i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1

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Post-operational characterization of solid oxide

fuel cell stacks

Peter Batfalsky a, Jurgen Malzbender b,*, Norbert H. Menzler b

a
Forschungszentrum Julich GmbH, Central Institute of Engineering, Electronics and Analytics, ZEA-1, 52425 Julich,
Germany
b
Forschungszentrum Julich GmbH, Institute of Energy and Climate Research, IEK, 52425 Julich, Germany

article info abstract

Article history: Progress in solid oxide fuel cell (SOFC) cell and stack development depends strongly on
Received 11 March 2016 improvements stimulated by post-operational characterizations. Although highly moti-
Received in revised form vated by the analysis of unintended interruptions or stack failures, detailed characteriza-
4 May 2016 tion of SOFC stacks after operation provides information on the behaviour of advanced
Accepted 7 May 2016 materials and optimized microstructures as well as interactions during start-up, operation,
Available online 27 May 2016 and shut-down, hence, also with respect to manufacturing quality control and stack
structural integrity and its relationship to manufacturing, design, dimensions and toler-
Keywords: ances. This work summarized the experience of more than 300 post-test analyses that
Solid oxide fuel cell have been carried out in the past 15 years, their careful dissection, photography, and
Post-test characterization subsequent detailed characterization that included numerous detailed examinations of all
Methodology stack components. Particular analyses' concerning the different stack components are
Stack dissection highlighted, exemplifying useful analytical methods. Finally, conclusions are presented
with respect to ongoing R&D work and future directions.
2016 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.

Forschungszentrum Julich (Julich) has been working on

Introduction
Nowadays, after decades of research and development, solid
oxide fuel cells (SOFCs) are promising electrochemical devices
for stationary and mobile applications, where the operation in
electrolysis mode as well as coupling to metal oxide storage
devices enhance their potential for the global energy market
[1e5]. Current stack technology verified operation for more
than 70,000 h and promising voltage degradation rates of less
than 1% per 1000 h [6]. Nevertheless, understanding of stack
failure as well as long-term degradation mechanisms are still
main aspects for the production of reliable and cost efficient
devices for envisaged stationary and mobile applications.
SOFC development since around 1990. Since then, more than
600 stacks of various sizes and designs have been operated.
Cross-sectional and explosion drawings on the different Julich
stack designs can be found in Refs. [6e8]. Roughly half of the
operated stacks received a detailed post-operational inspec-
tion, which is necessary to understand degradation and fail-
ure mechanisms, for example, failure reasons, electrical
characteristics during stack operation or the relationship be-
tween interaction phenomena and operation conditions. In a
stringent post-test methodology, advanced characterization
methods are an essential element to understand the stack
performance within the frame-work of systematic testing,
where in particular in the last decade new characterization

* Corresponding author. Tel.: 49 2461 616964; fax: 49 2461 613699.

E-mail address: j.malzbender@fz-juelich.de (J. Malzbender).
http://dx.doi.org/10.1016/j.ijhydene.2016.05.065
0360-3199/ 2016 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.
11400 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1
methods have been implemented and existing ones improved.
Furthermore, it has to be emphasised that the analyses aid
the development of promising prospective materials and
suitable material combinations to ensure high and even
enhanced power outputs along with long-term stability and
low stack degradation. Also interrelated with post-test anal-
ysis and its observation, geometrical contacting,
manufacturing accuracy and tolerances and their relationship
to the stack operation are typically considered. Disassembling
is carried out with selected experts depending on expected
outcome of the post-operational analysis and/or goals set in
initiating the stack experiment, hence post-test analysis al-
ways need to consider the stack operation along with all de-
tails known from the assembling and production of the
individual stack and its components with respect to quality
assurance and unusual events or changes in boundary con-
ditions. Experts are available from synthesis, production, and
interaction of materials, thermo-mechanics, corrosion,
thermo-chemistry, sealants, stack/system operation, single
cell testing, optical and scanning electron microscopy.
Currently information on post-test analysis, methods and
results is limited [9e12], concentrating often on single effects
after stack operation, single cell or model experiments and
theoretical considerations, such as corrosion, thermody-
namics or Cr-poisoning [13e36]. Post-test characterization
results of stacks can be found for example in Refs. [11,37e39].
In the Julich procedure, during the post-operational anal-
ysis, electro-chemical results and irregular events receive
special attention. In particular, cells and components that
display unusual operational behaviour are inspected in detail.
During disassembly a digital photographic image is taken of
every stack plane. Unusual observations are investigated
microscopically. After dismantling, if necessary more detailed
scanning electron microscopy (SEM) and/or transmission
electron microscopy (TEM) investigations are carried out. All
techniques along with particular observations will be
described later. Investigation methods cover graphical and
image analysis to gain insight into macroscopic changes and
associated shifts in colour. SEM and energy dispersive X-ray
analysis (EDX) deliver information on microscopic/structural
changes, in order to acquire a qualitative chemical analysis.
Furthermore, wet chemical analysis is used in a coarsely
localized quantitative analysis. Thermography and computer
tomography have been used successfully in determination of
the origins of short circuits and localization of porosities. X-
ray diffraction (XRD) offers insight into structural changes,
TEM into local changes at interfaces and reactions. Leakages
are localized using liquid dyes. Hence, the current work
summarizes in detail the dissection methodology, considering
also underlying reasons for analysis, individual characteriza-
tion methods and results.
Reasons for post-test analysis
The necessity for post-test characterizations originates from
the need to understand typical and untypical operational be-
haviours; examples from the work of the authors are:
- Characterization of failure during operation, that might be
related to short circuiting, non-contacted planes, leakage,
low open circuit voltage (OCV) of cells, spontaneous voltage
drop below a certain level (reaching the range of the Ni re-
oxidation potential) or external reasons, such as failure of
control or measurement unit or furnace, lightning strike or
voltage breakdown.
- Stack objective were achieved therefore subsequent
component characterization needed to be carried out
considering material changes, such as materials chemis-
try, crystallographic phases, microstructural changes,
development of oxide scales, material interactions (i.e.
sealant-metal, sealant-electrolyte, cell materials, contact
materials-metal) or geometrical aspects (i.e. component
thickness, creep, distances, tolerances, contact situation,
comparison to initial design measures).
- Search for specific phenomena and their dependence on
operational conditions, i.e. degradation phenomena on
anode side (such as coke formation, metal dusting, sulphur
poisoning, re-oxidation damage), chromium poisoning on
cathode side, metal (corrosion) or sealant (devitrification,
secondary phase formation), material interactions or
changes based on different operational conditions such as
influence of temperature, applied current density, used
fuel gas, fuel and air utilization, and during thermal-, load-
or redox-cycling tests.
Typically it can be defined in advance which of these rea-
sons are the basis for the post-test characterization and/or
whether the stack characterization has to answer a specific
question. This leads to the first important decision: will the
stack be dissected plane-by-plane and components subse-
quently characterized individually or should either the entire
stack or stack parts should be embedded in a polymeric resin
in order to retain geometry and contact situation and samples
thereafter have to be extracted via typically water jet cutting
in well-defined positions for individual post-test analysis. If
the stack is partly embedded a decision has to be made con-
cerning which area is to be embedded and in which direction
(parallel or perpendicular to the gas flow) it will be cut. Even if
the stack is not embedded, it is possible after plane-by-plane
dissection to extract single samples from individual parts
such as the frame with cell, interconnect or bottom and top
plate typically by laser cutting for subsequent investigations.
Post-test analysis methodology
Especially in order to assess changes of stack planes, it is
important to document images of the planes before assem-
bling and after dissection. To ensure good and long-term stack
operation the post-test characterization starts, due the strong
interrelationship of both aspects, with a quality assurance
system for the single components, e.g. cells [40e42], sealant
[43e45] and metal parts (interconnect and frame) [46], con-
tinues during stack assembling, stack operation, stack
dissection and ends with the special post-test analysis. Fig. 1a
explains this schematically. For simplification, the diagram
only includes cells, sealant and metallic components. In real
stack assemblies contact materials such as anodic nickel
mesh or contact layers on cathode side and evaporation pro-
tection layers or electronic insulating layers are applied
[2,6,12] and hence also analysed.
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1
Fig. 1 e a: Scheme of stack life including necessary quality assurance to ensure high quality of post-test analysis, b: Flow
chart of possible stack post-test analyses'.
Quality and reproducibility of materials and processes are
ensured by sequential numbering of all stack parts (cells, in-
terconnects, frames, glass-ceramic batches), handling in-
structions for all processing steps, standardized stack
operation and stack dissection protocols. All information is
collected on a central server. Thus after stack testing, dissec-
tion and post-analysis, conclusions can be drawn with respect
to the used materials, processes and testing. Hence, there is a
complete uninterrupted chain from the initial starting mate-
rials to the post-test analysis which is also necessary to
develop SOFC systems for marketability.
Various characterization methods exist for stack, compo-
nents or individual samples, i.e.:
- entire stack, for example leak testing in assembled condi-
tion and leak detection with colour intrusion method,
thermography to localize short circuiting, photography of
all stack sides, optical microscopy (including distance
measurements), distance and thickness measurements
with micrometer screw and feeler gauge.
- stack planes, for example photography of every plane
(anode and cathode side) in sequence of stack disassembly,
optical microscopy (defects, cracks, corrosion, and topog-
raphy to characterize warpage or surfaces state).
- stack components (cell, frame, interconnect), i.e. photog-
raphy, optical microscopy, topography to characterize
warpage, surfaces or roughness, SEM (surfaces, fractured
or polished cross sections) along with EDX, TEM, XRD of
crystal phases, wet chemical analysis for composition,
incorporation of foreign elements, stoichiometries
Stack dissection
Due to the importance of this aspect, a special laboratory has
been set up in Julich for stack dissection. It contains all
necessary tools for dimensional assessment, dissection,
documentation and basic characterization methods and is
11401
equipped with an extractor hood in which the plane-by-plane
dissection is carried out. A CCD camera is mounted above the
dissection place in the hood to photograph the planes with
transfer to PC based collector software to label specific pho-
tographs permitting the addition of comments and findings.
An optical microscope for documentation of visible areas is
available which is also equipped with a CCD camera (pictures
are later included in the dissection protocol). All necessary
tools for stack dismantling and measuring are available. All
stacks are stored in cabinets for several years so that samples
might be extracted later for further investigations that might
be triggered by later stack tests and dissections and the in-
terest in finding correlations.
Thermography
The arranged stack dissection sequence follows the questions
emerging during stack operation and subsequent shut down.
For example, if short-circuiting was measured, as long as the
stack does not exceed a certain number of planes, it is char-
acterized thermographically before dismantling (if it has too
many planes it heats-up rather uniformly and local charac-
terization is not possible) [35,36]. Thermographical analysis is
carried out by feeding an electrical current to the stack and
electrically conducting paths lead to local heating, however,
due to equilibration effect the thermographic images change
with time. An example is presented in Fig. 2. If the stack with
short circuit consists of more than around five planes plus
bottom and top plate, it is first partly dissected and subse-
quently the remaining partition is characterized by thermog-
raphy. Hence, this method cannot only be used for small
stacks but also for large power stacks.
After taking thermographic images, the stack can be
dismantled and the localized short circuit inducing area
characterized in detail. As an example, in the stack presented
in Fig. 2 a metallic particle in the glass-ceramic sealing was
identified as reason for the short-circuiting. The metallic
particle might have been induced by interconnect or frame
11402 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1
Fig. 2 e Thermography image showing area of short-circuiting.
conditioning or was introduced during stack assembling. Such
malfunctions can be avoided by assembling the stack in a low-
dust laboratory supported in terms of quality control by
photographing every plane during stack assembly.
Stack embedding
Occasionally stacks are embedded either partly or completely
into a polymeric resin in order to permit a characterization of
contacting situation and interfacial reactions [47]. The
embedding must be done carefully to ensure venting of the
stack; hence to fill all cavities with the liquid resin, otherwise
artefacts might be induced by the subsequent water jet cut-
ting. Water jet cutting has various advantages. First, the stack
thickness with adjacent bottom and top plate is in the centi-
metre range, which is a challenge for other techniques such as
laser cutting. Second, the stack consists of different materials
and material combinations and all of them should be cut in a
comparable manner. Third, water jet cutting does not lead to
melting of cutting edge effects typical for laser cutting. If for
example sawing is used, material differences between metal
or ceramic and polymeric resin become a key problem, since
the polymer may become liquid and subsequently it may
smear other parts and again cutting procedure related arte-
facts are produced. The contamination from the cutting parts
is negligible in the case of water jet cutting since all samples
are post-processed by grinding and polishing and thus
remnant contaminations are removed. If the stack is only
partly embedded, samples might be cut from embedded and
remaining part, permitting for example, chemical analysis of
cell parts with direct comparison and analysis of embedded
contact zones.
Photography and distance measurements
As mentioned above, if a stack is dissected plane-by-plane,
starting with the upper side of the top plate and ending with
the lower side of the bottom plate (gas connection side),
photographs are taken and directly transferred into a PC-
based image collecting software. However, before dissection,
especially since typically glass-ceramics are used for stack
sealing, distances between the planes (interconnect-frame-
interconnect) are measured by a feeler gauge on all four stack
edges. The distance control along with the measured total
heights of all sealing levels indicates whether there are sig-
nificant differences within one plane or within the entire
stack. Hence, also uniform settling during the stack start-up
joining procedure can be controlled.
After plane-by-plane dismantling every plane side (inter-
connect or frame with cell) is photographed to completely
characterize the stack, irrespective of whether there are areas
of special interest or changes during stack operation. Such
initial photographs answer many questions: Was the stack
assembly correct? Does every plane side (anode, cathode) look
alike as expected? Are there unusual colour or morphological
changes or anomalies? Is it necessary to analyse stack parts or
surfaces in more detail? Are there visible foreign phases? Are
cells unchanged (re-oxidation, cracking, coking) and undam-
aged? Are there indications of leakages (visible by remnants of
burning or gas streams)? Where does the sealant fracture
during dismantling (within glass-ceramic or at metal oxide-
glass interface)?
If during dismantling areas of special interest become
obvious, the plane is directly inspected by optical microscopy
permitting characterizations at higher magnifications. If
necessary, photographs are taken or parts are selected for
further characterization, e.g. SEM/EDX.
Most stacks are characterized already after operation with
respect to leakage, yielding information on internal (fuel to air
side) and external leakage (fuel and air side to surrounding
environment). The so-called colour intrusion method [47]
has evolved to be one of the most powerful tools for charac-
terizing of especially external stack leakages with high accu-
racy, i.e. even smaller leaks and/or cracks can be detected
than with for example a bubble test.
The stack is painted with a red colour, which is normally
used for crack detection of welded seams. After a few minutes
the outside of the stack is rinsed with water to remove the
excess colour. Then the stack is dried either overnight at
ambient conditions or at slightly higher temperatures so that
it can be dismantled later. Due to the colouring, the leakage
location in the glass-ceramic sealant can be easily
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1 11403

differentiated from the gas-tight regions during plane-by-
plane dissection. Additionally, it is also possible to differen-
tiate between complete cracking, which means that the cracks
run through the entire sealant hence bridging the stack inte-
rior to the outside, and partial cracking (overall gas tightness
still maintained). Via this optical visualization procedure it is
also possible to verify whether leakages are related to singular
regions or whether they are distributed randomly. Therefore
this method and analysis can also be used as a tool to detect
problem areas related to geometrical effects and/or non-ideal
structures. Fig. 3 presents some stack photographs after stack
dismantling revealing different leakages types. In Fig. 3a and
b, two planes from one particular F20 design power stack (for
design see Refs. [6,7]) after a thermo-cycling test are shown.
One plane reveals significant leakages, while the second one
appears to be gas-tight. The reason for this untypical result
was a strong thermal gradient in the z-direction consciously
applied to characterize the sealing behaviour. Fig. 3c presents
another plane from a F20 design stack with significant leakage
at one of the air-inlet channels. Possible reasons were again
thermal gradients or non-ideal sealant paths, i.e. 90 angles.
Finally, in Fig. 3d a plane from a cassette-type stack to be used
for auxiliary power units in mobile applications is presented,
which was severely thermo-cycled. Sealant cracks are visible
in the region where cold air entered the stack; i.e. a region
with major thermal differences. The results confirm that se-
vere temperature gradients within stacks induce large local
tensile stresses that lead to sealant cracking [7].
Optical microscopy
Optical microscopy is used, in addition to the detection of
surface-related changes or irregularities during dissection,
also for characterizing contact zones or to obtain an overview
with respect to geometrical issues of the stack or stack parts.
Hence, stack parts need to be cut and prepared by embedding,
grinding and polishing. Fig. 4 presents an optical photograph
taken during stack dissection showing a colour change at the
anode side of the cell in one plane. Optical microscopy directly
confirmed that the colour change is a result of an unwanted
interaction between cathode material and glass-ceramic
sealant due to imprecise application of the glass paste since
both materials should have no contact during assembly or
testing. The interaction causes local stresses within the
sealant region and subsequently cracks and a gas crossover
between air and hydrogen leads to burning. Additionally, the
formed interdiffusion phase is electrically conductive and
may cause short-circuiting if it bridges the sealing gap.
Another example of visible changes or interactions during
stack testing is associated with re-oxidation phenomena,
which are obvious since anode colour changes from grey
(reduced Ni) to green (oxidized Ni), see Fig. 5a [34]. A typical re-
oxidation phenomenon is presented in Fig. 5b. The electrolyte
cracks due to tensile stresses caused by Ni re-oxidation and
volume change when forming a porous NiO structure
[33,34,36]. This fine-structured electrolyte cracking network is
typically a visible proof of re-oxidation. In Fig. 5c a cell defect
is shown which caused cell cracking and subsequently re-
oxidation, finally leading to stack failure.
Optical microscopy is also used for post-test analysis of
cut, ground and polished samples, requiring analysis of
structures with a dimension of at least ~10 mm, i.e. contact
areas, microstructures, geometrical aspects such as toler-
ances, distances etc. and overview pictures as guidance for
further SEM/EDX characterization. The technique was also
partially successful to analyse the behaviour of silver based
brazes [8,43] in lightweight planar SOFCs (design see Ref. [8]),

Fig. 3 e Photographs of stack planes after applying the colour intrusion method and plane-by-plane dismantling; a) plane of
a F20 design stack (for design see Refs. [6,7]) with massive leakages; b) plane from the same stack as in a) but without any
leakage; c) F20 design stack plane showing leakage in one air inlet channel; d) cassette-type stack plane with leakage near
the air inlet channels. (For interpretation of the references to colour in this figure legend, the reader is referred to the web
version of this article.)
11404 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1

Fig. 4 e Characterization of areas of special interest during stack dissection by optical microscopy; a) stack overview photo,
b) higher magnification of marked rectangle in a), c) optical microscopy photography from the rear side of the colour-
changed zone showing unwanted interaction between cathode and glass-ceramic sealant. (For interpretation of the
references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 5 e Left: top view photograph of the anode side from a re-oxidized stack, being visible by the green colour of the re-
oxidized Ni and the gas stream in the gas-out manifold in a); b) typical cracking structure of the electrolyte after anodic re-
oxidation (top view from the cathode side); c) optical microscopy top photograph of a cell defect (view from cathode side).
(For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

revealing sealant micro-pores that terminated stack opera-
tion [48].
Fig. 6a and b give some other examples of cross-sections.
The overview of three repeating units of one embedded stack
in Fig. 6a permitted to measure directly the anodic and cathodic
distances and sealant thickness, therefore being an easy, but
destructive technology to verify stack assembling quality. The
cross-section of an unusual stack is shown in Fig. 6b. In this
stack with five repeating units the cathodic contact area was
deliberately modified. Normally, contact on the cathode side is
ensured by a channelled structure. An additional perovskite
contact layer material ensures contacting between the inter-
connect channel and the cathode. The contact area was delib-
erately reduced by milling some of the channels. In this stack,
the contact area of two planes was kept in the typical geometric
arrangement and the others were reduced. The reason for
reducing the channel size only by milling was to limit effects
onto the gas stream, i.e. avoiding a change two parameters at
the same time (contact area and pressure drop). After testing,
the stack was embedded completely and then cut in the direc-
tion transverse to the channel to characterize the contact
zones. It can be seen that the contacts are not ideally, but have a
convex structure, related to the contact layer wet powder
spraying process, i.e. the thicker the contact layer the more it
tends to form this lens-like structure.
This embedding, cutting, polishing and subsequent
characterizing by optical microscopy can also be used to
compare contacting, tolerances and dimensions in a real
stack to the blueprint as shown in Fig. 6c, which represents
an optical photograph of a cassette-type light-weight stack
(for design see Ref. [8]). In this picture, various on-line
measurement locations were devised in order to charac-
terize the distances after stack assembly and testing and to
verify thicknesses and width of the contact layer applied by
a dispenser system. Hence, a measurement system within a
optical microscope can be used as a quality assurance sys-
tem with optional automatization; however, it is a destruc-
tive method.
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1 11405

Fig. 6 e a) optical microscopy photograph showing a part repeating units in one embedded stack (cross-section parallel to
gas channels), b) optical microscopy photograph showing five repeating units of one embedded stack (cross-section
perpendicular to gas channels), upper cell interconnect contact area reduced by 25%, middle cell reduced by 67%, c) cross-
section of two repeating units of a cassette-type stack.

Laser or white light triangulation
The warpage of a component, its deflection, layer thicknesses
and surface roughness as well as distances and heights can be
assessed by laser or white-light topography. It also can be used
for example after dissection to characterize geometrical
changes of interconnects, which might be induced by me-
chanical loads and creep effects. To minimize plane warpage
effects caused by the dissection procedure, the stack might also
be topographically measured as a whole stack or stack parts,
before and after stack testing. Two examples of a cassette-type
stack plane with different sealed cells before stack assembly
have been presented in Ref. [47]. The topography is typically
carried out using laser head with automatic x-y-table, which
works according to the laser triangulation method [49]. With
different sensors, either sample warpage (up to the mm range)
or surface roughness (mm range) can be measured. There are
various reasons for different bending behaviour such as cell
thickness, substrate manufacturing process, but also oxide
layers on the interconnects (see also [50,51]).
Scanning electron microscopy and electron-dispersive X-ray
analysis
SEM is typically used on cut, embedded, ground and polished
specimens extracted from cell, sealant and/or interconnects,
but can also be applied to fractured surfaces. Using SEM/EDX
(possible only for polished samples) mostly microstructures,
layer thicknesses, materials interactions and formation of, for
example, foreign phases are characterized (see Fig. 7), where
EDX permits insight into chemical compositions and inter-
diffusional effects. Four examples from different post-test
11406 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1

Fig. 7 e SEM cross-sectional images of various stack zones after stack testing; a) interdiffusion between Crofer22APU
interconnect and metallic Ni mesh; b) sealing situation between interconnect, cell and sealant; c) cathodic contact zone
interconnect and cell; d) microstructural changes within LSM cathode after interaction with volatile chromium species.

SEM analysis are given in Fig. 7. First, Fig. 7a shows the
interaction between the metallic interconnect material and
contacting Ni-mesh on the anode side after more than
17,000 h of stack operation [52], with obvious interdiffusion of
iron and chromium from interconnect and nickel. Due to Ni
diffusion into the original ferritic Crofer22APU, it becomes
austenitic. The austenitic phase is typically more brittle,
which might lead to the risk to loss contact during stack
thermo-cycling.
The sealing situation on the cathode side is presented in
Fig. 7b. Two sealing zones can be seen: one is the cell sealing
to interconnect and the other one is the sealing of inter-
connect to metallic frame, which is bearing the cell. The
sealant microstructure is very homogeneous and it bonds
well to all interfaces. The contact situation on the cathode
side between interconnect channel and cathode is high-
lighted in Fig. 7c. The contact layer, which is applied by wet
powder spraying, covers all channel areas (bottom, top and
flanks) and is on the top side quite homogeneous and flat,
ensuring good contact. Finally, the microstructural change
within the cathode, at the boundary to the electrolyte, is
presented in Fig. 7d. This microstructural change is a result
of interaction of the lanthanum strontium manganite (LSM)
cathode material with volatile chromium species. A foreign
phase (MnCrO3 or Cr2O3) is formed leading to cathode
coarsening [13,25,26].
If local materials analysis or concentration profiles are
required, EDX analysis can be carried out as spot, line or area
analysis. In some cases, also wavelength-dispersive X-ray
analysis (WDX) is an option (e.g. to verify whether a phase
consists of minimal amounts of Cr, or whether the Cr-Ka1 line
overlaps with the La-Lb2 line from the cathode). In fact, the
interaction with volatile chromium species is regarded as a
major cause of SOFC stack degradation [25e28]. The reaction
between the volatile Cr species, mostly CrO2(OH)2 and the
cathode depends, from a materials point of view, on the
cathode type. In the case of LSM-based cathodes, the Cr reacts
at the interface between cathode and electrolyte forming
chromia or a CreMn-spinel. In the case of the LSCF
(LaeSreCoeFe) type cathodes, the reaction is different. While
between Cr and LSM two main interactions are the chemical
formation of chromia and the reduction reaction of Cr-VI to
Cr-III at the triple phase boundaries and the subsequent re-
action with Mn from the LSM, the chemical reaction between
Cr and LSCF is presumably not based on a reduction reaction.
The volatile Cr species reacts with Sr from the LSCF in a gas
phase or gas/solid SrO interaction. During this reaction, stable
SrCrO4 is formed; however, the new phase does not
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1
precipitate at the interface cathode/electrolyte, but at the top
of the cathode surface.
The fact that the reaction between Cr and Sr is favourably a
gas phase reaction was supported by the post-test findings of
one particular stack. It had LSCF-based cathodes and was
thermo-cycled a number of times. SEM surface micrographs of
the zone between cathode/contact layer area and gas channel
in Fig. 8 reveal a multitude of SrCrO4 needles in this area,
where the air stream is hindered. Higher magnifications of the
needles revealed a layered microstructure being typical of
evaporationecondensation reactions, i.e. with every thermo-
cycle SrCrO4 precipitates during the cooling preferentially at
the surface of the already existing needles. These micrographs
also indicated that the Sr-chromate needles formed primarily
at mud-cracks of the cathode surface. These cracks originate
from the drying step of the screen printing paste. The needles
show some kind of outward growth from the cracks into the
gas phase space. EDX dot analysis confirmed the formation of
SrCrO4 (only qualitatively). These basic findings that the
foreign phase formation occurs preferentially on the cath-
odes surface is supported by various other authors [14,53], but
a recent work also confirms the formation of the same SrCrO4
phase also at the cathode/electrolyte interface [54]. However,
the overall interplay between volatile Cr-species and SOFC
cathodes is not completely understood.
Fig. 8 e SEM micrographs of the LSCF cathode surface of a thermo-cycled stack showing SrCrO4 formation in the
intermediate zone between contact area and air channel.
11407
X-ray diffraction (XRD)
X-ray diffraction is used after stack dissection and sample
cutting to characterize the crystal structure of the various
materials. Additionally, their changes due to interactions,
segregation, incorporation of additional elements, thus
forming foreign phases or decompositions, can be assessed.
The cathode surface of a stack with LaeSreFe-cobaltite
cathode, which has experienced long-term operation has
been analysed via X-ray analysis in Refs. [47], revealing three
crystallographic phases: copper, from the copper strip used
for covering the areas not to be analysed; the orthorhombic
perovskite of the cathode material and as a third phase,
monoclinic SrCrO4. Comparison of the two diffractograms
presented in Ref. [47] (at bar and channel) reveals that the Sr-
chromate reflections are more pronounced in the area
beneath the channel bar. Here the secondary Sr chromate
phase is formed between the Sr from cathode and volatile Cr
species. The foreign phase amount at the cathode surface
beneath the gas channel is significantly lower, indicating that
the reaction between Sr and Cr species is preferentially a gas
phase reaction and that both gas phases are removed from the
stack by the air stream [27], while the SrCrO4 precipitates
within the porous interface of the contact area, where the air
stream is limited. Hence the non-destructive technique XRD
11408 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1
confirms the SEM findings (cf. Section Scanning electron
microscopy and electron-dispersive X-ray analysis), but can
also be used before or alternatively to SEM characterization if
the intact state of the sample is still necessary (but the mea-
surement accuracy of XRD is far lower than that of SEM).
Other interesting aspects for X-ray diffraction studies are,
for example, deterioration of the 8YSZ electrolyte (8 mol%
yttria-stabilized zirconia) from a cubic to monoclinic/tetra-
hedral [39] structure after long-term operation or austenite
formation in the interconnect by Ni diffusion [46].
Wet chemical analysis
Wet chemical analysis can be used for example to quantify
amounts of incorporated foreign elements into anode or
cathode structure. However, the method is destructive, it
does not permit a local resolution (i.e. only whether but not
where the foreign element is in cathode, phase boundary or
current collector) and finally, sample preconditioning is
necessary, which complicates the analysis process. It needs
to be determined which acid leaching works, which acid/acid
mixture dissolves all the material and whether other com-
ponents that should not be dissolved are also entering the
solution, e.g. if the cathode material is dissolved Ni may also
be partly dissolved. In fact, recent publications also push
forward the wet chemical analysis of e.g. LSCF-cathodes for
distinguishing between surface enriched SrO und bulk LSCF
[55]. Hence, this technique might also be used in future for
differentiating between various phases within SOFC
electrodes.
One major aspect leading to wet chemical analysis in the
past was the assessment of chromium incorporated into the
cathode during stack operation with metallic interconnects
[29]. Typically cell parts with typical dimensions of 1 cm2 were
extracted by laser cutting and the cathode was subsequently
removed by leaching in perchloric acid [30,32]. Hence, the
perovskite itself and formed foreign phases such as chromia
or CreMn-spinel were completely dissolved with almost no Y
or Zr from the electrolyte and only small amounts of nickel
from the anode. By taking the starting cathode composition as
a reference and considering a specific sample area, the
amount of incorporated foreign elements can be calculated
per square centimetre or with respect to stoichiometry. An
additional comparison with SEM micrographs (or XRD) from
the same sample can give twofold information: first, amount
from the wet chemical analysis and, secondly, macro- or
micro-local resolution of the detection of Cr within cathode,
current collector or other cell or contact layers, hence,
combining optical and elemental analysis.
An overview of Cr incorporation results into cathodes from
stacks operated for different times and operational condi-
tions, which permitted to draw some conclusions with respect
to the interaction of chromium species with SOFC cathodes
has been presented in Ref. [47]. This work indicates that, first,
there is an obvious time dependency, but additionally there
seems to be some saturation effect (in particular at a current
density of 0.5 A/cm2). After approximately 3000 h of operation
there appears to be no additional Cr incorporation anymore
into the cathode. Another result that can be deduced from this
work is that LSCF cathodes incorporate more Cr than LSM
cathodes and that there is little difference in the amount of Cr
for stack operation times of 1900 h and more than 17,000 h.
These results triggered further R&D in the field of Cr-related
degradation [30,32], aiding a better understanding of the
basic interactions, chemical/electrochemical reactions, de-
pendencies on temperature, time, current density, Cr partial
pressure and impact on cell/stack performance.
Long-term testing
Topics that received special consideration are post-test anal-
ysis result and their relationship to degradation phenomena
under steady state operation in the case of long-term testing.
Chromium poisoning is believed to be one influential param-
eter and has received significant attention in Julich, hence, as
outlined above, post-test analysis and methodological im-
provements concentrated strongly on this aspect [25,52,56].
Within the framework of post-test investigation on the
degradation phenomena of long-term operated stacks
detailed analyses have been carried out for stacks operated
17,000 h at 700  C with an average degradation rate of 10 mV
per 1000 h at 500 mA cm2 [11] and about 19,000 h at 800  C
(with additional protective layer) with 4 mV per 1000 h at
500 mA cm2 [39]. In addition to the differences in operation
temperature it should be noted that the stack operated at
700  C had an LSCF cathode with GDC (gadolinia-doped ceria)
diffusion barrier and a protective slurry coating on the inter-
connect and the one operated at 800  C had an LSM cathode
and an atmospheric plasma sprayed coating. Whilst the stack
operated at 700  C was shut down after progressive degrada-
tion, the stack operated at 800  C was shut down after failure
of one cell.
In summary, parts of the stack operated at 700  C, that
received detailed post-test analysis, indicated only small
changes and interactions [11]. The cell microstructure
appeared to be slightly changed. Two findings appeared play a
role with respect to long-term stack stability. Local dot-like
iron oxide formation may cause eventually short circuiting if
the oxide bridges the sealing gap after even longer operating
times and it was suggested that the progressive degradation
might be a result of strontium chromate formation.
For the stack operated at 800  C no significant Cr contents
could be found in the cathode thus verifying that the MCF
(manganese-cobalt-iron-oxide) layer applied by APS (atmo-
spheric plasma spraying) is an efficient Cr barrier [28]. How-
ever, Mn diffusion into 8YSZ led to local accumulation at the
grain boundaries, which appeared to induce a decrease in
conductivity and a mechanical weakening and eventual
micro-cracking at the grain boundaries followed by
continuing crack growth [39]. The growth of these cracks
eventually resulted in the fracture of one cell, burning of fuel
gas and stack failure.
From the results of both stacks, it can be concluded that the
targeted operation times of SOFC stacks can become realistic
by combining an LSCF cathode with an APS protective coating,
which is realized in a currently ongoing stack test [6]. Because
all stack tests have been performed with pure hydrogen (gas
purity better than 99.9%) nothing can be stated with respect to
the effect of impurities within the fuel gas, especially sulfur
compounds.
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1
Lessons learned from post-test stack dissection and analysis
SOFC stack tests are complex, time- and material-consuming
but an absolute necessity for the progress of the technology.
Although, from single cell tests a lot of information with
respect to mimicking stack testing behaviour can be obtained,
e.g. basic material interactions, interdiffusions, material
coarsening, poisoning, the stack environment has additional
special boundary conditions, for example: geometrical re-
lationships, real anodic and cathodic contacting, air and fuel
gas streams, degree of gas utilization and pressure differences
between stack and environment or between anode and cath-
ode. Hence, some complex interactions, problems, events and
operational results only appear in stack testing. Thus careful
QA before stack assembling, a careful recording of stack as-
sembly and procedure, testing and stack post-test analysis are
indispensable to understand SOFC operational behaviour and
degradation. In this respect, post-test analysis, which is
interlinked and overlaps with all other aspects, is one of the
keys to enhance lifetime and minimize stack degradation and
thus to minimize the gap from R&D to SOFC market entry.
In many cases no correlations were found between the
electrochemical events and the post-test analysis. However,
for a number of events, degradation phenomena and in-
teractions, a careful, reproducible and scientific post-test
analysis was able to answer question. Examples are the
interaction of volatile chromium species with various cathode
materials, the influences of design, air steam, current density
etc. can only be assessed using stack testing. Many of the re-
sults obtained so far were observed first time within a stack
and subsequently single cell tests could be adopted to un-
derstand the basic reaction mechanisms and dependencies.
Another example are the interactions of metallic inter-
connect material with some glass-ceramics, resulting in short-
circuiting after rather short stack operation times [52], which
was not found in single cell tests since here the sealing is
typically realized with gold or silver wires and not glass-
ceramics. In subsequent basic R&D the origin of the severe
interaction was found, reactions due to small amounts of Al
and Si in the metal and Pb in the glass and the formation of an
outward-growing conductive phase, and could then be avoi-
ded. A third example is the lens-like structure of the contact
material on channel bars. If only 50% of the channel bar con-
tacts the cathode, the real current density is rather different
from the one applied and calculated. Optimizing channel bar
structure and coating process led to better more even contact
zones. Most of these findings and associated improvements
would not have been realized without post-test characterized.
Besides the widely used tools discussed above, a few ex-
amples of other techniques are given in the following, but this
list does not claim to be exhaustive:
- transmission electron microscopy (TEM), including focused ion
beam (FIB) for high-resolution investigations concerning
particle sizes and structures, chemical and crystallo-
graphic analysis', detection of foreign phases or inclusions
etc.; destructive method,
- computer tomography to characterize sealing regions, in
particular porosities or geometrical situations (currently
11409
limited by relative low resolution); non-destructive
method,
- atomic force microscopy (AFM) and confocal microscopy for
higher magnification of surface structures, roughness (also
micro-roughness), and small defects; destructive method
- chemical analysis techniques in z-direction (depth) such as
LIBS (laser-induced breakdown spectroscopy), GDOS (glow
discharge optical emission spectroscopy), SIMS (secondary
ion mass spectroscopy), SNMS (secondary neutron mass
spectroscopy), LEIS (low-energy ion scattering), XPS (X-ray
photoelectron spectroscopy) ; mostly destructive due to
sample size.
Conclusions
Modern analytical methods are being increasingly utilized to
characterize SOFC stacks after operation. Besides non-
destructive analysis technologies such as tomography,
topography measurement and thermography, a wide variety
of destructive methods can and, hence, have been applied.
Typically, post-test characterization has to reply upon more
than one analytical method since each has advantages and
limitations, e.g.: only numerical information such as the
amount of elements or thickness can be obtained, but no in-
formation with respect to the (micro)structure or location;
structural information but no elemental information or
microstructural, elemental but no crystallographic informa-
tion and so forth. Hence, in most cases it is necessary to
combine different analytical methods and, after careful
interpretation of individual result, conclusions can be drawn
concerning degradation effects, materials incompatibilities,
necessary quality assurance efforts or differences between
real and envisaged tolerances.
Before analytical methods can be selected to individually
characterize the stack components, a basic decision must be
made with respect to embedding or not. Fig. 1b is a flow chart
of these decision chains. In future, it can be expected that not
only post-test analysis will become more and more important,
but also in-situ characterizations during stack operation. In
addition to classical measurement of temperature at various
stack positions also optical technologies might be applied,
assessing stack settling, warpages, creep deformation etc.
Additionally, outlet gases are to be analysed, high-
temperature leak testing can be applied and acoustic emis-
sion tests to analyse cracking, depending on, for example,
thermo-cycling.
In the last decade the post-test analysis became an
important basis for stack improvement and development of
new stack designs. This permitted the operation of SOFC
stacks for long times and particularly low degradation rates
[2,6], which required the improvements triggered by the post-
operation inspection. Advanced methods were implemented
and methodologies were developed, that have been published
in a number of separate works [11,35,47]. Particular aspects
that received a lot of attention and led to detailed advanced
studies to understand underlying mechanisms and techno-
logical aspects were the interaction of glass-ceramic sealants
with metallic interconnect material [10], Cr interaction with
cathode materials [25,29,30,32], formation of pores in silver
11410 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 1 ( 2 0 1 6 ) 1 1 3 9 9 e1 1 4 1 1
based sealants and its relationship to the operation under
dual atmosphere and leakage of glass-ceramic sealant mate-
rials [43,48], that led to advanced stack operation procedures
[7], design improvements [2] and a number of studies on the
mechanical behaviour of sealant materials and its relation-
ship to the time at elevated temperatures [43e45,48]. An
aspect of ongoing studies and improvements is still the
interaction of cathode and contact layers with glass-ceramic
materials, which can lead to electric short circuiting [47],
however, also occasional stochastic short circuiting related to
metallic contaminations has been found. Short circuiting has
also been observed for thin metallic interconnects based APU
designs (for design see Ref. [8]) related to creep deformation of
the metallic materials along with design induced small
tolerances.
Improved quality assurance methods applied to the start-
ing materials, processes and components, better equipped
stack test facilities with in-situ measuring methods and more
sophisticated and standardized post-test analysis will help to
warrant longer lifetime, lower degradation and thus greater
marketability of the SOFCs. Future SOFC directions will aim at
power stacks with larger number of cells and operation in
combined SOFC e electrolysis mode operation as well as use
of the SOFC to charge metallic storage devices. Such applica-
tions will led to high demands with respect to materials
degradation, where also new interaction phenomena might be
expected [13], and in understanding mechanical stability as-
pects of cells and sealants related to subcritical crack growth
under moist atmosphere and related failure probability. A
future aspect is also the operation at lower temperature,
which will raise new questions related to the novel materials
and extremely thin electrolytes required to fulfil the electronic
demands, where the post-test analysis of stacks will be a main
tool to understand effects and trigger improvements.
Acknowledgements
The authors gratefully acknowledge the support, co-operation
and discussions within the Forschungszentrum Julich SOFC
Stack Dissection Group.
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