TY - JOUR A1 - Wallis, Theophilus A1 - Ratanaphan, Sutatch A1 - Darvishi Kamachali, Reza T1 - Linking atomistic and phase-field modeling of grain boundaries I: Coarse-graining atomistic structures N2 - The longstanding gap between atomistic and mesoscale simulations partly lies in the absence of a direct, physically grounded connection between atomic structure and mesoscale fields. In this work, we present a robust coarse-graining approach to systematically investigate the connection between phase-field and atomistic simulations of grain boundaries (GBs). The atomistic structures of 408 GBs in BCC-Fe and -Mo were studies to compute and analyze a continuous atomic density field. We discover a fundamental relationship between the GB density---defined as the average atomic density at the GB plane---and the GB excess free volume, an integral property of the boundary. An almost perfect linear correlation between the GB atomic density and GB excess free volume is identified. We also show that the width of BCC GBs, when scaled by the lattice constant, approaches a universal constant value. The relationships among GB density, width, and energy are systematically examined for various GB planes, and the GB energy--density correlations are classified with respect to GB types. It turns out that the atomic planes forming the GB strongly influence both the GB density and excess volume. The current results establish a dependable framework to bridge across scales, enabling density-based phase-field modeling of GBs with atomistic fidelity and enhancing the predictive reliability of mesoscale simulations. KW - Density-based model KW - Grain boundary structure KW - Grain boundary thermodynamic KW - Atomistic simulations PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654872 DO - https://doi.org/10.1016/j.actamat.2025.121786 SN - 1359-6454 VL - 305 SP - 1 EP - 14 PB - Elsevier Inc. AN - OPUS4-65487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wallis, Theophilus A1 - Darvishi Kamachali, Reza T1 - Linking atomistic and phase-field modeling of grain boundaries II: Incorporating atomistic potentials into free energy functional N2 - The density-based phase-field model for grain boundary (GB) thermodynamics and kinetics has offered a broad range of applications in alloy and microstructure design. Originally, this model is based on a potential energy terms that is connected to the cohesive energy of a given substance. A more rigorous approach, however, is a full consideration of an interatomic potential over the possible range of distance and therefore density. In Manuscript I of this series, we developed and thoroughly analyzed the coarse-graining of atomistic GB structures. In this work (Manuscript II), we complete the coupling between atomic and mesoscale modeling of GBs by incorporating the full interatomic potentials into the density-based free energy functional. Using GB energies calculated from atomistic simulations, the coarse-graining approach and the atomistic-integrated density-based Gibbs free energy, we effectively evaluate the density gradient energy coefficient. We found that coupling the density-based model with atomistic potentials reveal physically-sound trends in the GB equilibrium properties. A universal equation was derived to describe the potential energy contribution to the GB energy and the gradient energy coefficient for BCC-Fe and -Mo GBs, similar to the universal equation for GB excess free volume presented in Manuscript I. The proposed approach provides a mesoscale density-based model rooted in atomic-scale characteristics for reliable predictions of GB properties. KW - Density-based model KW - Phase-field KW - Grain boundary structure KW - Grain boundary thermodynamics PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654904 DO - https://doi.org/10.1016/j.actamat.2025.121787 SN - 1359-6454 VL - 305 SP - 1 EP - 17 PB - Elsevier AN - OPUS4-65490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Das, A. A1 - Dufresne, E.M. A1 - Maaß, Robert T1 - Structural dynamics and rejuvenation during cryogenic cycling in a Zr-based metallic glass N2 - Subjecting metallic glasses repeatedly to liquid nitrogen temperature has become a popular method to homogeneously rejuvenate the material. Here we reveal the atomic-scale structural dynamics using in- situ x-ray photon correlation spectroscopy (XPCS) during and after cryogenic cycling of a Zr-based metallic glass in two structural states (plate and ribbon). Heterogeneous structural dynamics is observed at 300 K that changes to monotonic aging at 78 K. It is found that cryogenic cycling homogenizes the relaxation time distribution. This effect is much more pronounced in the ribbon, which is the only structural state that rejuvenates upon cycling. We furthermore reveal how fast atomic-scale dynamics is correlated with longtime structural relaxation times irrespective of the structural state, and that the ribbon exhibits unexpected additional fast atomic-scale relaxation in comparison to the plate material. A structural picture emerges that points towards heterogeneities in the fictive temperature as a requirement for cryogenic energy storage. KW - Structural dynamics KW - Metallic glass KW - Relaxation KW - Rejuvenation KW - Cryogenic cycling PY - 2020 DO - https://doi.org/10.1016/j.actamat.2020.06.063 SN - 1359-6454 VL - 196 SP - 723 EP - 732 PB - Elsevier Ltd. AN - OPUS4-51311 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abboud, M. A1 - Motallebzadeh, A. A1 - Duygulu, O. A1 - Maaß, Robert A1 - Özerinc, S. T1 - Microstructure and nanomechanical behavior of sputtered CuNb thin films N2 - We report on the mechanical properties of Cu–Nb alloys produced by combinatorial magnetron sputtering. Depending on the composition, the microstructure is either fully amorphous (~30–65 at.% Cu), a dispersion of Cu crystallites in an amorphous matrix (~70 at.%), or a dominant crystalline phase with separated nanoscale amorphous zones (~80 at.% Cu). Nanomechanical probing of the different microstructures reveals that the hardness of the fully amorphous alloy is much higher than a rule of mixture would predict. We further demonstrate a remarkable tunability of the resistance to plastic flow, ranging from ca. 9 GPa in the amorphous regime to ca. 2 GPa in the fully crystalline regime. We rationalize these findings based on fundamental structural considerations, thereby highlighting the vast structure-property design space that this otherwise immiscible binary alloy provides. KW - Deposition microstructure KW - Metallic glasses KW - Thin films KW - Mechanical properties KW - Nanocrystalline structure PY - 2021 DO - https://doi.org/10.1016/j.intermet.2021.107249 SN - 0966-9795 VL - 136 SP - 1 EP - 7 PB - Elsevier CY - Amsterdam AN - OPUS4-52777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rizzardi, Q. A1 - Derlet, P. M. A1 - Maaß, Robert T1 - Microstructural signatures of dislocation avalanches in a high-entropy alloy N2 - Here, we trace in situ the slip-line formation and morphological signature of dislocation avalanches in a highentropy alloy with the aim of revealing their microstructural degree of localization. Correlating the intermittent microplastic events with their corresponding slip-line patterns allows defining two main event types, one of which is linked to the formation of new slip lines, whereas the other one involves reactivation of already existing slip lines. The formation of new slip lines reveals statistically larger and faster avalanches. The opposite tendency is seen for avalanches involving reactivation of already existing slip lines. The combination of both these types of events represents the highest degree of spatial avalanche delocalization that spans the entire sample, forming a group of events that determine the truncation length scale of the truncated power-law scaling. These observations link the statistics of dislocation avalanches to a microstructural observable. KW - High-entropy alloy KW - Dislocation avalanches PY - 2021 DO - https://doi.org/10.1103/PhysRevMaterials.5.043604 SN - 2475-9953 VL - 5 IS - 4 SP - 3604 PB - American Physical Society CY - College Park, MD AN - OPUS4-52458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Honrao, S. J. A1 - Rizzardi, Q. A1 - Maaß, Robert A1 - Trinkle, D. R. A1 - Hennig, R. G. T1 - Split-vacancy defect complexes of oxygen in hcp and fcc cobalt N2 - One of the most ubiquitous and important defects in solids is oxygen. Knowledge about the solubility and diffusivity of oxygen in materials is crucial to understand a number of important technological processes, such as oxidation, corrosion, and heterogeneous catalysis. Density-functional theory calculations of the thermodynamics and kinetics of oxygen in cobalt show that oxygen diffusing into the two close-packed phases, namely α (hcp) and β (fcc), strongly interacts with vacancies.We observe the formation of oxygen split-vacancy centers (V-Oi-V) in both phases, and we show that this defect complex exhibits a similar migration energy barrier to the vacancy and oxygen interstitials. In contrast to the vacancy and oxygen interstitials, the oxygen split-vacancy centers exhibit an anisotropic strain field that couples to applied stress, making it possible to observe them through an internal friction experiment on quenched cobalt. KW - Split-vacancy defect complexes PY - 2020 DO - https://doi.org/10.1103/PhysRevMaterials.4.103608 VL - 4 IS - 10 SP - 103608-1 EP - 103608-9 PB - American Physical Society AN - OPUS4-51582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ikeda, Yuki A1 - Mancias, J. A1 - Gan, B. A1 - Maaß, Robert T1 - Evidence of room-temperature shear-deformation in a Cu-Al intermetallic N2 - Lamellar eutectics are known to evidence plastic shear in otherwise brittle intermetallics, if the lamella spacing is small enough. Here we pursue this idea of confined plasticity in intermetallics further and demonstrate room-temperature shear-deformation in a two-phase CuAl 2 -CuAl intermetallic nano- composite. The presence of a phase with a 3-fold symmetry is also revealed after deformation. Simula- tion of transmission electron microscopy images shows this to be monoclinic CuAl. These observations are made in the deformation zone underneath locations of nanoindents, of which the force-displacement curves exhibit an unusual response of continuously increasing pop-in sizes with load. KW - Nanoindentation KW - Intermetallic KW - Nano-composite KW - Shear bands KW - Plasticity PY - 2021 DO - https://doi.org/10.1016/j.scriptamat.2020.08.033 VL - 190 SP - 126 EP - 130 PB - Elsevier Ltd. AN - OPUS4-52455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzer, Marco A1 - Waurischk, Tina A1 - George, Janine A1 - Maaß, Robert A1 - Müller, Ralf T1 - Silicate glass fracture surface energy calculated from crystal structure and bond-energy data N2 - We present a novel method to predict the fracture surface energy, γ, of isochemically crystallizing silicate glasses using readily available crystallographic structure data of their crystalline counterpart and tabled diatomic chemical bond energies, D0. The method assumes that γ equals the fracture surface energy of the most likely cleavage plane of the crystal. Calculated values were in excellent agreement with those calculated from glass density, network connectivity and D0 data in earlier work. This finding demonstrates a remarkable equivalence between crystal cleavage planes and glass fracture surfaces. KW - Glass KW - Fracture surface energy KW - Toughness KW - Modeling KW - Mechanical properties PY - 2023 DO - https://doi.org/10.1016/j.jnoncrysol.2023.122679 SN - 0022-3093 VL - 622 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-58767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Derlet, P. M. A1 - Maaß, Robert T1 - Optimally rejuvenated model binary glasses N2 - Using the creation relaxation algorithm developed for the atomistic modeling of the high-dose irradiation limit of crystalline systems, we explore the limits of the structural rejuvenation of a highly excited model binary glass. This high-energy athermal amorphous structure exhibits a direct transition to homogeneous plastic flow and a microstructure that is largely insensitive to this flow, being characterized by a porous system-spanning network of minimally frustrated structural motifs. The observed homogeneous plasticity is mediated by the same string-like structural excitations, which mediate structural relaxation and microplasticity at finite temperature in more relaxed structures. This highly rejuvenated structural asymptote is not far from the structural state of regions, which have experienced athermal shear localization in more relaxed samples, suggesting an optimally rejuvenated glassy structure will always be limited by that produced by shear localization. KW - Metallic glasses KW - Creation-relaxation algorithm KW - Shear PY - 2022 DO - https://doi.org/10.1103/PhysRevMaterials.6.125604 VL - 6 IS - 12 SP - 1 EP - 13 PB - American Physical Society AN - OPUS4-56741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kar, S. A1 - Ikeda, Yuki A1 - Lünser, K. A1 - Woodcock, Th. G. A1 - Nielsch, K. A1 - Reith, H. A1 - Maaß, Robert A1 - Fähler, S. T1 - Growth Twins and Premartensite Microstructure in Epitaxial Ni-Mn-Ga Films N2 - Magnetic shape memory alloys have been examined intensively due to their multifunctionality and multitude of physical phenomena. For both areas, epitaxial films are promising since the absence of grain boundaries is beneficial for applications in microsystems and they also allow to understand the influence of a reduced dimension on the physical effects. Despite many efforts on epitaxial films, two particular aspects remain open. First, it is not clear how to keep epitaxial growth up to high film thickness, which is required for most microsystems. Second, it is unknown how the microstructure of premartensite, a precursor state during the martensitic transformation, manifests in films and differs from that in bulk. Here, we focus on micrometer-thick austenitic Ni-Mn-Ga films and explain two distinct microstructural features by combining high-resolution electron microscopy and X-ray diffraction methods. First, we identify pyramid-shaped defects, which originate from {1 1 1} growth twinning and cause the breakdown of epitaxial growth. We show that a sufficiently thick Cr buffer layer prevents this breakdown and allows epitaxial growth up to a thickness of at least 4 μm. Second, premartensite exhibits a hierarchical microstructure in epitaxial films. The reduced dimension of films results in variant selection and regions with distinct premartensite variants, unlike its microstructure in bulk. KW - Alloy KW - Epitaxial films KW - Hierarchical microstructure Premartensite KW - Twinning KW - Magnetic shape memory PY - 2023 DO - https://doi.org/10.1016/j.actamat.2023.118902 SN - 1359-6454 VL - 252 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-57301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Das, A. A1 - Ott, C. A1 - Pechimuthu, Dinesh A1 - Moosavi, Robabeh A1 - Stoica, M. A1 - Derlet, P. M. A1 - Maaß, Robert T1 - Shear-band cavitation determines the shape of the stress-strain curve of metallic glasses N2 - Metallic glasses are known to have a remarkably robust yield strength, admitting Weibull moduli as high as for crystalline engineering alloys. However, their postyielding behavior is strongly varying, with large scatter in both flow stress levels and strains at failure. Using x-ray tomography, we reveal how a strain-dependent internal evolution of shear-band cavities underlies this unpredictable postyielding response.We demonstrate how macroscopic strain softening coincides with the first detection of internal shear-band cavitation. Cavity growth during plastic flow is found to follow a power law, which yields a fractal dimension and a roughness exponent in excellent agreement with self-similar surface properties obtained after fracture. These findings demonstrate how internal microcracking coexists with shear-band plasticity along the plastic part of a stress-strain curve, rationalizing the large variability of plastic flow behavior seen for metallic glasses. KW - Shear-band cavitation KW - Metallic glasses PY - 2023 DO - https://doi.org/10.1103/PhysRevMaterials.7.023602 SN - 2475-9953 VL - 7 IS - 2 SP - 1 EP - 11 PB - American Physical Society AN - OPUS4-57042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riechers, Birte A1 - Ott, C. A1 - Das, S. M. A1 - Liebscher, C. A1 - Samwer, K. A1 - Derlet, P. M. A1 - Maaß, Robert T1 - On the elastic microstructure of bulk metallic glasses N2 - Metallic glasses (MGs) are known to be structurally heterogeneous at the nanometer (nm) scale. In addition, elastic property mapping has indicated the presence of at least an order-of-magnitude larger length scales, of which the origin continues to remain unknown. Here we demonstrate the existence of an elastic decorrelation length of the order of 100 nm in a Zr-based bulk MG using spatially resolved elastic property mapping via nanoindentation. Since compositional modulations sufficiently large to account for this elastic microstructure were not resolved by analytical scanning-transmission electron microscopy, chemical phase separation such as spinodal decomposition cannot explain their occurrence as previously suggested. Instead, we argue that the revealed long-range elastic modulations stem from structural variations affecting the local density. These emerge during solidification and are strongly influenced by the cooling constraints imposed on bulk MGs during the casting process. KW - Metallic glasses KW - Nanoindentation KW - Elastic microstructure PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573504 DO - https://doi.org/10.1016/j.matdes.2023.111929 SN - 0264-1275 VL - 229 SP - 1 EP - 8 PB - Elsevier Ltd. CY - Amsterdam, Niederlande AN - OPUS4-57350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darvishi Kamachali, Reza A1 - Wallis, Theophilus A1 - Ikeda, Yuki A1 - Saikia, U. A1 - Ahmadian, A. A1 - Liebscher, C. A1 - Hickel, Tilmann A1 - Maaß, Robert T1 - Giant segregation transition as origin of liquid metal embrittlement in the Fe-Zn system N2 - A giant Zn segregation transition is revealed using CALPHAD-integrated density-based modeling of segregation into Fe grain boundaries (GBs). The results show that above a threshold of only a few atomic percent Zn in the alloy, a substantial amount of up to 60 at.% Zn can segregate to the GB. We found that the amount of segregation abruptly increases with decreasing temperature, while the Zn content in the alloy required for triggering the segregation transition decreases. Direct evidence of the Zn segregation transition is obtained using high-resolution scanning transmission electron microscopy. Base on the model, we trace the origin of the segregation transition back to the low cohesive energy of Zn and a miscibility gap in Fe-Zn GB, arising from the magnetic ordering effect, which is confirmed by ab-initio calculations. We also show that the massive Zn segregation resulting from the segregation transition greatly assists with liquid wetting and reduces the work of separation along the GB. The current predictions suggest that control over Zn segregation, by both alloy design and optimizing the galvanization and welding processes, may offer preventive strategies against liquid metal embrittlement. KW - CALPHAD KW - Microstructure Design KW - Grain boundary engineering KW - Steels KW - Density-based Model KW - Segregation Engineering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584292 DO - https://doi.org/10.1016/j.scriptamat.2023.115758 SN - 1359-6462 SN - 1872-8456 VL - 238 SP - 1 EP - 5 PB - Elsevier CY - Amsterdam AN - OPUS4-58429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kar, Satyakam A1 - Ikeda, Yuki A1 - Nielsch, Kornelius A1 - Reith, Heiko A1 - Maaß, Robert A1 - Fähler, Sebastian T1 - Multiferroic Microstructure Created from Invariant Line Constraint N2 - Ferroic materials enable a multitude of emerging applications, and optimum functional properties are achieved when ferromagnetic and ferroelectric properties are coupled to a first‐order ferroelastic transition. In bulk materials, this first‐order transition involves an invariant habit plane, connecting coexisting phases: austenite and martensite. Theory predicts that this plane should converge to a line in thin films, but experimental evidence is missing. Here, the martensitic and magnetic microstructure of a freestanding epitaxial magnetic shape memory film is analyzed. It is shown that the martensite microstructure is determined by an invariant line constraint using lattice parameters of both phases as the only input. This line constraint explains most of the observable features, which differ fundamentally from bulk and constrained films. Furthermore, this finite‐size effect creates a remarkable checkerboard magnetic domain pattern through multiferroic coupling. The findings highlight the decisive role of finite‐size effects in multiferroics. KW - Epitaxial films KW - Finite-size effects KW - Multiferroics KW - Martensite KW - Magnetic shape memory alloys PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637910 DO - https://doi.org/10.1002/adfm.202416638 SN - 1616-301X VL - 35 IS - 10 SP - 1 EP - 11 PB - Wiley AN - OPUS4-63791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maaß, Robert A1 - Derlet, P. T1 - Micro-plasticity in a fragile model binary glass N2 - Atomistic deformation simulations in the nominally elastic regime are performed for a model binary glass with strain rates as low as 10 4 /s (corresponding to 0.01 shear strain per 1 μs). A strain rate dependent elastic softening due to a micro-plasticity is observed, which is mediated by thermally-activated localized structural transformations (LSEs). A closer inspection of the atomic-scale structure indicates the material response is distinctly different for two types of local atomic environments. A system spanning iscosahe- drally coordinated substructure responds purely elastically, whereas the remaining substructure admits both elastic and microplastic evolution. This leads to a heterogeneous internal stress distribution which, upon unloading, results in negative creep and complete residual-strain recovery. A detailed structural analysis in terms of local stress, atomic displacement, and SU(2) local bonding topology shows such mi- croscopic processes can result in large changes in local stress and are more likely to occur in geomet- rically frustrated regions characterized by higher free volume and softer elastic stiffness. The thermally- activated LSE activity also mediates structural relaxation, and in this way should be distinguished from stress-driven shear transformation activity which only rejuvenates glass structure. The frequency of LSE activity, and therefore the amount of micro-plasticity, is found to be related to the degree to which the glassy state is relaxed. These insights shed atomistic light onto the structural origins that may govern re- cent experimental observations of significant structural evolution in response to elastic loading protocols. KW - Molecular dynamics KW - Bulk metallic glasses KW - Plasticity KW - Residual strains PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523782 DO - https://doi.org/10.1016/j.actamat.2021.116771 VL - 209 SP - 116771 PB - Elsevier Ltd. AN - OPUS4-52378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ikeda, Yuki A1 - Yuan, R. A1 - Chakraborty, A. A1 - Ghassemi-Armaki, H. A1 - Zuo, J. M. A1 - Maaß, Robert T1 - Early stages of liquid-metal embrittlement in an advanced high-strength steel N2 - Grain-boundary degradation via liquid-metal embrittlement (LME) is a prominent and long-standing failure process in next generation advanced high-strength steels. Here we reveal, well ahead of the crack tip, the presences of nano-scale grains of intermetallic phases in Zn-infiltrated but uncracked grain boundaries with scanning- and 4D transmission electron microscopy. Instead of the often-reported Znrich Fe-Zn intermetallics, the nano-scale phase in the uncracked infiltrated grain boundaries is identified as the G-phase, and its presence reveals the local enhancement of strain heterogeneities in the grain boundary network. Based on these observations, we argue that intermetallic phase formation is not occurring after cracking and subsequent liquid Zn infiltration but is instead one of the primary nanoscopic drivers for grain-boundary weakening and crack initiation. These findings shift the focus of LME from micro- and meso-scale crack investigations to the very early stages immediately following Zn diffusion, after which secondary phase nucleation and growth emerge as the root-cause for failure. KW - Advanced high strength steels KW - Liquid metal embrittlement KW - Transmission electron microscopy KW - 4-Dimensional scanning transmission KW - electron microscopy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539716 DO - https://doi.org/10.1016/j.mtadv.2021.100196 SN - 2590-0498 VL - 13 IS - 196 SP - 1 EP - 8 PB - Elsevier Ltd. AN - OPUS4-53971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maaß, Robert T1 - Beyond Serrated Flow in Bulk Metallic Glasses: What Comes Next? N2 - This manuscript is based on an oral contribution to the TMS 2020 annual meeting and is dedicated to Prof. Peter Liaw, who for decades has shown great interest in serrated plastic flow. Here we will focus on the case of bulk metallic glasses, and begin with briefly summarizing some aspects of serrated and non-serrated inhomogeneous flow—a phenomenon that has perplexed materials scientists for decades. Four directions of research are identified that emerged out of the desire to fundamentally understand the intermittent inhomogeneous flow response. These research directions gear away from the phenomenological stress–strain behavior but put the underlying shear defect into focus. Unsolved problems and future research topics are discussed. KW - Non-serrated inhomogeneous flow PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513106 DO - https://doi.org/10.1007/s11661-020-05985-w SN - 1073-5623 SP - 1 EP - 11 PB - Springer Nature AN - OPUS4-51310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ávila Calderón, Luis A1 - Shakeel, Y. A1 - Gedsun, A. A1 - Forti, M. A1 - Hunke, S. A1 - Han, Ying A1 - Hammerschmidt, T. A1 - Aversa, R. A1 - Olbricht, Jürgen A1 - Chmielowski, M. A1 - Stotzka, R. A1 - Bitzek, E. A1 - Hickel, Tilmann A1 - Skrotzki, Birgit T1 - Management of reference data in materials science and engineering exemplified for creep data of a single-crystalline Ni-based superalloy N2 - The identification of process-structure-property relationships of materials inevitably requires the combination of research data from different measurements. Therefore, the concepts related to FAIR (findable, accessible, interoperable, reusable) data handling, increasingly reported in literature, are particularly important in the materials science and engineering domain. However, they have not yet been integrated into a single, overarching methodological framework, particularly for reference data. Here, we introduce such a framework. Our concept covers data generation, documentation, handling, storage, sharing, data search and discovery, retrieval, and usage. Furthermore, we prototypically implement it using a real dataset with creep data of a single-crystal CMSX-6 Ni-based superalloy. The presented implementation is traceable and permanently accessible through open repositories. The individual elements considered in the framework ensure the functionality and usability of the data and, thus, the adherence to the FAIR principles. In conjunction with this, we present a definition for reference data of materials. Our definition underlines particularly the importance of a comprehensive documentation, e.g., on material provenance, data processing procedures, and the software and hardware used, including software-specific input parameters, as these details enable data users or independent parties to assess the quality of the datasets and to reuse and reproduce the results. Reference data that is managed according to the proposed framework can be used to advance knowledge in the materials science and engineering domain, e.g., by identifying new process-structure-property relations. KW - Referenzdaten KW - NFDI-MatWerk KW - Data schema KW - Research Data Management KW - Reference Data PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625047 DO - https://doi.org/10.1016/j.actamat.2025.120735 VL - 286 SP - 1 EP - 15 PB - Elsevier Inc. AN - OPUS4-62504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaiser, Erika A1 - Fareed, Adnan A1 - Manzoni, Anna Maria A1 - Paulisch-Rinke, Melanie C. A1 - Hsu, Wei-Che A1 - Yeh, An-Chou A1 - Murakami, Hideyuki A1 - Vogel, Florian A1 - Maaß, Robert T1 - Pinning-dominated strengthening in high-entropy superalloys N2 - Hierarchical microstructural design of high-entropy superalloys offers novel strengthening pathways beyond classical superalloys. Here we assess the strength of isolated γ’ precipitates with and without an additional internal γ nanophase. The results show that nano-precipitation within the γ’ phase leads to a marked statistical reduction of the dislocation-nucleation limited yield strength. In concert with disorder-driven chemical weakening of the γ’ phase, these findings indicate that bulk strengthening due to hierarchical microstructural design in high entropy superalloys must primarily be pinning dominated. KW - High-entropy alloys KW - Superalloys KW - Dislocation nucleation KW - Plasticity PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637590 DO - https://doi.org/10.1016/j.scriptamat.2025.116874 SN - 1359-6462 VL - 268 SP - 1 EP - 6 PB - Elsevier Inc. AN - OPUS4-63759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ikeda, Yuki A1 - Han, Seungchang A1 - Wallis, Theophilus A1 - Darvishi Kamachali, Reza A1 - Maaß, Robert T1 - On the preference of liquid-metal embrittlement along high-angle grain-boundaries in galvanized steels N2 - Focusing on the early stages of liquid-metal embrittlement (LME) of Zinc (Zn) coated advanced high-strength steels, we show that the Zn infiltration path prior to grain-boundary decohesion and therefore cracking distinctly follows high-angle grain boundaries (HAGBs). This selective transport prior to LME-induced microcracking rationalizes the experimentally observed post-mortem cracking along martensitic HAGBs. We discuss the selective Zn transport and GB-weakening in terms of an misorientation-angle dependent atomic density and diffusivity, and its effect on GB-segregation. KW - Liquid-metal embrittlement KW - Advanced high-strength steels KW - Grain boundaries PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631103 DO - https://doi.org/10.1016/j.scriptamat.2025.116723 SN - 1359-6462 VL - 265 SP - 1 EP - 5 PB - Elsevier Inc. AN - OPUS4-63110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geffroy, P.-M. A1 - Schubert, Nils Hendrik A1 - Günster, Jens A1 - Zocca, Andrea T1 - Quantification of in-plane stress development during drying of tape-cast ceramic layers by cantilever deflection method N2 - The control of stress development in cast ceramics during drying is usually one of critical steps in ceramic processes, which is important also for additive manufacturing technologies using a suspension as feedstock. This work introduces a method based on the cantilever deflection method, to simultaneously quantify the kinetics of solvent evaporation, the shrinkage and the intensity of in-plane stresses developed during drying. Particular attention is given here to the experimental limits of the method and to the optimization of the experimental conditions to suitably measure the intensity of in-planar stress in the coating. The optimized method is applied to four alumina slurries for the water-based additive manufacturing technology LSD-print. Four stages of drying are identified and discussed in relation with the granulometry and morphology of the alumina ceramic particles. KW - Additive Manufacturing KW - Tape casting KW - Ceramic layers KW - Drying stress PY - 2025 DO - https://doi.org/10.1016/j.jeurceramsoc.2024.116868 VL - 45 IS - 1 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-61044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falkenberg, Rainer A1 - Kamachali, Reza Darvishi T1 - Segregation-induced hydrogen embrittlement in titanium N2 - Although titanium offers an optimal combination of strength, low weight, and toughness for various applications, it suffers from a drawback: loss of ductility upon exposure to hydrogen. In this work, we couple CALPHAD-integrated density-based thermodynamic modelling of hydrogen segregation with an experimentally calibrated fracture model to investigate its on crack propagation in titanium. Here we propose to model the crack propagation path as a quasi-interface with slightly opened structure and reduced atomic density, enabling interstitial hydrogen segregation. The atomic density is then directly linked with the damage parameter. We found that hydrogen segregation in titanium undergoes a significant transition such that above a threshold of only few atomic percent hydrogen in the solid solution, the interfacial hydrogen concentration exceeds 20 at.%. Integrating this information into our fracture model, the material damage evolution could be explained by a segregation-affected Griffith crack energy, resulting in material decohesion. We found that the segregation transition and subsequent embrittlement effects are critically sensitive to the temperature in the system. The present results suggest a mechanism underlying the sudden loss of fracture toughness during crack propagation, in relation to the ductile-to-brittle transition observed in titanium alloys exposed to hydrogen. The proposed CALPHAD-integrated chemo-mechanical framework can be further generalised for studying more complex failure mechanisms in various materials. KW - Segregation transition KW - Hydrogen embrittlement KW - Titanium alloys KW - Crack propagation KW - Ductile-to-brittle transition PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655451 DO - https://doi.org/10.1016/j.mtla.2025.102411 SN - 2589-1529 VL - 41 SP - 1 EP - 12 PB - Elsevier Inc. AN - OPUS4-65545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodricks, Carol Winnifred A1 - Prockat, Annabell A1 - Kalinka, Gerhard A1 - Trappe, Volker T1 - Novel Recyclable Hierarchical Carbon Fiber/Epoxy Composites: Preserving Fiber Length and Orientation Using Elium N2 - Current recycling methods for polymer matrix composites produce short, unoriented carbon fibers, limiting their use to intermediate‐strength applications. A method is therefore needed to recycle fibers while preserving their original length and orientation, enabling a circular economy for carbon fiber composites. This study proposes a novel hierarchical composite designed to retain fiber length and orientation during recycling. Virgin carbon fibers are encased in an insoluble epoxy matrix to form tapes that act as the primary units of the structure. The primary tape matrix shields the fibers from chemical degradation while preserving their alignment throughout recycling. The tapes are then embedded in a secondary recyclable matrix, Elium, a thermoplastic polymer soluble in acetone with mechanical properties comparable to epoxy. The composite is recycled by dissolving the secondary Elium matrix in acetone and recovering the primary tape units with intact fiber length and orientation. The primary units can then be used to assemble new composites. In this study, hierarchical composite laminates underwent recycling up to three times. Their mechanical properties were assessed after each cycle. Laminates with an Elium secondary matrix retained 60%–90% of the mechanical performance of epoxy‐based laminates. Minimal degradation was observed between cycles, and fiber length, orientation, and volume fraction were fully preserved. Pushout tests confirmed that fibers in the primary tapes were sufficiently shielded during the recycling process. These results validate the feasibility of a hierarchical recyclable composite that combines recyclability with high mechanical performance, serving as a proof of concept and providing opportunities for future development. KW - Review KW - Interface KW - Micromechanics KW - Polymer matrix composites KW - Glass fibre reinforced composites PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655276 DO - https://doi.org/10.1002/pc.70869 SN - 0272-8397 SP - 1 EP - 16 PB - Wiley Periodicals LLC. AN - OPUS4-65527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sänger, Johanna Christiane A1 - Pauw, Brian Richard A1 - Riechers, Birte A1 - Zocca, Andrea A1 - Rosalie, Julian A1 - Maaß, Robert A1 - Sturm, Heinz A1 - Günster, Jens T1 - Entering a new dimension in powder processing for advanced ceramics shaping N2 - Filigree structures can be manufactured via two-photon-polymerization (2PP) operating in the regime of non-linear light absorption. For the first time it is possible to apply this technique to the powder processing of ceramic structures with a feature size in the range of the critical defect size responsible for brittle fracture and, thus, affecting fracture toughness of high-performance ceramics. In this way, tailoring of advanced properties can be achieved already in the shaping process. Traditionally, 2PP relies on transparent polymerizable resins, which is diametrically opposed to the usually completely opaque ceramic resins and slurries. Here we present a transparent and photocurable suspension of nanoparticles (resin) with very high mass fractions of yttria-stabilized zirconia particles (YSZ). Due to the extremely well dispersed nanoparticles, scattering of light can be effectively suppressed at the process-relevant wavelength of 800 nm. Sintered ceramic structures with a resolution of down to 500 nm were obtained. Even at reduced densities of 1 to 4 g/cm³, the resulting compressive strength with 4,5 GPa is equivalent or even exceeding bulk monolithic yttria stabilized zirconia. A ceramic metamaterial is born, where the mechanical properties of yttria stabilized zirconia are altered by changing geometrical parameters and gives access to a new class of ceramic materials. KW - Two-photon-polymerization KW - Ceramics KW - Powder processing KW - Transparency KW - Meta material KW - Yttria stabilized zirconia PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564598 DO - https://doi.org/10.1002/adma.202208653 SN - 1521-4095 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ginés-Palomares, J.-C. A1 - Fateri, M. A1 - Schubert, T. A1 - de Peindray d’Ambelle, L. A1 - Simon, Sebastian A1 - Gluth, Gregor A1 - Günster, Jens A1 - Zocca, Andrea T1 - Material aspects of sintering of EAC-1A lunar regolith simulant N2 - Future lunar exploration will be based on in-situ resource utilization (ISRU) techniques. The most abundant raw material on the Moon is lunar regolith, which, however, is very scarce on Earth, making the study of simulants a necessity. The objective of this study is to characterize and investigate the sintering behavior of EAC-1A lunar regolith simulant. The characterization of the simulant included the determination of the phase assemblage, characteristic temperatures determination and water content analysis. The results are discussed in the context of sintering experiments of EAC-1A simulant, which showed that the material can be sintered to a relative density close to 90%, but only within a very narrow range of temperatures (20–30 °C). Sintering experiments were performed for sieved and unsieved, as well as for dried and non-dried specimens of EAC-1A. In addition, an analysis of the densification and mechanical properties of the sintered specimens was done. The sintering experiments at different temperatures showed that the finest fraction of sieved simulant can reach a higher maximum sintering temperature, and consequently a higher densification and biaxial strength. The non-dried powder exhibited higher densification and biaxial strength after sintering compared to the dried specimen. This difference was explained with a higher green density of the non-dried powder during pressing, rather than due to an actual influence on the sintering mechanism. Nevertheless, drying the powder prior to sintering is important to avoid the overestimation of the strength of specimens to be fabricated on the Moon. KW - Lunar regolith KW - Ceramics KW - Microstructure KW - Sintering KW - Softening temperature PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-592668 DO - https://doi.org/10.1038/s41598-023-50391-y SN - 2045-2322 VL - 13 SP - 1 EP - 14 PB - Springer Nature AN - OPUS4-59266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Fateri, M. A1 - Al-Sabbagh, Dominik A1 - Günster, Jens T1 - Investigation of the sintering and melting of JSC-2A lunar regolith simulant N2 - Future lunar exploration can benefit greatly from In-Situ Resource Utilization. Accordingly, the in-Situ Resource Utilization approach highlights the need for detailed analysis of lunar regolith. In this study, JSC-2A Simulant was studied regarding its sintering and melting behaviour using Differential Thermal Analysis under ambient and inert conditions. The minerals at the crystalline peaks were determined using X-Ray Diffraction analysis. Moreover, melting droplet shape and wetting behaviour of pressed regolith samples of different particle size distributions were studied by Hot Stage Microscopy technique. Hot Stage Microscopy experiments were performed at different heating rates under ambient conditions. Bloating effects within the solidified samples were then qualitatively examined by X-ray tomography. Lastly, the optimization of processing strategies for the Additive Manufacturing of lunar regolith is discussed. KW - Lunar regolith KW - Sintering KW - Melting KW - Hot stage microscopy PY - 2020 DO - https://doi.org/10.1016/j.ceramint.2020.02.212 VL - 46 IS - 9 SP - 14097 EP - 14104 PB - Elsevier Ltd. AN - OPUS4-50869 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Günster, Jens A1 - Wang, Gong A1 - Tian, Xiaoyong T1 - 3D Printing Technologies for Extreme Environment in Space N2 - 3D printing technology can realize the rapid fabrication of complicated structures with short production chain, which just meet the requirements for space manufacturing in the future. However, 3D printing technologies in space are still challenging due to the harsh conditions, such as microgravity, high vacuum, and large temperature difference. Meanwhile, in-situ resource utilization and recycling must be considered as a cost effective and resilient resource for 3D printing in space. On the contrary, extreme environmental conditions such as high vacuum and microgravity can also offer significant advantages for advanced materials with high purity and performance. In-situ fabrication of ultra-large components would overcome the weight and structural limitations imposed by rocket launch and change the future strategy for space exploration. The aim of this specially issue is therefore to provide a platform for discussing the potential technologies for 3D printing in space. KW - Additive Manufacturing KW - space PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652654 DO - https://doi.org/10.1016/j.amf.2025.200248 SN - 2950-4317 VL - 4 IS - 3 SP - 1 EP - 2 PB - Elsevier AN - OPUS4-65265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chouquet, Xavier A1 - Bolten, Julia A1 - Prinz, Carsten A1 - Günster, Jens A1 - Zocca, Andrea ED - Vincenzini, P. T1 - Direct ink writing of zeolite-like AQSOA Z02 for envisioned applications in solar-driven atmospheric water harvesting: Paste formulation and effect of thermal treatments on the water sorption propertie N2 - This work presents the development of porous water adsorbent bodies with complex geometries shaped by direct ink writing additive manufacturing. AQSOA FAM Z02 (Z02), a commercial material similar to SAPO-34 with chabazite structure, was selected as sorbent material. Dynamic vapor sorption analysis demonstrated that Z02 adsorbs and desorbs up to 30 % of its own mass in each cycle, highlighting its potential for this application. To optimize its printability for direct ink writing, aqueous pastes composed of Z02 and bentonite were formulated. Bentonite served as the inorganic binder and was responsible for the mechanical stability of the printed porous bodies after heat treatment. The most suitable paste composition was identified and used to fabricate scaffold structures. These structures were then subjected to different heat treatments at 650 °C, 750 °C and 850 °C to find a suitable compromise between mechanical stability and retention of the sorption properties. Scaffold structures printed with a 20 wt% of bentonite binder were mechanically stable (1.9 ± 1.1 MPa compressive strength) and retained a maximum water uptake of ca. 25 wt% after heat treatment at 750 °C for 1 h. KW - Direct ink writing KW - Zeolite KW - Direct ink wriDynamic vapor sorption KW - Bentonite Water harvesting PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643150 DO - https://doi.org/10.1016/j.ceramint.2025.09.314 SN - 0272-8842 SP - 1 EP - 12 PB - Elsevier Ltd. AN - OPUS4-64315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Bauer, Felix A1 - Uhlemann, Patrick A1 - Thärig, Steffen A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Mechanical testing dataset of cast copper alloys for the purpose of digitalization N2 - This data article presents a set of primary, analyzed, and digitalized mechanical testing datasets for nine copper alloys. The mechanical testing methods including the Brinell and Vickers hardness, tensile, stress relaxation, and low-cycle fatigue (LCF) testing were performed according to the DIN/ISO standards. The obtained primary testing data (84 files) mainly contain the raw measured data along with the testing metadata of the processes, materials, and testing machines. Five secondary datasets were also provided for each testing method by collecting the main meta- and measurement data from the primary data and the outputs of data analyses. These datasets give materials scientists beneficial data for comparative material selection analyses by clarifying the wide range of mechanical properties of copper alloys, including Brinell and Vickers hardness, yield and tensile strengths, elongation, reduction of area, relaxed and residual stresses, and LCF fatigue life. Furthermore, both the primary and secondary datasets were digitalized by the approach introduced in the research article entitled “Toward a digital materials mechanical testing lab” [1]. The resulting open-linked data are the machine-processable semantic descriptions of data and their generation processes and can be easily queried by semantic searches to enable advanced data-driven materials research. KW - FAIR principles KW - Hardness KW - Low-Cycle Fatigue (LCF) KW - Tensile testing KW - Stress relaxation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605005 DO - https://doi.org/10.1016/j.dib.2024.110687 SN - 2352-3409 SP - 1 EP - 15 PB - Elsevier BV AN - OPUS4-60500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Han, Ying A1 - Kruse, Julius A1 - Rosalie, Julian A1 - Radners, J. A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Influence of mean stress and overaging on fatigue life of aluminum alloy EN AW-2618A N2 - Fatigue tests were performed on the forged aluminum alloy EN AW-2618A in the T61 state. Different stress ratios (R = -1, R = 0.1) were selected to study the influence of mean stress on fatigue life. Two overaged states (10 h/230 ◦C, 1000 h/230 ◦C) were also tested to investigate the influence of overaging on fatigue life. Transmission electron microscopy (TEM) was used to characterize the precipitates (S-phase), which are mainly responsible for the strength of the alloy. A fractographic analysis was also performed to determine the failure mode. Overaging reduces the fatigue life compared to the T61 state. The longer the aging time, the lower the fatigue resistance. The reason is the decrease in (yield) strength, which correlates with the radius of the S-phase: the precipitate radius increases by a factor of approximately two for the overaged states compared to the initial state. The analysis of the fracture surfaces showed crack initiation occurs predominantly on the outer surface and is associated with the primary phases. KW - Aluminum alloys KW - Aging KW - Fatigue KW - Microstructure KW - Electron microscopy KW - S-Phase PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583708 DO - https://doi.org/10.1016/j.msea.2023.145660 SN - 0921-5093 VL - 886 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-58370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rehmer, Birgit A1 - Bayram, Faruk A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Skrotzki, Birgit T1 - Elastic modulus data for additively and conventionally manufactured variants of Ti-6Al-4V, IN718 and AISI 316 L N2 - This article reports temperature-dependent elastic properties (Young’s modulus, shear modulus) of three alloys measured by the dynamic resonance method. The alloys Ti-6Al-4V, Inconel IN718, and AISI 316 L were each investigated in a variant produced by an additive manufacturing processing route and by a conventional manufacturing processing route. The datasets include information on processing routes and parameters, heat treatments, grain size, specimen dimensions, and weight, as well as Young’s and shear modulus along with their measurement uncertainty. The process routes and methods are described in detail. The datasets were generated in an accredited testing lab, audited as BAM reference data, and are hosted in the open data repository Zenodo. Possible data usages include the verification of the correctness of the test setup via Young’s modulus comparison in low-cycle fatigue (LCF) or thermo-mechanical fatigue (TMF) testing campaigns, the design auf VHCF specimens and the use as input data for simulation purposes. KW - Elastic modulus KW - Young's modulus KW - Shear modulus KW - Additive manufacturing KW - AISI 316L KW - IN 718 KW - Ti-6Al-4V KW - Reference data KW - Temperature dependence PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579716 DO - https://doi.org/10.1038/s41597-023-02387-6 VL - 10 IS - 1 SP - 1 EP - 9 PB - Springer Nature AN - OPUS4-57971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Jürgens, Maria A1 - Uhlemann, Patrick A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Experimental data from service-like creep-fatigue experiments on grade P92 steel N2 - This article refers to the research article entitled “Creep-Fatigue of P92 in Service-Like Tests with Combined Stress- and Strain-Controlled Dwell Times” [1]. It presents experimental mechanical data from complex service-like creep-fatigue experiments performed isothermally at 620 °C and a low strain amplitude of 0.2 % on tempered martensite-ferritic grade P92 steel. The data sets in text file format provide cyclic deformation (min. and max. stresses) and the total (hysteresis) data of all recorded fatigue cycles for three different creep-fatigue experiments: 1) a standard relaxation fatigue (RF) test with symmetrical dwell times of three minutes introduced at minimum and maximum strain, 2) a fully strain-controlled service-like relaxation (SLR) test combining these three-minute peak strain dwells with a 30-minute dwell in between at zero strain, and 3) a partly stress-controlled service-like creep (SLC) test combining the three-minute peak strain dwells with 30-minute dwells at constant stress. Such service-like (SL) tests with additional long-term stress- and strain-controlled dwell times are non-standard, rare, and expensive, making these data very valuable. They may be used to approximate cyclic softening in the technically relevant range, for the design of complex SL experiments, or for detailed analyses of stress-strain hystereses (e.g., for stress or strain partitioning methods, for the determination of hysteresis energies (work), inelastic strain components, etc.). In addition, the latter analyses may supply important input for advanced parametric lifetime modeling of components under creep-fatigue loading or model calibration parameters. KW - Tempered martensite-ferritic steel KW - Creep KW - Stress relaxation KW - Creep-fatigue KW - Dwell times PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578407 DO - https://doi.org/10.1016/j.dib.2023.109333 SN - 2352-3409 VL - 49 SP - 1 EP - 9 PB - Elsevier Inc. AN - OPUS4-57840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jentzsch, Stefan A1 - Stock, Daniel A1 - Häcker, Ralf A1 - Skrotzki, Birgit A1 - Darvishi Kamachali, Reza A1 - Klingbeil, Dietmar A1 - Kindrachuk, Vitaliy T1 - Shear Band Formation with Split Hopkinson Bar Experiments N2 - The essence of dynamic failure is closely linked to dramatic shear deformations which often lead to the formation of adiabatic shear bands (ASB). Under high loading velocities and the subsequent rapid temperature increase, the localization of shear strain is crucial in view of safety issues of systems in mechanical and aircraft engineering, especially with respect to fast rotating components and diverse crash scenarios. In this research, we perform high speed impact tests at the split Hopkinson pressure bar (SHPB) setup and use particular hat-shaped specimen geometries that resemble the stresses and failure conditions at the component level. In the first step, we specify a notched specimen geometry using finite element (FE) simulations to ensure pure shear. Further, quasi-static compressive tests and a series of impact tests at high strain rates of 10^3-10^4 s^-1 are conducted on specimens manufactured from a fine-grain structural steel with the properties of S355. Optical microscopy and electron backscatter diffraction (EBSD) of the sheared zones unveil significant localization to maximal shear strains of about 0.9 accompanied by grain refinement by factors 5 to 14. The displacements across the surface of the specimens are captured with subset-based local digital image correlation (DIC) during the impact time, and serve as an objective to validate a viscoplastic constitutive relationship. More precisely, the deformation distribution is accurately reproduced by the widely recognized Johnson-Cook (JC) model, which features an enhanced description of damage evolution. Thus, combining experimental and characterization techniques, continuum mechanics and reasonable optimization strategies for the identification of model parameters provides an efficient approach for comprehensive insights into the strain localization behaviour and its impact on the mechanical performance of S355 under extreme strain rates and deformations. KW - Adiabatic shear bands KW - Finite element analysis KW - Viscoplastic material modelling KW - Split Hopkinson pressure bar KW - Hat-shaped specimen KW - Johnson–Cook parameter identification PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613339 DO - https://doi.org/10.1016/j.ijmecsci.2024.109749 VL - 284 SP - 1 EP - 14 PB - Elsevier BV AN - OPUS4-61333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisenbart, Miriam A1 - Hanke, Thomas A1 - Bauer, Felix A1 - Beygi Nasrabadi, Hossein A1 - Junghanns, Kurt A1 - Dziwis, Gordian A1 - Tikana, Ladji A1 - Parvez, Ashak Mahmud A1 - van den Boogaart, Karl Gerald A1 - Sajjad, Mohsin A1 - Friedmann, Valerie A1 - Preußner, Johannes A1 - Ramakrishnan, Anantha Narayanan A1 - Klengel, Sandy A1 - Meyer, Lars‐Peter A1 - Martin, Michael A1 - Klotz, Ulrich Ernst A1 - Skrotzki, Birgit A1 - Weber, Matthias T1 - KupferDigital: Ontology‐Based Digital Representation for the Copper Life Cycle N2 - The copper life cycle comprises numerous stages from the alloy production to the manufacturing and usage of engineered parts until recycling. At each step, valuable data are generated and stored; some are transferred to the subsequent stations. A thorough understanding of the materials’ behavior during manufacturing processes or throughout their product lifetime is highly dependent on a reliable data transfer. If, for example, a failure occurs during the service life, information about the manufacturing route can be of decisive importance for detecting the root cause of the failure. Additionally, the life cycle assessment hinges on the availability of data. Recording and storing interoperable structured data is, therefore, a thriving research field with huge implications for the economic strength of the manufacturing industry. In the KupferDigital project, it is demonstrated how an ontology‐based data space can be utilized not only as an innovative method for storing and providing interoperable life cycle data but also as a means to enable automated data analysis and evaluation, leading to new insights and the creation of new knowledge using semantic data and technologies. This work illustrates how data recorded at different research facilities can be integrated into one single data space, allowing queries across heterogeneous sources. KW - Copper Alloy KW - Ontology KW - Digitalization KW - Data Space KW - Semantic Representation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630213 SN - 1527-2648 DO - https://doi.org/10.1002/adem.202401735 VL - 27 IS - 8 SP - 1 EP - 29 PB - Wiley AN - OPUS4-63021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jürgens, Maria A1 - Sonntag, Nadja A1 - Olbricht, Jürgen A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - The effect of dwell times on the thermomechanical fatigue life performance of grade P92 steel at intermediate and low strain amplitudes N2 - Results of an extended TMF test program on grade P92 steel in the temperature range of 620 °C - 300 °C, comprising in-phase (IP) and out-of-phase (OP) tests, partly performed with symmetric dwells at Tmax/Tmin, are presented. In contrast to previous studies, the low-strain regime is also illuminated, which approaches flexible operation in a power plant with start/stop cycles. At all strain amplitudes, the material performance is characterized by continuous cyclic softening, which is retarded in tests at lower strains but reaches similar magnitudes in the course of testing. In the investigated temperature range, the phase angle does not affect fatigue life in continuous experiments, whereas the IP condition is more detrimental in tests with dwells. Fractographic analyses indicate creep-dominated and fatigue-dominated damage for IP and OP, respectively. Analyses of the (micro)hardness distribution in the tested specimens suggest an enhanced microstructural softening in tests with dwell times for the low- but not for the high-strain regime. To rationalize the obtained fatigue data, the fracture-mechanics-based D_TMF concept, which was developed for TMF life assessment of ductile alloys, was applied. It is found that the D_TMF parameter correlates well with the measured fatigue lives, suggesting that subcritical growth of cracks (with sizes from a few microns to a few millimeters) governs failure in the investigated range of strain amplitudes. KW - 9-12%Cr steel KW - Thermomechanical fatigue KW - Symmetric dwell periods KW - Low strain KW - Parametric modeling PY - 2021 DO - https://doi.org/10.1016/j.msea.2020.140593 VL - 805 SP - 140593 PB - Elsevier B.V. AN - OPUS4-52374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Waqfi, R. A. A1 - Khan, C. J. A1 - Irving, O. J. A1 - Matthews, Lauren A1 - Albrecht, T. T1 - Crowding Effects during DNA Translocation in Nanopipettes N2 - Quartz nanopipettes are an important emerging class of electric single-molecule sensors for DNA, proteins, their complexes, as well as other biomolecular targets. However, in comparison to other resistive pulse sensors, nanopipettes constitute a highly asymmetric environment and the transport of ions and biopolymers can become strongly directiondependent. For double-stranded DNA, this can include the characteristic translocation time and tertiary structure, but as we show here, nanoconfinement can also unlock capabilities for biophysical and bioanalytical studies at the single-molecule level. To this end, we show how the accumulation of DNA inside the nanochannel leads to crowding effects, and in some cases reversible blocking of DNA entry, and provide a detailed analysis based on a range of different DNA samples and experimental conditions. Moreover, using biotin-functionalized DNA and streptavidinmodified gold nanoparticles as target, we demonstrate in a proof-of-concept study how the crowding effect, and the resulting increased residence time in nanochannel, can be exploited by first injecting the DNA into the nanochannel, followed by incubation with the nanoparticle target and analysis of the complex by reverse translocation. We thereby integrate elements of sample processing and detection into the nanopipette, as an important conceptual advance, and make a case for the wider applicability of this device concept. KW - DNA translocation KW - Transport KW - Resistive-pulse sensing KW - Nanopores KW - Nanopipettes KW - Crowding KW - Confinement PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630448 DO - https://doi.org/10.1021/acsnano.5c01529 SN - 1936-086X VL - 19 IS - 17 SP - 1 EP - 9 PB - ACS Publications AN - OPUS4-63044 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 - Hajian, A. A1 - Konegger, T. A1 - Bielecki, K. A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Schwarz, S. A1 - Zellner, C. A1 - Schmid, U. T1 - Wet chemical porosification with phosphate buffer solutions for permittivity reduction of LTCC substrates N2 - The wireless high-frequency technology requires a robust, cost-effective, and highly integrated substrate technology offering the capability for areas of tailored permittivity. The wet-chemical porosification of low temperature co-fired ceramics (LTCC) substrates offers such an approach by locally embedding air. Porosification of LTCC in both extremely acidic and alkaline media has been investigated in previous works. However, for improving the available knowledge on the porosification of LTCC with H3PO4 as a standard and a widely used etching solution, the impact of solution concentration was systematically investigated and a substantial improvement in the etching performance was achieved. Moreover, in the present study, for the first time, the intermediate pH values, and the impact of pH as a key parameter on the etching process have been investigated. For this purpose, the applicability of phosphate buffer solution (PBS) as a prospective novel etchant mixture for the porosification of a commercially available LTCC tape (Ceramtape GC) was explored. Valuable information about surface morphology, crystalline composition, and the pore structure of the etched LTCCs was gathered employing scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and mercury porosimetry measurements. Based on these findings, the performance of PBS-based etchant systems towards the generation of porous LTCCs combining high depths of porosification with acceptable surface characteristics for subsequent metallization is demonstrated. Based on the obtained results, by application of a 0.2 mol L−1 solution of PBS, the effective relative permittivity of test samples with a thickness of approximately 600 µm and a porosification depth of 186 µm from each side, could be reduced up to 10% of its initial “as fired” value. Also, based on the measurement results and by measuring the depth of porosification, the permittivity of the etched layer was estimated to show a reduction of up to 22% compared to the initial “as fired” value. KW - LTCC KW - Porosification KW - Wet chemical etching KW - Permittivity reduction PY - 2020 DO - https://doi.org/10.1016/j.jallcom.2020.158059 SN - 0925-8388 VL - 863 SP - 158059 PB - Elsevier B.V. AN - OPUS4-51800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evans, Alexander A1 - Schröder, Jakob A1 - Pirling, T. A1 - Ulbricht, Alexander A1 - Suárez Ocaño, Patricia A1 - Bruno, Giovanni T1 - Resolving the Subsurface Residual Stress Maximum in Laser Powder Bed-Fused 316L Stainless Steel by Diffraction-Based Analysis N2 - Laser powder bed fusion (PBF-LB/M) is a metal additive manufacturing process. Due to the complex nature of the layer-wise, repeated heating and cooling cycles, it tends to generate high-magnitude residual stresses. If not correctly understood and mitigated through in- or post-process approaches, these residual stresses can be detrimental as they are often tensile at the surface. However, determining the magnitude and location of peak tensile residual stresses is not trivial as they are often located subsurface. This work focuses on determining the magnitude and location of these deleterious tensile residual stresses in a PBF-LB/316L specimen. Two diffraction-based Methods are used to reveal the relationship between the residual stresses and the underlying microstructure. On the one hand, high spatial resolution Neutron diffraction is used to determine triaxial stresses from the bulk to a depth of 0.15 mm. On the other hand, laboratory X-ray diffraction coupled with electrolytical layer removal allows the biaxial residual stress depth profile to be probed from the surface to a depth of about 0.6 mm. The results show a good agreement between the two methods. The peak residual stress is shown to be 500 MPa, which appears as a plateau between 0.08 and 0.35 mm in depth. KW - Residual stress KW - Diffraction KW - Laser Powder Bed Fusion KW - 316L KW - Additive manufacturing KW - Microstructure KW - AGIL PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652138 DO - https://doi.org/10.1007/s11837-025-07719-y SN - 1543-1851 VL - 77 IS - 12 SP - 9726 EP - 9737 PB - Springer Nature AN - OPUS4-65213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Evans, Alexander A1 - Polatidis, E. A1 - Čapek, J. A1 - Mohr, Gunther A1 - Serrano-Munoz, Itziar A1 - Bruno, Giovanni T1 - Understanding the impact of texture on the micromechanical anisotropy of laser powder bed fused Inconel 718 N2 - The manufacturability of metallic alloys using laser-based additive manufacturing methods such as laser powder bed fusion has substantially improved within the last decade. However, local melting and solidification cause hierarchically structured and crystallographically textured microstructures possessing large residual stress. Such microstructures are not only the origin of mechanical anisotropy but also pose metrological challenges for the diffraction-based residual stress determination. Here we demonstrate the influence of the build orientation and the texture on the microstructure and consequently the mechanical anisotropy of as-built Inconel 718. For this purpose, we manufactured specimens with [001]/[011]-, [001]- and [011]/[111]-type textures along their loading direction. In addition to changes in the Young’s moduli, the differences in the crystallographic textures result in variations of the yield and ultimate tensile strengths. With this in mind, we studied the anisotropy on the micromechanical scale by subjecting the specimens to tensile loads along the different texture directions during in situ neutron diffraction experiments. In this context, the response of multiple lattice planes up to a tensile strain of 10% displayed differences in the load partitioning and the residual strain accumulation for the specimen with [011]/[111]-type texture. However, the relative behavior of the specimens possessing an [001]/[011]- and [001]-type texture remained qualitatively similar. The consequences on the metrology of residual stress determination methods are discussed. KW - Laser powder bed fusion KW - Additive manufacturing KW - Electron backscatter diffraction KW - Tensile testing KW - Diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555840 DO - https://doi.org/10.1007/s10853-022-07499-9 SN - 1573-4803 VL - 2022 IS - 57 SP - 15036 EP - 15058 PB - Springer Science + Business Media B.V. CY - Dordrecht AN - OPUS4-55584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Evans, Alexander A1 - Luzin, V. A1 - Abreu Faria, G. A1 - Degener, Sebastian A1 - Polatidis, E. A1 - Čapek, J. A1 - Kromm, Arne A1 - Dovzhenko, G. A1 - Bruno, Giovanni T1 - Texture-based residual stress analysis of laser powder bed fused Inconel 718 parts N2 - Although layer-based additive manufacturing methods such as laser powder bed fusion (PBF-LB) offer an immense geometrical freedom in design, they are typically subject to a build-up of internal stress (i.e. thermal stress) during manufacturing. As a consequence, significant residual stress (RS) is retained in the final part as a footprint of these internal stresses. Furthermore, localized melting and solidification inherently induce columnar-type grain growth accompanied by crystallographic texture. Although diffraction-based methods are commonly used to determine the RS distribution in PBF-LB parts, such features pose metrological challenges in their application. In theory, preferred grain orientation invalidates the hypothesis of isotropic material behavior underlying the common methods to determine RS. In this work, more refined methods are employed to determine RS in PBF-LB/M/IN718 prisms, based on crystallographic texture data. In fact, the employment of direction-dependent elastic constants (i.e. stress factors) for the calculation of RS results in insignificant differences from conventional approaches based on the hypothesis of isotropic mechanical properties. It can be concluded that this result is directly linked to the fact that the {311} lattice planes typically used for RS analysis in nickel-based alloys have high multiplicity and less strong texture intensities compared with other lattice planes. It is also found that the length of the laser scan vectors determines the surface RS distribution in prisms prior to their removal from the baseplate. On removal from the baseplate the surface RS considerably relaxes and/or redistributes; a combination of the geometry and the scanning strategy dictates the sub-surface RS distribution. KW - Additive manufacturing KW - Electron backscattered diffraction KW - Principal stress KW - Residual stress PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578331 DO - https://doi.org/10.1107/S1600576723004855 SN - 1600-5767 VL - 56 IS - Pt 4 SP - 1076 EP - 1090 AN - OPUS4-57833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Ávila Calderón, Luis A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Evans, Alexander A1 - Skrotzki, Birgit A1 - Bruno, Giovanni T1 - Evolution of Creep Damage of 316L Produced by Laser Powder Bed Fusion N2 - The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed. KW - Creep KW - Computed Tomography KW - PBF-LB/M/316L KW - Laser Powder Bed Fusion KW - Microstructure KW - AISI 316L KW - Additive Manufacturing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574127 DO - https://doi.org/10.1002/adem.202201581 SP - 1 EP - 9 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-57412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belli, Renan A1 - Hartmann, Sabine A1 - Lubauer, Julia A1 - Pereira, Raíssa Monteiro A1 - Hurle, Katrin A1 - Yin, Ling A1 - Mieller, Björn A1 - Lohbauer, Ulrich T1 - Improving the chipping resistance of pre-sintered zirconia white-bodies N2 - Objectives: The high occurrence of fractures, cracking and chipping of zirconia pre-sintered blanks and blocks during machining decreases their yield and can transfer lifetime-limiting racks to the final sintered restoration. This study has the objective of characterizing the mechanical and fracture properties of two zirconia compositions while varying temperature and time of pre-sintering, in order to assess the space for possible improvement. Methods: We selected two typical granular powders with 3 mol% (3YSZ, Zpex®, Tosoh) or 5 mol% (5YSZ, Zpex Smile®, Tosoh) yttria-stabilized zirconia and two pre-sintered commercial analogs (IPS e.max® ZirCAD MO, Ivoclar and Katana™ STML, Kuraray). The debinding and pre-sintering stages of the experimental powders were characterized using thermal analyses (differential scanning calorimetry and thermogravimetry), and the crystal phase composition was quantified using X-ray diffraction (XRD). Physical and mechanical properties such as density, hardness, flexural modulus, biaxial flexural strength and fracture toughness were measured for two pre-sintering temperatures (1000 ◦C, 1100 ◦C) and increasing holding times at those temperatures (2 h, 4 h, 6 h). The chipping resistance for those conditions was quantified using the edge chipping test using a Vickers diamond indenter. Results: Thermal analyses revealed that both powders show comparable debinding behavior and contained approx. 3.8 mass % organic binder, which burns-out completely between 300 and 400 ◦C. The crystallographic phase changes occurring during the 2–6 h at 1000 ◦C and 1100 ◦C was not detectable in the DSC signal, but quantifiable by XRD. Namely, a major content of monoclinic phase in both powders transforms completely into the two tetragonal phases, starting below 1000 ◦C and concluding above 1100 ◦C. All physical and mechanical properties increased with holding time for both temperatures, though more steeply for pre-sintering at 1100◦C. Edge chipping resistance response was well aligned with other fracture properties, with a more marked improvement for 3YSZ pre-sintered at 1100 ◦C. For all properties, the 3YSZ zirconia showed statistically-higher values for the same temperature-time conditions, in agreement with the values obtained for the commercial materials as well. Significance: The results demonstrate the weakness of pre-sintered zirconia products concerning fracture properties, but also the potential for improvement as related to type of zirconia and pre-sintering conditions. This study outlines the use of a set of mechanical tests that can characterize chipping resistance and guide future research engaging in optimizing the machining resistance of pre-sintered zirconia products. KW - Zirconia KW - Fracture KW - White body KW - Dental materials KW - Pre-sintering PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653457 DO - https://doi.org/10.1016/j.dental.2025.12.012 SN - 0109-5641 SP - 1 EP - 12 PB - Elsevier Inc. AN - OPUS4-65345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Bayerlein, Bernd A1 - von Hartrott, Philipp A1 - Waitelonis, Jörg A1 - Birkholz, Henk A1 - Portella, Pedro Dolabella A1 - Skrotzki, Birgit T1 - FAIR and Structured Data: A Domain Ontology Aligned with Standard‐Compliant Tensile Testing N2 - The digitalization of materials science and engineering (MSE) is currently leading to remarkable advancements in materials research, design, and optimization, fueled by computer‐driven simulations, artificial intelligence, and machine learning. While these developments promise to accelerate materials innovation, challenges in quality assurance, data interoperability, and data management have to be addressed. In response, the adoption of semantic web technologies has emerged as a powerful solution in MSE. Ontologies provide structured and machine‐actionable knowledge representations that enable data integration, harmonization, and improved research collaboration. This study focuses on the tensile test ontology (TTO), which semantically represents the mechanical tensile test method and is developed within the project Plattform MaterialDigital (PMD) in connection with the PMD Core Ontology. Based on ISO 6892‐1, the test standard‐compliant TTO offers a structured vocabulary for tensile test data, ensuring data interoperability, transparency, and reproducibility. By categorizing measurement data and metadata, it facilitates comprehensive data analysis, interpretation, and systematic search in databases. The path from developing an ontology in accordance with an associated test standard, converting selected tensile test data into the interoperable resource description framework format, up to connecting the ontology and data is presented. Such a semantic connection using a data mapping procedure leads to an enhanced ability of querying. The TTO provides a valuable resource for materials researchers and engineers, promoting data and metadata standardization and sharing. Its usage ensures the generation of finable, accessible, interoperable, and reusable data while maintaining both human and machine actionability. KW - Data Interoperability KW - Domain Ontology Development KW - FAIR Data Management KW - Knowledge Representation KW - Tensile Test Ontology KW - Semantic Web Technologies PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598142 DO - https://doi.org/10.1002/adem.202400138 SN - 1438-1656 SP - 1 EP - 19 PB - Wiley VHC-Verlag AN - OPUS4-59814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhadeliya, Ashok A1 - Rehmer, Birgit A1 - Fedelich, Bernard A1 - Jokisch, T. A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Fatigue and fracture in dual-material specimens of nickel-based alloys fabricated by hybrid additive manufacturing N2 - The integration of additive manufacturing with traditional processes, termed hybrid additive manufacturing, has expanded its application domain, particularly in the repair of gas turbine blade tips. However, process-related defects in additively manufactured materials, interface formation, and material property mismatches in dual-material structures can significantly impact the fatigue performance of components. This investigation examines the low cycle fatigue and fatigue crack growth behaviors in dual-material specimens of nickel-based alloys, specifically the additively manufactured STAL15 and the cast alloy 247DS, at elevated temperatures. Low cycle fatigue experiments were conducted at temperatures of 950 °C and 1000 °C under a range of strain levels (0.3%–0.8%) and fatigue crack growth tests were conducted at 950 °C with stress ratios of 0.1 and −1. Fractographic and microscopic analyses were performed to comprehend fatigue crack initiation and crack growth mechanisms in the dual-material structure. The results consistently indicated crack initiation and fatigue fracture in the additively manufactured STAL15 material. Notably, fatigue crack growth retardation was observed near the interface when the crack extended from the additively manufactured STAL15 material to the perpendicularly positioned interface. This study highlights the importance of considering yield strength mismatch, as well as the potential effects of residual stresses and grain structure differences, in the interpretation of fatigue crack growth behavior at the interface. KW - Hybrid additive manufacturing KW - Dual-material nickel-based alloys KW - High-temperature fatigue crack growth KW - Low cycle fatigue PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609340 DO - https://doi.org/10.1016/j.jmrt.2024.08.211 SN - 2238-7854 VL - 32 SP - 3737 EP - 3749 PB - Elsevier B.V. AN - OPUS4-60934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Norouzi, Ebrahim A1 - Sack, Harald A1 - Skrotzki, Birgit T1 - Performance Evaluation of Upper‐Level Ontologies in Developing Materials Science Ontologies and Knowledge Graphs N2 - This study tackles a significant challenge in ontology development for materials science: selecting the most appropriate upper‐level ontologies for creating application‐level ontologies and knowledge graphs. Focusing on the use case of Brinell hardness testing, the research assesses the performance of various top‐level ontologies (TLOs)—basic formal ontology (BFO), elementary multiperspective material ontology (EMMO), and provenance ontology (PROVO)—in developing Brinell testing ontologies (BTOs). Consequently, three versions of BTOs are created using combinations of these TLOs along with their integrated mid‐ and domain‐level ontologies. The performance of these ontologies is evaluated based on ten parameters: semantic richness, domain coverage, extensibility, complexity, mapping efficiency, query efficiency, integration with other ontologies, adaptability to different data contexts, community acceptance, and documentation and maintainability. The results show that all candidate TLOs can effectively develop BTOs, each with its distinct advantages. BFO provides a well‐structured, understandable hierarchy, and excellent query efficiency, making it suitable for integration across various ontologies and applications. PROVO demonstrates balanced performance with strong integration capabilities. Meanwhile, EMMO offers high semantic richness and domain coverage, though its complex structure impacts query efficiency and integration with other ontologies. KW - Materials Science KW - Ontology KW - Knowledge Graph PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612227 DO - https://doi.org/10.1002/adem.202401534 SN - 1527-2648 SP - 1 EP - 18 PB - Wiley AN - OPUS4-61222 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 - Bhadeliya, Ashok A1 - Rehmer, Birgit A1 - Fedelich, Bernard A1 - Jokisch, T. A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Fatigue crack growth behavior of Alloy 247DS brazed joints at high temperatures N2 - Gas turbine components made of nickel-based alloys can be repaired through diffusion brazing. However, process-induced imperfections, defects within the brazing zone, and material property mismatches between the braze alloy and base material may facilitate crack initiation and propagation, ultimately leading to early component failure. To gain insight into the crack growth mechanism and quantitatively characterize fatigue crack growth behavior within brazing zones, fatigue crack growth (FCG) experiments were conducted on brazed joint specimens of nickel-based alloy Alloy 247DS at a temperature of 950 ◦C and a stress ratio R = 0.1. The FCG tests were complemented by fractographic and microstructural analyses, to elucidate the relationship between crack growth mechanisms and the microstructure of the brazed joint. The results demonstrate stable crack propagation within the brazing zone and the nickel-based braze alloy. The latter contains brittle eutectic boride phases and intermetallic phases that reduce the resistance to crack propagation compared to the parent material. This study demonstrates the applicability of standard FCG experimental procedures to fusion zones, thereby enabling a preliminary understanding of crack growth behavior in brazing zones. KW - Diffusion brazing KW - High-temperature fatigue crack growth KW - Nickel-based alloys KW - Alloy 247DS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615250 DO - https://doi.org/10.1016/j.msea.2024.147488 SN - 0921-5093 VL - 918 SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-61525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Hanke, Thomas A1 - Skrotzki, Birgit T1 - Semantic Representation of Low‐Cycle‐Fatigue Testing Data Using a Fatigue Test Ontology and ckan.kupferdigital Data Management System N2 - Addressing a strategy for publishing open and digital research data, this article presents the approach for streamlining and automating the process of storage and conversion of research data to those of semantically queryable data on the web. As the use case for demonstrating and evaluating the digitalization process, the primary datasets from low‐cycle‐fatigue testing of several copper alloys are prepared. The fatigue test ontology (FTO) and ckan.kupferdigital data management system are developed as two main prerequisites of the data digitalization process. FTO has been modeled according to the content of the fatigue testing standard and by reusing the basic formal ontology, industrial ontology foundry core ontology, and material science and engineering ontology. The ckan.kupferdigital data management system is also constructed in such a way that enables the users to prepare the protocols for mapping the datasets into the knowledge graph and automatically convert all the primary datasets to those machine‐readable data which are represented by the web ontology language. The retrievability of the converted digital data is also evaluated by querying the example competency questions, confirming that ckan.kupferdigital enables publishing open data that can be highly reused in the semantic web. KW - Accessible KW - CKAN KW - Interoperable KW - Digitalizations KW - Ontologies KW - Reusable data KW - Fatigue testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604991 UR - https://onlinelibrary.wiley.com/doi/10.1002/adem.202400675 DO - https://doi.org/10.1002/adem.202400675 SN - 1527-2648 SP - 1 EP - 11 PB - Wiley AN - OPUS4-60499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Singh, Shobhit Pratap A1 - Löwe, Peter A1 - Schriever, Sina A1 - Olbricht, Jürgen A1 - Rehmer, Birgit A1 - Nolze, Gert A1 - Skrotzki, Birgit T1 - High-throughput creep evaluation of IN738LC in bending using digital image correlation at 850 °C N2 - High-temperature alloys, when used in structural applications, undergo slow time-dependent deformation known as creep. Assessing creep behavior is critical for estimating the in-service life of these alloys. Conventionally, uniaxial creep tests are widely conducted at elevated temperatures to determine creep rates. In recent years, bending creep of cantilevers, when combined with digital image correlation (DIC), has emerged as a promising high-throughput technique for rapidly estimating creep life. However, the applicability of bending creep above 700 ◦C for high-temperature alloys using DIC has not been fully established. In this work, we compare uniaxial creep rates of the nickel-based superalloy IN738LC with bending creep rates measured at 850 ◦C using high-temperature DIC. The bending creep data show excellent agreement with uniaxial creep results in the stress range of 240–360 MPa. The measured creep xponent, a critical rate-determining parameter, is found to be ~8 for both uniaxial and bending creep, with the rate data scattered within a factor of two. An in-house experimental setup was developed to perform bending creep tests at high temperatures, with strain monitored through DIC. Our results demonstrate that bending creep, combined with DIC, provides a reliable and efficient method for creep testing of high-temperature alloys. Compared to conventional uniaxial creep experiments, this approach requires significantly less time and material, thereby reducing effort, energy, and cost. We anticipate that this technique will serve as a foundation for testing precious high-temperature materials. For instance, in ongoing rapid discoveries of advanced alloys, in-service creep life can be evaluated much faster with reduced material requirements. Moreover, this method holds strong potential for application to high-entropy alloys and additively manufactured alloys designed for demanding high-temperature environments. KW - Digital image correlation KW - Bending creep KW - Nickel-based superalloys KW - High throughput testing KW - High-temperature materials PY - 2025 UR - https://www.sciencedirect.com/science/article/pii/S0921509325017034?via%3Dihub DO - https://doi.org/10.1016/j.msea.2025.149479 VL - 950 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-64814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -