TY - JOUR A1 - Durlo Tambara, Luís Urbano A1 - Nikoonasab, Ali A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Gluth, Gregor T1 - Determination of the oxidation depths of ground granulated blast furnace slag-containing cement pastes using Mn K-edge X-ray absorption near-edge structure spectroscopy N2 - The redox potential of the pore solution of hardened cements containing ground granulated blast furnace slag (GGBFS) affects reinforcement corrosion and immobilization of radioactive waste. Here, Mn K-edge X-ray absorption near-edge structure (XANES) spectroscopy was applied to determine the depth profile of the oxidation state of manganese in hardened GGBFS-containing cement pastes. Manganese was oxidized in the outer regions of some of the pastes, but the depth to which this occurred was not identical with the ‘blue-green/white color change front’, usually interpreted as indicating oxidation of sulfur species. For CEM III/B, the color change of the material was gradual and thus unsuitable for a precise determination of the oxidation depth, while for the alkali-activated slag, a distinct color change front was found, but full oxidation of manganese and sulfur had not occurred in the brighter region. Mn K-edge XANES spectroscopy is thus a more reliable method than the determination of the visual color change front to follow the ingress of the oxidation front. KW - Manganese KW - Oxidation KW - Sulfide KW - Alkali-activated materials KW - Redox conditions PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651469 DO - https://doi.org/10.1111/jace.70445 SN - 0002-7820 SN - 1551-2916 VL - 109 IS - 1 SP - 1 EP - 11 PB - Wiley CY - Oxford AN - OPUS4-65146 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roters, F. A1 - Aslam, A. A1 - Bai, Y. A1 - Büschelberger, M. A1 - Bulert, K. A1 - Butz, A. A1 - Hickel, Tilmann A1 - Jogi, T. A1 - Klitschke, S. A1 - Martin, M. A1 - Meyer, L.-P. A1 - Morand, L. A1 - Nahshon, Y. A1 - Radtke, N. A1 - Saikia, Ujjal A1 - Trondl, A. A1 - Wessel, A. A1 - Zierep, P. A1 - Helm, D. T1 - StahlDigital: Ontology-Based Workflows for the Steel Industry N2 - The innovative strength of the steel industry is based on the mastery of microstructure–property relationships. Digital workflows can largely contribute to this aim by making the complexity of workflows reproducible and their execution user independent. In this work, the tools and workflows developed in the project StahlDigital as part of the German MaterialDigital initiative are presented and application examples are provided. A steel ontology builds the foundation for data collection and storage as well as for the semantic description of experimental and simulation data processing workflows. A dataspace powered by the Dataspace Management System (DSMS) digitally represents such workflows and manages data along them in a Findable, Accessible, Interoperable, Reusable manner aiming to derive new knowledge. Experimental data processed via DSMS can be further evaluated and used as input for simulation workflows. The simulations included in such workflows are run by the workflow system pyiron, which has been semantically extended in StahlDigital for this purpose. KW - Steel KW - Rolling KW - Multiscale simulation KW - Ontology KW - Workflow PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627187 DO - https://doi.org/10.1002/adem.202402148 SN - 1527-2648 SP - 1 EP - 13 PB - Wiley VHC-Verlag AN - OPUS4-62718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Schäfers, F. A1 - Adam, Christian T1 - Chemical state of chromium, sulfur, and iron in sewage sludge ash based phosphorus fertilizers N2 - As an essential element of all life forms, phosphorus (P) is vital to the fertilizer industry. With decreasing quantity and quality of phosphate rock resources, recycling P-fertilizers from wastewater is of increasing interest. The P-fertilizer products of a recently developed thermochemical process for P recovery from sewage sludge ash (SSA) were investigated by chromium, sulfur, and iron K-edge X-ray near-edge structure (XANES) spectroscopy. This paper focuses the formation and prevention of toxic chromium(VI) and toxic sulfides during the thermochemical processes. Reducing conditions prevent the oxidation of chromium(III) in the SSA to toxic chromium(VI). Sulfides formed under the reducing conditions are nontoxic iron sulfides. Hematite (Fe2O3) present in the SSA is reduced to magnetite (Fe3O4). A gentle post-treatment at 400 °C under oxidizing conditions converts the iron sulfides into plant-available iron sulfates. This oxidative post-treatment does not form undesired chromium(VI) compounds. KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Phosphorus recovery KW - Sewage sludge ash KW - Chromium KW - Sulfur KW - Iron PY - 2015 DO - https://doi.org/10.1021/acssuschemeng.5b00678 SN - 2168-0485 VL - 3 IS - 10 SP - 2376 EP - 2380 PB - ACS Publ. CY - Washington, DC AN - OPUS4-34166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valentim Gelamo, Rogério A1 - Bueno Leite, Natália A1 - de Sousa Amadeu, Nader A1 - Reis Pedreira Muniz Tavares, Michel A1 - Oberschmidt, Dirk A1 - Klemm, Sophie A1 - Fleck, Claudia A1 - Cakir, Cafer-Tufan A1 - Radtke, Martin A1 - Aparecido Moreto, Jéferson T1 - Exploring the Nb2O5 coating deposited on the Ti-6Al-4V alloy by a novel GE-XANES technique and nanoindentation load-depth N2 - This research group has been demonstrating the significant advantages of using Nb2O5 coatings for functionalizing titanium, aluminium, and stainless steels. Regarding the biomedical sector and considering Ti-6Al-4V alloy, the reactive sputtering technique improved the cell viability, the osteogenic performance of cells involved in the osseointegration process as well as the ability to delay bacterial proliferation. The characteristics of the Nb2O5 coatings were assessed before by using standard methods, which provide information only a few tens of nanometers depth. Given that the Nb2O5 coating fabricated in this work exhibits a thickness of approximately 300 nm, the GE-XANES technique emerges as the most suitable method for this analysis. Additional information was provided with the aid of nanoindentation load-depth (P-h) curves. GE-XANES results indicated the formation of a homogeneous layer of Nb2O5 coating on the Ti-6Al-4V surfaces. The deposition process improved the surface hardness of the Ti-6Al-4V alloy (4.38 GPa versus 5.62 GPa) considering the 2 mN load. KW - BAMline KW - GE-XANES KW - Synchrotron PY - 2024 DO - https://doi.org/10.1016/j.matlet.2023.135584 SN - 0167-577X VL - 355 SP - 1 EP - 4 PB - Elsevier B.V. AN - OPUS4-60835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cancella, Erick Paiva A1 - de Paula Guarnieri, Guilherme A1 - de Sousa Amadeu, Nader A1 - Radtke, Martin A1 - Garcia, Rodrigo Henrique A1 - de Azevedo, Eduardo Ribeiro A1 - Cosentino, Ivana Conte A1 - Mascarenhas, Yvonne Primerano A1 - Nery, José Geraldo T1 - Synthesis and physicochemical characterization of a novel bismuth silicate templated by tetrapropylammonium bromide and polydiallyldimethylammonium chloride N2 - A bismuth silicate (BiSi-1) was hydrothermally synthesized using tetrapropylammonium bromide (TPA·Br) as the organic structure-directing agent and shown by multi-scale characterization to be distinct from known Bi–silicates. Powder X-ray diffraction is indexable with an orthorhombic metric (a = 23.234 Å, b = 17.109 Å, c = 3.897 Å), consistent with a highly anisotropic, possibly layered framework. High-resolution TEM/SAED reveals nanocrystalline, plate-like domains assembled into sub-micrometric aggregates with locally oriented lamellae; lattice fringes (0.27–0.32 nm) match the strongest XRD spacings. Solid-state NMR establishes a silica-rich network with a dominant Q4 population (77%) and minor Q3 (11%) and Q2 (12%) sites; the contact-time dependence of 1H to 29Si cross-polarization is consistent with increasing proximal-proton density from Q4 to Q2. Aging to 24 h sharpens the 29Si lineshape, while calcination progressively removes the OSDA and vicinal hydroxyls; at 750 °C, 29Si spectra indicate framework densification/rearrangement. XANES/EXAFS places bismuth predominantly as Bi3+ in an oxide-like environment with a pronounced Bi–O first shell and no detectable Bi⁰ or Bi–Br contributions. ICP–OES yields a reproducible Bi/Si atomic ratio of 1:3. Thermogravimetry shows stepwise desorption, dehydroxylation, and template removal, with thermal stability maintained to 750 °C. Nitrogen sorption confirms mesoporosity in the as-made and Soxhlet-extracted solids (the latter exhibiting the highest surface area), whereas high-temperature calcination reduces porosity. Collectively, BiSi-1 emerges as a nanocrystalline, anisotropic Bi–silicate whose connectivity, local Bi–O environment, and accessible texture are tunable by aging and post-treatments, positioning it as a promising platform for heterogeneous catalysis and environmental remediation. KW - 29Si NMR KW - Bismuth KW - Silicate PY - 2025 DO - https://doi.org/10.1007/s10853-025-11732-6 SN - 0022-2461 VL - 60 IS - 45 SP - 22615 EP - 22635 PB - Springer Science and Business Media LLC AN - OPUS4-64755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - Witte, S. A1 - Beyer, S. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, H. A1 - Streli, C. T1 - A new experimental setup for time- and laterally-resolved X-ray absorption fine structure spectroscopy in a 'single shot' N2 - In this work, a new setup for dispersive XAFS measurements is presented. This reproducible and scanningfree setup yields both time- and laterally-resolved XAFS experiments in a ‘single-shot’. It allows a straightforward adjustment for probing different elements covering many relevant applications in materials science. An incoming energetic broadband beam is diffracted by a Si (111) crystal after passing through the sample and collected by an area sensitive detector. Depending on the energy range of the incoming beam, XANES and/or EXAFS spectra can be recorded with a time resolution down to 1 s. The feasibility of this setup was demonstrated at the BAMline at BESSY II (Berlin, Germany) with reference Fe and Cu foils and the results are hereby presented and discussed. Additionally, an application where time resolution on the second scale is required is briefly evaluated. The presented example concerns studying early stages of zinc(II)2-methylimidazolate (ZIF-8) crystallization. This is particularly important for biomedical applications. KW - X-ray spectroscopy KW - X-ray absorption fine structure KW - Time-resolved KW - Laterally-resolved KW - Experimental setup PY - 2019 DO - https://doi.org/10.1039/c8ja00313k SN - 0267-9477 SN - 1364-5544 VL - 34 IS - 1 SP - 239 EP - 246 PB - Royal Society of Chemistry CY - London AN - OPUS4-47207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Vincze, L. A1 - Reuter, Dirk T1 - X-ray scattering in X-ray fluorescence spectra with X-ray monochromatic, polarised excitation - modelling, experiment, and Monte-Carlo simulation N2 - A systematic series of measurements has been carried out with monochromatic X-ray excitation with synchrotron radiation in order to check a physical model on X-ray scattering. The model has recently been successfully tested for the case of polychromatic, unpolarised excitation emitted by an X-ray tube. Our main purpose is the modelling of a physical background in X-ray fluorescence spectra, so that improved quantitative results can be achieved especially for strongly scattering specimens. The model includes single Rayleigh and Compton scattering in the specimen, the effect of bound electrons, the challenging Compton broadening and the polarisation degree. Representative specimens, measurement geometries and excitation energies have been selected with synchrotron monochromatic light at BAMline/BESSY II. Monte-Carlo simulations have been also carried out in order to evaluate the quality of the results achieved with the model. KW - X-ray scattering KW - Monochromatic excitation KW - Polarisation KW - Modelling KW - Monte-Carlo simulation PY - 2011 DO - https://doi.org/10.1016/j.nimb.2011.04.009 SN - 0168-583X SN - 1872-9584 VL - 269 IS - 13 SP - 1493 EP - 1498 PB - Elsevier CY - Amsterdam AN - OPUS4-23765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Michael A1 - Buzanich, Günter A1 - Jähn, Katharina A1 - Reinholz, Uwe A1 - Radtke, Martin T1 - Analysis of cobalt deposition in periprosthetic bone specimens by high-resolution synchroton XRF in undecalcified histological thin sections N2 - Increasing numbers of implant revisions are a current clinical issue. Interactions of the endoprosthesis biomaterial with the body affect implantation time by wear processes, i.e. corrosion and abrasion. Previously, cobalt-chrome implants were shown to cause high levels of cobalt ions being deposited in the bone matrix. To determine a poten- tial functional role of these ions on bone homeostasis, we have developed a non-destructive dual analysis of highly sensitive elemental analysis by synchrotron XRF directly in undecalcified histological bone thin sections (4 μm). In this study, samples from 28 bone samples from hip endoprosthesis carriers (Surface Replacement Arthroplasty, metal-on-metal bearing) with an implant lifetime of 17–1750 days were used. Results were compared to age- matched control specimens. The histological analysis identified areas of bone cell activity and assigned them for XRF measurements. Co-Cr wear particles were identified in the bone marrow. In addition, Co ions were highly enriched in the mineralized bone matrix. The cobalt deposits were not homogeneously distributed, and areas of high signal intensity were identified. Co was distinctly deposited in the newly formed osteoid layer, but also within deeper layers of the bone matrix, whereby the Co concentration increased with higher degrees of bone matrix mineralization. In the current study, we determined cobalt accumulations in the bone matrix and showed for the first time via synchrotron XRF with a high spatial resolution direct on histological slides, that cobalt deposits in the mineralized bone matrix in a mineral-specific way that is dependent upon the implant lifetime. KW - Implant material KW - Cobalt deposition KW - Bone matrix KW - High-resolution synchrotron XRF KW - Histology PY - 2019 DO - https://doi.org/10.1016/j.mtla.2019.100290 SN - 2589-1529 VL - 6 SP - 100290, 1 EP - 8 PB - Elsevier Inc. CY - Amsterdam, Niederlande AN - OPUS4-47620 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 - JOUR A1 - Fittschen, U.E.A. A1 - Möckel, R. A1 - Schreiner, M. A1 - klinger, M. A1 - Radtke, Martin A1 - Meyer, B. A1 - Guhl, S. A1 - Renno, A. A1 - Godinho, J. A1 - Gloaguen, R. A1 - Gutzmer, J. T1 - Bundling analytical capacities to understand phase formation in recycling of functional materials N2 - Transitioning from combustion engine-driven transportation to e-mobility demands a paradigm shift – from a system geared to maximize energy efficiency (i.e. fuel consumption) to a system that may be constrained by the availability of high technology (critical) metals required for electrical energy storage systems and drives. In the wake of these developments efforts in securing new resources of these metals from recycling of end-of-life products are increasing steadily. Recycling of Li-Ion batteries has recently been evaluated. The results pinpoint to a critical need for understanding slag Formation and its dependence on metal components like Mn under extreme conditions. This will allow researchers to predict optimal Operation setting and to react quickly to changing market demands (which may be Li or Co at one point but may also shift to Ni or rare earth elements (REE)). The long-term goal is to control the formation of specific phases in slags allowing for a Maximum yield of elements of interest and optimal recovery in the separation processes that follows. The combination of data on the physical micro structure and local chemistry of the multi-Phase products during and after processing will help to understand and derive thermodynamic and kinetic data on its formation. In this paper we are giving an overview on the analytical challenges and approaches to provide robust data on local element concentration and species (especially Mn which is a common component of next generation Li-ion batteries cathodes), spanning the dimensions from the nanometer scale to the bulk material. The complementary interactions of X-rays and electrons make them ideal probes to collect Interface and “in-depth” information. Before- and -after studies as well as in situ structural changes and Phase (trans)formation, changes in elemental and elemental species (e.g. oxidation state) distribution may be tracked by X-ray diffraction (XRD), X-ray fluorescence microscopy and X-ray Absorption spectroscopy. The application of such advanced analytical tools will not only provide essential clues during early lab-based experiments towards the development of new recycling technologies, but may also be deployed for on-line and in-line monitoring of industrial processes. KW - Synchrotron KW - XANES KW - Slags KW - Battery PY - 2019 DO - https://doi.org/10.4028/www.scientific.net/MSF.959.183 SN - 1662-9752 VL - 959 SP - 183 EP - 190 PB - Trans Tech Publ. AN - OPUS4-48900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning for direct quantification of XRF measurements N2 - In X-ray fluorescence (XRF), a sample is excited with X-rays, and the resulting characteristic radiation is detected to detect elements quantitatively and qualitatively. Quantification is traditionally done in several steps: 1. Normalization of the data 2. Determination of the existing elements 3. Fit of the measured spectrum 4. Calculation of concentrations with fundamental parameters / MC simulations / standard based The problem with standard based procedures is the availability of corresponding standards. The problem with the calculations is that the measured intensities for XRF measurements are matrix-dependent. Calculations must, therefore, be performed iteratively (= time consuming) in order to determine the chemical composition. First experiments with gold samples have shown the feasibility of machine learning based quantification in principle. A large number of compositions were simulated (> 10000) and analyzed with a deep learning network. For first experiments, an ANN (Artificial Neural Network) with 3 hidden layers and 33x33x33 neurons was used. This network learned the mapping of spectra to concentrations using supervised learning by multidimensional regression. The input layer was formed by the normalized spectrum, and the output layer directly yielded the searched values. The applicability for real samples was shown by measurements on certified reference materials. T2 - Denver X-ray Conference CY - Lombard, IL, USA DA - 05.08.2019 KW - Machine learning KW - Artificial intelligence KW - Neural network KW - XRF KW - Synchrotron PY - 2019 AN - OPUS4-48903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Lippitz, Andreas A1 - Hodoroaba, Vasile-Dan A1 - Schmid, Thomas A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Zirconium permanent modifiers for graphite furnaces used in absorption spectrometry: understanding their structure and mechanism of action N2 - The mechanism of action of zirconium permanent modifiers on graphite surfaces was investigated in order to understand its influence on the analytical signal in atomic and molecular absorption spectrometry (AAS/MAS). For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEMEDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. We propose here a mechanism, where ZrO2 acts as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. No evidence of the formation of zirconium carbide was found. Consequently, as the CaF formation is catalysed by a heterogeneous catalyst, surface modifications with ZrO2 nanoparticles and ZrO xerogels were investigated in order to increase the surface area. Their influence was evaluated in the molecule formation of CaF, CaCl, CaBr, and CaI. Graphite furnace modification with zirconium oxide nanoparticles proves to be the best choice for fluorine analysis with a signal enhancement of more than eleven times with respect a non-coated graphite furnace. However, the influence of zirconium modifications in the analytical signals of Cl, and I is lower than the F signals or even negative in case of the Br. Understanding zirconium modifiers as heterogeneous catalysts offers a new perspective to AAS and MAS, and reveals the potential of surface analytical methods for development of improved permanent modifiers and graphite furnace coatings. KW - Zirconium KW - HR-CS-MAS KW - Graphite furnace KW - Nanoparticles KW - Xerogel KW - Calcium monofluoride KW - Absorption spectrometry PY - 2018 UR - https://pubs.rsc.org/en/content/articlelanding/2018/ja/c8ja00190a DO - https://doi.org/10.1039/C8JA00190A SN - 0267-9477 VL - 33 IS - 12 SP - 2034 EP - 2042 PB - Royal Society of Chemistry AN - OPUS4-46775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -