TY - JOUR A1 - Chambers, M. S. A1 - Hunter, R. D. A1 - Hollamby, M. J. A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Danks, A. E. A1 - Schnepp, Z. T1 - In Situ and Ex Situ X‑ray Diffraction and Small-Angle X‑ray Scattering Investigations of the Sol−Gel Synthesis of Fe3N and Fe3C N2 - Iron nitride (Fe3N) and iron carbide (Fe3C) nanoparticles can be prepared via sol−gel synthesis. While sol−gel methods are simple, it can be difficult to control the crystalline composition, i.e., to achieve a Rietveld-pure product. In a previous in situ synchrotron study of the sol−gel synthesis of Fe3N/Fe3C, we showed that the reaction proceeds as follows: Fe3O4 → FeOx → Fe3N → Fe3C. There was considerable overlap between the different phases, but we were unable to ascertain whether this was due to the experimental setup (side-on heating of a quartz capillary which could lead to thermal gradients) or whether individual particle reactions proceed at different rates. In this paper, we use in situ wide- and small-angle X-ray scattering (wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS)) to demonstrate that the overlapping phases are indeed due to variable reaction rates. While the initial oxide nanoparticles have a small range of diameters, the size range expands considerably and very rapidly during the oxide−nitride transition. This has implications for the isolation of Rietveld-pure Fe3N, and in an extensive laboratory study, we were indeed unable to isolate phasepure Fe3N. However, we made the surprising discovery that Rietveld-pure Fe3C nanoparticles can be produced at 500 °C with a sufficient furnace dwell time. This is considerably lower than the previous reports of the sol−gel synthesis of Fe3C nanoparticles. KW - Small-angle X-ray Scattering KW - SAXS KW - Diffraction KW - XRD KW - Scattering KW - Sol-gel KW - Iron nitride KW - Nanoparticles KW - Iron carbide KW - Catalyst KW - In-situ KW - Ex-situ KW - Synthesis KW - Synchrotron PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548226 DO - https://doi.org/10.1021/acs.inorgchem.1c03442 VL - 61 IS - 18 SP - 6742 EP - 6749 PB - ACS Publications CY - Washington AN - OPUS4-54822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Combination of complementary methods For in situ studies N2 - This talk explores the synergistic application of complementary synchrotron methods for in situ investigations, providing a comprehensive approach to enhance analytical capabilities in materials research and characterization. T2 - INSYNX - DEUTSCH-BRASILIANISCHER WORKSHOP ON BREAKING BOUNDARIES OF IN SITU SYNCHROTRON X-RAY METHODS CY - Sao Paulo, Brazil DA - 06.03.2023 KW - In situ KW - Synchrotron PY - 2023 AN - OPUS4-59025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matamoros-Veloza, A. A1 - Stawski, Tomasz A1 - Vargas, S. A1 - Neville, A. T1 - Study of a Local Structure at the Interface between Corrosion Films and Carbon Steel Surface in Undersaturated CO2 Environments N2 - Industries transporting CO2 gas-saturated fluids have infrastructures made of carbon steel. This is a good material with great mechanical properties but prone to corrosion and potential failure. Corrosion in sweet environments involves the formation of FeCO3 as a corrosion film, which is recognized to play a protective role under certain conditions. This work on the dissolution of corrosion films in sweet environments, under acidic and undersaturated conditions, demonstrates that the effects on the integrity of steel are far more significant than the damage observed on the surface of the corrosion film. Our results prove that dissolution of FeCO3 involved the presence of an amorphous phase, the intermediate formation of FeCl2 or FeCl+, and the presence of a phase with short distance atom–atom correlations. The amorphous phase was identified as a mixture of retained γ-Fe and Fe3C. Partially broken α-Fe and Fe3C structures were identified to prove the damage on the material, confirming the interface zone without evident damage on the corrosion film. Dissolution affected both the α-Fe and FeCO3, with the lattice [102̅] from the FeCO3 crystalline structure being the fastest to dissolve. The damage of steel at the molecular scale was evident at the macroscale with pit depths of up to 250 μm. The impact on the integrity of steel can be, therefore, more drastic than frequently reported in industrial operations of CO2 transport industries that use cleaning procedures (e.g., acid treatment, pigging) as part of their operational activities. KW - Steel KW - Corrosion KW - Siderite KW - Diffraction KW - Pair distribution function KW - Synchrotron PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572156 DO - https://doi.org/10.1021/acsomega.2c07631 SN - 2470-1343 VL - 8 IS - 9 SP - 8497 EP - 8504 PB - ACS AN - OPUS4-57215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - Synchrotron based absorption edge tomography for §D characterization of the microstructure of MG-Y-Zn alloys N2 - Absorption edge tomography is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. The beamline BAMline at BESSY II, which is operated by the Federal Institute for Materials Research and Testing, can provide a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%. Together with the microtomography setup, this enables differential tomography sensitive to any element with N >= 24 (Cr) by using an appropriate K- or L-edge in this range. Here, absorption edge tomography at the Yttrium edge is employed to perform a non-destructive 3D characterization of the microstructure of a high strength Mg-Y-Zn alloy. The long period stacking ordered (LPSO) phase which forms fibres in this material was extracted based on the Yttrium content and the fibre length distribution was analysed. T2 - Ninth Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Synchrotron KW - Computed Tomography KW - Absorption edge KW - BAMline PY - 2017 AN - OPUS4-43854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfretzschner, Beate T1 - In-situ ED-XRD und Radiographie während eines Zugversuchs an wasserstoffbeladenem Supermartensit N2 - In diesem Vortrag werden Ergebnisse von in situ Experimenten am Berliner Elektronenspeicherring (BESSY II) vorgestellt. Es wurden Zugversuche an wasserstoffbeladenen und wasserstofffreien supermartensitischen Proben durchgeführt und gleichzeitig sowohl Diffraktionsspektren als auch röntgenradiographische Bilder aufgenommen. Die energiedispersive Röntgendiffraktion ermöglichte dabei in-situ die dehnungsinduzierte Phasenumwandlung von Restaustenit zu Martensit zu beobachten. Die Radiographiebilder der zerreisenden Probe gaben Einblicke in das Bruchverhalten in Abhängigkeit vom Wasserstoffgehalt des Supermartensits. T2 - WerkstoffWoche 2017 CY - Dresden, Germany DA - 27.09.2017 KW - Synchrotron KW - Wasserstoff KW - Phasenumwandlung PY - 2017 AN - OPUS4-42625 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - Synchrotron based absorption edge tomography for 3D characterization of the microstructure of Mg-Y-Zn alloys N2 - Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the BundesanstaltfürMaterialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well. In this work, the absorption edge tomography is employed to perform a non-destructive, three-dimensional characterization of the microstructure of metallic alloys. As an example, a high strength Mg-Y-Zn alloy containing long period stacking ordered (LPSO) phases is analysed. The alloy with a nominal composition of Mg97Y2Zn1 was synthesized by melting highly pure magnesium, zinc and a Mg-22%Y master alloy and casting an ingot, which was homogenised at 350 °C and then extruded using an extrusion ratio of 18:1. The results demonstrate that synchrotron based absorption edge tomography is a promising technique to perform a 3D characterization of the microstructure of metallic alloys. T2 - iCT 2018 CY - Wels, Austria DA - 13.02.2018 KW - Absorption edge KW - Synchrotron KW - Alloy KW - Tomography PY - 2018 AN - OPUS4-46427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stawski, Tomasz M. A1 - Salvalaglio, Matteo A1 - Wallace, Adam F. A1 - De Yoreo, James J. T1 - The Birth of Minerals: From Single Step to Multiple Step Mechanisms N2 - Mineral formation from ions in aqueous solutions begins with complex initial stages, where amorphous and liquid-like precursors play pivotal roles before crystalline growth occurs. Both classical and non-classical nucleation and growth theories, introduced in previous chapters, offer explanations, each with their own strengths and limitations, for the complex intermediate phases observed in experimental research. Analytical techniques play a critical role in detecting and characterizing precursor phases, offering valuable insights into nucleation and growth mechanisms across various temporal and spatial scales. Molecular dynamics and modelling provide in-depth perspectives on these phases, allowing for a closer examination of their nucleation and growth mechanisms at the molecular level, and revealing the intricate processes that govern their behaviour. KW - Crystallisation KW - Nucleation KW - Synchrotron KW - Thermodynamics KW - Minerals PY - 2025 DO - https://doi.org/10.2138/gselements.21.1.25 SN - 1811-5217 VL - 21 IS - 1 SP - 25 EP - 32 PB - Mineralogical Society of America AN - OPUS4-62841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz T1 - Scattering is a powerful tool to follow nucleation and growth of minerals from solutions N2 - In recent years, we have come to appreciate the astounding intricacy of the processes leading to the formation of minerals from ions in aqueous solutions. The original, and rather naive, ‘textbook’ image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. Does it, however, mean that all the minerals grow through intermediate phases, following a non-classical pathway? In general, the precursor or intermediate species constitute different, often short-lived, points along the pathway from dissolved ions to the final solids (typically crystals in this context). In this regard synchrotron-based scattering (SAXS/WAXS/total scattering) appears to be the perfect tool to follow in situ and in a time-resolved manner the crystallization pathway because of the temporal and spatial length scales that can be directly accessed with these techniques. In this presentation we show how we used scattering to probe the crystallisation mechanisms of calcium sulfate, This system contains minerals that are widespread in diverse natural environments, but they are also important in various industrial settings. Our data demonstrate that calcium sulfate precipitation involves formation and aggregation of sub-3 nm anisotropic primary species. The actual crystallisation and formation of imperfect single crystals of calcium sulfate phases, takes place from the inside of the in itial aggregates. Hence, calcium sulfate follows a non-classical pathway. T2 - X-ray Powder Diffraction at DESY - new opportunities for research and industry CY - Online meeting DA - 22.06.2020 KW - Nucleation KW - Calcium sulfate KW - Diffraction KW - Scattering KW - Synchrotron KW - SAXS/WAXS PY - 2020 AN - OPUS4-50943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scheffler, F. A1 - Tielemann, Christopher T1 - Crystallization of glasses studied with PEEM N2 - A heat treated glass that formed crystals under controlled conditions can be a glass ceramic. A proper understanding of crystallization in glassy melts is needed yet still lacking. Involved processes include the mobility of Elements within the glass during heat treatment and the reorganization of atomic bonds during crystallization. This change in coordination number of certain elements is easily observable in bulk glass samples during heat treatment with XAS. Our plan was to monitor these reorganization processes in situ at the immediate surface during heat treatment with PEEM to get time and spatial resolved data. T2 - Joint Meeting of the Polish Synchrotron Radiation Society and SOLARIS Users CY - Online meeting DA - 09.09.2020 KW - Glass KW - Surface KW - Peem KW - Synchrotron PY - 2020 AN - OPUS4-51336 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kromm, Arne T1 - Phase Transformation and Strain Evolution during Welding of Low Transformation Temperature Alloys N2 - In this work, the phase and strain formation in multipass welding of LTT gas metal arc welds were observed under realistic restraints by means of time resolved angular-dispersive synchrotron X-ray diffraction at the High Energy Materials Science beamline HEMS at PETRA III (DESY), Hamburg Germany. It was shown that the strain evolution during cooling correlates with the amount of martensite formed. Both, the strain of martensite and austenite are affected during phase transformation. Even though dilution processes limit the LTT effect in the root compared to the top layer, the strains are significantly reduced compared to the conventional weld metal. The observed effects are found for both Ni and Mn based LTT filler metals regardless of their respective Ms temperature. T2 - 2nd International Conference on Advanced Joining Processes AJP 2021 CY - Sintra, Portugal DA - 21.10.2021 KW - Welding KW - Residual Stress KW - In-situ diffraction KW - Synchrotron PY - 2021 AN - OPUS4-53609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -