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 - Epishin, A. A1 - Camin, B. A1 - Hansen, L. A1 - Heuser, M. A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Theisen, W. A1 - Fedelich, Bernard T1 - Refinement and Experimental Validation of a Vacancy Model of Pore Annihilation in Single-Crystal Nickel-Base Superalloys during Hot Isostatic Pressing N2 - Initially, as-cast and homogenized single crystals of nickel-base superalloy CMSX-4 are subjected to hot isostatic pressing at 1288 °C. Two series of experiments are conducted: under the same pressure of 103 MPa but with different durations, between 0.5 and 6 h, and under different pressures, between 15 and 150 MPa, but for the same time of 0.5 h. The porosity annihilation is investigated metallographically and by high-resolution synchrotron X-ray tomography. The obtained experimental results are compared with the predictions of the vacancy model proposed recently in the group. Herein, the model is further refined by coupling with X-ray tomography. The model describes the evolution of the pore arrays enclosed in the 3D synchrotron tomograms during hot isostatic pressing and properly predicts the time and stress dependences of the pore annihilation kinetics. The validated model and the obtained experimental results are used for selecting the optimal technological parameters such as applied pressure and processing time KW - Superalloys KW - HIP KW - Single-Crystal KW - Diffusion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526859 DO - https://doi.org/10.1002/adem.202100211 VL - 23 IS - 7 SP - 211 AN - OPUS4-52685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falk, Florian A1 - Sobol, Oded A1 - Stephan-Scherb, Christiane T1 - The impact of the microstructure of Fe-16Cr-0.2C on high-temperature oxidation – sulphidation in SO2 N2 - This study elucidates the impact of the microstructure of Fe-16Cr-0.2C on oxide layer formation at 650 ◦C in Ar-0.5 % SO2. A cold-rolled and two heat-treated states of the alloy were exposed for up to 1000 h. The samples were characterised in detail from microstructural and chemical perspectives using scanning electron microscopy (SEM), X-ray diffraction (XRD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The microstructural modification of the alloy by heat-treatment was advantageous. It was found that Cr-carbides support chromia formation and reduce sulphidation when their area fraction is low and diameter is small. KW - Steel KW - Iron KW - SIMS KW - SEM KW - High temperature corrosion KW - Oxidation KW - Sulphidation PY - 2021 DO - https://doi.org/10.1016/j.corsci.2021.109618 VL - 190 SP - 109618 PB - Elsevier Ltd. AN - OPUS4-53001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Fedelich, Bernard A1 - Finn, Monika A1 - Künecke, Georgia A1 - Rehmer, Birgit A1 - Nolze, Gert A1 - Leistner, C. A1 - Petrushin, N. A1 - Svetlov, I. T1 - Investigation of Elastic Properties of the Single-Crystal Nickel-Base Superalloy CMSX-4 in the Temperature Interval between Room Temperature and 1300 °C N2 - The elastic properties of the single-crystal nickel-base superalloy CMSX-4 used as a blade material in gas turbines were investigated by the sonic resonance method in the temperature interval between room temperature and 1300 °C. Elastic constants at such high temperatures are needed to model the mechanical behavior of blade material during manufacturing (hot isostatic pressing) as well as during technical accidents which may happen in service (overheating). High reliability of the results was achieved using specimens of different crystallographic orientations, exciting various vibration modes as well as precise measurement of the material density and thermal Expansion required for modeling the resonance frequencies by finite element method. Combining the results measured in this work and literature data the elastic constants of the gamma and gamma' phases were predicted. This prediction was supported by measurement of the temperature dependence of the gamma'fraction. All data obtained in this work are given in numerical or analytical forms and can be easily used for different scientific and engineering calculations. KW - Nickel-base superalloys KW - Single-crystals KW - Characterization KW - Elastic constants PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520972 DO - https://doi.org/10.3390/cryst11020152 VL - 11 IS - 2 SP - 152 PB - MDPI AN - OPUS4-52097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Lei A1 - Darvishi Kamachali, Reza T1 - Density-based grain boundary phase diagrams: Application to Fe-Mn-Cr, Fe-Mn-Ni, Fe-Mn-Co, Fe-Cr-Ni and Fe-Cr-Co alloy systems N2 - Phase diagrams are the roadmaps for designing bulk phases. Similar to bulk, grain boundaries can possess various phases, but their phase diagrams remain largely unknown. Using a recently introduced density-based model, here we devise a strategy for computing multi-component grain boundary phase diagrams based on available bulk (CALPHAD) thermodynamic data. Fe-Mn-Cr, Fe-Mn-Ni, Fe-Mn-Co, Fe-Cr-Ni and Fe-Cr-Co alloy systems, as important ternary bases for several trending steels and high-entropy alloys, are studied. We found that despite its solute segregation enrichment, a grain boundary can have lower solubility limit than its corresponding bulk, promoting an interfacial chemical decomposition upon solute segregation. This is revealed here for the Fe-Mn-base alloy systems. The origins of this counter-intuitive feature are traced back to two effects, i.e., the magnetic ordering effect and the low cohesive energy of Mn solute element. Different aspects of interfacial phase stability and GB co-segregation in ternary alloys are investigated as well. We show that the concentration gradient energy contributions reduce segregation level but increase grain boundary solubility limit, stabilizing the GB against a chemical decomposition. Density-based grain boundary phase diagrams offer guidelines for systematic investigation of interfacial phase changes with applications to microstructure defects engineering. KW - Densty-based Thermodynamics KW - Microstrucrue Design KW - Grain Boundary Phase Diagram PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522207 DO - https://doi.org/10.1016/j.actamat.2021.116668 SN - 1359-6454 VL - 207 SP - 116668 PB - Elsevier Ltd. AN - OPUS4-52220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, X. A1 - Darvishi Kamachali, Reza A1 - Boyce, B.L. A1 - Clark, B.G. A1 - Raabe, D. A1 - Thompson, G.B. T1 - Spinodal Decomposition in Nanocrystalline Alloys N2 - For more than half a century, spinodal decomposition has been a key phenomenon in considering the formation of secondary phases in alloys. The most prominent aspect of the spinodal phenomenon is the lack of an energy barrier on its transformation pathway, offering an alternative to the nucleation and growth mechanism. The classical description of spinodal decomposition often neglects the influence of defects, such as grain boundaries, on the transformation because the innate ability for like-atoms to cluster is assumed to lead the process. Nevertheless, in nanocrystalline alloys, with a high population of grain boundaries with diverse characters, the structurally heterogeneous landscape can greatly influence the chemical decomposition behavior. Combining atom-probe tomography, precession electron diffraction and density-based phase-field simulations, we address how grain boundaries contribute to the temporal evolution of chemical decomposition within the miscibility gap of a Pt-Au nanocrystalline system. We found that grain boundaries can actually have their own miscibility gaps profoundly altering the spinodal decomposition in nanocrystalline alloys. A complex realm of multiple interfacial states, ranging from competitive grain boundary segregation to barrier-free low-dimensional interfacial decomposition, occurs with a dependency upon the grain boundary character. KW - Density-based Thermodynamics KW - Nanocrystalline alloys KW - Spinodal decomposition KW - Defects engineering PY - 2021 DO - https://doi.org/10.1016/j.actamat.2021.117054 VL - 215 SP - 117054 PB - Elsevier Ltd. AN - OPUS4-52918 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 - Charmi, Amir A1 - Falkenberg, Rainer A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Sommer, Konstantin A1 - Ulbricht, Alexander A1 - Sprengel, Maximilian A1 - Saliwan Neumann, Romeo A1 - Evans, Alexander A1 - Skrotzki, Birgit T1 - Mechanical anisotropy of additively manufactured stainless steel 316L: An experimental and numerical study N2 - The underlying cause of mechanical anisotropy in additively manufactured (AM) parts is not yet fully understood and has been attributed to several different factors like microstructural defects, residual stresses, melt pool boundaries, crystallographic and morphological textures. To better understand the main contributing factor to the mechanical anisotropy of AM stainless steel 316L, bulk specimens were fabricated via laser powder bed fusion (LPBF). Tensile specimens were machined from these AM bulk materials for three different inclinations: 0◦, 45◦, and 90◦ relative to the build plate. Dynamic Young’s modulus measurements and tensile tests were used to determine the mechanical anisotropy. Some tensile specimens were also subjected to residual stress measurement via neutron diffraction, porosity determination with X-ray micro-computed tomography (μCT), and texture analysis with electron backscatter diffraction (EBSD). These investigations revealed that the specimens exhibited near full density and the detected defects were spherical. Furthermore, the residual stresses in the loading direction were between −74 ± 24 MPa and 137 ± 20 MPa, and the EBSD measurements showed a preferential ⟨110⟩ orientation parallel to the build direction. A crystal plasticity model was used to analyze the elastic anisotropy and the anisotropic yield behavior of the AM specimens, and it was able to capture and predict the experimental behavior accurately. Overall, it was shown that the mechanical anisotropy of the tested specimens was mainly influenced by the crystallographic texture. KW - Mechanical anisotropy KW - Residual stress KW - Crystal plasticity KW - Selective laser melting (SLM) KW - Laser beam melting (LBM) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511719 DO - https://doi.org/10.1016/j.msea.2020.140154 SN - 0921-5093 VL - 799 SP - 140154 PB - Elsevier B.V. AN - OPUS4-51171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lin, Y.-Y. A1 - Schleifer, F. A1 - Holzinger, M. A1 - Ta, N. A1 - Skrotzki, Birgit A1 - Darvishi Kamachali, Reza A1 - Glatzel, U. A1 - Fleck, M. T1 - Quantitative Shape-Classification of Misfitting Precipitates during Cubic to Tetragonal Transformations: Phase-Field Simulations and Experiments N2 - The effectiveness of the mechanism of precipitation strengthening in metallic alloys depends on the shapes of the precipitates. Two different material systems are considered: tetragonal γ′′ precipitates in Ni-based alloys and tetragonal θ′ precipitates in Al-Cu-alloys. The shape formation and evolution of the tetragonally misfitting precipitates was investigated by means of experiments and phase-field simulations. We employed the method of invariant moments for the consistent shape quantification of precipitates obtained from the simulation as well as those obtained from the experiment. Two well-defined shape-quantities are proposed: (i) a generalized measure for the particles aspect ratio and (ii) the normalized λ2, as a measure for shape deviations from an ideal ellipse of the given aspect ratio. Considering the size dependence of the aspect ratio of γ′′ precipitates, we find good agreement between the simulation results and the experiment. Further, the precipitates’ in-plane shape is defined as the central 2D cut through the 3D particle in a plane normal to the tetragonal c-axes of the precipitate. The experimentally observed in-plane shapes of γ′′-precipitates can be quantitatively reproduced by the phase-field model. KW - γ″ phase KW - Phase-field simulation KW - Misfitting precipitate KW - Nickel-base alloy KW - Al-Cu alloy KW - θ′ phase KW - Precipitate shape PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522743 DO - https://doi.org/10.3390/ma14061373 VL - 14 IS - 6 SP - 1373 PB - MDPI AN - OPUS4-52274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ta, N. A1 - Bilal, M. U. A1 - Häusler, I. A1 - Saxena, A. A1 - Lin, Y.-Y. A1 - Schleifer, F. A1 - Fleck, M. A1 - Glatzel, U. A1 - Skrotzki, Birgit A1 - Darvishi Kamachali, Reza T1 - Simulation of the θ′ Precipitation Process with Interfacial Anisotropy Effects in Al-Cu Alloys N2 - The effects of anisotropic interfacial properties and heterogeneous elasticity on the growth and ripening of plate-like θ′-phase (Al2Cu) in Al-1.69 at.% Cu alloy are studied. Multi-phase-field simulations are conducted and discussed in comparison with aging experiments. The precipitate/matrix interface is considered to be anisotropic in terms of its energy and mobility. We find that the additional incorporation of an anisotropic interfacial mobility in conjunction with the elastic anisotropy result in substantially larger aspect ratios of the precipitates closer to the experimental observations. The anisotropy of the interfacial energy shows comparably small effect on the precipitate’s aspect ratio but changes the interface’s shape at the rim. The effect of the chemo-mechanical coupling, i.e., the composition dependence of the elastic constants, is studied as well. We show that the inverse ripening phenomenon, recently evidenced for δ’ precipitates in Al-Li alloys (Park et al. Sci. Rep. 2019, 9, 3981), does not establish for the θ′ precipitates. This is because of the anisotropic stress fields built around the θ′ precipitates, stemming from the precipitate’s shape and the interaction among different variants of the θ′ precipitate, that disturb the chemo-mechanical effects. These results show that the chemo-mechanical effects on the precipitation ripening strongly depend on the degree of sphericity and elastic isotropy of the precipitate and matrix phases. KW - Aging KW - Phase-field simulation KW - Interfacial anisotropy KW - Chemo-mechanical coupling KW - Precipitation KW - Elasticity KW - θ′-(Al2Cu) precipitate phase PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522672 DO - https://doi.org/10.3390/ma14051280 VL - 14 IS - 5 SP - 1280 PB - MDPI AN - OPUS4-52267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritsch, Tobias A1 - Sprengel, Maximilian A1 - Evans, Alexander A1 - Farahbod-Sternahl, L. A1 - Saliwan Neumann, Romeo A1 - Hofmann, M. A1 - Bruno, Giovanni T1 - On the determination of residual stresses in additively manufactured lattice structures N2 - The determination of residual stresses becomes more complicated with increasing complexity of the structures investigated. Additive manufacturing techniques generally allow the production of ‘lattice structures’ without any additional manufacturing step. These lattice structures consist of thin struts and are thus susceptible to internal stress-induced distortion and even cracks. In most cases, internal stresses remain locked in the structures as residual stress. The determination of the residual stress in lattice structures through nondestructive neutron diffraction is described in this work. It is shown how two difficulties can be overcome: (a) the correct alignment of the lattice structures within the neutron beam and (b) the correct determination of the residual stress field in a representative part of the structure. The magnitude and the direction of residual stress are discussed. The residual stress in the strut was found to be uniaxial and to follow the orientation of the strut, while the residual stress in the knots was more hydrostatic. Additionally, it is shown that strain measurements in at least seven independent directions are necessary for the estimation of the principal stress directions. The measurement directions should be chosen according to the sample geometry and an informed choice on the possible strain field. If the most prominent direction is not measured, the error in the calculated stress magnitude increases considerably. KW - Additive manufacturing KW - Laser powder bed fusion KW - Residual stress KW - Principal stress components KW - Neutron diffraction KW - Lattice structures PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520663 DO - https://doi.org/10.1107/S1600576720015344 SN - 1600-5767 VL - 54 SP - 228 EP - 236 AN - OPUS4-52066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Artzt, K. A1 - Rehmer, Birgit A1 - Haubrich, J. A1 - Ávila Calderón, Luis A1 - Schoenstein, F. A1 - Serrano-Munoz, Itziar A1 - Requena, G. A1 - Bruno, Giovanni T1 - Separation of the impact of residual stress and microstructure on the fatigue performance of LPBF Ti-6Al-4V at elevated temperature N2 - Manufacturing defects, high residual stress (RS), and microstructures affect the structural integrity of laser powder bed fusion (LPBF) Ti-6Al-4V. In this study, the individual effect of these factors on fatigue performance at elevated temperature (300 °C) was evaluated. Material in as-built condition and subjected to post-processing, including two heat treatments and hot isostatic pressing, was investigated. It was found that in the absence of tensile RS, the fatigue life at elevated temperature is primary controlled by the defects; and densification has a much stronger effect than the considered heat treatments on the improvement of the mechanical performance. KW - Additive manufacturing KW - Ti-6Al-4V KW - Residual stress KW - Fatigue performance KW - Computed tomography PY - 2021 DO - https://doi.org/10.1016/j.ijfatigue.2021.106239 SN - 0142-1123 VL - 148 SP - 106239 PB - Elsevier Ltd. AN - OPUS4-52369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprengel, Maximilian A1 - Ulbricht, Alexander A1 - Evans, Alexander A1 - Kromm, Arne A1 - Sommer, Konstantin A1 - Werner, Tiago A1 - Kelleher, J. A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - Towards the optimization of post-laser powder bed fusion stress-relieve treatments of stainless steel 316L N2 - This study reports on the stress relaxation potential of stress-relieving heat treatments for laser powder bed fused 316L. The residual stress is monitored non-destructively using neutron diffraction before and after the heat treatment. Moreover, the evolution of the microstructure is analysed using scanning electron microscopy. The results show, that a strong relaxation of the residual stress is obtained when applying a heat treatment temperature at 900°C. However, the loss of the cellular substructure needs to be considered when applying this heat treatment strategy. KW - Residual stress KW - Additive manufacturing KW - Neutron diffraction KW - Projekt AGIL - Alterung additiv gefertigter metallischer Materialien und Komponenten PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536045 DO - https://doi.org/10.1007/s11661-021-06472-6 SN - 1543-1940 VL - 52 IS - 12 SP - 5342 EP - 5356 PB - Springer CY - Boston AN - OPUS4-53604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Mrkwitschka, Paul A1 - Moos, R. A1 - Rabe, Torsten T1 - Glass-ceramic composites as insulation material for thermoelectric oxide multilayer generators N2 - Thermoelectric generators can be used as energy harvesters for sensor applications. Adapting the ceramic multilayer technology, their production can be highly automated. In such multilayer thermoelectric generators, the electrical insulation material, which separates the thermoelectric legs, is crucial for the performance of the device. The insulationmaterial should be adapted to the thermoelectric regarding its averaged coefficient of thermal expansion α and its sintering temperature while maintaining a high resistivity. In this study, starting from theoretical calculations, a glass-ceramic Composite material adapted for multilayer generators fromcalciummanganate and Calcium cobaltite is developed. The material is optimized towards an α of 11 × 10−6 K−1 (20–500◦C), a sintering temperature of 900◦C, and a high resistivity up to 800◦C. Calculated and measured α are in good agreement. The chosen glass-ceramic composite with 45 vol.% quartz has a resistivity of 1 × 107 Ωcm and an open porosity of <3%. Sintered multilayer samples from tape-cast thermoelectric oxides and screen-printed insulation show only small reaction layers. It can be concluded that glass-ceramic composites are a well-suited material class for insulation layers as their physical properties can be tuned by varying glass composition or dispersion phases. KW - Electrical insulators KW - Glass-ceramics KW - Multilayers KW - Thermal expansion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538898 DO - https://doi.org/10.1111/jace.18235 SN - 0002-7820 SP - 1 EP - 10 PB - Wiley Online Library AN - OPUS4-53889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadammal, Naresh A1 - Mishurova, Tatiana A1 - Fritsch, Tobias A1 - Serrano-Munoz, Itziar A1 - Kromm, Arne A1 - Haberland, C. A1 - Portella, Pedro Dolabella A1 - Bruno, Giovanni T1 - Critical role of scan strategies on the development of microstructure, texture, and residual stresses during laser powder bed fusion additive manufacturing N2 - Laser based powder bed fusion additive manufacturing offers the flexibility to incorporate standard and userdefined scan strategies in a layer or in between the layers for the customized fabrication of metallic components. In the present study, four different scan strategies and their impact on the development of microstructure, texture, and residual stresses in laser powder bed fusion additive manufacturing of a nickel-based superalloy Inconel 718 was investigated. Light microscopy, scanning electron microscopy combined with electron backscatter diffraction, and neutron diffraction were used as the characterization tools. Strong textures with epitaxially grown columnar grains were observed along the build direction for the two individual scan strategies. Patterns depicting the respective scan strategies were visible in the build plane, which dictated the microstructure development in the other planes. An alternating strategy combining the individual strategies in the successive layers and a 67◦ rotational strategy weakened the texture by forming finer microstructural features. Von Mises equivalent stress plots revealed lower stress values and gradients, which translates as lower distortions for the alternating and rotational strategies. Overall results confirmed the scope for manipulating the microstructure, texture, and residual stresses during laser powder bed fusion additive manufacturing by effectively controlling the scan strategies. KW - Additive manufacturing KW - Laser powder bed fusion KW - Nickel-based superalloys KW - Scan strategies KW - Residual stresses KW - Microstructure and texture PY - 2021 DO - https://doi.org/10.1016/j.addma.2020.101792 VL - 38 SP - 1792 PB - Elsevier B.V. AN - OPUS4-51944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belli, R. A1 - Hurle, K. A1 - Schürrlein, J. A1 - Petschelt, A. A1 - Werbach, K. A1 - Peterlik, H. A1 - Rabe, Torsten A1 - Mieller, Björn A1 - Lohbauer, U. T1 - Relationships between fracture toughness, Y2O3 fraction and phase content in modern dental Yttria-doped zirconias N2 - The relationship between fracture toughness and Yttria content in modern zirconia ceramics was revised. For that purpose, we evaluated here 10 modern Y2O3-stabilized zirconia (YSZ) materials currently used in biomedical applications, namely prosthetic and implant dentistry. The most relevant range between 2-5 mol% Y2O3 was addressed by selecting from conventional opaque 3 mol% YSZ up to more translucent compositions (4-5 mol% YSZs). A technical 2YSZ was used to extend the range of our evaluation. The bulk mol% Y2O3 concentration was measured by X-Ray Fluorescence Spectroscopy. Phase quantification by Rietveld refinement considered two tetragonal phases or an additional cubic phase. A first-account of the fracture toughness (KIc) of the pre-sintered blocks is given, which amounted to 0.4 – 0.7 MPa√m. In the fully-densified state, an inverse power-law behavior was obtained between KIc and bulk mol% Y2O3 content, whether using only our measurements or including literature data, challenging some established relationships. A linear relationship between KIc and the fraction of the transformable t-phase was established within the range of 30–70 vol%. KW - Ceramics KW - Dental KW - Zirconia KW - Fracture toughness KW - X-ray-diffraction KW - Power law PY - 2021 DO - https://doi.org/10.1016/j.jeurceramsoc.2021.08.003 VL - 41 IS - 15 SP - 7771 EP - 7782 PB - Elsevier Ltd. AN - OPUS4-53107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockenhäuser, Christian A1 - Rowolt, C. A1 - Milkereit, B. A1 - Darvishi Kamachali, Reza A1 - Kessler, O. A1 - Skrotzki, Birgit T1 - On the long-term aging of S-phase in aluminum alloy 2618A N2 - The aluminum alloy 2618A is applied for engine components such as radial compressor wheels which operate for long time at elevated temperatures. This results in coarsening of the hardening precipitates and degradation in mechanical properties during the long-term operation, which is not taken into account in the current lifetime prediction models due to the lack of quantitative microstructural and mechanical data. To address this issue, a quantitative investigation on the evolution of precipitates during long-term aging at 190 °C for up to 25,000 h was conducted. Detailed transmission electron microscopy (TEM) was combined with Brinell hardness measurements and thorough differential scanning calorimetry (DSC) experiments. The results showthat GPB zones and S-phase Al2CuMg grow up to < 1,000 h during which the GPB zones dissolve and S-phase precipitates form. For longer aging times, only S-phase precipitates coarsen, which can be well described using the Lifshitz–Slyozov Wagner theory of ripening. A thorough understanding of the underlying microstructural processes is a prerequisite to enable the integration of aging behavior into the established lifetime models for components manufactured from alloy 2618A. KW - Long-term aging KW - Transmission electron microscopy (TEM) KW - Differential scanning calorimetry (DSC) KW - Microstructure KW - S-phase KW - Ostwald ripening PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519899 DO - https://doi.org/10.1007/s10853-020-05740-x SN - 0022-2461 VL - 56 IS - 14 SP - 8704 EP - 8716 PB - Springer Nature AN - OPUS4-51989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, A. A1 - Nolze, Gert A1 - Cios, G. A1 - Tokarski, T. A1 - Bala, P. T1 - Refined Calibration Model for Improving the Orientation Precision of Electron Backscatter Diffraction Maps N2 - For the precise determination of orientations in polycrystalline materials, electron backscatter diffraction (EBSD) requires a consistent calibration of the diffraction geometry in the scanning electron microscope (SEM). In the present paper, the variation of the projection center for the Kikuchi diffraction patterns which are measured by EBSD is calibrated using a projective transformation model for the SEM beam scan positions on the sample. Based on a full pattern matching approach between simulated and experimental Kikuchi patterns, individual projection center estimates are determined on a subgrid of the EBSD map, from which least-square fits to affine and projective transformations can be obtained. Reference measurements on single-crystalline silicon are used to quantify the orientation errors which result from different calibration models for the variation of the projection center. KW - Scanning electron microscopy KW - Electron backscatter diffraction KW - Kikuchi diffraction KW - Projection center KW - Orientation precision PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509342 DO - https://doi.org/10.3390/ma13122816 VL - 13 IS - 12 SP - 2816 PB - MDPI AN - OPUS4-50934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheuerlein, C. A1 - Andrieux, J. A1 - Michels, M. A1 - Lackner, F. A1 - Chiriac, R. A1 - Hagner, M. A1 - Di Michiel, M. A1 - Meyer, Christian A1 - Toche, F. ED - Foley, C. P. T1 - Effect of the fabrication route on the phase and volume changes during the reaction heat treatment of Nb3Sn superconducting wires N2 - Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation. KW - Nb3Sn KW - Microstructure KW - Phase transformations KW - Volume changes KW - X-ray diffraction KW - Differential scanning calorimetry KW - Synchrotron micro-tomography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505128 DO - https://doi.org/10.1088/1361-6668/ab627c VL - 33 IS - 3 SP - 034004 PB - IOP Publishing CY - Bristol (UK) AN - OPUS4-50512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Cios, G. A1 - Winkelmann, A. T1 - Manual measurement of angles in backscattered and transmission Kikuchi diffraction patterns N2 - A historical tool for crystallographic analysis is provided by the Hilton net, which can be used for manually surveying the crystal lattice as it is manifested by the Kikuchi bands in a gnomonic projection. For a quantitative analysis using the Hilton net, the projection centre as the relative position of the signal source with respect to the detector plane needs to be known. Interplanar angles are accessible with a precision and accuracy which is estimated to be ≤0.3o. Angles between any directions, e.g. zone axes, are directly readable. Finally, for the rare case of an unknown projection-centre position, its determination is demonstrated by adapting an old approach developed for photogrammetric applications. It requires the indexing of four zone axes [uvw]i in a backscattered Kikuchi diffraction pattern of a known phase collected under comparable geometric conditions. KW - Electron backscatter diffraction KW - EBSD KW - Angle measurement KW - Gnomonic projections KW - Kikuchi patterns PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507625 DO - https://doi.org/10.1107/S1600576720000692 VL - 53 SP - 435 EP - 443 AN - OPUS4-50762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matz, R. A1 - Rabe, Torsten A1 - Töpfer, J. A1 - Ziesche, S. T1 - Circuit-Board-Integrated Transformers Design and Manufacture N2 - Transformers couple two sections of a circuit by electromagnetic induction. They are widely used to either transform alternating voltage levels or to transmit power or signals across galvanic isolation. Both of these functions are essential for the operation of sensors and controllers. Covering all aspects from idea to circuit performance and from design to manufacture, this paper presents the first comprehensive description of the making of miniaturized, rugged, up-to-100W transformers for embedding into multilayer circuit boards. For circular coils, the well-manageable Ampere-Laplace law is shown to yield reliable designs, predicting correctly the performance of manufactured hardware. This enables fast design without lengthy finite element modelling. In the low-power linear regime, basic relations describe how the device’s characteristics evolve from the material properties and device structure. While scattering Parameters are useful for the analysis of isolated transformers with their intrinsic parasitics, the interaction with the components of the final circuit and the aspects of power and efficiency are addressed by chain matrixes. While these design rules are similar for multilayer boards of different material (like epoxy, Teflon, ceramics), the manufacturing of ceramic board transformers is considered here in detail. Low-temperature-cofired ceramic (LTCC) boards being sintered at 900 °C are particularly suited for harsh environments with chemical or thermal stress as frequently found at sensor positions. The transformer performance usually benefits from or even requires an integrated ceramic core of higher permeability, a ferrite, to shape the magnetic flux. Methods to sinter ferrites inside a dielectric ceramic multilayerandto measure their performance are therefore described in detail.Asthe sintering behaviour of dielectricandmagnetic ceramics differs considerably, their simultaneous sintering is challenging.However, the sintering temperatures of the usefulMnZnand NiZnCu ferrites can be lowered to that of the dielectric material with only moderate loss of permeability by glass additives. Furthermore, thermal mismatch between materials causes catastrophic failure or at least stress and loss of magnetic performance during cooling to room temperature after sintering. This is avoidable by either adjusting the thermal expansion coefficient of the ferrite or by enclosing the ferrite between stressreleasing separation layers.We present the state of the art in materials development according to the first approach as well as fully functional devices made with the second technique. Other applications not directly addressed but well related to this work are characterized by low load resistance in relation to the coil resistance of the transformer. Efficient power transmission then requires that technological solutions are applied to achieve the lowest possible resistive loss inside the coils by an enlarged conductor cross-section. As this is particularly challenging for LTCC boards, a technique is discussed to fabricate conductor traces with a thickness larger than their width. KW - Multilayer ceramic technology KW - LTCC KW - Transformer PY - 2020 DO - https://doi.org/10.4416/JCST2019-00071 SN - 2190-9385 VL - 11 IS - 1 SP - 44 EP - 61 PB - Göller Verlag CY - Baden-Baden AN - OPUS4-50751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, A. A1 - Cios, G. A1 - Tokarski, T. A1 - Nolze, Gert A1 - Hielscher, R. A1 - Koziel, T. T1 - EBSD orientation analysis based on experimental Kikuchi reference patterns N2 - Orientation determination does not necessarily require complete knowledge of the local atomic arrangement in a crystalline phase. We present a method for microstructural phase discrimination and orientation analysis of phases for which there is only limited crystallographic information available. In this method, experimental Kikuchi diffraction patterns are utilized to generate a self-consistent master reference for use in the technique of Electron Backscatter Diffraction (EBSD). The experimentally derived master data serves as an application-specific reference in EBSD pattern matching approaches. As application examples, we map the locally varying orientations in samples of icosahedral quasicrystals observed in a Ti40Zr40Ni20 alloy, and we analyse AlNiCo decagonal quasicrystals. KW - EBSD KW - Quasicrystal KW - Crystal orientation KW - Pattern matching PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507611 DO - https://doi.org/10.1016/j.actamat.2020.01.053 VL - 188 SP - 376 EP - 385 PB - Elsevier Ltd. AN - OPUS4-50761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cios, G. A1 - Nolze, Gert A1 - Winkelmann, A. A1 - Tokarski, T. A1 - Hielscher, R. A1 - Strzalka, R. A1 - Buganski, I. A1 - Wolny, J. A1 - Bala, P. T1 - Approximant-based orientation determination of quasicrystals using electron backscatter diffraction N2 - Orientation mapping of quasicrystalline materials is demonstrated using crystalline approximant structures in the technique of electron backscatter diffraction (EBSD). The approximant-based orientations are symmetrised according to the rotational point group of the quasicrystal, including the visualization of orientation maps using proper colour keys for quasicrystal symmetries. Alternatively, approximant-based orientation data can also be treated using pseudosymmetry post-processing options in the EBSD system software, which enables basic grain size estimations. Approximant-based orientation analyses are demonstrated for icosahedral and decagonal quasicrystals. KW - EBSD KW - Quasicrystal KW - Approximant KW - Chrystal orientation KW - Data processing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514221 DO - https://doi.org/10.1016/j.ultramic.2020.113093 VL - 218 SP - 113093 PB - Elsevier B.V. AN - OPUS4-51422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koclega, Damian A1 - Radziszewska, A. A1 - Dymek, S. A1 - Morgiel, J. A1 - Maj, L. A1 - Kranzmann, Axel T1 - Improvement of Corrosion Resistance of 13CrMo4-5 Steel by Ni-Based Laser Cladding Coatings N2 - The 13CrMo4-5 ferritic steel is commonly used in power plants, due to its favorable mechanical properties. According to EN 10028-2, this steel can be used at temperatures up to 570°C because of its creep behavior. The inefficient corrosion resistance limits the application of this steel to lower temperatures depending on the gas temperature and slag formation. Therefore, the application of a highly resistant Ni-based coating is proposed to extend the corrosion resistance of elements made of ferritic steel. The corrosion test was performed in an environment containing a mixture of gases, like O2, COx, and SOx, and deposited ashes with elements, e.g., Na, Cl, Ca, Si, C, Fe, and Al. The exposure time was, respectively, 240 h, 1000 h and 4500 h at a temperature of 600°C. The oxide scale formed on the 13CrMo4-5 steel was significantly thicker than on the IN686 coating. The microstructure and chemical and phase compositions of the oxide scale were investigated using light optical microscopy together with scanning and transmission electron microscopy techniques. Energy dispersive x-ray analyses were performed when appropriate. KW - Aggressive environments KW - Corrosion resistance KW - High - temperature KW - Inconel 686 KW - Laser cladding PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514289 DO - https://doi.org/10.1007/s11665-020-04867-x SN - 1059-9495 VL - 29 IS - 6 SP - 3702 EP - 3713 PB - Springer AN - OPUS4-51428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scherb, T. A1 - Fantin, Andrea A1 - Checcia, S. A1 - Stephan-Scherb, Christiane A1 - Escolástico, S. A1 - Franz, A. A1 - Seeger, J. A1 - Meulenberg, W. A. A1 - d'Acapito, F. A1 - Serra, J. M. T1 - Unravelling the crystal structure of Nd5.8WO12-d and Nd5.7W0.75Mo0.25O12-d mixed ionic electronic conductors N2 - Mixed ionic electronic conducting ceramics Nd6-yWO12-d (d is the Oxygen deficiency) provide excellent stability in harsh environments containing strongly reactive gases such as CO2, CO, H2, H2O or H2S. Due to this chemical stability, they are promising and cost-efficient candidate materials for gas separation, catalytic membrane reactors and protonic ceramic fuel cell technologies. As in La6-yWO12-d, the ionic/electronic transport mechanism in Nd6-yWO12-d is expected to be largely controlled by the crystal structure, the conclusive determination of which is still lacking. This work presents a crystallographic study of Nd5.8WO12-d and molybdenum-substituted Nd5.7W0.75Mo0.25O12-d prepared by the citrate complexation route. High-resolution synchrotron and neutron powder diffraction data were used in combined Rietveld refinements to unravel the crystal structure of Nd5.8WO12-d and Nd5.7W0.75Mo0.25O12-d. Both investigated samples crystallize in a defect fluorite crystal structure with space group Fm3m and doubled unit-cell parameter due to cation ordering. Mo replacesWat bothWyckoff sites 4a and 48h and is evenly distributed, in contrast with La6-yWO12-d. X-ray absorption spectroscopy as a function of partial pressure pO2 in the near-edge regions excludes oxidation state changes of Nd (Nd3+) and W(W6+) in reducing conditions: the enhanced hydrogen permeation, i.e. ambipolar conduction, observed in Mo-substituted Nd6-yWO12-d is therefore explained by the higher Mo reducibility and the creation of additional – disordered – oxygen vacancies. KW - Powder diffraction KW - Mixed conductors KW - X-ray absorption spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514607 DO - https://doi.org/10.1107/S1600576720012698 VL - 53 SP - 1471 EP - 1483 AN - OPUS4-51460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duarte, Larissa A1 - Andrade, Ana Carolina A1 - Bettge, Dirk T1 - Fractographic Analysis of Fatigue Striations Formation under different Microstructures and Loading Conditions T1 - Fraktographische Untersuchung der Bildung von Schwingstreifen bei unterschiedlichen Gefügezuständen und Belastungsbedingungen N2 - Fatigue failure of a component can occur at service loads considerably lower than the yield strength of the material. Under fatigue loading condition, the material in the vicinity of the tip of a propagating crack repeatedly deforms plastically, leaving microscopic marks on the crack surface, commonly known as fatigue striations. Counting and measuring fatigue striations is a method in estimating the number of loading cycles a component went through until fracture. Some studies suggest a one-to-one relation between the number of fatigue striations and the number of load cycles, but this relation is still debatable, given that there are many factors influencing the formation of those striations. The main purpose of this work is to analyze the influence of microstructure and mechanical strength on the formation of fatigue striations in structural steels, in order to understand how these material properties are related to the fatigue crack behavior. For such, standard Charpy-V samples were subjected to hardness, fatigue and impact testing. Metallography was performed to characterize the microstructure, and a fractographic analysis by using optical and scanning electron microscopy was carried out to investigate the fracture surface. This study shows that steels with higher ductility have a closer one-to-one relation than those with a higher tensile strength. Above a certain level of tensile strength, fatigue striations do form rarely or completely disappear. N2 - Weit unterhalb der Streckfestigkeit des Werkstoffs kann es durch Schwingbruch zum Bauteilversagen kommen. Unter Schwingbeanspruchung wird der Werkstoff in der Nähe der Spitze eines sich ausbreitenden Risses wiederholt plastisch verformt. Dabei entstehen allgemein als Schwingstreifen bekannte mikroskopische Spuren. Das Zählen und Vermessen von Schwingstreifen ist ein Verfahren zum Schätzen der Anzahl von Belastungszyklen, denen ein Bauteil bis zum Bruch ausgesetzt war. Einige Studien legen hier eine 1 : 1-Beziehung zwischen der Anzahl von Schwingstreifen und der Anzahl von Lastspielen nahe. Dies erscheint angesichts der zahlreichen, die Bildung solcher Streifen beeinflussenden Faktoren allerdings fraglich. Hauptziel dieser Arbeit ist die Untersuchung der Auswirkungen des Gefüges und der mechanischen Festigkeit auf die Bildung von Schwingstreifen in Baustählen, um Zusammenhänge zwischen diesen Werkstoffeigenschaften und dem Schwingbruchverhalten verstehen zu können. Dafür wurden an Standard-Charpy-V-Proben Härte- sowie Schwing- und Schlagprüfungen durchgeführt. Zur Gefügecharakterisierung wurden die Proben metallographisch untersucht. Die Bruchfläche wurde zur Analyse fraktographisch licht- und rasterelektronenmikroskopisch untersucht. Die vorliegende Untersuchung zeigt dabei auf, dass Stähle mit einer höheren Duktilität näher an eine solche 1 : 1-Beziehung herankommen als solche mit einer höheren Zugfestigkeit. Oberhalb einer bestimmten Zugfestigkeit bilden sich selten oder gar keine Schwingstreifen. KW - Schwingstreifen KW - Fatigue striations PY - 2020 DO - https://doi.org/10.3139/147.110668 VL - 57 IS - 12 SP - 869 EP - 886 PB - Carl Hanser Verlag CY - München AN - OPUS4-51952 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taketa, I. A1 - Kalinka, Gerhard A1 - Gorbatikh, L. A1 - Lomov, S. A1 - Verpoest, I. T1 - Influence of cooling rate on the properties of carbon fiber unidirectional composites with polypropylene, polyamide 6, and polyphenylene sulfide matrices N2 - The longitudinal and transverse strength of three unidirectional thermoplastic prepreg systems: carbon fiber/polypropylene (CF/PP), polyamide 6 (CF/PA6), and polyphenylene sulfide (CF/PPS) are studied and analytical formulas are proposed for the estimation of matrix and fiber/matrix interface properties from composites properties. Since the matrices are semi-crystalline thermoplastics, the influence of cooling rate on the strength is statistically evaluated. While the 0° tensile strength is found to be independent of the cooling rate, the 90° tensile strength is strongly influenced by the matrix type and cooling rate. The matrix modulus increases as the cooling rate is decreased; the degree of crystallinity also increases. The matrix residual stress, interfacial shear strength, and mode II interlaminar fracture toughness are also found to depend on the cooling rate, with the trends different for different matrices. KW - Matrix residual stress KW - Thermoplastic prepreg KW - Unidirectional composites KW - Cooling rate KW - Interfacial strength PY - 2020 DO - https://doi.org/10.1080/09243046.2019.1651083 SN - 0924-3046 SN - 1568-5519 N1 - Die originale japanische Version des Artikels erschien in: Journal of the Japan Society for Composite Materials, Jg. 44, Nr. 4 (2018), S. 123-128. - The original Japanese version of the article was published in: Journal of the Japan Society for Composite Materials, vol. 44, no. 4 (2018), pp. 123-128. VL - 29 IS - 1 SP - 101 EP - 113 PB - Taylor & Francis CY - London AN - OPUS4-45433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Schulz, Wencke A1 - Schneider, M. A1 - Karafiludis, Stephanos A1 - Laplanche, G. T1 - High-Temperature Oxidation in Dry and Humid Atmospheres of the Equiatomic CrMnFeCoNi and CrCoNi High- and Medium-Entropy Alloys N2 - Surface degradation phenomena of two model equiatomic alloys from the CrMnFeCoNi alloy system were investigated in 2% O2 and 10% H2O (pO2 = 0.02 and 10−7 atm, respectively) at 800 °C for times up to 96 h. The crystallographic structures, morphologies, and chemical compositions of the corrosion layers developing on CrMnFeCoNi and CrCoNi were comparatively analyzed by mass gain analysis, X-ray diffraction, and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy and electron backscatter diffraction. The oxidation resistance of CrMnFeCoNi is relatively poor due to the fast growth of porous Mnoxide(s). CrCoNi forms an external chromia layer that is dense and continuous in a dry 2% O2 atmosphere. This layer buckles and spalls off after exposure to 10% H2O atmosphere. Beneath the chromia layer, a Cr-depleted zone forms in the CrCoNi alloy in both environments. As the oxide scale spalls off in the H2O-containing atmosphere, a secondary chromia layer was observed and correspondingly enlarges the Cr-depleted zone. In contrast, as the chromia layer remains without significant spallation when CrCoNi is exposed to a dry oxidizing atmosphere, the region depleted in Cr is narrower. KW - High temperature oxidation KW - High entropy alloys KW - Medium entropy alloys KW - CrMnFeCoNi KW - CrCoNi KW - Mn-oxides PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517859 DO - https://doi.org/10.1007/s11085-020-10014-7 SN - 0030-770X VL - 95 IS - 1-2 SP - 105 EP - 133 PB - Springer AN - OPUS4-51785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüders, C. A1 - Kalinka, Gerhard A1 - Li, Wei A1 - Sinapius, M. A1 - Wille, T. T1 - Experimental and numerical multiscale approach to thermally cycled FRP N2 - Due to the different thermal expansion of the constituent materials, cyclic thermal loading of FRP induces alternating stresses in the material at two scales: at the micro scale (level of fibre–matrix-interaction) and at the macro scale (level of the multidirectional laminate). Especially the micro scale effect is not comprehensively investigated yet. Additionally, computational investigations mostly neglect this effect due to the homogenous modelling of the composite material. As this effect is assumed to significantly contribute to the fatigue of FRP at thermal loads, the present paper suggests an experimental and numerical multiscale approach including Experiments at the different involved material scales to separately observe the effects acting at these scales. The approach also includes numerical modelling for each scale to complement the knowledge gained from the Experiments and to create a basis for the consideration of the micro effect even in macroscopic fatigue models treating homogeneous modelled composites. The main focus of the contribution is to bring the overall Approach up for discussion, rather than to present the multiscale modelling details. KW - Fatigue KW - Thermal cycling KW - Fibre reinforced plastic KW - Cryogenic KW - Carbon Fibre KW - Epoxy Resin PY - 2020 DO - https://doi.org/10.1016/j.compstruct.2020.112303 SN - 0263-8223 VL - 244 SP - 112303 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-50844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Thieme, C. A1 - Rüssel, C. T1 - Crystal growth velocities of a highly anisotropic phase obtained via surface and volume crystallization of barium–strontium–zinc silicate glasses N2 - In the past few years, a new phase, Ba0.5Sr0.5Zn2Si2O7 with negative thermal expansion has been described in the literature. Some excess of SiO2 is necessary to produce glasses from which the Ba0.5Sr0.5Zn2Si2O7 phase can be crystallized. Unfortunately, in such glasses usually surface crystallization occurs; however, the addition of nucleating agents such as trace quantities of platinum or relatively high quantities of ZrO2 is necessary to achieve bulk nucleation. These additional components also affect the crystal growth velocity, which furthermore is different for crystal growth from the surface and in the bulk. In this paper, three different chemical compositions containing different ZrO2 concentrations, where one composition additionally contains 100 ppm platinum, are studied with respect to their crystallization behaviour. Although the compositions do not differ much, the crystallization behaviour and also the Crystal growth velocities are surprisingly different. KW - Glass ceramic KW - Crystal growth velocity KW - Low expansion PY - 2020 DO - https://doi.org/10.1007/s10853-020-04773-6 SN - 0022-2461 VL - 55 SP - 10364 EP - 10374 PB - Springer AN - OPUS4-50853 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Niebergall, Ute A1 - Wachtendorf, Volker A1 - Böhning, Martin T1 - Evaluation of UV-induced embrittlement of PE-HD by Charpy impact test N2 - The impact fracture behavior of two common high-density polyethylene grades for container applications were intensively studied by the instrumented Charpy impact test after well-defined exposure to UV-irradiation. Individual stages of the impact event, such as crack initiation and crack propagation energy as well as maximum impact load, were investigated from the recorded load–deflection curves. UV-induced material property changes were further investigated by infrared spectroscopy, differential scanning calorimetry, and dynamic-mechanical analysis as well as density measurements. Based on the results of the Charpy impact test, three indicators were identified to describe the extend of photooxidation on high-density polyethylene: (a) a reduced Charpy impact strength—at least to half of its initial value for a distinctly brittle impact fracture, (b) a marked decrease in the crack propagation contribution to the impact strength, and (c) an increase of the brittle features of the fracture surface. KW - Degradation KW - Mechanical properties KW - Packaging KW - Polyolefins KW - Polyethylene PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509130 DO - https://doi.org/10.1002/APP.49069 SN - 0021-8995 VL - 137 IS - 36 SP - 49069 PB - Wiley AN - OPUS4-50913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xu, F. A1 - Ren, H. A1 - Zheng, M. A1 - Shao, X. A1 - Dai, T. A1 - Wu, Y. A1 - Tian, L. A1 - Liu, Y. A1 - Liu, B. A1 - Günster, Jens A1 - Liu, Y. A1 - Liu, Y. T1 - Development of biodegradable bioactive glass ceramics by DLP printed containing EPCs/BMSCs for bone tissue engineering of rabbit mandible defects N2 - Bioactive glass ceramics have excellent biocompatibility and osteoconductivity; and can form direct chemical bonds with human bones; thus, these ceramic are considered as “Smart” materials. In this study, we develop a new type of bioactive glass ceramic (AP40mod) as a scaffold containing Endothelial progenitor cells (EPCs) and Mesenchymal stem cells (BMSCs) to repair critical-sized bone defects in rabbit mandibles. For in vitro experiments: AP40mod was prepared by Dgital light processing (DLP) system and the optimal ratio of EPCs/BMSCs was screened by analyzing cell proliferation and ALP activity, as well as the influence of genes related to osteogenesis and angiogenesis by direct inoculation into scaffolds. The scaffold showed suitable mechanical properties, with a Bending strength 52.7 MPa and a good biological activity. Additionally, when EPCs/BMSCs ratio were combined at a ratio of 2:1 with AP40mod, the ALP activity, osteogenesis and angiogenesis were significantly increased. For in vivo experiments: application of AP40mod/EPCs/BMSCs (after 7 days of in vitro spin culture) to repair and reconstruct critical-sized mandible defect in rabbit showed that all scaffolds were successfully accurately implanted into the defect area. As revealed by macroscopically and CT at the end of 9 months, defects in the AP40mod/EPCs/BMSCs group were nearly completely covered by normal bone and the degradation rate was 29.9% compared to 20.1% in the AP40mod group by the 3D reconstruction. As revealed by HE and Masson staining analyses, newly formed blood vessels, bone marrow and collagen maturity were significantly increased in the AP40mod/EPCs/BMSCs group compared to those in the AP40mod group. We directly inoculated cells on the novel material to screen for the best inoculation ratio. It is concluded that the AP40mod combination of EPCs/BMSCs is a promising approach for repairing and reconstructing large load bearing bone defect. KW - Three-dimensional Bone tissue engineering KW - Endothelial progenitor cell KW - Bone marrow-derived mesenchymal stem cell KW - Bioactive glass scaffold PY - 2020 DO - https://doi.org/10.1016/j.jmbbm.2019.103532 SN - 1751-6161 VL - 103 SP - 103532 EP - 103532 PB - Elsevier Ltd. AN - OPUS4-50491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Lawrence, M. J. A1 - Celorrio, V. A1 - Wang, Q. A1 - Gu, M. A1 - Sun, Z. A1 - Agudo Jácome, Leonardo A1 - Russell, A. E. A1 - Huang, L. A1 - Rodriguez, P. T1 - Nickel confined in 2D earth-abundant oxide layers for highly efficient and durable oxygen evolution catalysts N2 - Low cost, high-efficiency catalysts towards water splitting are urgently required to fulfil the increasing demand for energy. In this work, low-loading (<20 wt%) Ni-confined in layered metal oxide anode catalysts (birnessite and lepidocrocite titanate) have been synthesized by facile ion exchange methodology and subjected to systematic electrochemical studies. It was found that Ni-intercalated on K-rich birnessite (Ni-KMO) presents an onset overpotential (ηonset) as low as 100 mV and overpotential at 10 mA cm−2 (η10) of 206 mV in pH = 14 electrolyte. By combining electrochemical methods and X-ray absorption and emission spectroscopies (XAS and XES), we demonstrate Ni sites are the active sites for OER catalysis and that the Mn3+ sites facilitate Ni intercalation during the ion-exchange process, but display no observable contribution towards OER activity. The effect of the pH and the nature of the supporting electrolyte on the electrochemical performance was also evaluated. KW - Confined catalyst KW - Low-loading KW - Layered manganese oxide KW - Oxygen evolution reaction KW - Transmission electron microscopy (TEM) PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515027 DO - https://doi.org/10.1039/D0TA04031B SN - 2050-7496 SN - 2050-7488 VL - 8 IS - 26 SP - 13340 EP - 13350 PB - Royal Society of Chemistry CY - London AN - OPUS4-51502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gadelmeier, C. A1 - Haas, S. A1 - Lienig, T. A1 - Manzoni, Anna Maria A1 - Feuerbacher, M. A1 - Glatzel, U. T1 - Temperature Dependent Solid Solution Strengthening in the High Entropy Alloy CrMnFeCoNi in Single Crystalline State N2 - The main difference between high entropy alloys and conventional alloys is the solid solution strengthening effect, which shifts from a single element to a multi-element matrix. Little is known about the effectiveness of this effect at high temperatures. Face-centered cubic, equiatomic, and single crystalline high entropy alloy CrMnFeCoNi was pre-alloyed by arc-melting and cast as a single Crystal using the Bridgman process. Mechanical characterization by creep testing were performed at temperatures of 700, 980, 1100, and 1200°C at different loads under vacuum and compared to single-crystalline pure nickel. The results allow a direct assessment of the influence of the chemical composition without any disturbance by grain boundary sliding or diffusion. The results indicate different behaviors of single crystalline pure nickel and CrMnFeCoNi. At 700°C CrMnFeCoNi is more creep-resistant than Ni, but at 980°C both alloys show a nearly similar creep strength. Above 980°C the creep behavior is identical and the solid solution strengthening effect of the CrMnFeCoNi alloy disappears. KW - High entropy alloys KW - Single crystal PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514572 DO - https://doi.org/10.3390/met10111412 VL - 10 IS - 11 SP - 1412 PB - MDPI AN - OPUS4-51457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Famy, A. A1 - Agudo Jácome, Leonardo A1 - Schönhals, Andreas T1 - Effect of Silver Nanoparticles on the Dielectric Properties and the Homogeneity of Plasma Poly(acrylic acid) Thin Films N2 - For the first time, structure−electrochemical relationships of thin films of a plasma-polymerized acrylic acid/carbon dioxide AA/CO2 (75/25%) copolymer modified by implanted silver nanoparticles are discussed. The pulsed plasma polymerization of AA/CO2 was utilized and adjusted to obtain a maximal amount of COOH Groups forming an almost uncross-linked polymer structure. The prepared polymer layer is rinsed by a silver nitrate solution to impregnate Ag+ ions. This step is followed by its reduction of Ag+ with NaBH4 as a chemical route in comparison to the reduction by sunlight as an ecofriendly photoreduction method. The chemical composition and morphology of the topmost surface layer of the AA/CO2 polymer thin film were investigated by X-ray photoelectron spectroscopy and atomic force microscopy. Moreover, the molecular mobility, conductivity, and thermal stability of the polymer layer were analyzed using broadband dielectric spectroscopy. The dielectric properties of the AA/ CO2 polymer thin film were studied in the presence of Ag+ ions or Ag0. It was found that a cross-linked polymer layer with a smooth surface and high conductivity was obtained in the presence of Ag+/ Ag0. KW - Nanoparticles PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c06712 SN - 1932-7447 VL - 124 IS - 41 SP - 22817 EP - 22826 PB - ACS AN - OPUS4-51468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Kiefer, P. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. T1 - Crack Growth in Hydrous Soda-Lime Silicate Glass N2 - Stable crack growth was measured for nominal dry and water-bearing (6 wt%) soda-lime silicate glasses in double cantilever beam geometry and combined with DMA studies on the effects of dissolved water on internal friction and glass transition, respectively. In vacuum, a decreased slope of logarithmic crack growth velocity versus stress intensity factor is evident for the hydrous glass in line with an increase of b-relaxation intensity indicating more energy Dissipation during fracture. Further, inert crack growth in hydrous glass is found to be divided into sections of different slope, which indicates different water related crack propagation mechanism. In ambient air, a largely extended region II is observed for the hydrous glass, which indicates that crack growth is more sensitive to ambient water. KW - Internal friction KW - Soda-lime silicate glass KW - Water content KW - Stable crack growth KW - DCB geometry KW - Stress intensity factor PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506829 DO - https://doi.org/10.3389/fmats.2020.00066 VL - 7 SP - Articel 66 AN - OPUS4-50682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kiefer, P. A1 - Maiwald, M. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Automated Analysis of Slow Crack Growth in Hydrous Soda-Lime Silicate Glasses N2 - To explore the impact of ambient and structural water on static fatigue, the initiation and growth of 3279 Vickers induced median radial cracks were automatically recorded and analyzed. We find that humidity is more efficient in initiating cracks and promoting their growth than water, which is dissolved in the glass structure. In particular for slow crack growth (< 3x10-6 m s-1), tests in dry nitrogen showed a considerable decrease in the crack growth exponent with increasing water content of the glasses. On the other hand, if tests were performed in humid air, the crack growth exponent was independent of the water content of the hydrous glasses, while stress intensity decreased slightly. These observations indicate that water promotes the processes at the crack-tip regardless of its origin. However, ambient water is more efficient. KW - Indentation fracture toughness KW - Slow crack growth KW - Automated analysis KW - Hydrous glass KW - Vickers indentation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513085 DO - https://doi.org/10.3389/fmats.2020.00268 VL - 7 SP - 268 AN - OPUS4-51308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Kiefer, P. A1 - Deubener, J. A1 - Fechtelkord, M. T1 - Water in Alkali Aluminosilicate Glasses N2 - To understand the influence of water and alkalis on aluminosilicate glasses, three polymerized glasses with varying ratios of Na/K were synthesized [(22. 5-x)Na2O-xK2O-22.5 Al2O3-55 SiO2 with x = 0, 7.5, and 11.25]. Subsequently, these glasses were hydrated (up to 8 wt% H2O) in an internally heated gas pressure vessel. The density of hydrous glasses linearly decreased with water content above 1 wt%, consistent with the partial molar volume of H2O of 12 cm3/mol. Near-infrared spectroscopy revealed that hydroxyl groups are the dominant species at water content of <4 wt%, and molecular water becomes dominating at water content of >5 wt%. The fraction of OH is particularly high in the pure Na-bearing glass compared to the mixed alkali glasses. 27Al magic angle spinning-NMR spectroscopy shows that aluminum is exclusively fourfold coordinated with some variations in the local geometry. It appears that the local structure around Al becomes more ordered with increasing K/Na ratio. The incorporation of H2O reinforces this effect. The differential thermal analysis of hydrous glasses shows a significant mass loss in the range of glass transition already during the first upscan, implying the high mobility of water in the glasses. This observation can be explained by the open structure of the aluminosilicate network and by the low dissociation enthalpy of H2O in the glasses (≈ 8 kJ/mol). The effect of the dissolved H2O on the glass transition temperature is less pronounced than for other aluminosilicate glasses, probably because of the large fraction of Al in the glasses. KW - NMR spectroscopy KW - Alkali aluminosilicate glasses KW - Water speciation KW - Glass transition KW - Infrared spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509497 DO - https://doi.org/10.3389/fmats.2020.00085 VL - 7 SP - 85 AN - OPUS4-50949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manzoni, Anna Maria A1 - Haas, S. A1 - Kropf, H. A1 - Duarte, J. A1 - Cakir, Cafer Tufan A1 - Dubois, F. A1 - Többens, D. A1 - Glatzel, U. T1 - Temperature evolution of lattice misfit in Hf and Mo variations of the Al 10 Co 25 Cr 8 Fe 15 Ni 36 Ti 6 compositionally complex alloy N2 - Misfits of γ- γ’ based Al10Co25Cr8Fe15Ni36Ti6 and its Mo- and Hf-variations are studied up to a temperature of 980 °C and compared with Ni- and Co-based superalloys. The trace elements decrease (Hf) or increase (Mo) the edge radii of the γ’ cuboids without changing their sizes. Atom probe measurements revealed that the Hf alloy prefers the γ’ phase while Mo prefers the γ matrix, leading to a lattice parameters enhancement of both phases, as could be revealed by synchrotron X-ray diffraction. The misfit is influenced in opposite ways: Hf increases the positive misfit, while Mo reduces it at all investigated temperatures. KW - Metal and alloys KW - Transmission electron microscopy KW - X-ray diffraction KW - Atom probe tomography KW - High entropy alloy PY - 2020 DO - https://doi.org/10.1016/j.scriptamat.2020.07.013 VL - 188 SP - 74 EP - 79 PB - Elsevier Ltd. AN - OPUS4-51025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cao, L. A1 - Thome, P. A1 - Agudo Jácome, Leonardo A1 - Somsen, C. A1 - Cailletaud, G. A1 - Eggeler, G. T1 - On the influence of crystallography on creep of circular notched single crystal superalloy specimens N2 - The present work contributes to a better understanding of the effect of stress multiaxiality on the creep behavior of single crystal Ni-base superalloys. For this purpose we studied the creep deformation and rupture behavior of double notched miniature creep tensile specimens loaded in three crystallographic directions [100], [110] and [111] (creep conditions: 950 °C and 400 MPa net section stress). Crystal plasticity finite element method (CPFEM) was used to analyze the creep stress and strain distributions during creep. Double notched specimens have the advantage that when one notch fails, the other is still intact and allows to study a material state which is close to rupture. No notch root cracking was observed, while microstructural damage (pores and micro cracks) were frequently observed in the center of the notch root region. This is in agreement with the FEM results (high axial stress and high hydrostatic stress in the center of the notched specimen). Twinning was observed in the notch regions of [110] and [111] specimens, and <112> {111} twins were detected and analyzed using orientation imaging scanning electron microscopy. The present work shows that high lattice rotations can be detected in SXs after creep fracture, but they are associated with the high strains accumulated in the final rupture event. KW - Single crystal Ni-Base superalloys KW - Double notched creep specimen KW - Stress distribution KW - Lattice rotation KW - Cracks PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506060 DO - https://doi.org/10.1016/j.msea.2020.139255 SN - 0921-5093 VL - 782 SP - 139255 PB - Elsevier B. V. AN - OPUS4-50606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Weber, Kathrin A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Elucidation of orientation relations between Fe-Cr alloys and corrosionproducts after high temperature SO2 corrosion N2 - The early stages of corrosion of Fe-Cr-model alloys (2 and 9 % Cr) were investigated after exposure at 650 °C in0.5 % SO2containing gas by electron backscattered diffraction (EBSD) and transmission electron microscopy(TEM). The impact of the grain orientation of the base alloy on the orientation relations of the corrosion productsis presented. After 2 min–5 min exposure the formation of a multi-layered corrosion zone was discovered. Aclear orientation relationship between ferrite and the (Fe,Cr)3O4 spinel could be demonstrated. The obtainedresults show the importance of the grain orientation on oxidation resistance. KW - Iron KW - TEM KW - SEM KW - High temperature corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508911 DO - https://doi.org/10.1016/j.corsci.2020.108809 VL - 174 SP - 1 EP - 11 PB - Elsevier AN - OPUS4-50891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fantin, Andrea A1 - Orazio Lepore, G. A1 - Manzoni, Anna Maria A1 - Kasatikov, S. A1 - Scherb, T. A1 - Huthwelker, T. A1 - d'Acapito, F. A1 - Schumacher, G. T1 - Short-range chemical order and local lattice distortion in a compositionally complex alloy N2 - This work presents an X-ray absorption spectroscopy study on a single-phase state of the Al8Cr17Co17Cu8Fe17Ni33 compositionally complex alloy, focused on the local crystal structure around each alloying element. The comparison of 1st shell bond lengths, obtained by the analysis of extended X-ray absorption fine structure (EXAFS) measured at the K-edges of each alloying element, indicates that Al8Cr17Co17Cu8Fe17Ni33 crystallizes in a distorted arrangement of an fcc lattice. A modest bond length dependence of the alloying elements with increasing atomic number is observed, with minima and maxima at Cr/Co, and Al/Cu, respectively. 1st shell bond lengths spread over ~0.03 Å; consequently, such variations cannot result in lattice distortions greater than ~0.04 Å. EXAFS results clearly indicate short-range order in the alloy: pairing of Al with Ni and Cu is favored, correlating well with a g’ precipitate composition (Al-Ni-Cu rich) reported in previous work, while Al-Cr bonding is unfavored and no Al-Al pairs are observed. Electronic structure information was obtained through comparison between near-edge regions of alloying Elements and corresponding pure metals. Intensity comparison of K-edge features agree with a charge variation of p states in Al8Cr17Co17Cu8Fe17Ni33, where Ni and Cu act as p states electron acceptors, suggesting an orbital hybridization with Al, responsible for a shrinkage in Al metallic radius in the alloy by 0.17 Å. KW - High entropy alloys KW - EXAFS KW - Compositionally complex alloys PY - 2020 DO - https://doi.org/10.1016/j.actamat.2020.04.034 VL - 193 SP - 329 EP - 337 PB - Elsevier Ltd. AN - OPUS4-50830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Kleinbub, Sherin A1 - Wachtendorf, Volker A1 - Schütter, Jan David A1 - Niebergall, Ute A1 - Böhning, Martin A1 - Koerdt, Andrea T1 - Photo-oxidation of PE-HD affecting polymer/fuel interaction and bacterial attachment N2 - In the present study, a simple approach was used to investigate the effect of UV-exposure on two high density Polyethylene materials (PE-HD), commonly used for storage tanks, on fuel sorption behavior and colonization by microorganisms. The aim was to investigate whether the sorption behavior of the fuels (diesel/biodiesel) and the colonization by microorganisms, frequently occurring in the fuel, is affected and may lead to undesirable or safety-relevant material changes. We showed that the UV-irradiation leads to significant changes of the sorption behavior due to chemi-crystallization and crosslinking. The fuel Sorption is affected by the UV-induced formation of polar carbonyl and hydroxyl groups predominantly occurring at the surface. With respect to microbial colonization behavior for Bacillus subtilis and Pseudomonas aeruginosa, isolated from a contaminated diesel sample, differences of the initial adhesion could be shown depending on the initial type of polyethylene as well as on the degree of UV-induced degradation. KW - High density polyethylene KW - Bacterial attachment KW - UV-irradiation KW - Fuel sorption PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510001 DO - https://doi.org/10.1038/s41529-020-0122-1 VL - 4 IS - 1 SP - Article number: 18 PB - Nature Partner Journals AN - OPUS4-51000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Melo Bernardino, Raphael A1 - Valentino, S. A1 - Franchin, G. A1 - Günster, Jens A1 - Zocca, Andrea T1 - Manufacturing of ceramic components with internal channels by a novel additive/subtractive hybridizazion process N2 - A new approach for fabrication of ceramic components with inner channels is proposed, as a result of the combination of two additive and one subtractive manufacturing processes. In this project, porcelain parts are manufactured by the Layerwise Slurry Deposition (LSD) process, meanwhile end milling and Direct Ink Writing (DIW) are applied to create channels on the surface of the deposited ceramic. Unique to the LSD process is the Formation of a freestanding powder bed with a mechanical strength comparable to conventional slip casted ceramic green bodies. Combining these three processes allows the manufacturing of ceramic objects containing an internal path of ink, which in this case was a graphite-based ink that can be further eliminated by heat treatment to obtain a porcelain object embedded with channels. The results show the capabilities of this method and its potential to fabricate not only parts with inner channels, but also multi-material and multi-functional components (such as integrated electronic circuits). KW - Additive Manufacturing KW - Layerwise Slurry Deposition KW - Hybrid Manufacturing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510012 UR - https://www.sciencedirect.com/science/article/pii/S2666539520300109?via%3Dihub DO - https://doi.org/10.1016/j.oceram.2020.100010 VL - 2 SP - 100010 PB - Elsevier Ltd. AN - OPUS4-51001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilbig, Janka A1 - Borges de Oliveira, F. A1 - Obaton, A.-F. A1 - Schwentenwein, M. A1 - Rübner, Katrin A1 - Günster, Jens T1 - Defect detection in additively manufactured lattices N2 - This paper investigates fast and inexpensive measurement methods for defect detection in parts produced by Additive Manufacturing (AM) with special focus on lattice parts made of ceramics. By Lithography-based Ceramic Manufacturing, parts were built both without defects and with typical defects intentionally introduced. These defects were investigated and confirmed by industrial X-ray Computed Tomography. Alternative inexpensive methods were applied afterwards on the parts such as weighing, volume determination by Archimedes method and gas permeability measurement. The results showed, that defects resulting in around 20% of change in volume and mass could be separated from parts free of defects by determination of mass or volume. Minor defects were not detectable as they were in the range of process-related fluctuations. Permeability measurement did not allow to safely identify parts with defects. The measurement methods investigated can be easily integrated in AM process chains to support quality control. KW - Additive manufacturing KW - Quality assurance KW - Defect detection KW - Lattices KW - Ceramics PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513547 DO - https://doi.org/10.1016/j.oceram.2020.100020 VL - 3 SP - 100020 PB - Elsevier Ltd. AN - OPUS4-51354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kratzig, A. A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Menneken, M. A1 - Bäßler, Ralph T1 - Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature N2 - The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products. KW - Corrosion KW - CCUS KW - In-situ ED-XRD KW - CO2 pipeline transport KW - Oxyfuel KW - Carbon steel KW - Impurities PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506303 DO - https://doi.org/10.3390/pr8040421 SN - 2227-9717 VL - 8 IS - 4 SP - 421-1 EP - 421-19 PB - MDPI CY - Basel AN - OPUS4-50630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Orlov, Nikolai A1 - Kiseleva, A. K. A1 - Milkini, P. A. A1 - Evdokimov, P. V. A1 - Putlayev, V. I. A1 - Günster, Jens T1 - Potentialities of Reaction Sintering in the Fabrication of High-Strength Macroporous Ceramics Based on Substituted Calcium Phosphate N2 - Calcium alkali metal (potassium and sodium) double and triple phosphates have been synthesized in different ways. Was for the first time used reaction sintering to produce ceramics based on calcium alkali metal mixed phosphates and investigated the densification behavior of mixed phosphate-based multiphase materials during sintering by this method. Was presented the microstructure of polished surfaces of sintered samples differing in phase composition and determined the density of ceramics prepared using reaction mixtures differing in composition. The effect of reaction sintering on the porosity of the ceramics has been assessed. Using stereolithographic printing and reaction sintering, was produced macroporous mixed Calcium phosphate-based ceramic implants. Their compressive strength has been determined to be 0.78 ± 0.21 MPa for two-phase samples and 1.02 ± 0.13 MPa for three-phase samples. KW - Reaction Sintering KW - Bio Ceramics PY - 2020 DO - https://doi.org/10.1134/s0020168520120146 VL - 56 IS - 12 SP - 1298 EP - 1306 PB - Pleiades Publishing LTD AN - OPUS4-52004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karl, D. A1 - Duminy, T. A1 - Lima, P. A1 - Kamutzki, F. A1 - Gili, A. A1 - Zocca, Andrea A1 - Günster, Jens A1 - Gurlo, A. T1 - Clay in situ resource utilization with Mars global simulant slurries for additive manufacturing and traditional shaping of unfired green bodies N2 - The wet processing of regolith simulant for clay in situ resource utilization (ISRU) on Mars is presented. The two raw materials from the Mars global simulant family, one without clay (MGS-1) and one with clay - sodium montmorillonite smectite - (MGS-1C) were milled and mixed to produce a simulant with small particle size and reduced clay content (MGS-1C/8). All three simulants and the pure clay raw material were extensively characterized using XRF, synchrotron XRD, gas adsorption and gas pycnometry methods. In a straightforward processing approach, MGS-1C/8 was mixed with water and different dispersant approaches were investigated, all of which gave stable slurries. Particle size distribution, rheology, ion concentration, pH and electrical conductivity of these slurries were characterized. The slurry systems can easily be adapted to fit all typical ceramic shaping routes and here parts of varying complexity from slip casting, throwing on a potter's wheel and additive manufacturing, including material extrusion (robocasting) and binder jetting (powder bed 3D printing) were produced. The unique properties of the sodium montmorillonite clay, which is readily accessible in conjunction with magnesium sulfate on the Martian surface, acted as a natural nanosized binder and produced high strength green bodies (unfired ceramic body) with compressive strength from 3.3 to 7.5 MPa. The most elaborate additive manufacturing technique layerwise slurry deposition (LSD) produced water-resistant green bodies with a compressive strength of 30.8 ± 2.5 MPa by employing a polymeric binder, which is similar or higher than the strength of standard concrete. The unfired green bodies show sufficient strength to be used for remote Habitat building on Mars using additive manufacturing without humans being present. KW - Mars KW - Smectite KW - Clay ISRU KW - MGS-1 regolith simulant KW - 3D printing KW - Additive manufacturing PY - 2020 DO - https://doi.org/10.1016/j.actaastro.2020.04.064 VL - 174 SP - 241 EP - 253 PB - Elsevier Ltd. AN - OPUS4-50870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chinellato, Fabio A1 - Wilbig, Janka A1 - Al-Sabbagh, Dominik A1 - Colombo, P. A1 - Günster, Jens T1 - Gas flow assisted powder deposition for enhanced flowability of fine powders: 3D printing of alpha-tricalcium phosphate N2 - The possibility of creating patient-specific individual implants makes Additive Manufacturing technologies of special interest for the medical sector. For substitution of bone defects, powder based Additive Manufacturing by Binder Jetting is a suitable method to produce complex scaffold-like structures made of bioceramics with easily adapted geometries and controlled porosity. The process inherent residual porosity in the printed part, even though desired as it supports bone ingrowth, also leads to limited mechanical strength. Currently, bioceramic scaffolds made by Binder Jetting feature suitable biocompatible and biodegradable properties, while a sufficient mechanical stability is rather challenging. The purpose of this work is to apply the gas flow assisted powder deposition introduced in 2014 by Zocca et al., to the powder bed during printing of bioceramic tablets and scaffolds using α-TCP powder as feedstock. This enables exploiting the advantages of an increased powder bed density, thereby improving the mechanical properties of the printed parts. KW - Additive Manufacturing KW - Binder Jetting KW - Gas flow assisted powder deposition KW - Alpha-tricalcium phosphate KW - Scaffold PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510138 DO - https://doi.org/10.1016/j.oceram.2020.100003 SN - 2666-5395 VL - 1 SP - 100003 PB - Elsevier Ltd. AN - OPUS4-51013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -