TY - JOUR A1 - Sommer, Konstantin A1 - Agudo Jácome, Leonardo A1 - Hesse, René A1 - Bettge, Dirk T1 - Revealing the nature of melt pool boundaries in additively manufactured stainless steel by nano-sized modulation N2 - In the current study, the 3D nature of the melt pool boundaries (MPBs) in a 316 L austenitic steel additively manufactured by laser-based powder bed fusion (L-PBF) is investigated. The change of the cell growth direction and its relationship to the MPBs is investigated by transmission electron microscopy. A hitherto unreported modulated substructure with a periodicity of 21 nm is further discovered within the cell cores of the cellular substructure, which results from a partial transformation of the austenite, which is induced by a Ga+ focused ion beam. While the cell cores show the modulated substructure, cell boundaries do not. The diffraction pattern of the modulated substructure is exploited to show a thickness ≥200 nm for the MPB. At MPBs, the cell walls are suppressed, leading to continuously connecting cell cores across the MPB. This continuous MPB is described either as overlapping regions of cells of different growing directions when a new melt pool solidifies or as a narrow planar growth preceding the new melt pool. KW - Additive manufacturing KW - Austenitic steel 316L KW - Melt pool boundary KW - Microstructural characterization KW - Transmission electron microscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547295 DO - https://doi.org/10.1002/adem.202101699 SN - 1527-2648 VL - 24 IS - 6 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Lawrence, M. J. A1 - Celorrio, V. A1 - Wang, Q. A1 - Gu, M. A1 - Sun, Z. A1 - Agudo Jácome, Leonardo A1 - Russell, A. E. A1 - Huang, L. A1 - Rodriguez, P. T1 - Nickel confined in 2D earth-abundant oxide layers for highly efficient and durable oxygen evolution catalysts N2 - Low cost, high-efficiency catalysts towards water splitting are urgently required to fulfil the increasing demand for energy. In this work, low-loading (<20 wt%) Ni-confined in layered metal oxide anode catalysts (birnessite and lepidocrocite titanate) have been synthesized by facile ion exchange methodology and subjected to systematic electrochemical studies. It was found that Ni-intercalated on K-rich birnessite (Ni-KMO) presents an onset overpotential (ηonset) as low as 100 mV and overpotential at 10 mA cm−2 (η10) of 206 mV in pH = 14 electrolyte. By combining electrochemical methods and X-ray absorption and emission spectroscopies (XAS and XES), we demonstrate Ni sites are the active sites for OER catalysis and that the Mn3+ sites facilitate Ni intercalation during the ion-exchange process, but display no observable contribution towards OER activity. The effect of the pH and the nature of the supporting electrolyte on the electrochemical performance was also evaluated. KW - Confined catalyst KW - Low-loading KW - Layered manganese oxide KW - Oxygen evolution reaction KW - Transmission electron microscopy (TEM) PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515027 DO - https://doi.org/10.1039/D0TA04031B SN - 2050-7496 SN - 2050-7488 VL - 8 IS - 26 SP - 13340 EP - 13350 PB - Royal Society of Chemistry CY - London AN - OPUS4-51502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocano, Patricia A1 - Manzoni, Anna Maria A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Laplanche, G. A1 - Agudo Jácome, Leonardo T1 - Influence of cooling rate on the microstructure and room temperature mechanical properties in the refractory AlMo0.5NbTa0.5TiZr superalloy N2 - Refractory chemically complex alloys with bcc-based microstructures show great potential for high-temperature applications but most of them exhibit limited room-temperature ductility, which remains a challenge. One such example is the AlMo0.5NbTa0.5TiZr alloy, mainly consisting of a nano-scaled structure with an ordered B2 matrix and a high-volume fraction of aligned cuboidal and coherently embedded A2 precipitates. This work aims to investigate how the cooling rate after hot isostatic pressing of the AlMo0.5NbTa0.5TiZr alloy affects its microstructure and its resulting hardness and fracture toughness at room temperature. A slow cooling rate of 5 °C/min leads to a coarse microstructure consisting of aligned slabs (mean A2 precipitate ≈ 25 nm) with a nanohardness of about 8 GPa. In contrast, after the fastest cooling rate (30 °C/min), the A2 precipitates become more cubic with an edge length of ≈ 16 nm, resulting in an increase in nanohardness by 10 %. The fracture toughness is roughly independent of the cooling rate and its mean value (≈ 4.2 MPa∙m1/2) resembles that of some B2 intermetallics and other A2/B2 alloys. As the lattice misfit between the A2 and B2 phases is known to play a key role in microstructure formation and evolution, its temperature dependence between 20 and 900 °C was investigated. These findings offer insights into the evolution of the microstructure and room-temperature mechanical properties of the AlMo0.5NbTa0.5TiZr alloy, which could help the development of advanced chemically complex alloys. KW - High entropy alloy KW - Lattice misfit KW - Scanning electron microscopy KW - Transmission electron microscopy KW - X-ray diffraction KW - Refractory alloy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572809 DO - https://doi.org/10.1016/j.jallcom.2023.169871 SN - 0925-8388 VL - 949 SP - 169871 PB - Elsevier B.V. AN - OPUS4-57280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gadelmeier, C. A1 - Agudo Jácome, Leonardo A1 - Suárez Ocano, Patricia A1 - Glatzel, U. T1 - Effect of stacking fault energy (SFE) of single crystal, equiatomic CrCoNi and Cantor alloy on creep resistance N2 - Compared to mechanisms like solid solution strengthening, the stacking fault energy (SFE) should be considered as a further factor that influences the material properties. The effect of SFE of alloys or individual elements on strength and resistance can vary considerably. In the high-temperature regime above 700 ◦C, there are still significant gaps in the knowledge about the effect of the SFE on the mechanical properties of single-phase alloys. The effect of SFE on creep resistance of two face-entered cubic equiatomic medium and high entropy alloys, CrCoNi and CrMnFeCoNi, respectively, is evaluated to fill parts of these gaps. Using the Bridgman solidification process, the alloys were produced as single crystals and crept under vacuum at 700 ◦C up to 1100 ◦C. This work shows a significant impact of the lower SFE of CrCoNi on the creep behavior compared to the results of previous investigations of CrMnFeCoNi. The creep resistance of the former is higher over the complete temperature range. At very high temperatures, the strengthening effect of the stacking faults is significantly present. The formation of tetragonal stacking faults and extended dislocation nodes can be identified as the reason for this effect. KW - Medium entropy alloy KW - MEA KW - HEA KW - Single crystal KW - CrCoNi PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602620 DO - https://doi.org/10.1016/j.msea.2024.146779 SN - 0921-5093 VL - A 908 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-60262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - Manzoni, Anna Maria A1 - Mohring, Wencke A1 - Hesse, René A1 - Agudo Jácome, Leonardo A1 - Stephan-Scherb, C. T1 - Early material damage in equimolar CrMnFeCoNi in mixed oxidizing/sulfiding hot gas atmosphere N2 - The challenges to use more varied fuels at medium and high temperatures above 500 °C need to be addressed by tuning the materials toward a better resistance against increased corrosion. As a first step the corrosion processes need to be better understood, especially in the case of the unavoidable and highly corrosive sulfur-based gases. Herein, oxidation/sulfidation of an equimolar CrMnFeCoNi high-entropy alloy is studied at an early stage after hot gas exposure at 600 °C for 6 h in 0.5% SO2 and 99.5% Ar. The oxidation process is studied by means of X-ray diffraction, scanning and transmission electron microscopy, and supported by thermodynamic calculations. It is found that the sulfur does not enter the bulk material but interacts mainly with the fast-diffusing manganese at grain boundary triple junctions at the alloy surface. Submicrometer scaled Cr–S–O-rich phases close to the grain boundaries complete the sulfur-based phase formation. The grains are covered in different Fe-, Mn-, and Cr-based spinels and other oxides. KW - High entropy alloy KW - Sulfiding KW - Corrosion KW - Transmission electron microscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543495 DO - https://doi.org/10.1002/adem.202101573 SN - 1527-2648 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Serrano-Munoz, Itziar A1 - Agudo Jácome, Leonardo A1 - Thompsom, Sean A1 - Schneider, Judy T1 - On the transferability of post-processing heat treatments designed for PBF-LB IN718 alloys to directed energy deposition specimens N2 - Many processes are being developed for metal additive manufacturing (AM) which vary by their heat source and feedstock. The use of directed energy deposition (DED) is growing due to its ability to build larger structures outside of a contained powder bed chamber. However, the only standard exclusively for post-build heat treatment of AM IN718 is ASTM standard F3055-14a, developed for powder bed fusion (PBF). This study evaluates the applicability of this current heat treatment standard to AM IN718 specimens produced using two methods of DED: laser-blown powder (LP)-DED and arc-wire (AW)-DED. Electron microscopy and X-ray diffraction techniques were used to characterize the specimens in the as-built condition and after the full heat treatment (FHT) specified in F3055. No evidence of remaining Laves phase was observed in the two DED specimens after the FHT. Yield strengths for the DED specimens were 1049 MPa for FHT AW-DED and 1096 MPa for LP-DED, higher than the minimum stated for PBF-LB IN718 of 920 MPa. The size, morphology, inter-spacing, and diffraction patterns of the γ´ and γ´´ strengthening precipitates are found to be similar for both DED processes. Differences were observed in the microstructure evolution where the F3055 heat treatments resulted in partial recrystallization of the grain structure, with a higher content of annealing twins observed in the AW-DED. These microstructural differences correlate with differences in the resulting elongation to failure. Thus, it is proposed that variations in heat treatments are needed for optimizing IN718 produced by different AM processes. KW - Additive manufacturing variants KW - Directed energy deposition (DED) KW - Post-process heat treatments KW - SEM-EBSD and TEM microscopy KW - XRD phase analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628165 DO - https://doi.org/10.1007/s00170-025-15386-1 SN - 1433-3015 VL - 137 IS - 7-8 SP - 3949 EP - 3965 PB - Springer Science and Business Media LLC AN - OPUS4-62816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weinel, Kristina A1 - Hahn, Marc Benjamin A1 - Lubk, Axel A1 - González Martínez, Ignacio Guillermo A1 - Büchner, Bernd A1 - Agudo Jácome, Leonardo T1 - Nanoparticle Synthesis by Precursor Irradiation with Low-Energy Electrons N2 - Nanoparticles (NPs) and their fabrication routes are intensely studied for their wide range of application in optics, chemistry, and medicine. Γ-ray and ion irradiation of precursor matter are established methods that facilitate tailored NP synthesis without complicated chemistry. Here, we develop and explore NP synthesis based on irradiating precursor microparticles with low-energy electron beams. We specifically demonstrate the fabrication of plasmonic gold nanoparticles of sizes between 3 and 350 nm on an amorphous SiOx substrate using a 30 kV electron beam. By detailed comparison with electron scattering simulations and thermodynamic modeling, we reveal the dominant role of inelastic electron–matter interaction and subsequent localized heating for the observed vaporization of the precursor gold microparticles. This general principle suggests the suitability of electron-beam irradiation for synthesizing NPs of a wide class of materials. KW - Gold Nanoparticle KW - Scanning Electron Microscopy KW - In situ irradiation KW - Thermodynamic modelling KW - Heat Transfer PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627609 DO - https://doi.org/10.1021/acsanm.4c06033 SN - 2574-0970 VL - 8 IS - 10 SP - 4980 EP - 4988 PB - ACS Publications CY - Washington, DC AN - OPUS4-62760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, Wen A1 - Schulz, Johannes A1 - Wolf, Daniel A1 - Pylypenko, Sergii A1 - Gemming, Thomas A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, Bernd A1 - Lubk, Axel T1 - Secondary electron emission from gold microparticles in a transmission electron microscope: comparison of Monte Carlo simulations with experimental results N2 - We measure the electron beam-induced current to analyze the electron-induced secondary electron (SE) emission from micron-sized gold particles illuminated by 80 and 300 keV electrons in a transmission electron microscope. A direct comparison of the experimental and simulated SE emission (SEE) employing Monte Carlo scattering simulations based on the GEANT4 toolkit yields overall good agreement with a noticeable discrepancy arising from the shortcoming of the GEANT4 scattering cross sections in the low-loss regime. Thus, the electron beam-induced current analysis allows to quantify the inelastic scattering including SEE in the transmission electron microscope and provides further insight into the charging mechanisms. KW - Electron beam-induced current KW - Transmission electron microscopy KW - Secondary electron emission KW - Secondary electron yield KW - Gold micronoparticle PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622557 DO - https://doi.org/10.1088/1361-6463/ad9840 VL - 58 IS - 8 SP - 1 EP - 7 PB - IOP Publishing CY - Bristol, GB AN - OPUS4-62255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weinel, Kristina A1 - Schultz, Johannes A1 - Kalady, Mohammed Fayis A1 - Wolf, Daniel A1 - Agudo Jácome, Leonardo A1 - Lubk, Axel T1 - Fabrication of 2-dimensional disordered assemblies of gold nanoparticles and investigation of localized surface plasmon resonances N2 - Interaction of electromagnetic waves, such as electron beams or light, with conductive material can lead to localized surface plasmon resonances (LSPRs) where the incoming energy can be deposited in a collective excitation of electrons of the conduction band, which in turn can result in coherent localized plasmon oscillations. LSPR in metallic nanostructures, such as nanoparticles (NPs), which are sensitive to geometry, material composition and environment, are currently utilized in a wide range of applications, such as surface-enhanced Raman spectroscopy, plasmonic wave guides, improved solar cells, on-chip particle accelerators and nanoantennas. A host of studies that focus on plasmonic NPs ranging from single NPs with several shapes (cubic, spherical, tetrahedral) over 1D assemblies of NPs such as chains, to ordered 2D assemblies of NPs show an increase of the complexity regarding the hybridization behavior of LSPRs eventually lead to delocalized Surface Plasmons. Furthermore, Anderson predicted in 1977 the absence of diffusion or delocalization of waves in disordered systems, which has been discussed as the underlying mechanism for LSPRs localization in disordered metallic thin films and ultrathin 2D networks. Our aim is to further develop these studies on the surface plasmon localization in disordered structures by (1) developing a novel NPs assembly fabrication method that allows fabricating disordered assemblies of NPs of a wide range of NPs sizes, and (2) probing the LSPR with high-resolution electron energy-loss spectroscopy (EELS). Moreover, the dominant dipolar interaction between the NPs, also facilitates an efficient numerical modeling of these systems, which in comparison with the experiments allows for an in-depth study of the impact of various geometric parameters as well as retardation and life-time damping on the observed localization behavior. To synthesize 2D disordered assemblies of gold NPs on a TEM transparent silicon oxide substrate, a new synthesis routine was developed. This procedure is based on sublimation and redeposition of a gold microparticle precursor induced by an electron beam in a scanning electron microscope (SEM) operated at 30 kV. To characterize the assembly of synthesized NPs in terms of size, shape and spreading over the substrate, TEM measurements were conducted subsequently. To study LSPRs experimentally, EELS in scanning transmission electron microscopy (STEM) mode was carried out. The numerical modelling of LSPRs was performed using a self-consistent dipole model. The synthesized 2D disordered gold NPs assemblies exhibit a gradient in the NPs mean size, which ranges from 100 nm close to the precursor location down to 2 nm at a distance of more than 20 µm from the precursor location. Additionally, the interparticle distance between the gold NPs increases with increasing distance to the precursor location. The experimental investigation as well as the numerical simulation of the LSPRs demonstrate a localization behavior that decreases toward larger energies, which is driven by the disorder of the NPs assembly (mainly the random particle distance). That localization behavior stays in contrast to what was found in ultrathin 2D gold networks showing increasing of localization towards higher LSPRs energies. By varying the geometric parameters of the NPs assembly in the simulation, we could identify the NPs thickness as the parameter, that determines the energy-dependence of the localization. Specifically, a critical thickness of approx. 10 nm separates the two localization regimes, which correlates to the energy of the dipole mode resonance crucially depending on the thickness of the NPs. 2D disordered assemblies of gold NPs of a wide range of NPs sizes and distances can be synthesized directly on thin substrates facilitating structural characterization and EELS measurements in a TEM. It could be shown that such assemblies exhibit LSPRs with a localization behavior that may be tuned by the NPs sizes (including thickness) and interparticle distances. The proposed synthesis of random NPs assemblies opens new avenues for fundamental studies on Anderson localization in disordered plasmonic structures as well as its applications such as surface-enhanced Raman spectroscopy where localization behavior must be tuned to specific wave lengths. T2 - 17th European Microscopy Congress (EMC 2024) CY - Copenhagen, Denmark DA - 26.08.2024 KW - Scanning electron microscopy KW - Gold nanoparticle synthesis KW - Disordered assemblies KW - Localized surface plasmon resonances KW - Transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618330 DO - https://doi.org/10.1051/bioconf/202412932007 VL - 129 SP - 1 EP - 2 PB - EDP Sciences CY - Les Ulis AN - OPUS4-61833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paulisch-Rinke, M. C. A1 - Manzoni, Anna Maria A1 - Agudo Jácome, Leonardo A1 - Vogel, F. A1 - Reimers, W. T1 - Influence of chemical composition on microstructure and mechanical properties in the extruded aluminum alloys 7021B and 7175 N2 - The aim of this study is to improve the mechanical properties of Al 7xxx series alloys by achieving the strengthening benefits typically provided by Cu while avoiding the formation of low-melting eutectic phases associated with excessive Cu content. This is accomplished through a tailored combination of alloying elements and optimized thermomechanical treatments. Alloys 7021B (high Zn content) and 7175 (high Cu and Mg content) are analyzed and optimized threefold in this study: the heat treatment, the microstructural evolution and the mechanical properties are investigated by several methods and compared with the aim of improving the process parameters for subsequent application. The peak-aging process is optimized via compression tests to overcome the strength-ductility trade-off. Microstructure and phase chemistry analyses by transmission electron microscopy and atom probe tomography enable a better understanding of the underlying morphological features such as the spatial distribution, and the chemical composition of the hardening phases. The mechanical properties of the peak-aged alloys are determined by compression and tensile tests. Both alloys exhibit very high strength – even by 7xxx series standards. It can be traced back to the dislocation movement: it is impeded both by homogeneously distributed cuttable Guinier–Preston zones in both alloys and by non-cuttable η’ precipitates. As a result, we demonstrate that alloy 7021B offers novel possibilities for processing and industrial application: high strength, typically associated with Cu containing alloys, can also be obtained in Cu free alloys, if the Zn content is sufficiently high. We can thus suggest new opportunities for processing and industrial applications by reducing the risk of forming low-melting eutectic phases. KW - Aluminium alloys KW - Transmission electron microscopy KW - Atom probe tomography KW - Extrusion KW - Mechanical properties PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640338 DO - https://doi.org/10.1016/j.matdes.2025.114649 SN - 0264-1275 VL - 258 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-64033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cao, L. A1 - Thome, P. A1 - Agudo Jácome, Leonardo A1 - Somsen, C. A1 - Cailletaud, G. A1 - Eggeler, G. T1 - On the influence of crystallography on creep of circular notched single crystal superalloy specimens N2 - The present work contributes to a better understanding of the effect of stress multiaxiality on the creep behavior of single crystal Ni-base superalloys. For this purpose we studied the creep deformation and rupture behavior of double notched miniature creep tensile specimens loaded in three crystallographic directions [100], [110] and [111] (creep conditions: 950 °C and 400 MPa net section stress). Crystal plasticity finite element method (CPFEM) was used to analyze the creep stress and strain distributions during creep. Double notched specimens have the advantage that when one notch fails, the other is still intact and allows to study a material state which is close to rupture. No notch root cracking was observed, while microstructural damage (pores and micro cracks) were frequently observed in the center of the notch root region. This is in agreement with the FEM results (high axial stress and high hydrostatic stress in the center of the notched specimen). Twinning was observed in the notch regions of [110] and [111] specimens, and <112> {111} twins were detected and analyzed using orientation imaging scanning electron microscopy. The present work shows that high lattice rotations can be detected in SXs after creep fracture, but they are associated with the high strains accumulated in the final rupture event. KW - Single crystal Ni-Base superalloys KW - Double notched creep specimen KW - Stress distribution KW - Lattice rotation KW - Cracks PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506060 DO - https://doi.org/10.1016/j.msea.2020.139255 SN - 0921-5093 VL - 782 SP - 139255 PB - Elsevier B. V. AN - OPUS4-50606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Weber, Kathrin A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Elucidation of orientation relations between Fe-Cr alloys and corrosionproducts after high temperature SO2 corrosion N2 - The early stages of corrosion of Fe-Cr-model alloys (2 and 9 % Cr) were investigated after exposure at 650 °C in0.5 % SO2containing gas by electron backscattered diffraction (EBSD) and transmission electron microscopy(TEM). The impact of the grain orientation of the base alloy on the orientation relations of the corrosion productsis presented. After 2 min–5 min exposure the formation of a multi-layered corrosion zone was discovered. Aclear orientation relationship between ferrite and the (Fe,Cr)3O4 spinel could be demonstrated. The obtainedresults show the importance of the grain orientation on oxidation resistance. KW - Iron KW - TEM KW - SEM KW - High temperature corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508911 DO - https://doi.org/10.1016/j.corsci.2020.108809 VL - 174 SP - 1 EP - 11 PB - Elsevier AN - OPUS4-50891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ferrari, Bruno A1 - Fantin, Andrea A1 - Said, D. A1 - Fitch, A. N. A1 - Suárez Ocano, Patricia A1 - Mishurova, Tatiana A1 - Roveda, Ilaria A1 - Kromm, Arne A1 - Darvishi Kamachali, Reza A1 - Bruno, Giovanni A1 - Evans, Alexander A1 - Requena, G. A1 - Agudo Jácome, Leonardo A1 - Serrano Munoz, Itziar T1 - The impact of scanning strategy on cell structures in PBF-LB/M/IN718: an in situ synchrotron x-ray diffraction study N2 - In additive manufacturing, any change of the process parameters, such as scanning strategy, directly affects the cooling rates, heat accumulation, and overall thermal history of the build. Consequently, parts built with different process parameters tend to have different levels of crystallographic texture, residual stress, and dislocation density. These features can influence the properties of the material and their development during post-processing operations. In this study, IN718 prisms were built by laser powder bed fusion (PBF-LB/M) using two different scanning strategies (continuous 67° rotations around the build direction, ROT, and alternating 0°/67° scans, ALT) to provide two different as-built conditions. In situ time-resolved synchrotron diffraction was performed during a solution heat treatment at 1027 °C for 1 h. Ex situ scanning electron microscopy was used to support and complement the in situ observations. An approach to quantify the effect of elemental microsegregation at the cell walls is developed based on the deconvolution of asymmetric γ-nickel matrix peaks. Following this approach, the scanning strategies are shown to affect the as-built fraction of cell walls in the material, resulting in a difference of approximately 5 %, in weight fraction, between ROT and ALT (19 % vs. 24 %, respectively). This microsegregation was observed to be rapidly homogenized during the heating ramp, and no significant changes to the peak shape in the γ peaks occurred during the isothermal part of the heat treatment, regardless of the scanning strategy. KW - Additive manufacturing KW - Inconel 718 KW - Synchrotron x-ray diffraction KW - Heat treatment KW - Laser powder bed fusion KW - Cellular microstructure PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650958 DO - https://doi.org/10.1016/j.jmrt.2025.11.214 SN - 2238-7854 VL - 41 SP - 593 EP - 608 PB - Elsevier B.V. AN - OPUS4-65095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Piesker, Benjamin A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Rehmer, Birgit A1 - Agudo Jácome, Leonardo A1 - Hilgenberg, Kai A1 - Evans, Alexander A1 - Skrotzki, Birgit T1 - Tensile and Low‐Cycle Fatigue Behavior of Laser Powder Bed Fused Inconel 718 at Room and High Temperature N2 - This study investigates the room‐ and high‐temperature (650 °C) tensile and low‐cycle‐fatigue behavior of Inconel 718 produced by laser powder bed fusion (PBF‐LB/M) with a four‐step heat treatment and compares the results to the conventional wrought material. The microstructure after heat treatment is characterized on different length scales. Compared to the wrought variant, the elastic and yield properties are comparable at both test temperatures while tensile strength, ductility, and strain hardening capacity are lower. The fatigue life of the PBF‐LB/M variant at room temperature is slightly lower than that of the wrought material, while at 650 °C, it is vice versa. The cyclic stress response for both material variants is characterized by cyclic softening, which is more pronounced at the higher test temperature. High strain amplitudes (≥0.7%) at room temperature and especially a high testing temperature result in the formation of multiple secondary cracks at the transitions of regions comprising predominantly elongated grain morphology and columns of stacked grains with ripple patterns in the PBF‐LB/M material. This observation and pronounced crack branching and deflection indicate that the cracks are controlled by sharp micromechanical gradients and local crystallite clusters. KW - Additive manufacturing KW - Fatigue damage KW - Heat treatment KW - Inconel 718 KW - Laser powder bed fusion KW - Low-cycle fatigue KW - Tensile strength PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599316 DO - https://doi.org/10.1002/adem.202302122 SN - 1527-2648 SP - 1 EP - 17 PB - Wiley AN - OPUS4-59931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ávila Calderón, Luis A1 - Rehmer, Birgit A1 - Schriever, Sina A1 - Ulbricht, Alexander A1 - Agudo Jácome, Leonardo A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Skrotzki, Birgit A1 - Evans, Alexander T1 - Creep and creep damage behavior of stainless steel 316L manufactured by laser powder bed fusion N2 - This study presents a thorough characterization of the creep properties of austenitic stainless steel 316L produced by laser powder bed fusion (LPBF 316L) contributing to the sparse available data to date. Experimental results (mechanical tests, microscopy, X-ray computed tomography) concerning the creep deformation and damage mechanisms are presented and discussed. The tested LPBF material exhibits a low defect population, which allows for the isolation and improved understanding of the effect of other typical aspects of an LPBF microstructure on the creep behavior. As a benchmark to assess the material properties of the LPBF 316L, a conventionally manufactured variant of 316L was also tested. To characterize the creep properties, hot tensile tests and constant force creep tests at 600 °C and 650 °C are performed. The creep stress exponents of the LPBF material are smaller than that of the conventional variant. The primary and secondary creep stages and the times to rupture of the LPBF material are shorter than the hot rolled 316L. Overall the creep damage is more extensive in the LPBF material. The creep damage of the LPBF material is overall mainly intergranular. It is presumably caused and accelerated by both the appearance of precipitates at the grain boundaries and the unfavorable orientation of the grain boundaries. Neither the melt pool boundaries nor entrapped gas pores show a significant influence on the creep damage mechanism. KW - 316L KW - Laser Powder Bed Fusion (LPBF) KW - Creep behavior KW - Additive Manufacturing KW - AGIL PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539373 DO - https://doi.org/10.1016/j.msea.2021.142223 SN - 0921-5093 VL - 830 SP - 142223 PB - Elsevier B.V. AN - OPUS4-53937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocaño, Patricia A1 - Ávila Calderón, Luis A1 - Agudo Jácome, Leonardo A1 - Rehmer, Birgit A1 - Mohr, Gunther A1 - Evans, Alexander A1 - Skrotzki, Birgit T1 - Effect of 700–900 °C heat treatments and room and high temperature tensile deformation on the microstructure of laser powder bed fused 316L stainless steel N2 - The effect of post-processing heat treatments on the hierarchical microstructure evolution and mechanical strength of the austenitic stainless steel 316L produced by laser powder bed fusion has been investigated. Heat treatments between 700 and 900 ◦C and 0.5 to 3 h, were applied to samples treated at 450 ◦C for 4 h. The results showed a stable microstructure at all studied temperatures and times in terms of grain size, morphology, aspect ratio, density of low-angle grain boundaries, and texture. However, temperature and time promoted the diffusion of segregated elements together with a reduction in dislocation density and disappearance of the cellular structure. This was associated with a reduction in hardness and tensile proof strength at both room and high temperature. In addition, microstructural characterization coupled with thermodynamic CALPHAD-based equilibrium calculations showed that the formation of carbides and intermetallic phases was already visible after annealing at 800 ◦C for 3 hours, although these intermetallics did not affect the tensile properties at this level. Analysis of the microstructure evolution after tensile deformation showed differences in the deformation mechanisms at room and high temperature, with twinning and martensitic transformation occurring at room temperature, the latter not widely reported for additively manufactured 316L. Finally, comparisons with similar materials produced under comparable conditions showed differences in the tensile properties, attributed to differences in chemical composition and the associated presence of stacking faults in the undeformed state. KW - Additive manufacturing KW - 316L stainless steel KW - Heat treatments KW - Tensile properties KW - Microstructure PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632471 DO - https://doi.org/10.1016/j.msea.2025.148469 SN - 0921-5093 VL - 939 SP - 1 EP - 24 PB - Elsevier CY - Amsterdam AN - OPUS4-63247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocano, Patricia A1 - Agudo Jácome, Leonardo A1 - Lopez-Galilea, I. A1 - Darvishi Kamachali, Reza A1 - Fries, S. G. T1 - Data regarding the experimental findings compared with CALPHAD calculations of the AlMo0.5NbTa0.5TiZr refractory high entropy superalloy N2 - This contribution contains the raw data used to compare experimental results with thermodynamic calculations using the CALPHAD method, which is related to the research article “The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: experimental findings and comparison with calculations using the CALPHAD method” [1] , and therefore this article can be used as a basis for interpreting the data contained therein. The AlMo0.5NbTa0.5TiZr refractory superalloy was characterized in the cast and annealed condition (1400 °C for 24 h) in order to measure grain size and to identify and measure the size and area fraction of the phases present. The raw data of this article include X-ray diffraction (XRD) measurements, microstructural characterization by scanning and transmission electron microscopy (SEM and TEM), and elemental analysis by energy dispersive X-ray spectroscopy (EDX). XRD includes the determination of phases and the lattice parameters (A2, B2, and hexagonal structure). Microstructural analysis by scanning and transmission electron microscopy includes (1) identification of composition, size, and volume fraction of the present phases and (2) determination of grain size. Based on these experimental data, it is possible to identify similarities and discrepancies with the data calculated using the CALPHAD method for the alloy under study in Ref. [1] , which provides the basis for better and more efficient development of reliable databases. KW - Transmission electron microscopy KW - Scanning electron microscopy KW - Microstructural characterization KW - Refractory high entropy alloys PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568009 DO - https://doi.org/10.1016/j.dib.2022.108858 SN - 2352-3409 VL - 46 SP - 1 EP - 19 PB - Elsevier CY - Amsterdam AN - OPUS4-56800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - Lopez-Galilea, I. A1 - Darvishi Kamachali, Reza A1 - Roik, J. A1 - Agudo Jácome, Leonardo T1 - The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: Experimental findings and comparison with calculations using the CALPHAD method N2 - Detailed microstructural characterization of the AlMo0.5NbTa0.5TiZr refractory high entropy superalloy in the as-cast state is reported for first time and compared with the state annealed at 1400 oC for 24 h. The former shows a dendritic structure, with a mixture of A2/B2 phases < 20 nm in both the dendritic and interdendritic regions. A mostly amorphous phase, rich in Al and Zr, is found within the interdendritic region. The annealed state reproduced the combination of A2/B2/Al-Zr-rich phases reported previously. Calculations from two relevant ThermoCalc databases were compared with the experimental results. Equilibrium calculations were compared with results for the annealed alloy, whereas solidification paths calculated using Scheil-Gulliver model were used for comparison with the as-cast alloy. A previously hypothesized spinodal decomposition during cooling as the mechanism responsible for the patterned A2/B2 microstructure is confirmed via the CALPHAD calculations, pointing to its use as an efficient design tool for such alloys. Finally, the comparison between the experimental and computational findings allowed better understanding the solidification path and equilibrium stability of this alloy, giving a base to make better decisions on the field of new refractory superalloy design. KW - CALPHAD database analysis KW - Refractory superalloys KW - Chemically complex alloy KW - Characterization KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545906 DO - https://doi.org/10.1016/j.matdes.2022.110593 SN - 1873-4197 VL - 217 SP - 1 EP - 13 PB - Elsevier CY - Amsterdam AN - OPUS4-54590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hickel, Tilmann A1 - Waske, Anja A1 - Tehranchi, Ali A1 - Bhattacharya, Biswajit A1 - Stawski, Tomasz M. A1 - Fellinger, Tim-Patrick A1 - Mehmood, Asad A1 - Witt, Julia A1 - Ozcan, Ozlem A1 - Guilherme Buzanich, Ana A1 - Kumar, Sourabh A1 - Mishra, Rajesh Kumar A1 - Holzer, Marco A1 - Stucchi de Camargo, Andrea Simone A1 - Agudo Jácome, Leonardo A1 - Manzoni, Anna A1 - Fantin, Andrea A1 - John, Elisabeth A1 - Hodoroaba, Vasile-Dan A1 - Bührig, Sophia A1 - Murugan, Jegatheesan A1 - Marschall, Niklas A1 - George, Janine A1 - Darvishi Kamachali, Reza A1 - Maaß, Robert A1 - Emmerling, Franziska T1 - Chemically complex materials enable sustainable high-performance materials N2 - Chemically complex materials (CCMats) 􀀀 including high-entropy alloys, oxides, and related multi-principal element systems 􀀀 offer a paradigm shift in materials design by leveraging chemical diversity to simultaneously optimize functional, structural, and sustainability criteria. The vastness of the compositional and structural space in CCMats propels the field into an expanding exploratory state. To reconcile functional and structural performance across this immense parameter space remains an open challenge. This Perspective evaluates the opportunities and challenges associated with harnessing chemical complexity across a broad spectrum of applications, such as hydrogen storage, ionic conductors, catalysis, magnetics, dielectrics, semiconductors, optical materials, and multifunctional structural systems. It is delineated how three central design strategies: targeted substitution (SUB), defect engineering (DEF), and diversity management (DIV) enable the reconciliation of high functional performance with long-term structural stability and environmental responsibility. Advances in computational thermodynamics, microstructure simulations, machine learning, and multimodal characterization are accelerating the exploration and optimization of CCMats, while robust data infrastructures and automated synthesis workflows are emerging as essential tools for navigating their complex compositional space. By fostering cross-disciplinary knowledge transfer and embracing data-driven design, CCMats are poised to deliver next-generation materials solutions that address urgent technological, energy, and environmental demands. KW - Chemically complex materials KW - Structural stability KW - Functional performance KW - Design strategies KW - Sustainability PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655598 UR - https://www.sciencedirect.com/science/article/pii/S1359028626000033?via%3Dihub DO - https://doi.org/10.1016/j.cossms.2026.101256 SN - 1359-0286 VL - 42 SP - 1 EP - 26 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-65559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -