TY - JOUR A1 - Müller, Bernd R. A1 - Cooper, R.C. A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Wheeler, M. A1 - Hentschel, Manfred P. A1 - Staude, Andreas A1 - Pandey, A. A1 - Shyam, A. A1 - Bruno, Giovanni T1 - Stress-induced microcrack density evolution in β-eucryptite ceramics: Experimental observations and possible route to strain hardening N2 - In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measure the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. The mechanisms proposed would allow the development of a strain hardening route in ceramics. KW - Beta-eucryptite KW - Microcracked ceramics KW - X-ray refraction KW - Tensile load KW - Strain hardening KW - Synchrotron KW - BAMline KW - Computed Tomography KW - CT PY - 2018 UR - http://www.sciencedirect.com/science/article/pii/S1359645417308881 DO - https://doi.org/10.1016/j.actamat.2017.10.030 SN - 1359-6454 SN - 1873-2453 VL - 144 IS - Supplement C SP - 627 EP - 641 PB - Elsevier B.V. AN - OPUS4-43024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schob, D. A1 - Sagradov, I. A1 - Roszak, R. A1 - Sparr, H. A1 - Franke, R. A1 - Ziegenhorn, M. A1 - Kupsch, Andreas A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Experimental determination and numerical simulation of material and damage behaviour of 3D printed polyamide 12 under cyclic loading N2 - The material and damage behaviour of additively manufactured polyamide 12 under cyclic loading was characterized by cyclic tests and microstructure analysis by using microscopy, X-ray refraction, and computed tomography. The results were used to determine parameters for the viscoplastic material model by Chaboche and a damage model by Gurson-Tvergaard-Needleman. The temperature was monitored during the experiments and the self-heating effect was observed. By including this effect, a higher accuracy could be achieved with the results of mechanical experiments. KW - 3D printing Polyamide 12 KW - Chaboche model KW - GTN model KW - Material and damage behaviour KW - X-ray refraction KW - Computed tomography PY - 2020 DO - https://doi.org/10.1016/j.engfracmech.2019.106841 SN - 0013-7944 VL - 229 SP - 106841-1 EP - 106841-13 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Haußmann, J. A1 - Alink, R. A1 - Dittmann, K. A1 - Tötzke, C. A1 - Krüger, P. A1 - Klages, M. A1 - Arlt, Tobias A1 - Müller, Bernd R. A1 - Riesemeier, Heinrich A1 - Scholta, J. A1 - Gerteisen, D. A1 - Manke, I. A1 - Banhart, J. T1 - Investigation of fuel cell materials and liquid water transport by means of synchrotron imaging N2 - Synchrotron imaging allows addressing various important issues in fuel cell research, for example water distribution and transport. The water distribution in polymer electrolyte membrane fuel cells (PEMFCs) was observed quasi in-situ directly after operation by means of synchrotron tomography. The 3D data set was compared with the tomogram of a dry cell in order to separate the water distribution from cell materials. Engineered transport pathways realized by perforating holes through the gas diffusion layer (GDL) are a recent approach to optimize water transport and cell performance. For some parameter sets a cell performance increase and an improvement of stabilization have already been proven. We present high resolution investigations of the water distribution in perforated GDLs of operating PEMFCs by means of in-situ synchrotron radiography. The surrounding areas of the holes exhibited a distinct hydrophilic character. KW - Gas-diffusion layers KW - Resolution neutron-radiography KW - X-ray radiography KW - Visualization KW - PEMFC PY - 2013 DO - https://doi.org/10.1149/04529.0195ecst SN - 1938-6737 SN - 1938-5862 VL - 45 IS - 29 SP - 195 EP - 202 CY - Pennington, NJ, USA AN - OPUS4-30545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Schob, D. A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Sagradov, I. A1 - Roszak, R. A1 - Sparr, H. A1 - Franke, R. A1 - Ziegenhorn, M. A1 - Bruno, Giovanni T1 - Bestimmung der Mikrostruktur und Simulation des Schädigungsverhaltens von lasergesintertem Polyamid 12 unter quasistatischer Zugbelastung N2 - Um das Material- und Schädigungsverhalten von additiv gefertigtem Polyamid 12 (PA12) unter quasistatischer Belastung zu charakterisieren, wurden mechanische Tests und Röntgenverfahren zur Bestimmung der Mikrostruktur eingesetzt. Die Proben wurden nach dem Prinzip des Selektiven Lasersinterns (SLS) hergestellt. Unter quasistatischer Belastung mit Haltezeiten ergab sich ein viskoplastisches Materialverhalten. Im Zugversuch wurde eine maximale Zugfestigkeit von 40.6 MPa und eine Bruchdehnung von 7.4% beobachtet. Mittels Röntgenrefraktion wurde eine Erhöhung von inneren Oberflächen beobachtet, die senkrecht zur Zugrichtung orientiert sind. Die Analyse der Gesamtporosität aus Computertomographie-Messungen ergab keine Änderung infolge der Zugbelastung. Jedoch wurde eine bimodale Porengrößenverteilung und eine steigende Sphärizität festgestellt. Das Materialverhalten wurde mit dem Chaboche-Modell simuliert und ergab eine sehr gute Übereinstimmung mit den experimentellen Ergebnissen. Allerdings gestattet dieses Modell nicht, das Schädigungsverhalten abzubilden. Daher wurde zur Simulation des Schädigungsverhaltens das Modell gemäß dem Ansatz von Gurson, Tvergaard und Needleman unter Berücksichtigung der mikrostrukturellen Parameter erweitert. Der Schwerpunkt des Beitrags liegt auf den Röntgenverfahren zur experimentellen Bestimmung der Mikrostruktur. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Additive Fertigung (AM) KW - Polyamid 12 KW - Röntgenrefraktion KW - Computertomographie KW - Numerische Simulation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526833 UR - https://jahrestagung.dgzfp.de/Portals/jt2021/bb/P16.pdf SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-52683 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schob, D. A1 - Roszak, R. A1 - Sagradov, I. A1 - Sparr, H. A1 - Ziegenhorn, M. A1 - Kupsch, Andreas A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Experimental determination and numerical simulation of material and damage behaviour of 3D printed polyamide 12 under quasi-static loading N2 - In order to characterise the material and damage behaviour of additively manufactured polyamide 12 (PA12) under quasi-static load and to implement it in a numerical model, experiments under quasi-static load as well as microstructural investigations were carried out. Selective laser sintering (SLS) was used as the manufacturing process. For the classification of the material behaviour, quasi-static cyclic tests with holding times as well as tensile tests were performed. X-ray refraction and computed tomography (CT) were used to investigate the damage behaviour. The Chaboche model, which has already been applied for metallic materials under thermomechanical loading, served as the basis for the selection of the numerical material model. The same procedure was used for the selection of the damage model, where the Gurson–Tvergaard–Needleman (GTN) model was chosen, which was already used for porous metallic materials. The Chaboche model shows very good agreement with experimental results. Furthermore, the coupling with the GTN model allows a very good modelling of the damage behaviour. Finally, it could be shown that the selected models are suitable to simulate the material and damage behaviour of 3D printed PA12. KW - Polyamide 12 KW - 3D printing KW - Viscoplastic KW - Chaboche model KW - Damage KW - GTN model KW - X-ray refraction KW - Computed tomography PY - 2019 DO - https://doi.org/10.24423/aom.3162 SN - 0373-2029 VL - 71 IS - 4-5 SP - 507 EP - 526 PB - IPPT PAN - Polish Academy of Sciences, Institute of Fundamental Technological Research CY - Warsaw AN - OPUS4-49409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nellesen, J. A1 - Laquai, René A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Hentschel, M. P. A1 - Anar, N. B. A1 - Soppa, E. A1 - Tillmann, W. A1 - Bruno, Giovanni T1 - In situ analysis of damage evolution in an Al/Al2O3 MMC under tensile load by synchrotron X-ray refraction imaging N2 - The in situ analysis of the damage evolution in a metal Matrix composite (MMC) using synchrotron X-ray refraction radiography (SXRR) is presented. The investigated material is an Al alloy (6061)/10 vol% Al2O3 MMC after T6 heat treatment. In an interrupted tensile test the gauge section of dog bone-shaped specimens is imaged in different states of tensile loading. On the basis of the SXRR images, the relative change of the specific surface (proportional to the amount of damage) in the course of tensile loading was analyzed. It could be shown that the damage can be detected by SXRR already at a stage of tensile loading, in which no Observation of damage is possible with radiographic absorption-based imaging methods. Moreover, the quantitative analysis of the SXRR images reveals that the amount of damage increases homogeneously by an average of 25% with respect to the Initial state. To corroborate the experimental findings, the damage distribution was imaged in 3D after the final tensile loading by synchrotron X-ray refraction computed tomography (SXRCT) and absorption-based synchrotron X-ray computed tomography (SXCT). It could be evidenced that defects and damages cause pronounced indications in the SXRCT images. KW - Composite materials KW - Defects KW - Micro analysis PY - 2018 DO - https://doi.org/10.1007/s10853-017-1957-x SN - 0022-2461 SN - 1573-4803 VL - 53 IS - 8 SP - 6021 EP - 6032 PB - Springer US AN - OPUS4-44241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tötzke, C. A1 - Gaiselmann, G. A1 - Osenberg, M. A1 - Bohner, J. A1 - Arlt, Tobias A1 - Markötter, Henning A1 - Hilger, A. A1 - Wieder, F. A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. A1 - Banhart, J. A1 - Schmidt, V. A1 - Lehnert, W. A1 - Manke, I. T1 - Three-dimensional study of compressed gas diffusion layers using synchrotron X-ray imaging N2 - We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets. KW - Synchrotron X-ray tomography KW - Gas diffusion layer (GDL) KW - Microstructure KW - Water transport path KW - Pore size analysis KW - Geometrical tortuosity PY - 2014 DO - https://doi.org/10.1016/j.jpowsour.2013.12.062 SN - 0378-7753 VL - 253 SP - 123 EP - 131 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-29979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tötzke, C. A1 - Gaiselmann, G. A1 - Osenberg, M. A1 - Arlt, Tobias A1 - Markötter, Henning A1 - Hilger, A. A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Schmidt, V. A1 - Lehnert, W. A1 - Manke, I. T1 - Influence of hydrophobic treatment on the structure of compressed gas diffusion layers N2 - Carbon fiber based felt materials are widely used as gas diffusion layer (GDL) in fuel cells. Their transport properties can be adjusted by adding hydrophobic agents such as polytetrafluoroethylene (PTFE). We present a synchrotron X-ray tomographic study on the felt material Freudenberg H2315 with different PTFE finishing. In this study, we analyze changes in microstructure and shape of GDLs at increasing degree of compression which are related to their specific PTFE load. A dedicated compression device mimicking the channel-land pattern of the flowfield is used to reproduce the inhomogeneous compression found in a fuel cell. Transport relevant geometrical parameters such as porosity, pore size distribution and geometric tortuosity are calculated and consequences for media transport discussed. PTFE finishing results in a marked change of shape of compressed GDLs: surface is smoothed and the invasion of GDL fibers into the flow field channel strongly mitigated. Furthermore, the PTFE impacts the microstructure of the compressed GDL. The number of available wide transport paths is significantly increased as compared to the untreated material. These changes improve the transport capacity liquid water through the GDL and promote the discharge of liquid water droplets from the cell. KW - Gas diffusion layer KW - Synchrotron Tomography KW - Compression KW - Hydrophobic treatment KW - Water transport PY - 2016 DO - https://doi.org/10.1016/j.jpowsour.2016.05.118 SN - 0378-7753 VL - 324 SP - 625 EP - 636 PB - Elsevier CY - Amsterdam AN - OPUS4-36918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wonneberger, R. A1 - Gräf, S. A1 - Bonse, Jörn A1 - Wisniewski, W. A1 - Freiberg, K. A1 - Hafermann, M. A1 - Ronning, C. A1 - Müller, F. A. A1 - Undisz, A. T1 - Tracing the Formation of Femtosecond Laser-Induced Periodic Surface Structures (LIPSS) by Implanted Markers N2 - The generation of laser-induced periodic surface structures (LIPSS) using femtosecond lasers facilitates the engineering of material surfaces with tailored functional properties. Numerous aspects of their complex formation process are still under debate, despite intensive theoretical and experimental research in recent decades. This particularly concerns the challenge of verifying approaches based on electromagnetic effects or hydrodynamic processes by experiment. In the present study, a marker experiment is designed to conclude on the formation of LIPSS. Well-defined concentration depth profiles of 55Mn+- and 14N+-ions were generated below the polished surface of a cast Mn- and Si-free stainless steel AISI 316L using ion implantation. Before and after LIPSS generation, marker concentration depth profiles and the sample microstructure were evaluated by using transmission electron microscopy techniques. It is shown that LIPSS predominantly formed by material removal through locally varying ablation. Local melting and resolidification with the redistribution of the material occurred to a lesser extent. The experimental design gives quantitative access to the modulation depth with a nanometer resolution and is a promising approach for broader studies of the interactions of laser beams and material surfaces. Tracing LIPSS formation enables to unambiguously identify governing aspects, consequently guiding the path to improved processing regarding reproducibility, periodicity, and alignment. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser processing KW - Ion implantation KW - Transmission Electron Microscopy (TEM) KW - Stainless steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623990 DO - https://doi.org/10.1021/acsami.4c14777 SN - 1944-8244 (Print) SN - 1944-8252 (Online) VL - 17 IS - 1 SP - 2462 EP - 2468 PB - ACS Publications AN - OPUS4-62399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Götschel, S. A1 - Maierhofer, Christiane A1 - Müller, Jan P. A1 - Rothbart, Nick A1 - Weiser, M. T1 - Quantitative defect reconstruction in active thermography for fiber-reinforced composites N2 - Carbon-fiber reinforced composites are becoming more and more important in the production of light-weight structures, e.g., in the automotive and aerospace industry. Thermography is often used for non-destructive testing of These products, especially to detect delaminations between different layers of the composite. In this presentation, we aim at methods for defect reconstruction from thermographic measurements of such carbon-fiber reinforced composites. The reconstruction results shall not only allow to locate defects, but also give a quantitative characterization of the defect properties. We discuss the simulation of the measurement process using finite element methods, as well as the experimental validation on flat bottom holes. Especially in pulse thermography, thin boundary layers with steep temperature gradients occurring at the heated surface need to be resolved. Here we use the combination of a 1D analytical solution combined with numerical solution of the remaining defect equation. We use the simulations to identify material Parameters from the measurements. Finally, fast heuristics for reconstructing defect geometries are applied to the acquired data, and compared for their accuracy and utility in detecting different defects like back surface defects or delaminations. T2 - 19th World Conference on Non-Destructive Testing 2016 CY - München, Germany DA - 13.06.2016 KW - Active thermography KW - Numerical simulation KW - Time-resolved thermogram KW - Thermal wave PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366644 UR - https://www.wcndt2016.com/Programme/show/Th-4-C-4 VL - 2016 SP - Th.4.C.4-1 EP - Th.4.C.4-10 AN - OPUS4-36664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eichelbaum, M. A1 - Rademann, K. A1 - Müller, Ralf A1 - Radtke, Martin A1 - Görner, Wolf T1 - Zur Chemie des Goldes in Silicatgläsern: Untersuchungen zum nicht-thermisch aktivierten Wachstum von Goldclustern KW - Glas KW - Goldcluster KW - Nanophotonik PY - 2005 DO - https://doi.org/10.1002/ange.200502174 SN - 0044-8249 SN - 0932-2140 SN - 1521-3757 VL - 117 IS - 48 SP - 8118 EP - 8122 PB - Wiley-VCH CY - Weinheim AN - OPUS4-7691 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -