TY - JOUR A1 - Scherb, Tobias A1 - Kimber, S. A. J. A1 - Stephan, Christiane A1 - Henry, P. F. A1 - Schumacher, G. A1 - Escolástico, S. A1 - Serra, J. M. A1 - Seeger, J. A1 - Just, J. A1 - Hill, A.H. A1 - Banhart, J. T1 - Nanoscale order in the frustrated mixed conductor La5.6WO12-Delta N2 - This article reports a comprehensive investigation of the average and local structure of La5.6WO12-δ, which has excellent mixed proton, electron and oxide ion conduction suitable for device applications. Synchrotron X-ray and neutron powder diffraction show that a cubic fluorite supercell describes the average structure, with highly disordered lanthanum and oxide positions. On average, the tungsten sites are sixfold coordinated and a trace [3.7 (1.3)%] of anti-site disorder is detected. In addition to sharp Bragg reflections, strong diffuse neutron scattering is observed, which hints at short-range order. Plausible local configurations are considered and it is shown that the defect chemistry implies a simple 'chemical exchange' interaction that favours ordered WO6 octahedra. The local model is confirmed by synchrotron X-ray pair distribution function analysis and EXAFS experiments performed at the La K and W L-3 edges. It is shown that ordered domains of similar to 3.5 nm are found, implying that mixed conduction in La5.6WO12-δ is associated with a defective glassy-like anion sublattice. The origins of this ground state are proposed to lie in the nonbipartite nature of the face-centred cubic lattice and the pairwise interactions which link the orientation of neighbouring octahedral WO6 sites. This 'function through frustration' could provide a means of designing new mixed conductors. KW - neutron diffraction KW - x-ray diffraction KW - proton conductors PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366756 DO - https://doi.org/10.1107/S1600576716006415 SN - 1600-5767 VL - 49 IS - Issue 3 SP - 997 EP - 1008 PB - International Union of Crystallography CY - Chester, UK AN - OPUS4-36675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arlt, Tobias A1 - Klages, M. A1 - Messerschmidt, M. A1 - Riesemeier, Heinrich A1 - Scholta, J. A1 - Banhart, J. A1 - Manke, I. T1 - Influence of artificial aging of gas diffusion layers on the water management of PEM fuel cells N2 - The influence of artificial aging of gas diffusion layers (GDL) on the water management within the GDL was investigated in-operando by synchrotron X-ray radiography. One GDL was subjected to an accelerated aging procedure in 30% H2O2 solution, while another GDL was pristine. Radiographic measurements were combined with temporally resolved electrical analyzes. Significant differences in cell voltage and water accumulation were observed during cell operation at steady-state conditions. The cell which contained the aged GDL featured a higher water amount especially at the anode side and a lower cell voltage. KW - Degradation KW - Liquid water PY - 2014 DO - https://doi.org/10.1149/2.004402eel SN - 2162-8726 VL - 3 IS - 2 SP - F7 EP - F9 PB - ECS CY - Pennington, NJ, USA AN - OPUS4-32410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, Y. A1 - Schumacher, G. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Change in atomic coordination in a heavily deformed metallic glass N2 - The local structure around Ni and La atoms in Al85Ni10La5 amorphous powder after ball milling was investigated by X-ray absorption spectroscopy. A continuous decrease in coordination number of Ni and La as a function of milling time was observed, while the nearest neighbour distance and the mean square atomic displacement did not change, pointing at the creation of free volume around the Ni and La atoms. These structural changes resemble those of a liquid upon temperature increase. The results are described by a shear band model in which the coordination numbers of Ni and La are different within and outside a shear band. KW - X-ray-diffraction KW - Shear bands KW - Electron-irradiation KW - Positron lifetime KW - Structural model KW - Amorphous-alloys KW - Deformation KW - Temperature KW - EXAFS KW - State PY - 2014 DO - https://doi.org/10.1063/1.4879682 SN - 0021-8979 SN - 1089-7550 VL - 115 IS - 20 SP - 203510-1 EP - 203510-8 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-32409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arlt, Tobias A1 - Manke, I. A1 - Wippermann, K. A1 - Schröder, A. A1 - Mergel, J. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Röntgen-Kanten-Tomografie und -Radiografie zur Untersuchung von Alterungseffekten in Brennstoffzellenmaterialien KW - Resolution neutron-radiography KW - Local current distribution KW - Water transport KW - Carbon-dioxide KW - Methanol KW - Platinum KW - Oxidation PY - 2010 SN - 0025-5300 VL - 52 IS - 10 SP - 692 EP - 697 PB - Hanser CY - München AN - OPUS4-23045 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manke, I. A1 - Hartnig, C. A1 - Kardjilov, N. A1 - Riesemeier, Heinrich A1 - Goebbels, Jürgen A1 - Kuhn, R. A1 - Krüger, P. A1 - Banhart, J. T1 - In situ synchrotron X-ray radiography investigations of water transport in PEM fuel cells N2 - Water transport in an operating PEM fuel cell was investigated with synchrotron X-ray radiography with a spatial resolution of 3 µm and a temporal resolution of 5 s. This method allows for the detection of water accumulations with less than 10 µm diameter. We demonstrate that synchrotron X-ray imaging can dramatically expand the possibilities of imaging with high spatial and time resolution, especially as a complement to neutron radiography. Water transport processes from the first appearance of small water accumulations in the gas diffusion layer to their transport into the channel system were analysed in situ. Correlations between local effects such as water formation and operating conditions of the whole system, e.g. power variations, were found. A recently described eruptive water transport mechanism is analysed in detail. KW - Fuel cell KW - Gas diffusion layer KW - Imaging KW - Synchrotron KW - X-ray radiography KW - Two-phase flow KW - Water transport PY - 2010 DO - https://doi.org/10.1002/fuce.200800123 SN - 1615-6846 SN - 1615-6854 VL - 10 IS - 1 SP - 26 EP - 34 PB - Wiley-VCH CY - Weinheim AN - OPUS4-22730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zabler, S. A1 - Rueda, A. A1 - Rack, A. A1 - Riesemeier, Heinrich A1 - Zaslansky, P. A1 - Manke, I. A1 - Garcia-Moreno, F. A1 - Banhart, J. T1 - Coarsening of grain-refined semi-solid Al-Ge32 alloy: X-ray microtomography and in situ radiography KW - Microtomography KW - Radiography KW - 2D/3D imageanalysis KW - Technical binary alloys KW - LSW PY - 2007 DO - https://doi.org/10.1016/j.actamat.2007.05.028 SN - 1359-6454 SN - 1873-2453 VL - 55 IS - 15 SP - 5045 EP - 5055 PB - Elsevier Science CY - Kidlington AN - OPUS4-20583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hartnig, C. A1 - Manke, I. A1 - Schloesser, J. A1 - Krüger, P. A1 - Kuhn, R. A1 - Riesemeier, Heinrich A1 - Wippermann, K. A1 - Banhart, J. T1 - High resolution synchrotron X-ray investigation of carbon dioxide evolution in operating direct methanol fuel cells N2 - The carbon dioxide evolution and bubble formation in an operating fuel has been studied by means of synchrotron X-ray radiography. Two different observation directions have been chosen: a through-plane insight has been employed to track the formation of bubbles starting at the corner of the lands of the flow field; a depth profile of the carbon dioxide evolution has been derived from cross sectional studies describing an affected area of up to 100 µm. The dynamics of the bubble formation and detachment of the bubbles from the position of formation is strongly correlated with the current density. Cracks and breaks in the catalyst layer which result from the preparation process are visible under operating conditions and a possible swelling of the catalyst layer does not reach a complete vanishing of the cracks. KW - DMFC KW - Carbon dioxide evolution KW - Synchrotron radiography KW - In situ study KW - Cross section KW - Through-plane PY - 2009 DO - https://doi.org/10.1016/j.elecom.2009.05.047 SN - 1388-2481 VL - 11 IS - 8 SP - 1559 EP - 1562 PB - Elsevier CY - Amsterdam AN - OPUS4-20577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maier, W. A1 - Arlt, Tobias A1 - Wannek, C. A1 - Manke, I. A1 - Riesemeier, Heinrich A1 - Krüger, P. A1 - Scholta, J. A1 - Lehnert, W. A1 - Banhart, J. A1 - Stolten, D. T1 - In-situ synchrotron X-ray radiography on high temperature polymer electrolyte fuel cells N2 - In contrast to classical low temperature polymer electrolyte fuel cells (LT-PEFCs), the membrane conductivity in high temperature polymer electrolyte fuel cells (HT-PEFCs) (operating temperature ~ 160 °C) is based on proton transport within phosphorus-oxygen acids at different levels of hydration, orthophosphoric acid (H3PO4) being the simplest example. We present for the first time in-situ synchrotron X-ray radiography measurements applied to a HT-PEFC to gain insight into the local composition of the membrane electrode assembly (MEA) under dynamic operating conditions. Transmission changes during the radiographic measurements exhibit a clear influence of the formation of product water on the membrane composition. KW - HT-PEFC KW - Synchrotron x-ray radiography KW - Membrane electrode assembly (MEA) KW - Phosphoric acid PY - 2010 DO - https://doi.org/10.1016/j.elecom.2010.08.002 SN - 1388-2481 VL - 12 IS - 10 SP - 1436 EP - 1438 PB - Elsevier CY - Amsterdam AN - OPUS4-23962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tötzke, C. A1 - Manke, I. A1 - Hartnig, C. A1 - Kuhn, R. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Investigation of carbon fiber gas diffusion layers by means of synchrotron X-ray tomography N2 - The 3-dimensional spatial distribution of liquid water in different gas diffusion layer (GDL) materials was analyzed using synchrotron X-ray tomography. The capability of the method was demonstrated by virtually separating the GDL components in order to facilitate individual analysis of fiber material, liquid water and gas filled pore spaces. The influence of hydrophobic surface treatment on the water distribution in the GDL was illustrated by analyzing three GDL materials with different degrees of hydrophobicity. In the least hydrophobic sample, liquid water tends to form larger clusters which stretch out about several hundred µm inside the porous GDL. In contrast, only small water clusters were found in the strongly hydrophobic material with high Polytetrafluoroethylene (PTFE)-content as the liquid is partially pressed out of the GDL. Additionally, the influence of fiber orientation on the water distribution in the felt material was demonstrated. KW - Synchrotron X-ray tomography KW - Fuel cell KW - Gas diffusion layer (GDL) materials KW - Analysis of fiber material PY - 2011 DO - https://doi.org/10.1149/1.3635571 SN - 1938-6737 SN - 1938-5862 VL - 41 IS - 1 SP - 379 EP - 386 CY - Pennington, NJ, USA AN - OPUS4-25348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arlt, Tobias A1 - Manke, I. A1 - Wippermann, K. A1 - Riesemeier, Heinrich A1 - Mergel, J. A1 - Banhart, J. T1 - Investigation of the local catalyst distribution in an aged direct methanol fuel cell MEA by means of differential synchrotron X-ray absorption edge imaging with high energy resolution N2 - Synchrotron X-ray absorption edge imaging with high energy resolution was applied to study aging of fuel cell catalyst materials. The combination of an imaging and a high X-ray energy resolution set-up allows acquiring spatially resolved XAS (XANES and EXAFS) spectra. We analyzed the two-dimensional distribution of Pt and Ru in fresh and aged fuel cell catalysts. Spatially resolved XAS images were taken at the RuK edge and at the PtL3 edge. Taking radiographs above and below the absorption edges provides quantitative information about the thickness of the catalytic materials and additional chemical information. A strong influence of the flow field channels and the structure of the gas diffusion layers on the thicknesses of the catalytic elements were found: a thinner catalyst layer was found below the ribs of the flow field geometries as well as under crossing points of fiber bundles of the woven gas diffusion layers. KW - XAS KW - X-ray energy edge KW - Membrane electrode assembly KW - Direct methanol fuel cell KW - Aging mechanism KW - X-ray synchrotron radiography PY - 2013 DO - https://doi.org/10.1016/j.jpowsour.2012.08.038 SN - 0378-7753 VL - 221 SP - 210 EP - 216 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-27372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -