TY - JOUR A1 - Nolze, Gert T1 - Characterization of the fcc/bcc orientation relationship by EBSD using pole figures and variants JF - Zeitschrift für Metallkunde N2 - The orientation relationship (OR) between fcc and bcc lattices are described by crystallographic fundamentals using the example of Kurdjumov-Sachs (K-S) and Nishiyama-Wassermann (N-W). Complete pole figures containing all variants will be used to distinguish even between slightly different ORs. EBSD on iron meteorites and duplex steel has been used to analyse a large number of crystal orientations with regard to a high statistical significance and a high probability to capture all variants in a single measurement. It is shown that the use of fixed OR models like K-S, N-W, Bain, Pitsch, or Greninger-Troiano does not satisfacturally reflect the observed experimental pole distributions. It is not convenient to use high-indexed lattice planes and directions to describe the small deviations from the given models. The Euler subspace representation offers a readily comprehensible tool to get an idea about the characteristic of the experimentally detected OR. KW - EBSD KW - Duplex steel KW - Iron meteorite KW - Pole figure KW - Orientation relationship PY - 2004 DO - https://doi.org/10.1515/ijmr-2004-0142 SN - 0044-3093 VL - 95 IS - 9 (85 Jahre DGM) SP - 744 EP - 755 PB - Hanser CY - München AN - OPUS4-13972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yukhvid, V. A1 - Gorshkov, V. A1 - Miloserdov, P. A1 - Skachkova, N. A1 - Alymov, M. I. A1 - Nolze, Gert A1 - Epishin, A. T1 - Synthesis of Molybdenum and Niobium Mono- and Binary Silicides by the Method of SHS-Metallurgy JF - Advanced engineering materials N2 - The process of self-propagating high-temperature synthesis of the Mo–Nb–Si silicides from the powder mixtures has been investigated. Based on performed experiments, the composition of powder mixtures as well as technological parameters are proposed which provide the synthesis of monosilicides MoSi₂, NbSi₂, and binary silicides Mo₁-хNbxSi₂ with different ratios of Nb/Mo by adding different contents of MoO₃ and Nb₂O₅. Microstructure and phase compositions of the obtained silicide ingots are characterized by scanning electron microscopy, electron probe microanalysis, X-ray diffraction, and backscatter electron diffraction. KW - Synthesis KW - EBSD KW - XRD PY - 2016 DO - https://doi.org/10.1002/adem.201600334 SN - 1438-1656 SN - 1527-2648 SP - 1 EP - 6 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-37209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Holzlechner, Gerald A1 - Nolze, Gert A1 - Wirth, Thomas A1 - Eliezer, D. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging of deuterium assisted cracking in a 2205 duplex stainless steel microstructure JF - Materials Science & Engineering A N2 - In the present work, the influence of deuterium on the microstructure of a duplex stainless steel type EN 1.4462 has been characterized by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) supported by scanning electron microscopy (SEM), focused ion beam (FIB), electron back scattered diffraction(EBSD) and energy dispersive x-ray (EDX) investigations. Characterization has been carried out before and after electrochemical charging with deuterium which has been used as a tracer, due to its similar behavior to hydrogen in the steel microstructure. In a first approach, the distribution of the deuterium occurring at temperatures above 58 °C has been visualized. Further it turned out that sub-surface micro blisters are formed in the ferrite-austenite interface, followed by the formation of needle shaped plates and subsequent cracking at the ferrite surface. In the austenite phase, parallel cracking alongside twins and hexagonal close packed (martensitic) regions has been observed. In both phases and even in the apparent interface, cracking has been associated with high deuterium concentrations, as compared to the surrounding undamaged microstructure. Sub-surface blistering in the ferrite has to be attributed to the accumulation and recombination of deuterium at the ferrite-austenite interface underneath the respective ferrite grains and after fast diffusing through this phase. Generally, the present application of chemometric imaging and structural analyses allows characterization of hydrogen assisted degradation at a sub-micron lateral resolution. KW - ToF-SIMS KW - Hydrogen assisted cracking KW - Hydrogen embrittlement KW - SEM KW - FIB KW - EBSD PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S0921509316310334 DO - https://doi.org/10.1016/j.msea.2016.08.107 SN - 0921-5093 VL - 676 SP - 271 EP - 277 PB - Elsevier B.V. AN - OPUS4-37298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Payton, E. A1 - Nolze, Gert T1 - The Backscatter Electron Signal as an Additional Tool for Phase Segmentation in Electron Backscatter Diffraction JF - Microscopy and Microanalysis N2 - The advent of simultaneous energy dispersive X-ray spectroscopy (EDS) data collection has vastly improved the phase separation capabilities for electron backscatter diffraction (EBSD) mapping. A major problem remains, however, in distinguishing between multiple cubic phases in a specimen, especially when the compositions of the phases are similar or their particle sizes are small because the EDS interaction volume is much larger than that of EBSD, and the EDS spectra collected during spatial mapping are generally noisy due to time limitations and the need to minimize sample drift. The backscatter electron (BSE) signal is very sensitive to the local composition due to its atomic number (Z) dependence. BSE imaging is investigated as a complimentary tool to EDS to assist phase segmentation and identification in EBSD through examination of specimens of meteorite, Cu dross, and steel oxidation layers. The results demonstrate that the simultaneous acquisition of EBSD patterns, EDS spectra, and the BSE signal can provide new potential for advancing multiphase material characterization in the scanning electron microscope. KW - Electron backscatter diffraction KW - Energy dispersive x-ray spectroscopy KW - Scanning electron microscopy KW - Multiphase microstructure KW - Phase identification KW - Backscattered electron imaging KW - Meteorite KW - Monte Carlo simulation PY - 2013 DO - https://doi.org/10.1017/S1431927613000305 VL - 19 IS - 4 SP - 929 EP - 941 AN - OPUS4-37895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Link, T. A1 - Svetlov, I. L. A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Lucas, H. T1 - Mechanism of porosity growth during homogenisation in single crystal nickel-based superalloys JF - International Journal of Materials Research N2 - Several mechanisms for porosity growth in single crystal nickel-based superalloys during homogenisation heat treatment have been proposed in the literature. They were carefully checked using different experimental methods, namely quantitative light microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and density measurements. It is shown that the main mechanism is the Kirkendall–Frenkel effect, i.e. generation of voids due to uncompensated efflux of Al atoms from dissolving γ/γ′-eutectic areas. The Al diffusion is supported by the afflux of vacancies from surrounding γ-matrix which results in porosity growth. This conclusion is confirmed by the estimation of the vacancy afflux towards the dissolving eutectic. KW - Ni-base superalloy KW - Eutectic KW - Vacancies KW - Porosity PY - 2013 VL - 104 IS - 8 SP - 776 EP - 782 PB - Carl Hanser Verlag AN - OPUS4-37983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Payton, E. J. A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Phase Identification by Image Processing of EBSD Patterns JF - Microscopy and Microanalysis N2 - Automated electron backscatter diffraction (EBSD) is generally unable to distinguish between multiple cubic phases in a specimen without additional information, such as that obtained by simultaneous energy dispersive X-ray spectroscopy (EDS). Small particles of phases with relatively similar compositions push the limits of phase identification using simultaneous EBSD and EDS, and a mismatch exists between the spatial resolutions of these two techniques due to them having different electron interaction volumes. In a recent paper, the present authors explored using backscatter detectors mounted on top of the EBSD detector to obtain atomic number (Z) contrast images that could be used for phase segmentation in cases where the results from the EBSD and EDS signals remain ambiguous. In the present work, we show that similar information can be obtained from the raw EBSD patterns themselves at higher spatial resolution than was obtained from the backscatter detectors, with the additional advantage of having no spatial mismatch between the data collection grids. KW - Phase identification KW - Backscattered electrons KW - EBSD KW - SEM PY - 2013 DO - https://doi.org/10.1017/S143192761300620X VL - 19 IS - Suppl. 2 SP - 842 EP - 843 AN - OPUS4-37985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Payton, E. A1 - Winkelmann, Aimo T1 - Advanced EBSD Pattern Interpretation through Iterative Post-Processing JF - Microscopy and Microanalysis N2 - Since the BSE signal depends on many factors, like the chemistry of the phase and the acceleration voltage, the size and position of the detector array is (slightly) different from phase to phase so that an (iterative) post-processing of the stored patterns is highly recommended. The derived BSE signal can be used for phase assignment in high resolution and high speed maps when EBSD fails and/or EDS (energy dispersive spectroscopy) needs too much time for a suitable and parallel signal acquisition. KW - Electron backscatter diffraction KW - Phase identification KW - Microstructure KW - SEM PY - 2013 DO - https://doi.org/10.1017/S1431927613005631 VL - 19 IS - Suppl. 2 SP - 728 EP - 729 AN - OPUS4-37986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Combination of colored patterns and cubes for crystallographic point group visualization JF - Crystal Research and Technology N2 - A concept based on the application of a cube as a general polyhedron is presented for the visualization of point group symmetry. The cube is used to represent both the highest and lowest crystal symmetries, with differences observable as patterns characteristic to each point group. Patterns are generated using direction-specific color keys, which enable the recognition of point group-specific distribution of vectors in an external reference frame. For the visualization of the incoherent hexagonal crystal classes, two twinned cubes are applied in order to generate symmetry operators that would otherwise be missing. The resulting hexagonal dipyramid is described in the frame of a cube, reducing the number of used symmetry operators from 72 to 60. The complete set of 32 polyhedra are suitable, for example, as a visual aid for understanding the crystal symmetry and/or sub- and supergroup relationships. KW - Subgroup KW - Crystal class KW - Color key KW - Fundamental zone KW - Teaching PY - 2013 DO - https://doi.org/10.1002/crat.201300134 VL - 48 IS - 7 SP - 476 EP - 489 PB - WILEY-VCH AN - OPUS4-37988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Azimuthal Projections: Data Rotation and Projection Switching in Real Time JF - Microscopy and Microanalysis N2 - Pole figures are often used to present crystal orientation data. The huge number of single orientation measurements acquired by electron backscatter diffraction (EBSD) poses a challenge for pole figure representation due to the large number of calculations required. This significantly reduces the speed at which the data may be rotated and affects the ability to switch between different projection types. In the present work, it will be shown that satisfactory representation of orientation data in different projection types can generally be achieved by an imaging of a spherical projection. With this approach, explicit calculation of the projections is no longer required, allowing for both real-time dataset rotation and real-time switching between all projection types relevant to materials science. The technique can be applied to any other directional property distribution, for example, not only for EBSD orientation presentation. KW - Stereographic projection KW - Equal area projection KW - Gnomonic projection KW - Azimuthal projection KW - Crystal orientation KW - Projection imaging KW - Coordinate transformation KW - Real-time rotation PY - 2013 DO - https://doi.org/10.1017/S1431927613001414 VL - 19 SP - 950 EP - 958 PB - Microscopy Society of America AN - OPUS4-37989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reith, F. A1 - Fairbrother, L. A1 - Nolze, Gert A1 - Wilhelmi, O. A1 - Clode, P. L. A1 - Gregg, A. O. A1 - Parsons, J. E. A1 - Wakelin, S. A. A1 - Pring, A. A1 - Hough, R. A1 - Southam, G. A1 - Brugger, J. T1 - Nanoparticle factories: Biofilms hold the key to gold dispersion and nugget formation JF - Geology N2 - Biofilms living on gold (Au) grains play a key role in the biogeochemical cycle of Au by promoting the dispersion of Au via the formation of Au nanoparticles as well as the formation of secondary biomorphic Au. Gold grains from Queensland, Australia, are covered by a polymorphic, organic-inorganic layer that is up to 40 μm thick. It consists of a bacterial biofilm containing Au nanoparticles associated with extracellular polymeric substances as well as bacterioform Au. Focused ion beam (FIB) sectioning through the biofilm revealed that aggregates of nanoparticulate Au line open spaces beneath the active biofilm layer. These aggregates (bacterioform Au type 1) resulted from the reprecipitation of dissolved Au, and their internal growth structures provide direct evidence for coarsening of the Au grains. At the contact between the polymorphic layer and the primary Au, bacterioform Au type 2 is present. It consists of solid rounded forms into which crystal boundaries of underlying primary Au extend, and is the result of dealloying and Ag dissolution from the primary Au. This study demonstrates that (1) microbially driven dissolution, precipitation, and aggregation lead to the formation of bacterioform Au and contribute to the growth of Au grains under supergene conditions, and (2) the microbially driven mobilization of coarse Au into nanoparticles plays a key role in mediating the mobility of Au in surface environments, because the release of nanoparticulate Au upon biofilm disintegration greatly enhances environmental mobility compared to Au complexes only. KW - Nanomaterial KW - Gold KW - Electron backscatter diffraction PY - 2010 DO - https://doi.org/10.1130/G31052.1 VL - 38 IS - 9 SP - 843 EP - 846 PB - Geological Society of America AN - OPUS4-37995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Hielscher, R. A1 - Winkelmann, Aimo T1 - Electron backscatter diffraction beyond the mainstream JF - Crystal Research and Technology N2 - We present special applications of electron backscatter diffraction (EBSD) which aim to overcome some of the limitations of this technique as it is currently applied in the scanning electron microscope. We stress that the raw EBSD signal carries additional information which is useful beyond the conventional orientation determination. The background signal underlying the backscattered Kikuchi diffraction (BKD) patterns reflects the chemical composition and surface topography but also contains channeling-in information which is used for qualitative real-time orientation imaging using various backscattered electron signals. A significantly improved orientation precision can be achieved when dynamically simulated pattern are matched to the experimental BKD patterns. The breaking of Friedel’s rule makes it possible to obtain orientation mappings with respect to the point-group symmetries. Finally, we discuss the determination of lattice parameters from individual BKD patterns. Subgrain structure in a single quartz grain. The increased noise level in the left map reflects the lower precision of a standard orientation determination using band detection by the Hough transform. The right map results from the same experimental raw data after orientation refinement using a pattern matching approach. The colors correspond an adapted inverse pole figure color key with a maximum angular deviation of about 2° from the mean orientation. KW - Electron backscatter diffraction PY - 2017 DO - https://doi.org/10.1002/crat.201600252 SN - Online 1521-4079 VL - 52 IS - 1 SP - Special Issue - Article Number: UNSP 1600252, 1 EP - 24 PB - WILEY-VCH AN - OPUS4-37935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Link, T. A1 - Nolze, Gert A1 - Svetlov, I. L. A1 - Bokshtein, B. S. A1 - Rodin, A. O. A1 - Saliwan Neumann, Romeo A1 - Oder, Gabriele T1 - Diffusion processes in multicomponent nickel-base superalloy-nickel system JF - The Physics of Metals and Metallography N2 - Optical and scanning electron microscopy, as well as electron microprobe analysis and electron backscatter diffraction, have been used to study diffusion processes that occur in a diffusion pair that consistsof a single-crystal CMSX-10 nickel-base superalloy and polycrystalline nickel, at temperatures of 1050–1250°C. It has been found that, in this system, the distributions of γ-stabilizing elements (Cr, Co, W, and Re) are described by the Boltzmann solution for diffusion between two semiinfinite plates of a binary alloy. The processing of these distributions has shown that the diffusion coefficients of Cr, Co, W, and Re in the multicomponent system are close to those in binary alloys of these elements with Ni. The diffusion redistribution of the elements leads to the dissolution of the γ′ phase in the nickel-base superalloy, growth of nickel grains toward the superalloy constituent of the diffusion pair, and the formation of porosity on both sides of the migrating interface, which is determined from a crystal misorientation of the alloy single crystal and nickel grains. KW - Ni-base superalloy KW - Interface KW - Diffusion KW - Phase transformation KW - Porosity PY - 2014 SN - 0031-918X VL - 115 IS - 1 SP - 21 EP - 29 AN - OPUS4-37980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Payton, E. T1 - Messengers from Space: A Scanning Electron Microscopy Investigation JF - Imaging & Microscopy N2 - The macro- and microstructure of iron meteorites provide valuable insights into both the inner structure of our planet and the history of our solar system. High speed collision events in the asteroid belt send the meteorites careening toward Earth. The collisions produce unique deformation microstructures. With cooling rates on the scale of a few degrees per million years, iron meteorites can consist of crystal sizes on the order of meters prior to the collision events. These extremely slow cooling rates result in phase transformations occurring at conditions near thermodynamic equilibrium. Preserving meteorite fragments is important for future studies of phase transformations, material behavior at high strain rates, and the origin of the universe. KW - Meteorite KW - Phase identification KW - Hibbingite KW - Orientation relationship KW - Electron backscatter diffraction KW - Energy dispersive x-ray spectroscopy KW - EDX PY - 2013 IS - 3 SP - 2 EP - 4 PB - GIT Verlag AN - OPUS4-37981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin, S. A1 - Walnsch, A. A1 - Nolze, Gert A1 - Leineweber, A. A1 - Léaux, F. A1 - Scheuerlein, C. T1 - The crystal structure of (Nb0.75Cu0.25)Sn-2 in the Cu-Nb-Sn system JF - Intermetallics N2 - During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite. KW - Electron backscatter diffraction KW - X-ray diffraction KW - Intermetallic compound KW - Structure solution KW - Superconductor PY - 2017 DO - https://doi.org/10.1016/j.intermet.2016.09.008 SN - 0966-9795 SN - 1879-0216 VL - 80 SP - 16 EP - 21 PB - Elsevier Ltd. AN - OPUS4-37874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Petrushin, N. V. A1 - Link, T. A1 - Nolze, Gert A1 - Loshchinin, Yu. V. A1 - Gerstein, G. T1 - Thermal stability of the structure of a heat-resistant cobalt alloy hardened with intermetallic γ'-phase precipitates JF - Russian Metallurgy N2 - The thermal stability of the microstructure of a heat-resistant cobalt alloy, which consists of a γ solid solution strengthened with γ'-phase precipitates, has been studied. The temperature behavior of the dissolution of the hardening γ' phase and the kinetics of its coarsening at 700 and 800°C have been determined. It is found that, during prolonged annealing at 800°C, the γ' → β phase transformation occurs. KW - Superalloy KW - Microstructure KW - Hardening KW - Electron backscatter diffraction KW - TEM PY - 2016 DO - https://doi.org/10.1134/S0036029516040078 SN - 0036-0295 VL - 2016 IS - 4 SP - 286 EP - 291 PB - Pleiades Publishing AN - OPUS4-37768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vos, M. A1 - Winkelmann, Aimo A1 - Nolze, Gert T1 - Element-specific Kikuchi patterns of Rutile JF - Ultramicroscopy N2 - The kinetic energy of keV electrons backscattered from a rutile (TiO2) surface depends measurably on the mass of the scattering atom. This makes it possible to determine separately the angular distribution of electrons backscattered elastically from either Ti or O. Diffraction effects of these backscattered electrons inside the rutile crystal lead to the formation of Kikuchi patterns. The element-resolved Kikuchi patterns of Ti and O differ characteristically, but each can be described fairly well in terms of the dynamical theory of diffraction. Qualitatively, much of the differences can be understood by considering the relative arrangement of the Ti and O atoms with respect to planes defined by the crystal lattice. KW - Electron Rutherford backscattering KW - TiO2 KW - Kikuchi pattern KW - EBSD pattern KW - Simulation PY - 2015 DO - https://doi.org/10.1016/j.ultramic.2015.04.018 SN - 0304-3991 VL - 156 SP - 50 EP - 58 AN - OPUS4-37787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lühr, T. A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Krull, D. A1 - Westphal, C. T1 - Direct Atom Imaging by Chemical-Sensitive Holography JF - Nano Letters N2 - In order to understand the physical and chemical properties of advanced materials, functional molecular adsorbates, and protein structures, a detailed knowledge of the atomic arrangement is essential. Up to now, if subsurface structures are under investigation, only indirect methods revealed reliable results of the atoms’ spatial arrangement. An alternative and direct method is three-dimensional imaging by means of holography. Holography was in fact proposed for electron waves, because of the electrons’ short wavelength at easily accessible energies. Further, electron waves are ideal structure probes on an atomic length scale, because electrons have a high scattering probability even for light elements. However, holographic reconstructions of electron diffraction patterns have in the past contained severe image artifacts and were limited to at most a few tens of atoms. Here, we present a general reconstruction algorithm that leads to high-quality atomic images showing thousands of atoms. Additionally, we show that different elements can be identified by electron holography for the example of FeS₂ . KW - holography KW - electron diffraction KW - atomic imaging KW - photoemission KW - electron backscattering PY - 2016 DO - https://doi.org/10.1021/acs.nanolett.6b00524 VL - 16 IS - 5 SP - 3195 EP - 3201 PB - American Chemical Society AN - OPUS4-37739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Hielscher, R. ED - Hielscher, Ralf T1 - Orientations - perfectly colored JF - Journal of Applied Crystallography N2 - The inverse pole figure (IPF) coloring for a suitable evaluation of crystal orientation data is discussed. The major goal is a high correlation between encoding color and crystal orientation. Revised color distributions of the fundamental sectors are introduced which have the advantages of (1) being applicable for all point groups, (2) not causing color discontinuities within grains, (3) featuring carefully balanced regions for red, cyan, blue, magenta, green and yellow, and (4) an enlarged gray center in opposition to a tiny white center. A new set of IPF color keys is proposed which is the result of a thorough analysis of the colorization problem. The discussion considers several topics: (a) the majority of presently applied IPF color keys generate color discontinuities for specifically oriented grains; (b) if a unique correlation between crystal direction and color is requested, discontinuity-preventing keys are possible for all point groups, except for 4, 3 and 1; (c) for a specific symmetry group several IPF color keys are available, visualizing different features of a microstructure; and (d) for higher symmetries a simultaneous IPF mapping of two or three standard reference directions is insufficient for an unequivocal orientation assignment. All color keys are available in MTEX, a freely available MATLAB toolbox. KW - Electron backscatter diffraction KW - Color coding KW - Symmetry groups KW - Orientation description PY - 2016 DO - https://doi.org/10.1107/S1600576716012942 SN - 0021-8898 SN - 1600-5767 VL - 49 IS - 5 SP - 1786 EP - 1802 AN - OPUS4-37741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, Aimo A1 - Nolze, Gert T1 - Channeling-enhanced EDX for polarity resolved crystal orientation determination JF - Crystal Research and Technology N2 - Using channeling-enhanced energy-dispersive X-ray spectroscopy (EDX), we demonstrate polarity sensitive orientation determination of a non-centrosymmetric crystal in the scanning electron microscope. The authors observe a characteristic asymmetry in the channeling-enhanced, angle-dependent EDX data of a GaAs sample, which is in good agreement to simulations using the dynamical theory of diffraction for the incident electron beam. This allows us to assign the orientation of the GaAs crystal according to the non-centrosymmetric point group. The method shown here overcomes the limitation of a reduced point-group sensitivity of electron backscatter diffraction Patterns and electron channeling patterns for crystalline phases that contain atoms of approximately equal electron scattering cross sections. KW - Channeling KW - EDX KW - EDS KW - Composition KW - GaAs KW - GaP PY - 2016 DO - https://doi.org/10.1002/crat.201600258 SN - 0232-1300 SN - 0023-4753 VL - 51 IS - 12 SP - 752 EP - 756 AN - OPUS4-38098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Glowacka, A. A1 - Wozniak, M. J. A1 - Nolze, Gert A1 - Swiatnicki, W. A. T1 - Hydrogen induced phase transformations in austenitic-ferritic steel JF - Solid State Phenomena N2 - The hydrogen influence on the microstructure of the austenitic-ferritic Cr22-Ni5-Mo3 stainless steel was investigated. Cathodic hydrogen charging was performed electrochemically from aqueous solution of 0.1M H2SO4 with hydrogen entry promoter addition. The aim of this study was to reveal microstructural changes appearing during the hydrogen charging and particularly to clarify the occurrence of phase transformations induced by hydrogen. The specific changes in both phases of steel were observed. In the ferritic phase, strong increase of dislocation density was noticed. Longer time of hydrogen charging leaded also to the strips and twin plates formation in ferrite phase. In the austenitic phase, the generation of stacking faults, followed by the formation of α' martensite was remarked. KW - Steel KW - Hydrogen KW - Embrittlement KW - Electron backscatter diffraction KW - SEM PY - 2006 DO - https://doi.org/10.4028/www.scientific.net/SSP.112.133 SN - 1662-9779 VL - 112 SP - 133 EP - 140 AN - OPUS4-38031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Geist, V. T1 - A new method for the investigation of orientation relationships in meteoritic plessite JF - Crystal Research and Technology N2 - The orientation relationship (OR) between the bcc and fcc phase in the plessite microstructure of the iron meteorites Watson, Agpalilik and Gibeon has been analysed in a scanning electron microscope using electron back-scattered diffraction (EBSD). A very strong OR exists, independently on the analysed plessite type and the observed spreading of single orientation data. The agreement between the experimental orientation distribution and existing models varies for each meteorite. The black plessite in the Agpalilik corresponds to the Nishiyama-Wassermann model whereas the Duplex plessite of the Gibeon meteorite shows an OR close to the Kurdjumov-Sachs model. The Watson meteorite is strongly deformed so that a general OR is difficult to determine due to the blurred experimental orientation distribution. KW - Meteorite KW - Orientation relationship KW - Steel KW - Electron backscatter diffraction KW - Kurdjumov-Sachs KW - Nishiyama-Wassermann PY - 2004 DO - https://doi.org/10.1002/crat.200310193 SN - 0023-4753 SN - 0232-1300 VL - 39 IS - 4 SP - 343 EP - 352 AN - OPUS4-38032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Irrational orientation relationship derived from rational orientation relationships using EBSD data JF - Crystal Research and Technology N2 - The determination of the orientation relationship (OR) between α-Fe matrix (bcc) and γ-Fe precipitates (fcc) is discussed using orientation data collected by electron backscatter diffraction (EBSD). The comparatively low accuracy of EBSD is compensated by the high number of measurements what allows a general statement regarding to the mean OR existing in a sample. The representation and discussion is realized on a part of the Bain zone in a {001} pole figure. A discussion of some selected rational OR which are commonly used for the phase boundary characterization between α and γ shows that the pole figures describing a transformation from γ → α are different to those for α → γ. A technique is proposed based on at least three misorientation angles between the experimental OR to the rational OR's as reference. For the misorientation angle distribution a refinement is applied to extract the mean values. They are used to detect the mean OR, what is also possible for only a few or even a single precipitate if the number of measurements describing the phase boundary is sufficiently high. KW - Orientation mapping KW - Orientation relationship KW - Electron backscatter diffraction KW - Kurdjumov-Sachs KW - Nishiyama-Wassermann KW - Misorientation PY - 2008 DO - https://doi.org/10.1002/crat.200711058 VL - 43 IS - 1 SP - 61 EP - 73 PB - WILEY-VCH AN - OPUS4-38009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Link, T. A1 - Nolze, Gert T1 - SEM investigation of interfacial dislocations in nickel-base superalloys JF - Journal of Microscopy N2 - A new technique for investigation of interfacial dislocations in nickel-base superalloys by scanning electron microscopy is presented. At high temperatures the pressure of interfacial dislocations against the gamma/gamma'-interface causes grooves. This 'fingerprint of the dislocation network' is visualized by deep selective etching, which removes the gamma'-phase down to the gamma/gamma'-interface. Compared with transmission electron microscopy, the proposed method has important advantages: observation of large sample areas, no superposition of dislocations lying in different specimen depths, possibility of three-dimensional view of dislocation configurations, information about the dislocation mobility, reduced time for preparation and visualization. The method can be applied for multiphase materials where the interface is grooved by interfacial dislocations. KW - Dislocation structure KW - Interface KW - Nickel alloys KW - SEM PY - 2007 VL - 228 IS - 2 SP - 110 EP - 117 PB - The Royal Microscopical Society AN - OPUS4-38016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sitzman, S. D. A1 - Nolze, Gert A1 - Nowell, M. M. T1 - EBSD Pattern Quality and its Use in Evaluating Sample Surface Condition JF - Microscopy and Microanalysis N2 - Modern EBSD systems perform diffraction pattern “quality” (PQ) calculations, essentially measurements of the contrast of the brighter bands in the pattern above background, for every pattern analyzed. Since the calculations are independent of EBSD indexing, data are generated from all points on the analyzed sample surface, regardless of indexability or the state of the material beneath. EBSD maps generated from PQ data are like microstructurally sensitive SEM images, collected at EBSD speeds and grid resolutions, with contrast arising from phase density, crystal structure, crystallographic orientation, grain boundary location, near-surface plastic strain, coating density/thickness, and to some extent topography. Grain boundaries and other aspects of sample microstructure are readily revealed, so the PQ map is a very useful characterization tool in its own right, and serves as a reference for EBSD maps generated from indexing-derived data, such as orientation, grain boundary character, phase distribution and strain maps. KW - Electron backscatter diffraction KW - Sample preparation KW - Pattern quality PY - 2010 DO - https://doi.org/10.1017/S143192761005467X VL - 16 IS - Suppl. 2 SP - 698 EP - 699 PB - Microscopy Society of America AN - OPUS4-37997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, Aimo T1 - Progress in dynamic EBSD pattern simulation JF - Microscopy and Microanalysis N2 - EBSD is nowadays a common technique for the characterization of crystalline microstructures in scanning electron microscopy. The diffraction patterns are often interpreted by superimposing individual Kikuchi bands which are geometrically described by band edges derived from Braggs law. For the typically very simple crystal structures of technically applied materials, such a simplification of the Kikuchi pattern interpretation works sufficiently well, especially for orientation determinations as a main application of EBSD. The more complex crystal structures, however, are a challenge for EBSD indexing routines which in such cases often fail unpredictably. The use of only the intensities of single reflectors for a description of the Kikuchi band intensity and as a cut-off criterion for a pre-selection of the strongest bands are not satisfactory. Often the result will match too many phases, or there are certain deviations in the intensity prediction which must be adapted manually. This is already problematic if one is absolutely sure that the patterns are originating from the expected phase and it becomes a very questionable procedure for an unknown phase. KW - Electron backscatter diffraction KW - Dynamical simulation KW - Geometrical model KW - Kinematic approach KW - Intensity PY - 2010 DO - https://doi.org/10.1017/S1431927610063324 VL - 16 IS - Suppl. 2 SP - 62 EP - 63 PB - Microscopy Society of America AN - OPUS4-38000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abou-Ras, D. A1 - Gibmeier, J. A1 - Nolze, Gert A1 - Gholinia, A. A1 - Konijnenberg, P. T1 - On the capability of revealing the pseudosymmetry of the chalcopyrite-type crystal structure JF - Crystal Research and Technology N2 - The tetragonal crystal- structure type of chalcopyrites (chemical formula AIBIIICVI2) is a superstructure of sphalerite type. The c/a ratio differs generally from the ideal value 2, i.e., the crystal structure is pseudocubically distorted. For CuInSe2 and CuGaSe2 thin films, simulations demonstrate that it is theoretically possible to reveal the tetragonality in electron backscatter-diffraction (EBSD) patterns for CuGaSe2, whereas it may not be possible for CuInSe2. EBSD experiments on CuGaSe2 thin films using the ”Advanced Fit” band-detection method show that it is possible to extract accurate misorientation-angle distributions from the CuGaSe2 thin film. Pole figures revealing the texture of the CuGaSe2 thin film are shown, which agree well with X-ray texture measurements from the same layer. KW - Pseudosymmetry KW - Chalcopyrite KW - Electron backscatter diffraction KW - Pattern simulation KW - Pattern matching KW - Sphalerite PY - 2008 DO - https://doi.org/10.1002/crat.200711082 VL - 43 IS - 3 SP - 234 EP - 239 PB - WILEY-VCH AN - OPUS4-38003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wendt, U. A1 - Nolze, Gert T1 - Correlation between Crystal Orientation, Channeling Contrast and Topography during FIB Milling of Cu Studied by FIB, EBSD, SEM, and AFM JF - Praktische Metallographie N2 - We have studied the anisotropic milling of Cu with respect to the milling rate and the milling topography, as well. The background is twofold: i) anisotropic milling has to be taken into account during the preparation of TEM specimens and in the manufacturing of micro parts from crystalline materials, and ii) the orientation depending milling behaviour can be used to generate topographies with specific properties with respect to, for example, adsorption, wear, and corrosion. KW - FIB KW - AFM KW - Crystal orientation KW - SEM PY - 2007 VL - 44 IS - 5 SP - 236 EP - 238 PB - Carl Hanser Verlag AN - OPUS4-38026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wendt, U. A1 - Nolze, Gert A1 - Heyse, H. T1 - Effect of crystal orientation on imaging contrast and sputter results during focused ion beam milling of Cu studied by FIB, EBSD, SEM, and AFM JF - Microscopy and Microanalysis N2 - During focused ion beam microscopy (FIB) of crystalline materials imaging contrast and milling result are effected by orientation of the crystals with respect to the incident ion beam. This is due to the possibility of ion channeling along preferred crystal directions which effects the depth at which interaction between ions and specimen atoms takes place. As a result of channeling emission of ion induced secondary electrons (iiSE) and secondary ions (SI) as well as the sputter rate decreases. Theoretical channeling orientations and critical angles can be calculated. These effects have been studied quantitatively for polycrystalline recrystallized Cu as a typical model case. KW - Electron backscatter diffraction KW - FIB KW - AFM KW - Crystal orientation PY - 2006 DO - https://doi.org/10.1017/S1431927606061812 SN - 1431-9276 SN - 1435-8115 VL - 12 IS - Suppl. 2 SP - 1302 EP - 1303 AN - OPUS4-38027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Nolze, Gert T1 - Investigation of the competitive grain growth during solidification of single crystals of nickel-based superalloys JF - Crystallography Reports N2 - The competitive growth of columnar grains in a single-grain selector, which is used for directional solidification of single-crystal blades from nickel-based superalloys, has been investigated by electron backscattered diffraction and local X-ray diffraction analysis. It has been found that the competitive grain growth in a starter block is determined by the crystallographic factor: rapidly growing grains with the axial orientation close to the [001] direction dominate in this part of the casting. For the competitive grain growth in a helicoidal separator, the geometric factor (the position of a grain at the input of the separator) is also important. The results obtained suggest that an appropriate geometry of the single-grain selector was chosen. In addition, the distribution of the orientations of columnar grains obtained by electron backscattered diffraction, can be used for approximate estimation of the yield of suitable (i.e., with the deviation of the axial orientation from the [001] direction within a specified tolerance) single-crystal blades. KW - Electron backscatter diffraction KW - Single crystal KW - Growth competition KW - Nickel alloy PY - 2006 DO - https://doi.org/10.1134/S1063774506040298 SN - 1063-7745 SN - 1562-689X VL - 51 IS - 4 SP - 710 EP - 714 AN - OPUS4-38028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Glowacka, A. A1 - Nolze, Gert A1 - Swiatnicki, W. A. T1 - EBSD study of corrosion fatigue of austenitic-ferritic steel JF - Archives of Metallurgy and Materials N2 - Fatigue crack propagation investigations have been performed in austenitic-ferritic duplex stainless steel H22N5M3 in air and during hydrogen charging, using various frequencies of loading. Strong differences of crack propagation velocity depending on the test conditions were noticed. Lower frequency with applied hydrogen charging led to the huge increase of crack propagation velocity compared to the tests performed in air. To understand such a behaviour in each case and characterize crack mode, the samples were observed using electron back-scattered diffraction (EBSD). It was shown that in air, the fatigue crack propagation involved plastic deformation and the resulting cracks had ductile character. The presence of hydrogen led to more brittle mode of cracking. This effect was also connected with frequency of loading: lower frequency, which assured longer time for hydrogen-crack tip interaction, resulted in the highest crack propagation velocity and the brittle cracking mode with lower amount of plastic deformation. The performed observations indicated that the path of the crack went mostly transgranularly through both austenite and ferrite phases. Phase and grain boundaries were not the preferred paths for crack propagation. KW - Hydrogen KW - Embrittlement KW - Electron backscatter diffraction KW - Steel PY - 2006 SN - 1733-3490 SN - 0004-0770 SN - 0860-7052 VL - 51 IS - 1 SP - 7 EP - 10 AN - OPUS4-38029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Interphase boundary characterization in duplex steel and iron meteorites using EBSD technique JF - Archives of Metallurgy and Materials N2 - The properties of materials are mainly described by the orientation distribution of the crystalline phases in a material. Beside the so considered anisotropy also the grain as well as phase boundaries are of extreme importance for a whole string of properties, e.g. the strength of a material. On the example of the interface between fcc and bcc iron the discovered and derived models are discussed. Although the common models are based on the crystal lattice description, the atomic configuration on the interface is analysed. Since experimentally a wide spread of orientations data appears the consideration of the frequency distribution is proposed to find at least the main orientation relationship between fcc and bcc. High-indexed pole figures as well as the Euler subspace are introduced in order to increase the accuracy and to compare different measurements. For the sake of simplicity EBSD measurements on iron meteorites are used since they commonly consist of large fcc single crystals which transformed to a low and very specific number of bcc grains. In special cases the described procedure could also be used for steels. KW - Orientation relationships KW - Electron backscatter diffraction KW - Steel KW - Iron meteorites KW - Kurdjumov-Sachs KW - Nishiyama-Wassermann PY - 2006 SN - 1733-3490 SN - 0004-0770 SN - 0860-7052 VL - 51 IS - 1 SP - 15 EP - 22 AN - OPUS4-38030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Glenn, A.M. A1 - Hughes, A.E. A1 - Torpy, A. A1 - Nolze, Gert A1 - Birbilis, N. T1 - Defect density associated with constituent particles in AA2024-T3 and its role in corrosion JF - Surface and interface analysis N2 - Electron backscatter diffraction (EBSD) and scanning electron microscopy were combined to study the effect of residual defect density on corrosion initiation in aluminium alloy AA2024-T3. EBSD was used to determine the level of misorientation (MO), from pixel to pixel, within individual grains. The MO can be determined with respect to either the average orientation angle of the grain or with respect to the average orientation angle of the surrounding pixels (in this instance, a matrix of 7×7 surrounding pixels has been applied). Herein, the MO, determined using the surrounding pixels, was used as the means for the assessing the level of defect density within a grain. It was found that there was a noteworthy, but not definitive, correlation of MO with corrosion initiation after 1 min exposure to 0.1 M NaCl solution. Additionally, the S and θ-phase particles were also identified using EBSD, displaying a range of MO and therefore defect density. KW - Al-alloy KW - S-phase KW - EBSD KW - Corrosion KW - AA2024-T3 KW - Defect density PY - 2016 DO - https://doi.org/10.1002/sia.5813 SN - 0142-2421 SN - 1096-9918 VL - 48 IS - 8 (SI) SP - 780 EP - 788 PB - Wiley CY - Chichester AN - OPUS4-34476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, Aimo T1 - Crystallometric and projective properties of Kikuchi diffraction patterns JF - Journal of Applied Crystallography N2 - Kikuchi diffraction patterns can provide fundamental information about the lattice metric of a crystalline phase. In order to improve the possible precision and accuracy of lattice parameter determination from the features observed in Kikuchi patterns, some useful fundamental relationships of geometric crystal-lography are reviewed, which hold true independently of the actual crystal symmetry. The Kikuchi band positions and intersections and the Kikuchi band widths are highly interrelated, which is illustrated by the fact that all lattice plane trace positions of the crystal are predetermined by the definition of only four traces. If, additionally, the projection centre of the gnomonic projection is known, the lattice parameter ratios and the angles between the basis vectors are fixed. A further definition of one specific Kikuchi band width is sufficient to set the absolute sizes of all lattice parameters and to predict the widths of all Kikuchi bands. The mathematical properties of the gnomonic projection turn out to be central to an improved interpretation of Kikuchi pattern data, emphasizing the importance of the exact knowledge of the projection centre. KW - EBSD KW - Crystallography KW - Kikuchi patterns KW - Projective geometry PY - 2017 DO - https://doi.org/10.1107/S1600576716017477 SN - 1600-5767 VL - 50 IS - Part 1 SP - 102 EP - 119 PB - International Union of Crystallography AN - OPUS4-39061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wäsche, Rolf A1 - Brandt, Guido A1 - Ehrke, Roman A1 - Nolze, Gert A1 - Schmid, Thomas A1 - Sasaki, S. A1 - Woydt, Mathias T1 - Wear behaviour of alpha-alumina in hot steam at high contact pressure JF - Wear N2 - The work examines the wear behaviour of α-aluminium oxide by combining thermodynamic modelling with advanced wear testing as well as analytical methods to get a better understanding of this structural ceramic material wear behavior and its possible use in high temperature steam environment. KW - Aluminium oxide KW - Temperature KW - Hot steam KW - Diaspore KW - Ceramic KW - Wear PY - 2018 DO - https://doi.org/10.1016/j.wear.2018.02.012 SN - 0043-1648 SN - 1873-2577 VL - 404-405 SP - 22 EP - 30 PB - Elsevier B.V. AN - OPUS4-44449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Dietrich, D. A1 - Lampke, T. A1 - Del-Solar-Velarde, N. A1 - Nickel, D. A1 - Chapoulie, R. A1 - Castillo Butters, L.J. T1 - The potential of EBSD and EDS for ceramics investigations - Case studies on sherds of pre-Columbian pottery JF - archaeometry N2 - The work focuses on the potential of structural and chemical examinations by scanning electron microscopy based methods for archaeometric studies on ceramics. Achieved by a single preparation technique (polished block sections), the feasibility and benefits of electron backscatter diffraction are demonstrated as case studies using polychrome examples of pre-Columbian pottery (Wari, Moche and Cajamarca). Elemental and phase maps allow for separate consideration of clay and temper. Identification of mineral phases and intergrowths of temper particles provide information for clarifying clay procurement and firing techniques with respect to local versus non-local pottery to enlighten trade relations, technological transfer and shared heritage of pre-Columbian cultures. KW - SEM–EDS/EBSD KW - Pre-Columbian ceramics KW - Temper KW - Pseudobrookite KW - Titanite PY - 2017 VL - 60 IS - 3 SP - 489 EP - 501 AN - OPUS4-45096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Fedelich, Bernard A1 - Nolze, Gert A1 - Schriever, Sina A1 - Feldmann, Titus A1 - Farzik Ijaz, M. A1 - Viguier, B. A1 - Poquillon, D. A1 - Le Bouar, Y. A1 - Ruffini, A. A1 - Finel, A. T1 - Creep of single crystals of nickel-based superalloys at ultra-high homologous temperature JF - Metallurgical and materials transactions A N2 - The creep behavior of single crystals of the nickel-based superalloy CMSX-4 was investigated at 1288 °C, which is the temperature of the hot isostatic pressing treatment applied to this superalloy in the industry. It was found that at this super-solvus temperature, where no gammaPrime-strengthening occurs, the superalloy is very soft and rapidly deforms under stresses between 4 and 16 MPa. The creep resistance was found to be very anisotropic, e.g., the creep rate of [001] crystals was about 11 times higher than that of a [111] crystal. The specimens of different orientations also showed a very different necking behavior. The reduction of the cross-sectional area psi of [001] crystals reached nearly 100 pct, while for a [111] crystal psi = 62 pct. The EBSD analysis of deformed specimens showed that despite such a large local strain the [001] crystals did not recrystallize, while a less deformed [111] crystal totally recrystallized within the necking zone. The recrystallization degree was found to be correlated with deformation behavior as well as with dwell time at high temperature. From the analysis of the obtained results (creep anisotropy, stress dependence of the creep rate, traces of shear deformation, and TEM observations), it was concluded that the main strain contribution resulted from <01-1>{111} octahedral slip. T2 - 3rd European Conference on Superalloys (‘Eurosuperalloys 2018’) CY - Oxford, UK DA - 9.9.2018 KW - Single-crystal KW - Superalloy KW - Creep KW - Isostatic hot pressing (HIP) PY - 2018 DO - https://doi.org/10.1007/s11661-018-4729-6 SN - 1073-5623 SN - 1543-1940 VL - 49A IS - 9 SP - 3973 EP - 3987 PB - Springer Sciences & Business Media CY - New York, NY AN - OPUS4-45660 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Naresh-Kumar, G. A1 - Vilalta-Clemente, A. A1 - Jussila, H. A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Vespucci, S. A1 - Nagarajan, S. A1 - Wilkinson, A. J. A1 - Trager-Cowan, C. T1 - Quantitative imaging of anti-phase domains by polarity sensitive orientation mapping using electron backscatter diffraction JF - Scientific Reports N2 - Advanced structural characterisation techniques which are rapid to use, non-destructive and structurally definitive on the nanoscale are in demand, especially for a detailed understanding of extended-defects and their influence on the properties of materials. We have applied the electron backscatter diffraction (EBSD) technique in a scanning electron microscope to non-destructively characterise and quantify antiphase domains (APDs) in GaP thin films grown on different (001)Si substrates with different offcuts. We were able to image and quantify APDs by relating the asymmetrical intensity distributions observed in the EBSD patterns acquired experimentally and comparing the same with the dynamical electron diffraction simulations. Additionally mean angular error maps were also plotted using automated cross-correlation based approaches to image APDs. Samples grown on substrates with a 4° offcut from the [110] do not show any APDs, whereas samples grown on the exactly oriented substrates contain APDs. The procedures described in our work can be adopted for characterising a wide range of other material systems possessing non-centrosymmetric point groups. KW - Polarity KW - Semiconductor KW - Antiphase boundary PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-420167 SN - 2045-2322 VL - 7 SP - Article 10916, 1 EP - 10 AN - OPUS4-42016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Eliezer, D. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Novel approach to image hydrogen distribution and related phase transformation in duplex stainless steels at the sub-micron scale JF - International Journal of Hydrogen Energy N2 - The effect of electrochemical charging of hydrogen on the structure of a lean duplex stainless steel LDX 2101® (EN 1.4162, UNS S32101) was examined by both Time-of-Flight secondary ion mass spectrometry and electron back-scatter diffraction. The goal is to correlate hydrogen concentration and induced structural changes. Chemical and structural characterizations were done for the same region at the sample's surface with sub-micron spatial resolution. Regions of interest were varying in size between 50 × 50 μm and 100 × 100 μm. The results show a phase transformation of austenite to mainly a defect-rich BCC and scarcely a HCP phase. The phase transformation occurred in deuterium rich regions in the austenite. KW - Time-of-flight secondary ion mass spectrometry KW - ToF-SIMS KW - Electron backscatter diffraction KW - EBSD KW - Hydrogen-assisted cracking KW - Data fusion KW - Lean duplex stainless steel PY - 2017 DO - https://doi.org/10.1016/j.ijhydene.2017.08.016 SN - 0360-3199 VL - 42 IS - 39 SP - 25114 EP - 25120 AN - OPUS4-42022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, J. A1 - Farris, L. A1 - Nolze, Gert A1 - Reinsch, Stefan A1 - Cios, G. A1 - Tokarski, T. A1 - Thompson, S. T1 - Microstructure evolution in Inconel 718 produced by powder bed fusion additive manufacturing JF - Journal of manufacturing and materials processing N2 - Inconel 718 is a precipitation strengthened, nickel-based super alloy of interest for the Additive Manufacturing (AM) of low volume, complex parts to reduce production time and cost compared to conventional subtractive processes. The AM process involves repeated rapid melting, solidification and reheating, which exposes the material to non-equilibrium conditions that affect elemental segregation and the subsequent formation of solidification phases, either beneficial or detrimental. These variations are difficult to characterize due to the small length scale within the micron sized melt pool. To understand how the non-equilibrium conditions affect the initial solidification phases and their critical temperatures, a multi-length scale, multi modal approach has been taken to evaluate various methods for identifying the initial phases formed in the as-built Inconel 718 produced by laser-powder bed fusion (L-PBF) additive manufacturing (AM). Using a range of characterization tools from the bulk differential thermal analysis (DTA) and x-ray diffraction (XRD) to spatially resolved images using a variety of electron microscopy tools, a better understanding is obtained of how these minor phases can be properly identified regarding the amount and size, morphology and distribution. Using the most promising characterization techniques for investigation of the as-built specimens, those techniques were used to evaluate the specimens after various heat treatments. During the sequence of heat treatments, the initial as-built dendritic structures recrystallized into well-defined grains whose size was dependent on the temperature. Although the resulting strength was similar in all heat treated specimens, the elongation increased as the grain size was refined due to differences in the precipitated phase distribution and morphology. KW - Metal additive manufacturing KW - Inconel 718 KW - Heat treatment KW - Grain boundary precipitates KW - Laves phase PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542758 DO - https://doi.org/10.3390/jmmp6010020 SN - 2504-4494 VL - 6 IS - 1 SP - 1 EP - 20 PB - MDPI CY - Basel AN - OPUS4-54275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Svetlov, I. L. A1 - Epishin, A. I. A1 - Petrushin, N. V. A1 - Gerstein, G. A1 - Nolze, Gert A1 - Maier, H. J. T1 - Creep of Directionally Solidified Eutectics Ni/Ni3 Al–NbC under Thermal Cycling JF - Inorganic Materials: Applied research N2 - A nickel-based eutectic alloy with a γ/γ'-NbC structure was directionally solidified with a planar front. The specimens were tested for creep under sawtooth thermal cycling in the temperature range from 600 to 1100°C. It has been established that the lifetime under the conditions of thermal cycling is about five times shorter than it is predicted by the linear damage accumulation rule on the basis of results of isothermal creep tests. Faster creep under thermal cycling is caused by the rapid coarsening of the γ/γ' microstructure due to the periodic partial dissolution and reprecipitation of the γ' phase in heating and cooling half-cycles. KW - High temperature nickel-based eutectic alloys KW - γ/γ' matrix KW - Carbide phase NbC KW - In-situ composites KW - Creep under thermal cycling PY - 2022 DO - https://doi.org/10.1134/S2075113322040347 SN - 2075-1133 VL - 13 IS - 4 SP - 1099 EP - 1108 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-55163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A.I. A1 - Nolze, Gert A1 - Alymov, M.I. T1 - Pore Morphology in Single Crystals of a Nickel-Based Superalloy After Hot Isostatic Pressing JF - Metallurgical and Materials Transactions a-Physical Metallurgy and Materials Science N2 - The morphology of pores partially shrunk during a half-hour HIP at temperature of 1288 °C and pressure of 103 MPa has been investigated in nickel-based superalloy CMSX-4. The investigation resulted in the following findings: surrounding the shrinking pores by a c¢-shell (Ni3Al), faceting of the pores surface by {023} and {011} planes, and formation the submicroscopic satellite pores connected by channels with the neighboring larger pores. It is assumed that the formation of the c¢-shell around the pores and the faceting of the pore surface is due to diffusion processes occurring during pore shrinkage, and therefore these findings can be considered as arguments supporting the vacancy model of pore annihilation. The submicroscopic satellite pores are expected to be the result of dividing the casting pores of a complex initial shape during their shrinking. The connecting channels are probably required for the gas to escape from the rapidly shrinking small satellite pores into the slowly shrinking large pore. Thus, it is reasonable to assume that the casting pores may contain some amount of gas. KW - HIP KW - Superalloy KW - Porosity KW - Faceting KW - negative crystal growth PY - 2022 DO - https://doi.org/10.1007/s11661-022-06893-x SN - 1073-5623 SP - 1 EP - 9 PB - Springer Nature AN - OPUS4-56409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Treninkov, I. A. A1 - Petrushin, N. V. A1 - Epishin, A. I. A1 - Svetlov, I. L. A1 - Nolze, Gert A1 - Elyutin, E. S. T1 - Experimental Determination of Temperature Dependence of Structural–Phase Parameters of Nickel-Based Superalloy JF - Inorganic Materials: Applied Research N2 - The temperature dependences of the periods of the crystal lattices of the γ and γ' phases, their dimensional mismatch (misfit), and volume fraction of the γ' phase of an experimental single-crystal hightemperature nickel-based alloy have been determined by X-ray diffraction analysis in the temperature range of 18–1150°C. The temperature ranges in which intense changes in the structural and phase characteristics of the alloy under study take place have been determined. KW - X-ray diffraction analysis KW - High temperatures KW - Nickel-based superalloys KW - Single crystal KW - Crystal lattice period PY - 2022 DO - https://doi.org/10.1134/s2075113322010373 SN - 2075-1133 VL - 13 IS - 1 SP - 171 EP - 178 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-54466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Malakhov, A. A1 - Epishin, A. A1 - Denisov, I. A1 - Saikov, I. A1 - Nolze, Gert T1 - Morphology and Structure of Brass–Invar Weld Interface after Explosive Welding JF - Materials N2 - This paper presents the results of a study of the morphology and structure at the weld interface in a brass–Invar bimetal, which belongs to the class of so-called thermostatic bimetals, or thermobimetals. The structure of the brass–Invar weld interface was analyzed using optical microscopy and scanning electron microscopy (SEM), with the use of energy-dispersive X-ray (EDX) spectrometry and back-scattered electron diffraction (BSE) to identify the phases. The distribution of the crystallographic orientation of the grains at the weld interface was obtained using an e-Flash HR electron back-scatter diffraction (EBSD) detector and a forward-scatter detector (FSD). The results of the study indicated that the weld interface had the wavy structure typical of explosive welding. The wave crests and troughs showed the presence of melted zones consisting of a disordered Cu–Zn–Fe–Ni solid solution and undissolved Invar particles. The pattern quality map showed that the structure of brass and Invar after explosive welding consisted of grains that were strongly elongated towards the area of the highest intensive plastic flow. In addition, numerous deformation twins, dislocation accumulations and shear bands were observed. Thus, based on the results of this study, the mechanism of Cu–Zn–Fe–Ni structure formation can be proposed. KW - Explosive welding KW - Thermobimetal KW - Grain structure KW - Brass KW - Invar PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565964 DO - https://doi.org/10.3390/ma15238587 SN - 1996-1944 VL - 15 IS - 23 SP - 1 EP - 10 PB - MDPI AN - OPUS4-56596 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 JF - Inorganic Materials: Applied Research 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 - 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 JF - Journal of Microscopy 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 - 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 JF - Journal of Microscopy 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 - OPUS4-53584 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 JF - ФИЗИЧЕСКИЕ ОСНОВЫ МАТЕРИАЛОВЕДЕНИЯ JF - Materialovedenie 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 JF - Ultramicroscopy 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 - 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 JF - Advanced Engineering Materials 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 - 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 JF - Crystals 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 -