TY - JOUR A1 - Scheuerlein, C. A1 - Andrieux, J. A1 - Michels, M. A1 - Lackner, F. A1 - Chiriac, R. A1 - Hagner, M. A1 - Di Michiel, M. A1 - Meyer, Christian A1 - Toche, F. ED - Foley, C. P. T1 - Effect of the fabrication route on the phase and volume changes during the reaction heat treatment of Nb3Sn superconducting wires N2 - Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation. KW - Nb3Sn KW - Microstructure KW - Phase transformations KW - Volume changes KW - X-ray diffraction KW - Differential scanning calorimetry KW - Synchrotron micro-tomography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505128 DO - https://doi.org/10.1088/1361-6668/ab627c VL - 33 IS - 3 SP - 034004 PB - IOP Publishing CY - Bristol (UK) AN - OPUS4-50512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Bhattacharya, Biswajit A1 - Akhmetova, Irinia A1 - Emmerling, Franziska T1 - Mechanochemical and solution syntheses of two novel cocrystals of orcinol with two N,N0-Dipyridines: Structural diversity with varying ligand flexibility N2 - We studied the influence of coformers flexibility on the supramolecular assembly of 5-substituted resorcinol. Two cocrystals of orcinol (ORL) with two dipyridine molecules, i.e. 1,2-di(4-pyridyl)ethane (ORLeBPE) and 1,2-di(4-pyridyl)ethylene (ORLeBPY), were prepared by mechanochemical synthesis and slow evaporation of solvent. The new crystalline solids were thoroughly characterized by single crystal Xray diffraction (SCXRD), powder X-ray diffraction analysis (PXRD), Fourier-transform infrared spectroscopy (FT-IR), differential thermal analysis (DTA), and thermogravimetric analysis (TGA). Structural determination reveals that in both cocrystals, the phenolepyridine, i.e. OeH/N(py) heterosynthon takes the main role in the formation of cocrystals. In ORLeBPE, the components form infinite 1D zig-zag chains, which are extended to 2D layer structure by inter-chain CeH/O interactions between BPE hydrogen atoms and hydroxyl oxygen atoms of ORL. In ORLeBPY, the components form a 0D fourcomponent complex. Formation of the discrete assemblies is attributed to the comparative rigid nature of BPY, which restricts the formation of an extended network. KW - Cocrystal KW - Single crystal KW - X-ray diffraction KW - Mechanochemistry PY - 2020 DO - https://doi.org/10.1016/j.molstruc.2020.128303 SN - 0022-2860 VL - 1217 SP - 128303 PB - Elsevier B.V. AN - OPUS4-51023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roveda, Ilaria T1 - Investigation of residual stresses and microstructure effects on the fatigue behaviour of a L-PBF AlSi10Mg alloy N2 - Laser Powder Bed Fusion (L-PBF) allow the fabrication of lightweight near net shape AlSi10Mg components attractive to the aerospace, automotive, biomedical and military industries. During the build-up process, high cooling rates occur. Thus, L-PBF AlSi10Mg alloys exhibit a Si-nanostructure in the as-built condition, which leads to superior mechanical properties compared to conventional cast materials. At the same time, such high thermal gradients generally involve a deleterious residual stress (RS) state that needs to be assessed during the design process, before placing a component in service. To this purpose post-process heat treatments are commonly performed to relieve detrimental RS. In this contribution two low-temperature stress-relief heat treatments (SRHT) are studied and compared with the as-built state: a SRHT at 265°C for 1 hour and a SRHT at 300°C for 2 hours. At these temperatures microstructural changes occur. In the as-built state, Si atoms are supersaturated in the α-aluminium matrix, which is enveloped by a eutectic Si-network. At 265°C the Si precipitation from the matrix to the pre-existing network is triggered. Thereafter, above 295°C the fragmentation and spheroidization of the Si branches takes place, presumably by Al–Si interdiffusion. After 2 hours the original eutectic network is completely replaced by uniformly distributed blocky particles. The effect of the heat and the microstructure modification on the RS state and the fatigue properties is investigated. Energy dispersive x-ray and neutron diffraction are combined to investigate the near-surface and bulk RS state of a L-PBF AlSi10Mg material. Differences in the endurance limit are evaluated experimentally by high cycle fatigue (HCF) tests and cyclic R-curve determination. T2 - 43rd Materials Mechanics Seminar CY - Sani, Chalkidiki, Greece DA - 05.06.2022 KW - AlSi10Mg KW - Fatigue KW - Neutron diffraction KW - X-ray diffraction PY - 2022 AN - OPUS4-55090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Simulation of powder diffraction patterns N2 - The theory of powder diffraction simulation is explained at the example of PowderCell, a free-available software of BAM. T2 - PowderCell Users meeting CY - Joinville, Brazil DA - 21.09.2015 KW - Powder diffraction KW - X-ray diffraction KW - Phase analysis KW - Simulation PY - 2015 AN - OPUS4-37789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Haferkamp, Sebastian A1 - Akhmetova, Irina A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical one-pot syntheses N2 - We present an in situ triple coupling of synchrotron X-ray diffraction with Raman spectroscopy, and thermography to study milling reactions in real time. This combination of methods allows a correlation of the structural evolution with temperature information. The temperature information is crucial for understanding both the thermodynamics and reaction kinetics. The reaction mechanisms of three prototypical mechanochemical syntheses, a cocrystal formation, a C@C bond formation (Knoevenagel condensation), and the formation of a manganese-phosphonate, were elucidated. Trends in the temperature development during milling are identified. The heat of reaction and latent heat of crystallization of the product contribute to the overall temperature increase. A decrease in temperature occurs via release of, for example, water as a byproduct. Solid and liquid intermediates are detected. The influence of the mechanical impact could be separated from temperature effects caused by the reaction. KW - In situ studies KW - Mechanochemistry KW - Raman spectroscopy KW - Thermography KW - X-ray diffraction PY - 2018 DO - https://doi.org/10.1002/anie.201800147 SN - 1433-7851 SN - 1521-3773 VL - 57 IS - 20 SP - 5930 EP - 5933 PB - Wiley-VCH CY - Weinheim AN - OPUS4-44946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liehr, Alexander A1 - Dingel, Kristina A1 - Kottke, Daniel A1 - Degener, Sebastian A1 - Meier, David A1 - Sick, Bernhard A1 - Niendorf, Thomas T1 - Data selection strategies for minimizing measurement time in materials characterization N2 - Every new material needs to be assessed and qualified for an envisaged application. A steadily increasing number of new alloys, designed to address challenges in terms of reliability and sustainability, poses significant demands on well-known analysis methods in terms of their efficiency, e.g., in X-ray diffraction analysis. Particularly in laboratory measurements, where the intensities in diffraction experiments tend to be low, a possibility to adapt the exposure time to the prevailing boundary conditions, i.e., the investigated microstructure, is seen to be a very effective approach. The counting time is decisive for, e.g., complex texture, phase, and residual stress measurements. Traditionally, more measurement points and, thus, longer data collection times lead to more accurate information. Here, too short counting times result in poor signal-to-background ratios and dominant signal noise, respectively, rendering subsequent evaluation more difficult or even impossible. Then, it is necessary to repeat experiments with adjusted, usually significantly longer counting time. To prevent redundant measurements, it is state-of-the-art to always consider the entire measurement range, regardless of whether the investigated points are relevant and contribute to the subsequent materials characterization, respectively. Obviously, this kind of approach is extremely time-consuming and, eventually, not efficient. The present study highlights that specific selection strategies, taking into account the prevailing microstructure of the alloy in focus, can decrease counting times in X-ray energy dispersive diffraction experiments without any detrimental effect on data quality for the subsequent analysis. All relevant data, including the code, are carefully assessed and will be the basis for a widely adapted strategy enabling efficient measurements not only in lab environments but also in large-scale facilities. KW - Materials characterization KW - Machine learning KW - X-ray diffraction KW - Measurement optimization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630831 DO - https://doi.org/10.1038/s41598-025-96221-1 SN - 2045-2322 VL - 15 IS - 1 SP - 1 EP - 12 PB - Springer Science and Business Media LLC AN - OPUS4-63083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin, S. A1 - Walnsch, A. A1 - Nolze, Gert A1 - Leineweber, A. A1 - Léaux, F. A1 - Scheuerlein, C. T1 - The crystal structure of (Nb0.75Cu0.25)Sn-2 in the Cu-Nb-Sn system N2 - During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite. KW - Electron backscatter diffraction KW - X-ray diffraction KW - Intermetallic compound KW - Structure solution KW - Superconductor PY - 2017 DO - https://doi.org/10.1016/j.intermet.2016.09.008 SN - 0966-9795 SN - 1879-0216 VL - 80 SP - 16 EP - 21 PB - Elsevier Ltd. AN - OPUS4-37874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröpfer, Dirk T1 - Multi-axial analyses of welding stresses in high-strength steel welds N2 - Today’s efforts for lightweight design result in a growing application of high-strength structural steels from 960 MPa. In welded structures of these steels increased demands regarding component safety and a high elastic ratio should be considered. Hence, the prevention of an evolution of high welding induced tensile residual stresses is required. Recent studies showed that component related restraint conditions of welds are able to elevate welding induced stresses to critical values, depending on material characteristics, the welding process and parameters. This work involves multi-axial welding loads as a consequence of the superposition of local residual stresses, global reaction stresses and moments, varying the welding parameters under different restraint conditions. The global welding loads are measured via GMA-weld tests in a special testing facility and via a DIC(Digital Image Correlation)-system in a slot weld. Local transverse residual stresses were analysed by means of X-ray diffraction. The application of a less amount of weld runs due to a modified welding parameters and welds seam configurations revealed as a beneficial approach to reduce welding loads in high-strength steels. T2 - 10th International Conference on Residual Stresses CY - Sydney, Australia DA - 04.07.2016 KW - X-ray diffraction KW - High-strength Steel KW - Welding KW - Reaction Stress PY - 2016 AN - OPUS4-38788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roveda, Ilaria T1 - Effect of heat treatment on the microstructure, residual stress state and fatigue properties of PBF-LB/M AlSi10Mg N2 - Al-Si alloys produced by Laser Powder Bed Fusion (PBF-LB/M) techniques allow the fabrication of lightweight free-shape components. Due to the extremely heterogeneous cooling and heating, PBF-LB/M induces high magnitude residual stress (RS) and a fine Si microstructure. As the RS can be deleterious to the fatigue resistance of engineering components, great efforts are focused on understanding their evolution before and after post-process heat treatments (HT). T2 - Alloys for Additive Manufacturing Symposium 2022 (AAMS22) CY - Munich, Germany DA - 12.09.2022 KW - Neutron diffraction KW - X-ray diffraction KW - Crack propagation PY - 2022 AN - OPUS4-55871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Marquardt, Julien A1 - Emmerling, Franziska T1 - Structural changes in Ba-compounds of different hardness induced by high-energy ball milling – evidenced by 137Ba NMR and X-ray powder diffraction N2 - Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors. KW - Mechanochemistry KW - X-ray diffraction KW - Solid state NMR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547397 DO - https://doi.org/10.1002/zaac.202200026 SN - 0044-2313 VL - 648 IS - 10 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -