum possible resolution and variability of the materials to be
investigated. Now it is possible to visualize structures down to the
nanometer scale, as they are prevailing in the GDE, not only with TEM but
also with SEM. Nevertheless, the detection and quantification of light
elements and especially F, which is a major constituent of Nafion via EDX,
is still a challenge. Beam damage of the polymers or vaporisation of e.g. F is
unavoidable which makes its quantification at least for small spots or areas
inaccurately. In the present work insight is given to amount of F-loss due to
the beam damage in respect to the investigated excitation volume or
duration of the measurement. A routine is presented for correction of the
measured values of the F-content and its limitations will be discussed with
regard to the effect of the microstructure on the properties and performance
of the cell.
add to my program
15:30 Coffee break
Materials for Energy Systems : Acha Hessler-Wyser
16:00 On the help of microscopies in the understanding of degradation
mechanisms observed on materials in Pressurized Water Reactor
Authors : Laurent LEGRAS
Affiliations : EDF R&D MAI, France
Resume : Even if temperature, pressure and chemistry of the cooling water
are not very high and aggressive, materials used in Pressurized Water
Reactor (PWR) are exposed to different degradation mechanisms. Some of
these materials (internal components, vessel,..) are also exposed to
irradiation leading to more complex degradation mechanisms. One of the
main goal of the research programs launch in that field is to develop
physical modelling of the mechanism down to the atomic scale. Such
approach need a clear description and understanding of the degradation
mechanism at the same scale. This talk will aim at illustrating the benefit of
microscopy (TEM, atom probe, dual beam microscopes, EBSD,...) up to the
very new promising possibilities of monochromated and aberrations
corrected TEM. A specific focus will be done on four different degradation
mechanism : irradiation aging, fatigue corrosion, stress corrosion cracking
and corrosion of stainless steel. 1- Irradiation aging : In the internal
structures of the PWR vessel are made of stainless steel. Irradiation induces
continuously punctual defects (vacancies and interstitials) which can be
eliminated on sink (surfaces, grain boundaries, dislocations). Interstitials
can aggregate forming disk shape i.e. dislocations loops or segregate on
grain boundaries. Vacancies could lead to the formation of cavities or
bubbles when combining with gas diffusion, or to reverse flux of species
when segregating on boundaries. The kinetics and the quantification of
these phenomena are performed using TEM and (tomographic) atom probe
and are used as key data for the understanding of mechanisms and for
modelling live time extension of actual PWR. 2- Fatigue corrosion : Specific
areas of primary circuit in PWR reactor can be affected by thermal fatigue.
Recent TEM studies on fatigue crack tips clearly showed that the effect of
corrosion is combined to the fatigue solicitation and thus that it have to be
taken into account. 3D images using FIB are now used as a first step to
understand and quantify this coupled effect. 3- Stress corrosion cracking
(SCC): Strain gradients and preferential sites of intergranular SCC initiation
appeared recently to be correlated. Combining complex strain on specimen
pre-mapped by EBSD and pre-covered by gold microgrids and the possibility
of extracting TEM thin foils on a precise location using dual beam offer a
promising possibility to understand fracture mechanism ahead crack tips.
Actual TEM studies using EFTEM, EELS & EDX of such specimen are trying to
understand the stability of oxides films at the cracks tips as a function of
crystallographic orientation and strain degree. 4- Corrosion SCC and
corrosion behaviour are controlled by the properties of the oxides films. The
well known duplex structure of the oxides is still suffering of some
uncertainties such as on the very first step of their growth and their
crystallographic structure. These two questions are currently under
4 1
investigation up to the atomic scale on very short exposure time using
monochromated and aberrations corrected electron microscope TITAN.
HRTEM and Astar software developed by Nanomegas and E. Rauch is used
to study crystallographic relationship between metal and oxide as well
EFTEM and HREELS to study the local chemistry of the oxide.
add to my program
16:30 Designing Semiconductor Photocatalyst/ Metal Cocatalyst Composites for
Water Splitting.
Authors : N.S. Hondow, Y-H. Chou, K. Sader, Y. Chimoupara, R. Mitchell, R.E.
Douthwaite and R.Brydson
Affiliations : Institute for Materials Research, SPEME, University of Leeds, U.K.;
Department of Chemistry, University of York, U.K.
Resume : One potential method for the conversion of solar into storable
energy is the use of semiconductors (so called photocatalysts) which
mediate the decomposition of water to hydrogen and oxygen. Oxide
semiconductors are a common choice due to their corrosion resistance and
the possibility of engineering their band gaps via doping. However
application of these materials is currently limited because of a low overall
efficiency, due to absorption being confined to the UV periphery of the solar
spectrum, rapid electron-hole recombination, and potentially poor surface
chemistry. To overcome the latter two problems cocatalysts, such as Pt,
RuO2 and NiO, are intentionally added to the surface of the photocatalyst to
act as electron traps and hydrogen evolution sites, thus increasing activity.
In this paper we detail a structural investigation of the semiconductors
NiTa2O6 and InTaO4 decorated with nickel/nickel oxide core shell cocatalyst
nanoparticles, similar to those presented in the literature and draw some
general conclusions about the design and stability of such co-catalysts. We
also discuss the possibilities for creating macroporous photonic band gap
structures from photocatalysts to enhance their overall efficiency.
4 2
add to my program
17:00 Structural and chemical investigations of the oxides formed on 316L alloy in
PWR environment
Authors : R. Soulas (1), L. Legras (1), M. Cheynet (2), T. Neisius (3), Y. Brechet (4)
Affiliations : (1) EDF R&D, 77250 Moret-Sur-Loing, France; (2) INP Grenoble CNRS
UJF, SIMAP, F-38402 St Martin Dheres, France; (3) Universit Paul Czanne, F-
13397 Marseille, France; (4) SIMaP INP Grenoble, F-38402 Saint Martin
dHegraveres, France
Resume : To improve the durability of PWR primary circuits with respect to
stress corrosion cracking, understanding of oxidation mechanisms is crucial.
316L alloy composing vessel internals and primary circuits is in contact with
PWR environment. This leads to the formation of an oxide with a double
layer (an inner part composed with a chromium enriched oxide and an outer
part composed with magnetite) in which cracks may be initiated in presence
of stress with or without irradiation. It appears, today, that oxidation
mechanisms are achieved during the first exposure minutes to the oxidizing
environment. It is, thus, essential to describe precisely the morphology, the
structure and the chemistry of the oxides forming the protective layers.
Thanks to a special oxidation loop allowing exposure times ranging from
minutes to few hours, it is possible to study the first steps of oxidation. To
avoid averaging effects resulting from crystallographic features, FIB thin
foils are taken out from grains with different orientations ([111], [110]),
after different oxidation times (1 minutes, 2 minutes, 10 minutes, 1 hour, 5
hours and 24 hours). TEM observations are carried out using either a
Tecnai20F (image, diffraction and EFTEM), a Titan 80-300 kV with objective
lens corrector (HRTEM) or a Titan 80-300 kV with monochromator and probe
lens corrector (HR-EELS and STEM). These observations provide precise
information at the nanometer scale concerning the chemistry (elemental
quantification, elemental electronic structure), the microstructure of oxide
layers (using ASTAR simulation) and the epitaxial relation between the inner
oxide layer and the metal. Macroscopic observations using XPS, Raman
spectroscopy and GIDRX are performed in parallel to confirm and generalize
microscopic conclusions about oxide formation. The amorphous chromium
enriched passive layer initially present at the surface of the specimen as
soon as air exposition, begins to crystallize as oxidation in primary water
occurs. ASTAR simulations from aberrations corrected HRTEM images
showed that the Cr rich inner oxide layer evolves from nano-grains to
monocrystalline grain. The unique cristal of fcc spinel AB2O4 oxide has a
close epitaxial relationship with the sublying metal grain. A double network
4 3
of misfit dislocation is observed at the metal/oxide interface. Edge
dislocations with burger of [220] and [202] are localized every seven atomic
planes of the metal compensating the 16% of misfit between oxide and
metal lattice parameters. The outer layer is formed of well shaped
crystallites of magnetite. The fine electronic structure obtained using HR-
EELS are also confident with the spinel AB2O4.
add to my program
17:15 Radiation induced structural and magnetic changes in Fe-Cr alloys
Authors : A. Idhil (1), C.N. Borca (1), A.-C. Uldry (1), D. Grolimund (1), C. Hebert
(2), M. Samaras (3)
Affiliations : (1) Paul Scherrer Institute, CH-5232 Villigen, Switzerland; (2) cole
Polytechnique Fdrale de Lausanne, CH-1015 Lausanne, Switzerland; (3)
Switzerland
Resume : We investigate irradiation damage mechanisms and changes in
microstructure upon ion-beam implantation of the model Fe1-xCrx alloys,
with x up to 20%. Fe+-beam implantation simulates the effect of neutron
irradiation with respect to formation and evolution of atomic displacement
cascades. Using EXAFS and micro-XRD techniques we could investigate the
changes in atomic structure leading to formation of displacement cascades
which affect the fundamental mechanical properties of these materials.
Additionally, the influence of irradiation on the elemental magnetic moments
has been investigated using XMCD. We observed that the implantation
temperature has the biggest impact on the atomic and magnetic structures
of the model Fe1-xCrx alloys. These experiments not only bring insight into
the material structure, but also enable a robust modeling tool to be
developed.
4 4
add to my program
17:30 Structure determination and chemical analyses in complex tungstates
materials
Authors : L. Patout (1), T. Renovato dos Santos (1,2), A.L. Lopez-Moriyama (1,2),
C. Pereira de Souza (2), M. Arab (1), Ch. Leroux(1)
Affiliations : (1) IM2NP UMR CNRS 6242 Universit Sud Toulon Var, BP20132,
83957 La Garde Cedex, France; (2) Universidade Federal do Rio Grande do Norte,
DEQ/PPGEQ/LTRC, Campus Universitrio, Lagoa Nova, 59072-970, Natal, Brasil
Resume : It is possible to produce syngas (CO and H2) from natural gas in
presence of catalysts. The reform of natural gas CH4, followed by an
adequate filtering, is an alternative for the hydrogen production. However,
due to the high stability of methane it is necessary to develop new high
temperature materials. We developed chemical routes to synthesize
nanostructured materials based on tungstate of rare earths elements. We
focused on cerium and strontium based tungstates. Only SrWO4 and Ce2
(WO4)3 have known structures. We tentatively synthesised cerium
tungstate with Ce4+ and obtained mixed powder of a new phase with
stoichiometry CeW2O8 , and Ce2(WO4)3. The space group of this new
phase is determined by means of various quantitative electron diffraction,
among them microdiffraction. Microdiffraction patterns of high symmetry
zone axes reveal the Bravais lattice, the presence of glide mirrors and
helicoidal axis. Precession experiments are also envisaged. First results
indicate this new phase is orthorhombic. Stoichiometric SrWO4 as well as
powders with excess of W or Sr were synthesized in order to determine if
Sr1 W1 O4 may exist. The EDS analyses of these compounds revealed
a failure of commercial EDS software in the relative quantification of Sr and
W. The ternary tungstates with Sr and Ce exhibit unexpected tetragonal
scheelite structures, as the few ternary tungstate found in the literature are
monoclinic. This work was supported by the CAPES -COFECUB and ARCUS-
BRAZIL funds.
4 5
add to my program
17:45 TEM analysis of nanoporous Ptn+-CeOx catalyst on CNTs
Authors : V. Potin (1)*, S. Bruyre (1), V. Matoln (2), I. Matolnov (2), M.
Vorokhta (2), and S. Bourgeois (1)
Affiliations : (1) I.C.B. - Laboratoire Interdisciplinaire Carnot de Bourgogne, UMR
5209 CNRS - Universit de Bourgogne, 21078 Dijon CEDEX, France; (2) Charles
University, Faculty of Mathematics and Physics, Department of Surface and Plasma
Science
Resume : In this study we report TEM study of carbon nanotubes coating
by Pt-CeO2 catalyst by using simultaneous magnetron sputtering of
platinum and cerium oxide. This technique permits to prepare oxide layers
continuously doped with Pt atoms during the growth. The Pt doped
4 6
sputtered cerium oxide films contain high concentration of cationic platinum
Pt2+ and Pt4+ (nearly 100%) which opens the way for using such systems
as highly active thin film catalysts. Different samples were investigated, with
different Pt content. Platinum and cerium were deposited simultaneously by
rf-magnetron sputtering on multiwall carbon nanotubes (MWCNT) deposited
by sedimentation on silicon substrate or grown perpendicularly to the silicon
wafer by the chemical vapor deposition technique. SEM and STEM
experiments reveal the high porosity of the deposited layers. Studies of
HRTEM images indicate the presence of CeO2 crystallized nanoparticles.
Pt4+ cations are in substitution positions of the face centered cubic lattice of
cerium oxide, as Ce4+1-x Pt4+xO2. Moreover, in the case of MWCNT
deposited by sedimentation, STEM images show that the deposition is
inhomogeneous, as one face is more exposed to the deposited species. With
EDX experiments performed in STEM mode, the Ce/Pt ratio was studied in
function of the deposit localization. EELS experiments were also performed
to study the evolution of Ce4+/Ce3+ ratio. This research is supported by
ANR within IMAGINOXE project (ANR-11-JS10-001).
add to my program
18:00 Tungsten carbide identification in a re-deposited layer on an ASDEX
Upgrade divertor tile
Authors : M. Rasinski (1), M. Balden (2), M. Mayer (2), R. Neu (2), T. Pociski (1),
M. Lewandowska (1), K.J. Kurzydlowski (1)
Affiliations : ASDEX Upgrade Team (1) Warsaw University of Technology; Faculty of
Material Science and Engineering Woloska 141, 02-507, Poland, (2) Max-Planck-
Institut fr Plasmaphysik, Euratom Association, Boltzmannstrae 2, D-85748
Garching, Germany
Resume : Erosion and redeposition of plasma-facing materials is one of the
most important issues in fusion devices and therefore is an area of interest
for many research groups. However, the structure and composition of re-
deposited layers as well as the mechanism and condition of their formation
are not fully described and understood yet. In the present study, structure
and phase composition of the deposited layer (500 - 1000 nm in thickness),
which grew during the 2007 campaign on a tile from the inner strike point
region in the ASDEX Upgrade divertor, were examined. High resolution
scanning transmission electron microscopy (HR STEM) combined with local
nano-diffraction technique have been used to identify the deposits phase
composition, supported by energy-dispersive X-ray spectroscopy (EDX) and
electron energy loss spectroscopy (EELS). In the deposited layer two types
of tungsten carbide (WC1-x and W2C) were identified. The phase
composition results from the layer deposited in the divertor were compared
with those obtained from amorphous carbon thin films doped with different
tungsten concentration which were subjected to annealing at different
temperatures. Such specimens can be considered as model system for the
re-deposit creation on the divertor. The correlation between the phase
composition of the model system layers and the real deposit from the
divertor provides information about local conditions during the creation of
the deposits.
4 7
add to my program

Back

strasbourg.com
14 May 2012 15 May 2012 16 May 2012
hide a
Symposium : X

Photovoltaics : Wolfgang Jger
08:30 Electron energy-loss spectroscopy of dopant concentration profiles and
optical absorption in thin film silicon solar cells
Authors : Rafal E. Dunin-Borkowski, Martial Duchamp, Chris B. Boothroyd, M. Sergio
Moreno, Bas B. Van Aken, Wim J. Soppe
Affiliations : Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons,
Peter Grnberg Insititute, Forschungszentrum Jlich, D-52425 Jlich, Germany;
Centro Atmico Bariloche, 8400 S. C. de Bariloche, Argentina; ECN Solar Energy,
P.O. Box 1, NL-1755 ZG Petten, The Netherlands
Resume : We use electron energy-loss spectroscopy (EELS) to study thin
film silicon solar cells on plastic, glass and metallic substrates prepared for
transmission electron microscopy (TEM) using focused ion beam milling. For
a solar cell in which an intrinsic amorphous silicon layer is sandwiched
between 10-nm-thick n-doped and p-doped amorphous silicon layers, we
use core loss EELS to measure the boron concentration quantitatively and
compare our measurements with real space ab initio multiple scattering
calculations. For a sample that contains 200-nm-thick i-SiC, p+-SiC and
p++-SiC layers sandwiched between back (ZnO/Ag) and front (ITO) contact
layers, we use monochromated EELS to correlate changes in plasmon
energy with measurements of boron concentration made using secondary
ion mass spectrometry. We discuss whether the observed changes in
plasmon energy across the device can be related directly to the boron
concentration in the doped layers. We also assess whether monochromated
EELS can be used to map plasmon absorption in Ag reflector layers
sputtered onto rough ZnO with a spatial resolution of better than 10 nm.
The correlation of such measurements with the microcrystalline structure of
the layers, including variations in composition at grain boundaries, is
important for understanding the origin of parasitic optical absorption, which
decreases the photo-generated current.
5 1
add to my program
09:00 Microscopy study of thin-film polycrystalline silicon solar cells, were optical
electrical and structural material characterization, in the sub micron range,
meets each other
Authors : D. Van Gestel, J. Deckers, I. Gordon, J. Poortmans
Affiliations : IMEC vzw, Kapeldreef 75, B-3001 Leuven, Belgium
Resume : Thin-film polycrystalline-silicon (pc-Si) solar cells with a grain
size in the order of 1-100 micron could substantially lower the price of
photovoltaic (PV) energy. Similar to bulk silicon PV there is a need to
combine electrical optical and structural characterization to support R&D.
However because many properties of pc-Si material are one or more orders
smaller then for bulk Si, advanced new and or improved characterization
techniques are needed. In this contribution we will discuss and show the
usefulness of different quantitative characterization methods throughout the
whole pc-Si solar cell production process. The pc-Si material was made by
epitaxial thickening of a seed layer. Structural properties were measured
with electron back scattered diffraction (EBSD), transmission and scanning
electron microscopy (TEM,SEM), defect etch, atomic force microscopy
(AFM), X-ray diffraction (XRD) and Raman microscopy. For electrical
characterization mainly current-voltage (IV) measurement, electron beam
5 2
induced current (EBIC) measurement and scanning spreading resistant
microscopy (SSRM) were used. Transmission-reflection and quantum
efficiency measurements were applied to study optical properties whereas
photoluminescence (PL), secondary ion mass spectroscopy (SIMS) and total
X-ray reflection measurements (TXRF) were used to monitor contamination
issues. All these methods were successfully combined to study the influence
of different variations throughout the whole solar cell processing.
add to my program
09:30 Evolution of surface roughness and grain size in the transition from
amorphous to microcrystalline silicon thin films growth
Authors : E. Farsari, A.G. Kalampounias, N. Spiliopoulos, E. Amanatides, D. Mataras
Affiliations : Plasma Technology Lab., Dpt. of Chemical Engineering, University of
Patras Patra GR26504, Greece
Resume : Hydrogenated microcrystalline silicon is a mixed phase material
consisting of micro- and nano-crystallites embedded in an amorphous
matrix. This material has attracted great scientific interest due to its
application in thin film transistors and solar cells. The physical,
morphological and chemical properties of the material, determined by the
deposition conditions, affect the final performance of the optoelectronic
devices. Several microscopic techniques such as TEM, STM, AFM, KPFM,
SNOM have been used in order to examine the morphological, electronic and
optoelectonic properties of microcrystalline Si:H thin films. The purpose of
this work is to use conventional and conductive AFM for the characterization
of Si:H films deposited near the transition to a-Si:H growth. The materials
deposited under such conditions present the best performance when
incorporated to the devices. The samples were deposited by Silane-
Hydrogen glow discharges at different experimental conditions in order to
cross the transition from amorphous to microcrystalline growth. The
topography of the samples was examined by AFM measurements and the
variation of the surface roughness was calculated. The estimation of the
crystallinity and the distribution of crystallites size were achieved by
conductive AFM under ambient conditions, while oxidation effects were also
examined. The above mentioned results are compared with FESEM and
Raman Spectroscopy measurements and the observed differences are
discussed.
5 3
add to my program
09:45 EFTEM studies of Si nanowire networks in SiO2 for thin film PV cells
Authors : B. Liedke (1), A. Mcklich (1), K.-H. Heinig (1), B. Schmidt (1), D.
Friedrich (1), U. Keles (2), C. Bulutay (2)
Affiliations : (1) Helmholtz-Zentrum Dresden-Rossendorf, 01314 Dresden,
Germany; (2) Bilkent University, Physics Department, 06800 Bilkent, Ankara, Turkey
Resume : Si based nanostructures became in the last years a promising
material for the PV cells. The quantum confinement effect of Si
nanostructures allows for band gap engineering by size manipulation which
can be used for optimization sun light absorption. Here, we consider SiOx
layers deposited by magnetron sputtering. By subsequent rapid thermal
processing, SiOx decays by spinodal decomposition into a network of Si
nanowires (NWs) in SiO2. To get images of the morphology of Si NWs in
SiO2 it is not sufficient to use mass contrast or lattice plane imaging. The Si
and SiO2 phases can only be distinguished by energy filtering of the
transmitted electrons (EFTEM). Here, the relative energy shifts of the
plasmonic valence band resonances of Si and SiO2 are used. HR-EFTEM
techniques are applied to study morphology and crystallinity of the Si NW
networks fabricated from different metastable SiOx. To facilitate
understanding of the TEM images, details of decomposition are studied using
kinetic Monte-Carlo (KMC) simulations. For the EFTEM images, density-
density correlations are calculated to determine the structure size of NW
network, which are then compared with the 3D morphologies provided by
KMC. Combining EFTEM with KMC allows us to predict and control the
average size of the NWs. Former studies and our electronic structure
calculations provide a guideline for band gap optimization of Si NW
networks, thus paving the way to band gap engineering via control of the
mean NW diameter.
5 4
add to my program
10:00 Coffee break
10:30 Material science for high-efficiency III-V solar cells
Authors : F. Dimroth, T. Roesener, V. Klinger, R. Kellenbenz, A. Wekkeli
Affiliations : Fraunhofer Institute for Solar Energy Systems ISE, Heidenhofstrasse
2, 79110 Freiburg, Germany
Resume : III-V multi-junction solar cells are reaching the highest
conversion efficiencies of sunlight into electricity. These solar cells consist of
complex layer structures which can contain up to 40 different layers.
Excellent material quality and low dislocation density is a requirement for
these high efficiency devices. In 2009, Fraunhofer ISE reached for the first
time an efficiency of 41.1 % under concentrated sunlight with a
metamorphic (lattice mismatched) Ga0.35In0.65P/Ga0.83In0.17As cell
structure on Ge. Today, lattice-mismatched growth is used in many cell
architectures including III-V solar cells on silicon and inverted metamorphic
structures. Understanding the origin and propagation of dislocations is an
important requirement for the development of these solar cells. Structural
analysis of the layer stack by transmission electron microscopy helps to
understand the formation and propagation of misfit and threading
dislocations in the metamorphic layers. But these techniques have to be
combined with additional methods like high-resolution x-ray diffraction, EPD
of threading dislocation densities, measurements of material hardness and
surface roughness to generate a full picture of suitable growth conditions
and materials. The presentation will give an insight into the essential
methods which support the development of todays highest efficiency solar
cells.
5 5
add to my program
11:00 High Resolution Characterisation of CdCl2-treated CdTe Thin-film Solar Cells
Authors : Ali Abbas (1), Paul Rowley (2), Geoff West (1), John Walls (2), Jake
Bowers (2), Piotr Kaminski (2)
Affiliations : (1) School of Materials; (2) CREST, School of Electronic, Electrical and
Systems Engineering, Loughborough University, Leics. LE11 3TU, U.K.
Resume : Cadmium Telluride (CdTe)-based photovoltaic devices represent a
promising route towards the realisation of low cost thin film solar cells of
efficiencies above 16%. However, the current level of fundamental
understanding of key process routes towards optimised cells, such as
improved doping, cadmium chloride recrystallization and contacting is
somewhat poor. In this paper, we present the results of a comprehensive
programme of high-resolution characterisation of CdTe solar cells, with a
focus on the analysis of cadmium chloride (CdCl2) treatments and the
objective of gaining a deeper mechanistic understanding of their impacts on
cell performance. A range of characterisation techniques, including EBSD
(Electron Backscatter Diffraction) analysis, STEM (Scanning Transmission
Electron Microscopy) and electron nano-spectroscopic elemental mapping
were applied. Analysis of CdCl2-treated cells shows the presence of chlorine
rich regions at the CdTe/CdS interface, along with an indication of chlorine
and sulphur segregation at CdTe grain boundaries. Furthermore, in addition
to significant grain refinement, an impact on the prevalence of intragranular
stacking faults is indicated. The results of grain orientation mapping before
and after treatment are also presented. Finally, the relevance of the work to
the construction of numerical models that aid the understanding of
fundamental aspects of cell function such as electron trapping and diffusion
are presented.
5 6
add to my program
11:15 Structure-property relationships in thin-film solar cells by electron
microscopy
Authors : Daniel Abou-Ras (1), Sebastian Schmidt (1), Jaison Kavalakkatt (1),
Melanie Nichterwitz (1), Hubert Schulz (2), Katja Tsyrulin (2), Frank Bauer (3),
Christoph T. Koch (4), Bernhard Schaffer (5), Miroslava Schaffer (5)
Affiliations : (1) Helmholtz-Zentrum Berlin fr Materialien und Energie, Hahn-
Meitner-Platz 1, 14109 Berlin, Germany; (2) Carl Zeiss NTS GmbH, Carl-Zeiss-
Strasse 56, 73447 Oberkochen, Germany; (3) Oxford Instruments GmbH,
NanoAnalysis, Otto-von-Guericke-Ring 10, 65205 Wiesbaden, Germany, (4) Institute
for Experimental Physics , Ulm University, Albert-Einstein-Allee 11, 89081 Ulm,
Germany, (5) SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington,
WA4 4AD, U.K.
Resume : Among all thin-film solar cells, those with polycrystalline Cu
(In,Ga)Se2 absorber layers have shown the highest power-conversion
efficiencies of currently more than 20 %. It is an essential issue of further
improvements of this kind of solar cells to relate microstructural properties
5 7
of the Cu(In,Ga)Se2 thin films to the corresponding device performances.
Optimizing the microstructure is key for power-conversion efficiencies of 21
% and beyond. For this aim, electron microscopy provides various imaging
and analysis techniques. Cross-section preparation, imaging, and also
analysis can all be performed by applying a focused ion beam (FIB)
machine. However, the incongruent ion-beam sputtering of Cu(In,Ga)Se2
leads to formation of agglomerates, which can be reduced substantially by
use of reactive gases. The introduction of XeF2 during FIB slicing resulted in
excellent images, in which the microstructures of most layers in the Cu
(In,Ga)Se2 thin-film stack are visible, including the microstructure of the 20
nm thin MoSe2 layer. Acquisition of high-quality two-dimensional and also
three-dimensional electron backscatter diffraction (EBSD) data was possible.
Combination of EBSD with energy-dispersive X-ray spectrometry provides
means for unambiguous phase analysis, while the acquisition of EBSD,
electron-beam-induced current, and cathodoluminescence measurements on
identical specimen positions give information on the electrical and
optoelectronic properties of grain boundaries in polycrystalline Cu(In,Ga)Se2
layers. Electron holography measurements provide insight in potential
distributions around structural defects, which, for grain boundaries, can be
related directly to a change in composition.
add to my program
Organic Photovoltaics : Hugo Bender
11:30 Investigation of aged organic solar cells stacks by cross-sectional
transmission electron microscopy coupled with elemental analysis
Authors : P. Favia (1), E. Voroshazi (2), P. Heremans (1), H. Bender (1)
Affiliations : (1) imec, Kapeldreef 75, B-3001 Leuven, Belgium; (2) Katholieke
Universiteit, Arenberg Kasteelpark 10, ESAT, B-3001, Leuven, Belgium
Resume : Polymer solar cells are of great interest as candidates for future
low-cost and light-weight energy sources. One of the major reliability
problems of these devices is the thermal instability of the blend morphology
composed of poly(3-hexylthiophene) and [6,6]-phenyl-C61-butyric acid
methyl ester (P3HT, PCBM). Phase segregation of the blend has been
extensively investigated by transmission electron microscopy (TEM) on free-
standing films. In this study, we investigate in cross-section the morphology
reorganization of P3HT:PCBM layers confined between poly(3,4-
ethylenedioxythiophene)poly- (styrenesulfonate)(PEDOT:PSS) and a metal
electrode similarly to solar cell devices. Combining TEM imaging of the layer
stack with energy dispersive spectroscopy (EDS), we not only gain insight
into the vertical phase segregation process but also explore the
interdiffusion and adhesion in the layer stack. Over 100 C annealing leads
to the formation of elongated particles of ~ 300 nm height, which are mostly
composed of carbon, signature of PCBM. Thinning of the neighboring areas
indicates the direction of the diffusion. Interestingly, the metal cathode
remains conformal to these large aggregates and the particles protrude
through the metal layer only after 300 h. Furthermore, we also show the
crystalline nature of these particles embedded in the amorphous matrix.
Elemental analysis confirms that the diffusion of the electrode materials (In,
Na and Yb) remains below the detection limit.
6 1
add to my program
12:00 Impact of thermal annealing on the morphology and interfacial composition
of bulk heterojunction organic solar cells
Authors : P. G. Karagiannidis, N. Kalfagiannis, A. Laskarakis, D. Georgiou, C.
Pitsalidis, S. Logothetidis
Affiliations : Laboratory for Thin Films-Nanosystems and Nanometrology (LTFN),
Physics Department, Aristotle University of Thessaloniki, GR-54124, Thessaloniki,
Greece
Resume : Nowadays, organic solar cells have attracted enormous interest
due to their great technological potential as a renewable energy source, the
advantage of high efficiency-to-cost ratio, the low weight and mechanical
flexibility of organic materials and the easy thin-film casting technology.
Since the introduction of bulk heterojunction, a substantial progress in
organic solar cell performance has been achieved. Although a lot of research
has been made at the efficiency race, the morphology evolution that defines
the device performance and lifetime is still under investigation. In this work,
we have studied the effect of thermal annealing on the morphology and the
interfacial composition of poly(3-hexylthiophene) (P3HT): Phenyl-C61-
6 2
butyric acid methyl ester (PCBM) blends. Lateral phase separation was
identified by Atomic Force Microscopy and Optical Microscopy, and its
evolution with the duration of annealing and temperature from the nano- to
the micro-scale was quantified by the statistical parameters of surface
roughness and the power spectral density. Spectroscopic Ellipsometry in the
NIR-Vis-farUV spectral region revealed P3HT segregation at the top region of
the films and PCBM accumulation at the bottom interface. This vertical
phase separation, which is related to the difference in the surface energies
of the P3HT, PCBM and the substrate, was found to have a dramatic effect
on the device performance.
add to my program
12:15 Solution-processed LiF for work function tuning in organic solar cells
Authors : Taner Aytun, Ayse Turak, Iain Baikie, Grzegorz Halek, and Cleva W. Ow-
Yang
Affiliations : Sabanci University, Max Planck Institute for Metals Research, KP
Technology, Ltd.
Resume : The indium-tin-oxide/active layer interface is critical to the
performance of organic solar cell devices. Though PEDOT:PSS is widely used
as an interlayer, poor energy level matching with the active polymer blend
can lead to poor long term performance. The possibility of tailoring the work
function to match the energy level of the active organic layer is of great
interest in the fabrication of organic devices to form barrier-free Ohmic
contacts, where the work function no longer controls device performance. In
this study, submonolayer films of LiF nanoparticles are deposited on the
electrode surface with the assistance of polymeric micelle reactors that also
enable particle deposition with controlled nanoscale surface coverage.
Scanning Kelvin probe microscopy is used to determine the global average
surface work function of the LiF/ITO bilayer. The results reveal a work
function tunable with nanoparticle coverage with higher values than that of
bare indium tin oxide (ITO). As thermally evaporated LiF typically lowers the
surface work function, the tunable behavior of the solution-processed LiF
nanoparticles on ITO is attributed to a lateral depolarization effect, with the
effective dipole direction switching as full surface coverage is obtained.
Incorporation of the solution-processed bilayer electrodes into a
conventional P3HT:PCBM device shows significant improvement in device
performance, especially when used in combination with a PEDOT:PSS layer.
The results indicate that interface energy level engineering is an essential
tool for future device optimization requirements.
6 3
add to my program
12:30 Lunch
14:15 Microstructure imaging and chemical analysis of photoactive thin films on
carbon tube biohybrids by HR SEM and FT-IR spectroscopy
Authors : O. Kysil (1), V. Frolov (2), I. Tomylko (1), O. Ivanyuta (1), E. Buzaneva
(1), U. Ritter (3), P. Scharff (3)
Affiliations : (1) National Taras Shevchenko University of Kyiv, 01601 Kyiv,
Ukraine; (2) Paramed Company, 03187 Kyiv, Ukraine; (3) TU Ilmenau, Institut fr
Chemie und Biotechnology, 98684 Ilmenau, Germany
Resume : The investigation is aimed to develop architectures models, to
biodesign and to test microstructure, chemical content of photoactive in UV-
visible range thin films on carbon single-, multiwall tubes integrated by
biomolecules that control optical properties of the films. Selected
biomolecules (cysteine and phenylalanine) non-covalently interact with the
hydroxyl and oxygen surface groups of carbon tubes to form film
microstructure, chemical content and their photoactivity in UV-visible range
for PV cells. HR SEM images and elemental mapping are taken to visualize
the organized film microstructures from the biomolecules and carbon tubes
during drying of their suspensions on silicon surface. FT-IR spectroscopy is
used for chemical analysis and characterization of the interactions between
tubes and biomolecules during the film microstructure organization. The film
microstructures were also characterized by optical absorbance in 200-
650nm wavelength range and photoluminescence spectra for the laser
illumination (337, 420 nm). The experimental results confirm the developed
model for donor-acceptor pair organization in photoactive biohybrids carbon
nanotubes networks into the films. The concept of these microstructure and
elemental mapping influence on an optical activity in different ranges of the
thin film PV cells is based on developed model for photoresponse of
6 4
biohybrids materials on carbon nanotube that has bond with modified by
biomolecule ends and/or walls carbon nanotube.
add to my program
14:30 Study of the microstructure of inkjet printed P3HT:PCBM blend for
photovoltaic applications
Authors : Immacolata Angelica Grimaldi (1,2), Rosita Diana (1), Pasquale Morvillo
(1), Fausta Loffredo (1), Fulvia Villani (1)
Affiliations : (1) ENEA, UTTP-NANO,Piazzale Enrico Fermi 1, 80055 Portici (Naples),
Italy; (2) Department of Physics Science, University of Naples Federico II, Piazzale
Tecchio 80125, Naples, Italy
Resume : Recently, great interest has been devoted to cost-effective
alternative energy sources such as organic solar cells due to the low cost of
fabrication, the mechanical flexibility and the versatility of chemical
structure and ease of processing. As concerning this last point, the
possibility of organic materials processing by solutions at low temperatures
makes them employable for fabricating printed solar cells by using inkjet
printing technology. The most exploited active material for photovoltaic
devices is the regioregular poly(3-hexylthiophene) (P3HT), p-type
conjugated polymer, blended with [6,6]-phenyl-C61-butyric acid methyl
ester (PCBM), n-type material. In the present work, we studied the influence
of the chemico-physical properties of the solvents on the morphology of the
active layer through optical and morphological (AFM, SEM) analyses. The
micostructure of the photoactive material was optimized by combining the
mixing ratios of the solvents and the printing parameters (drop emission
frequency, drops overlapping degree, substrate temperature) thus
improving the electrical performances of the organic solar cells.
6 5
add to my program
14:45 Understanding the morphology of the active layer in organic solar cells: A
TEM based approach
Authors : Kulpreet Singh Virdi, Alaa Abdellah, Markus Dblinger, Paolo Lugli,
Giuseppe Scarpa, Christina Scheu
Affiliations : Department of Chemistry, Ludwig-Maximilians-Universitt Mnchen,
Germany; Institute for Nanoelectronics, Department of Electrical Engineering and
Information Technology, Technische Universitt Mnchen, Germany
Resume : The increasing push for cleaner energy sources has fuelled
research in the direction of photovoltaics and other light harvesting devices.
Conventionally, the harvesting of solar energy has been dominated by
silicon based photovoltaic devices. However recently fully organic solar cells
comprising of an active layer of organic materials have acquired the
spotlight. These organic solar cells offer exciting prospects because of their
economical fabrication and easy integration into circuitry. Despite a varied
choice of materials available for active layer, [6,6]-phenyl-C61 butyric
methyl ester (PCBM) and poly(3-hexylthiophene) (P3HT) have been used as
acceptor and donor respectively. It has been widely reported in literature
that annealing improves the device performance, though the mechanism of
microstructure evolution due to annealing is not yet fully understood. We
have investigated fully organic solar cells fabricated using spray coating
technology using transmission electron microscopy (TEM), selected area
electron diffraction (SAED), scanning transmission electron microscopy
(STEM) and energy dispersive X-ray spectroscopy (EDS). Results indicate
the annealed active layer to comprise of a highly crystalline PCBM layer
widely varying in thickness and a P3HT rich layer uniform in thickness.
These results do comply with some recent reports postulating diffusion of
PCBM into P3HT during annealing, however further work is necessary to
strengthen the theory for better understanding of such device interfaces.
6 6
add to my program
15:00 Microstructural aspects of transition metal oxide p-type doping of organic
semiconductors
Authors : L. Dieterle (1,2), K. Schultheiss (1,2), M. Pfannmller (3), D. Donhauser
(1,2), M. Krger (1,2), R.R. Schrder (2,3), W. Kowalsky (1,2)
Affiliations : (1) Institut fr Hochfrequenztechnik, Technische Universitt
Braunschweig, Germany; (2) InnovationLab GmbH, Heidelberg, Germany; (3)
CellNetworks, Universitt Heidelberg, Germany
Resume : Electrochemical doping is essential to overcome limitations in
organic semiconductors devices imposed by low intrinsic conductivity and
high charge injection barriers at the contacts. Materials with very deep lying
HOMO-levels like 4,4'-Bis(N-carbazolyl)-1,1'-biphenyl (CBP) can be p-type
doped with transition metal oxides, e.g., MoO3. CBP or other wide bandgap
6 7
materials are commonly used in organic light emitting diodes (OLEDs).
However, dopant activation meaning the relation between charge carrier
density and MoO3 doping concentration is in the range of 1-2 %.
Therefore, high doping ratios, which can exceed 10 mol %, are often applied
for doping CBP. To find the origin of this effect, the microstructure of MoO3-
doped CBP organic thin films was studied by transmission electron
microscopy, electron spectroscopic imaging (ESI) and electron tomography.
Instead of homogenously dispersed MoO3 dopants, MoO3 forms amorphous
agglomerates. Electron tomography revealed the filament-like nature of
these agglomerates, which are preferentially oriented along the growth
direction of the thin film. Because charge carriers in organic thin films are
normally localized at single molecules, it can be expected from our results
that charge transfer occurs at the interface of CBP and the MoO3 nano-
filaments. First results on co-evaporated CBP/MoO3-films on cooled
substrates show homogeneously dispersed MoO3 without agglomeration
indicating a possibility to enhance the low doping efficiency.
add to my program
15:15 Coffee break
Poster session : Acha Hessler-Wyser, Thomas Hche, Hugo Bender, Wolfgang
Jger
16:00 Cross-Section STEM Study of Bonding Concepts for Solar Cells
Authors : D. Hussler (1), M. Kurttepeli (1), S. Essig (2), K. Derendorf (2), F.
Dimroth (2), W. Jger (1)
Affiliations : (1) Microanalysis of Materials, Christian-Albrechts-University Kiel,
24143 Kiel, Germany; (2) Fraunhofer Institute for Solar Energy Systems ISE, 79110
Freiburg, Germany
Resume : Crystalline silicon based multi-junction solar cells are a promising
way to circumvent the conversion efficiency limits of conventional single-
junction photovoltaic cells. In GaInP/GaAs/Si multi-junction solar cells, the
visible and near infrared wavelength range of the solar spectrum is
converted more efficiently when compared to solar cells produced
conventionally. As a decisive step of the technology a bonding process is
aimed in which a GaInP/GaAs sub-cell is contacted with a Si substrate. The
interface between GaAs and Si is of great importance for the total efficiency
of this multi-junction cell. Cross-section TEM samples are prepared from two
types of GaInP/GaAs/Si multi-junction solar cell specimens. In order to
investigate the bonding concepts, between the GaAs middle-cell and the Si
bottom-cell, in the vicinity of the bonding interface, elemental distributions
have been analyzed using STEM / EDXS and pictured using spectra and
elemental maps. With the help of HRTEM micrographs an amorphous layer
has been detected in the samples and gauged with high accuracy.
P 1
add to my program
16:00 Microstructural studies of fluorine-implanted titanium aluminides for
enhanced environmental durability
Authors : Rossen A. Yankov (1)*, Andreas Kolitsch (1), Johannes von Borany (1),
Frans Munnik (1), Arndt Mcklich (1), Alexander Alexewicz (2), Hartmut Bracht (2),
Harald Rsner (2), Alexander Donchev (3), Michael Schtze (3)
Affiliations : (1) Institute of Ion Beam Physics and materials Research, Helmholtz-
Zentrum Dresden-Rossendorf e.V,. POB 510119, 01314 Dresden, Germany; (2)
Institute of Materials Physics, University of Muenster, Wilhelm-Klemm-Str. 10, D-
48149 Muenster; (3) Karl-Winnacker-Institut, High-Temperature Materilas,
DECHEMA e.V., Theodor-Heuss-Allee 25, D-60486 Frankfurt am Main, Germany
Resume : Titanium aluminides based on the gamma-phase (gamma-TiAl)
are promising materials for advanced power generation, aerospace and
automobile applications. Oxidation-resistance problems, however, limit the
maximal service temperature of these alloys to about 700C. A significant
improvement in environmental durability of gamma-TiAl up to 1050C can
be achieved by ion-implanting fluorine into the alloy subsurface relying on
the so-called halogen effect. In this work, characterization of the
microstructure of F-implanted gamma-TiAl has been undertaken using cross-
sectional transmission electron microscopy in conjunction with energy-
dispersive X-ray spectroscopy and electron energy loss spectroscopy.
Preliminary studies by elastic recoil detection analysis have revealed
P 2
anomalously broad, high-concentration (up to 70 at. %) F profiles of either
Gaussian or plateau-like shape extending to much larger depths than those
predicted by theory. It has been found that the F profiles are not associated
with standard F diffusion, but rather result from a complex
amorphiztation/phase-transition process, which occurs via the implant
zone/substrate interface progressing toward the bulk. The final F distribution
is implantation-temperature dependent, with higher temperatures causing
partial dynamic self-annealing of the amorphized material and profile
shrinkage. The analyses have been helpful in understanding the behavior of
the F-implanted TiAl from both a basic scientific and a technological
standpoint.
add to my program
16:00 FIB-SEM and HRTEM investigations of microstructure of chalcogenide films
Authors : R. Brinia, G. Schmerberb. M. Kanzaria, B. Reziga
Affiliations : (1) Laboratoire de Photovoltaque et Matriaux Semiconducteurs
(LPMS), Ecole Nationale d'Ingenieurs de Tunis (ENIT), 1002 Tunis, Tunisia; (2)
Institut de Physique et Chimie des Matriaux Strasbourg (IPCMS), UMR 7504 CNRS-
UDS, 67034 Strasbourg, France.
Resume : We investigate the microstructure of CuAlS2 thin films deposited
on Silicon (111). The polycristaline films with different preferred grain
orientations are grown by thermal evaporation from powder of synthesis
deposited inelemental sources. The CuAlS2 film was analyzed using focused
ion beam-scanning electron microscopy (FIB-SEM), and HRTEM. FIB-SEM
cross-sectioned images revealed that the irregular-shaped particles were
embedded in the film and that the surface region and the bulk are
structurally similar, with no ordered defect chalcopyrite structure observed.
However, their composition is slightly different, indicating that they can have
different point defect physics. Microstructure properties of the films was with
a transmission electron microscope. (112) textured films show sharp
contrasts at the grain boundaries, whereas grain boundaries in (220/204)
textured films give only very weak contrasts indicating a preferential
population of electronically rather inactive grain boundaries. Nonchalcopyrite
ordering of the metal atoms in CuAlS2 is observed by TEM, which is
identified as CuAu-type ordering. Sharp spots in electron diffraction patterns
reveal the ordered Cu and Al atom planes alternating along the [001]
direction over a long range. High-resolution electron microscopy confirms
this ordering. The CuAu-ordered structure coexists with the chalcopyrite
ordered structure, in agreement with theoretical prediction. This paper
shows that dual beam FIB-SEM seems to be an easy, less time consuming
and useful method to characterize the cross-sectioned particles of CuAlS2
films
P 3
add to my program
16:00 Quantitative study of structure factors at large reciprocal vectors using
convergent beam electron diffraction: Application to anharmonicity of the
thermal motion in Mg2Si
Authors : Kjetil Valset (1), Oystein Prytz (1), Vidar Hansen (2), Johan Tafto (1)
Affiliations : (1) Department of Physics, University of Oslo, P.O. Box 1048, N-0316
Oslo, Norway; (2) Faculty of Science and Technology, University of Stavanger, 4036
Stavanger, Norway
Resume : A wide angle convergent beam electron diffraction technique is
used to determine structure factors with high accuracy from nanoscale
volumes. With this technique the electron probe is focused on a nanometer
sized area, and many reflections with large reciprocal vectors are
simultaneously at the Bragg position. We demonstrate the power of the
technique by studying the anharmonic thermal motion of atoms in the
promising thermoelectric material Mg2Si. As reported previously from
neutron and x-ray diffraction on different crystals with the fluorite structure,
we observe anharmonic motion of the Mg atoms in their tetrahedral
environment. We conclude that the Mg atoms at room temperature vibrate
around positions displaced 4.50 0.14 pm from the center of the tetrahedron
[1]. [1] K.Valset, J.Taft?. Wu and Y. Zhu, Physical Review B 84, 22031(R)
(2011) Supported by the Norwegian Research Council through the
NANOMAT program.
P 4
add to my program
16:00 Structure-property correlation of DyBa2Cu3O7- (DyBCO) coated
conductors with critical currents exceeding 1000 A/cm
Authors : Z. Aabdin, M. Drrschnabel, O. Eibl
P 5
Affiliations : Institute of Applied Physics, Auf der Morgenstelle 10, D-72076
Tbingen, Germany.
Resume : DyBCO thin films are deposited on metallic tapes yielding Coated
Conductors (CCs) which are second generation superconducting wires for
the magnet and energy technology. The most significant property of the CC
is the critical current density, high critical current densities can only be
obtained by biaxially-textured DyBCO and require effective pinning of
magnetic flux lines by the nanostructure. Therefore, TEM with its resolution
capabilities is required for analyzing the nanostructure for structure-property
correlation. Inclined Substrate Deposition (ISD) yields biaxially-textured
buffer layers on randomly oriented polycrystalline substrates suitable for
long length CCs. DyBCO films were grown on biaxially-textured MgO buffer
layers deposited on Hastelloy substrates. Typical critical current densities
were 2.1 MA cm-2 at 77 K in self-field, yielding a record total critical current
of about 1000 A/cm for 5 m thick films. Different to other technologies the
critical current density does not decrease with increasing film thickness
when ISD is used. Cross-section imaging and electron diffraction in the TEM
was used to quantify the biaxial-texture of the MgO films, the facet
orientation, and the DyBCO texture. The DyBCO grain size was about 250-
650 nm, only small-angle grain boundaries appeared over the complete
DyBCO film thickness (up to 5 m). A detailed analysis of the microstructure
will be summarized and a growth model for the DyBCO film will be
presented.
add to my program
16:00 Metal nanoparticles studied by SEM in transmission mode
Authors : Ulrich Herr, Balati Kuerbanjiang
Affiliations : Institute of Micro- and Nanomaterials, Ulm University, 89081 Ulm,
Germany
Resume : Metallic nanoparticles are of interest for various applications, e.g.
for the concentration of light (plasmonics) or in magnetic data storage
applications. Since many properties depend sensitively on the size of the
particles, a precise characterization of the particle size distribution is
mandatory. A standard technique frequently used is electron microscopy.
Scanning electron microscopy is often preferred due to the low effort for
sample preparation. However, artefacts such as apparently larger size of
particles may occur due to electron scattering effects. These artefacts can
be reduced by using thin support structures, like those used in TEM
investigations. Using a specially designed sample holder, it is possible to use
transmitted electrons to generate an image in a conventional SEM without
further modification. We compare the images and size distributions obtained
by the standard technique, and in transmission mode. We find a pronounced
reduction of the particles sizes measured in transmission mode, together
with an improved resolution as demonstrated by resolving individual
nanoparticles inside agglomerates.
P 6
add to my program
16:00 The effect of phase transformation on the thermal expansion property in
Al/ZrW2O8 composites
Authors : Yi Wu, HaoWei Wang, Zhe Chen, MingLiang Wang, Naiheng Ma
Affiliations : State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong
University, Shanghai 200240, Peoples Republic of China
Resume : This paper studied the effect of phase transformation on the
thermal expansion property in Al/ZrW2O8 composites. The Al/ZrW2O8
composites of low thermal expansion were fabricated by a squeeze casting
method. However, the coefficient of thermal expansion (CTE) of as-made
composites was discovered sharply increased at around 130 degree C. The X
-ray diffraction (XRD) showed the existence of high-pressure gamma-phase
in the as-made composites. This high-pressure gamma-phase was
considered to be induced by the compressive residual stress originated from
the thermal mismatch between Al matrix and ZrW2O8 particles. The high
temperature XRD and the differential scanning calorimetry technique were
used to study this thermally expanded abruption phenomenon. It was found
that the phase transformation from high-pressure gamma-phase to the low
pressure phases (alpha/beta phase) in the composites should be responsible
for fluctuation in the CTE of composites. Furthermore, using a proper heat
treatment to eliminate the high-pressure phase in the composite, the
Al/ZrW2O8 composites of low and uniform CTE Al/ZrW2O8 composite was
successfully achieved.
P 7
add to my program
16:00 Evolution of texture during hot extrusion of in-situ TiB2 particles reinforced
7075 aluminum composites investigated by neutron diffraction
Authors : Z. Chen (1), M. H. Mathon (2), M. L. Wang (1), D. Chen (1), S. Y. Zhong
(2), H. W. Wang (1)
Affiliations : (1) State Key Laboratory of Metal Matrix Composites, Shanghai Jiao
Tong University, Shanghai 200240, PR China; (2) Science of Matter Direction,
IRAMIS, CEA/Saclay, 91191 Gif-sur-Yvette, France
Resume : The bulk texture evolution of hot extrusion TiB2/Al composites
with different TiB2 particles volume fraction was investigated by neutron
diffraction. The dominant texture of the composites was the typical
extrusion {001} and {111} fiber texture with scatter around the ideal
orientations. Compared with the typical extrusion textures for pure 7075
aluminum alloy, the {111} fiber texture was found to be weaker in
composites, while the {001} fiber texture remained at the same level.
Furthermore, the {111} fiber texture decreased with the particle volume
fraction, and the {001} fiber texture did not change in the composites. The
evolution of texture with different TiB2 particles volume fraction was
discussed in term of aluminums deformation mechanisms combined with
particles effect.
P 8
add to my program
16:00 Study of dispersoids found in Cr-rich oxide dispersion strengthened steels
as a function of heat treatments
Authors : Zvi Foxman (1), Malki Pinkas (2), Alex Landau (2), Peter Hhner (3),
Vladimir Krsjak (3), Louisa Meshi (1)
Affiliations : (1) Department of Materials Engineering, Ben-Gurion University, Beer
Sheva, Israel; (2) Nuclear Research Center-Negev, P.O.Box 9001, Beer-Sheva,
Israel; (3) Joint Research Centre, Institute for Energy, P.O. Box 2, 1755ZG Petten,
The Netherlands
Resume : Oxide dispersion strengthened (ODS) steels, produced by
mechanical alloying, are known for their good mechanical strength, high
creep resistance at temperatures up to 1100C [1,2] and good radiation
resistance. Both the strength and radiation resistance are attributed to the
presence of nano-sized Y based oxides finely dispersed in the ferritic matrix.
These oxides may possess different compositions and structures and may be
metastable, depending on the manufacturing process. Some of the ODS
alloys contain high Cr levels (~18wt.%), which contribute to the oxidation
resistance of the alloy. Yet, the addition of Cr makes the steel susceptible to
the "475C embrittlement" of high Cr ferrous alloys, caused by the
separation of the ferritic phase into Cr-rich and Cr-poor regions. In the
current research, we have investigated the effect of the exposure to 475oC
on the composition and structure of the oxide phases using mainly
transmission electron microscopy (TEM). The study focused on four
commercial ODS steels (PM2000, MA956, ODM 751 and EUROFER) differing
in composition. The alloys were studied in their as received state and
following exposure to 475C for 100 to 1000 hours. The extraction replica
technique was applied in order to best characterize the dispersoids and
eliminate the influences of the magnetic ferritic matrix on the TEM study.
The as-recrystallized samples were characterized by a nano-scaled complex-
oxide particles dispersed in the ferritic matrix. After heat treatment a
change in the morphology, size, distribution and prevailing structure of the
dispersoids was observed. References: 1. A. Czyrska-Filemonowicz, B.
Dubiel, Journal of Materials Processing Technology 64, 1-3, (1997), 53-64.
2. H. Bhadeshia, Mat. Science and Eng. A-Structural Materials Properties
Microstructure and Processing, 223, (1997), 64-77.
P 9
add to my program
16:00 In-situ TEM observation of microstructure transition in Au wire caused by
electromigration
Authors : Yosuke MURAKAMI, Masashi ARITA, Kouichi HAMADA, Yasuo TAKAHASHI
Affiliations : Graduate School of Information Science and Technology, Hokkaido
University, Sapporo 060-0814, Japan
Resume : The phenomenon that metal atoms are moved by collision with
electrons contribution the current flow is called Electromigration. In recent
years, many works are performed to apply this phenomenon on
nanostructure fabrication. For more advanced application to control the size
less than 10 nm, analyzes on atom transfer mechanism is necessary in more
microscopic scale. For this reason, we performed in-situ transmission
electron microscopy (TEM) observation of electromigration. Samples are
polycrystalline narrow Au thin films on Si-N membrane which was fabricated
P 10
by photolithography and lift-off techniques. Narrowing process and
destruction of the wire by electromigration were clearly observed in real
time during the current flow. During the current flow, grain growth and void
formation were simultaneously occurred, and the balance of these two
phenomena closely related to the change in resistance. In addition, the
narrowing rate was changed due to change of nanostructure of the Au wire
region. When the wire width became nearly identical to the grain size, the
narrowing rate became slow. This may indicates that atom transfer
mechanism was influenced by nanostructure such as grain boundaries.
add to my program
16:00 Light Scattering from Microscopic Structure and Its Role on Enhanced Haze
Factor
Authors : Hyeongsik Park(1), Sk Md Iftiquar(1), Jeong Chul Lee(2), JunHee Jung
(3) , Youngkuk Kim(1), Juyeon Jang(1), Youn-Jung Lee(1), Junsin Yi(1,3)
Affiliations : (1) School of Information and Communication Engineering,
Sungkyunkwan University 300 Chunchun-dong, Jangan-gu, Suwon, 440-746,
Republic of Korea; (2) Korea Institute of Energy Research 152 Gajeong-ro, Yuseong-
gu, Daejeon 305-343, Republic of Korea; (3) Department of Energy Science,
Sungkyunkwan University, 300 Chunchun-dong, Jangan-gu, Suwon, 440-746,
Republic of Korea
Resume : Efficiency of amorphous silicon (a-Si) solar cell partly depends
upon its light trapping ability, in which a prolonged passage of unabsorbed
light make it more likely to be absorbed. A conventional technique is
texturization of end layers, where sometime acid etching is used, that
chemically and structurally change the surface in such a way that total light
transmission into the solar cell may also fall significantly. Generally the
texture is of micrometer size, however, it is possible to achieve light
scattering from sub-micron structures of as deposited films and obtain a
haze comparable to that obtained in textured surface. The micro-crystalline
Si (uc-Si) layers as well as the aluminum doped zinc oxide (AZO) surfaces
are most likely to have sub-micron sized structures, which is comparable or
smaller than wavelength of visible light. We found that the haze factor
obtained from as deposited AZO films follow conventional scattering
principle to a great extent and show a significant light re-distribution. This
will be useful in enhancement of solar cell efficiency. The uc-Si and AZO
films investigated for this, were deposited by VHF PECVD technique and DC
magnetron sputtering. For AZO as a back reflector of a solar cell, this
principle may be more useful as any chemical or mechanical texturing of the
AZO back reflector, after the solar cell fabrication has been completed, has a
risk of damaging the device.
P 11
add to my program
16:00 Studies on the dielectric properties of YSZ doped 10% Ni thin films
deposited by PLD and RF PLD at different substrate temperature
Authors : R. Pascu, G. Epurescu, V. Ion, F. Stokker, A. Andrei, M. Dinescu
Affiliations : National Institute for Laser Plasma and Radiation, Photonic Processing
of Advanced Materials Group, 077125 Magurele, Romania
Resume : YSZ doped 10% Ni thin films were deposited by Pulsed Laser
Deposition and Radiofrequency Assisted Pulsed Laser Deposition on different
substrate temperatures (Ts = RT, 3500C, 4500C, 5500C, 6000C) starting
from a ceramic target. A complete morphological, structural, optical and
electrical characterization was performed by Atomic Force Microscopy, X-Ray
Diffraction, Spectro-Ellipsometry and Dielectric Spectroscopy respectively.
The influence of the oxygen excited and ionized beam generated by the
radiofrequency discharge and of the substrate temperature on the dielectric
properties was studied, with the aim of using the layers for anode material
in SOFC. Key words: 10% Ni- YSZ, thin film, different substrate, AFM,
VASE
P 12
add to my program
16:00 Preparation and microstructural properties of erbium doped alumina-yttria
oxide thin films deposited by aerosol MOCVD
Authors : Salhi Rached (1,2), Jean-Luc Deschanvres (2), Carmen Jimenez (2),
Laetitia Rapenne (2), Ramzi Malej (3), Mohieddine Fourati (4)
Affiliations : (1) Laboratoire de Science et Ingnierie des Matriaux et Procds, F-
38402 Saint Martin DHres, France; (2) Laboratoire des Matriaux et du Gnie
Physique, CNRS UMR 5628, INP Grenoble-Minatec, F-38016 Grenoble, France; (3)
Laboratoire de Chimie Industrielle, Ecole Nationale d'Ingnieur de Sfax, University of
Sfax BP W 3038 Sfax, Tunisia; (4) Laboratoire de Physique Applique, Groupe de
P 13
Physique Thorique, Dpartement de Physique, Facult des Sciences de Sfax,
University of Sfax 3018 Sfax, Tunisia.
Resume : The ultimate goal of the present research activities was to
develop technological deposition processes leading to low-cost, highly
effective rare earth doped thin optical coating for application in solar
spectrum conversion. As rare earth doped matrix the purpose of the present
work is to study alumina-yttria (Al2O3-Y2O3) oxide films and to analyse the
correlation between deposition conditions, compositions, treatment after
deposition and the physical, microstructure and the optical properties of the
erbium-doped films. The Erbium-doped Al2O3-Y2O3 oxide films were
prepared by aerosol-UV assisted metal-organic chemical vapour deposition
(MOCVD). The deposition conditions were optimized to obtain films with
good quality on different compositions. The effect of humidity of carrier gas
and UV-assistance on their composition structure and optical properties
were investigated on the as-deposited and thermal annealed films using
infrared spectroscopy, X-ray diffraction and transmission electron
microscopy. After annealing tow composition 10 and 88 mol% Al203 in the
film, were studied. The 10 mol% Al2O3 film crystallises in the two different
structural cubic and monoclinic phases of Y2O3 whereas the 88 mol% Al2O3
film appears as a mixture of YAG grains and amorphous phase. This result is
confirmed by the Er3+ luminescence properties in the visible and IR region
transitions.
add to my program
16:00 Quantitative Surface Force Microscopy
Authors : David Haviland (1), Daniel Platz (1), Daniel Forchheimer (1), Erik A.
Tholen (2)
Affiliations : (1) Nanostructure Physics, Royal Institute of Technology (KTH),
Roslagstullsbacken 21, Stockholm, Sweden SE-10691; (2) Intermodulation Products
AB, Vasavgen 29, Solna, Sweden, SE-16958
Resume : Quantitative Atomic Force Microscopy (AFM) relies on the
accurate measurement of tip-surface force. This force can be determined by
monitoring the cantilever dynamics in a frequency band around one
resonance of the cantilever, where sensitivity is highest and where good
calibration methods exist. In order to increase the information content
available in this limited frequency band, we measure intermodulation, or the
frequency mixing of two pure tones that are driving the cantilever. Using a
specially designed intermodulation lockin, we simultaneously acquire the
amplitude and phase of the response at 32 intermodulation product
frequencies, which gives a highly compressed representation of the
cantilevers motion in the phase plane. From analysis of this motion, we can
determine both conservative and dissipative tip-surface forces at every pixel
of an AFM scan. Fitting these forces to various tip-surface interaction
models, we can generate very high-resolution surface parameter maps.
Intermodulation AFM works with standard, inexpensive cantilevers, it can
easily be implemented on nearly any AFM, and the basic measurement
technique can be adapted to enhance many AFM modalities. A commercial
spin-off was recently established which sells the intermodulation lockin and
a software package for calibration, data acquisition, image display and data
analysis.
P 14
add to my program
16:00 Chemical Maps Obtained by Laser-Based Spectroscopy Technique on Boiler
Tubes
Authors : M.P. Mateo, V. Pion, G. Nicolas
Affiliations : Universidad de A Corua, Laboratorio de Aplicaciones Industriales del
Lser, Campus de Ferrol, Spain
Resume : In this work, boiler tubes used in a thermal power plant have
been analyzed by laser-induced breakdown spectroscopy (LIBS) in order to
demonstrate its capability to characterize specimens which are complex in
terms of shape and composition. This laser-based spectroscopy method
offers several advantages in comparison to traditional surface techniques,
being able to provide fast spatially-resolved multielemental analysis of solid
samples. In the case of boiler watertubes, the presence of deposits
produced on the inside surfaces due to the heated water circulation has
been determined by LIBS. From the acquired spectroscopic data, 3D
chemical maps and in-depth profiles of representative elements have been
plotted showing the distribution of these elements on the surface and at
different depth levels of the sample.
P 15
add to my program
16:00 Electronic properties for the ground state of alkaline-earth hydride cations
Authors : Hla Habli, Riadh Dardouri, Brahim Oujia, Florent Xavier Gada
Affiliations : (1) Laboratoire de Physique Quantique, Facultes Sciences de Monastir,
Monastir, Tunisia; (2) Laboratoire de Chimie et Physique Quantique, UMR5626 du
CNRS, Universite Toulouse, UPS, F-31062 Toulouse, France.
Resume : By an ab-initio approach involving a non empirical pseudo
potential for the Mg, Ca, and Ba cores, imperatorial core valence correlation
and full valence configuration interaction, the potential energy curves for the
ground state of the CaH , MgH and BaH molecular ions are determined.
Moreover, the spectroscopic constants and the vibrational levels of this state
for the three ions are presented in the same table in order to facilitate their
comparison. Besides, the permanent and transition dipole moments are
extensively studied and presented as function of the interatomic distances.
The electronic properties of these cations are investigated, using large
Gaussian basis sets, to discuss general trends of their behavior. A very good
agreement with experimental and theoretical data is obtained.
P 16
add to my program
16:00 Study of Vinylidene Polyfluoride Copolymers by Scanning Electron
Microscopy
Authors : A. Serdani (1), A. Sakri (2), A. Djebaili (2), J.P. Chopart (3)
Affiliations : (1) Laboratory of Polymers - LEP, University of Skikda, Algeria; (2)
Laboratory of chemistry and environmental chemistry L.C.C.E - University of Batna,
Algeria; (3) Laboratory of Mechanical Stress-Transfer Dynamics at Interfaces
LACMDTI URCA, BP 1039, 51687 University of Reims, France
Resume : This work made it possible to see the emulsifying effect of
copolymer synthesised using SEM to examine the surface quality of the
prepared alloys fractures. The examination of the stereotypes obtained on
various alloys allowed the visualisation of the two involved phases. We
observed on the initial mixture a continuous phase made up of PVDF in
which polystyren PS nodules were inserted more or less extended forming a
heterogeneous system. In addition, we noticed on other films that as the
emulsifying rate in the mixture increases, the density of PS nodules as their
size decreases significantly. Thus, the role of the emulsifier in these
mixtures appears in the phase size reduction and subsequently by an
increase in the state of dispersion. When we go on to a higher concentration
of emulsifier agent from 3 % to 9 %, the size of the phases decrease from
19 m to 10 m, knowing that the initial value in the basic mixture was 24
m. All these measurements confirm the emulsifying effect of our
copolymer. Key Words : Morphology Copolymer PVDF S.E.M - PS -
Synthesis
P 17
add to my program
16:00 Resolving the surface structure of iron-silicide alloy nanocrystals
Authors : A. Kovcs, R. Imlau, H. Wiggers, E. Mehmedovic, and M. Luysberg
Affiliations : Ernst Ruska-Centre and Peter Grnberg Institute, Research Centre
Jlich, D-52425, Germany University of Duisburg-Essen, Institute for Combustion
and Gasdynamics and CeNIDE, D-47057, Duisburg, Germany
Resume : Accurate understanding of the surface structure of nanocrystals is
fundamentally important in predicting their properties. However, the
characterization of the surface is challenging if more than one element is
present in the structure. In this work we use aberration-corrected
transmission electron microscopy (TEM) techniques to characterize the
surface of beta-iron-disilicide nanocrystals that were produced by gas phase
reaction of silane and iron pentacarbonyl. An amorphous shell was observed
around the nanocrystals that was sensitive to the electron beam irradiation.
The beta phase (space group 64, symbol Cmce) formation was confirmed
using electron diffraction patterns. In order to directly interpret the surface
location of individual Fe and Si atomic columns under the amorphous shell,
we have used a defocus series of high-resolution TEM images and exit wave
reconstruction technique. The surface structure was verified by comparing
the experimental images to multislice simulation of the structure. Results
revealed no distinct facets of the nanocrystals and a surface that contained
both Fe and Si atoms.
P 18
add to my program
16:00 Y/Ti ratio effect on the evolution of oxides precipitation in ODS Fe-14%Cr
alloys
Authors : S.Y. Zhong, J. Ribis, V. Klosek, Y. de Carlan, N. Lochet, M.H. Mathon
P 19
Affiliations : LLB CEA Saclay; SRMA CEA Saclay; LLB CEA Saclay; SRMA CEA
Saclay; SRMA CEA Saclay; LLB CEA Saclay
Resume : Compared to conventional alloys, oxide-dispersion-strengthened
(ODS) ferritic alloys are promising candidate materials for next generation
nuclear energy systems. They present excellent mechanical resistance at
high temperature governed in part by the distribution of nano-oxides in the
matrix. These materials are obtained by powder metallurgy. One fabrication
route is to produce alloyed powders by mechanical alloying and to
consolidate the material by hot extrusion or HIP (Hot Isostatic Pressing).
Oxide precipitation (particles with different chemical compositions such as
Y2O3, Y2Ti2O7 may precipitate depending on the alloying elements)
occurs during the hot consolidation step or during subsequent annealing at
high temperature. However, the tensile or creep behavior of ODS steels
varies with the oxide distribution. It is therefore of the utmost importance to
control the oxide size distribution evolution during the different stages of the
fabrication and during thermal treatments. With a view to understanding the
mechanisms of formation and evolution of these particles, the oxides
precipitation kinetics were studied as a function of nominal content of Y, Ti
and O of the alloys using small-angle neutron scattering technique (SANS).
TEM investigations were performed to characterize the structure of the
precipitations, and their coherent relations affected to the yield stress. An
analysis of hardness was carried out to correlate nano-precipitation and
mechanical properties.
add to my program

Back

strasbourg.com
14 May 2012 15 May 2012 16 May 2012
hide a
Symposium : X

Quantitative microstructure imaging and chemical analysis : Thomas Hche
09:00 Advances in Spectroscopic Nano-scale Characterization in Electron-Optical
Instruments
Authors : Nestor J. Zaluzec
Affiliations : Argonne National Laboratory, Materials Science Division, Electron
Microscopy Center, Argonne, Illinois 60439, U.S.A.
Resume : Spectroscopy in electron-optical instrumentation is undergoing a
transformation in capabilities. Part of this is due to advances in the detector
systems, the remainder is due to the evolution of our electron-optical tools
and how they are interfaced to ancilliary devices. Modern electron-optical
instruments are now allowing us unprecedented capabilities for probing the
nature of how nanomaterials are characterized today. In this overview we
will discuss the latest advances in high collection angle x-ray energy
dispsersive spectroscopy (XEDS) where solid angles in excess of pi
steradians have been achieved and a direct comparison with conventional
detectors and geometries will be discussed for both the TEM/STEM and SEM.
In addition, we will compare and contrast this with electron energy loss
spectroscopy (EELS) highlighting the merits and limitations of both
technologies with respect to nanomaterials characterization in the
TEM/STEM. Finally, we will consider the propects of studying electronic
excitations in plasmonic, excitonic and hybrid systems.
7 1
add to my program
09:30 Quantitative analysis of Electron Diffraction Ring Patterns using the MAUD
program
Authors : P. Boullay (1), L. Lutterotti (2), D. Chateigner (1)
Affiliations : (1) CRISMAT, CNRS UMR 6508, 6 Bd du Marchal JUIN 14050 CAEN
Cedex, France; (2) Department of Materials Engineering and Industrial Technologies,
University of Trento, 38123 TRENTO, Italy
Resume : The growing interest on nanosized polycrystalline samples raises
problems such as phase identification, structure and microstructure
characterization with quantitative and reliable approaches. Among the
different techniques available in transmission electron microscopy, the
authors would like to focus on new features in the MAUD program dedicated
to the quantitative analysis of electron diffraction ring patterns (ED-RP). The
data collection is performed using a parallel beam illumination from an area
ranging from about 200m2 down to 1m2 provided the number of
diffracting particules is sufficient to give a ED-RP. The intensity extraction
along the rings is performed with ImageJ. The structural and microstructural
informations are extracted using the Rietveld method. Phase identification
and volume fraction analysis can be performed automatically using the
Crystallographic Open Database. All these steps are implemented and
accessible via the MAUD interface. The results obtained by electron
diffraction on few oxides will be presented and systematically compared to
similar X-ray diffraction experiments. Interestingly it is shown that the use
of the electron scattering factors in the kinematical approximation or the
pattern matching mode is sufficient to obtain quantitative information such
as cell parameters, average size and shape of an assembly of nano-
particules. Texture effects and a certain amount of graininess in the ring
patterns can also be accounted for.
7 2
add to my program
09:45 Strain Driven Oxygen Deficiency in Nanostructured Superconductors: High
Resolution Z-contrast Imaging and O K-edge ELNES analysis
Authors : Leopoldo Molina (1), Stuart Turner (1), Gerardo T Martinez (1), Manuela
Erbe (2), Thomas Freudenberg (2), Bernhard Holzapfel (2), Sandra Van Aert (1), Jo
Verbeeck (1), Oliver Eibl (3), Gustaaf Van Tendeloo (1)
Affiliations : (1) EMAT, University of Antwerp, Groenenborgerlaan 171, 2020
Antwerp, Belgium; (2) Leibniz Institute for Solid State and Materials Research
Dresden, D-01069 Dresden, Germany; (3) Eberhard Karls Universitt Tbingen, D-
72070, Tbingen, Germany
Resume : Precipitates in YBCO thin films yield a significant improvement of
the magnetic flux pinning properties and a reduced anisotropy of the critical
current density in coated conductors. Therefore, controlling precipitates in
size and density, but also understanding their associated strain fields is of
crucial importance for applications. YBa2Cu3O7-x (YBCO) superconducting
films containing nanosized BaHfO3 precipitates were prepared by Metal
Organic Deposition (MOD). Strain-fields of crystal defects associated with
these precipitates were measured quantitatively by High-Angle Annular Dark
-Field (HAADF) aberration-corrected Scanning Transmission Electron
Microscopy (STEM). Experimental images were evaluated with respect to the
strain tensor components by a geometrical phase analysis and a model-
based parameter estimation method. EELS spectra provide fingerprints of
the oxygen sublattices of YBCO. Changes in the O K-edge electron energy
loss near-edge fine structure (ELNES), in particular of the first peak (which
originates from the interaction of the O 2p and the partially occupied Cu d
orbital), allowed to distinguish superconducting from non-superconducting
areas with a sub-nm spatial resolution. STEM-EELS maps of regions
containing precipitates were carried out using an aberration corrected
(Scanning) Transmission Electron Microscope TITAN cubed operating at
120 kV and with an energy resolution of <250 meV. The possibilities of the
applied techniques for a structure-property correlation will be discussed.
7 3
add to my program
10:00 Coffee break
10:30 Use of atomically resolved annular dark-field scanning transmission electron
microscopy of (Al, In)GaN for measuring segregation with sub-monolayer
precision
Authors : H. Amari, I.M. Ross, T. Wang, T. Walther
Affiliations : Kroto Centre for High-Resolution Imaging and Analysis, Dept.
Electronic and Electrical Engineering, University of Sheffield, Mappin Building, Mappin
Street, Sheffield S1 3JD, UK
Resume : We have performed lattice resolved annular dark-field (ADF)
scanning transmission electron microscopy (STEM) and combined this with
energy-dispersive X-ray spectroscopy (EDXS) as well as image simulations
to measure quantitatively segregation across interfaces in AlGaN/GaN and
GaN/InGaN multiple quantum wells of nominal thicknesses between 8nm
and 0.5nm. The compositional profiles obtained were corrected for detector
dark current and non-linearity of the Z-contrast imaging process before we
fitted exponential functions to the interface regions to determine the
segregation lengths. Experimental values for the wider quantum wells are of
the order of only ~1nm and, when converted to (0002) monolayers in the
hexagonal structure, have error bars of the order of about half a monolayer,
which is precise enough to allow us a comparison with simulations based on
a simple 2-state exchange model for surface segregation of aluminium or
indium atoms, respectively.
7 4
add to my program
10:45 Indium concentration in (In, Ga)N/ GaN nanowires determined by low-loss
electron energy-loss spectroscopy
Authors : X. Kong (1), S. Albert (2), A. Bengoechea (2), M. A. Sanchez-Garcia (2),
E. Calleja (2), A. Trampert (1)
Affiliations : (1) Paul-Drude-Institut fur Festkorperelektronik, D-10117 Berlin,
Germany; (2) Dpto. Ingenieria Electronica, ETSI Telecomunicacion, Universidad
Politecnica, Ciudad Universitaria, 28040 Madrid, Spain
Resume : (In, Ga)N ternary alloy has been intensely studied in recent years
because the bandgap tunability of this material covers the whole visible
spectral range, offering a huge potential for most light-emitting diodes and
7 5
laser diodes devices. Moreover, (In,Ga)N nanowires provide a natural
growth mechanism for relaxing the epitaxial lattice strain at the interface
and drastically increasing the critical thickness on the lattice-mismatched
substrate. The concentration and spatial distribution of Indium atoms in (In,
Ga)N nanowires (NWs) have a crucial influence on the optical emission
energy and intensity of NWs. Based on the lattice distortion and local strain,
high-resolution transmission electron microscopy (HRTEM) has been widely
used to measure local In content in (In, Ga)N/GaN quantum wells. However,
the method becomes rather complex in this small three-dimensional objects,
in particular when the elastic and plastic relaxations occur for high In
concentrations. In our presentation, we will demonstrate that low-loss
electron energy-loss spectroscopy (EELS) is an alternative method for
Indium composition analysis. In low-loss EELS, the semiconductor volume
plasmon excitation is characteristic of unbound valence electrons performing
collective oscillations, which is strongly related with interband transitions
beyond the bandgap and thus offers valuable fingerprint information of the
chemical composition in the semiconductor. Therefore the plasmon peak
energy (Ep) is utilized to quantitatively determinate In concentration in (In,
Ga)N nanowires. A linear dependency of plasmon peak on In concentration
for (In, Ga)N is determined over the wide composition range measuring
complementary the In content by N-K edge and In-M4,5 edges in core-loss
EELS region. It is remarkable that, in spite of the presence of bandgap
bowing, a linear relationship is measured. We will apply the low-loss EELS
method to study two sets of (In, Ga)/GaN NWs heterostructure realized by
plasma-assisted molecular beam epitaxy (MBE) on Si(111) substrates. In
the first case, the (In, Ga)N section is composed of high density of stacking
faults resulting a pronounced lateral growth; and in the second case, strain
relaxation of (In,Ga)N section occurs plastically with a similar In content as
the first case. The results with high spatial resolution will contribute to a
basic understanding of morphology changes during (In, Ga)N/GaN NWs
growth.
add to my program
Thermoelectrics : Hugo Bender
11:00 HAADF-STEM of layered structures in materials for photonics,
thermoelectrics and photovoltaics
Authors : M. eh (1), S. turm (1), K. agar (1), H. Saijo (2), J.T. Hsu (3), M.J.
Chen (4), J.R. Yang (4), M. Shiojiri (5)
Affiliations : (1) Department for Nanostructured Materials, Joef Stefan Institute,
Ljubljana, Slovenia; (2) School of Biology-Oriented Science and Technology, Kinki
University, 649-6493 Japan, (3) Industrial Technology Research Institute, Hsinchu,
Taiwan 310, ROC; (4) Institute of Materials Science and Engineering, National
Taiwan University, Taipei, Taiwan 106, ROC; (5) Professor Emeritus of Kyoto
Institute of Technology, 1-297 Wakiyama, Kyoto 618-0091, Japan
Resume : High-angle annular dark-field scanning-transmission electron
microscopy (HAADF-STEM) has become an important electron microscopy
technique for imaging materials down to an atom scale. Thermal diffuse
scattering (TDS) represents main contribution to the HAADF-STEM image
intensity. Since TDS strongly depends on the atomic number (Z) of
investigated material, the HAADF-STEM images consequently contain
information on the chemical composition. This is why qualitative
interpretation of the HAADF-STEM images is relatively straightforward.
However, for the quantitative interpretation of the HAAD-STEM images, i.e.
determination of the chemical composition of a single atom column based on
the measured intensity requires image simulations and image matching. In
present work we report on the use of HAADF-STEM for characterization of
various layered structures, primarily in materials for photonics,
thermoelectrics and photovoltaics. All HAADF-STEM images were recorded in
a JEM-2010F TEM/STEM microscope (Cs=0.48 mm) with a 10-mrad semi-
angle of the probe and an ADF detector range from 100 to 200 mrad. The
results of the use of HAADF-STEM imaging for chemical and structural
characterization of layered structures from nanoscale to atom scale for the
following materials will be presented: Al-doped ZnO films and AlGaN/GaN
superlattice (photonics), Ruddlesden-Popper planar faults in ceramics with
the perovskite structure (thermoelectrics) and anodized TiO2 nanotubes
(photovoltaics).
8 1
add to my program
11:30 Correlation Between Microstructure and Thermoelectric Properties in Ag(1-
x)Pb18Sb(1+y)Te20
Authors : S. Perlt (1), Th. Hche (2), J. Dadda (3), E. Mller (3)
Affiliations : (1) Leibniz Institute of Surface Modification, Permoserstr. 15, D-04318
Leipzig, Germany; (2) Fraunhofer Institute for Mechanics of Materials IWM, Walter-
Hlse-Str. 1, D-06120 Halle, Germany; (3) German Aerospace Center, Institute of
Materials Research, D-51170 Kln, Germany
Resume : One feasible way to enhance the ZT value (figure of merit) of a
thermoelectric (TE) material is to decrease the thermal conductivity kappa
by introducing nanoprecipitates acting as phonon scatterers. Therefore,
precipitation of nanosized secondary phases in Ag(1-x)Pb18Sb(1+y)Te20
(Lead-Antimony-Silver-Tellurium, LAST) is highly promising for TE
applications in the intermediate temperature range. The high thermoelectric
performance of LAST is, amongst others, assumed to be caused by
nanoscale precipitates formed by nucleation and growth and/or spinodal
decomposition. Recent findings suggest structural disorder on the atomic
scale as an additional influence factor. Based on properties monitored by a
Seebeck scanning microprobe, structure-property relationships are studied
by SEM and TEM analysis. Site-specific liftout of TEM lamellae from
thermoelectrically characterised samples is made by focused ion beam (FIB)
machining. In addition, high-resolution TEM is used to reveal orientation
relationship and the atomistics of structural defects. Based on a gradient
annealing experiment, a favourable temperature range (T_ann=500-550 C)
regarding TE performance was defined already. Thus, further investigations
will deal with a new set of temperature-gradient samples referring to a finer
gradient within the favoured region. Furthermore, studies are complemented
with an optimization of the Ag/Sb ratio to explore the impact of the electrical
conductivity sigma on the overall performance.
8 2
add to my program
11:45 Structural properties of iron disilicide nanocrystals from gas phase
investigated by advanced electron microscopy
Authors : R. Imlau(1), A. Kovcs(1), A. Stewart(2), E. Mehmedovic(3), H. Wiggers
(3), U. Kolb(2), M. Luysberg(1)
Affiliations : (1) Ernst Ruska-Centre and Peter Grnberg Institut, Research Centre
Jlich, 52425 Jlich, Germany; (2) Institut fr Physikalische Chemie, Johannes
Gutenberg-Universitt, D-55099 Mainz, Germany; (3) Institute for Combustion and
Gasdynamics and CeNIDE, University of Duisburg-Essen, D-47057 Duisburg,
Germany
Resume : Beta-phase-iron-disilicide (beta-FeSi2) is a promising material
because of its thermoelectric and semiconducting properties. In addition iron
and silicon are abundant in earths crust. However, fabrication of beta-FeSi2
nanostructures is challenging due to its complex crystallographic structure.
In this work we report on structural and chemical properties of beta-FeSi2
nanocrystals synthesized from gas phase by thermal decomposition of silane
(SiH4) and iron pentacarbonyl (Fe(CO)5) in a hot wall reactor. Conventional,
analytical and aberration-corrected transmission electron microscopy are
employed to investigate structure and chemical composition of the beta-
FeSi2 nanocrystals. The grain size of the particles, which are aggregated, is
10 to 30 nm. All of the particles are surrounded by an amorphous shell,
which is rich in Si and O. Both X-ray diffraction and electron diffraction
reveal the crystalline nature of the nanocrystals; where all diffraction peaks
comply with the beta phase of FeSi2. Interestingly, the peak intensities
differ from that of the bulk. Nano-beam diffraction and automated diffraction
tomography of individual nanocrystals were used to reveal a structural
disorder in the beta-FeSi2 nanoparticles.
8 3
add to my program
12:00 Advanced structural and chemical characterization of thermoelectric Bi2Te3
based nanomaterials
Authors : N. Peranio(1);Z. Aabdin(1); O. Eibl(1); M. Luysberg(2)
Affiliations : (1) Institut fr Angewandte Physik, Eberhard Karls Universitt
Tbingen, Auf der Morgenstelle 10, 72076 Tbingen, Germany; 2() Ernst Ruska
Center for Microscopy and Spectroscopy with Electrons, Forschungszentrum Jlich
GmbH, 52425 Jlich
Resume : Bi2Te3 is the compound with the highest thermoelectric figure of
merit ZT at room temperature and its alloys are intensively used in
technological applications. Nanostructured bulk, thin films, and nanowires
were prepared in a research cluster and analyzed by advanced TEM methods
for structure-property correlation. High-precision, quantitative EDX analysis
8 4
in the TEM turned out to be essential for controlling the growth of nanowires
with defined chemical composition and was also applied to determine the
chemical homogeneity of thin films and nanostructured bulk. Energy-filtered
TEM was combined with quantitative EDX analysis to identify blocking layers
at grain boundaries that limited the electrical conductivity and thus ZT. A
natural nanostructure with a wavelength of 10 nm was found and gliding
dislocations were observed in-situ with a high mobility at room temperature,
both reducing thermal conductivity. Angle-resolved electron energy-loss
spectroscopy (EELS) was carried out and yielded an anisotropic plasmon
dispersion in the basal plane of Bi2Te3 compounds. The dispersion followed
the anisotropy of the effective masses and allows access to the band
structure. Aberration corrected STEM allows simultaneous acquisition of
images and EEL spectra with atomic resolution. In Z contrast images of
alloyed materials Bi atomic columns appear as bright dots. Such images
were supplemented by image simulation allowing to study alloying on the
atomic scale.
add to my program
12:15 Lunch
Energy Storage Systems : Acha Hessler-Wyser
14:00 Nanostructured Reactive Hydride Composites for Hydrogen Storage
Authors : Thomas Klassen, Ulrike Bsenberg, Gagik Barkhordarian, Claudio Pistidda,
Christian Bonatto-Minella, Martin Dornheim
Affiliations : Helmholtz-Zentrum Geesthacht, Centre for Materials and Coastal
Research, Geesthacht, Germany; Helmut Schmidt University Hamburg, Germany
Resume : In view of increasing pollution and exploitation of fossile fuel
reserves, renewable energy concepts are essential for the future of our
society. Hydrogen is the ideal clean energy carrier, e.g. for the zero-
emission vehicle. The storage of hydrogen for mobile applications is still one
of the major problems for implementation. Hydrides offer the highest
storage capacity by volume, and are one of the most promising alternatives
for reversible storage of hydrogen. Reactive Hydride Composites (RHC) will
be presented that release or store hydrogen by redox reactions between at
least two hydrides. Upon desorption, components from both hydrides react
exothermally, thus reducing the overall reaction enthalpy. Up to 11 wt.%
hydrogen may be stored reversibly at technically relevant temperatures. In
spite of a significantly lowered reaction enthalpy and thus high
thermodynamic driving force for desorption, hydrogen release from
LiBH4/MgH2-RHC still requires temperatures above 250C. Reaction
mechanisms have been investigated by TEM as well as synchrotron and
neutron scattering methods. An overview will be given on reaction
mechanisms, thermodynamic properties and sorption behaviour of
nanocrystalline RHCs: 2LiBH4+MgH2, 2NaBH4+MgH2 and Ca(BH4)2+MgH2.
References [1] G. Barkhordarian et al., J. Alloys and Compounds 440 (2007)
L18-L21. [2] U. Bsenberg et al.; Acta Materialia 58, (2010) p. 3381-3389.
[3] M. Dornheim, T. Klassen, Encyclopedia of Electrochem. Power Sources
(2009) 459-472
9 1
add to my program
14:30 In-situ TEM on (de)hydrogenation of Pd at 0.5-4.5 bar hydrogen pressure
and 20-400C
Authors : Tadahiro Yokosawa (1), Tuncay Alan (2), Gregory Pandraud (2), Bernard
Dam (3), Henny Zandbergen (1)
Affiliations : (1) Kavli Institute of NanoScience, HREM, Delft University of
Technology, Delft, The Netherlands; (2) DIMES-ECTM, Delft University of
Technology, Delft, The Netherlands; (3) MECS, Chemical Engineering, Delft
University of Technology, Delft, The Netherlands
Resume : In order to understand loading and unloading mechanism of
hydrogen storage materials, it is important to study this process at the
atomic level. In-situ transmission electron microscopy (TEM) at application
pressures (1-10 bar) of hydrogen gas is expected to provide the most direct
information. We have developed a nanoreactor, sample holder and gas
system for in-situ TEM of hydrogen storage materials up to at least 4.5 bar.
The MEMS-based nanoreactor has a microheater, two electron-transparent
windows and a gas inlet and outlet. The holder contains various O-rings to
9 2
have leak-tight connections with the nanoreactor. The system was tested
with the (de)hydrogenation of Pd at pressures up to 4.5 bar. The Pd film
consisted of islands being 15 nm thick and 50 to 500 nm wide. In electron
diffraction mode we observed reproducibly a crystal lattice expansion and
shrinkage owing to hydrogenation and dehydrogenation, respectively. In
selected-area electron diffraction and bright/dark-field modes the (de)
hydrogenation of individual Pd particles was followed. Some Pd islands are
consistently hydrogenated faster than others. Experiments at 0.8 bar and
3.2 bar showed that the (de)hydrogenation temperature is not affected by
the electron beam. This result shows that this is a fast method to investigate
hydrogen storage materials with information at the nanometer scale.
add to my program
14:45 Integrated Platform for Nanometrology of Electrochemical Energy Storage
Devices
Authors : V.P. Oleshko (1), D. Ruzmetov (2,3), P. Haney (2), H. Lezec (2), K. Karki
(4), K.H. Baloch (4), A. Agrawal (2,3), A.V. Davydov (1), S. Krylyuk (1), K.-W. Moon
(1), J. Bonevich (1), Y. Liu (5), J. Y. Huang (5), M. Tanase (2,3), J. Cumings (4),
A.A. Talin (2)
Affiliations : (1) Material Measurement Laboratory and (2) Center for Nanoscale
Science and Technology, National Institute of Standards and Technology,
Gaithersburg, MD 20899, U.S.A.; (3) Institute for Research in Electronics and Applied
Physics and (4) Dept. of Materials Science and Engineering, University of Maryland,
College Park, MD 20742, U.S.A.; (5) Center for Integrated Nanotechnologies Sandia
National Laboratories, Albuquerque, NM 87123, U.S.A.
Resume : Complex interfacial phenomena and phase transformations that
govern the operation of rechargeable Li-ion batteries (LIBs) need reliable
nanoscale 3D structural measurements which can be directly related to the
capacity and electrical transport characteristics. To realize the potential of
electron microscopy for solving this problem, we develop a flexible MEMS-
based inter-instrumentation platform for nanometrology of LiBs using E-
chips compatible with FIB, FESEM and S/TEM. Miniature all solid-state LiBs
comprising: a) a LiCoO2 cathode, a LiPON electrolyte and Si anode
contacted by electron-beam-deposited metallized Si nanowires; b)
LiCoO2/LiPON/Si thin film stacks were designed for in situ S/TEM or FESEM
electrical testing in a sub-pA range. Such diagnostic devices allow the
correlation of electrochemical properties tailored for specific performance
with their structure being analyzed in various imaging, diffraction and
spectroscopic modes up to the atomic level. We employ S/TEM coupled with
EELS/EDX spectral imaging to clarify effects of scaling on the LiBs
performance.
9 3
add to my program
15:00 Characterization of Bifunctional Electrodes of Li-O2 batteries using Electron
Microscopy
Authors : Santhana K. Eswara Moorthy, Johannes Biskupek, Ute Kaiser
Affiliations : Materialwissenschaftliche Elektronenmikroskopie, University of Ulm, D-
89069 Ulm, Germany
Resume : One of the most severe limitations in the commercialization of
the Li-O2 batteries is that the oxygen reduction reaction (ORR) during
discharging and oxygen evolution reaction (OER) during charging must have
fast kinetics. In order to enhance the reaction kinetics of the ORR and OER,
innovations in developing suitable electrocatalysts are necessary. In the
current work, we employ aberrations-corrected high-resolution TEM and
electron energy-loss spectroscopy to characterize the reaction products and
the electrocatalysts and gain a deeper understanding of the underlying
reaction mechanisms in order to improve reaction efficiencies. The
experimental challenges in this study are two-fold: Firstly, the typical end
products of the ORR, i.e., lithium oxides (Li2O2 and/or Li2O) tend to react
with CO2 of air and a fraction of the oxides could transform to carbonates
(Li2CO3). Thus, they must be studied with very little exposure to air during
sample preparation and loading. Secondly, a more technically challenging
issue arises from the fact that Li is a light-element and hence severe
irradiation-damage, via radiolysis or sputtering, occurs during electron-
microscopic investigation. Thus, structural and chemical characterization
must be performed at suitable low acceleration voltages to avoid irradiation
induced effects. In this work, we will present recent results on the structural
and chemical characterization of the lithium oxides.
9 4
add to my program
15:15 In-situ EELS studies on the dehydrogenation of nanocrystalline MgH2
Authors : A. Surrey, I. Lindemann, C. Bonatto Minella, O. Gutfleisch, L. Schultz, B.
Rellinghaus
Affiliations : IFW Dresden, Institute for Metallic Materials, Helmholtzstrae 20, D-
01069 Dresden, Germany
Resume : In the field of hydrogen storage there is a still ongoing search for
a material that provides both high H2 storage density and good H2 sorption
properties. Here, nanosized or nanoconfined hydrides promise improved
thermodynamics and kinetics. As for the structural characterization utilizing
TEM, however, most materials degrade fast upon the irradiation with the
imaging electron beam. MgH2 is one of the best studied binary hydrides due
to its relatively high storage capacity of 7.6 wt.% H2. Therefore, ball milled
MgH2 was used as a reference material for in-situ TEM experiments on
submicron particles in order to shed some light on the interaction of the
electron beam with the sample material. Hereto, EELS measurements were
conducted in an aberration-corrected FEI Titan3 80-300 microscope
operated at 80 kV. From an observation of the plasmonic absorptions it is
found that MgH2 successively converts into Mg upon electron irradiation.
The temporal evolution of the spectra is analyzed quantitatively to
determine the fractions of pure and hydrogenated Mg at different stages of
the reaction. This allows for an investigation of the dehydrogenation kinetics
which strongly depends on the particle size, the local temperature, and the
enthalpy of formation. The results of our in-situ TEM-EELS studies on MgH2
are compared to those obtained from more and less stable hydrides such as
LiBH4 and NaAlH4, respectively.
9 5
add to my program
15:30 Coffee break

Back

strasbourg.com

Emrs 2012

Caricato da

Informazioni sul documento

Titolo originale

Copyright

Formati disponibili

Condividi questo documento

Condividi o incorpora il documento

Opzioni di condivisione

Hai trovato utile questo documento?

Questo contenuto è inappropriato?

Copyright:

Formati disponibili

Emrs 2012

Caricato da

Copyright:

Formati disponibili

A B C D E F G H I J K L M N O P Q R S T U V W X Y

E-MRS Spring 2012 - Symposium X

Potrebbero piacerti anche