TY - JOUR A1 - D'Agostino, G. A1 - Bergamaschi, L. A1 - Giordani, L. A1 - Oddone, M. A1 - Kipphardt, Heinrich A1 - Richter, Silke T1 - Use of instrumental neutron activation analysis to investigate the distribution of trace elements among subsamples of solid materials N2 - The results of analytical measurements performed with solid-sampling techniques are affected by the distribution of the analytes within the matrix. The effect becomes significant in case of determination of trace elements in small subsamples. In this framework we propose a measurement model based on Instrumental Neutron Activation Analysis to determine the relative variability of the amount of an analyte among subsamples of a material. The measurement uncertainty is evaluated and includes the counting statistics, the full-energy gamma peak efficiency and the spatial gradient of the neutron flux at the irradiation position. The data we obtained in a neutron activation experiment and showing the relative variability of As, Au, Ir, Sb and W among subsamples of a highly pure Rh foil are also presented. KW - Instrumental neutron activation analysis KW - Homogeneity KW - Rhodium KW - Uncertainty PY - 2014 SN - 0026-1394 SN - 1681-7575 VL - 51 SP - 1 EP - 6 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-30302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schönhals, Andreas A1 - Goering, Harald A1 - Costa, F. R. A1 - Wagenknecht, U. A1 - Heinrich, G. T1 - Dielectric properties of nanocomposites based on polyethylene and layered double hydroxide N2 - Nanocomposites with a predominantly exfoliated morphology were prepared by melt blending of organically modified doubled layered hydroxide (LDH) and low density polyethylene (PE). The prepared materials were investigated by differential scanning calorimetry (DSC) and in detail by dielectric spectroscopy. The DSC experiments show that the degree of crystallinity decreases linearly with increasing content of the LDH. The extrapolation of this dependence to zero results in a limiting concentration of ca. 50 wt % LDH were the crystallization of PE is completely suppressed by the nanofiller. The dielectric response of pure polyethylene shows different weak relaxation processes. The intensity of dynamic glass transition (β-relaxation) increases with the concentration of LDH. This is attributed to the increasing concentration of the exchanged anion dodecyl benzene sulfonate (SDBS). The SDBS molecules are strongly adsorbed at the exfoliated LDH layers. Therefore, a detailed analysis of the β-relaxation provides information about the structure and the molecular dynamics in the interfacial region between the exfoliated LDH layers and the polyethylene matrix. This analysis shows that the β-relaxation region consists of two processes: both of them obey glassy dynamics. The difference in corresponding Vogel (ideal glass transition) temperatures is about 30 K. The relaxation process at lower frequency is assigned to polyethylene segments with a reduced molecular mobility close to LDH layers. The process at higher frequencies is related to polyethylene segments in a farer distance for the surface of the nanofiller. In the nanocomposite materials an additional process due to Maxwell-Wagner-Sillars (MWS) polarization was observed. The time constant of this MWS process can be correlated with characteristic length scales in nanocomposites and therefore provides additional information on dispersion and delamination/exfoliation of the LDH layers in these materials. PY - 2009 DO - https://doi.org/10.1021/ma900077w SN - 0024-9297 SN - 1520-5835 VL - 42 IS - 12 SP - 4165 EP - 4174 PB - American Chemical Society CY - Washington, DC AN - OPUS4-19594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wang, D. A1 - Costa, F. R. A1 - Leuteritz, A. A1 - Purohit, Purv A1 - Schönhals, Andreas A1 - Vyalikh, A. A1 - Scheler, U. A1 - Wagenknecht, U. A1 - Kutlu, B. A1 - Heinrich, G. ED - Mittal, V. T1 - Polyolefin nanocomposites with layered double hydroxides PY - 2010 SN - 978-1-4398-1454-3 SP - 225 EP - 245 PB - CRC Press AN - OPUS4-23039 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 - 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 - TY - CONF A1 - Heidt, Heinrich A1 - Basler, G. T1 - Belichtungsrechner für technische Radiographie T2 - 2. Europäische Tagung für Zerstörungsfreie Prüfung CY - Wien DA - 1981-09-14 PY - 1981 SP - 163 EP - 164 CY - Wien AN - OPUS4-33313 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shipov, A. A1 - Zaslansky, P. A1 - Riesemeier, Heinrich A1 - Segev, G. A1 - Atkins, A. A1 - Kalish-Achrai, N. A1 - Weiner, S. A1 - Shahar, R. T1 - The influence of estrogen deficiency on the structural and mechanical properties of rat cortical bone N2 - Background. Post-menopausal osteoporosis is a common health problem worldwide, most commonly caused by estrogen deficiency. Most of the information regarding the skeletal effects of this disease relates to trabecular bone, while cortical bone is less studied. The purpose of this study was to evaluate the influence of estrogen deficiency on the structure and mechanical properties of cortical bone. Methods. Eight ovariectomized (OVH) and eight intact (control) Sprague Dawley rats were used. Structural features of femoral cortical bone were studied by light microscopy, scanning electron microscopy and synchrotron-based microcomputer-tomography and their mechanical properties determined by nano-indentation. Results. Cortical bone of both study groups contains two distinct regions: organized circumferential lamellae and disordered bone with highly mineralized cartilaginous islands. Lacunar volume was lower in the OVH group both in the lamellar and disorganized regions (182 ± 75 µm3 vs 232 ± 106 µm3 , P < 0.001 and 195 ± 86 µm3 vs. 247 ± 106 µm3 , P < 0.001, respectively). Lacunar density was also lower in both bone regions of the OVH group (40 ± 18 ×103 lacunae/mm3 vs. 47 ± 9×103 lacunae/mm3 in the lamellar region, P = 0.003 and 63 ± 18×103 lacunae/mm3 vs. 75 ± 13×103 lacunae/mm3 in the disorganized region, P < 0.001). Vascular canal volume was lower in the disorganized region of the bone in the OVH group compared to the same Region in the control group (P < 0.001). Indentation moduli were not different between the study groups in both bone regions. Discussion. Changes to cortical bone associated with estrogen deficiency in rats require high-resolution methods for detection. Caution is required in the application of These results to humans due to major structural differences between human and rat bone. KW - Estrogen KW - Disorganized bone KW - Rat KW - Lacunae KW - Ovariectomy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520798 DO - https://doi.org/10.7717/peerj.10213 VL - 9 SP - e10213 AN - OPUS4-52079 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 - TY - JOUR A1 - Purohit, Purv A1 - Huacuja Sánchez, Jesús A1 - Wang, D.-Y. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Heinrich, G. A1 - Schönhals, Andreas T1 - Structure - property relationships of nanocomposites based on polypropylene and layered double hydroxides N2 - Nanocomposites based on polypropylene (PP) and organically modified ZnAl layered double hydroxides (ZnAl-LDH) were prepared by melt blending and investigated by a combination of differential scanning calorimetry (DSC), small- and wide-angle X-ray scattering (SAXS and WAXS), and dielectric relaxation spectroscopy (DRS). An average number of stack size of LDH layers is calculated by analyzing the SAXS data which is close to that of pure organically modified ZnAl-LDH. Scanning microfocus SAXS investigations show that the ZnAl-LDH is homogeneously distributed in the PP matrix as stacks of 4–5 layers with an intercalated morphology. DSC and WAXS results show that the degree of crystallinity decreases linearly with the increasing content of LDH. The extrapolation of this dependence to zero estimates a limiting concentration of ca. 40% LDH where the crystallization of PP is completely suppressed by the nanofiller. The dielectric spectra of the nanocomposites show several relaxation processes which are discussed in detail. The intensity of the dynamic glass transition (β-relaxation) increases with the concentration of LDH. This is attributed to the increasing concentration of the exchanged anion dodecylbenzenesulfonate (SDBS) which is adsorbed at the LDH layers. Therefore, a detailed analysis of the β-relaxation provides information about the structure and the molecular dynamics in the interfacial region between the LDH layers and the polypropylene matrix which is otherwise dielectrically invisible (low dipole moment). As a main result, it is found that the glass transition temperature in this interfacial region is by 30 K lower than that of pure polypropylene. This is accompanied by a drastic change of the fragility parameter deduced from the relaxation map. KW - Nanocomposites KW - Layered double hydroxide KW - Dielectric spectroscopy KW - X-ray scattering KW - Polypropylene PY - 2011 DO - https://doi.org/10.1021/ma200323k SN - 0024-9297 SN - 1520-5835 VL - 44 IS - 11 SP - 4342 EP - 4354 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Purohit, Purv A1 - Wang, D.-Y. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Heinrich, G. A1 - Schönhals, Andreas T1 - Arrangement of layered double hydroxide in a polyethylene matrix studied by a combination of complementary methods N2 - Organically modified ZnAl Layered Double Hydroxides (ZnAl-LDH) was synthesized and melt blended with polyethylene to obtain nanocomposites. The resulting morphology was investigated by a combination of Differential Scanning Calorimetry (DSC), Small and Wide-angle X-ray scattering (SAXS and WAXS) and dielectric relaxation spectroscopy (DRS). The arrangement (intercalation) of polyethylene chains between LDH stacks was investigated employing SAXS. The homogeneity of the nanocomposites and average number of stack size (4–6 layers) were determined using scanning microfocus SAXS (BESSY II). DSC and WAXS results show that the degree of crystallinity decreases linearly with the increasing content of LDH. The extrapolation of this dependence to zero estimates a limiting concentration of ca. 45% LDH where the crystallization of PE is completely suppressed by the nanofiller. The dielectric spectra of the nanocomposites show several relaxation processes which are discussed in detail. The intensity of the dynamic glass transition (β-relaxation) increases with the concentration of LDH. This is attributed to the increasing concentration of the exchanged anion sodium dodecylbenzene sulfonate (SDBS) which is adsorbed at the LDH layers. Therefore, a detailed analysis of the β-relaxation provides information about the structure and the molecular dynamics in the interfacial region between the LDH layers and the polyethylene matrix which is otherwise dielectrically invisible (low dipole moment). KW - Dielectric spectroscopy KW - Polyethylene nanocomposites KW - Layered double hydroxides PY - 2012 DO - https://doi.org/10.1016/j.polymer.2012.03.041 SN - 0032-3861 SN - 1873-2291 VL - 53 IS - 11 SP - 2245 EP - 2254 PB - Springer CY - Berlin AN - OPUS4-25810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mandel, K. A1 - Szczerba, Wojciech A1 - Thünemann, Andreas A1 - Riesemeier, Heinrich A1 - Girod, Matthias A1 - Sextl, G. T1 - Nitric acid-stabilized superparamagnetic iron oxide nanoparticles studied with X-rays N2 - Agglomerated superparamagnetic iron oxide nanoparticles can easily and in large scale be precipitated from iron salt solutions. Although the process is well known, it is ambiguously either assumed that magnetite or maghemite is obtained. The first part of our study clarifies this question using X-ray absorption spectroscopy. For further processing of the nanoparticles, i.e., for giving them a surface functionality or incorporating them into composites, it is important to break the agglomerates and individualize the particles at first. This can effectively be done with nitric acid treatment. The influence of this process on the particles chemistry and structure was analyzed in great detail using X-ray diffraction, X-ray absorption, and smallangle X-ray scattering. In contrast to our expectation, no oxidation from magnetite (Fe3O4) to maghemite (γ- Fe2O3) was found; the formal valence of the particles in any case is magnetite (Fe3O4). Instead, an increase in the particles' surface disorder was discovered from X-ray absorption analyses and high-resolution transmission electron microscopy. The acid treatment roughens and distorts the surface of the nanoparticles which is connected with an increased spin disorder. KW - XANES KW - EXAFS KW - SAXS KW - Coprecipitation KW - Iron oxide spectra KW - Ferrofluid PY - 2012 DO - https://doi.org/10.1007/s11051-012-1066-3 SN - 1388-0764 SN - 1572-896X VL - 14 IS - 8 SP - 1066/1 EP - 9 PB - Kluwer CY - Dordrecht AN - OPUS4-26357 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 - De Samber, B. A1 - Scharf, Oliver A1 - Buzanich, Günter A1 - Garrevoet, J. A1 - Tack, P. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Evens, R. A1 - De Schamphelaere, K. A1 - Falkenberg, G. A1 - Janssen, C. A1 - Vincze, L. T1 - Three-dimensional X-ray fluorescence imaging modes for biological specimens using a full-field energy dispersive CCD camera N2 - Besides conventional scanning X-ray fluorescence imaging at synchrotron sources, full-field X-ray fluorescence (FF-XRF) imaging techniques that do not implicitly require spatial scanning of the sample have become available. FF-XRF has become achievable thanks to the development of a new type of energy dispersive CCD-based 2D detector, also referred to as a 'color X-ray camera (CXC)' or 'SLcam'. We report on different imaging schemes for biological samples using FF-XRF imaging: (a) 2D 'zoom' imaging with pinhole optics using the 'camera obscura' principle; (b) 2D 'fixed magnification' imaging using magnifying polycapillary optics; and (c) 3D-FF-XRF imaging using an X-ray sheet beam or computed tomography (CT). The different FF-XRF imaging modes are illustrated using the crustacean Daphnia magna, a model organism for investigating the effects of metals on organism/ecosystem health, and foraminifera, a class of amoeboid protist. Detailed analytical characterization of the set-up is performed through analyzing various reference materials in order to determine limits of detection (LODs) and sensitivities. Experiments were performed using the BAMline at the BESSY synchrotron (Berlin, Germany) and using the P06 Hard X-ray Microprobe at the PETRAIII synchrotron (Hamburg, Germany). KW - CXC KW - BAMline KW - Maia detector KW - Synchrotron PY - 2019 DO - https://doi.org/10.1039/c9ja00198k VL - 34 IS - 10 SP - 2083 EP - 2093 PB - Royal Society of Chemistry CY - Cambridge, United Kingdom AN - OPUS4-49359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reiche, I. A1 - Berger, Achim A1 - Bevers, H. A1 - Dupuis, G. A1 - Duval, A. A1 - Görner, Wolf A1 - Guicharnaud, H. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich A1 - Roth, M. T1 - Spatially resolved SR-XRF analyses of complex drawings by the Holbein family and silverpoint drawings by Rembrandt KW - X-ray spectrometry KW - XRF KW - Röntgenfluoreszenzanalyse KW - RFA KW - Silverpoint drawing KW - Silberstiftzeichnung PY - 2005 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2004.pdf#page=491 SN - 0179-4159 SP - 491 EP - 493 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-7380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ordavo, I. A1 - Ihle, S. A1 - Arkadiev, V. A1 - Scharf, Oliver A1 - Soltau, H. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, S. A1 - Buzanich, Günter A1 - Gubzhokov, R. A1 - Günther, A. A1 - Hartmann, R. A1 - Holl, P. A1 - Kimmel, N. A1 - Kühbacher, M. A1 - Lang, M. A1 - Langhoff, N. A1 - Liebel, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Schaller, G. A1 - Schopper, F. A1 - Strüder, L. A1 - Thamm, C. A1 - Wedell, R. T1 - A new pnCCD-based color X-ray camera for fast spatial and energy-resolved measurements N2 - We present a new high resolution X-ray imager based on a pnCCD detector and a polycapillary optics. The properties of the pnCCD like high quantum efficiency, high energy resolution and radiation hardness are maintained, while color corrected polycapillary lenses are used to direct the fluorescence photons from every spot on a sample to a corresponding pixel on the detector. The camera is sensitive to photons from 3 to 40 keV with still 30% quantum efficiency at 20 keV. The pnCCD is operated in split frame mode allowing a high frame rate of 400 Hz with an energy resolution of 152 eV for Mn Kα (5.9 keV) at 450 kcps. In single-photon counting mode (SPC), the time, energy and position of every fluorescence photon is recorded for every frame. A dedicated software enables the visualization of the elements distribution in real time without the need of post-processing the data. A description of the key components including detector, X-ray optics and camera is given. First experiments show the capability of the camera to perform fast full-field X-Ray Fluorescence (FF-XRF) for element analysis. The imaging performance with a magnifying optics (3×) has also been successfully tested. KW - X-ray CCD camera KW - pnCCD KW - Fast X-ray imaging KW - XRF KW - Full-field X-ray fluorescence KW - Elemental analysis KW - High quantum efficiency KW - High energy resolution KW - Polycapillary optics PY - 2011 DO - https://doi.org/10.1016/j.nima.2011.05.080 SN - 0168-9002 SN - 0167-5087 VL - 654 SP - 250 EP - 257 PB - North-Holland CY - Amsterdam AN - OPUS4-24370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kühbacher, M. A1 - Weseloh, G. A1 - Bertelsmann, H. A1 - Özaslan, M. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Kyriakopoulos, A. A1 - Behne, D. T1 - Analysis of metal- and metalloid-containing proteins by SRXRF at the BAMline N2 - Pilot studies have been carried out at the BAMline at BESSY II in collaboration with the Bundesanstalt für Materialforschung und -prüfung (BAM) on metal- and metalloid-containing compounds in biological samples after electrophoretic protein separation. After sodium dodecylsulfate polyacrylamide gel electrophoresis (SDS-PAGE) and transfer onto a blotting membrane the distribution of selenium among the proteins of testis homogenate of a rat and a wallaby was determined. The comparison with the autoradiogram of 75Se-labeled proteins separated in the same way showed that of nine seleniumcontaining proteins found in rat testis homogenate by autoradiography four could be detected by synchrotron radiation X-ray fluorescence analysis (SRXRF). PY - 2003 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2002.pdf#page=333 SN - 0179-4159 SP - 333 EP - 335 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-2495 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 - Nusser, K. A1 - Mosbauer, T. A1 - Schneider, G.J. A1 - Brandt, K. A1 - Weidemann, Gerd A1 - Goebbels, Jürgen A1 - Riesemeier, Heinrich A1 - Göritz, D. T1 - Silica dispersion in styrene butadiene rubber composites studied by synchrotron tomography N2 - By means of synchrotron X-ray computed tomography, model composites consisting of silica and styrene–butadiene rubber were studied with a very high spatial resolution. By our analysis technique we were able to determine the nano- and micro dispersion from the experimental results by our numerical analysis. These results are discussed with respect to crucial advantages of the generically 3-dimensional tomography technique as compared to 2-dimensional methods. Our quantitative analysis of the 3d images demonstrates that in the case of our model composites the filler dispersion is good, independent on the filler concentration. Our new 3-dimensional results evidence that considering only 2-d pictures may lead to ambiguities that can lead to wrong conclusions. KW - X-ray tomography KW - Silica KW - Styrene butadiene rubber KW - Dispersion PY - 2012 DO - https://doi.org/10.1016/j.jnoncrysol.2011.10.009 SN - 0022-3093 VL - 358 IS - 3 SP - 557 EP - 563 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-26105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yao, Dongxu A1 - Xia, Y. A1 - Zuo, K.-h. A1 - Jiang, D. A1 - Günster, Jens A1 - Zeng, Y.-P. A1 - Heinrich, J.G. T1 - Porous Si3N4 ceramics prepared via partial nitridation and SHS N2 - Porous Si3N4 ceramics were prepared via partial nitridation and self-propagating high temperature synthesis (SHS) process. Raw Si and additive Y2O3 were mixed and molded under 10 MPa into a compact, the compact was partial nitridation at 1300 °C to form a porous Si/Si3N4, and then it was buried in a Si/Si3N4 bed for SHS to obtain porous Si3N4 with rod-like β-Si3N4 morphology. The processing combined the advantages of the nitridation of Si and SHS with low cost, low shrinkage and time saving. Porous Si3N4 with a porosity of 47%, a strength of 143 MPa were obtained by this method. KW - Si3N4 KW - Strength KW - Porosity PY - 2013 DO - https://doi.org/10.1016/j.jeurceramsoc.2012.08.033 SN - 0955-2219 SN - 1873-619X VL - 33 IS - 2 SP - 371 EP - 374 PB - Elsevier CY - Oxford AN - OPUS4-31282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Colombo, P. A1 - Günster, Jens A1 - Mühler, T. A1 - Heinrich, J.G. T1 - Selective laser densification of lithium aluminosilicate glass ceramic tapes N2 - Tapes, cast by blade deposition of a lithium aluminosilicate glass slurry, were sintered using a YAG-fiber laser, with the aim of finding suitable parameters for an additive manufacturing process based on layer-wise slurry deposition and selective laser densification. The influence of the laser parameters (output power and scan velocity) on the sintering was evaluated, by scanning electron microscopy and by X-ray diffraction, on the basis of the quality of the processed layer. Well densified samples could be obtained only in a small window of values for the output power and the scan velocity. The measurement of the width of a set of single scanned lines allowed also to estimate the minimum resolution of the system along the layer plane. KW - Selective laser sintering (SLS) KW - Laserwise-slurry-deposition (LSD) KW - Glass-ceramic KW - LAS PY - 2013 UR - http://ac.els-cdn.com/S0169433212020168/1-s2.0-S0169433212020168-main.pdf?_tid=4ba0c92c-31d4-11e4-84f1-00000aab0f02&acdnat=1409575040_15d5256291262aca99cc5321374ab879 DO - https://doi.org/10.1016/j.apsusc.2012.11.058 SN - 0169-4332 SN - 1873-5584 VL - 265 SP - 610 EP - 614 PB - North-Holland CY - Amsterdam AN - OPUS4-31283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wirth, Cynthia A1 - Müller, Ralf A1 - Günster, Jens A1 - Mühler, T. A1 - Görke, R. A1 - Heinrich, J.G. T1 - Submicrometer silica spheres generated by laser fuming N2 - The production of agglomerate-free SiO2 particles exhibiting a monomodal distribution of particle sizes of around 300 nm by means of direct laser fuming of micrometric SiO2 powders has been successfully demonstrated. With a 12 kW cw CO2 laser system, a production rate of up to 1 kilogram powder per hour was achieved. Almost ideal spherical amorphous SiO2 particles in a broad particle size distribution between 10 nm and several 100 nm (d50 ≈ 300 nm) were synthesized. Several observations suggest weak agglomeration forces between the particles. A temperature reduction of 200 °C for sintering powder compacts was observed. KW - Laser KW - SiO2 KW - Nanopowder PY - 2013 DO - https://doi.org/10.4416/JCST2012-00033 SN - 2190-9385 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. VL - 4 IS - 1 SP - 11 EP - 18 PB - Göller CY - Baden-Baden AN - OPUS4-31423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oelgardt, C. A1 - Günster, Jens A1 - Heinrich, J.G. T1 - Characterization of the crystallization behavior of laser-fused transparent microspheres with the eutectic composition Al2O3-Y2O3-ZrO2 (AYZ) N2 - Transparent microspheres with the eutectic composition 65 Al2O3-16 Y2O3-19 ZrO2 (mol%) have been produced by laser fusing with a CO2 laser. The influence of the starting material – not pre-calcined and pre-calcined – as well as the laser power on the resulting microspheres – was investigated. After fabrication, the microspheres were analyzed by means of XRD to quantify the amorphous content of the spheres as well as to identify the residual crystalline phases, with a laser granulometer to measure the particle sizes of the starting material and the resulting microspheres, with DSC to characterize the glass transition temperature and crystallization behavior, and with SEM to investigate the microstructure of the microspheres. The laser-treated materials consist of transparent and opaque beads as well as sintered particles. The amorphous amount in the samples was detected to be ~ 85 %. Based on these results transparent beads were collected and annealed over a range of temperatures to analyze the crystallization behavior. KW - Eutectic ceramics KW - Al2O3-Y2O3-ZrO2 KW - Laser processing KW - Crystallization behavior KW - Microstructure PY - 2011 DO - https://doi.org/10.4416/JCST2011-00010 SN - 2190-9385 VL - 02 IS - 02 SP - 103 EP - 110 PB - Göller CY - Baden-Baden AN - OPUS4-23763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yao, Dongxu A1 - Xia, Y. A1 - Zuo, K.-h. A1 - Jiang, D. A1 - Günster, Jens A1 - Zeng, Y.-P. A1 - Heinrich, J.G. T1 - The effect of fabrication parameters on the mechanical properties of sintered reaction bonded porous Si3N4 ceramics N2 - Porous silicon nitride ceramics were prepared via sintered reaction bonded silicon nitride at 1680 °C. The grain size of nitrided Si3N4 and diameter of post-sintered ß-Si3N4 are controlled by size of raw Si. Porosity of 42.14–46.54% and flexural strength from 141 MPa to 165 MPa were obtained. During post-sintering with nano Y2O3 as sintering additive, nano Y2O3 can promote the formation of small ß-Si3N4 nuclei, but the large amount of ß-Si3N4 (>20%) after nitridation also works as nuclei site for precipitation, in consequence the growth of fine ß-Si3N4 grains is restrained, the length is shortened, and the improvement on flexural strength is minimized. The effect of nano SiC on the refinement of the ß-Si3N4 grains is notable because of the pinning effect, while the effect of nano C on the refinement of the ß-Si3N4 grains is not remarkable due to the carbothermal reaction and increase in viscosity of the liquid phase. KW - Porous ceramics KW - Silicon nitride KW - Reaction bonding KW - Anisotropic grain growth KW - Ceramic PY - 2014 DO - https://doi.org/10.1016/j.jeurceramsoc.2014.06.018 SN - 0955-2219 SN - 1873-619X VL - 34 IS - 15 SP - 3461 EP - 3467 PB - Elsevier CY - Oxford AN - OPUS4-32542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yao, Dongxu A1 - Xia, Y. A1 - Zuo, K.-h. A1 - Zeng, Y.-P. A1 - Jiang, D. A1 - Günster, Jens A1 - Heinrich, J.G. T1 - Gradient porous silicon nitride prepared via vacuum foaming and freeze drying N2 - Gradient porous silicon nitride (Si3N4) was fabricated by a novel vacuum foaming and freeze drying process. Aqueous Si3N4 slurries were foamed at vacuum pressure of 50–90 kPa, the green body was obtained by the freeze drying process, a gradient pore structure with porosities of 72–90% was achieved after pressureless sintering at 1680 °C. The porosity was increased with decreasing vacuum pressure. The pore structure consists of large pores (~100 μm) on top, medium pores (~45 μm) on the wall of the large pores, and small pores (~0.7 μm) in the matrix. Such gradient porous Si3N4 with macro- and micro-pores has potential application as high temperature filters. KW - Silicon nitride KW - Graded PY - 2015 DO - https://doi.org/10.1016/j.matlet.2014.11.067 SN - 0167-577x SN - 1873-4979 VL - 141 SP - 138 EP - 140 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-35177 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hu, H.-L. A1 - Zeng, Y.-P. A1 - Xia, Y. A1 - Yao, Dongxu A1 - Zuo, K.-H. A1 - Günster, Jens A1 - Heinrich, J.G. T1 - Rapid fabrication of porous Si3N4/SiC ceramics via nitridation of silicon powder with ZrO2 as catalyst N2 - Porous Si3N4/SiC ceramics were rapidly prepared with Y2O3 as sintering additive and ZrO2 as nitrided catalyst, using Si and SiC as starting powders. Porous Si3N4/SiC ceramics with 5 wt% ZrO2 addition showed a complete nitridation and good mechanical properties (with a high porosity of 34.96%, flexural strength of 150±4.2 MPa, linear shrinkage of 0.02%). It was revealed that the reciprocal formation of ZrO2 and ZrN effectively enhanced nitridation by inhibiting the melting of silicon in micro-regions. KW - D. ZrO2 KW - Rapid nitridation KW - Si3N4/SiC porous ceramics PY - 2014 DO - https://doi.org/10.1016/j.ceramint.2013.11.098 SN - 0272-8842 SN - 1873-3956 VL - 40 IS - 5 SP - 7579 EP - 7582 PB - Ceramurgia CY - Faenza AN - OPUS4-30295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Kipphardt, Heinrich A1 - del Rocío Arvizu Torres, M. A1 - Manzano, J.V.L. A1 - Rodrigues, J.M. A1 - de Sena, R.C. A1 - Yim, Y.-H. A1 - Heo, S.W. A1 - Zhou, T. A1 - Turk, G.C. A1 - Winchester, M. A1 - Yu, L. L. A1 - Miura, T. A1 - Methven, B. A1 - Sturgeon, R. A1 - Jährling, R. A1 - Rienitz, O. A1 - Tunc, M. A1 - Can, S.Z. T1 - Final report of the key comparison CCQM-K72: Purity of zinc with respect to six defined metallic analytes N2 - KEY COMPARISON High purity elements can serve as a realization of the SI unit amount of substance for the specific element. Solutions prepared from high purity metals by applying gravimetric preparation and the concept of molar mass are used as 'calibration' solutions in many fields of analytical chemistry and provide the metrological basis in elemental analysis. Since ideal purity does not exist for real materials, the actual purity of the high purity material must be known with a specified uncertainty. As required uncertainties around 10-4 relative on the purity statement are not accessible in almost all cases by a direct measurement of the element in itself, the indirect approach is followed, where all elements excepting the matrix element itself are measured and their sum is subtracted from the value for ideal purity, which is 1 kg/kg. It was the aim of this comparison to demonstrate the capability of national metrology institutes and designated institutes to determine the purity of pure elements. In order to limit the effort within this comparison, only six metallic impurities (Ag, Al, Cd, Cr, Ni, Tl) in the low mg/kg range are considered in a zinc matrix. It has to be underlined here that the task was to measure the purity of zinc based on the determination of six analytes. The task is not trace analysis of specific analytes in zinc. This subtle distinction defines different measurands. The sample, pure Zn, was cut in pieces of cubic geometry for wet chemical analysis or of pin geometry for GDMS analysis and was sent to the participants. The comparison was run under the auspices of the Inorganic analysis Working Group (IAWG) of the CCQM and was piloted by the BAM Federal Institute for Materials Research and Testing, Berlin, Germany. The majority of the participants applied ICP-MS techniques and only two participants used additionally atomic absorption spectrometry. GDMS was used only by one participant. The observed spreads for the measurement results reported by the participants were significantly lower than those of the preceding study CCQM-P107 and were well below the target uncertainty of 30% relative. As a consequence, comparability within the participating laboratories is demonstrated to be established. The individual measurement results, mean values and medians derived were in all cases very consistent with the reference values obtained by IDMS and so the accuracy of the measurement results for the participating laboratories is as well demonstrated to be established. Especially with the results of CCQM-P62 and CCQM-P107 in mind, the outcome of CCQM-K72 can be considered as a big step forward in the community. CCQM is aware of the difference between a characterization based on only six analytes and a complete characterization. Therefore, the pilot study CCQM-P149 has been initiated and already started, which focuses on the fit-for-purpose approaches for the purity determination of metals (here: zinc) to be used as primary standards in elemental analysis. Another follow-up in the form of a pilot study on non-metal impurities is mandatory, because non-metal impurities such as oxygen, nitrogen and sulfur often make up the largest contributions. 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 (CIPM MRA). KW - CCQM KW - Metrology KW - Purity PY - 2014 DO - https://doi.org/10.1088/0026-1394/51/1A/08008 SN - 0026-1394 SN - 1681-7575 VL - 51 IS - 1A (Tech.Suppl. 2014) SP - 08008, 1 EP - 40 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-30772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Schott, M. A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Kurth, D.G. T1 - Thermally induced structural rearrangement of the Fe(II) coordination geometry in metallo-supramolecular polyelectrolytes N2 - Rigid rod-type metallo-supramolecular coordination polyelectrolytes with Fe(II) centres (Fe-MEPEs) are produced via the self-assembly of the ditopic ligand 1,4-bis(2,2':6',2''-terpyridine-4'-yl)benzene (tpy-ph-tpy) and Fe(II) acetate. Fe-MEPEs exhibit remarkable electrochromic properties; they change colour from blue to transparent when an electric potential is applied. This electrochemical process is generally reversible. The blue colour in the ground state is a result of a metal-to-ligand charge transfer at the Fe(II) centre ion in a quasi-octahedral geometry. When annealed at temperatures above 100 °C, the blue colour turns into green and the formerly reversible electrochromic properties are lost, even after cooling down to room temperature. The thermally induced changes in the Fe(II) coordination sphere are investigated in situ during annealing of a solid Fe-MEPE using X-ray absorption fine structure (XAFS) spectroscopy. The study reveals that the thermally induced transition is not accompanied by a redox process at the Fe(II) centre. From the detailed analysis of the XAFS spectra, the changes are attributed to structural changes in the coordination sphere of the Fe(II) site. In the low temperature state, the Fe(II) ion rests in a quasi-octahedral coordination environment surrounded by six nitrogen atoms of the pyridine rings. The axial Fe–N bond length is 1.94 Å, while the equatorial bond length amounts to 1.98 Å. In the high temperature state, the FeN6-site exhibits a distortion with the axial Fe–N bonds being shortened to 1.88 Å and the equatorial Fe–N bonds being elongated to 2.01 Å. KW - Metallo-supramolecular polyelectrolytes KW - Electrochromism KW - XANES KW - EXAFS KW - Local structure KW - Thermal stability PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-317331 DO - https://doi.org/10.1039/c4cp01187b SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 36 SP - 19694 EP - 19701 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-31733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -