TY - JOUR A1 - Bevilacqua, N. A1 - Asset, T. A1 - Schmid, M. A. A1 - Markötter, Henning A1 - Manke, I. A1 - Atanassov, P. A1 - Zeis, R. T1 - Impact of catalyst layer morphology on the operation of high temperature PEM fuel cells N2 - Electrochemical impedance spectroscopy (EIS) is a well-established method to analyze a polymer electrolyte membrane fuel cell (PEMFC). However, without further data processing, the impedance spectrum yields only qualitative insight into the mechanism and individual contribution of transport, kinetics, and ohmic losses to the overall fuel cell limitations. The distribution of relaxation times (DRT) method allows quantifying each of these polarization losses and evaluates their contribution to a given electrocatalyst's depreciated performances. We coupled this method with a detailed morphology study to investigate the impact of the 3D-structure on the processes occurring inside a high-temperature polymer electrolyte membrane fuel cell (HT-PEMFC). We tested a platinum catalyst (Pt/C), a platinum-cobalt alloy catalyst (Pt3Co/C), and a platinum group metal-free iron-nitrogen-carbon (Fe–N–C) catalyst. We found that the hampered mass transport in the latter is mainly responsible for its low performance in the MEA (along with its decreased intrinsic performances for the ORR reaction). The better performance of the alloy catalyst can be explained by both improved mass transport and a lower ORR resistance. Furthermore, single-cell tests show that the catalyst layer morphology influences the distribution of phosphoric acid during conditioning. KW - High-temperature polymer electrolyte membrane fuel cell KW - Platinum-free catalyst KW - Mass transport KW - Oxygen reduction reaction KW - Distribution of relaxation times analysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520917 DO - https://doi.org/10.1016/j.powera.2020.100042 VL - 7 SP - 100042 PB - Elsevier Ltd. AN - OPUS4-52091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziesche, R. F. A1 - Robinson, J. B. A1 - Markötter, Henning A1 - Bradbury, R. A1 - Tengattini, A. A1 - Lenoir, N. A1 - Helfen, L. A1 - Kockelmann, W. A1 - Kardjilov, N. A1 - Manke, I. A1 - Brett, D. J. L. A1 - Shearing, P. R. T1 - Editors’ Choice—4D Neutron and X-ray Tomography Studies of High Energy Density Primary Batteries: Part II. Multi-Modal Microscopy of LiSOCl2 Cells N2 - The ability to track electrode degradation, both spatially and temporally, is fundamental to understand performance loss during operation of lithium batteries. X-ray computed tomography can be used to follow structural and morphological changes in electrodes; however, the direct detection of electrochemical processes related to metallic lithium is difficult due to the low sensitivity to the element. In this work, 4-dimensional neutron computed tomography, which shows high contrast for lithium, is used to directly quantify the lithium diffusion process in spirally wound Li/SOCl2 primary cells. The neutron dataset enables the quantification of the lithium transport from the anode and the accumulation inside the SOCl2 cathode to be locally resolved. Complementarity between the collected neutron and X-ray computed tomographies is shown and by applying both methods in concert we have observed lithium diffusion blocking by the LiCl protection layer and identified all cell components which are difficult to distinguish using one of the methods alone. KW - Lithium-ion battery KW - Room-temperature KW - Thermal runaway KW - Gas evolution KW - Cells PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520890 DO - https://doi.org/10.1149/1945-7111/abbfd9 VL - 167 SP - 140509 PB - IOP Science AN - OPUS4-52089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yao, J. A1 - Zhu, G. A1 - Dong, K. A1 - Osenberg, M. A1 - Hilger, A. A1 - Markötter, Henning A1 - Ju, J. A1 - Sun, F. A1 - Manke, I. A1 - Cui, G. T1 - Progress and Perspective of Controlling Li Dendrites Growth in All-Solid-State Li Metal Batteries via External Physical Fields N2 - Li dendrites penetration through solid electrolytes (SEs) challenges the development of solid-state Li batteries (SSLBs). To date, significant efforts are devoted to understand the mechanistic dynamics of Li dendrites nucleation, growth, and propagation in SEs, and various strategies that aim to alleviate and even inhibit Li dendrite formation have been proposed. Nevertheless, most of these conventional strategies require either additional material processing steps or new materials/layers that eventually increase battery cost and complexity. In contrast, using external fields, such as mechanical force, temperature physical field, electric field, pulse current, and even magnetic field to regulate Li dendrites penetration through SEs, seems to be one of the most cost-effective strategies. This review focuses on the current research progress of utilizing external physical fields in regulating Li dendrites growth in SSLBs. For this purpose, the mechanical properties of Li and SEs, as well as the experimental results that visually track Li penetration dynamics, are reviewed. Finally, the review ends with remaining open questions in future studies of Li dendrites growth and penetration in SEs. It is hoped this review can shed some light on understanding the complex Li dendrite issues in SSLBs and potentially guide their rational design for further development. KW - Li dendrites KW - Li dendrites penetration mechanisms KW - Solid electrolytes KW - Solid-state batteries PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588331 DO - https://doi.org/10.1002/aesr.202300165 SN - 2699-9412 SP - 1 EP - 44 PB - Wiley-VCH CY - Weinheim AN - OPUS4-58833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Z. A1 - Dong, K. A1 - Mazzio, K. A. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Heinemann, T. A1 - Manke, I. A1 - Adelhelm, P. T1 - Phase transformation and microstructural evolution of CuS electrodes in solid-state batteries probed by in situ 3D X-ray tomography N2 - Copper sulfide shows some unique physico-chemical properties that make it appealing as a cathode active material (CAM) for solid-state batteries (SSBs). The most peculiar feature of the electrode reaction is the reversible formation of μm-sized Cu crystals during cycling, despite its large theoretical volume change (75%). Here, the dynamic microstructural evolution of CuS cathodes in SSBs is studied using in situ synchrotron X-ray tomography. The formation of μm-sized Cu within the CAM particles can be clearly followed. This process is accompanied by crack formation that can be prevented by increasing the stack pressure from 26 to 40 MPa. Both the Cu inclusions and cracks show a preferential orientation perpendicular to the cell stack pressure, which can be a result of a z-oriented expansion of the CAM particles during lithiation. In addition, cycling leads to a z-oriented reversible displacement of the cathode pellet, which is linked to the plating/stripping of the Li counter electrode. The pronounced structural changes cause pressure changes of up to 6 MPa within the cell, as determined by operando stack pressure measurements. Reasons for the reversibility of the electrode reaction are discussed and are attributed to the favorable combination of soft materials. KW - Copper sulfide KW - Crack evolution KW - Digital volume correlation KW - Phase transformation KW - Solid-state batteries PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564577 DO - https://doi.org/10.1002/aenm.202203143 IS - 2203143 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-56457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Van Tran, K. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Abou-Ras, D. A1 - Puplampu, S. A1 - Förster, C. A1 - Penumadu, D. A1 - Dahlberg, C. F. O. A1 - Banhart, J. A1 - Manke, I. T1 - Torsion of a rectangular bar: Complex phase distribution in 304L steel revealed by neutron tomography N2 - Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale. KW - Neutron tomography KW - Phase distribution KW - Rectangular cross-section KW - Torsion KW - Geometrical effect PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561649 DO - https://doi.org/10.1016/j.matdes.2022.111037 SN - 0264-1275 VL - 222 SP - 111037 PB - Elsevier Ltd. AN - OPUS4-56164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tran, K. V. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Abou-Ras, D. A1 - Puplampu, S. A1 - Förster, C. A1 - Penumadu, D. A1 - Dahlberg, C. F. O. A1 - Banhart, J. A1 - Manke, I. T1 - Torsion of a rectangular bar: Complex phase distribution in 304L steel revealed by neutron tomography N2 - Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale. KW - Neutron tomography KW - Phase distribution KW - Rectangular cross-section KW - Torsion KW - Geometrical effect PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569101 DO - https://doi.org/10.1016/j.matdes.2022.111037 VL - 222 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-56910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pacheco, V. A1 - Marattukalam, J. J. A1 - Karlsson, D. A1 - Dessieux, L. A1 - Tran, K. V. A1 - Beran, P. A1 - Manke, I. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Sahlberg, M. A1 - Woracek, R. T1 - On the relationship between laser scan strategy, texture variations and hidden nucleation sites for failure in laser powder-bed fusion N2 - While laser powder-bed fusion has overcome some of the design constraints of conventional manufacturing methods, it requires careful selection of process parameters and scan strategies to obtain favorable properties. Here we show that even simple scan strategies, complex ones being inevitable when printing intricate designs, can inadvertently produce local alterations of the microstructure and preferential grain orientation over small areas – which easily remain unnoticed across the macroscale. We describe how a combined usage of neutron imaging and electron backscatter diffraction can reveal these localized variations and explain their origin within cm-sized parts. We explain the observed contrast variations by linking the neutron images to simulated data, pole figures and EBSD, providing an invaluable reference for future studies and showing that presumably minor changes of the scan strategy can have detrimental effects on the mechanical properties. In-situ tensile tests reveal that fracture occurs in a region that was re-melted during the building process. KW - Laser powder-bed fusion KW - Texture KW - Preferential orientation KW - Diffraction contrast neutron imaging KW - Bragg-edge PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568054 DO - https://doi.org/10.1016/j.mtla.2022.101614 VL - 26 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-56805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duan, K. A1 - Zhu, L. A1 - Li, M. A1 - Xiao, L. A1 - Bevilacqua, N. A1 - Eifert, L. A1 - Manke, I. A1 - Markötter, Henning A1 - Zhang, R. A1 - Zeis, R. A1 - Sui, P. -C. T1 - Multiphase and Pore Scale Modeling on Catalyst Layer of High-Temperature Polymer Electrolyte Membrane Fuel Cell N2 - Phosphoric acid as the electrolyte in high-temperature polymer electrolyte membrane fuel cell plays an essential role in ist performance and lifetime. Maldistribution of phosphoric acid in the catalyst layer (CL) may result in performance degradation. In the present study, pore-scale simulations were carried out to investigate phosphoric acid’s multiphase flow in a cathode CL. A reconstructed CL model was built using focused ion beam-SEM images, where distributions of pore, carbon support, binder, and catalyst particles can be identified. The multi-relaxation time lattice Boltzmann method was employed to simulate phosphoric Acid invading and leaching from the membrane into the CL during the membrane electrode assembly fabrication process. The predicted redistribution of phosphoric acid indicates that phosphoric acid of low viscosity or low wettability is prone to leaching into the CL. The effective transport properties and the active electrochemical active surface area (ECSA) were computed using a pore-scale model. They were subsequently used in a macroscopic model to evaluate the cell performance. A parametric study shows that cell performance first increases with increasing phosphoric acid content due to the increase of ECSA. However, further increasing phosphoric acid content results in performance degradation due to mass transfer limitation caused by acid flooding. KW - Gas diffusion layers KW - Lattice Boltzmann simulation KW - Electrochemical impedance spectra KW - Phosphoric acid KW - HT-PEFC PY - 2021 DO - https://doi.org/10.1149/1945-7111/abff03 VL - 168 IS - 5 SP - 054521 PB - IOP Science AN - OPUS4-53836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tang, F. A1 - Li, D. A1 - Liu, X. A1 - Huang, H. A1 - Wu, C. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Manke, I. A1 - Sun, F. A1 - Chen, L. T1 - Exploring optimal Li composite electrode anodes for lithium metal batteries through in situ X-ray computed tomography N2 - The uncontrolled Li dissolution/deposition dynamics and rapid Li pulverizations hinder the widespread deployment of Li metal batteries (LMB). Designing a Li composite electrode possessing a mechanically robust and lithiophilic three-dimensional (3D) framework represents a promising strategy to address these challenges. This study involves the preparation of three uniquely tailored Li-B-Mg composites using a combined metallurgical process of melting, casting, and rolling, along with the synergistic application of in situ X-ray computed tomography (CT) and post-mortem failure analysis to explore the most promising composite electrode candidate for LMBs. During the in-depth investigation, the optimal 70Li-B-Mg composite electrode stands out due to its robust skeleton fiber structure, uniform Li dissolution/deposition characteristics and high capacity of free-Li. Its promising prospects for enabling high-performance LMBs are showcased by the superior performance of the built Li||O2, Li||LiFePO4, Li||NCM622 and Li||NCM811 battery systems. This work offers a novel approach for exploring universally applicable and robust Li composite electrodes to realize high-performance LMBs using in situ CT analysis. KW - Li metal batteries KW - Li composite electrode KW - X-ray computed tomography KW - Li-B-Mg PY - 2024 DO - https://doi.org/10.1016/j.ensm.2024.103746 VL - 72 SP - 12 PB - Elsevier B.V. AN - OPUS4-61039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zheng, Y. A1 - Zhang, S. A1 - Ma, J. A1 - Sun, F. A1 - Osenberg, M. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Manke, I. A1 - Hu, Z. A1 - Cui, G. T1 - Codependent failure mechanisms between cathode and anode in solid state lithium metal batteries: mediated by uneven ion flux N2 - An in-depth understanding of the degradation mechanisms is a prerequisite for developing the nextgeneration all solid-state lithium metal battery (ASSLMB) technology. Herein, synchrotron X-ray computed tomography (SXCT) together with other probing tools and simulation method were employed to rediscover the decaying mechanisms of LiNi0.8Co0.1Mn0.1O2 (NCM)|Li6PS5Cl (LPSCl)|Li ASSLMB. It reveals that the detachment and isolation of NCM particles cause the current focusing on the remaining active regions of cathode. The extent of Li stripping and the likelihood of Li+ plating into LPSCl facing the active NCM particles becomes higher. Besides, the homogeneity of Li stripping/plating is improved by homogenizing the electrochemical reactions at the cathode side by LiZr2(PO4)3 (LZP) coating. These results suggest a codependent failure mechanism between cathode and anode that is mediated by uneven Li ion flux. This work contributes to establish a holistic understanding of the degradation mechanisms in ASSLMBs and opens new opportunities for their further optimization and evelopment. KW - Current density distribution KW - Lithium ion flux KW - Solid-state lithium metal batteries KW - Codependent failure mechanism KW - Cathode deactivation PY - 2023 DO - https://doi.org/10.1016/j.scib.2023.03.021 SN - 2095-9273 VL - 68 IS - 8 SP - 813 EP - 825 PB - Elsevier B.V. AN - OPUS4-57309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tang, F A1 - Wu, Z A1 - Yang, C A1 - Osenberg, M A1 - Hilger, A A1 - Dong, K A1 - Markötter, Henning A1 - Manke, I A1 - Sun, F A1 - Chen, L A1 - Cui, G T1 - Synchrotron X-ray tomography for rechargeable battery research: Fundamentals, setups and applications N2 - Understanding the complicated interplay of the continuously evolving electrode materials in their inherent 3D states during the battery operating condition is of great importance for advancing rechargeable battery research. In this regard, the synchrotron X-ray tomography technique, which enables non-destructive, multi-scale, and 3D imaging of a variety of electrode components before/during/after battery operation, becomes an essential tool to deepen this understanding. The past few years have witnessed an increasingly growing interest in applying this technique in battery research. Hence, it is time to not only summarize the already obtained battery-related Knowledge by using this technique, but also to present a fundamental elucidation of this technique to boost future studies in battery research. To this end, this review firstly introduces the fundamental principles and experimental Setups of the synchrotron X-ray tomography technique. After that, a user guide to ist application in battery research and examples of its applications in Research of various types of batteries are presented. The current review ends with a discussion of the future opportunities of this technique for next-generation rechargeable batteries research. It is expected that this review can enhance the reader’s understanding of the synchrotron X-ray tomography technique and stimulate new ideas and opportunities in battery research. KW - 3D imaging KW - Batteries KW - Synchrotron X-Ray KW - Tomography PY - 2021 DO - https://doi.org/10.1002/smtd.202100557 VL - 5 IS - 9 SP - 2100557 PB - Wiley-VCH AN - OPUS4-53394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohseninia, A A1 - Eppler, M A1 - Kartouzian, D A1 - Markötter, Henning A1 - Kardjilov, N A1 - Wilhelm, F A1 - Scholta, J A1 - Manke, I T1 - PTFE Content in Catalyst Layers and Microporous Layers: Effect on Performance and Water Distribution in Polymer Electrolyte Membrane Fuel Cells N2 - This work describes the effects of catalyst layers (CLs) consisting of hydrophobic PTFE on the performance and water management of PEM fuel cells. Catalyst inks with various PTFE contents were coated on Nafion membranes and characterized using contact angle measurements, SEX-EDX, and mercury porosimetry. Fuel cell tests and electrochemical impedance spectroscopy (EIS) were conducted under varying operating conditions for the prepared materials. At dry conditions, CLs with 5 wt.% PTFE were advantageous for cell performance due to improved membrane hydration, whereas under humid conditions and high air flow rates CLs with 10 wt.% PTFE improved the performance in high current density region. Higher PTFE contents (⩾20 wt.%) increased the mass transport resistance due to reduced porosity of the CLs structure. Operando neutron radiography was utilized to study the effects of hydrophobicity gradients within CLs and cathode microporous layer (MPLC) on liquid water distribution. More hydrophobic CLs increased the water content in adjacent layers and improved performance, especially at dry conditions. MPLC with higher PTFE contents increased the overall liquid water within the CLs and GDLs and escalated the water transfer to the anode side. Furthermore, the role of back-diffusion transport mechanism on water distribution was identified for the investigated cells. KW - Neutron imaging KW - Polymer Electrolyte Membrane Fuel Cell KW - Catalyst Layer KW - Microporous Layer KW - Water Distribution PY - 2021 DO - https://doi.org/10.1149/1945-7111/abec53 VL - 168 IS - 3 SP - 034509 PB - IOP Science AN - OPUS4-52402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kardjilov, N A1 - Manke, I A1 - Hilger, A A1 - Arlt, T A1 - Bradbury, R A1 - Markötter, Henning A1 - Woracek, R A1 - Strobel, M A1 - Treimer, W A1 - Banhart, J T1 - The Neutron Imaging Instrument CONRAD — Post‐Operational Review N2 - The neutron imaging instrument CONRAD was operated as a part of the user program of the research reactor BER‐II at Helmholtz‐Zentrum Berlin (HZB) from 2005 to 2020. The Instrument was designed to use the neutron flux from the cold source of the reactor, transported by a curved neutron guide. The pure cold neutron spectrum provided a great advantage in the use of different neutron optical components such as focusing lenses and guides, solid‐state polarizers, Monochromators and phase gratings. The flexible setup of the instrument allowed for implementation of new methods including wavelength‐selective, dark‐field, phase‐contrast and imaging with polarized neutrons. In summary, these developments helped to attract a large number of scientists and industrial customers, who were introduced to neutron imaging and subsequently contributed to the Expansion of the neutron imaging community. KW - Neutron imaging KW - Neutron scattering KW - Neutron instrument KW - Tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534190 DO - https://doi.org/10.3390/ jimaging7010011 VL - 7 IS - 11 SP - 7010011 PB - MDPI AN - OPUS4-53419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Falahat, A M A1 - Kardjilov, N A1 - Woracek, R A1 - Boin, M A1 - Markötter, Henning A1 - Kuhn, L T A1 - Makowska, M A1 - Strobl, M A1 - Pfretzschner, B A1 - Banhart, J A1 - Manke, I T1 - Temperature dependence in Bragg edge neutron transmission measurements N2 - A systematic study has been carried out to investigate the neutron transmission signal as a function of sample temperature. In particular, the experimentally determined wavelength-dependent neutron attenuation spectra for a martensitic steel at temperatures ranging from 21 to 700°C are compared with simulated data. A theoretical description that includes the Debye–Waller factor in order to describe the temperature influence on the neutron cross sections was implemented in the nxsPlotter software and used for the simulations. The analysis of the attenuation coefficients at varying temperatures shows that the missing contributions due to elastic and inelastic scattering can be clearly distinguished: while the elastically scattered intensities decrease with higher temperatures, the inelastically scattered intensities increase, and the two can be separated from each other by analysing unique sharp features in the form of Bragg edges. This study presents the first systematic approach to quantify this effect and can serve as a basis , for example, to correct measurements taken during in situ heat treatments, in many cases being a prerequisite for obtaining quantifiable results. KW - Neutron Bragg edge imaging KW - Debye–Waller factor KW - Temperature-dependent neutron transmission KW - Super martensitic stainless steel PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556896 DO - https://doi.org/10.1107/S1600576722006549 VL - 55 IS - Pt 4 SP - 919 EP - 928 PB - International Union of Crystallography AN - OPUS4-55689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, H A1 - Paulisch, M C A1 - Gebhard, M A1 - Osiewacz, J A1 - Kutter, M A1 - Hilger, A A1 - Arlt, T A1 - Kardjilov, N A1 - Ellendorff, B A1 - Beckmann, F A1 - Markötter, Henning A1 - Luik, M A1 - Turek, T A1 - Manke, I A1 - Roth, C T1 - Development of a Modular Operando Cell for X-ray Imaging of Strongly Absorbing Silver-Based Gas Diffusion Electrodes N2 - Metal-based gas diffusion electrodes are utilized in chlor-alkali electrolysis or electrochemical reduction of carbon dioxide, allowing the reaction to proceed at high current densities. In contrast to planar electrodes and predominantly 2D designs, the industrially required high current densities can be achieved by intense contact between the gas and liquid phase with the catalytically active surfaces. An essential asset for the knowledge-based design of tailored electrodes is therefore in-depth information on electrolyte distribution and intrusion into the electrode’s porous structure. Lab-based and synchrotron radiography allow for monitoring this process operando. Herein, we describe the development of a cell design that can be modularly adapted and successfully used to monitor both the oxygen reduction reaction and the electrochemical reduction of CO2 as exemplary and currently very relevant examples of gas-liquid reactions by only minor modifications to the cell set-up. With the reported cell design, we were able to observe the electrolyte distribution within the gas diffusion electrode during cell operation in realistic conditions. KW - X-Ray imaging KW - Gas diffusion electrodes KW - Operando cell PY - 2022 DO - https://doi.org/10.1149/1945-7111/ac6220 VL - 169 IS - 4 SP - 044508 PB - IOP science AN - OPUS4-55027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -