TY - JOUR A1 - Grothausmann, R. A1 - Manke, I. A1 - Zehl, G. A1 - Dorbandt, I. A1 - Bogdanoff, P. A1 - Fiechter, S. A1 - Hentschel, Manfred P. A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Hilger, A. T1 - Charakterisierung von Katalysatormaterialien für Brennstoffzellen mittels Elektronentomografie JF - MP materials testing N2 - Zur Optimierung moderner Katalysatoren für Brennstoffzellen werden diese elektronen-tomografisch charakterisiert. Die Elektronentomografie ermöglicht einzigartige Einblicke in die Nanometer-Strukturen der metallischen Katalysatorpartikel, die auf einem elektrisch leitenden, inerten Kohlenstoffträger abgeschieden werden. Die dreidimensional bildgebende Methode ermöglicht über qualitative Untersuchungen hinaus detaillierte quantitative Form- und Strukturanalysen der Katalysatormaterialien. So werden beispielsweise die Positionen der Katalysatorpartikel relativ zum Trägermaterial analysiert. Ihre Form und Einbettung in den Träger, welche die für die katalytische Reaktion maßgebliche "freie Oberfläche" definieren, werden bestimmt. Die Elektronentomografie ermöglicht somit quantitative Vergleiche zwischen verschiedenen Katalysatormaterialien und Herstellungsverfahren. Sie erweitert die Möglichkeiten der Korrelation gewünschter elektrochemischer Eigenschaften mit der Nanostruktur dieser Materialien und macht so weitere Optimierungen der Katalysatormaterialien möglich. KW - Computed tomography KW - Reconstruction algorithm KW - Electron tomography KW - Catalyst KW - Fuel cell PY - 2010 SN - 0025-5300 VL - 52 IS - 10 SP - 706 EP - 711 PB - Hanser CY - München AN - OPUS4-22072 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grothausmann, R. A1 - Zehl, G. A1 - Manke, I. A1 - Fiechter, S. A1 - Bogdanoff, P. A1 - Dorbandt, I. A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Schumacher, G. A1 - Banhart, J. T1 - Nanometer-Tomographie: kleinste Katalysatorteilchen erblicken - Mit Elektronen und Computern die mobile Brennstoffzelle erforschen JF - Materials and corrosion KW - Electron tomography KW - Polymer electrolyte membrane fuel cell (PEMFC) KW - Reconstruction algorithm KW - DIRECTT PY - 2012 DO - https://doi.org/10.1002/maco.201290007 SN - 0947-5117 SN - 1521-4176 VL - 63 IS - 2 SP - 1 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-26348 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grothausmann, R. A1 - Zehl, G. A1 - Manke, I. A1 - Fiechter, S. A1 - Bogdanoff, P. A1 - Dorbandt, I. A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Schumacher, G. A1 - Banhart, J. T1 - Quantitative structural assessment of heterogeneous catalysts by electron tomography JF - Journal of the American chemical society N2 - We present transmission electron microscope (TEM) tomography investigations of ruthenium-based fuel cell catalyst materials as employed in direct methanol fuel cells (DMFC). The digital three-dimensional representation of the samples not only enables detailed studies on number, size, and shape but also on the local orientation of the ruthenium particles to their support and their freely accessible surface area. The shape analysis shows the ruthenium particles deviate significantly from spherical symmetry which increases their surface to volume ratio. The morphological studies help to understand the structure formation mechanisms during the fabrication as well as the high effectiveness of these catalysts in the oxygen reduction reaction at the cathode side of fuel cells. KW - Electron tomography KW - Reconstruction algorithm KW - Catalyst KW - Fuel cell PY - 2011 DO - https://doi.org/10.1021/ja2032508 SN - 0002-7863 SN - 1520-5126 VL - 133 IS - 45 SP - 18161 EP - 18171 PB - American Chemical Society CY - Washington, DC AN - OPUS4-24833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Lück, S. A1 - Schmidt, V. A1 - Grothausmann, R. A1 - Hilger, A. A1 - Manke, I. T1 - Missing wedge computed tomography by iterative algorithm DIRECTT JF - Journal of microscopy N2 - A strategy to mitigate typical reconstruction artefacts in missing wedge computed tomography is presented. These artefacts appear as elongations of reconstructed details along the mean direction (i.e. the symmetry centre of the projections). Although absent in standard computed tomography applications, they are most prominent in advanced electron tomography and also in special topics of X-ray and Neutron tomography under restricted geometric boundary conditions. We investigate the Performance of the DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm to reduce the directional artefacts in standard procedures. In order to be sensitive to the anisotropic nature of missing wedge artefacts, we investigate isotropic substructures of metal foam as well as circular disc models. Comparison is drawn to filtered backprojection and algebraic techniques. Reference is made to reconstructions of complete data sets. For the purpose of assessing the reconstruction Quality, Fourier transforms are employed to visualize the missing wedge directly. Deficient reconstructions of disc models are evaluated by a length-weighted boundary orientations. The DIRECTT results are assessd at different signal-to-noise ratios by means of local and integral evaluation Parameters. KW - Tomography KW - Algorithm KW - Reconstruction KW - Computed tomography KW - Electron tomography KW - Image morphology KW - Iterative reconstruction KW - Missing wedge PY - 2016 DO - https://doi.org/10.1111/jmi.12313 SN - 1365-2818 VL - 261 IS - 1 SP - 36 EP - 45 PB - Wiley CY - Hoboken, New Jersey, USA AN - OPUS4-35801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Manke, I. A1 - Kardjilov, N. A1 - Arlt, Tobias A1 - Grothausmann, R. T1 - Rekonstruktion limitierter CT-Messdatensätze von Brennstoffzellen mit Directt JF - MP materials testing N2 - Die Aufklärung spezifischer Fragestellungen zur Funktionalität von PEM(polymer electrolyte membrane)- und DMFC(Direct Methanol)-Brennstoffzellen bedarf der 3D-Abbildung der spezifischen Komponenten mit unterschiedlichen Strahlungsarten: des Wassergehalts in den Flow Fields mit Neutronen, der Katalysator-Alterung in der MEA (membrane electrode assembly) mit Synchrotronstrahlung und der freien (reaktiven) Katalysator-Oberfläche von Nano-Partikeln mit TEM-Elektronen-Tomografie. Diese Messungen im Bereich der mm- bis nm-Skala unterliegen dabei erheblichen Restriktionen: einer ortsabhängigen Verschmierung der Neutronenradiogramme, Manipulatorinstabilitäten der Synchrotronmessungen sowie einer Kombination von Limited-View-Datensätzen, wenigen Projektionswinkeln und teilweiser Nichtdurchstrahlbarkeit in der Elektronen-CT. Die Vorteile eines fortentwickelten Directt-Algorithmus für die Bewältigung dieser Randbedingungen gegenüber gefilterten Rückprojektionen werden aufgezeigt. KW - Computed tomography KW - Reconstruction algorithm KW - Electron tomography KW - Neutron tomography KW - Catalyst KW - Fuel cell PY - 2010 SN - 0025-5300 VL - 52 IS - 10 SP - 676 EP - 683 PB - Hanser CY - München AN - OPUS4-22070 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Hentschel, Manfred P. A1 - Manke, I. A1 - Kardjilov, N. A1 - Arlt, Tobias A1 - Grothausmann, R. T1 - Reconstruction of limited computed tomography data of fuel cell components using direct iterative reconstruction of computed tomography trajectories JF - Journal of power sources N2 - CT (computed tomography) reconstructions of fuel cell components of a yet unrivaled spatial resolution and quality are presented. This is achieved by application of the novel DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm. We focus on two different key issues which essentially rule the fuel cell's durability on different length scales and physical interactions. On the resolution scale of some 100 µm agglomerations of condensed water in flow-field channels are detected by means of quasi-in situ neutron CT (after operation). Five orders of magnitude below nanometer sized Ru catalyst particles on carbon black support are visualized by electron tomography. Both types of experiments are especially adapted to the type of material involved but they are accompanied by severe deviations from ideal CT measuring conditions, as well. In order to overcome the tremendous reconstruction artifacts of standard algorithms, we employ DIRECTT which is described in detail. Comparisons of DIRECTT reconstructions to the conventional filtered back projection, prove the significant improvements in both experimental methods. KW - PEM fuel cell KW - Neutron computed tomography KW - Electron tomography KW - Reconstruction algrorithm KW - Water management KW - Catalyst PY - 2011 DO - https://doi.org/10.1016/j.jpowsour.2010.10.106 SN - 0378-7753 VL - 196 IS - 12 SP - 5293 EP - 5298 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-23589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zou, T. A1 - Nonappa, N. A1 - Khavani, M. A1 - Vuorte, M. A1 - Penttilä, P. A1 - Zitting, A. A1 - Valle-Delgado, J. J. A1 - Elert, Anna Maria A1 - Silbernagl, Dorothee A1 - Balakshin, M. A1 - Sammalkorpi, M. A1 - Österberg, M. T1 - Experimental and Simulation Study of the Solvent Effects on the Intrinsic Properties of Spherical Lignin Nanoparticles JF - The journal of physical chemistry. B N2 - Spherical lignin nanoparticles (LNPs) fabricated via nanoprecipitation of dissolved lignin are among the most attractive biomass-derived nanomaterials. Despite various studies exploring the methods to improve the uniformity of LNPs or seeking more application opportunities for LNPs, little attention has been given to the fundamental aspects of the solvent effects on the intrinsic properties of LNPs. In this study, we employed a variety of experimental techniques and molecular dynamics (MD) simulations to investigate the solvent effects on the intrinsic properties of LNPs. The LNPs were prepared from softwood Kraft lignin (SKL) using the binary solvents of aqueous acetone or aqueous tetrahydrofuran (THF) via nanoprecipitation. The internal morphology, porosity, and mechanical properties of the LNPs were analyzed with electron tomography (ET), small-angle X-ray scattering (SAXS), atomic force microscopy (AFM), and intermodulation AFM (ImAFM). We found that aqueous acetone resulted in smaller LNPs with higher uniformity compared to aqueous THF, mainly ascribing to stronger solvent−lignin interactions as suggested by MD simulation results and confirmed with aqueous 1,4-dioxane (DXN) and aqueous dimethyl sulfoxide (DMSO). More importantly, we report that both LNPs were compact particles with relatively homogeneous density distribution and very low porosity in the internal structure. The stiffness of the particles was independent of the size, and the Young’s modulus was in the range of 0.3−4 GPa. Overall, the fundamental understandings of LNPs gained in this study are essential for the design of LNPs with optimal performance in applications. KW - Lignin KW - Electron tomography KW - Intermodulation AFM KW - Modulus KW - SAXS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546948 DO - https://doi.org/10.1021/acs.jpcb.1c05319 SN - 1520-5207 VL - 125 IS - 44 SP - 12315 EP - 12328 PB - ACS AN - OPUS4-54694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -