TY - JOUR A1 - Feng, Wen A1 - Gemming, Thomas A1 - Giebeler, Lars A1 - Qu, Jiang A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, Bernd A1 - González-Martínez, Ignacio T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600247 DO - https://doi.org/10.1016/j.ultramic.2024.113978 SN - 1879-2723 VL - 262 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-60024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aree, T. A1 - McMonagle, C. J. A1 - Michalchuk, Adam A1 - Chernyshov, D. T1 - Low-frequency lattice vibrations from atomic displacement parameters of a-FOX-7, a high energy density material N2 - Highly anharmonic thermal vibrations may serve as a source of structural instabilities resulting in phase transitions, chemical reactions and even the mechanical disintegration of a material. Ab initio calculations model thermal motion within a harmonic or sometimes quasi-harmonic approximation and must be complimented by experimental data on temperature-dependent vibrational frequencies. Here multi-temperature atomic displacement parameters (ADPs), derived from a single-crystal synchrotron diffraction experiment, are used to characterize low-frequency lattice vibrations in the alpha-FOX-7 layered structure. It is shown that despite the limited quality of the data, the extracted frequencies are reasonably close to those derived from inelastic scattering, Raman measurements and density functional theory (DFT) calculations. Vibrational anharmonicity is parameterized by the Grüneisen parameters, which are found to be very different for in-layer and out-of-layer vibrations. KW - Energetic Materials KW - DFT KW - Structural dynamics KW - X-ray diffraction PY - 2022 DO - https://doi.org/10.1107/S2052520622002700 SN - 2052-5206 VL - 78 SP - 376 EP - 384 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-54832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kromm, Arne T1 - Combining sectioning method and x-ray diffraction for evaluation of residual stresses in welded high strength steel components N2 - Residual stresses and distortions in welded I-girders for steel construction are relevant when evaluating the stability of steel beams and column members. The application of high strength steels allows smaller wall thicknesses compared to conventional steels. Therefore, the risk of buckling has to be considered carefully. Due to the lack of knowledge concerning the residual stresses present after welding in high strength steel components conservative assumptions of their level and distribution is typically applied. In this study I-girders made of steels showing strengths of 355 MPa and 690 MPa were welded with varying heat input. Due to the dimension of the I-girders and the complex geometry the accessibility for residual stress measurement using X-ray diffraction was limited. Therefore, saw cutting accompanied by strain gauge measurement has been used to produce smaller sections appropriate to apply X-ray diffraction. The stress relaxation measured by strain gauges has been added to residual stresses determined by X-ray diffraction to obtain the original stress level and distribution before sectioning. The combination of both techniques can produce robust residual stress values. From practical point of view afford for strain gauge application can be limited to a number of measuring positions solely to record the global amount of stress relaxation. X-ray diffraction can be applied after sectioning to determine the residual stresses with sufficient spatial resolution. T2 - International Conference on Residual Stresses 10 CY - Sydney, Australia DA - 03.07.2016 KW - Residual stress KW - Sectioning method KW - X-ray diffraction PY - 2016 AN - OPUS4-36887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Amadeus A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Determination of residual stress evolution during repair welding of high-strength steel components N2 - During the assembly of steel structures, unacceptable weld defects may be found. An economical solution is local thermal gouging of the affected areas and re-welding. Due to high shrinkage restraints of repair weld and sur- rounding structure, high global and local welding stresses superimpose, and may lead to cracking and component failure, especially in connection with the degraded microstructure and mechanical properties of high-strength steels during the repair process. Component-related investigations of high-strength steels (FOSTA P1311/ IGF20162N) focus on welding residual stress evolution during local thermal gouging and rewelding. In this study, repair welding of S500MLO (EN 10225) is carried out using in-situ digital image correlation (DIC) and ex- situ X-ray diffraction (XRD) to analyse strains and stresses. Self-restrained slit specimen geometries were identified representing defined rigidity conditions of repair welds of real components, which were quantified using the restraint intensity concept. The specimens were rewelded with constant welding heat control and parameters. Weld specimens exhibited significantly increased transverse residual stresses with higher transverse restraint intensities, in the weld metal, and in the heat affected zone. Transverse stresses along the weld seam decrease at the weld seam ends leading to different stress state during gouging and welding. XRD analysis of the longitudinal and transverse local residual stresses after cooling to RT showed a good comparability with global DIC analyses. KW - Repair-welding KW - High-strength steels KW - X-ray diffraction KW - Digital image correlation KW - Residual stresses PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555672 DO - https://doi.org/10.1016/j.finmec.2022.100073 SN - 2666-3597 VL - 6 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-55567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Hannemann, Andreas A1 - Kannengießer, Thomas ED - Seefeldt, Marc T1 - In-situ determination of critical welding stresses during assembly of thick-walled components made of high-strength steel N2 - The performance and safety of welded high-strength low-alloyed steel (HSLA) components are substantially affected by the stresses occurring during and after welding fabrication, especially if welding shrinkage and distortion are severely restrained. The surrounding structure of the whole component affects loads in the far-field superimposing with welding stresses in the near-field of the weld. In this study a unique testing facility was used to restrain shrinkage and bending while analyse multiaxial far-field loads (max. 2 MN) during assembly of thick-walled component. A novel approach for the assessment of the in-situ-measured far-field data in combination with the actual weld geometry was elaborated. For the first time, analyses of the global bending moments of restrained welds based on the neutral axis of the actual weld load bearing section were achieved. Hence, far-field measurements offered the possibility to determine critical near-field stresses of the weld crosssections for the entire joining process. This work presents the approach for far-to-near field in-situ determination of stresses in detail for the 2-MN-testing system based on an extensive experimental work on HSLA steel welds, which demonstrates sources and consequences of these high local welding stresses. Thus, it was clarified, why the first weld beads are crucial regarding welding stresses and cold cracking, which is well known, but has never been measured so far. Accompanying analyses using X-ray diffraction (XRD) after welding show effects on local residual stress distributions. These analyses indicated viable prospects for stress reduction during assembly of thick-walled HSLA steel components. T2 - European Conference on Residual Stresses 2018 - ECRS-10 CY - Leuven, Belgium DA - 11.09.2018 KW - Residual stress KW - Welding KW - Large-scale test KW - X-ray diffraction KW - HSLA steel PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-466053 SN - 978-1-9452-9188-3 SN - 978-1-9452-9189-0 DO - https://doi.org/10.21741/9781945291890-30 SN - 2474-395X SN - 2474-3941 VL - 6 SP - 191 EP - 196 PB - Materials Research Forum LLC CY - Millersville, PA, USA AN - OPUS4-46605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröpfer, Dirk T1 - In-situ determination of critical welding stresses during assembly of thick-walled components made of high-strength steel N2 - The performance and safety of welded high-strength low-alloyed steel (HSLA) components are substantially affected by the stresses occurring during and after welding fabrication, especially if welding shrinkage and distortion are severely restrained. The surrounding structure of the whole component affects loads in the far-field superimposing with welding stresses in the near-field of the weld. In this study a unique testing facility was used to restrain shrinkage and bending while analyse multiaxial far-field loads (max. 2 MN) during assembly of thick-walled component. A novel approach for the assessment of the in-situ-measured far-field data in combination with the actual weld geometry was elaborated. For the first time, analyses of the global bending moments of restrained welds based on the neutral axis of the actual weld load bearing section were achieved. Hence, far-field measurements offered the possibility to determine critical near-field stresses of the weld crosssections for the entire joining process. This work presents the approach for far-to-near field in-situ determination of stresses in detail for the 2-MN-testing system based on an extensive experimental work on HSLA steel welds, which demonstrates sources and consequences of these high local welding stresses. Thus, it was clarified, why the first weld beads are crucial regarding welding stresses and cold cracking, which is well known, but has never been measured so far. Accompanying analyses using X-ray diffraction (XRD) after welding show effects on local residual stress distributions. These analyses indicated viable prospects for stress reduction during assembly of thick-walled HSLA steel components. T2 - European Conference on Residual Stresses 2018 - ECRS-10 CY - Leuven, Belgium DA - 11.09.2018 KW - Residual stress KW - Welding KW - Large-scale test KW - X-ray diffraction KW - HSLA steel PY - 2018 AN - OPUS4-46607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Amadeus T1 - Adequate repair concepts for high-strength steel weld joints considering design influences N2 - The sustainable and resource-efficient production of wind energy plants requires the use of modern high-strength fine-grain structural steels. This applies to both foundation and erection structures. During the assembly of steel structures, unacceptable defects can occasionally be found in the weld area. In most cases, the economical solution would be local thermal gouging of the affected areas and re-welding. Due to the high shrinkage restraint of the joint groove in the overall structure, the superposition of design and welding-induced residual stress can lead to crack formation and ultimately to component failure, particularly in interaction with the degradation of the microstructure and mechanical properties high-strength steels during the repair process. In this context, component-related investigations (FOSTA-P1311/IGF-Nr. 20162 N) focusing on welding residual stress evolution during local thermal gouging and rewelding of S500MLO and S960QL are carried out using in-situ digital image correlation (DIC) and ex-situ X-ray diffraction methods (XRD). Therefore, self-restrained specimens were systematically gouged and rewelded with defined welding heat control (heat input, working temperature) and parameters. By means of structural mechanics calculations, geometries of self-restrained specimens were identified, that represent defined rigidity conditions of repair welds of real components. It could be shown that with increasing restraint intensity significantly higher residual stresses occur in the weld metal and heat affected zone. Furthermore, it revealed that the transverse stresses along the weld seam decrease at the weld seam ends leading to different stress state during gouging and welding. XRD analysis of the local residual stresses after cooling to RT longitudinal and transverse to the weld direction showed a good comparability with global DIC analyses. T2 - Bachelor-, Master-, Doktoranden-Kolloquium der Otto-von-Guericke Universität Magdeburg CY - Magdeburg, Germany DA - 20.10.2021 KW - High-strength steels KW - Repair welding KW - X-ray diffraction KW - Digital image correlation PY - 2021 AN - OPUS4-53640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ulbricht, Alexander T1 - Tales from Within: Residual Stress and Void Formation in LPBF 316L N2 - An unusual microstructure, inherent residual stresses and void formation are the three key aspects to control when assessing metallic parts made by LPBF. This talk explains an experiment to unravel the interlinked influence of the two mechanisms for the formation of residual stresses in LPBF: the temperature gradient mechanism and constricted solidification shrinkage. The impact of each mechanism on the shape and magnitudes of the residual stress distribution is described. Combined results from neutron diffraction, X-ray diffraction, computed tomography and in-situ thermography are presented. Also, influence of scan strategies as well as surface roughness of subjacent layers on void formation is shown. Results from computed tomography and in-situ thermography of a specimen dedicated to study the interaction of the melt pool with layers of powder underneath the currently illuminated surface are presented. T2 - 2nd Workshop on In-situ Monitoring and Microstructure Development in Additive Manufacturing CY - Online meeting DA - 19.04.2021 KW - Neutron diffraction KW - Laser powder bed fusion KW - In-situ thermography KW - Computed tomography KW - X-ray diffraction KW - Residual stress KW - Pore formation KW - AISI 316L PY - 2021 AN - OPUS4-52819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaiser, E. A1 - Fantin, Andrea A1 - Manzoni, Anna Maria A1 - Hesse, René A1 - Többens, D. M. A1 - Hsu, W.-C. A1 - Murakami, H. A1 - Yeh, A.-C. A1 - Pavel, M. J. A1 - Weaver, M. L. A1 - Zhu, H. A1 - Wu, Y. A1 - Vogel, F. T1 - Elucidating hierarchical microstructures in high entropy superalloys: An integrated multiscale study N2 - In this study, we examine a high entropy superalloy (HESA-Y1: Ni49.37Co20Cr7Fe4Al11.6Ti6Re1Mo0.5W0.5Hf0.03 at%), focusing on hierarchical microstructure formation and its effects on mechanical properties. Thermodynamic modeling using Thermo-Calc predicts equilibrium phase fractions, compositions, and transition temperatures,which are validated by experimental data from differential scanning calorimetry (DSC). Transmission electronmicroscopy (TEM) reveals that secondary aging induces nanometer-sized γ particles within γ’ precipitates, forming a hierarchical γ/γ’ microstructure. Atom probe tomography (APT) confirms supersaturation of γ’ precipitates with γ-forming elements (Co, Cr, Fe), driving γ particle formation, and measures interfacial widths between γ’ and γ phases. Partitioning coefficients derived from APT align with Thermo-Calc predictions for most elements. Vickers microhardness testing shows an increase of about 50 HV in the hierarchical microstructure compared to the conventional one. In situ synchrotron X-ray diffraction (XRD) from 25 to 750 ◦C determines a small, negative lattice misfit δ between γ and γ’ phases, suggesting enhanced microstructural stability, consistent with Thermo-Calc calculations. Our methodological approach enables measurement of the unconstrained lattice parameter of phase-extracted γ’ in a single-crystal XRD setup. Due to their small size and low volume fraction, γ particles do not produce distinct reflections in the X-ray diffractogram. Elucidating hierarchical microstructures across multiple scales, we establish that the presence of Re and Hf and controlled aging processes lead to enhanced mechanical properties, offering valuable insights for the design of advanced high entropy superalloys. KW - High entropy alloys KW - Transmission electron microscopy KW - X-ray diffraction KW - Superalloy PY - 2025 DO - https://doi.org/10.1016/j.matchar.2024.114642 VL - 220 SP - 1 EP - 13 PB - Elsevier Inc. AN - OPUS4-62348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manzoni, Anna Maria A1 - Haas, S. A1 - Kropf, H. A1 - Duarte, J. A1 - Cakir, Cafer Tufan A1 - Dubois, F. A1 - Többens, D. A1 - Glatzel, U. T1 - Temperature evolution of lattice misfit in Hf and Mo variations of the Al 10 Co 25 Cr 8 Fe 15 Ni 36 Ti 6 compositionally complex alloy N2 - Misfits of γ- γ’ based Al10Co25Cr8Fe15Ni36Ti6 and its Mo- and Hf-variations are studied up to a temperature of 980 °C and compared with Ni- and Co-based superalloys. The trace elements decrease (Hf) or increase (Mo) the edge radii of the γ’ cuboids without changing their sizes. Atom probe measurements revealed that the Hf alloy prefers the γ’ phase while Mo prefers the γ matrix, leading to a lattice parameters enhancement of both phases, as could be revealed by synchrotron X-ray diffraction. The misfit is influenced in opposite ways: Hf increases the positive misfit, while Mo reduces it at all investigated temperatures. KW - Metal and alloys KW - Transmission electron microscopy KW - X-ray diffraction KW - Atom probe tomography KW - High entropy alloy PY - 2020 DO - https://doi.org/10.1016/j.scriptamat.2020.07.013 VL - 188 SP - 74 EP - 79 PB - Elsevier Ltd. AN - OPUS4-51025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -