TY - JOUR A1 - Guerra, E. S. S. A1 - Silva, B. L. A1 - Melo, J. D. D. A1 - Kalinka, Gerhard A1 - Barbosa, A. P. C. T1 - Microscale evaluation of epoxy matrix composites containing thermoplastic healing agent N2 - Among the strategies to produce healable thermosetting systems is their modification by the addition of thermoplastic particles. This work investigates the influence of poly(ethylene-co-methacrylic acid) (EMAA) on fibermatrix interfacial properties of a glass fiber reinforced epoxy matrix composite. Epoxy-EMAA interactions were evaluated using differential scanning calorimetry (DSC) and infrared spectroscopy. The effects of EMAA on the epoxy network formation were evidenced by changes in glass transition temperature, cure kinetics and alteration of chemical groups during cure. Interfacial shear strength (IFSS) measurements obtained by single fiber pull-out tests indicate similar interfacial properties for pure and EMAA modified epoxy. Additionally, the potential for self-healing ability of an EMAA modified epoxy was demonstrated. However, IFSS after a healing cycle for the EMAA modified epoxy was lower as compared to the pure epoxy, because of the lower fiber-EMAA interfacial shear strength. So, thermoplastic healing agents has not only to fill cracks in the matrix material, but also have to be optimized regarding its interface properties to the reinforcing fibers. KW - Interfacial strength KW - Fiber/matrix bond KW - Self-healing KW - Polymer-matrix composites (PMC) PY - 2022 DO - https://doi.org/10.1016/j.compscitech.2022.109843 SN - 0266-3538 VL - 232 SP - 1 EP - 9 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-56379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Petrushin, N. V. A1 - Svetlov, I. L. A1 - Nolze, Gert T1 - Model for Forecasting Temperature Dependence of γ/γ' Misfit in Heat-Resistant Nickel Alloys N2 - An analytical model for forecasting the temperature dependence of γ/γ' misfit in heat-resistant nickel alloys is proposed. The model accounts for the concentration dependences of the periods of crystalline lattices of the γ and γ' phases (Vegard law), thermal expansion of the γ and γ' lattices, and dissolution of the γ' phase at high temperatures. Adequacy of calculations of misfit is confirmed by comparison with the results of measurements using methods of X-ray and neutron diffraction. The model is applied for development of a nickel alloy with positive misfit. KW - Heat-resistant nickel alloys KW - Dimensional mismatch of crystalline lattice periods (misfit) KW - Microstructure evolution PY - 2022 DO - https://doi.org/10.1134/S2075113322010105 SN - 2075-1133 VL - 13 IS - 1 SP - 7 EP - 16 PB - Springer AN - OPUS4-54379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thuy, Maximilian A1 - Pedragosa-Rincon, M. A1 - Niebergall, Ute A1 - Oehler, H. A1 - Alig, I. A1 - Böhning, Martin T1 - Environmental Stress Cracking of High-Density Polyethylene Applying Linear Elastic Fracture Mechanics N2 - The crack propagation rate of environmental stress cracking was studied on high-density polyethylene compact tension specimens under static loading. Selected environmental liquids are distilled water, 2 wt% aqueous Arkopal N100 solution, and two model liquid mixtures, one based on solvents and one on detergents, representing stress cracking test liquids for commercial crop protection products. The different surface tensions and solubilities, which affect the energetic facilitation of void nucleation and craze development, are studied. Crack growth in surface-active media is strongly accelerated as the solvents induce plasticization, followed by strong blunting significantly retarding both crack initiation and crack propagation. The crack propagation rate for static load as a function of the stress intensity factor within all environments is found to follow the Paris–Erdogan law. Scanning electron micrographs of the fracture surface highlight more pronounced structures with both extensive degrees of plasticization and reduced crack propagation rate, addressing the distinct creep behavior of fibrils. Additionally, the limitations of linear elastic fracture mechanisms for visco-elastic polymers exposed to environmental liquids are discussed. KW - Crack propagation KW - Environmental stress cracking KW - Fracture toughness KW - Crop protection products KW - High-density polyethylene KW - Craze–crack mechanism KW - Linear elastic fracture mechanics KW - Stress intensity factor PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550476 DO - https://doi.org/10.3390/polym14122415 SN - 2073-4360 VL - 14 IS - 12 SP - 1 EP - 21 PB - MDPI CY - Basel AN - OPUS4-55047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thuy, Maximilian A1 - Niebergall, Ute A1 - Oehler, H. A1 - Alig, I. A1 - Böhning, Martin T1 - Damaging effect of admixtures used in crop protection products on high density polyethylene packaging material N2 - The phenomenon of environmental stress cracking is still a major issue in materials engineering as well as from a scientific perspective. Especially in the case of packaging materials made of high-density polyethylene, assessing the potential of premature damage due to environmental stress cracking is complex because of the large number of components in possible liquid filling goods. As a first guideline, the well-known effect of detergents and dispersants is usually considered, but the interplay with other components, such as organic solvents is often unknown. Particularly challenging in this respect are crop protection products, consisting of several different admixtures in addition to the biologically active ingredients. This study is based on two model liquids representing these admixtures that were established for testing in this context. The model liquids as well as their constituting components were used as liquid media in the Full Notch Creep Test to characterize the environmental stress cracking behavior of a typical high-density polyethylene. Complementary to the time-to failure of a notched specimen obtained from these tests, the crack opening was monitored optically, and the fracture surface was analyzed post-failure by laser scanning microscopy as well as scanning electron microscopy. Based on the results, the effect of various surfactants as well as the influence of organic solvents on environmental stress cracking are discussed. KW - Environmental stress cracking KW - High-density polyethylene KW - Crop protection products KW - Full notch creep test KW - Fracture surface analysis KW - Crack opening displacement PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554631 DO - https://doi.org/10.1016/j.polymertesting.2022.107672 SN - 0142-9418 VL - 114 SP - 1 EP - 16 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-55463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sommer, Konstantin A1 - Agudo Jácome, Leonardo A1 - Hesse, René A1 - Bettge, Dirk T1 - Revealing the nature of melt pool boundaries in additively manufactured stainless steel by nano-sized modulation N2 - In the current study, the 3D nature of the melt pool boundaries (MPBs) in a 316 L austenitic steel additively manufactured by laser-based powder bed fusion (L-PBF) is investigated. The change of the cell growth direction and its relationship to the MPBs is investigated by transmission electron microscopy. A hitherto unreported modulated substructure with a periodicity of 21 nm is further discovered within the cell cores of the cellular substructure, which results from a partial transformation of the austenite, which is induced by a Ga+ focused ion beam. While the cell cores show the modulated substructure, cell boundaries do not. The diffraction pattern of the modulated substructure is exploited to show a thickness ≥200 nm for the MPB. At MPBs, the cell walls are suppressed, leading to continuously connecting cell cores across the MPB. This continuous MPB is described either as overlapping regions of cells of different growing directions when a new melt pool solidifies or as a narrow planar growth preceding the new melt pool. KW - Additive manufacturing KW - Austenitic steel 316L KW - Melt pool boundary KW - Microstructural characterization KW - Transmission electron microscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547295 DO - https://doi.org/10.1002/adem.202101699 SN - 1527-2648 VL - 24 IS - 6 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Inui, H. A1 - Kishida, K. A1 - Li, L. A1 - Manzoni, Anna Maria A1 - Haas, S. A1 - Glatzel, U. T1 - Uniaxial mechanical properties of face‑centered cubic singleand multiphase high‑entropy alloys N2 - Since the high entropy concept was proposed at the beginning of the millennium, the research focus of this alloy family has been wide ranging. The initial search for single-phase alloys has expanded with the aim of improving mechanical properties. This can be achieved by several strengthening mechanisms such as solid-solution hardening, hot and cold working and precipitation hardening. Both single- and multiphase high- and medium-entropy alloys can be optimized for mechanical strength via several processing routes, as is the case for conventional alloys with only one base element, such as steels or Ni-based superalloys. KW - High entropy alloy KW - Compositionally complex alloys KW - Tensile properties PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543955 DO - https://doi.org/10.1557/s43577-022-00280-y VL - 47 IS - 2 SP - 168 EP - 174 PB - Springer AN - OPUS4-54395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Sintering and foaming of bioactive glasses N2 - Sintering, crystallization, and foaming of 44.8SiO2–2.5P2O3–36.5CaO–6.6Na2O–6.6K2O–3.0CaF2 (F3) and 54.6SiO2–1.7P2O3–22.1CaO–6.0Na2O–7.9K2O–7.7MgO (13–93) bioactive glass powders milled in isopropanol and CO2 were studied via heating microscopy, differential thermal analysis, vacuum hot extraction (VHE), Infrared spectroscopy, and time-of-flight secondary ion mass spectrometry. Full densification was reached in any case and followed by significant foaming. VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750◦C, which hints on a thermally very stable species or mechanical trapping. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas. KW - Bioactive Glass KW - Crystallization KW - Foaming KW - Sintering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552454 DO - https://doi.org/10.1111/jace.18626 SN - 0002-7820 SP - 1 EP - 11 PB - Wiley online library AN - OPUS4-55245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne A1 - Müller, Ralf A1 - Deubener, J. T1 - Silver dissolution and precipitation in an Na2O–ZnO–B2O3 metallization paste glass N2 - Thermally stimulated interactions between silver and glass, that is, silver dissolution as Ag+ and precipitation as Ag0 were studied in two glass series of molar target composition xAg2O–(19 − x)Na2O–28ZnO–53B2O3 with x = 0, 0.1, 0.5, 5 and (19Na2O–28ZnO–53B2O3)+yAg2O with y = 0.01, 0.05. These act as model for low-melting borate glasses being part of metallization pastes. The occurrence of metallic silver precipitates in melt-quenched glass ingots demonstrated that silver dissolved only in traces (< 0.01 mol%) in the glasses. The dissolved silver was detected by means of Raman spectroscopy and energy-dispersive X-ray spectroscopy. Increasing x in the batch could not lead to a significant increase of the silver ion fraction in the glass as possible in binary silver borate glasses. In situ observation of heated AgNO3 mixed with the base glass frit in a hot stage microscope showed that Ag0 precipitation occurs already at the solid state. At higher temperatures, small droplets of liquid silver were found to move freely within the melt, whereas coalescence caused a stepwise increase of their size. These results contribute to the understanding of formation of silver precipitates in metallization pastes described in the literature. KW - Silver metallization paste KW - Batch reactions KW - Borate KW - Glass forming melts KW - Glass manufacturing KW - Raman spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559433 DO - https://doi.org/10.1111/ijag.16613 SN - 2041-1286 SP - 1 EP - 11 PB - Wiley Online Library AN - OPUS4-55943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manzoni, Anna Maria A1 - Mohring, Wencke A1 - Hesse, René A1 - Agudo Jácome, Leonardo A1 - Stephan-Scherb, C. T1 - Early material damage in equimolar CrMnFeCoNi in mixed oxidizing/sulfiding hot gas atmosphere N2 - The challenges to use more varied fuels at medium and high temperatures above 500 °C need to be addressed by tuning the materials toward a better resistance against increased corrosion. As a first step the corrosion processes need to be better understood, especially in the case of the unavoidable and highly corrosive sulfur-based gases. Herein, oxidation/sulfidation of an equimolar CrMnFeCoNi high-entropy alloy is studied at an early stage after hot gas exposure at 600 °C for 6 h in 0.5% SO2 and 99.5% Ar. The oxidation process is studied by means of X-ray diffraction, scanning and transmission electron microscopy, and supported by thermodynamic calculations. It is found that the sulfur does not enter the bulk material but interacts mainly with the fast-diffusing manganese at grain boundary triple junctions at the alloy surface. Submicrometer scaled Cr–S–O-rich phases close to the grain boundaries complete the sulfur-based phase formation. The grains are covered in different Fe-, Mn-, and Cr-based spinels and other oxides. KW - High entropy alloy KW - Sulfiding KW - Corrosion KW - Transmission electron microscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543495 DO - https://doi.org/10.1002/adem.202101573 SN - 1527-2648 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, F. A1 - Cheng, J. A1 - Liang, S. B. A1 - Ke, C. B. A1 - Cao, S. S. A1 - Zhang, X. P. A1 - Zizak, I. A1 - Manzoni, Anna Maria A1 - Yu, J. M. A1 - Wanderka, N. A1 - Li, W. T1 - Formation and evolution of hierarchical microstructures in a Ni-based superalloy investigated by in situ high-temperature synchrotron X-ray diffraction N2 - Hierarchical microstructures are created when additional γ particles form in γ’ precipitates and they are linked to improved strength and creep properties in high-temperature alloys. Here, we follow the formation and evolution of a hierarchical microstructure in Ni86.1Al8.5Ti5.4 by in situ synchrotron X-ray diffraction at 1023 K up to 48 h to derive the lattice parameters of the γ matrix, γ’ precipitates and γ particles and misfits between phases. Finite element method-based computer simulations of hierarchical microstructures allow obtaining each phase's lattice parameter, thereby aiding peak identification in the in situ X-ray diffraction data. The simulations further give insight into the heterogeneous strain distribution between γ’ precipitates and γ particles, which gives rise to an anisotropic diffusion potential that drives the directional growth of γ particles. We rationalize a schematic model for the growth of γ particles, based on the Gibbs-Thomson effect of capillary and strain-induced anisotropic diffusion potentials. Our results highlight the importance of elastic properties, elastic anisotropy, lattice parameters, and diffusion potentials in controlling the behavior and stability of hierarchical microstructures. KW - XRD KW - Superalloy KW - Finite element method KW - Transmission electron microscopy PY - 2022 DO - https://doi.org/10.1016/j.jallcom.2022.165845 SN - 0925-8388 VL - 919 SP - 1 EP - 17 PB - Elsevier CY - Lausanne AN - OPUS4-55394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kingsbery, Phillip A1 - Stephan-Scherb, Christiane T1 - Effect of KCl deposits in high‐temperature corrosion on chromium‐rich steels in SO2‐containing atmosphere N2 - High‐temperature corrosion was studied under multiple chemical loads on ferritic‐austenitic model alloys (Fe–13Cr, Fe–18Cr–12Ni, and Fe‐25Cr–20Ni) with KCl deposit under 0.5% SO2/99.5% Ar gas atmosphere at 560°C. Postexposure characterization was done by X‐ray diffraction and scanning electron microscopy. In a pure SO2/Ar environment a protective Cr2O3 scale was formed by all samples. The introduction of KCl deposits causes the scale to be nonprotective and multilayered, consisting of CrS, FeS, Cr2O3, Fe3O4, and Fe2O3. The impact of the microstructure and alloying elements is discussed. KW - High‐temperature corrosion KW - KCl KW - Microstructure KW - SO2 KW - Steel alloy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543056 DO - https://doi.org/10.1002/maco.202112901 VL - 73 IS - 5 SP - 758 EP - 770 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodrigues, A. C. P. A1 - Feller, A. A1 - Agudo Jácome, Leonardo A1 - Azevedo, C. R. F. T1 - Use of synthetic Fe3O4-rich tribofilms to investigate the effect of microconstituents, temperature and atmosphere on the friction coefficient during pin-on-disc tribotest N2 - This work investigates the effect of the tribotesting parameters (temperature, atmosphere, and third body chemical composition) on the coefficient of friction (CoF) during pin-on-disc dry (PoD) sliding tribotests using artificial third bodies. The third body comprised nanometric Fe3O4-based binary to quaternary chemical compositions containing copper, graphite, and zirconia. These mixtures were manually or ball-milled prepared, and pin-on-disc tribotests were conducted at 23 °C and 400 °C under air or nitrogen atmospheres. Combining PoD and artificial third body to create synthetic tribofilms might be useful for testing new formulations of Cu-free friction materials. Microstructural characterisation of the tribofilms was used to study the stability of the Fe3O4, copper, and graphite nanoparticles under different testing conditions to understand their effects on the CoF. For the Fe3O4-C-ZrO2-X systems, the ball milling mixing promoted the formation of turbostratic graphite in the tribofilm, impairing the lubricating effect of the graphite under air atmosphere at 23 °C. The formation of monoclinic CuO in the tribofilms during tribotests at 400 °C under air and N2 atmospheres promoted a lubricating effect. KW - Tribology KW - Microstructure KW - Oxide KW - Transmission electron microscopy PY - 2022 DO - https://doi.org/10.1088/2051-672X/ac9d51 SN - 2051-672X VL - 10 IS - 4 SP - 044009-1 EP - 044009-18 PB - IOP Pobilishing AN - OPUS4-56467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fantin, Andrea A1 - Cakir, Cafer Tufan A1 - Kasatikov, S. A1 - Schumacher, G. A1 - Manzoni, Anna Maria T1 - Effects of heat treatment on microstructure, hardness and local structure in a compositionally complex alloy N2 - Unlike conventional alloys, high entropy alloys are characterized by one or more solid solution phase(s) without a clearly defined solvent, all element contribute to the matrix in a way that is still not entirely understood. In addition, it is not known to what extent classic thermodynamic rules can be applied to these multi-element alloys, especially concerning the question about what factor incites the matrix to undergo a phase transformation. This work tackles directly some of these aspects on a chosen alloy, Al8Cr17Co17Cu8Fe17Ni33 (at.%), which presents a high temperature single-phase γ state and a two-phase state with γ′ precipitates, above and below 900 ◦C, respectively. A combined investigation via microstructural observations, hardness testing, X-ray absorption and photoelectron spectroscopy was carried out above the γ′ formation temperature. Hardness values are independent of the annealing temperatures, microstructural analysis shows no phase formation and X-ray absorption spectroscopy does not reveal observable changes in neither local atomic nor electronic structure, indicating that approaching γ′ formation temperature is not influenced by atomic or electronic rearrangements. Interestingly, short-range chemical order remains quantitatively compatible at any annealing temperature in the single-phase γ state, and the observed preferred pairs Al–Cu and Al–Ni in the γ state match with the γ’ precipitates composition below 900 ◦C. KW - High entropy alloys KW - EXAFS KW - Short range order KW - Vickers hardness PY - 2022 DO - https://doi.org/10.1016/j.matchemphys.2021.125432 SN - 0254-0584 VL - 276 SP - 125432 PB - Elsevier B.V. AN - OPUS4-53760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diener, S. A1 - Schubert, Hendrik A1 - Held, A. A1 - Katsikis, N. A1 - Günster, Jens A1 - Zocca, Andrea T1 - Influence of the dispersant on the parts quality in slurry-based binder jetting of SiC ceramics N2 - Binder jetting is establishing more and more in the ceramic industry to produce large complex shaped parts. A parameter with a great impact on the quality of the parts is the binder–powder interaction. The use of ceramic slurries as feedstock for this process, such as in the layerwise slurry deposition–print technology, allows a great flexibility in the composition. Such slurries are typically composed of ceramic powder, water, and small amounts of various additives. The understanding of the effect of these components on the printing quality is thus essential for the feedstock development. Four models were developed regarding the impact of additives, such as dispersants on printing. These models were confirmed or rebutted by experiments performed for an SiC slurry system with two different concentrations of a dispersant and a commercial phenolic resin used as a binder. It is shown that for this system the influence of the dispersant on the curing behavior and the clogging of the pores by dispersant can be neglected. The redispersion of the dispersant after the curing of the resin has no or only a minor effect. However, the wetting behavior determined by the surface energies of the system seem to be most crucial. In case the surface energy of the slurry additive is significantly lower than the surface energy of the binder, the strength of the green parts and the printing quality will be low. This was shown by inverse gas chromatography, contact angle measurement, rheological characterization, and mechanical tests with casted samples. KW - Additive Manufacturing KW - Binder Jetting KW - Layerwise slurry deposition KW - Silicon carbide KW - Wetting PY - 2022 DO - https://doi.org/10.1111/jace.18693 SN - 1551-2916 VL - 2022 SP - 1 EP - 15 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-55542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bender, R. A1 - Féron, D. A1 - Mills, D. A1 - Ritter, S. A1 - Bäßler, Ralph A1 - Bettge, Dirk A1 - de Graeve, I. A1 - Dugstad, A. A1 - Grassini, S. A1 - Hack, T. A1 - Halama, M. A1 - Han, E.-H. A1 - Harder, T. A1 - Hinds, G. A1 - Kittel, J. A1 - Krieg, R. A1 - Leygraf, C. A1 - Martinelli, L. A1 - Mol, A. A1 - Neff, D. A1 - Nilsson, J.-O. A1 - Odnevall, I. A1 - Paterson, S. A1 - Paul, S. A1 - Prošek, T. A1 - Raupach, M. A1 - Revilla, R. I. A1 - Ropital, F. A1 - Schweigart, H. A1 - Szala, E. A1 - Terryn, H. A1 - Tidblad, J. A1 - Virtanen, S. A1 - Volovitch, P. A1 - Watkinson, D. A1 - Wilms, M. A1 - Winning, G. A1 - Zheludkevich, M. T1 - Corrosion challenges towards a sustainable society N2 - A global transition towards more sustainable, affordable and reliable energy systems is being stimulated by the Paris Agreement and the United Nation's 2030 Agenda for Sustainable Development. This poses a challenge for the corrosion industry, as building climate‐resilient energy systems and infrastructures brings with it a long‐term direction, so as a result the long‐term behaviour of structural materials (mainly metals and alloys) becomes a major prospect. With this in mind “Corrosion Challenges Towards a Sustainable Society” presents a series of cases showing the importance of corrosion protection of metals and alloys in the development of energy production to further understand the science of corrosion, and bring the need for research and the consequences of corrosion into public and political focus. This includes emphasis on the limitation of greenhouse gas emissions, on the lifetime of infrastructures, implants, cultural heritage artefacts, and a variety of other topics. KW - Corrosion KW - Corrosion costs KW - Corrosion protection KW - Preventive strategies PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554801 DO - https://doi.org/10.1002/maco.202213140 SN - 1521-4176 VL - 73 IS - 11 SP - 1730 EP - 1751 PB - Wiley-VCH CY - Weinheim AN - OPUS4-55480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cestari, F. A1 - Yang, Y. A1 - Wilbig, Janka A1 - Günster, Jens A1 - Motta, A. A1 - Sglavo, V. T1 - Powder 3D printing of bone scaffolds with uniform and gradient pore sizes using cuttlebone-derived calcium phosphate and glass-ceramic N2 - The pore geometry of bone scaffolds has a major impact on their cellular response; for this reason, 3D printing is an attractive technology for bone tissue engineering, as it allows for the full control and design of the porosity. Calcium phosphate materials synthesized from natural sources have recently attracted a certain interest because of their similarity to natural bone, and they were found to show better bioactivity than synthetic compounds. Nevertheless, these materials are very challenging to be processed by 3D printing due to technological issues related to their nanometric size. In this work, bone scaffolds with different pore geometries, with a uniform size or with a size gradient, were fabricated by binder jetting 3D printing using a biphasic calcium phosphate (BCP) nanopowder derived from cuttlebones. To do so, the nanopowder was mixed with a glass-ceramic powder with a larger particle size (45–100 µm) in 1:10 weight proportions. Pure AP40mod scaffolds were also printed. The sintered scaffolds were shown to be composed mainly by hydroxyapatite (HA) and wollastonite, with the amount of HA being larger when the nanopowder was added because BCP transforms into HA during sintering at 1150 ◦C. The addition of bio-derived powder increases the porosity from 60% to 70%, with this indicating that the nanoparticles slow down the glass-ceramic densification. Human mesenchymal stem cells were seeded on the scaffolds to test the bioactivity in vitro. The cells’ number and metabolic activity were analyzed after 3, 5 and 10 days of culturing. The cellular behavior was found to be very similar for samples with different pore geometries and compositions. However, while the cell number was constantly increasing, the metabolic activity on the scaffolds with gradient pores and cuttlebone-derived powder decreased over time, which might be a sign of cell differentiation. Generally, all scaffolds promoted fast cell adhesion and proliferation, which were found to penetrate and colonize the 3D porous structure. KW - Bioactivity KW - Cuttlefish KW - Biphasic calcium phosphate KW - Binder jetting KW - Scaffold geometry KW - Hausner ratio PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553627 DO - https://doi.org/10.3390/ma15155139 SN - 1996-1944 VL - 15 IS - 15 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-55362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rizzardi, Q. A1 - McElfresh, C. A1 - Sparks, G. A1 - Stauffer, D. A1 - Marian, J. A1 - Maaß, Robert T1 - Mild-to-wild plastic transition is governed by athermal screw dislocation slip in bcc Nb N2 - Plastic deformation in crystals is mediated by the motion of line defects known as dislocations. For decades, dislocation activity has been treated as a homogeneous, smooth continuous process. However, it is now recognized that plasticity can be determined by longrange correlated and intermittent collective dislocation processes, known as avalanches. Here we demonstrate in body-centered cubic Nb how the long-range and scale-free dynamics at room temperature are progressively quenched out with decreasing temperature, eventually revealing intermittency with a characteristic length scale that approaches the Burgers Vector itself. Plasticity is shown to be bimodal across the studied temperature regime, with conventional thermally-activated smooth plastic flow (‘mild’) coexisting with sporadic Bursts (‘wild’) controlled by athermal screw dislocation activity, thereby violating the classical Notion of temperature-dependent screw dislocation motion at low temperatures. An abrupt increase of the athermal avalanche component is identified at the critical temperature of the material. Our results indicate that plasticity at any scale can be understood in terms of the coexistence of these mild and wild modes of deformation, which could help design better alloys by suppressing one of the two modes in desired temperature Windows. KW - Plastic deformation KW - Microplastic stress KW - Intermittent microplasticity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543927 DO - https://doi.org/10.1038/s41467-022-28477-4 VL - 13 IS - 1 SP - 1 EP - 9 PB - Nature AN - OPUS4-54392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Maaß, Robert A1 - Deubener, J. A1 - Müller, Ralf T1 - Internal nucleation tendency and crystal surface energy obtained from bond energies and crystal lattice data N2 - We present an easy-to-apply method to predict structural trends in the internal nucleation tendency of oxide glasses. The approach is based on calculated crystal fracture surface energies derived from easily accessible diatomic bond energy and crystal lattice data. The applicability of the method is demonstrated on literature nucleation data for isochemically crystallizing oxide glasses. KW - Glass KW - Nucleation tendency KW - Fracture surface energy KW - Crystal lattice KW - Bond energy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548814 DO - https://doi.org/10.1016/j.nocx.2022.100093 SN - 2590-1591 VL - 14 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-54881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Lehmusto, Juho A1 - Falk, Florian A1 - Sobol, Oded A1 - Pint, Bruce T1 - Comprehensive insights into competitive oxidation/sulfidation reactions on binary ferritic alloys at high temperatures N2 - Interpreting high-temperature corrosion induced by mixed-gas atmospheres is challenging due to the different contributions of oxidizing gases. Here, a comprehensive study on the combined oxidation/sulfidation using label molecules is presented. Fe-Cr model alloys with 2 wt% and 9 wt% Cr were isothermally exposed using a volumetric mixture of 0.5%S16O2/27%H218O and 0.5%S16O2/7%H218O at 650 ◦C for 5 h and then characterized by secondary ion mass spectroscopy (SIMS). Additionally, the reactions were followed in-situ utilizing energy dispersive X-ray diffraction. The study showed that both S16O2 and H218O contribute to the oxidation of the alloys but to different extents depending on the Cr-content. KW - SEM KW - Steel KW - Iron KW - SIMS PY - 2022 DO - https://doi.org/10.1016/j.corsci.2022.110236 SN - 0010-938X VL - 203 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-58992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Rhode, Michael A1 - Boerner, Andreas A1 - Saliwan Neumann, Romeo A1 - Schneider, M. A1 - Laplanche, G. T1 - Influence of machining on the surface integrity of high- and medium-entropy alloys N2 - High- and medium-entropy alloys (HEAs) are a quite new class of materials. They have a high potential for applications from low to high temperatures due to the excellent combination of their structural properties. Concerning their application as components; processing properties, such as machinability, have hardly been investigated so far. Hence, machinability analyses with a focus on the influence of the milling process and its basic parameters (cutting speed, feed per cutting edge) on the resulting surface integrity of specimens from an equiatomic high- (CoCrFeMnNi) and a medium- (CoCrNi) entropy alloy have been carried out. A highly innovative milling process with ultrasonic assistance (USAM) was compared to conventional milling processes. Recent studies have shown that USAM has a high potential to significantly reduce the mechanical load on the tool and workpiece surface during milling. In this study, the basic machining and ultrasonic parameters were systematically varied. After machining, the surface integrity of the alloys was analyzed in terms of topography, defects, subsurface damage, and residual stresses. It was observed that USAM reduces the cutting forces and increases the surface integrity in terms of lower tensile residual stresses and defect density near the surfaces for the CoCrFeMnNi alloy. It was shown that the cutting forces and the metallurgical influence in the sub surface region are reduced by increasing the cutting speed and reducing the feed rate per cutting edge. With the CoCrNi alloy, the tool revealed severe wear. As a result, for this alloy no influence of the parameters on the machinability could be determined. KW - High Entropy Alloy KW - Medium Entropy Alloys KW - Ultrasonic assited machining PY - 2022 DO - https://doi.org/10.1016/j.matchemphys.2021.125271 SN - 0254-0584 VL - 275 SP - 125271 PB - Elsevier B.V. AN - OPUS4-53606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darvishi Kamachali, Reza A1 - Wang, L. T1 - Elastic energy of multi-component solid solutions and strain origins of phase stability in high-entropy alloys N2 - The elastic energy of mixing for multi-component solid solutions is derived by generalizing Eshelby's sphere-in-hole model. By surveying the dependence of the elastic energy on the chemical composition and lattice misfit, we derive a lattice strain coefficient λ*. Studying several high-entropy alloys and superalloys, we propose that most solid solution multi-component alloys are stable when λ*<0.16, generalizing the Hume-Rothery atomic-size rule for binary alloys. We also reveal that the polydispersity index δ, frequently used for describing strain in multi-component alloys, directly represents the elastic energy e with e=qδ², q being an elastic constant. Furthermore, the effects of (i) the number and (ii) the atomic-size distribution of constituting elements on the phase stability of high-entropy alloys were quantified. The present derivations and discussions open for richer considerations of elastic effects in high-entropy alloys, offering immediate support for quantitative assessments of their thermodynamic properties and studying related strengthening mechanisms. KW - Ordering KW - High-entropy alloys KW - Alloy design KW - Strain energy KW - Phase stability PY - 2022 DO - https://doi.org/10.1016/j.scriptamat.2021.114226 SN - 1359-6462 VL - 206 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-53427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rizzardi, Q. A1 - Derlet, P. M. A1 - Maaß, Robert T1 - Intermittent microplasticity in the presence of a complex microstructure N2 - We demonstrate the gradual shift from scale-free intermittent microplasticity to a scale-dependent behavior via the introduction of a variety of microstructural features within the Al-Cu binary alloy system. As long as the obstacles to dislocation motion remain shearable, the statistics of intermittent microplasticity has fat-tailed contributions. The introduction of incoherent precipitates leads to a complete transition from scale-free powerlaw scaling to an exponential and scale-dependent distribution. These results demonstrate how non-Gaussian interactions survive across different microstructures and further suggest that characteristic microstructural length scales and obstacle pinning-strengths are of secondary importance for the intermittency statistics, as long as dislocations can shear their local environment. KW - Scale-dependent behavior KW - Al-Cu binary alloy system PY - 2022 DO - https://doi.org/10.1103/PhysRevMaterials.6.073602 SN - 2475-9953 VL - 6 IS - 7 SP - 1 EP - 9 PB - American Physical Society AN - OPUS4-55387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wallis, Theophilus A1 - Darvishi Kamachali, Reza T1 - Grain boundary structural variations amplify segregation transition and stabilize co-existing spinodal interfacial phases N2 - Grain boundaries (GBs)’s role in determining the functional and mechanical properties of polycrystalline materials is inscribed in both their structure and chemistry. Upon solute segregation, the structure and composition of a GB can change concurrently. We study the co-evolution of GB’s structure and segregation by enhancing the density-based phase-field model to account for the in-plane structural variations in the GB. Significant mutual coupling is revealed between the GB’s chemical and structural states during Mn segregation in Fe-Mn alloys. We found that the structural degrees of freedom in a GB (the ability of the GB structure to respond to the chemical variation) amplifies Mn segregation transition, even when the GB structure stays unchanged. When the GB structure is not uniform, that is the usual case, the coupling between GB structure and segregation evolution also enables the spinodally formed low- and high-Mn phases (upon segregation transition) to co-exist within the GB region. These findings explain the stabilizing mechanism of pronounced interfacial segregation fluctuations, experimentally evidenced in Fe-Mn GBs, and give new insights on the structural sensitivity of GBs’ segregation phenomena and the mutual chemo-structural interplay. KW - Grain boundary engineering KW - Segregation engineering KW - Grain boundary structure KW - Fe-Mn steels PY - 2022 DO - https://doi.org/10.1016/j.actamat.2022.118446 SN - 1359-6454 VL - 242 PB - Elsevier Ltd. AN - OPUS4-56160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maximilian, Thuy A1 - Spyrantis, Alexander A1 - Böhning, Martin A1 - Niebergall, Ute A1 - Maaß, Robert T1 - Spatially resolved roughness exponent in polymer fracture N2 - The fracture surface of slow and continuous crack propagation during environmental stress cracking of a semicrystalline polyethylene exhibits isotropic roughness exponents at the local scale but resolved across the macroscopic fracture surface a clear position dependence is found. The spatially resolved roughness exponent admits values in the range between 0.1 and 0.4, demonstrating nontrivial exponents in the small length-scale regime. Instead, they vary across the fracture surface according to the stress-state distribution, which suggests that the exponents are intimately linked to the locally dominating dissipation processes during craze cracking. KW - Plasticity KW - Fracture KW - Material failure KW - Mechanical deformation PY - 2022 DO - https://doi.org/10.1103/PhysRevMaterials.6.L090601 VL - 6 IS - 9 SP - 1 EP - 7 PB - American Physical Society CY - USA, Maryland AN - OPUS4-55797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shimada, Y. A1 - Ikeda, Yuki A1 - Yoshida, K. A1 - Sato, M. A1 - Chen, J. A1 - Du, Y. A1 - Inoue, K. A1 - Maaß, Robert A1 - Nagai, Y. A1 - Konno, T. T1 - In situ thermal annealing transmission electron microscopy of irradiation induced Fe nanoparticle precipitation in Fe–Si alloy N2 - The typical experimental conditions inside a transmission electron microscope (TEM), such as ultra-high vacuum, high-energy electron irradiation, and surface effects of ultrathin TEM specimens, can be the origin of unexpected microstructural changes compared with that of bulk material during in situ thermal-annealing experiments. In this paper, we report on the microstructural changes of a Fe–15%Si alloy during in situ TEM annealing, where, in its bulk form, it exhibits an ordering transformation from D03 to B2 at 650 °C. Using a heating-pot type double tilt holder with a proportional–integral–differential control system, we observed the precipitation of α-Fe both at the sample surface and inside the sample. Surface precipitates formed via surface diffusion are markedly large, several tens of nm, whereas precipitates inside the specimen, which are surrounded by Fe-poor regions, reach a maximum size of 20 nm. This unexpected microstructural evolution could be attributed to vacancies on Si sites, which are induced due to high-energy electron irradiation before heating, as well as enhanced thermal diffusion of Fe atoms. KW - In situ thermal-annealing experiment KW - Microstructural changes of a Fe Si alloy KW - Microstructural evolution PY - 2022 DO - https://doi.org/10.1063/5.0070471 SN - 0021-8979 VL - 131 IS - 16 SP - 1 EP - 8 PB - AIP Publishing AN - OPUS4-54728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maaß, Robert T1 - The Federal Institute of Materials Research and Testing (BAM) – 150 Years of Enabling Scientific and Technological Breakthrough N2 - BAM! This issue of Advanced Engineering Materials celebrates 150 years of scientific and technical research at the interface between academia, industry and politics. Rooted in 1871 at the birth of the German Empire and at that time located in simple basements and barracks, the institutional development began around mechanical metallurgy of iron and steel and represents today a diverse portfolio of fore-front research that orients itself along tomorrow's societal challenges and long-term research horizons. KW - 150 Years KW - Adolf Martens PY - 2022 DO - https://doi.org/10.1002/adem.202200648 VL - 24 IS - 6 SP - 1 EP - 3 PB - Wiley-VCH GmbH AN - OPUS4-55388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Derlet, P. M. A1 - Maaß, Robert T1 - Optimally rejuvenated model binary glasses N2 - Using the creation relaxation algorithm developed for the atomistic modeling of the high-dose irradiation limit of crystalline systems, we explore the limits of the structural rejuvenation of a highly excited model binary glass. This high-energy athermal amorphous structure exhibits a direct transition to homogeneous plastic flow and a microstructure that is largely insensitive to this flow, being characterized by a porous system-spanning network of minimally frustrated structural motifs. The observed homogeneous plasticity is mediated by the same string-like structural excitations, which mediate structural relaxation and microplasticity at finite temperature in more relaxed structures. This highly rejuvenated structural asymptote is not far from the structural state of regions, which have experienced athermal shear localization in more relaxed samples, suggesting an optimally rejuvenated glassy structure will always be limited by that produced by shear localization. KW - Metallic glasses KW - Creation-relaxation algorithm KW - Shear PY - 2022 DO - https://doi.org/10.1103/PhysRevMaterials.6.125604 VL - 6 IS - 12 SP - 1 EP - 13 PB - American Physical Society AN - OPUS4-56741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sänger, Johanna Christiane A1 - Pauw, Brian Richard A1 - Riechers, Birte A1 - Zocca, Andrea A1 - Rosalie, Julian A1 - Maaß, Robert A1 - Sturm, Heinz A1 - Günster, Jens T1 - Entering a new dimension in powder processing for advanced ceramics shaping N2 - Filigree structures can be manufactured via two-photon-polymerization (2PP) operating in the regime of non-linear light absorption. For the first time it is possible to apply this technique to the powder processing of ceramic structures with a feature size in the range of the critical defect size responsible for brittle fracture and, thus, affecting fracture toughness of high-performance ceramics. In this way, tailoring of advanced properties can be achieved already in the shaping process. Traditionally, 2PP relies on transparent polymerizable resins, which is diametrically opposed to the usually completely opaque ceramic resins and slurries. Here we present a transparent and photocurable suspension of nanoparticles (resin) with very high mass fractions of yttria-stabilized zirconia particles (YSZ). Due to the extremely well dispersed nanoparticles, scattering of light can be effectively suppressed at the process-relevant wavelength of 800 nm. Sintered ceramic structures with a resolution of down to 500 nm were obtained. Even at reduced densities of 1 to 4 g/cm³, the resulting compressive strength with 4,5 GPa is equivalent or even exceeding bulk monolithic yttria stabilized zirconia. A ceramic metamaterial is born, where the mechanical properties of yttria stabilized zirconia are altered by changing geometrical parameters and gives access to a new class of ceramic materials. KW - Two-photon-polymerization KW - Ceramics KW - Powder processing KW - Transparency KW - Meta material KW - Yttria stabilized zirconia PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564598 DO - https://doi.org/10.1002/adma.202208653 SN - 1521-4095 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Evans, Alexander A1 - Polatidis, E. A1 - Čapek, J. A1 - Mohr, Gunther A1 - Serrano-Munoz, Itziar A1 - Bruno, Giovanni T1 - Understanding the impact of texture on the micromechanical anisotropy of laser powder bed fused Inconel 718 N2 - The manufacturability of metallic alloys using laser-based additive manufacturing methods such as laser powder bed fusion has substantially improved within the last decade. However, local melting and solidification cause hierarchically structured and crystallographically textured microstructures possessing large residual stress. Such microstructures are not only the origin of mechanical anisotropy but also pose metrological challenges for the diffraction-based residual stress determination. Here we demonstrate the influence of the build orientation and the texture on the microstructure and consequently the mechanical anisotropy of as-built Inconel 718. For this purpose, we manufactured specimens with [001]/[011]-, [001]- and [011]/[111]-type textures along their loading direction. In addition to changes in the Young’s moduli, the differences in the crystallographic textures result in variations of the yield and ultimate tensile strengths. With this in mind, we studied the anisotropy on the micromechanical scale by subjecting the specimens to tensile loads along the different texture directions during in situ neutron diffraction experiments. In this context, the response of multiple lattice planes up to a tensile strain of 10% displayed differences in the load partitioning and the residual strain accumulation for the specimen with [011]/[111]-type texture. However, the relative behavior of the specimens possessing an [001]/[011]- and [001]-type texture remained qualitatively similar. The consequences on the metrology of residual stress determination methods are discussed. KW - Laser powder bed fusion KW - Additive manufacturing KW - Electron backscatter diffraction KW - Tensile testing KW - Diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555840 DO - https://doi.org/10.1007/s10853-022-07499-9 SN - 1573-4803 VL - 2022 IS - 57 SP - 15036 EP - 15058 PB - Springer Science + Business Media B.V. CY - Dordrecht AN - OPUS4-55584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ávila Calderón, Luis A1 - Rehmer, Birgit A1 - Schriever, Sina A1 - Ulbricht, Alexander A1 - Agudo Jácome, Leonardo A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Skrotzki, Birgit A1 - Evans, Alexander T1 - Creep and creep damage behavior of stainless steel 316L manufactured by laser powder bed fusion N2 - This study presents a thorough characterization of the creep properties of austenitic stainless steel 316L produced by laser powder bed fusion (LPBF 316L) contributing to the sparse available data to date. Experimental results (mechanical tests, microscopy, X-ray computed tomography) concerning the creep deformation and damage mechanisms are presented and discussed. The tested LPBF material exhibits a low defect population, which allows for the isolation and improved understanding of the effect of other typical aspects of an LPBF microstructure on the creep behavior. As a benchmark to assess the material properties of the LPBF 316L, a conventionally manufactured variant of 316L was also tested. To characterize the creep properties, hot tensile tests and constant force creep tests at 600 °C and 650 °C are performed. The creep stress exponents of the LPBF material are smaller than that of the conventional variant. The primary and secondary creep stages and the times to rupture of the LPBF material are shorter than the hot rolled 316L. Overall the creep damage is more extensive in the LPBF material. The creep damage of the LPBF material is overall mainly intergranular. It is presumably caused and accelerated by both the appearance of precipitates at the grain boundaries and the unfavorable orientation of the grain boundaries. Neither the melt pool boundaries nor entrapped gas pores show a significant influence on the creep damage mechanism. KW - 316L KW - Laser Powder Bed Fusion (LPBF) KW - Creep behavior KW - Additive Manufacturing KW - AGIL PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539373 DO - https://doi.org/10.1016/j.msea.2021.142223 SN - 0921-5093 VL - 830 SP - 142223 PB - Elsevier B.V. AN - OPUS4-53937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Yue A1 - Schilling, Markus A1 - von Hartrott, P. A1 - Beygi Nasrabadi, Hossein A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Ontopanel: A Tool for Domain Experts Facilitating Visual Ontology Development and Mapping for FAIR Data Sharing in Materials Testing N2 - In recent years, the design and development of materials are strongly interconnected with the development of digital technologies. In this respect, efficient data management is the building block of material digitization and, in the field of materials science and engineering (MSE), effective solutions for data standardization and sharing of different digital resources are needed. Therefore, ontologies are applied that represent a map of MSE concepts and relationships between them. Among different ontology development approaches, graphical editing based on standard conceptual modeling languages is increasingly used due to its intuitiveness and simplicity. This approach is also adopted by the Materials-open-Laboratory project (Mat-o-Lab), which aims to develop domain ontologies and method graphs in accordance with testing standards in the field of MSE. To suit the actual demands of domain experts in the project, Ontopanel was created as a plugin for the popular open-source graphical editor diagrams.net to enable graphical ontology editing. It includes a set of pipeline tools to foster ontology development in diagrams.net, comprising imports and reusage of ontologies, converting diagrams to Web Ontology Language (OWL), verifying diagrams using OWL rules, and mapping data. It reduces learning costs by eliminating the need for domain experts to switch between various tools. Brinell hardness testing is chosen in this study as a use case to demonstrate the utilization of Ontopanel. KW - Materials Testing KW - Ontology KW - Visual ontology development KW - Data mapping KW - FAIR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560339 DO - https://doi.org/10.1007/s40192-022-00279-y SP - 1 EP - 12 PB - Springer AN - OPUS4-56033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ávila Calderón, Luis A1 - Graf, B. A1 - Rehmer, Birgit A1 - Petrat, T. A1 - Skrotzki, Birgit A1 - Rethmeier, Michael T1 - Characterization of Ti-6Al-4V fabricated by multilayer laser powder-based directed energy deposition N2 - Laser powder-based directed energy deposition (DED-L) is increasingly being used in additive manufacturing (AM). As AM technology, DED-L must consider specific challenges. It must achieve uniform volume growth over hundreds of layers and avoid heat buildup of the deposited material. Herein, Ti–6Al–4V is fabricated using an approach that addresses these challenges and is relevant in terms of transferability to DED–L applications in AM. The assessment of the obtained properties and the discussion of their relationship to the process conditions and resulting microstructure are presented. The quality of the manufacturing process is proven in terms of the reproducibility of properties between individual blanks and with respect to the building height. The characterization demonstrates that excellent mechanical properties are achieved at room temperature and at 400 °C. KW - AGIL KW - Laser powder-based directed energy deposition KW - Tensile properties KW - Ti-6Al-4V KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542262 DO - https://doi.org/10.1002/adem.202101333 SN - 1438-1656 SN - 1527-2648 SP - 1 EP - 15 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Hanke, T. A1 - Muth, Thilo A1 - Riedel, Jens A1 - Schilling, Markus A1 - Schweizer, C. A1 - Skrotzki, Birgit A1 - Todor, A. A1 - Moreno Torres, Benjami A1 - Unger, Jörg F. A1 - Völker, Christoph A1 - Olbricht, Jürgen T1 - A Perspective on Digital Knowledge Representation in Materials Science and Engineering N2 - The amount of data generated worldwide is constantly increasing. These data come from a wide variety of sources and systems, are processed differently, have a multitude of formats, and are stored in an untraceable and unstructured manner, predominantly in natural language in data silos. This problem can be equally applied to the heterogeneous research data from materials science and engineering. In this domain, ways and solutions are increasingly being generated to smartly link material data together with their contextual information in a uniform and well-structured manner on platforms, thus making them discoverable, retrievable, and reusable for research and industry. Ontologies play a key role in this context. They enable the sustainable representation of expert knowledge and the semantically structured filling of databases with computer-processable data triples. In this perspective article, we present the project initiative Materials-open-Laboratory (Mat-o-Lab) that aims to provide a collaborative environment for domain experts to digitize their research results and processes and make them fit for data-driven materials research and development. The overarching challenge is to generate connection points to further link data from other domains to harness the promised potential of big materials data and harvest new knowledge. KW - Data infrastructures KW - Digital representations KW - Digital workflows KW - Knowledge graphs KW - Materials informatics KW - Ontologies KW - Vocabulary providers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546729 DO - https://doi.org/10.1002/adem.202101176 SN - 1438-1656 SP - 1 EP - 14 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-54672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, R. A1 - Rabe, Torsten T1 - Lowering the sintering temperature of calcium manganate for thermoelectric applications N2 - This study combines three different approaches to lower the sintering temperature of Sm-doped CaMnO3 to save energy in production and facilitate co-firing with other low-firing oxides or metallization. The surface energy of the powder was increased by fine milling, sintering kinetics were enhanced by additives, and uniaxial pressure during sintering was applied. The shrinkage, density, microstructure, and thermoelectric properties were evaluated. Compared to micro-sized powder, the use of finely ground powder allows us to lower the sintering temperature by 150 K without reduction of the power factor. By screening the effect of various common additives on linear shrinkage of CaMnO3 after sintering at 1100 ○C for 2 h, CuO is identified as the most effective additive. Densification at sintering temperatures below 1000 ○C can be significantly increased by pressure-assisted sintering. The power factor at room temperature of CaMnO3 nano-powder sintered at 1250 ○C was 445 μW/(m K2). Sintering at 1100 ○C reduced the power factor to 130 μW/(m K2) for CaMnO3 nano-powder, while addition of 4 wt.% CuO to the same powder led to ∼290 μW/(m K2). The combination of fine milling, CuO addition, and pressureassisted sintering at 950 ○C resulted in a power factor of ∼130 μW/(m K2). These results show that nano-sized powder and CuO addition are successful and recommendable strategies to produce CaMnO3 with competitive properties at significantly reduced temperatures and dwell times. KW - Sintering additive KW - Liquid phase sintering KW - Pressure assisted sintering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555467 DO - https://doi.org/10.1063/5.0098015 SN - 2158-3226 VL - 12 IS - 8 SP - 1 EP - 9 PB - American Institute of Physics (AIP) CY - New York, NY AN - OPUS4-55546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - Lopez-Galilea, I. A1 - Darvishi Kamachali, Reza A1 - Roik, J. A1 - Agudo Jácome, Leonardo T1 - The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: Experimental findings and comparison with calculations using the CALPHAD method N2 - Detailed microstructural characterization of the AlMo0.5NbTa0.5TiZr refractory high entropy superalloy in the as-cast state is reported for first time and compared with the state annealed at 1400 oC for 24 h. The former shows a dendritic structure, with a mixture of A2/B2 phases < 20 nm in both the dendritic and interdendritic regions. A mostly amorphous phase, rich in Al and Zr, is found within the interdendritic region. The annealed state reproduced the combination of A2/B2/Al-Zr-rich phases reported previously. Calculations from two relevant ThermoCalc databases were compared with the experimental results. Equilibrium calculations were compared with results for the annealed alloy, whereas solidification paths calculated using Scheil-Gulliver model were used for comparison with the as-cast alloy. A previously hypothesized spinodal decomposition during cooling as the mechanism responsible for the patterned A2/B2 microstructure is confirmed via the CALPHAD calculations, pointing to its use as an efficient design tool for such alloys. Finally, the comparison between the experimental and computational findings allowed better understanding the solidification path and equilibrium stability of this alloy, giving a base to make better decisions on the field of new refractory superalloy design. KW - CALPHAD database analysis KW - Refractory superalloys KW - Chemically complex alloy KW - Characterization KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545906 DO - https://doi.org/10.1016/j.matdes.2022.110593 SN - 1873-4197 VL - 217 SP - 1 EP - 13 PB - Elsevier CY - Amsterdam AN - OPUS4-54590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xing, H. A1 - Jing, H. A1 - Dong, X. A1 - Wang, Lei A1 - Han, Y. A1 - Hu, R. T1 - Cellular growth during rapid directional solidification: Insights from quantitative phase field simulations N2 - In this paper, columnar cellular growth with kinetic effects including kinetic undercooling and solute trapping in rapid directional solidification of alloys was investigated by using a recent quantitative phase-field model for rapid solidification. Morphological transition and primary spacing selection with and without kinetic effects were numerically investigated. Numerical results show that doublon structure is an intermediate state in the primary spacing adjustment of cellular arrays. It was found that the inclusions of kinetic effects result in the increase of the solute in the solid phase and the solute enrichment in the interdendritic liquid channel. Moreover, predicted results indicate that the growth directions of the cellular arrays in rapid directional solidification with and without kinetic effects are independent of the Péclet number. Therefore, the kinetic effects play important roles in numerical simulations of the growth pattern selection and solute distribution during rapid solidification. Neglecting them will result in the inaccurately predicted results. KW - Rapid solidification KW - Phase-field model PY - 2022 DO - https://doi.org/10.1016/j.mtcomm.2022.103170 VL - 30 SP - 103170 PB - Elsevier Ltd. AN - OPUS4-54571 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruffini, A. A1 - Le Bouar, Y. A1 - Finel, A. A1 - Epishin, A. I. A1 - Fedelich, Bernard A1 - Feldmann, Titus A1 - Viguier, B. A1 - Poquillon, D. T1 - Dislocations interacting with a pore in an elastically anisotropic single crystal nickel-base superalloy during hot isostatic pressing N2 - The formation of pores in CMSX-4 nickel based superalloys is detrimental to the service life of the material. A way to avoid the problem is to treat the superalloys under Hot Isostatic Pressing (HIP), which enables a large volume fraction of pores to be annihilated. This paper aims to understand the contribution of plastic activity related to the gliding of dislocations on the pore annihilation. Simulations based on a phase-field model of dislocation are performed and make it possible to consider the strong anisotropy of the CMSX-4 under HIP conditions in conjunction to the strong elastic heterogeneity introduced by the pore. For pores with a radius of few micrometers, it is shown that edge parts of dislocation lines that present an extra half atomic plane oriented towards the pore are stacked above and under it in the direction which is perpendicular to their slip-planes, causing an increase of the number of dislocation along the four octahedral directions of the FCC single crystal which intersect the pore center. Results are streamlined within the isotropic elastic theory of dislocations. Effects of elastic anisotropy and dislocation reactions are also investigated in order to specify what would be the dislocation configuration around a pore in CMSX-4 under HIP conditions. Notably, the elastic anisotropy is shown to significantly modify the arrangement of dislocations close to the pore equator. Simulations also allow for the characterization of pore/dislocation interactions when dislocations are involved in Low Angle Boundaries as experimentally observed. KW - HIP KW - Superalloys KW - Dislocation KW - Pore KW - Phase-field PY - 2022 DO - https://doi.org/10.1016/j.commatsci.2021.111118 SN - 0927-0256 VL - 204 SP - 1 EP - 14 PB - Elsevier CY - Amsterdam AN - OPUS4-54220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mosquera Feijoo, Maria A1 - Oder, Gabriele A1 - Saliwan Neumann, Romeo A1 - Buchheim, Michaela A1 - Kranzmann, Axel A1 - Olbricht, Jürgen T1 - Impact of Sample Geometry and Surface Finish on VM12‑SHC Ferritic–Martensitic Steel Under Cyclic Steam Atmosphere Operating Conditions N2 - The steam side oxidation of ferritic–martensitic VM12-SHC steel was investigated under thermo-cyclic conditions in water steam at 620/320 °C and 30 bar with a focus on assessing the influence of pre-oxidation time, specimen geometry and surface finish. The specimens were pre-oxidized under isothermal conditions in water steam at 620 °C and 30 bar for 500 h or 1500 h. After pre-oxidation treatment, all specimens were subjected up to 258 thermal cycles. Three different geometries—rectangular coupons, U-shaped ring segments and ring samples—were investigated to evaluate the influence of open/closed shape, and flat/curved surface on corrosion rate. At the same time, two types of surface finish were considered: “as received” and “ground.” The formation of a protective scale by pre-oxidation was investigated. EBSD and ESMA analyses revealed that the Cr-content of the alloy appeared to be insufficient for obtaining a protective oxide scale under studied conditions, at the same time the anayses confirmed that initial oxidation depends on presence of minor alloying elements as Si and Mn, strong oxide formers which can alter the kinetics and morphology of the corrosion reaction. Moreover, rectangular coupons with small wall thickness and flat surface exhibited the highest corrosion rate, while “ground” curved samples showed only local oxidation. This indicates that for same pre-oxidation time, oxidation kinetics is controlled by curvature. KW - Cyclic steam oxidation KW - 12%Cr steel KW - Specimen geometry KW - Surface treatments PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551808 DO - https://doi.org/10.1007/s11085-022-10114-6 SN - 0030-770X SP - 1 EP - 18 PB - Springer AN - OPUS4-55180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, X. A1 - Wei, Y. A1 - Kühbach, M. A1 - Zhao, H. A1 - Vogel, F. A1 - Darvishi Kamachali, Reza A1 - Thompson, G. B. A1 - Raabe, D. A1 - Gault, B. T1 - Revealing in-plane grain boundary composition features through machine learning from atom probe tomography data N2 - Grain boundaries (GBs) are planar lattice defects that govern the properties of many types of polycrystalline materials. Hence, their structures have been investigated in great detail. However, much less is known about their chemical features, owing to the experimental difficulties to probe these features at the atomic length scale inside bulk material specimens. Atom probe tomography (APT) is a tool capable of accomplishing this task, with an ability to quantify chemical characteristics at near-atomic scale. Using APT data sets, we present here a machine-learning-based approach for the automated quantification of chemical features of GBs. We trained a convolutional neural network (CNN) using twenty thousand synthesized images of grain interiors, GBs, or triple junctions. Such a trained CNN automatically detects the locations of GBs from APT data. Those GBs are then subjected to compositional mapping and analysis, including revealing their in-plane chemical decoration patterns. We applied this approach to experimentally obtained APT data sets pertaining to three case studies, namely, Ni-P, Pt-Au, and Al-Zn-Mg-Cu alloys. In the first case, we extracted GB specific segregation features as a function of misorientation and coincidence site lattice character. Secondly, we revealed interfacial excesses and in-plane chemical features that could not have been found by standard compositional analyses. Lastly, we tracked the temporal evolution of chemical decoration from early-stage solute GB segregation in the dilute limit to interfacial phase separation, characterized by the evolution of complex composition patterns. This machine-learning-based approach provides quantitative, unbiased, and automated access to GB chemical analyses, serving as an enabling tool for new discoveries related to interface thermodynamics, kinetics, and the associated chemistry-structure-property relations. KW - Machine learning KW - Digitalization KW - Alloy microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543049 DO - https://doi.org/10.1016/j.actamat.2022.117633 SN - 1359-6454 VL - 226 SP - 1 EP - 15 PB - Elsevier CY - Amsterdam AN - OPUS4-54304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feldmann, Titus A1 - Fedelich, Bernard A1 - Epishin, A. T1 - Simulation of Hot Isostatic Pressing in a Single-Crystal Ni Base Superalloy with the Theory of Continuously Distributed Dislocations Combined with Vacancy Diffusion N2 - Single-crystal components made of nickel base superalloys contain pores after casting and homogenization heat treatment. Hot isostatic pressing (HIP), which is carried above the γ' -solvus temperature of the alloy, is industrially applied to reduce porosity. A modeling of HIP based on continuously distributed dislocations is developed in a 2D setting. Glide and climb of straight-edge dislocations, as well as vacancy diffusion, are the deformation mechanisms taken into account. Thereby, dislocation glide is controlled by dragging a cloud of large atoms, and climb is controlled by vacancy diffusion. Relying on previous investigations of the creep behavior at HIP temperatures, it is assumed that new dislocations are nucleated at low-angle boundaries (LAB) and move through subgrains until they either reach the opposite LABs or react with other dislocations and annihilate. Vacancies are created at the pore surface and diffuse through the alloy until they are either consumed by climbing dislocations or disappear at the LABs. The field equations are solved by finite elements. It is shown that pore shrinking is mostly controlled by vacancy diffusion as the shear stresses at the LABs are too low to nucleate a sufficient amount of dislocations. KW - Nickel-base superalloys KW - HIP KW - Dislocation KW - Creep KW - Model PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542309 DO - https://doi.org/10.1002/adem.202101341 VL - 2022 PB - Wiley AN - OPUS4-54230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Lei A1 - Hoyt, J. J. T1 - Layering misalignment and negative temperature dependence of interfacial free energy of B2-liquid interfaces in a glass forming system N2 - From molecular dynamics simulations and the capillary fluctuation method, the solid-liquid interfacial free energy has been computed for the B2-liquid interface in the Cu-Zr system. Consistent with previous results for the FCC-liquid interface in Cu-Zr and Al-Sm but atypical of most alloys, was found to increase as the temperature is lowered. In addition, the temperature dependence was obtained for model Lennard-Jones B2-liquid alloys. In all cases the unusual temperature dependence of is correlated with an atomic structure of the interfacial region characterized by a misalignment of the number density peaks between solvents and solutes. In cases where the number density peaks are aligned, the typical temperature dependence is observed. The results are discussed in terms of the Gibbs theory of the thermodynamics of interfaces. It is proposed that the unique interfacial structure and the atypical temperature dependence of are hallmarks of an easy glass forming alloy. KW - Atomistic simulations KW - Interfacial free energy KW - Layering misalignment KW - Glass forming PY - 2021 DO - https://doi.org/10.1016/j.actamat.2021.117259 SN - 1359-6454 VL - 219 SP - 117259 PB - Elsevier Ltd. AN - OPUS4-53650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gebhardt, M. A1 - Malolakis, I. A1 - Kalinka, Gerhard A1 - Deubener, J. A1 - Chakraborty, S. A1 - Meiners, D. T1 - Re-use potential of carbon fibre fabric recovered from infusible thermoplastic CFRPs in 2nd generation thermosetting-matrix composites N2 - The research presented here attempts to assess the potential for re-using carbon fibre (CF) fabrics recovered from recycling infusible acrylic thermoplastic carbon fibre reinforced polymer composites (CFRPs) in a universal manner, i.e. by combining with a wide variety of matrices to manufacture 2nd generation composite laminates by resin infusion. The 2nd generation composites have been compared in terms of bulk and interfacial properties against counteparts processed with virgin carbon fibre fabric infused with the same matrices. Generally, an increase in damping (tanδ) was observed in all 2nd generation composites, which can be attributed to a residual thin thermoplastic layer present on the recovered fibres. The interfacial adhesion of the 2nd generation Composites was investigated by shear tests and scanning electron micsoscopy, and also appears to be less influenced by the type of matrix. KW - Composite recycling KW - Thermoplastic matrix KW - Thermosetting resin KW - Fibre/matrix bonding PY - 2021 DO - https://doi.org/10.1016/j.coco.2021.100974 VL - 28 SP - 100974 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-53639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Plichta, T. A1 - Sirjovona, V. A1 - Zvonek, M. A1 - Kalinka, Gerhard A1 - Cech, V. T1 - The Adhesion of Plasma Nanocoatings Controls the Shear Properties of GF/Polyester Composite N2 - High-performance fibre-reinforced polymer composites are important construction materials based not only on the specific properties of the reinforcing fibres and the flexible polymer Matrix but also on the compatible properties of the composite interphase. First, oxygen-free (a-CSi:H) and oxygen-binding (a-CSiO:H) plasma nanocoatings of different mechanical and tribological properties were deposited on planar silicon dioxide substrates that closely mimic E-glass. The nanoscratch test was used to characterize the nanocoating adhesion expressed in terms of critical normal load and work of adhesion. Next, the same nanocoatings were deposited on E-glass fibres, which were used as reinforcements in the polyester composite to affect its interphase properties. The shear properties of the polymer composite were characterized by macro- and micromechanical tests, namely a short beam shear test to determine the short-beam strength and a single fibre push-out test to determine the interfacial shear strength. The results of the polymer composites showed a strong correlation between the short-beam strength and the interfacial shear strength, proving that both tests are sensitive to changes in fibre-matrix adhesion due to different surface modifications of glass fibres (GF). Finally, a strong correlation between the shear properties of the GF/polyester composite and the adhesion of the plasma nanocoating expressed through the work of adhesion was demonstrated. Thus, increasing the work of adhesion of plasma nanocoatings from 0.8 to 1.5 mJ·m−2 increased the short-beam strength from 23.1 to 45.2 MPa. The results confirmed that the work of adhesion is a more suitable parameter in characterising the level of nanocoating adhesion in comparison with the critical normal load. KW - Mechanical properties KW - Plasma nanocoatings KW - Glass fibre KW - Polymer composite KW - Short-beam strength KW - Interfacial shear strength KW - Work of adhesion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521844 DO - https://doi.org/10.3390/polym13040593 VL - 13 IS - 4 SP - 593 PB - MDPI CY - Basel,Schweiz AN - OPUS4-52184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Rychlowski, L. A1 - Cios, G. A1 - Winkelmann, A. T1 - Crystallographic analysis of the lattice metric (CALM) from single electron backscatter diffraction or transmission Kikuchi diffraction patterns N2 - A new software is presented for the determination of crystal lattice parameters from the positions and widths of Kikuchi bands in a diffraction pattern. Starting with a single wide-angle Kikuchi pattern of arbitrary resolution and unknown phase, the traces of all visibly diffracting lattice planes are manually derived from four initial Kikuchi band traces via an intuitive graphical user interface. A single Kikuchi bandwidth is then used as reference to scale all reciprocal lattice point distances. Kikuchi band detection, via a filtered Funk transformation, and simultaneous display of the band intensity profile helps users to select band positions and widths. Bandwidths are calculated using the first derivative of the band profiles as excess-deficiency effects have minimal influence. From the reciprocal lattice, the metrics of possible Bravais lattice types are derived for all crystal systems. The measured lattice parameters achieve a precision of <1%, even for good quality Kikuchi diffraction patterns of 400 x 300 pixels. This band-edge detection approach has been validated on several hundred experimental diffraction patterns from phases of different symmetries and random orientations. It produces a systematic lattice parameter offset of up to ±4%, which appears to scale with the mean atomic number or the backscatter coefficient. KW - Electron backscatter diffraction KW - Kikuchi patterns KW - Lattice parameters KW - Radon transform PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527076 DO - https://doi.org/10.1107/S1600576721004210 SN - 1600-5767 VL - 54 IS - Pt 3 SP - 1012 EP - 1022 AN - OPUS4-52707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, A. A1 - Cios, G. A1 - Tokarski, T. T1 - Tetragonality mapping of martensite in high-carbon steel by EBSD N2 - The locally varying tetragonality in martensite grains of a high-carbon steel (1.2 mass percent C) was resolved by electron backscatter diffraction (EBSD) with a spatial resolution in the order of 100 nm. Compared to spatially integrating X-ray diffraction, which yielded an average tetragonality fo c/a=1.05, the EBSD measurements in the scanning electron microscope allowed to image a local variation of the lattice papameter ration c/a in the range of 1.02 ≤ c/a ≤ 1.07. The local variation of tetragonality is confirmed by two different EBSD data analysis approaches based on the fitting of simulated to experimental EBSD patterns. The resulting EBSD-based tetragonality maps are pointing to a complex interaction of carbon concentration and local lattice distortions during the formation process of martensitic structures. KW - EBSD KW - Martensite KW - Tetragonal distortion KW - Pattern matching PY - 2021 DO - https://doi.org/10.1016/j.matchar.2021.111040 VL - 175 SP - 111040 PB - Elsevier Inc. AN - OPUS4-52343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Camin, B. A1 - Hansen, L. A1 - Chyrkin, A. A1 - Nolze, Gert T1 - Synchrotron Sub-μ X-ray Tomography of Kirkendall Porosity in a Diffusion Couple of Nickel-Base Superalloy and Nickel after Annealing at 1250 °C N2 - Kirkendall porosity that forms during interdiffusion in a diffusion couple of nickel-base superalloy CMSX-10 with pure nickel is investigated. The diffusion experiments are conducted at a temperature of 1250 °C, where the strengthening ƴ'-phase ist partially dissolved. The porosity is studied by X-ray sub-μ tomography with a spatial resolution of about 0.35³ μm³ at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France. It is found that depending on the distance from the interface the Kirkendall pores take different shapes: octahedral, rounded pyramidal, drop shaped, dendritic, pear shaped, and joint shapes. Such a variety of pore morphologies indicates a complex multistage process of porosity nucleation and growth under vacancy supersaturation of different degrees. The experimental findings are interpreted on the basis of the results of diffusion modeling. It is shown that the kinetics of porosity growth is essentially influenced by the dissolution of the ƴ'-phase. KW - Diffusion KW - Nickel alloys KW - Porous materials KW - Synchrotron radiations KW - Three-dimensional tomographies PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521476 DO - https://doi.org/10.1002/adem.202001220 VL - 23 IS - 4 SP - 1220 PB - Wiley Online Library AN - OPUS4-52147 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. A1 - Hourahine, B. A1 - Trager-Cowan, C. T1 - Kikuchi pattern simulations of backscattered and transmitted electrons N2 - We discuss a refined simulation approach which treats Kikuchi diffraction patterns in electron backscatter diffraction (EBSD) and transmission Kikuchi diffraction (TKD). The model considers the result of two combined mechanisms: (a) the dynamical diffraction of electrons emitted coherently from point sources in a crystal and (b) diffraction effects on incoherent diffuse intensity distributions. Using suitable parameter settings, the refined simulation model allows to reproduce various thickness- and energy-dependent features which are observed in experimental Kikuchi diffraction patterns. Excess-deficiency features are treated by the effect of gradients in the incoherent background intensity. Based on the analytical two-beam approximation to dynamical electron diffraction, a phenomenological model of excess-deficiency features is derived, which can be used for pattern matching applications. The model allows to approximate the effect of the incident beam geometry as a correction signal for template patterns which can be reprojected from pre-calculated reference data. As an application, we find that the accuracy of fitted projection centre coordinates in EBSD and TKDcan be affected by changes in the order of 10−3–10-2 if excess-deficiency features are not considered in the theoreticalmodel underlying a best-fit pattern matching approach. Correspondingly, the absolute accuracy of simulation-based EBSD strain determination can suffer frombiases of a similar order of magnitude if excess-deficiency effects are neglected in the simulation model. KW - Electron diffraction KW - EBSD KW - Kikuchi diffraction KW - Pattern matching PY - 2021 DO - https://doi.org/10.1111/jmi.13051 VL - 284 IS - 2 SP - 157 EP - 184 PB - Wiley Online Library AN - OPUS4-53109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Treninkov, И. A A1 - Petrushin, N. V. A1 - Epishin, А. I. A1 - Svetlov, I. L. A1 - Nolze, Gert A1 - Elyutin, E. S. T1 - ЭКСПЕРИМЕНТАЛЬНОЕ ОПРЕДЕЛЕНИЕ ТЕМПЕРАТУРНОЙ ЗАВИСИМОСТИ СТРУКТУРНО-ФАЗОВЫХ ПАРАМЕТРОВ НИКЕЛЕВОГО ЖАРОПРОЧНОГО СПЛАВА T1 - Experimental determination of temperature dependence of structural-phase parameters of nickel-based superalloy N2 - Методом рентгеноструктурного анализа в интервале температур 18—1150 °С определены температурные зависимости периодов кристаллических решеток γ- и γ'-фаз, их размерно-го несоответствия (мисфит) и объемной доли γ'-фазы экспериментального монокристал-лического жаропрочного никелевого сплава. Определены диапазоны температур, в которых происходят интенсивные изменения структурно-фазовых характеристик исследованного сплава. KW - рентгеноструктурный анализ KW - высокие температуры KW - жаропрочные нике- левые сплавы KW - монокристалл KW - γ- и γ'-фазы, период кристаллической решетки PY - 2021 DO - https://doi.org/10.31044/1684-579x-2021-0-7-3-12 IS - 7 SP - 3 EP - 12 AN - OPUS4-53110 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tokarski, T. A1 - Nolze, Gert A1 - Winkelmann, A. A1 - Rychlowski, L. A1 - Bala, P. A1 - Cios, G. T1 - Transmission Kikuchi diffraction: The impact of the signal-to-noise ratio N2 - Signal optimization for transmission Kikuchi diffraction (TKD) measurements in the scanning electron microscope is investigated by a comparison of different sample holder designs. An optimized design is presented, which uses a metal shield to efficiently trap the electron beam after transmission through the sample. For comparison, a second holder configuration allows a significant number of the transmitted electrons to scatter back from the surface of the sample holder onto the diffraction camera screen. It is shown that the secondary interaction with the sample holder leads to a significant increase in the background level, as well as to additional noise in the final Kikuchi diffraction signal. The clean TKD signal of the optimized holder design with reduced background scattering makes it possible to use small signal changes in the range of 2% of the camera full dynamic range. As is shown by an analysis of the power spectrum, the signal-to-noise ratio in the processed Kikuchi diffraction patterns is improved by an order of magnitude. As a result, the optimized design allows an increase in pattern signal to noise ratio which may lead to increase in measurement speed and indexing reliability. KW - EBSD KW - SEM KW - Transmission Kikuchi diffraction KW - Sample holder PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531743 DO - https://doi.org/10.1016/j.ultramic.2021.113372 SN - 0304-3991 SN - 1879-2723 VL - 230 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-53174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dub, S. A1 - Haftaoglu, Cetin A1 - Kindrachuk, Vitaliy T1 - Estimate of theoretical shear strength of C60 single crystal by nanoindentation N2 - The onset of plasticity in a single crystal C60 fullerite was investigated by nanoindentation on the (111) crystallographic plane. The transition from elastic to plastic deformation in a contact was observed as pop-in events on loading curves. The respective resolved shear stresses were computed for the octahedral slip systems ⟨011¯¯¯⟩{111}, supposing that their activation resulted in the onset of plasticity. A finite element analysis was applied, which reproduced the elastic loading until the first pop-in, using a realistic geometry of the Berkovich indenter blunt tip. The obtained estimate of the C60 theoretical shear strength was about 1/11 of the shear modulus on {111} planes. KW - Finite element analysis KW - Fullerite KW - Nanoindentation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523208 DO - https://doi.org/10.1007/s10853-021-05991-2 VL - 56 IS - 18 SP - 10905 EP - 10914 PB - Springer Nature AN - OPUS4-52320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -