TY - JOUR A1 - Markötter, H. A1 - Manke, I. A1 - Krüger, P. A1 - Arlt, Tobias A1 - Huassmann, J. A1 - Klages, M. A1 - Riesemeier, Heinrich A1 - Hartnig, C. A1 - Scholta, J. A1 - Banhart, J. T1 - Investigation of 3D water transport paths in gas diffusion layers by combined in-situ synchrotron X-ray radiography and tomography N2 - The three-dimensional water distribution and water transport paths in the gas diffusion layer (GDL) and the adjacent micro-porous layer (MPL) of a polymer electrolyte membrane fuel cell (PEMFC) were analyzed during cell operation. The technique of quasi in-situ X-ray tomography was used for a 3D visualization of the water distribution and the structure of the GDL at different operating conditions. Based on findings from in-situ radiographic measurements water transport paths were detected and subsequently examined by tomography. The combination of these 2D and 3D techniques allows for a fully three-dimensionally resolved visualization of transport paths through the GDL. KW - Polymer electrolyte membrane fuel cell (PEMFC) KW - Radiography KW - Tomography KW - Synchrotron X-ray imaging KW - Gas diffusion layer (GDL) KW - Water transport paths PY - 2011 DO - https://doi.org/10.1016/j.elecom.2011.06.023 SN - 1388-2481 VL - 13 IS - 9 SP - 1001 EP - 1004 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-25244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, H. A1 - Manke, I. A1 - Haußmann, J. A1 - Arlt, Tobias A1 - Klages, M. A1 - Krüger, P. A1 - Hartnig, C. A1 - Scholta, J. A1 - Müller, Bernd R. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Combined synchrotron X-ray radiography and tomography study of water transport in gas diffusion layers N2 - Synchrotron X-ray radiography and tomography investigations of a custom-made polymer electrolyte membrane fuel cell optimised for visualisation purposes are presented. The 3D water distribution and transport pathways in the porous carbon fibre gas diffusion layers (GDLs) were investigated. The authors found that water is not only moving from the GDL into the channel, but can also take the opposite way, that is, from the channel into free pore space of the GDL. Such movement of water into the opposite direction has been subject of speculations but has so far not yet been reported and might bring new insights into the general water transport behaviour, which might give new aspects to the general description of water transport processes and influence modelling assumptions to describe the process taking place in the GDL. KW - Synchrotron radiography KW - Synchrotron tomography KW - Gas diffusion layers KW - Water transport PY - 2012 DO - https://doi.org/10.1049/mnl.2012.0410 SN - 1750-0443 VL - 7 IS - 7 SP - 689 EP - 692 PB - IET CY - London AN - OPUS4-26282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, H. A1 - Alink, R. A1 - Haußmann, J. A1 - Dittmann, K. A1 - Arlt, Tobias A1 - Wieder, F. A1 - Tötzke, C. A1 - Klages, M. A1 - Reiter, C. A1 - Riesemeier, Heinrich A1 - Scholta, J. A1 - Gerteisen, D. A1 - Banhart, J. A1 - Manke, I. T1 - Visualization of the water distribution in perforated gas diffusion layers by means of synchrotron X-ray radiography N2 - Perforated gas diffusion layers (GDLs) of polymer electrolyte membrane fuel cells (PEMFCs) were investigated by means of in-situ synchrotron X-ray radiography during operation. We found a strong influence of perforations on the water distribution and transport in the investigated Toray TGP-H-090 GDL. The water occurs mainly around the perforations, while the holes themselves show varying water distributions. Some remain dry, while most of them fill up with liquid water after a certain period or might serve as drainage volume for effective water transport. KW - Polymer electrolyte membrane fuel cell (PEMFC) KW - Radiography KW - Synchrotron KW - X-ray imaging KW - Perforated gas diffusion layer (GDL) KW - Water transport PY - 2012 DO - https://doi.org/10.1016/j.ijhydene.2012.01.141 SN - 0360-3199 VL - 37 IS - 9 SP - 7757 EP - 7761 PB - Elsevier CY - Oxford AN - OPUS4-26434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, H. 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 - JOUR A1 - Markötter, H. A1 - Haußmann, J. A1 - Alink, R. A1 - Tötzke, C. A1 - Arlt, Tobias A1 - Klages, M. A1 - Riesemeier, Heinrich A1 - Scholta, J. A1 - Gerteisen, D. A1 - Banhart, J. A1 - Manke, I. T1 - Influence of cracks in the microporous layer on the water distribution in a PEM fuel cell investigated by synchrotron radiography N2 - Water evolution in the gas diffusion layer of a polymer electrolyte membrane fuel cell was visualized in situ by means of synchrotron X-ray radiography. Cracks in the microporous layer were identified as start points of efficient liquid water transfer paths through the gas diffusion layer. Quantitative analysis of the water flow rate through those arbitrarily distributed cracks into the gas channel revealed that they have a strong influence on the overall liquid water transport. This could find entry into future material design and simulation. KW - Polymer electrolyte membrane fuel cell (PEMFC) KW - Radiography KW - Synchrotron X-ray imaging KW - Microporous layer (MPL) KW - Water transport KW - Liquid water flow rate PY - 2013 DO - https://doi.org/10.1016/j.elecom.2013.04.006 SN - 1388-2481 VL - 34 SP - 22 EP - 24 PB - Elsevier CY - Amsterdam AN - OPUS4-30548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, P. A1 - Markötter, H. A1 - Klages, M. A1 - Haußmann, J. A1 - Arlt, Tobias A1 - Riesemeier, Heinrich A1 - Hartnig, C. A1 - Banhart, J. A1 - Manke, I. A1 - Scholta, J. T1 - Dreidimensionale Untersuchung der Wasserverteilung in einer Miniatur-PEM-Brennstoffzelle KW - Resolution neutron-radiography KW - Local current distribution KW - Cells KW - Quantification PY - 2010 SN - 0025-5300 VL - 52 IS - 10 SP - 712 EP - 717 PB - Hanser CY - München AN - OPUS4-23044 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Aregbe, Y. A1 - Valkiers, S. A1 - Norgaard, J. A1 - De Bièvre, P. A1 - Taylor, P.D.P. A1 - Poths, J. T1 - A primary isotopic gas standard for krypton with values for isotopic composition and molar mass traceable to the Système International d'Unités N2 - Isotope amount ratios of krypton were measured on subsamples from one large batch of high purity krypton separated from the atmosphere. Synthetic mixtures of enriched krypton isotopes were used to “calibrate” the measurements with small uncertainties. The result is a primary isotopic gas standard (PIGS) IRMM-2030 with certified values for isotope ratios, isotopic composition, and molar mass of krypton with small combined uncertainties uc, evaluated according to the ISO/BIPM Guide (GUM). It is commercially available from IRMM-Geel or from MESSER (Duisburg, D). The certified krypton isotope amount ratios in the PIGS IRMM-2030 are as follows: n(78Kr)/n(84Kr)=0.006 232 5(55), n(80Kr)/n(84Kr)=0.040 107(17), n(82Kr)/n(84Kr)=0.203 43(12), n(83Kr)/n(84Kr)=0.201 79(11), and n(86Kr)/n(84Kr)=0.303 205(59) with expanded uncertainty U=kuc and coverage factor k=2. The molar mass of Kr in this sample is M(Kr)=83.798 02(16) g/mol. These values are in good agreement with published measurements of atmospheric krypton but have smaller combined uncertainties and are “calibrated” by means of synthetic isotope mixtures. The values of the PIGS are traceable to the SI. Measurements of isotope amount ratios of krypton in other samples can be linked to SI using this PIGS. KW - Molar mass KW - Isotopic composition KW - Primary isotopic gas standard KW - Gas isotope mass spectrometry KW - Isotope amount ratio KW - Traceability KW - SI KW - Krypton PY - 2001 DO - https://doi.org/10.1016/S1387-3806(00)00397-3 SN - 0168-1176 SN - 0020-7381 SN - 1387-3806 SN - 1873-2798 VL - 206 SP - 129 EP - 136 PB - Elsevier CY - Amsterdam AN - OPUS4-1087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arlt, Tobias A1 - Manke, I. A1 - Wippermann, K. A1 - Tötzke, C. A1 - Markötter, H. A1 - Riesemeier, Heinrich A1 - Mergel, J. A1 - Banhart, J. T1 - Investigation of the three-dimensional ruthenium distribution in fresh and aged membrane electrode assemblies with synchrotron X-ray absorption edge tomography N2 - Synchrotron X-ray absorption edge imaging was used to investigate the ruthenium distribution in both fresh and aged Pt/Ru-based membrane electrode assemblies (MEA) of direct methanol fuel cells. MEAs aged in different ways were analyzed: artificially aged by MeOH depletion and aged for 1700 h in an operating fuel cell stack. An element sensitive tomographic technique – differential X-ray absorption edge tomography – was applied allowing for a 3D-visualization of the ruthenium distribution within the MEA. We found a markedly changed Ru distribution after aging which is correlated to the GDL structure, the flow field geometry, and CO2 transport in the methanol solution. KW - Edge tomography KW - Ruthenium distribution KW - Direct methanol fuel cells KW - Synchrotron X-ray KW - PtRu corrosion PY - 2011 DO - https://doi.org/10.1016/j.elecom.2011.05.013 SN - 1388-2481 VL - 13 IS - 8 SP - 826 EP - 829 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-25243 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 - 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 - 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 - 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 - 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 - Hmood, F. J. A1 - Günster, Jens A1 - Heinrich, J. T1 - Sintering and piezoelectric properties of K0.5Na0.5NbO3 glass microspheres N2 - Laser-fused K0.5Na0.5NbO3 (KNN) powder of 75% transparent fraction has been sintered by pressureless sintering, spark plasma sintering (SPS), and hot isostatic pressing (HIP). The laser-fused KNN has a fictive temperature of 503 °C and an onset crystallization temperature of around 529 °C. The results have shown that sintering of the laser-fused KNN powder utilizing the viscous flow of the transparent microspheres (amorphous content)–at the kinetic window (26 °C)–is possible. The highest yield relative density is around 83% at a sintering temperature of 525 °C and at a sintering pressure of 280 MPa. Limited density has been reached because of formation of crystalline surface layers around the amorphous areas. The samples hipped at 525 °C have low piezoelectric coefficient d33 of 5 pC/N because of the residual porosity that led to early dielectric breakdown during the polarization. The sintering behavior, the resulting microstructure as well as the measured properties will be discussed. KW - KNN KW - Glass microspheres PY - 2015 DO - https://doi.org/10.1016/j.jeurceramsoc.2015.07.035 SN - 0955-2219 SN - 1873-619X VL - 35 IS - 15 SP - 4143 EP - 4151 PB - Elsevier Ltd. CY - Oxford AN - OPUS4-34958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alrwashdeh, S. S. A1 - Markötter, H. A1 - Haußmann, J. A1 - Hilger, A. A1 - Klages, M. A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Riesemeier, Heinrich A1 - Scholta, J. A1 - Manke, I. T1 - Investigation of water transport in newly developed micro porous layers for polymer electrolyte membrane fuel cells N2 - In this investigation, synchrotron X-ray imaging was used to investigate the water distribution inside newly developed gas diffusion media in polymer electrolyte membrane fuel cells. In-situ radiography was used to reveal the relationship between the structure of the microporous layer (MPL) and the water flow in a newly developed MPL equipped with randomly arranged holes. A strong influence of these holes on the overall water transport was found. This contribution provides a brief overview to some of our recent activities on this research field. KW - Polymer electrolyte membrane fuel cell KW - Microporous layer KW - Water distribution KW - Radiography KW - Synchrotron X-ray imaging PY - 2017 DO - https://doi.org/10.9729/AM.2017.47.3.101 SN - 2287-4445 SN - 2287-5123 VL - 47 IS - 3 SP - 101 EP - 104 AN - OPUS4-43356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van der Hout, J. W. A1 - van der Veen, A. M. H. A1 - Ziel, P. R. A1 - Kipphardt, Heinrich A1 - Tuma, Dirk A1 - Maiwald, Michael A1 - Fernández, T. E. A1 - Gómez, C. A1 - Cieciora, D. A1 - Ochman, G. A1 - Dias, F. A1 - Silvino, V. A1 - Macé, T. A1 - Sutour, C. A1 - Marioni, F. A1 - Ackermann, A. A1 - Niederhauser, B. A1 - Fükő, J. A1 - Büki, T. A1 - Szilágyi, Z. N. A1 - Tarhan, T. A1 - Engin, E. T1 - International Comparison Euramet.QM-K111 – Propane in Nitrogen N2 - This key comparison aims to assess the core capabilities of the participants in gas analysis. Such competences include, among others, the capabilities to prepare Primary Standard gas Mixtures (PSMs), perform the necessary purity analysis on the materials used in the gas mixture preparation, the verification of the composition of newly prepared PSMs against existing ones, and the capability of calibrating the composition of a gas mixture. According to the Strategy for Key Comparisons of the Gas Analysis Working Group, this key comparison is classified as an RMO track A key comparison. The artefacts were binary mixtures of propane in nitrogen at a nominal amount-of-substance fraction level of 1000 μmol/mol. The values and uncertainties from the gravimetric gas mixture preparation were used as key comparison reference values (KCRVs). Each transfer standard had its own KCRV. The results are generally good. All results are within ± 1 % of the KCRV. KW - EURAMET.QM-K111 KW - Propane in nitrogen PY - 2017 DO - https://doi.org/10.1088/0026-1394/54/1A/08020 SN - 0026-1394 VL - 54 IS - Technical Supplement SP - 08020, 1 EP - 34 PB - IOP Science AN - OPUS4-44471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van der Veen, A. M H A1 - Zalewska, E. T. A1 - Kipphardt, Heinrich A1 - Beelen, R. R. A1 - Tuma, Dirk A1 - Maiwald, Michael A1 - Fükő, J. A1 - Büki, T. A1 - Szilágyi, Z. N. A1 - Beránek, J. A1 - Cieciora, D. A1 - Ochman, G. A1 - e.t al., T1 - Metrologia International Bureau of Weights and Measures (BIPM), find out more - KEY COMPARISON International comparison CCQM-K118 natural gas N2 - CCQM-K118 was an international key comparison on natural gas composition with two types of gases, i.e., a low calorific hydrogen-enriched natural gas and a high calorific LNG type of gas. There were 14 participating laboratories. The traveling standards (i.e., 14 mixtures each) were obtained from an external source and checked for homogeneity and stability before and after the participants' measurements at the two coordinating laboratories. The data evaluation was performed using a consensus value and a laboratory effect model. The results of the participants were benchmarked against a key comparison reference value computed from the largest consistent subset (LCS) of the submitted results, adjusted for the differences between the travelling standards. For the first time in a key comparison in gas analysis, the model included a term to account for excess variability in the LCS. Most of the participants reported one or a few (slightly) discrepant results. Partly this is due to the heterogeneity and heteroscedasticity of the datasets. In all, the results in this key comparison demonstrate the good comparability of the national measurement standards for natural gas composition maintained by the participating NMIs. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA). To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - CCQM-K PY - 2022 DO - https://doi.org/10.1088/0026-1394/59/1A/08017 SN - 0026-1394 VL - 59 IS - 1A PB - IOP Publishing LTD AN - OPUS4-56308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traulsen, C. H.-H. A1 - Kunz, V. A1 - Heinrich, Thomas A1 - Richter, S. A1 - Holzweber, Markus A1 - Schulz, A. A1 - von Krbek, L. K. S. A1 - Scheuschner, U. T. J. A1 - Poppenberg, J. A1 - Unger, Wolfgang A1 - Schalley, C. A. T1 - Synthesis and coordinative layer-by-layer deposition of pyridine-functionalized gold nanoparticles and tetralactam macrocycles on silicon substrates N2 - Coordination chemistry was applied to deposit pyridine-functionalized gold nanoparticles on silicon substrates. The particles were synthesized through the Brust/Schiffrin route with a subsequent ligand exchange reaction yielding well-defined particles of two different sizes. Multilayer deposition was carried out on a pyridine-terminated SAM, anchored on a hydroxyl-terminated silicon surface. Analogously, Hunter/Vögtle-type tetralactam macrocycle multilayers were deposited as well as mixed layers containing both either in an alternating sequence or as a macrocycle multilayer with a terminating nanoparticle layer. These composite layers were examined with respect to their ability to bind squaraine axles in the macrocycle cavities. The amount of guest bound is higher for the composite layer with alternating macrocycles and nanoparticles. KW - Layer-by-layer deposition KW - Functionalized Au nanoparticles KW - SEM KW - TEM KW - DLS KW - XPS KW - NEXAFS KW - ToF-SIMS KW - IR KW - UV-vis PY - 2013 DO - https://doi.org/10.1021/la403222x SN - 0743-7463 SN - 1520-5827 VL - 29 IS - 46 SP - 14284 EP - 14292 PB - American Chemical Society CY - Washington, DC AN - OPUS4-29699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bertram, R. A1 - Stephanowitz, H. A1 - Heinrich, Hans-Joachim A1 - Rost, H.-J. A1 - Lüdke, C. A1 - Hassler, J. ED - Möller, H. J. ED - Roewer, G. T1 - Spurenelementverteilung in Siliciumcarbid-Einkristallen - Vergleich analytischer Feststoffmethoden T2 - Freiberger Siliziumtage 2005 ; Freiberger Forschungsforum ; 56. Berg- und Hüttenmännischer Tag CY - Freiberg, Deutschland DA - 2005-06-15 KW - Einkristall KW - Siliciumcarbid KW - Halbleitereigenschaft KW - Leistungselektronik KW - Feststoffbestimmung KW - Chemische Analyse KW - Nachweisgrenze KW - Kristalldefekt KW - Spurenelement KW - Feststoffanalytik KW - ETV ICP OES KW - SS ET AAS KW - LA-ICP-MS KW - Elektrothermische Verdampfung KW - Laserablation PY - 2006 SN - 978-3-86012-295-2 SN - 0071-9420 N1 - Serientitel: Freiberger Forschungshefte / B – Series title: Freiberger Forschungshefte / B IS - 337 SP - 122 EP - 138 PB - Techn. Univ. Bergakad. CY - Freiberg AN - OPUS4-15834 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, Z. A1 - Han, Q. A1 - Wang, D. A1 - Macé, T. A1 - Kipphardt, Heinrich A1 - Maiwald, Michael A1 - Tuma, Dirk A1 - Uehara, S. A1 - Akima, D. A1 - Shimosaka, T. A1 - Jung, J. A1 - Oh, S.-H. A1 - van der Veen, A. A1 - van Wijk, J.I.T. A1 - Ziel, P. R. A1 - Konopelko, L. A1 - Valkova, M. A1 - Mogale, D.M. A1 - Botha, A. A1 - Brewer, P. A1 - Murugan, A. A1 - Minnaro, M.D. A1 - Miller, M. A1 - Guenther, F. A1 - Kelly, M.E. T1 - CCQM K101 Final report international comparison CCQM-K101:Oxygen in nitrogen-a track B comparison and that the matrix contains argon N2 - This key comparison aims to assess the capabilities of the participants to determine the amount-of-substance fraction oxygen in nitrogen. The GAWG has classified this as a track B comparison, due to the unexpected 50 μmol/mol argon mole fraction content of the transfer standards, which effects the achievable performance of some measurement techniques such a GC-TCD. The separation of oxygen and argon is challenging, and not all systems in use are equally well designed for it. As this analytical challenge due to a substantial fraction of argon in the transfer standards became a reality, the Gas Analysis Working Group (GAWG) decided to qualify this key comparison as a regular key comparison and not as a core comparison, which may be used to support calibration and measurement capabilities (CMCs) for oxygen in nitrogen, or for oxygen in nitrogen mixtures containing argon only (see also the section on support to CMCs). KW - CCQM-K101 KW - Gas analysis PY - 2016 UR - http://iopscience.iop.org/article/10.1088/0026-1394/53/1A/08013 SN - 1681-7575 SN - 0026-1394 VL - 53 IS - Techn Suppl SP - 08013, 1 EP - 71 PB - IOP publishing AN - OPUS4-40013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Haibel, A. A1 - Rack, A. A1 - Weidemann, Gerd A1 - Riesemeier, Heinrich A1 - Goebbels, Jürgen A1 - Banhart, J. T1 - Investigation of pore formation in metallic foams by synchrotron computed tomography PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=324 SN - 0179-4159 SP - 324 EP - 325 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Haibel, A. A1 - Rack, A. A1 - Bütow, A. A1 - Kropf, H. A1 - Helwig, H.-M. A1 - Banhart, J. A1 - Weidemann, Gerd A1 - Riesemeier, Heinrich A1 - Goebbels, Jürgen T1 - Synchrotron-µ-tomography on complex materials PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=326 SN - 0179-4159 SP - 326 EP - 328 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rühl, Karl H. A1 - Emschermann, Hans-Heinrich A1 - Jänicke, J. A1 - Flossmann, R. T1 - Untersuchungen über den Spannungsverlauf in stoßartig beanpruchungen Stäben und Trägern PY - 1962 SN - 0025-5300 VL - 4 IS - 7 SP - 234 EP - 242 PB - Carl Hanser Verlag CY - München AN - OPUS4-10232 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, G. A1 - Nellesen, J. A1 - Anar, N. B. A1 - Ehrig, Karsten A1 - Riesemeier, Heinrich A1 - Tillmann, W. T1 - 3D analysis of micro-deformation in VHCF-loaded nodular cast iron by µCT N2 - The impact of very high cycle fatigue (VHCF) load conditions on the microstructure of specimens consisting of nodular cast iron is analyzed by means of micro-computed tomography (µCT) utilizing both monochromatic synchrotron radiation and polychromatic X-ray tube radiation. Using 3D µCT, the microstructure in the region of the smallest cross-sections of shouldered round specimens is imaged in different stages of the VHCF loading. By digital image correlation (DIC) of these tomograms strain fields are analyzed three-dimensionally. Strain levels in the range of a few percent were detected. It is proven that a localization of strain allows to predict the site of the crack which precedes and induces the macroscopic failure of the specimens. KW - VHCF (very high cycle fatigue) KW - µCT KW - Micro-computed tomography KW - Strain analysis KW - Nodular cast iron PY - 2013 DO - https://doi.org/10.1016/j.msea.2013.04.057 SN - 0921-5093 SN - 1873-4936 VL - 577 SP - 202 EP - 209 PB - Elsevier CY - Amsterdam AN - OPUS4-28533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liebner, Christian A1 - Fischer, J. A1 - Heinrich, Sebastian A1 - Lange, T. A1 - Hieronymus, Hartmut A1 - Klemm, E. T1 - Are micro reactors inherently safe? An investigation of gas phase explosion propagation limits on ethene mixtures N2 - A method for the determination of safety properties for micro reactors and micro structured components is presented. Micro structured reactors are not inherently safe but the range of safe operating conditions of micro reactors are extended since the explosion region is reduced. The λ/3 rule was demonstrated to be applicable to micro scale tubes for stoichiometric mixtures of ethane–oxygen and ethane–nitrous oxide. Furthermore first results from an investigation concerning detonation propagation through a micro reactor of non-ideal geometry are shown. Initial pressure investigated is ranging from low pressure up to 100 kPa. KW - Micro reactor KW - Explosion propagation limits KW - Chemical safety KW - Investigation method PY - 2012 DO - https://doi.org/10.1016/j.psep.2011.08.006 SN - 0957-5820 SN - 1744-3598 VL - 90 IS - 2 SP - 77 EP - 82 PB - Elsevier CY - Amsterdam AN - OPUS4-25594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hieronymus, Hartmut A1 - Fischer, J. A1 - Heinrich, Sebastian A1 - Liebner, Christian A1 - Lange, T. A1 - Klemm, E. T1 - Sicherheitstechnische Untersuchungen zum Betrieb von Mikroreaktoren im Explosionsbereich N2 - Es wird eine Methode zur sicherheitstechnischen Untersuchung von Mikroreaktoren und mikrostrukturierten Komponenten, die im Explosionsbereich betrieben werden sollen, vorgestellt. Mikrostrukturierte Reaktoren sind nicht inhärent sicher, wenngleich der Bereich der sicheren Betriebsbedingungen gegenüber konventionellen Reaktoren erweitert ist. Der Explosionsbereich kann durch die Mikrostrukturen eingeengt werden. Am Beispiel von Ethylen/Sauerstoff-Gemischen und Ethylen/N2O-Gemischen wird hinsichtlich der Ausbreitung von Detonationen durch Kapillarrohre gezeigt, dass die sogenannte λ/3-Regel angewandt werden kann. Darüber hinaus werden erste Ergebnisse der Untersuchung der Ausbreitung von Explosionen durch einen Mikroreaktor mit rechteckigem Strömungskanal vorgestellt. KW - Detonationszellbreite KW - Explosionsgrenzen KW - Mikroreaktoren KW - Sicherheitstechnik KW - Detonation cell width KW - Explosion limit KW - Microreactor KW - Saftey engineering PY - 2011 DO - https://doi.org/10.1002/cite.201100112 SN - 0009-286X SN - 1522-2640 VL - 83 IS - 10 SP - 1742 EP - 1747 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-24486 LA - deu 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 - GEN A1 - Rack, A. A1 - Zabler, S. A1 - Riesemeier, Heinrich A1 - Weidemann, Gerd A1 - Müller, Bernd R. A1 - Helfen, L. A1 - Stiller, M. A1 - Knabe, C. A1 - Goebbels, Jürgen A1 - Banhart, J. T1 - Nondestructive 3D insights into foamy metals and bioregenerative ceramics KW - X-ray Computed Tomography KW - Metal foams KW - Bioregenerative ceramics PY - 2008 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/infos/bessy/highlights2007.pdf#page=34 SN - 1611-6127 SP - 34 EP - 35 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-17538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudtsch, S. A1 - Fahr, M. A1 - Fischer, J. A1 - Gusarova, Tamara A1 - Kipphardt, Heinrich A1 - Matschat, Ralf T1 - High-Purity Fixed Points of the ITS-90 with Traceable Analysis of Impurity Contents N2 - The International Temperature Scale of 1990 (ITS-90) is based on thermodynamic equilibrium states of ideally pure substances. The largest contribution to the uncertainty budgets of most metallic fixed points is the influence of impurities on the fixed-point temperature. Therefore, a traceable chemical analysis of the remaining impurities with small uncertainty is the basis of further progress. Further requirements are better knowledge of the phase diagrams at very low impurity contents, impurity segregation, and the quantification and correction of thermal effects during a fixed-point realization. In this article, current and future activities at PTB and BAM in order to develop improved metallic fixed-point cells of the ITS-90 are reviewed. KW - Chemical analysis KW - Fixed points KW - Impurities KW - ITS-90 KW - Phase diagrams KW - Thermal effects PY - 2008 DO - https://doi.org/10.1007/s10765-007-0358-9 SN - 0195-928X SN - 1572-9567 VL - 29 IS - 1 SP - 139 EP - 150 PB - Springer CY - Dordrecht AN - OPUS4-17455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rack, A. A1 - Riesemeier, Heinrich A1 - Zabler, S. A1 - Weitkamp, T. A1 - Müller, Bernd R. A1 - Weidemann, Gerd A1 - Modregger, P. A1 - Banhart, J. A1 - Helfen, L. A1 - Danilewsky, A.N. A1 - Gräber, H.G. A1 - Heldele, R. A1 - Mayzel, B. A1 - Goebbels, Jürgen A1 - Baumbach, T. ED - Stuart R. Stock, T1 - The high-resolution synchrotron-based imaging stations at the BAMline (BESSY) and TopoTomo (ANKA) N2 - The BAMline at the BESSY light source in Berlin and the TopoTomo beamline at the ANKA synchrotron facility in Karlsruhe (both Germany) operate in the hard X-ray regime (above 6 keV) with similiar photon flux density. For typical imaging applications, a double multilayer monochromator or a filtered white beam is used. In order to optimise the field of view and the resolution of the available indirect pixel detectors, different optical systems have been installed, adapted, respectively, to a large field of view (macroscope) and to high spatial resolution (microscope). They can be combined with different camera systems, ranging from 16-bit dynamic range slow-scan CCDs to fast CMOS cameras. The spatial resolution can be brought substantially beyond the micrometer limit by using a Bragg magnifier. The moderate flux of both beamlines compared to other 3rd generation light sources is compensated by a dedicated scintillator concept. For selected applications, X-ray beam collimation has proven to be a reliable approach to increase the available photon flux density. Absorption contrast, phase contrast, holotomography and refraction-enhanced imaging are used depending on the application. Additionally, at the TopoTomo beamline digital white beam synchrotron topography is performed, using the digital X-ray pixel detectors installed. KW - Microtomography KW - Non-destructive evaluation KW - Coherent imaging KW - X-ray refraction KW - X-ray phase contrast KW - Synchrotron-CT KW - Synchrotron instrumentation KW - Scintillator KW - Bragg magnification KW - Holotomography KW - X-ray topography PY - 2008 DO - https://doi.org/10.1117/12.793721 SN - 0277-786X VL - 7078 SP - 70780X-1 - 70780X-9 AN - OPUS4-18296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Hinrichs, J. A1 - Kipphardt, Heinrich T1 - Application of glow discharge mass spectrometry to multielement ultra-trace determination in ultrahigh-purity copper and iron: a calibration approach achieving quantification and traceability N2 - A new approach was developed for quantitative calibration in GD-MS which can afford reliable and metrologically traceable results for many trace elements and was exemplified for pure copper and pure iron. It can be assumed that the technique can be further improved and applied to the analysis of other pure metals. Pressed copper and iron powder samples were used to calibrate the glow discharge mass spectrometry applied to the analysis of pure copper and iron. The new type of glow discharge mass spectrometer—the Element GD (Thermo Electron Corporation)—was used with a Grimm-type discharge cell for flat samples. Two series of powder samples were prepared for each of the copper and iron matrixes. The powders were quantitatively doped with solutions of graduated and defined concentrations of 40 or 20 analytes, respectively. The mass fractions of the analytes in the dried and homogenized metal powder samples ranged from µg/kg levels up to 10 mg/kg levels. A special technique was developed to press the samples and to form mechanically stable pellets with low risk of contamination. Ion beam ratios of analyte ions to matrix ions were used as measurands. The calibration curves were determined and the linear correlation coefficients were calculated for different intervals of the curves. The linear correlation coefficients are very satisfactory for most of the calibration curves, which include the higher segments of mass fractions; however, they are less satisfactory for the lower segments of the calibration curves. Nevertheless, in many cases rather acceptable and rather promising values were achieved even for these lower segments, representing mass fractions of analytes at ultra-trace level. The comparison of the certified values of different reference materials with the measured values based on calibrations with the pressed powder samples led to deviations less than 30% for most of the considered examples. KW - Glow discharge mass spectrometry (GD-MS) KW - High-purity copper KW - High-purity iron KW - Doped and pressed metal powder samples KW - Grimm-type cell KW - Metrological traceability PY - 2006 DO - https://doi.org/10.1007/s00216-006-0645-5 SN - 1618-2642 SN - 1618-2650 VL - 386 IS - 1 SP - 125 EP - 141 PB - Springer CY - Berlin AN - OPUS4-12649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marcusson, J. A1 - Burchartz, Heinrich T1 - Prüfung der elastischen Eigenschaften von Urteerrückständen PY - 1922 VL - 40 IS - 1-2 SP - 88 EP - 90 PB - Springer CY - Berlin AN - OPUS4-15106 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Burchartz, Heinrich A1 - v. Wrochem, J. T1 - Versuche über die Einwirkung von Magnesiumsulfatlösung auf Zement PY - 1917 VL - 35 IS - 4-5 SP - 206 EP - 213 PB - Springer CY - Berlin AN - OPUS4-14191 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zabler, S. A1 - Rack, A. A1 - Manke, I. A1 - Thermann, K. A1 - Tiedemann, J. A1 - Harthill, N. A1 - Riesemeier, Heinrich T1 - High-resolution tomography of cracks, voids and micro-structure in greywacke and limestone N2 - Rocks are commonly very heterogeneous materials. Randomly distributed micro-flaws inside the rock are believed to initiate tensile cracks from which shear fractures develop and coalescence through en echelon interactions leads to fracture. In this paper, we describe the results of applying high-resolution X-ray tomography to samples of greywacke and limestone experimentally deformed under unconfined axial shortening at various loads equivalent to different fractions of the sample strength. Mineral grains, pores, micro-cracks and other voids were imaged with a resolution of 10 µm. 3D image analysis enabled us to monitor the initial state of the samples and the changes in them due to compression. Crack morphology is characterized and compared to the micro-structure of the sample before and after deformation. In the greywacke, formation of a macro-crack ~10° oblique to the stress direction is observed. It initiated in fine intergranular material at the top tip of the sample and is composed of tensile fractures connected by wing cracks. None of the voids defined in the initial state fractured, and the crack is interpreted to have started either as a micro-crack which was smaller than the resolution of the tomography, or, as a completely new crack. In the limestone, cracks are observed to initiate in features that are too small to be imaged by the tomography, or also in newly created cracks. KW - Rock porosity KW - Crack formation KW - X-ray imaging KW - Micro-tomography KW - 3D image analysis PY - 2008 DO - https://doi.org/10.1016/j.jsg.2008.03.002 SN - 0191-8141 SN - 1873-1201 VL - 30 IS - 7 SP - 876 EP - 887 PB - Pergamon Press CY - Oxford AN - OPUS4-18566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Danilewsky, A.N. A1 - Rack, A. A1 - Wittge, J. A1 - Weitkamp, T. A1 - Simon, R. A1 - Riesemeier, Heinrich A1 - Baumbach, T. T1 - White beam synchrotron topography using a high resolution digital X-ray imaging detector N2 - X-ray topography is a well known imaging technique to characterise strain and extended defects in single crystals. Topographs are typically collected on X-ray films. On the one hand such photographic films show a limited dynamic range and the production of films will be discontinued step by step in the near future. On the other hand new imaging detectors improved for X-ray tomography become more and more attractive even for topography because of increasing resolution, dynamic range, speed and active area. In this paper we report about the upgrade of the TOPO–TOMO beamline at the synchrotron light source ANKA, Research Centre Karlsruhe, with a high resolution digital camera for the topography use. KW - White beam topography KW - Synchrotron radiation KW - Digital X-ray detector KW - Scintillator KW - Synchrotron instrumentation KW - Digital radiography PY - 2008 DO - https://doi.org/10.1016/j.nimb.2008.02.065 SN - 0168-583X SN - 1872-9584 VL - 266 IS - 9 SP - 2035 EP - 2040 PB - Elsevier CY - Amsterdam AN - OPUS4-18567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poppenberg, J. A1 - Richter, S. A1 - Traulsen, C.H.-H. A1 - Darlatt, Erik A1 - Baytekin, B. A1 - Heinrich, T. A1 - Deutinger, P.M. A1 - Huth, K. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Programmable multilayers of nanometer-sized macrocycles on solid support and stimuli-controlled on-surface pseudorotaxane formation N2 - Mechanically interlocked molecules (MIMs) such as rotaxanes and catenanes are capable of mechanical motion on the nanoscale and are therefore promising prototypes for molecular machines in recent nanotechnology. However, most of the existing examples are isotropically distributed in solution, which prohibits concerted movement and with it the generation of macroscopic effects. Thus, arranging them in ordered arrays is of huge interest in recent research. We report the deposition of quite densely packed multilayers of tetralactam macrocycles on gold surfaces by metal-coordinated layer-by-layer self-assembly. Linear dichroism effects in angle-resolved NEXAFS spectra indicate a preferential orientation of the macrocycles. The sequence of the metal ions can be programmed by the use of different transition metal ions at each deposition step. Additionally, reversible on-surface pseudorotaxane formation was successfully realized by repeated uptake and release of axle molecules inside the macrocycles cavities. KW - ISO KW - Standard KW - Surface analysis KW - Imaging PY - 2013 DO - https://doi.org/10.1039/c3sc50558h SN - 2041-6520 SN - 2041-6539 VL - 4 SP - 3131 EP - 3139 PB - RSC CY - Cambridge AN - OPUS4-29049 LA - eng 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 - GEN A1 - Müller, Christina A1 - Bertovic, Marija A1 - Gaal, Mate A1 - Heidt, Heinrich A1 - Pavlovic, Mato A1 - Rosenthal, Martina A1 - Takahashi, K. A1 - Pitkänen, J. A1 - Ronneteg, U. T1 - Progress in evaluating the reliability of NDE systems - Paradigm shift N2 - The paper will give an overview of new methodology for evaluating the reliability of NDE systems accurately, reliably and efficiently in accordance with the specific requirements of industrial application. After a review of the substantive issues from the previous workshops, the go forward guidance from these interactions is considered. At the beginning of the reliability analysis, the actual safety demands have to be defined in order to fit the investigation to the level of risk when the component would fail. Next, all the essential influencing parameters need to be documented and transferred to an appropriate design of experiments (DOE) to determine the reliability in terms of a qualitative assessment for lower risk or in terms of a quantitative probability of detection (POD) or ROC (Receiver Operating Characteristics) curves for higher safety demands. A new paradigm is offered to consider the POD or reliability of the system as a function of the configuration of input variables and use it for optimisation rather than for a final judgement. An advantage for the end user is also to sample all single PODs to an integral 'Volume POD' of a part. Among the influencing parameters, the human factor is the most important one. A systematic psychological approach shall help to find out where the bottlenecks are but most importantly to provide best possible working conditions for the human inspectors. T2 - 4th European-American workshop on reliability of NDE CY - Berlin, Germany DA - 2009-06-24 KW - Zuverlässigkeit von ZfP-Systemen KW - Multiparameter POD PY - 2009 UR - http://www.ndt.net/article/reliability2009/Inhalt/we1a2.pdf SN - 978-3-940283-17-7 IS - DGZfP-BB 116 SP - 1 EP - 13 AN - OPUS4-20616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Christina A1 - Pavlovic, Mato A1 - Bertovic, Marija A1 - Gaal, Mate A1 - Heidt, Heinrich A1 - Rosenthal, Martina A1 - Takahashi, K. A1 - Pitkänen, J. A1 - Ronneteg, U. T1 - Fortschritte bei der Bewertung der Zuverlässigkeit von ZfP-Systemen N2 - Es werden die Fortschritte bei der Bewertung der Zuverlässigkeit von ZfP-Systemen in den vergangenen 10 Jahren vorgestellt. Der modulare Ansatz bzw. die systematische Auflistung aller wesentlichen Einflussfaktoren stehen am Anfang jeder Bewertung, die jeweils spezifisch für einen industriellen bzw. Feldeinsatz angelegt wird. Weiterhin legt die zu Grunde liegende Sicherheitsanforderung fest, ob ein exaktes quantitatives statistisches Ergebnis z. B. für die Fehlergröße, die mit hoher Sicherheit detektiert wird angestrebt wird oder ob man sich mit einer qualitativen Abschätzung zufrieden geben kann. Moderne Werkzeuge wie das 'Design of Experiments' (Statistische Versuchsplanung), die Volumen-POD für ein Bauteil als ganzes oder auch die systematische psychologische Betrachtung des menschlichen Faktors unterstützen die Treffsicherheit der Untersuchung für den gewünschten Einsatzfall. Die Ergebnisse der ZfP-Prüfungen können immer nur so gut sein, wie der Mensch mit den Bedingungen zurechtkommt. Weiterhin kann die POD im Zusammenhang mit den Prozessparametern als helfendes Optimierungswerkzeug eingesetzt werden und nicht als endgültige Be(Ver)urteilung. Es werden Beispiele aus Bereichen der Energieerzeugung und Endlagerung präsentiert. T2 - DGZfP-Jahrestagung 2009 CY - Münster, Deutschland DA - 2009-05-18 KW - POD KW - ROC KW - Paradigmenshift KW - Optimierung KW - Human factor PY - 2009 UR - http://www.ndt.net/article/dgzfp2009/Inhalt/mo3c2.pdf SN - 978-3-940283-16-0 IS - DGZfP-BB 115 (Mo.3.C.2) SP - 1 EP - 9 AN - OPUS4-20619 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Williams, S. H. A1 - Hilger, A. A1 - Kardjilov, N. A1 - Manke, I. A1 - Strobl, M. A1 - Douissard, P.A. A1 - Martin, T. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Detection system for microimaging with neutrons N2 - A new high-resolution detector setup for neutron imaging has been developed based on infinity-corrected optics with high light collection, combined with customized mounting hardware. The system can easily be installed, handled and fitted to any existing facility, avoiding the necessity of complex optical systems or further improved electronics (CCD). This is the first time optical magnification higher than 1:1 has been used with scintillator-based neutron detectors, as well as the first implementation of infinity corrected optics for neutron imaging, achieving the smallest yet reported effective pixel size of 3.375 µm. A novel transparent crystal scintillator (GGG crystal) has been implemented with neutrons for the first time to overcome limitations of traditional powder scintillators (Li6/ZnS, Gadox). The standardized procedure for resolution measurements with the Modulation Transfer Function (MTF) is summarized to facilitate comparison between instruments and facilities. Using this new detector setup, a resolution of 14.8 µm with a field of view of 6 mm × 6 mm has been achieved while maintaining reasonable count times. These advances open a wide range of new possible research applications and allow the potential for additional future developments. KW - Instrumentation for neutron sources KW - Neutron radiography KW - Neutron detectors (cold, thermal, fast neutrons) PY - 2012 DO - https://doi.org/10.1088/1748-0221/7/02/P02014 SN - 1748-0221 VL - 7 IS - P02014 SP - 1 EP - 26 PB - Inst. of Physics Publ. CY - London AN - OPUS4-26433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mühler, T. A1 - Heinrich, J. A1 - Wirth, Cynthia A1 - Günster, Jens T1 - Slurry-based additive manufacturing of ceramics N2 - Most additive manufacturing (AM) techniques have in common that material is spread out as thin layers of a dried powder/granulate by a roller or a shaker system. These layers are mostly characterized by a low packing rate. On the other hand, appreciable densities can be reached by the use of ceramic slurries. In this context, the layer-wise slurry deposition (LSD) has been developed. Specific features of the LSD process are reflected on the basis of already existing additive manufacturing technologies. The microstructure of laser-sintered bodies will be discussed, and strategies for an improved microstructure during sintering will be introduced. KW - Additive manufacturing KW - Ceramic KW - Selective laser sintering PY - 2015 DO - https://doi.org/10.1111/ijac.12113 SN - 1546-542X SN - 1744-7402 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. VL - 12 IS - 1 SP - 18 EP - 25 PB - American Ceramic Soc. CY - Westerville, Ohio AN - OPUS4-29937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Günster, Jens A1 - Heinrich, J. T1 - 2nd International symposium on materials processing science with lasers as energy sources KW - Materials science PY - 2012 SN - 0173-9913 SN - 0196-6219 VL - 89 IS - 6-7 SP - E 36 PB - Göller CY - Baden-Baden AN - OPUS4-31281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Traulsen, Christoph Hans-Henning A1 - Darlatt, Erik A1 - Richter, S. A1 - Poppenberg, J. A1 - Traulsen, N.L. A1 - Linder, I. A1 - Lippitz, Andreas A1 - Dietrich, Paul A1 - Dib, B. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - The versatility of 'Click' reactions at surfaces: Molecular recognition at interfaces N2 - In order to investigate molecular recognition on surfaces, an azide-functionalized monolayer was deposited on gold. The monolayer was characterized by X-ray photoelectron spectroscopy (XPS) and angle-resolved near-edge X-ray absorption fine structure (NEXAFS) experiments and the decomposition of the azide upon irradiation with X-ray beams was investigated. Subsequently, various alkyne-functionalized host and guest molecules were attached to the azide by 1,3-dipolar cycloaddition. These modified surfaces and their host–guest chemistry were analysed by XPS and angle-resolved NEXAFS. The reversibility of guest binding was shown for one example as a proof of principle. KW - 'Click' reaction KW - Azide-terminated surfaces KW - SAMs KW - Host guest molecules KW - Molecular recognition at interfaces PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-306463 DO - https://doi.org/10.1039/C4RA01730G SN - 2046-2069 VL - 4 IS - 34 SP - 17694 EP - 17702 PB - RSC Publishing CY - London AN - OPUS4-30646 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 - Markötter, H. A1 - Manke, I. A1 - Hartnig, C. A1 - Krüger, P. A1 - Wippermann, K. A1 - Arlt, Tobias A1 - Choinka, G. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Hochauflösende Synchrotron-Radiografie KW - PEM Fuel-cells KW - Local current distribution KW - Neutron imaging technique KW - Water transport PY - 2010 SN - 0025-5300 VL - 52 IS - 10 SP - 698 EP - 704 PB - Hanser CY - München AN - OPUS4-23046 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Schwarz, F. A1 - Heinrich, Thomas A1 - Kaufmann, J. O. A1 - Lippitz, Andreas A1 - Puttreddy, R. A1 - Rissanen, K. A1 - Schalley, C. A. T1 - Photocontrolled on-surface pseudorotaxane formation with well-ordered macrocycle multilayers N2 - The photoinduced pseudorotaxane formation between a photoresponsive axle and a tetralactam macrocycle was investigated in solution and on glass surfaces with immobilized multilayers of macrocycles. In the course of this reaction, a novel photoswitchable binding station with azobenzene as the photoswitchable unit and diketopiperazine as the binding station was synthesized and studied by NMR and UV/Vis spectroscopy. Glass surfaces have been functionalized with pyridine-terminated SAMs and subsequently withmultilayers of macrocycles through layer-by-layer self assembly. A preferred orientation of the macrocycles could be confirmed by NEXAFS spectroscopy. The photocontrolled Deposition of the axle into the surface-bound macrocycle-multilayers was monitored by UV/Vis spectroscopy and led to an increase of the molecular order, as indicated by more substantial linear dichroism effects in angle-resolved NEXAFS spectra. KW - Well-ordered macrocycle multilayers KW - XPS KW - NEXAFS PY - 2016 DO - https://doi.org/10.1002/chem.201603156 SN - 0947-6539 SN - 1521-3765 VL - 22 IS - 40 SP - 14383 EP - 14389 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-38270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brieger, C. A1 - Melke, J. A1 - van der Bosch, N. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Krishna Kayarkatte, M. A1 - Derr, I. A1 - Schökel, A. A1 - Roth, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A combined in-situ XAS–DRIFTS study unraveling adsorbate induced changes on Pt nanoparticle structure N2 - The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Δμ X-ray Absorption Near Edge Structure analysis (Δμ XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the Pt-Pt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from Pt-CO to Pt-O. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support. KW - X-ray absorption spectroscopy KW - DRIFTS KW - XANES KW - CO adsoprtion KW - Platinum KW - String metal support interaction KW - Silica support KW - Adsorbates KW - Infrared spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.jcat.2016.03.034 SN - 0021-9517 VL - 339 SP - 57 EP - 67 PB - Elsevier AN - OPUS4-38367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Traulsen, Christoph Hans-Henning A1 - Holzweber, Markus A1 - Richter, S. A1 - Kunz, V. A1 - Kastner, S.K. A1 - Krabbenborg, S.O. A1 - Huskens, J. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - Coupled molecular switching processes in ordered mono- and multilayers of stimulus-responsive rotaxanes on gold surfaces N2 - Interfaces provide the structural basis for function as, for example, encountered in nature in the membrane-embedded photosystem or in technology in solar cells. Synthetic functional multilayers of molecules cooperating in a coupled manner can be fabricated on surfaces through layer-by-layer self-assembly. Ordered arrays of stimulus-responsive rotaxanes undergoing well-controlled axle shuttling are excellent candidates for coupled mechanical motion. Such stimulus-responsive surfaces may help integrate synthetic molecular machines in larger systems exhibiting even macroscopic effects or generating mechanical work from chemical energy through cooperative action. The present work demonstrates the successful deposition of ordered mono- and multilayers of chemically switchable rotaxanes on gold surfaces. Rotaxane mono- and multilayers are shown to reversibly switch in a coupled manner between two ordered states as revealed by linear dichroism effects in angle-resolved NEXAFS spectra. Such a concerted switching process is observed only when the surfaces are well packed, while less densely packed surfaces lacking lateral order do not exhibit such effects. KW - Molecular machine KW - Rotaxane KW - LBL growth KW - XPS KW - NEXAFS KW - SIMS PY - 2015 DO - https://doi.org/10.1021/ja512654d SN - 0002-7863 SN - 1520-5126 VL - 137 IS - 13 SP - 4382 EP - 4390 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-33077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kaltenbach, A. A1 - Nordmann, J. A1 - Görlitz, V. A1 - Pape, C. A1 - Richter, Silke A1 - Kipphardt, Heinrich A1 - Kopp, G. A1 - Jährling, R. A1 - Rienitz, O. A1 - Güttler, B. T1 - Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium N2 - Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of Urel(w)<0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools. KW - Digestion KW - Rhodium KW - Molybdenum KW - Reference solution KW - Metrological traceability KW - ICP OES KW - MC-ICP-MS PY - 2015 DO - https://doi.org/10.1007/s00216-014-8395-2 SN - 1618-2642 SN - 1618-2650 VL - 407 IS - 11 SP - 3093 EP - 3102 PB - Springer CY - Berlin AN - OPUS4-33065 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 - 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 -