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 - TY - CONF A1 - Thomas, Sebastian T1 - WP8 RCS standardisation work, probabilistic safety assessment & statistic - PSB meeting #3 N2 - Achievements within WP8 in the TAHYA Project during the month 18 to 24, including ongoing work and next steps. Including safety definition, introduction to probabilistic Approach, failure rate, consequence and risk Definition, introduction monte-carlo-Simulation. T2 - TAHYA PSB meeting 3 CY - Berlin, Germany DA - 28.11.2019 KW - TAHYA project PY - 2019 AN - OPUS4-50118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bouabadi, Bouchra A1 - Hilger, André A1 - Kamm, Paul H. A1 - Neu, Tillmann R. A1 - Kardjilov, Nikolay A1 - Sintschuk, Michael A1 - Markötter, Henning A1 - Schedel‐Niedrig, Thomas A1 - Abou‐Ras, Daniel A1 - García‐Moreno, Francisco A1 - Risse, Sebastian T1 - Morphological Evolution of Sn‐Metal‐Based Anodes for Lithium‐Ion Batteries Using Operando X‐Ray Imaging N2 - Sn‐based electrodes are promising candidates for next‐generation lithium‐ion batteries. However, it suffers from deleterious micro‐structural deformation as it undergoes drastic volume changes upon lithium insertion and extraction. Progress in designing these materials is limited to complex structures. There is a significant need to develop an alloy‐based anode that can be industrially manufactured and offers high reversible capacity. This necessitates a profound understanding of the interplay between structural changes and electrochemical performance. Here, operando X‐ray imaging is used to correlate the morphological evolution to electrochemical performance in foil and foam systems. The 3D Sn‐foam‐like structure electrode is fabricated in‐house as a practical approach to accommodate the volume expansion and alleviate the mechanical stress experienced upon alloying/dealloying. Results show that generating pores in Sn electrodes can help manage the volume expansion and mitigate the severe mechanical stress in thick electrodes during alloying/dealloying processes. The foam electrode demonstrates superior electrochemical performance compared to non‐porous Sn foil with an equivalent absolute capacity. This work advances the understanding of the real‐time morphological evolution of Sn bulky electrodes. KW - Synchrotron radiation KW - X-ray imaging KW - Lithium-ion battery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640112 DO - https://doi.org/10.1002/advs.202414892 SN - 2198-3844 VL - 12 IS - 10 SP - 1 EP - 10 PB - Wiley AN - OPUS4-64011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peters, Stefan A1 - Kunkel, Benny A1 - Cakir, Cafer Tufan A1 - Kabelitz, Anke A1 - Witte, Steffen A1 - Bernstein, Thomas A1 - Bartling, Stephan A1 - Radtke, Martin A1 - Emmerling, Franziska A1 - Abdel-Mageed, Ali Mohamed A1 - Wohlrab, Sebastian A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy N2 - A novel setup for dispersive X-ray absorption spectroscopy (XAS) with simultaneous resolution of space, time and energy for in situ characterization of solid materials is demonstrated. KW - Dispersive XAS KW - Catalysis KW - In situ KW - Structure analysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584924 DO - https://doi.org/10.1039/d3cc03277a SN - 1359-7345 SP - 1 EP - 4 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -