TY - JOUR A1 - Vogl, Jochen A1 - Kipphardt, Heinrich A1 - Richter, Silke A1 - Bremser, Wolfram A1 - Arvizu Torres, M. A1 - Lara Manzano, J. A1 - Buzoianu, M. A1 - Hill, S. A1 - Petrov, P. A1 - Goenaga-Infante, H. A1 - Sargent, M. A1 - Fisicaro, P. A1 - Labarraque, G. A1 - Zhou, T. A1 - Turk, G. C. A1 - Winchester, M. A1 - Miura, T. A1 - Methven, B. A1 - Sturgeon, R. A1 - Jährling, R. A1 - Rienitz, O. A1 - Mariassy, M. A1 - Hankova, Z. A1 - Sobina, E. A1 - Krylov, A. I. A1 - Kustikov, Y. A. A1 - Smirnov, V. V. T1 - Establishing comparability and compatibility in the purity assessment of high purity zinc as demonstrated by the CCQM-P149 intercomparison N2 - For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute’s applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100 %, or 1 kg/kg. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011 %. The calculated reference value, w(Zn) = 0.999 873 kg/kg, was assigned an asymmetric combined uncertainty of + 0.000025 kg/kg and – 0.000028 kg/kg. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition / dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity of less pure elements and/or for those elements suffering difficulties with the decomposition process. KW - Purity assessment KW - Direct metal assay KW - Impurity assessment KW - Non-metal analysis KW - High-purity elements KW - SI-traceability PY - 2018 DO - https://doi.org/10.1088/1681-7575/aaa677 SN - 1681-7575 SN - 0026-1394 VL - 55 IS - 2 SP - 211 EP - 221 PB - Institute of Physics Publishing CY - Bristol AN - OPUS4-44257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mühler, T. A1 - Helsch, G. A1 - Heinrich, J.G. A1 - Yao, Dongxu A1 - Gräf, S. A1 - Müller, F.A. A1 - Günster, Jens T1 - Strategies for the selective volume sintering of ceramics N2 - The present study is dealing with the basic physics for a novel way to generate a free-formed ceramic body, not like common layer by layer, but directly by Selective Volume Sintering (SVS) in a compact block of ceramic powder. To penetrate with laser light into the volume of a ceramic powder compact it is necessary to investigate the light scattering properties of ceramic powders. Compared with polymers and metals, ceramic materials are unique as they offer a wide optical window of transparency. The optical window typically ranges from below 0.3 up to 5 µm wave length. In the present study thin layers of quartz glass (SiO2) particles have been prepared. As a function of layer thickness and the particle size, transmission and reflection spectra in a wave length range between 0.5 and 2.5 µm have been recorded. Depending on the respective particle size and by choosing a proper relation between particle size and wave length of the incident laser radiation, it is found that light can penetrate a powder compact up to a depth of a few millimeters. With an adjustment of the light absorption properties of the compact the initiation of sintering in the volume of the compact is possible. KW - Additive Manufacturing PY - 2014 DO - https://doi.org/10.1557/jmr.2014.174 SN - 0884-2914 VL - 29 IS - 17 SP - 2095 EP - 2099 PB - Materials Research Society CY - Warrendale, Pa. AN - OPUS4-32544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lahiri, D. A1 - Sharma, S.M. A1 - Verma, A.K. A1 - Vishwanadh, B. A1 - Dey, G.K. A1 - Schumacher, G. A1 - Scherb, T. A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Banerjee, S. T1 - Investigation of short-range structural order in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 glasses, using X-ray absorption spectroscopy and ab initio molecular dynamics simulations N2 - Short-range order has been investigated in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 metallic glasses using X-ray absorption spectroscopy and ab initio molecular dynamics simulations. While both of these alloys are good glass formers, there is a difference in their glass-forming abilities (Zr41.5Ti41.5Ni17 > Zr69.5Cu12Ni11Al7.5). This difference is explained by inciting the relative importance of strong chemical order, icosahedral content, cluster symmetry and configuration diversity. KW - Multi-component alloy KW - Glass-forming ability KW - XAFS KW - Local structure KW - AIMD simulation PY - 2014 DO - https://doi.org/10.1107/S1600577514017792 SN - 0909-0495 SN - 1600-5775 VL - 21 IS - 6 SP - 1296 EP - 1304 PB - Blackwell Publishing CY - Oxford AN - OPUS4-31837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Vogl, Jochen A1 - Gusarova, Tamara A1 - Czerwensky, Michael A1 - Heinrich, Hans-Joachim A1 - Hioki, A. A1 - Konopelko, L.A. A1 - Methven, B. A1 - Miura, T. A1 - Petersen, O. A1 - Riebe, Gundel A1 - Sturgeon, R. A1 - Turk, G.C. A1 - Yu, L. L. T1 - Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability N2 - Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established. KW - Interlaboratory comparison KW - Purity analysis KW - High purity metals KW - CCQM-P107 KW - Zinc PY - 2010 DO - https://doi.org/10.1007/s00769-009-0557-0 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 1 SP - 29 EP - 37 PB - Springer CY - Berlin AN - OPUS4-20767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Görner, Wolf A1 - Hentschel, Manfred P. A1 - Müller, Bernd R. A1 - Riesemeier, Heinrich A1 - Krumrey, M. A1 - Ulm, G. T1 - The first hard X-rays at the BAMline PY - 2001 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2000.pdf#page=329 SN - 0179-4159 SP - 329 EP - 331 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-1299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Görner, Wolf A1 - Hentschel, Manfred P. A1 - Riesemeier, Heinrich A1 - Krumrey, M. A1 - Ulm, G. A1 - Diete, W. A1 - Klein, U. A1 - Frahm, R. T1 - BAMlin - the first hard X-ray beamline at BESSY II N2 - The first hard X-ray beamline at BESSY II will be installed by BAM and PTB at a superconducting 7 T wavelength shifter. The main optical elements of the beamline are a Double-Multilayer-Monochromator and a Double-Crystal-Monochromator. The two devices can be used separately or in-line. Main applications of monochromatic radiation with photon energies up to 50 keV are X-ray fluorescence analysis, micro-computed tomography, X-ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV will be available for radiometric applications. KW - Double-Multilayer-Monochromator with meridional bender KW - Double-Crystal-Monochromator with sagittal bender KW - X-ray fluorescence analysis KW - Micro-computed tomography KW - X-ray topography KW - Detector calibration KW - Reflectometry PY - 2001 DO - https://doi.org/10.1016/S0168-9002(01)00466-1 SN - 0168-9002 SN - 0167-5087 VL - 467-468 IS - 1 SP - 703 EP - 706 PB - North-Holland CY - Amsterdam AN - OPUS4-1171 LA - eng 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 - Paris, O. A1 - Li, C. A1 - Siegel, S. A1 - Weseloh, G. A1 - Emmerling, Franziska A1 - Riesemeier, Heinrich A1 - Erko, A. A1 - Fratzl, P. T1 - A new experimental station for simultaneous X-ray microbeam scanning for small- and wide-angle scattering and fluorescence at BESSY II N2 - A new instrument for simultaneous microbeam small- and wide-angle X-ray scattering and X-ray fluorescence (SAXS/WAXS/XRF) is presented. The instrument is installed at the microfocus beamline at BESSY II and provides a beam of 10 µm size with a flux of about 109 photons s-1. A SAXS resolution up to 500 Å d-spacing and a range of scattering vectors of almost three orders of magnitude are reached by using a large-area high-resolution CCD-based detector for simultaneous SAXS/WAXS. The instrument is particularly suited for scanning SAXS/WAXS/XRF experiments on hierarchically structured biological tissues. The necessary infrastructure, such as a cryo-stream facility and an on-site preparation laboratory for biological specimens, are available. KW - Scanning SAXS KW - Scanning WAXS KW - Microbeam KW - Synchrotron radiation PY - 2007 SN - 0021-8898 SN - 1600-5767 VL - 40 IS - Supplement SP - s466 EP - s470 PB - Blackwell CY - Oxford AN - OPUS4-15049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mechler, S. A1 - Schumacher, G. A1 - Koteski, V. A1 - Riesemeier, Heinrich A1 - Schäfers, F. A1 - Mahnke, H.-E. T1 - Local structure and site substitution in amorphous and quasicrystalline Zr-Ti-Ni-(Cu) alloys N2 - Local structures of amorphous and quasicrystalline phases in Zr–Ti–Ni and Zr–Ti–Ni–Cu alloys have been studied by means of x-ray absorption spectroscopy. The amorphous phases show a high degree of icosahedral short-range order. In all investigated systems local order around Cu and Ni atoms was found to be nearly identical pointing to site substitution of Ni by Cu as the reason for an improved glass forming ability when Ni is partly substituted by Cu. The results strengthen an icosahedral cluster based approach for the structure of metallic glasses and indicate the importance of the medium-range order on glass formation. KW - Copper alloys KW - Frustration KW - Glass structure KW - Metallic glasses KW - X-ray absorption spectra PY - 2010 DO - https://doi.org/10.1063/1.3467265 SN - 0003-6951 SN - 1077-3118 VL - 97 IS - 4 SP - 041914-1 - 041914-3 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-22122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schott, M. A1 - Szczerba, Wojciech A1 - Posset, U. A1 - Vuk, A.S. A1 - Beck, M. A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Kurth, D. G. T1 - In operando XAFS experiments on flexible electrochromic devices based on Fe(II)-metallo-supramolecular polyelectrolytes and vanadium oxides N2 - Flexible electrochromic devices (ECDs) based on Fe(II)-metallo-supramolecular polyelectrolytes (Fe-MEPE) and vanadium oxide are studied in operando by means of x-ray absorption fine structure (XAFS) spectroscopy. The ECDs are blue-purple in the colored state at 0.0 V and become light yellow when a voltage of 1.6 V is applied. The XAFS studies at the K-edge of Fe(II) reveals that the absorption edge is shifted toward higher energies by 1.8 eV in the transparent state. Comparison of two different ECDs and different charge cycles demonstrates the reversibility and repeatability of the process. We attribute the shift to a charge transfer and a change of oxidation state of the ions from Fe2+ to Fe3+. The transition is not accompanied by a noticeable structural change of the octahedral coordination geometry as confirmed by analysis of the extended x-ray absorption fine structure (EXAFS) data. (C) 2015 Elsevier B.V. All rights reserved. KW - Metallo-supramolecular polyelectrolytes KW - Vanadium oxide KW - Electrochromism KW - Electrochromic device KW - Cyclic voltammetry KW - XAFS PY - 2016 DO - https://doi.org/10.1016/j.solmat.2015.10.015 SN - 0927-0248 VL - 147 SP - 61 EP - 67 PB - Elsevier B.V. CY - Amsterdam [u.a.] AN - OPUS4-35251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -