TY - JOUR A1 - Winkelmann, A. A1 - Nolze, Gert A1 - Cios, G. A1 - Tokarski, T. A1 - Bala, P. T1 - Refined Calibration Model for Improving the Orientation Precision of Electron Backscatter Diffraction Maps N2 - For the precise determination of orientations in polycrystalline materials, electron backscatter diffraction (EBSD) requires a consistent calibration of the diffraction geometry in the scanning electron microscope (SEM). In the present paper, the variation of the projection center for the Kikuchi diffraction patterns which are measured by EBSD is calibrated using a projective transformation model for the SEM beam scan positions on the sample. Based on a full pattern matching approach between simulated and experimental Kikuchi patterns, individual projection center estimates are determined on a subgrid of the EBSD map, from which least-square fits to affine and projective transformations can be obtained. Reference measurements on single-crystalline silicon are used to quantify the orientation errors which result from different calibration models for the variation of the projection center. KW - Scanning electron microscopy KW - Electron backscatter diffraction KW - Kikuchi diffraction KW - Projection center KW - Orientation precision PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509342 DO - https://doi.org/10.3390/ma13122816 VL - 13 IS - 12 SP - 2816 PB - MDPI AN - OPUS4-50934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Cios, G. A1 - Winkelmann, A. T1 - Manual measurement of angles in backscattered and transmission Kikuchi diffraction patterns N2 - A historical tool for crystallographic analysis is provided by the Hilton net, which can be used for manually surveying the crystal lattice as it is manifested by the Kikuchi bands in a gnomonic projection. For a quantitative analysis using the Hilton net, the projection centre as the relative position of the signal source with respect to the detector plane needs to be known. Interplanar angles are accessible with a precision and accuracy which is estimated to be ≤0.3o. Angles between any directions, e.g. zone axes, are directly readable. Finally, for the rare case of an unknown projection-centre position, its determination is demonstrated by adapting an old approach developed for photogrammetric applications. It requires the indexing of four zone axes [uvw]i in a backscattered Kikuchi diffraction pattern of a known phase collected under comparable geometric conditions. KW - Electron backscatter diffraction KW - EBSD KW - Angle measurement KW - Gnomonic projections KW - Kikuchi patterns PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507625 DO - https://doi.org/10.1107/S1600576720000692 VL - 53 SP - 435 EP - 443 AN - OPUS4-50762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, A. A1 - Cios, G. A1 - Tokarski, T. A1 - Nolze, Gert A1 - Hielscher, R. A1 - Koziel, T. T1 - EBSD orientation analysis based on experimental Kikuchi reference patterns N2 - Orientation determination does not necessarily require complete knowledge of the local atomic arrangement in a crystalline phase. We present a method for microstructural phase discrimination and orientation analysis of phases for which there is only limited crystallographic information available. In this method, experimental Kikuchi diffraction patterns are utilized to generate a self-consistent master reference for use in the technique of Electron Backscatter Diffraction (EBSD). The experimentally derived master data serves as an application-specific reference in EBSD pattern matching approaches. As application examples, we map the locally varying orientations in samples of icosahedral quasicrystals observed in a Ti40Zr40Ni20 alloy, and we analyse AlNiCo decagonal quasicrystals. KW - EBSD KW - Quasicrystal KW - Crystal orientation KW - Pattern matching PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507611 DO - https://doi.org/10.1016/j.actamat.2020.01.053 VL - 188 SP - 376 EP - 385 PB - Elsevier Ltd. AN - OPUS4-50761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cios, G. A1 - Nolze, Gert A1 - Winkelmann, A. A1 - Tokarski, T. A1 - Hielscher, R. A1 - Strzalka, R. A1 - Buganski, I. A1 - Wolny, J. A1 - Bala, P. T1 - Approximant-based orientation determination of quasicrystals using electron backscatter diffraction N2 - Orientation mapping of quasicrystalline materials is demonstrated using crystalline approximant structures in the technique of electron backscatter diffraction (EBSD). The approximant-based orientations are symmetrised according to the rotational point group of the quasicrystal, including the visualization of orientation maps using proper colour keys for quasicrystal symmetries. Alternatively, approximant-based orientation data can also be treated using pseudosymmetry post-processing options in the EBSD system software, which enables basic grain size estimations. Approximant-based orientation analyses are demonstrated for icosahedral and decagonal quasicrystals. KW - EBSD KW - Quasicrystal KW - Approximant KW - Chrystal orientation KW - Data processing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514221 DO - https://doi.org/10.1016/j.ultramic.2020.113093 VL - 218 SP - 113093 PB - Elsevier B.V. AN - OPUS4-51422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koclega, Damian A1 - Radziszewska, A. A1 - Dymek, S. A1 - Morgiel, J. A1 - Maj, L. A1 - Kranzmann, Axel T1 - Improvement of Corrosion Resistance of 13CrMo4-5 Steel by Ni-Based Laser Cladding Coatings N2 - The 13CrMo4-5 ferritic steel is commonly used in power plants, due to its favorable mechanical properties. According to EN 10028-2, this steel can be used at temperatures up to 570°C because of its creep behavior. The inefficient corrosion resistance limits the application of this steel to lower temperatures depending on the gas temperature and slag formation. Therefore, the application of a highly resistant Ni-based coating is proposed to extend the corrosion resistance of elements made of ferritic steel. The corrosion test was performed in an environment containing a mixture of gases, like O2, COx, and SOx, and deposited ashes with elements, e.g., Na, Cl, Ca, Si, C, Fe, and Al. The exposure time was, respectively, 240 h, 1000 h and 4500 h at a temperature of 600°C. The oxide scale formed on the 13CrMo4-5 steel was significantly thicker than on the IN686 coating. The microstructure and chemical and phase compositions of the oxide scale were investigated using light optical microscopy together with scanning and transmission electron microscopy techniques. Energy dispersive x-ray analyses were performed when appropriate. KW - Aggressive environments KW - Corrosion resistance KW - High - temperature KW - Inconel 686 KW - Laser cladding PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514289 DO - https://doi.org/10.1007/s11665-020-04867-x SN - 1059-9495 VL - 29 IS - 6 SP - 3702 EP - 3713 PB - Springer AN - OPUS4-51428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Lattice parameter determination with EBSD. Is that possible? N2 - CALM is software for determining the Bravais lattice type and the resulting lattice parameters from a single Kikuchi pattern. It requires the definition of 4 bands and a single bandwidth from which all other band positions as well as bandwidths are derived. For band detection, it uses the Funk transform, which allows detection of twice as many bands as usual. CALM works for any symmetry and requires low-noise patterns of at least 320x240 pixels. The resulting errors are <2% even for such small patterns, assuming good quality. The relative errors are <0.5%. However, this requires a projection centre position best derived from a sample of a cubic phase in CALM. However, this must have been recorded under identical conditions. Hundreds of Kikuchi patterns of phases with different symmetries were examined. T2 - Institutskolloquium Kassel CY - Online meeting DA - 30.10.2020 KW - Phasenidentifikation KW - EBSD KW - Gitterkonstanten PY - 2020 AN - OPUS4-51813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Focused ion beam techniques beyond the ordinary - Methodological developments within ADVENT N2 - This poster presents the focused ion beam preparation methodologies developed within the framework of the EU funded EURAMET project ADVENT (Advanced Energy-Saving Technology). It summarises the key breakthroughs achieved for various in situ investigation techniques, e.g. in situ experiments at the Synchrotron facility BESSY II (IR-SNOM and XRS), TEM and SMM instrumentation. The created experimental devices from diverse thin-film semiconductor materials paved the way to dynamic structural studies bearing the potential to determine nanoscale correlations between strain and electric fields and, moreover, for the fundamental development of new in situ capabilities. N2 - Dieses Poster zeigt die FIB Präparationstechniquen, die im Rahmen des EU-finanzierten EURAMET-Projekts ADVENT (Advanced Energy Saving Technology) entwickelt wurden. Es fasst die wichtigsten Errungenschaften zusammen, die für verschiedene in situ Untersuchungstechniken erzielt wurden, z.B. situ-Experimente in dem Synchrotronring BESSY II (IR-SNOM und XRS), in situ TEM Experimente und für die SMM Technik. Die experimentellen Probenstrukturen, die aus verschiedenen Dünnschicht-Halbleitermaterialien erzeugt wurden, ebneten den Weg für dynamische Strukturstudien, die das Potenzial haben, nanoskalige Korrelationen zwischen Dehnung und elektrischen Feldern zu bestimmen und darüber hinaus neue in situ Messmethoden zu entwickeln. T2 - Final Meeting CY - Online Meeting DA - 30.06.2020 KW - FIB KW - Sample preparation KW - In situ KW - TEM KW - AFM PY - 2020 AN - OPUS4-51606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Innovations- Plattform Material Digital N2 - Mit der Initiative MaterialDigital fördert das BMBF seit dem letzten Jahr ein wichtiges Instrument zur Digitalisierung der Materialwissenschaft und Werkstofftechnik in Deutschland. In der ersten Phase dieser Initiative wird seit Juli 2019 die Plattform MaterialDigital von einem Konsortium aufgestellt. Ziel dieser Plattform ist der Aufbau eines virtuellen Materialdatenraums, um zusammen mit allen Interessenten die Systematisierung des Umgangs mit Werkstoffdaten voranzutreiben. In einer zweiten Phase werden akademische F&E-Projekte voraussichtlich Anfang 2021 gefördert. In jedem dieser Projekte wird an einer konkreten Fragestellung das Themenfeld „Digitalisierung der Materialwissenschaft und Werkstofftechnik“ adressiert und multidisziplinär bearbeitet. In einer dritten Phase werden im Rahmen industriegeführter vorwettbewerblicher Verbundprojekte mit der gleichen Zielsetzung gefördert. T2 - Workshop - “Datenmanagement in der Additiven Fertigung” CY - Online meeting DA - 27.10.2020 KW - Digitalisierung KW - Plattform Material Digital KW - Virtueller Materialdatenraum KW - Vernetzung KW - Ontologien PY - 2020 AN - OPUS4-51609 LA - deu 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 - OPUS4-53584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duarte, Larissa A1 - Andrade, Ana Carolina A1 - Bettge, Dirk T1 - Fractographic Analysis of Fatigue Striations Formation under different Microstructures and Loading Conditions T1 - Fraktographische Untersuchung der Bildung von Schwingstreifen bei unterschiedlichen Gefügezuständen und Belastungsbedingungen N2 - Fatigue failure of a component can occur at service loads considerably lower than the yield strength of the material. Under fatigue loading condition, the material in the vicinity of the tip of a propagating crack repeatedly deforms plastically, leaving microscopic marks on the crack surface, commonly known as fatigue striations. Counting and measuring fatigue striations is a method in estimating the number of loading cycles a component went through until fracture. Some studies suggest a one-to-one relation between the number of fatigue striations and the number of load cycles, but this relation is still debatable, given that there are many factors influencing the formation of those striations. The main purpose of this work is to analyze the influence of microstructure and mechanical strength on the formation of fatigue striations in structural steels, in order to understand how these material properties are related to the fatigue crack behavior. For such, standard Charpy-V samples were subjected to hardness, fatigue and impact testing. Metallography was performed to characterize the microstructure, and a fractographic analysis by using optical and scanning electron microscopy was carried out to investigate the fracture surface. This study shows that steels with higher ductility have a closer one-to-one relation than those with a higher tensile strength. Above a certain level of tensile strength, fatigue striations do form rarely or completely disappear. N2 - Weit unterhalb der Streckfestigkeit des Werkstoffs kann es durch Schwingbruch zum Bauteilversagen kommen. Unter Schwingbeanspruchung wird der Werkstoff in der Nähe der Spitze eines sich ausbreitenden Risses wiederholt plastisch verformt. Dabei entstehen allgemein als Schwingstreifen bekannte mikroskopische Spuren. Das Zählen und Vermessen von Schwingstreifen ist ein Verfahren zum Schätzen der Anzahl von Belastungszyklen, denen ein Bauteil bis zum Bruch ausgesetzt war. Einige Studien legen hier eine 1 : 1-Beziehung zwischen der Anzahl von Schwingstreifen und der Anzahl von Lastspielen nahe. Dies erscheint angesichts der zahlreichen, die Bildung solcher Streifen beeinflussenden Faktoren allerdings fraglich. Hauptziel dieser Arbeit ist die Untersuchung der Auswirkungen des Gefüges und der mechanischen Festigkeit auf die Bildung von Schwingstreifen in Baustählen, um Zusammenhänge zwischen diesen Werkstoffeigenschaften und dem Schwingbruchverhalten verstehen zu können. Dafür wurden an Standard-Charpy-V-Proben Härte- sowie Schwing- und Schlagprüfungen durchgeführt. Zur Gefügecharakterisierung wurden die Proben metallographisch untersucht. Die Bruchfläche wurde zur Analyse fraktographisch licht- und rasterelektronenmikroskopisch untersucht. Die vorliegende Untersuchung zeigt dabei auf, dass Stähle mit einer höheren Duktilität näher an eine solche 1 : 1-Beziehung herankommen als solche mit einer höheren Zugfestigkeit. Oberhalb einer bestimmten Zugfestigkeit bilden sich selten oder gar keine Schwingstreifen. KW - Schwingstreifen KW - Fatigue striations PY - 2020 DO - https://doi.org/10.3139/147.110668 VL - 57 IS - 12 SP - 869 EP - 886 PB - Carl Hanser Verlag CY - München AN - OPUS4-51952 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmies, Lennart A1 - Sonntag, U. T1 - Quantitative Fraktographie unter Verwendung klassischer Verfahren, Topographie-Daten und Deep-Learning N2 - Die Analyse von Bruchflächen wird in der Schadensanalyse meist auf der Basis von Erfahrungswissen vorgenommen, welches aus vorliegenden Untersuchungen, eigenen Vergleichsversuchen und aus der Literatur stammt. Durch Vergleiche mit bereits vorliegenden Bildern werden qualitativ Bruchmechanismen ermittelt. Grundlage sind zumeist zweidimensionale Bilder aus licht- und elektronenoptischen Verfahren. Quantitative Aussagen beziehen sich bislang beispielsweise auf makroskopische Anteile von Bruchmechanismen oder die Ausmessung von Schwingstreifen. In jüngerer Zeit gibt es vermehrt Ansätze, Computer-Algorithmen einzusetzen, die in der Lage sind, unterschiedlich strukturierte Bruchmerkmale zu finden und zu klassifizieren. Im hier vorgestellten IGF-Vorhaben „iFrakto“, IGF Vorhaben Nr.: 21477 N, werden licht- und elektronen-optisch Topographie-Bilder erzeugt und die gewonnenen 3D-Informationen zusammen mit den klassischen 2D-Bildern ausgewertet. Analytische Algorithmen und Machine Learning werden eingesetzt, um Bruchmerkmale zu analysieren, zu bewerten und mit Informationen aus einer fraktographischen Datenbank zu verknüpfen. Ziel ist die Bereitstellung von Software zur Unterstützung der Fraktographie in der Schadensanalyse. In diesem Beitrag werden erste Ergebnisse des Vorhabens vorgestellt. T2 - 55. Metallographie-Tagung CY - Online meeting DA - 29.9.2021 KW - Fraktographie KW - Machine Learning KW - Datenbank KW - REM KW - Topographie PY - 2021 AN - OPUS4-53491 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Balzer, B T1 - „Auffällige große Streifen“ im Schwingbruch N2 - Die „auffälligen großen Streifen“ sind von echten Schwingstreifen nur sehr schwer zu trennen, weil sie parallel zu den Schwingstreifen verlaufen und meistens ebenfalls nicht sehr groß sind. Die im Labor getesteten Proben zeigten, dass diese großen Streifen zusammen mit Verreibungen auftraten und „tire tracks“ („Reifenspuren“) verursachten. Dies wurde durch eine hochauflösende REM-Untersuchung bestätigt, die „tire tracks“ auf den „großen Streifen“ zeigte. Ein weiterer Hinweis ist die Änderung des R-Werts von -1 auf 0,1, was zu einer Bruchfläche ohne große Streifen und „tire tracks“ führt. T2 - Treffen der AG Fraktographie im Gemeinschaftsausschuss Rasterelektronenmikroskopie in der Materialprüfung CY - Online meeting DA - 19.11.2021 KW - Fractography KW - Fracture surface KW - SEM KW - REM KW - Fraktographie KW - Schwingstreifen KW - Fatigue PY - 2021 UR - https://dgm.inventum.de/widget/preview/45d8c33d-622b-43e2-8459-ba783394a723/611d133ebdac0611d133ebdac1 AN - OPUS4-53796 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, A. T1 - About the reliability of EBSD measurements: Data enhancement N2 - An extensive set of information about the diffracting volume is carried by EBSD patterns: the crystal lattice, the reciprocal lattice, the crystal structure, the crystal symmetry, the mean periodic number of the diffracting phase, the source point from where it has been projected (projection centre), the crystal orientation, the sample topography (local tilt), the (preparation) quality of defect density of the crystal, and possible pattern overlaps. Some of this information is used regularly in conventional EBSD analyses software while others are still waiting for a more widespread application. Despite the wealth of information available, the accuracy and precision of the data that are presently extracted from conventional EBSD patterns are often well below the actual physical limits. Using a selection of example applications, we will demonstrate the gain in angular resolution possible using relatively low-resolution patterns of approximately 20k pixels in combination with pattern matching (PM) approaches. In this way, fine details in a microstructure can be revealed which would otherwise be hidden in the orientation noise. KW - EBSD KW - Orientation precision KW - Disorientation KW - Grain boundary KW - Phase transformation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521618 DO - https://doi.org/10.1088/1757-899X/891/1/012018 VL - 891 SP - 012018 PB - IOP Science AN - OPUS4-52161 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 - CONF A1 - Nolze, Gert T1 - CALM down: Identifying unknown phases N2 - CALM is software for determining the Bravais lattice type and the resulting lattice parameters from a single Kikuchi pattern. It requires the definition of 4 bands and a single bandwidth from which all other band positions as well as bandwidths are derived. For band detection, it uses the Funk transform, which allows detection of twice as many bands as usual. CALM works for any symmetry and requires low-noise patterns of at least 320x240 pixels. The resulting errors are <2% even for such small patterns, assuming good quality. The relative errors are <0.5%. However, this requires a projection centre position best derived from a sample of a cubic phase in CALM. However, this must have been recorded under identical conditions. Hundreds of Kikuchi patterns of phases with different symmetries were examined. T2 - Chemnitz MTEX Workshop 2021 CY - Online meeting DA - 08.03.2021 KW - EBSD KW - Gitterkonstanten KW - Phasenidentifikation PY - 2021 AN - OPUS4-52345 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 - CONF A1 - Sandoval Saldias, Janina T1 - Chloridische Salzschmelzen als latente Wärmespeicher N2 - Latente Wärmspeicher auf der Basis von NaCl-KCl-MgCl2 Mischungen stellen eine kostengünstige Option für die Energiespeicherung von Prozesswärme dar. Der Beitrag gibt einen Überblick über die materialwissenschaftlichen Herausforderungen im System Salz-Legierung, welche gelöst werden müssen, um diese Speichertechnologie industriell zu etablieren. T2 - DMG Sektionstreffen Angewandte Mineralogie und Kristallographie CY - Online Meeting DA - 25.02.2021 KW - Wärmespeicher KW - Korrosion KW - Salzschmelzen PY - 2021 AN - OPUS4-52234 LA - deu 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 - CONF A1 - Bettge, Dirk A1 - Le, Quynh-Hoa T1 - Entwicklung einer fraktographischen Symbolik N2 - Bei der Untersuchung von Bruchflächen werden zunächst Beobachtungen gemacht, d.h. makroskopische und mikroskopische Merkmale analysiert und in Bildern dokumentiert. Im zweiten Schritt werden anhand der gefundenen Merkmale Rissverlauf und Bruchmechanismen ermittelt. Abschließend sollen diese Ergebnisse in einem Bericht oder Gutachten zusammengefasst werden. Hierbei ist eine skizzenhafte Darstellung der fraktographischen Befunde hilfreich für das Verständnis des Lesers. Ein vorgefertigter fraktographischer Symbolsatz würde dies erheblich vereinfachen. Skizzen von fraktographischen Befunden sind in der Literatur recht häufig zu finden, z.B. in der VDI 3822 oder dem ASM Handbook Fractography, allerdings gibt es hierzu keine umfassende Systematik, wie sie z.B. aus der Meteorologie (Wetterkarten), Geographie (Landkarten, Seekarten) oder Geologie (Bodenkarten) seit langer Zeit bekannt sind. Deshalb wird hier der Versuch unternommen, einen Symbolsatz zu entwickeln und zur Verfügung zu stellen, mit dessen Hilfe fraktographische Befunde in eindeutiger und übersichtlicher Weise veranschaulicht werden können. Der fraktographische Symbolsatz ("Fracto Graphics") befindet sich in Entwicklung, ist offen zur Diskussion sowie für Verbesserungen. T2 - 55. Metallographie-Tagung CY - Online meeting DA - 29.9.2021 KW - Fraktographie KW - Symbolik KW - Schadensanalyse PY - 2021 AN - OPUS4-53433 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Wolf, Marcus A1 - Kranzmann, Axel T1 - Corrosion and corrosion fatigue of steels in downhole CCS environment - A summary N2 - Static immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4, and X5CrNiCuNb16-4 at T = 60 °C and ambient pressure, as well as p = 100 bar were performed for 700–8000 h in a CO₂-saturated synthetic aquifer environment similar to CCS sites in the Northern German Basin (NGB). Corrosion rates at 100 bar are generally lower than at ambient pressure. The main corrosion products are FeCO₃ and FeOOH with surface and local corrosion phenomena directly related to the alloy composition and microstructure. The appropriate heat treatment enhances corrosion resistance. The lifetime reduction of X46Cr13, X5CrNiCuNb16-4, and duplex stainless steel X2CrNiMoN22-5-3 in a CCS environment is demonstrated in the in situ corrosion fatigue CF experiments (axial push-pull and rotation bending load, 60 °C, brine: Stuttgart Aquifer and NGB, flowing CO₂: 30 L/h, +/- applied potential). Insulating the test setup is necessary to gain reliable data. S-N plots, micrographic-, phase-, fractographic-, and surface analysis prove that the life expectancy of X2CrNiMoN22-5-3 in the axial cyclic load to failure is clearly related to the surface finish, applied stress amplitude, and stress mode. The horizontal grain attack within corrosion pit cavities, multiple fatigue cracks, and preferable deterioration of austenitic phase mainly cause fatigue failure. The CF life range increases significantly when a protective potential is applied. KW - Steel KW - High alloyed steel KW - Corrosion KW - Corrosion fatigue KW - Carbon capture and storage PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531391 DO - https://doi.org/10.3390/pr9040594 SN - 2227-9717 VL - 9 IS - 4 SP - 1 EP - 33 PB - MDPI CY - Basel AN - OPUS4-53139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja A1 - Kranzmann, Axel T1 - Effects of saline aquifer water on the corrosion behaviour of martensitic stainless steels during exposure to CO2 environment N2 - Immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4 and X5CrNiCuNb16-4 at T=60 °C and ambient pressure and p=100 bar were performed for 700 h - 8000 h in a CO₂-saturated synthetic aquifer environment similar to CCS-sites in the Northern-German-Basin. Main corrosion products are FeCO₃ and FeOOH. Highest surface corrosion rates at ambient pressure are 0.8 mm/year for 42CrMo4 and lowest 0.01 mm/year for X5CrNiCuNb16-4. Corrosion rates at 100 bar (max. 0.01 mm/year for 42CrMo4, X20Cr13, X46Cr13) are generally lower than at ambient pressure (<0.01 mm/year for X35CrMo4, X5CrNiCuNb16-4). Heat treatment to martensitic microstructure offers good corrosion resistance. T2 - 15th International Conference on Greenhouse Gas Control Technologies, GHGT-15 CY - Abu Dhabi, United Arab Emirates DA - 15.03.2021 KW - CCS KW - Corrosion KW - High alloyed steels PY - 2021 DO - https://doi.org/10.2139/ssrn.3812248 SP - 1 EP - 12 PB - SSRN CY - Rochester, NY AN - OPUS4-53140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja A1 - Wolf, Marcus A1 - Kranzmann, Axel T1 - Evaluating corrosion and corrosion fatigue behavior via laboratory testing techniques in highly corrosive CCS-environment N2 - In CCS environment (carbon capture and storage) pipes are loaded statically and/or cyclically and at the same time exposed constantly to the highly corrosive hot thermal water. Experimental procedures such as ambient pressure immersions tests, in-situ corrosion fatigue experiments using a flexibly designed corrosion chamber at ambient pressure and a specially designed corrosion chamber at high pressure. Experimental set-ups for push/pull and rotation bending load are introduced. The corrosion behavior and lifetime reduction of high alloyed steels (X46Cr13, 1.4043), (X5CrNiCuNb16-4, 1.4542) and (X2CrNiMoN22-5-3, 1.4462) is demonstrated (T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 l/h, CO₂). T2 - 15th International Conference on Greenhouse Gas Control Technologies, GHGT-15 CY - Abu Dhabi, United Arab Emirates DA - 15.03.2021 KW - Steel KW - Supercritical CO2 KW - Pipeline KW - Corrosion KW - CO2-storage PY - 2021 DO - https://doi.org/10.2139/ssrn.3812193 SP - 1 EP - 11 PB - SSRN CY - Rochester, NY AN - OPUS4-53142 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 - CONF A1 - Werner, Tiago T1 - Comparison of the fatigue behavior of wrought and additively manufactured AISI 316L N2 - Additively Manufactured (AM) parts are still far from being used in safety-relevant applications, mainly due to a lack of understanding of the feedstock-process-propertiesperformance relationship. This work aims at providing a characterization of the fatigue behavior of the additively manufactured AISI 316L austenitic stainless steel and a direct comparison with the fatigue performance of the wrought steel. A set of specimens has been produced by laser powder bed fusion (L-PBF) and a second set of specimens has been machined out of hot-rolled plates. The L-PBF material shows a higher fatigue limit and better finite life performance compared to the wrought material, accompanied by an extensive amount of cyclic softening. T2 - Fatigue Design 2021 CY - Online meeting DA - 17.11.2021 KW - Additive Manufacturing KW - AM KW - 316L KW - Fatigue KW - High Cycle Fatigue KW - Low Cycle Fatigue PY - 2021 AN - OPUS4-53780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja T1 - Vom Blended Learning zum Full Online – so einfach geht es nicht – Praxiserfahrungen zum Einsatz von Lehrfilmen N2 - Mit Beginn der Covid-19 Pandemie und dem damit verbundenen ausschließlichen Lehren im online-Format war die Hoffnung verbunden ein Blended Learning Lehrformat für die Studieeingangsphase ohne viel konzeptionelle Änderungen übertragen zu können. Der Kurs Werkstofftechnik als Grundlagenfach für den Maschinenbau baut sich auf inverted classroom Lehrszenarien auf, deren Lerngrundlage hierfür eigens produzierte und auf das Lernziel abgestimmte Lehrfilme und Lightboard-Vorlesungen darstellen. Im Kontext der Studieneingangsphase bieten audiovisuell stimulierende Lehrfilme umfassende Lernmedien, wenn sie analog der Lerninhalte einem technischen und didaktischen Qualitätsanspruch genügen. In der Praxis des SS2020 und WS2020/21 hat sich gezeigt, dass die Moderation und Durchführung eines online-Kurses sich deutlich von dem eins blended learning-Kurses unterscheidet. Um denselben Lernerfolg bei Studierenden zu erzielen, müs-sen Anforderungen viel genauer und detaillierter verfasst werden, Studierende enger und persönlicher begleitet werden und Lehrfilme und Lernmedien in einen Gesamtzusammenhang gestellt werden. Im Folgenden werden aus persönlicher Erfahrung heraus niederschwellige, zum Teil ungewöhnliche praktische Erfahrungen zur erfolgreichen Umsetzung von Lehrfilm-basierten inverted classroom Lehrszenarien zusammengefasst und im Hinblick auf die online-Lehre bewertet. T2 - 19. Fachtagung Bildungstechnologien (DELFI) CY - Bonn, Germany DA - 13.09.2021 KW - Inverted classroom KW - Lehrfilm KW - Lehrfilmformate KW - Online KW - Covid-19 PY - 2021 SP - 289 EP - 295 AN - OPUS4-54154 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja T1 - Improving Learning Outcome for GSL (German as a Second Language) Students in a Blended Learning Cumulative Assessment Material Science Course N2 - First year students especially with migration background and language deficiencies rate material science in mechanical engineering as one of the fundamental courses with high work load and necessity of language skills due to the descriptive nature of the course. Therefore a blended learning course structure using based on inverted classroom teaching scenarios was established. Heart of the self-study period are visualizing peer-to-peer lecture films supported by micro-lectures along with various online teaching materials. Although students with migration background generally scored lower in tests due to the lack of language skills improved learning outcomes are demonstrated in high quality class discussions and in overall understanding. This paper introduces the learning structure and graded activities, evaluates the course and compares results of native German-speaking students to those of students with migration background. KW - Portfolio KW - Diversity KW - Blended learning KW - Inverted classroom KW - Lecture films PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-541557 DO - https://doi.org/10.17706/ijeeee.2021.11.3.93-100 SN - 2010-3654 VL - 11 IS - 3 SP - 93 EP - 100 AN - OPUS4-54155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja T1 - How flipped classroom teaching methods in first year studying succeed N2 - Flipping the classroom is a method to let students study on their own and then take time to discuss their questions and do extended hands-on lectures or exercises in class – or in the case of the covid-19 pandemic during plenary online sessions. First year mechanical engineering students use different teaching materials (mainly lecture videos, lightboard videos and micromodule lectures) to study from a distance and comprehend the principle underlying science in theory. Then the online plenary lectures offer the opportunity to apply their knowledge and transfer different scientific aspects of the course to get the bigger picture. Exercises, worked solutions, selfassessed tests and peer-instruction during present time help students to check on their learning progress. However, the self-study periods and (online) plenary sessions need to be guided carefully. To meet the course learning outcome and overcome the diversity of a first year class various practical leads have to be fulfilled to turn flipped classroom teaching into success. T2 - 7th International Conference on Higher Education Advances (HEAd’21) CY - Valencia, Spain DA - 20.06.2021 KW - Inverted classroom KW - Flipped classroom KW - Online teaching KW - Lecture videos KW - First year students PY - 2021 DO - https://doi.org/10.4995/HEAd21.2021.12792 SP - 1211 EP - 1219 AN - OPUS4-54156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Wolf, M. A1 - Kranzmann, Axel T1 - Corrosion and Corrosion Fatigue of Steels in Downhole CCS Environment—A Summary N2 - Static immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4, and X5CrNiCuNb16-4 at T = 60 °C and ambient pressure, as well as p = 100 bar were performed for 700–8000 h in a CO2-saturated synthetic aquifer environment similar to CCS sites in the Northern German Basin (NGB). Corrosion rates at 100 bar are generally lower than at ambient pressure. The main corrosion products are FeCO3 and FeOOH with surface and local corrosion phenomena directly related to the alloy composition and microstructure. The appropriate heat treatment enhances corrosion resistance. The lifetime reduction of X46Cr13, X5CrNiCuNb16-4, and duplex stainless steel X2CrNiMoN22-5-3 in a CCS environment is demonstrated in the in situ corrosion fatigue CF experiments (axial push-pull and rotation bending load, 60 °C, brine: Stuttgart Aquifer and NGB, flowing CO2: 30 L/h, +/− applied potential). Insulating the test setup is necessary to gain reliable data. S-N plots, micrographic-, phase-, fractographic-, and surface analysis prove that the life expectancy of X2CrNiMoN22-5-3 in the axial cyclic load to failure is clearly related to the surface finish, applied stress amplitude, and stress mode. The horizontal grain attack within corrosion pit cavities, multiple fatigue cracks, and preferable deterioration of austenitic phase mainly cause fatigue failure. The CF life range increases significantly when a protective potential is applied. KW - Steel KW - High alloyed steel KW - Corrosion fatigue KW - Cabon capture and storage KW - CCS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-541626 DO - https://doi.org/10.3390/pr9040594 VL - 9 IS - 4 SP - 594 PB - MDPI AN - OPUS4-54162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, A. A1 - Kranzmann, Axel T1 - Understanding the Anomalous Corrosion Behaviour of 17% Chromium Martensitic Stainless Steel in Laboratory CCS-Environment—A Descriptive Approach N2 - To mitigate carbon dioxide emissions CO2 is compressed and sequestrated into deep geological layers (Carbon Capture and Storage CCS). The corrosion of injection pipe steels is induced when the metal is in contact with CO2 and at the same time the geological saline formation water. Stainless steels X35CrMo17 and X5CrNiCuNb16-4 with approximately 17% Cr show potential as injection pipes to engineer the Northern German Basin geological onshore CCS-site. Static laboratory experiments (T = 60 ◦C, p = 100 bar, 700–8000 h exposure time, aquifer water, CO2-flow rate of 9 L/h) were conducted to evaluate corrosion kinetics. The anomalous surface corrosion phenomena were found to be independent of heat treatment prior to exposure. The corrosion process is described as a function of the atmosphere and diffusion process of ionic species to explain the precipitation mechanism and better estimate the reliability of these particular steels in a downhole CCS environment. KW - Corrosion KW - Steel KW - High alloyed steel KW - Corrosion mechanism KW - CCS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545700 DO - https://doi.org/10.3390/cleantechnol4020014 VL - 4 IS - 2 SP - 239 EP - 257 PB - MDPI AN - OPUS4-54570 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 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 - Rütters, H. A1 - Fischer, S. A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Bäßler, Ralph A1 - Maßmann, J. A1 - Ostertag-Henning, C. A1 - Wolf, J. L. A1 - Pumpa, M. A1 - Lubenau, U. A1 - Knauer, S. A1 - Jaeger, P. A1 - Neumann, A. A1 - Svensson, K. A1 - Pöllmann, H. A1 - Lempp, C. A1 - Menezes, F. F. A1 - Hagemann, B. T1 - Towards defining reasonable minimum composition thresholds – Impacts of variable CO2 stream compositions on transport, injection and storage N2 - To set up recommendations on how to define “reasonable minimum composition thresholds” for CO2 streams to access CO2 pipeline networks, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the CCS chain. All investigations were based on a generic “CCS cluster scenario” in which CO2 streams captured from a spatial cluster of eleven emitters (seven fossil-fired power plants, two cement plants, one refinery and one steel mill) are collected in a regional pipeline network. The resulting CO2 stream (19.78 Mio t impure CO2 per year) is transported in a trunk line (onshore and offshore) and injected into five generic replicate storage structures (Buntsandstein saline aquifers) offshore. Experimental investigations and modeling of selected impacts revealed beneficial as well as adverse impacts of different impurities and their combinations. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the considered variable compositions and mass flow rates were observed. We recommend to define minimum composition thresholds for each specific CCS project through limiting i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of concentrations of critical impurities, and defining impurity combinations to be avoided. KW - Impurities KW - CO2 quality KW - Pipeline network KW - Whole-chain CCS scenario KW - Recommendations PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543004 DO - https://doi.org/10.1016/j.ijggc.2022.103589 SN - 1750-5836 VL - 114 SP - 1 EP - 14 PB - Elsevier CY - New York, NY AN - OPUS4-54300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk T1 - MGA Round Robin Test on Al-AM Fatigue Testing - Fractographic Results N2 - Presentation of results of an investigation of fracture mechanisms and crack start sites of an additive manufactured aluminium alloy after fatigue testing. Collaboration within the MGA initiative (Mobility Goes Additive). T2 - MGA Mid Term Meeting 2022 CY - Berlin, Germany DA - 05.07.2022 KW - Aluminium Alloy KW - Fractography KW - Additive Manufacturing PY - 2022 AN - OPUS4-55192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia T1 - I n situ monitoring of growing oxidation of the chemically complex alloy AlMo 0.5 NbTa 0.5 TiZr in the high temperature regime using synchrotron radiation Preliminary results N2 - The chemically complex alloys (CCAs) that contain mostly refractory elements (rCCAs), may be highly resistant to heat and load, which makes them attractive candidates for use at extremely high temperatures associated with many technological applications, e.g. aeroengine turbines. However, the field of CCAs, especially their resistance in harsh (oxidative) and hot environment is still young and not much experimental evidence for the understanding mechanisms in this regime is available, which the proposed study addresses. For safe use in structural applications, in addition to their mechanical performance, the environmental resistance of this alloy is also critical. Surface degradation can significantly decrease the mechanical resistance during high temperature exposure, leading to premature failure. The AlMo0.5NbTa0.5TiZr rCCA only contains Al as a protection candidate and it is composed of a coherent B2/bcc nanoscopic cube-on-cube interweave and an hexagonal phase. The evaluation of the oxidation process in the AlMo0.5NbTa0.5TiZr rCCA in the heat-treated state has not been assessed yet. The proposed study focusses on a deeper understanding of the formation mechanism and growth kinetics of oxides at high temperature in the AlMo0.5NbTa0.5TiZr rCCA using synchrotron radiation. Due to the envisaged high temperature structural applications, the alloy is evaluated in an oxidation environment specifically between 800°C and 1000°C. T2 - Large scale facility-based techniques SPP meeting CY - Online meeting DA - 02.11.2021 KW - Refractory chemically complex alloys KW - Oxidation behavior KW - Microstructural analysis KW - Synchrotron radiation PY - 2021 AN - OPUS4-54383 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 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 - 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 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 - Zare Pakzad, S. A1 - Nasr Esfahani, M. A1 - Tasdemir, Z. A1 - Wollschläger, Nicole A1 - Li, T. A1 - Li, X. A1 - Yilmaz, M. A1 - Leblebici, Y. A1 - Erdem Alaca, B. T1 - Nanomechanical Modeling of the Bending Response of Silicon Nanowires N2 - Understanding the mechanical behavior of silicon nanowires is essential for the implementation of advanced nanoscale devices. Although bending tests are predominantly used for this purpose, their findings should be properly interpreted through modeling. Various modeling approaches tend to ignore parts of the effective parameter set involved in the rather complex bending response. This oversimplification is the main reason behind the spread of the modulus of elasticity and strength data in the literature. Addressing this challenge, a surface-based nanomechanical model is introduced in this study. The proposed model considers two important factors that have so far remained neglected despite their significance: (i) intrinsic stresses composed of the initial residual stress and surface-induced residual stress and (ii) anisotropic implementation of surface stress and elasticity. The modeling study is consolidated with molecular dynamics-based study of the native oxide surface through reactive force fields and a series of nanoscale characterization work through in situ threepoint bending test and Raman spectroscopy. The treatment of the test data through a series of models with increasing complexity demonstrates a spread of 85 GPa for the modulus of elasticity and points to the origins of ambiguity regarding silicon nanowire properties, which are some of the most commonly employed nanoscale building blocks. A similar conclusion is reached for strength with variations of up to 3 GPa estimated by the aforementioned nanomechanical models. Precise consideration of the nanowire surface state is thus critical to comprehending the mechanical behavior of silicon nanowires accurately. Overall, this study highlights the need for a multiscale theoretical framework to fully understand the size-dependent mechanical behavior of silicon nanowires, with fortifying effects on the design and reliability assessment of future nanoelectromechanical systems. KW - Silicon nanowires KW - Native oxide KW - Surface stress KW - Surface elasticity KW - Mechanical behavior PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581676 DO - https://doi.org/10.1021/acsanm.3c02077 SP - 1 EP - 14 PB - ACS Publications AN - OPUS4-58167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cios, G. A1 - Winkelmann, A. A1 - Nolze, Gert A1 - Tokarski, T. A1 - Rychlowski, L. A1 - Dan, L. A1 - Bala, P. T1 - Mapping of lattice distortion in martensitic steel—Comparison of different evaluation methods of EBSD patterns N2 - To visualize the varying tetragonal distortions in high carbon martensitic steels by EBSD, two different approaches have been applied on backscattered Kikuchi diffraction (BKD) patterns. A band-edge refinement technique called Refined Accuracy (RA) (Oxford Instruments) is compared with a technique called Pattern Matching (PM), which optimizes the fit to a simulated BKD signal. RA distinguishes between hypothetical phases of different fixed 𝑐∕𝑎, while PM determines a best fitting continuous 𝑐∕𝑎 by projective transformation of a master pattern. Both techniques require stored BKD patterns. The sensitivity of the 𝑐∕𝑎-determination was tested by investigating the microstructure of a ferritic steel with an expected 𝑐∕𝑎 = 1. The influence of the Kikuchi pattern noise on 𝑐∕𝑎 was compared for a single or 40 averaged frames per measuring point, and turned out to be not significant. The application of RA and PM on the martensitic microstructure delivered qualitatively similar maps of 𝑐∕𝑎. The comparison of RA and PM shows that RA is suitably fast and precise during mapping the martensite 𝑐∕𝑎 ratio in analyses of high carbon martensite, especially for fast initial surveys. As RA leads quantitatively to higher noise in 𝑐∕𝑎, the PM analysis can be used for higher precision results. KW - EBSD KW - Steel KW - Martensite KW - Tetragonality KW - Strain PY - 2023 DO - https://doi.org/10.1016/j.ultramic.2023.113824 VL - 253 SP - 1 EP - 11 AN - OPUS4-58158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk A1 - Klinger, Christian T1 - Schadensanalyse an Fahrradkomponenten - Fraktographie, Ursachen, Prävention N2 - Komponenten von Fahrrädern werden im Betrieb vorwiegend schwingend beansprucht. Typische Werkstoffe sind Stahl, Aluminiumlegierungen, Messing, CFK und thermoplastische Kunststoffe. Da es sich, unabhängig von der Preiskategorie, um konstruktiven Leichtbau handelt, werden einige Bauteile betriebsfest mehr oder weniger weit oberhalb der Dauerfestigkeit ausgelegt. Die im normalen Betrieb auftretenden Schäden sind daher weit überwiegend Schwingbrüche. Andere Schadensmechanismen wie z.B. Korrosion spielen quantitativ eine untergeordnete Rolle. Schwingbrüche treten nach einer Periode unbemerkten Risswachstums oft ohne Vorwarnung und ohne makroskopische Verformung auf. Im Falle von sicherheitsrelevanten Komponenten wie Rahmen, Gabeln, Lenkern, Sattelstützen, Kurbelarmen oder Pedalen kann dies zu erheblichen Personenschäden führen, die den Wert des ursächlichen Bauteilschadens weit überschreiten. Über einen langjährigen Zeitraum wurden gebrochene Komponenten aus dem Alltag und aus Gerichtsverfahren analysiert. Das Hauptaugenmerk lag hierbei auf der fraktographischen Analyse, teilweise wurden die zu Grunde liegenden Schadensursachen ermittelt. Einflussfaktoren sind beispielsweise konstruktive Kerben an ungünstigen Stellen, aber auch Werkstoffwahl und Fertigungsqualität spielen eine Rolle. In den meisten Fällen wurde jedoch die konstruktive Lebensdauer überschritten. Diese wird praktisch nie mitgeteilt, und eine wiederkehrende Prüfung sicherheitsrelevanter Bauteile findet nicht statt. Im Sinne der Vermeidung von Schäden und Unfällen könnte darauf hingewirkt werden, für sicherheitsrelevante Komponenten Lebensdauern besser abzuschätzen und von der Laufleistung abhängige Sichtprüfungen zu empfehlen. T2 - Werkstoffprüfung 2022 CY - Dresden, Germany DA - 27.10.2022 KW - Fahrrad KW - Fraktographie KW - Lebensdauer KW - Schadensanalyse KW - Schadensprävention KW - Öffentliche Sicherheit PY - 2023 UR - https://dgm.de/fileadmin/DGM/Veranstaltungen/2022/Werkstoffpruefung/Tagungsband/WP2022-Tagungsband-online.pdf SN - 978-3-88355-430-3 SP - 73 EP - 78 PB - DGM - Deutsche Gesellschaft für Materialkunde e.V CY - Sankt Augustin AN - OPUS4-56832 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Rychlowski, L. T1 - Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 1. Where is the Bragg angle? N2 - The derivation of a crystal structure and its phase-specific parameters from a single wide-angle backscattered Kikuchi diffraction pattern requires reliable extraction of the Bragg angles. By means of the first derivative of the lattice profile, an attempt is made to determine fully automatically and reproducibly the band widths in simulated Kikuchi patterns. Even under such ideal conditions (projection centre, wavelength and lattice plane traces are perfectly known), this leads to a lattice parameter distribution whose mean shows a linear offset that correlates with the mean atomic number Z of the pattern-forming phase. The consideration of as many Kikuchi bands as possible reduces the errors that typically occur if only a single band is analysed. On the other hand, the width of the resulting distribution is such that higher image resolution of diffraction patterns, employing longer wavelengths to produce wider bands or the use of higher interference orders is less advantageous than commonly assumed. KW - Bragg angles KW - Kikuchi bands KW - Kikuchi patterns KW - First derivative KW - Lattice parameters PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573141 DO - https://doi.org/10.1107/S1600576723000134 SN - 0021-8898 VL - 56 IS - Pt. 2 SP - 349 EP - 360 AN - OPUS4-57314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Rychlowski, L. T1 - Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 2. Offset corrections N2 - A band width determination using the first derivative of the band profile systematically underestimates the true Bragg angle. Corrections are proposed to compensate for the resulting offset Δa/a of the mean lattice parameters derived from as many Kikuchi band widths as possible. For dynamically simulated Kikuchi patterns, Δa/a can reach up to 8% for phases with a high mean atomic number Z, whereas for much more common low-Z materials the offset decreases linearly. A predicted offset Δa/a = f(Z) is therefore proposed, which also includes the unit-cell volume and thus takes into account the packing density of the scatterers in the material. Since Z is not always available for unknown phases, its substitution by Zmax, i.e. the atomic number of the heaviest element in the compound, is still acceptable for an approximate correction. For simulated Kikuchi patterns the offset-corrected lattice parameter deviation is Δa/a < 1.5%. The lattice parameter ratios, and the angles α, β and γ between the basis vectors, are not affected at all.1.5%. The lattice parameter ratios, and the angles � , � and � between the basis vectors, are not affected at all. KW - Mean atomic number KW - Kikuchi patterns KW - Lattice parameters KW - Automated Bragg angle determination KW - Lattice parameter determination PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573153 DO - https://doi.org/10.1107/s1600576723000146 SN - 0021-8898 VL - 56 IS - Pt. 2 SP - 361 EP - 366 AN - OPUS4-57315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Rychlowski, L. T1 - Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 3. Pseudosymmetry N2 - A pseudosymmetric description of the crystal lattice derived from a single wideangle Kikuchi pattern can have several causes. The small size (<15%) of the sector covered by an electron backscatter diffraction pattern, the limited precision of the projection centre position and the Kikuchi band definition are crucial. Inherent pseudosymmetries of the crystal lattice and/or structure also pose a challenge in the analysis of Kikuchi patterns. To eliminate experimental errors as much as possible, simulated Kikuchi patterns of 350 phases have been analysed using the software CALM [Nolze et al. (2021). J. Appl. Cryst. 54, 1012–1022] in order to estimate the frequency of and reasons for pseudosymmetric crystal lattice descriptions. Misinterpretations occur in particular when the atomic scattering factors of non-equivalent positions are too similar and reciprocal-lattice points are systematically missing. As an example, a pseudosymmetry prediction depending on the elements involved is discussed for binary AB compounds with B1 and B2 structure types. However, since this is impossible for more complicated phases, this approach cannot be directly applied to compounds of arbitrary composition and structure. KW - Bravais lattices KW - Pseudosymmetry KW - Lattice point density KW - Ordered/disordered structures KW - Lattice distortion PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573169 DO - https://doi.org/10.1107/s1600576723000845 SN - 0021-8898 VL - 56 IS - Pt. 2 SP - 367 EP - 380 AN - OPUS4-57316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Petrushin, N. V. A1 - Epishin, A. I. A1 - Svetlov, I. L. A1 - Nolze, Gert A1 - Elyutin, E. S. A1 - Solov'ev, A. E. T1 - Influence of the Sign of the γ/γ' Misfit on the Structure and Creep Strength of Single Crystals of Nickel-Based Superalloys N2 - Using the method of directional solidification, single crystals of experimental nickel-based superalloys with negative, zero, and positive γ/γ' misfits are obtained. The γ' solvus, solidus, and liquidus temperatures of the alloys are determined, and the microstructures of the alloys after directional solidification, heat treatment, and creep tests are investigated. Creep tests are performed at temperatures of 800 and 1000°C. It is found that single crystals of the alloy with a negative γ/γ' misfit have the highest creep resistance and lifetime (the crystal lattice period of the γ' phase is smaller than that of the γ matrix). KW - Nickel-based superalloys KW - Single crystal KW - Creep KW - Creep strength KW - Microstructure, γ/γ' misfit PY - 2023 DO - https://doi.org/10.1134/s207511332301029x SN - 2075-1133 VL - 14 IS - 1 SP - 13 EP - 22 AN - OPUS4-59505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaminathan, Srinivasan A1 - Sun, K. A1 - Was, G. S. T1 - Decoupling the roles of grain boundary oxidation and stress in IASCC of neutron-irradiated 304L stainless steel N2 - Irradiation assisted stress corrosion cracking (IASCC) is known to be a combination of applied stress, and a corrosive environment in irradiated materials, but an appropriate understanding of how each of these components affects cracking is not yet clear. In this work, we isolate the role of grain boundary (GB) oxidation in IASCC. For this purpose, solution-annealed 304L stainless steel irradiated in reactor to 5.4 or 69 dpa was studied using a miniaturized four-point bend technique. Two modes of bend tests were conducted; straining in simulated pressurized water reactor primary water (PW) at 320 ◦C in an incremental manner, and pre-oxidation in PW at 320 ◦C without application of stress followed by dynamic straining in purified Ar at the same temperature until crack initiation. Exposure of the 5.4 dpa sample for 210 h in high temperature water initiated cracks in Ar at 60% of the yield stress (0.6YS), whereas the companion sample of the same dose exposed for 1010 h cracked in Ar at 0.5YS. The long-term exposure in water led to GB oxidation that ultimately lowered the crack initiation stress. Dynamic straining in water resulted in larger crack lengths and greater crack depths indicating stress accelerated oxidation and cracking. Dislocation pile-ups at dislocation channel-grain boundary sites provide an amplification of the applied stress to a level consistent with the fracture stress of the grain boundary oxide, providing an explanation for IASCC that occurs at applied stresses well below the irradiated yield stress of the alloy. There was no evidence of cracking upon straining of an unoxidized 69 dpa sample in Ar to well above yield, confirming that the irradiated state is not inherently susceptible to intergranular (IG) cracking and that oxidized GBs are responsible for initiation of IG cracking. KW - Stress corrosion cracking KW - Grain boundary oxidation KW - Stainless steel KW - Crack initiation KW - IASCC PY - 2023 DO - https://doi.org/10.1016/j.jnucmat.2023.154604 SN - 0022-3115 VL - 585 SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-58233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemiasheuski, Anton A1 - Bajer, Evgenia A1 - Oder, Gabriele A1 - Göbel, Artur A1 - Hesse, Rene A1 - Bettge, Dirk T1 - Development of an Automated 3D Metallography System (RASI) and its Application in Microstructure Analysis N2 - Many microstructural features exhibit non-trivial geometries, which can only be derived to a limited extent from two-dimensional images. E.g., graphite arrangements in lamellar gray cast iron have complex geometries, and the same is true for additively manufactured materials and three-dimensional conductive path structures. Some can be visualized using tomographic methods, but some cannot be due to weak contrast and/or lack of resolution when analyzing macroscopic objects. Classic metallography can help but must be expanded to the third dimension. The method of reconstructing three-dimensional structures from serial metallographic sections surely is not new. However, the effort required to manually assemble many individual sections into image stacks is very high and stands in the way of frequent application. For this reason, an automated, robot-supported 3D metallography system is being developed at BAM, which carries out the steps of repeated preparation and image acquisition on polished specimen. Preparation includes grinding, polishing and optionally etching of the polished surface. Image acquisition comprises autofocused light microscopic imaging at several magnification levels. The image stacks obtained are then pre-processed, segmented, and converted into 3D models, which in the result appear like microtomographic models, but with high resolution at large volume. Contrasting by classical chemical etching reveals structures that cannot be resolved using tomographic methods. The integration of further imaging and measuring methods into this system is underway. Some examples will be discussed in the presentation. T2 - Euromat 2023 CY - Frankfurt a. M., Germany DA - 04.07.2023 KW - Metallography KW - 3D Reconstruction KW - Roboter KW - Automation KW - Microstructure PY - 2023 AN - OPUS4-58202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bettge, Dirk A1 - Schmies, Lennart T1 - Die Fraktographische Online-Datenbank der AG Fraktographie – Entwicklungsstand und Planung T1 - The WG Fractography Online Database – Stage of Development and Planning N2 - Die AG Fraktographie im DVM/DGM-Gemeinschaftsgremium „Elektronenmikroskopie in der Materialforschung“ betreibt seit 2013 eine fraktographische online-Datenbank („FractoDB“), die für das interessierte Fachpublikum kostenfrei zur Verfügung steht. Die Analyse und Bewertung von Bruchflächen und der darauf befindlichen Bruchmerkmale ist ein wichtiger Teilaspekt der Schadensanalyse bei der Suche nach Schadensmechanismen und Schadensursachen. Risse und Brüche an realen Bauteilen können nur dann bewertet werden, wenn gut dokumentierte Vergleichsbrüche aus Laborversuchen zur Verfügung stehen, sei es an Proben oder an Vergleichs-Bauteilen. Daher trägt die AG Fraktographie Bildmaterial zusammen, führt systematisch Laborversuche und Ringversuche durch und analysiert Brüche aus Schadensfällen. Die gewonnenen Daten werden zu Datensätzen zusammengestellt und über die Datenbank zugänglich gemacht. Derzeit ist ein Bestand von über 400 Datensätzen mit insgesamt über 4.500 Bildern verfügbar, welcher durchsucht werden kann und in Anlehnung an die VDI 3822 organisiert ist. Weitere Aktivitäten der AG Fraktographie, die in der FractoDB abgebildet werden, sind u.a. die Entwicklung einer fraktographischen Symbolik und die Analyse von Bruchmerkmalen mittels Machine Learning. Über die aktuellen Ergebnisse und Planungen wird berichtet. N2 - Since 2013, the AG Fraktographie (Working Group (WG) Fractography) in the DVM/DGM Joint Committee “Elektronenmikroskopie in der Materialforschung” (Electron Microscopy in Materials Research) maintains a fractographic online database (“FractoDB”) available to interested professionals. When it comes to identifying failure mechanisms and causes of damage, the analysis and evaluation of fracture surfaces and their characteristics constitute important aspects of the failure analysis. Cracks and fractures in real components can only be assessed if well-documented comparative fractures from laboratory tests are available – be it in samples or in comparison components. The WG Fractography therefore gathers image material, systematically carries out laboratory and round robin tests, and analyzes fractures from damage cases. From the thus obtained data, datasets are compiled and made available via the database. Currently, a browsable inventory of more than 400 datasets with a total of more than 4500 images is available. It is organized in line with guideline VDI 3822. Other activities of the WG Fractography represented in the FractoDB include, amongst others, the development of a fractographic set of symbols and the analysis of fracture characteristics using machine learning. This contributbution reports on latest results and plans. KW - Fraktographie KW - Datenbank KW - Schadensanalyse KW - Bruchflächen KW - Machine Learning PY - 2023 DO - https://doi.org/10.1515/pm-2023-0048 SN - 0032-678X VL - 60 IS - 9 SP - 569 EP - 579 PB - De Gruyter CY - Berlin AN - OPUS4-58200 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Suárez Ocano, Patricia T1 - Thermodynamic and microstructural stabilities at high temperatures and their effects on mechanical properties in an AlMo0.5NbTa0.5TiZr refractory high entropy superalloy N2 - Today’s industrial demands challenge the research and development sector to make advances in the design and properties of materials that can withstand harsh environments. The AlMo0.5NbTa0.5TiZr refractory high-entropy superalloy (RSA), with a remarkable morphological similarity to the γ/γ' microstructure of Ni-based superalloys and promising high-temperature compressive properties, has been considered as a candidate for structural applications. However, additional properties need to be investigated in order to assess the suitability of this alloy for high temperature applications. Therefore, this work investigates the thermodynamic and microstructural stabilities of the RSA at room temperature and between 900 and 1100 °C, and their influence on the mechanical properties. Although it is possible to improve the mechanical properties at 20 °C by tuning the cooling rate, long-term high temperature exposures lead to phase instabilities that negatively influence the creep behavior. N2 - Die heutigen industriellen Anforderungen erfordern Fortschritte bei Werkstoffdesign und -entwicklung, insbesondere für raue Umgebungen. Die hochentropische Refraktärsuperlegierung (RSA) AlMo0.5NbTa0.5TiZr, die eine bemerkenswerte morphologische Ähnlichkeit mit der γ/γ'-Mikrostruktur von Ni-Basis-Superlegierungen und vielversprechende Hochtemperatur-Druckeigenschaften aufweist, wurde als Kandidat für strukturelle Anwendungen erwägt. Weitere Eigenschaften müssen untersucht werden, um die Eignung dieser Legierung für Hochtemperaturanwendungen zu beurteilen. In dieser Arbeit werden die thermodynamischen und mikrostrukturellen Stabilitäten von RSA bei Raumtemperatur und zwischen 900 und 1100°C sowie deren Einfluss auf die mechanischen Eigenschaften untersucht. Obwohl es möglich ist, die mechanischen Eigenschaften bei 20 °C durch Abstimmung der Abkühlrate zu verbessern, führen langfristige Hochtemperaturexpositionen zu Phaseninstabilitäten, die das Kriechverhalten negativ beeinflussen. KW - Hochentropielegierung KW - Gefüge (Werkstoffkunde) KW - Mikrostruktur KW - Kriechen KW - Thermodynamische Stabilität KW - High entropy alloys KW - Microstructure KW - Creep KW - Thermodynamic stability PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:hbz:294-108415 DO - https://doi.org/10.13154/294-10841 SP - 1 EP - 170 CY - Bochum AN - OPUS4-59929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andreoli, A. F. A1 - Fantin, Andrea A1 - Kasatikov, S. A1 - Bacurau, V. P. A1 - Widom, M. A1 - Gargarella, P. A1 - Mazzer, E. M. A1 - Woodcock, T. G. A1 - Nielsch, K. A1 - Coury, F. G. T1 - The impact of chemical short-range order on the thermophysical properties of medium- and high-entropy alloys N2 - The unusual behavior observed in the coefficient of thermal expansion and specific heat capacity of CrFeNi, CoCrNi, and CoCrFeNi medium/high-entropy alloys is commonly referred to as the K-state effect. It is shown to be independent of the Curie temperature, as demonstrated by temperature-dependent magnetic moment measurements. CoCrFeNi alloy is chosen for detailed characterization; potential reasons for the K-state effect such as texture, recrystallization, and second-phase precipitation are ruled out. An examination of the electronic structure indicates the formation of a pseudo-gap in the Density of States, which suggests a specific chemical interaction between Ni and Cr atoms upon alloying. Hybrid Monte Carlo/Molecular Dynamic (MC/MD) simulations indicate the presence of non-negligible chemical short-range order (CSRO). Local lattice distortions are shown to be negligible, although deviations around Cr and Ni elements from those expected in a fully disordered structure are experimentally observed by X-ray absorption spectroscopy. The determined bonding distances are in good agreement with MC/MD calculations. A mechanism is proposed to explain the anomalies and calorimetric experiments and their results are used to validate the mechanism. KW - Mechanical Engineering KW - Mechanics of Materials KW - General Materials Science PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595869 DO - https://doi.org/10.1016/j.matdes.2024.112724 SN - 0264-1275 VL - 238 SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-59586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmies, Lennart A1 - Hemmleb, Matthias A1 - Bettge, Dirk T1 - Relevant input data for crack feature segmentation with deep learning on SEM imagery and topography data N2 - Fractography plays a critical role in failure analysis of engineering components and has a considerable importance for safety investigations. Usually, the interpretation of fracture surfaces is done by experts with the help of literature and experimental data, that requires a lot of experience. The use of deep learning (DL) with neural networks in failure analysis becomes more and more relevant with the rapidly developing possibilities. Especially, the modern network architectures can assist fractographers in determining various fracture features on SEM images of the fracture surfaces. The basis for the best possible evaluation is the understanding of the influence of the input data used for training deep neural networks (DNN). Therefore, this study discusses the influence of the selection of the input data used for the prediction quality of these networks in order to take this into account for future data acquisition. Specimens of various metallic materials were subjected to fatigue cracking experiment under laboratory conditions. The fractured surfaces were then imaged using various modes or detectors (such as SE, BSE and topography) in SEM, and those captured images were used to create a training data set. The relevance of the individual data for the quality of the prediction is determined by a specific combination of the different detector data. For the training, the well-established architecture of a UNet-ResNet34 with a fixed set of hyperparameters is used. It has been found in this present study that the combination of all input data significantly increases the prediction accuracy, whereby even the combination of SE and BSE data provides considerable advantages over the exclusive use of SE images. KW - Fractography KW - Machine Learning KW - Deep Learning KW - KI PY - 2023 DO - https://doi.org/10.1016/j.engfailanal.2023.107814 VL - 156 SP - 1 EP - 8 PB - Elsevier AN - OPUS4-58918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weinel, Kristina T1 - Electron-beam induced particle synthesis: Phenomenological study of the physical mechanisms N2 - Several studies have shown that the electron beam (e-beam) can be used to create nanomaterials from microparticles in situ in a TEM. However, attempts to produce gold nanoparticles (NPs) on silicon oxide substrate remained to be accomplished. Here, we show that the production of gold NPs is possible by using the e-beam in a SEM, under a set of parameters. To understand the physical mechanisms leading to the gold NPs, the mechanisms of e-beam induced charging as well as e-beam induced heating of the MPs were discussed. Several hints point to heating as the driving mechanism. T2 - IFW Dresden, Seminar CY - Dresden, Germany DA - 06.12.2023 KW - Electron-beam-induced modification KW - Nanoparticle synthesis KW - Scanning electron microscopy KW - Driving physical mechanism KW - Negative charged microparticle KW - Temperature driven process PY - 2023 AN - OPUS4-59081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weinel, Kristina T1 - Electron-beam-induced production of gold nanoparticles N2 - Several studies have shown that the electron beam (e-beam) can be used to create nanomaterials from microparticles in situ in a TEM. However, attempts to produce gold nanoparticles (NPs) on silicon oxide substrate remained to be accomplished. Here, we show that the production of gold NPs is possible by using the e-beam in a SEM, under a set of parameters. The NPs produced present a size gradient along the radial direction. A parameter study shows that the microparticles may: 1) flicker away without producing NPs, 2) fragment to form NPs and/or 3) react with the silicon oxide substrate, depending on the applied current. A hypothesis regarding the driving physical phenomena that lead the microparticles to fragment into NPs is discussed. Fabrication of gold NPs in the SEM provides a more cost-effective option as compared to the established method in the TEM. T2 - PhD Seminar CY - Berlin, Germany DA - 26.11.2023 KW - Electron-beam-induced modification KW - Gold nanoparticles KW - Fabrication method KW - Scanning electron microscope KW - Nano-assemblies PY - 2023 AN - OPUS4-59080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lemiasheuski, Anton A1 - Bajer, Evgenia A1 - Oder, Gabriele A1 - Göbel, Artur A1 - Hesse, Rene A1 - Pfennig, A. A1 - Bettge, Dirk T1 - Entwicklung eines automatisierten 3D-Metallographie-Systems und erste Beispiele für die Anwendung in der Gefüge-Analyse T1 - Development of an automated 3D metallography system and some first application examples in microstructural analysis N2 - Die klassische Metallographie basiert auf Abbildungen einzelner Schliffebenen und kann auf räumliche Formen und Anordnungen des Gefüges nur bedingt schließen. Die Idee, aus metallographischen Serienschliffen dreidimensionale Gefügestrukturen zu rekonstruieren, ist daher naheliegend und nicht neu. Allerdings ist der Aufwand, in Handarbeit viele Einzel-Schliffe zu präparieren und zu Bildstapeln zusammenzusetzen, sehr hoch und steht einer häufigen Anwendung entgegen. Deshalb wird an der BAM ein Roboter-gestütztes 3D-Metallographie-System entwickelt, das an einer Schliffprobe die Schritte Präparation und Bildeinzug vollautomatisch mit vielen Wiederholungen ausführt. Die Präparation umfasst Schleifen, Polieren und optional Ätzen der Schlifffläche, der Bildeinzug autofokussierte lichtmikroskopische Aufnahmen bei mehreren Vergrößerungsstufen. Der erhaltene Bildstapel wird anschließend vorverarbeitet, segmentiert und in ein 3D-Modell umgesetzt, das einer mikrotomographischen Aufnahme ähnelt, allerdings mit besserer lateraler Auflösung bei großem Volumen. Im Gegensatz zu tomographischen Verfahren besteht die Möglichkeit der Kontrastierung durch klassische chemische Ätzung. Die Integration eines REMs ist geplant. Bislang durchgeführte Arbeiten verdeutlichen die Möglichkeiten der Darstellung von Heißgas-Korrosionsschichten, Grauguss-Werkstoffen und Keramik-basierten mikroelektronischen Strukturen (Vias). N2 - Traditional metallography relies on the imaging of individual section planes. However, conclusions as to spatial shapes and microstructural arrangements can only be drawn to a limited extent. The idea to reconstruct three-dimensional microstructures from metallographic serial sections is therefore obvious and not at all new. However, the manual process of preparing a great number of individual sections and assembling them into image stacks is time-consuming and laborious and therefore constitutes an obstacle to frequent use. This is why the Federal Institute for Materials Research and Testing, or BAM for short (Bundesanstalt für Materialforschung und -prüfung), is developing a robot-assisted 3D metallography system performing the tasks of preparation and image acquisition on a metallographic section fully automatically and repeatedly. Preparation includes grinding, polishing and optional etching of the section surface. Image acquisition is performed using a light optical microscope with autofocus at several magnification levels. The obtained image stack is then pre-processed, segmented and converted to a 3D model resembling a microtomographic image, but with a higher lateral resolution when large volumes are sampled. As opposed to tomographic techniques, it is possible to perform traditional chemical etching for contrasting. The integration of a SEM is in the planning stages. Studies conducted so far have demonstrated the possibility of visualizing hot gas corrosion layers, grey cast irons and ceramic-based microelectronic structures (vias). KW - 3D-Metallographie KW - Gefügeanalyse KW - Serienschnitte KW - Gefügerekonstruktion KW - 3D metallography KW - Microstructure analysis KW - Serial sectioning KW - Microstrucure reconstruction PY - 2023 DO - https://doi.org/10.1515/pm-2023-0057 SN - 0032-678X VL - 60 IS - 10 SP - 676 EP - 691 PB - De Gruyter CY - Berlin/Boston AN - OPUS4-58593 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk A1 - Schmies, Lennart T1 - Die Fraktographische Online-Datenbank der AG Fraktographie – Entwicklungsstand und weitere Planung N2 - Vortrag zum aktuellen Stand der fraktographischen online-Datenbank. Darstellung des AGM/DVM Gemeinschaftsausschusses REM in der Materialforschung und seiner Arbeitsgruppen Fraktographie, EBSD und 2D/3D-Prüfung. Ziele und Inhalte der fraktographischen Datenbank, Aufruf zum Mitmachen. Durchführung von Vergleichsversuchen, Entwicklung einer fraktographischen Symbolik, Ringversuch, Vorhaben iFrakto mit Entwicklung einer KI-gestützten Bruchflächenanalyse. T2 - Metallographietagung 2023 CY - Leoben, Austria DA - 13.09.2023 KW - Fraktographie KW - Machine Learning KW - Datenbank PY - 2023 AN - OPUS4-58467 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmies, Lennart A1 - Botsch, B. A1 - Le, Q.-H. A1 - Yarysh, A. A1 - Sonntag, U. A1 - Hemmleb, M. A1 - Bettge, Dirk T1 - Classification of fracture characteristics and fracture mechanisms using deep learning and topography data T1 - Klassifikation von Bruchmerkmalen und Bruchmechanismen mittels Deep Learning und unter Verwendung von Topographiedaten N2 - In failure analysis, micro-fractographic analysis of fracture surfaces is usually performed based on practical knowledge which is gained from available studies, own comparative tests, from the literature, as well as online databases. Based on comparisons with already existing images, fracture mechanisms are determined qualitatively. These images are mostly two-dimensional and obtained by light optical and scanning electron imaging techniques. So far, quantitative assessments have been limited to macrocopically determined percentages of fracture types or to the manual measurement of fatigue striations, for example. Recently, more and more approaches relying on computer algorithms have been taken, with algorithms capable of finding and classifying differently structured fracture characteristics. For the Industrial Collective Research (Industrielle Gemeinschaftsforschung, IGF) project “iFrakto” presented in this paper, electron-optical images are obtained, from which topographic information is calculated. This topographic information is analyzed together with the conventional 2D images. Analytical algorithms and deep learning are used to analyze and evaluate fracture characteristics and are linked to information from a fractography database. The most important aim is to provide software aiding in the application of fractography for failure analysis. This paper will present some first results of the project. N2 - Die mikrofraktographische Analyse von Bruchflächen wird in der Schadensanalyse meist auf der Basis von Erfahrungswissen vorgenommen, welches aus vorliegenden Untersuchungen, eigenen Vergleichsversuchen und aus der Literatur und online Datenbanken stammt. Durch Vergleiche mit bereits vorliegenden Bildern werden qualitativ Bruchmechanismen ermittelt. Grundlage dafür sind zumeist zweidimensionale Aufnahmen aus licht- und elektronenoptischen Verfahren. Quantitative Aussagen beschränken sich bislang beispielsweise auf makroskopische Anteile von Bruchmechanismen oder die manuelle Ausmessung von Schwingstreifen. In jüngerer Zeit gibt es vermehrt Ansätze, Computer-Algorithmen einzusetzen, die in der Lage sind, unterschiedlich strukturierte Bruchmerkmale zu finden und zu klassifizieren. Im hier vorgestellten IGF-Vorhaben „iFrakto“ werden elektronenoptische Aufnahmen erzeugt und daraus Topographie-Informationen berechnet. Diese gewonnenen Topographie-Informationen werden zusammen mit den klassischen 2D-Bildern ausgewertet. Analytische Algorithmen und Deep Learning werden eingesetzt, um Bruchmerkmale zu analysieren, zu bewerten und mit Informationen aus einer fraktographischen Datenbank zu verknüpfen. Wichtigstes Ziel ist die Bereitstellung von Software zur Unterstützung der Fraktographie in der Schadensanalyse. In diesem Beitrag werden erste Ergebnisse des Vorhabens vorgestellt. KW - Fractography KW - Deep Learning KW - Classification PY - 2023 DO - https://doi.org/10.1515/pm-2022-1008 SN - 0032-678X VL - 60 IS - 2 SP - 76 EP - 92 PB - De Gruyter AN - OPUS4-56962 LA - mul 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 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 - Lemiasheuski, Anton A1 - Kranzmann, Axel A1 - Pfennig, Anja T1 - Herausforderungen und Möglichkeiten des manuellen metallografischen Serienschnittverfahrens anhand einer quantitativen Gefügeanalyse der Grafite eines Gusseisens T1 - Challenges and possibilities of the manual metallographic serial sectioning process using the example of a quantitative microstructural analysis of graphite in cast iron N2 - Die in dieser Studie vorgestellte 3D-Gefüge-Analyse konzentriert sich auf die Kugelgrafite eines Gusseisens des Typs EN-GJS. Es werden die Form anhand des Formfaktors und des Seitenverhältnisses sowie die durchschnittliche Teilchengröße und -verteilung untersucht. Die Form der Grafite in Gusseisenwerkstoffen ist mitentscheidend für die mechanischen Eigenschaften dieser Legierungen und ist bei der Charakterisierung des Werkstoffs unumgänglich. Mittels Metallografischen Serienschnittverfahrens wird von dem Schicht für Schicht abgetragenen und lichtmikroskopisch schichtweise dargestellten Werkstoff ein digitaler Zwilling erstellt. Von diesem dreidimensionalen Zwilling lassen sich beliebige Ebenen digital projizieren und analysieren. Eine konventionelle quantitative 3D-Analyse untersucht die Voxelmenge und -zusammensetzung eines Körpers im 3D-Raum. Die hier vorgestellte Analyse wendet stereologische 2D-Analyseverfahren auf drei Raumebenen des Werkstoffs an. Dabei sind zwei der Ebenen digitale Projektionen des Zwillings. Die zwei rekonstruierten Ebenen des Werkstoffs sind so gewählt, dass die Richtungsvektoren aller drei Ebenen einen 90°-Winkel zueinander bilden. Diese Methodik wird eingehend beschrieben sowie Herausforderungen und Möglichkeiten des hier vorgestellten Serienschnittverfahrens diskutiert. N2 - The 3D microstructure analysis presented in this study focuses on the nodular graphite of an EN-GJS grade cast iron. The shape is analyzed based on shape factor and aspect ratio as well as average particle size and distribution. The shape of graphites in cast iron materials is critical to the mechanical properties of these alloys and is essential for the characterization of the material. Metallographic serial sectioning creates a digital twin of the material, which is removed layer by layer and visualized layer by layer under an optical microscope. From this three-dimensional twin, any number of planes can be digitally projected and analyzed. Conventional quantitative 3D analysis examines the voxel count and composition of a body in 3D space. The analysis presented here applies stereological 2D analysis methods to three spatial planes of the material. Two of the planes are digital projections of the twin. The two reconstructed planes of the material are chosen so that the direction vectors of all three planes form an angle of 90° to each other. The methodology is described in detail and the challenges and opportunities of the serial section method presented here are discussed. KW - Dreidimensionale Gefügeanalyse KW - Three-dimensional microstructure analysis KW - 3D-Metallografie KW - Serienschnittverfahren KW - Gefügerekonstruktion KW - Quantitative Gefügeanalyse KW - 3D metallography KW - Serial sectioning KW - Microstructure reconstruction KW - Quantitative microstructure analysis PY - 2024 DO - https://doi.org/10.1515/pm-2024-0066 SN - 0032-678X VL - 61 IS - 9-10 SP - 746 EP - 768 PB - De Gruyter CY - Berlin/Boston AN - OPUS4-60976 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk A1 - Klinger, Christian T1 - Schadensanalyse an Fahrradkomponenten - Fraktographie, Ursachen, Prävention N2 - Komponenten von Fahrrädern werden im Betrieb vorwiegend schwingend beansprucht. Typische Werkstoffe sind Stahl, Aluminiumlegierungen, Messing, CFK und thermoplastische Kunststoffe. Da es sich, unabhängig von der Preiskategorie, um konstruktiven Leichtbau handelt, werden einige Bauteile betriebsfest mehr oder weniger weit oberhalb der Dauerfestigkeit ausgelegt. Die im normalen Betrieb auftretenden Schäden sind daher weit überwiegend Schwingbrüche. Andere Schadensmechanismen wie z.B. Korrosion spielen quantitativ eine untergeordnete Rolle. Schwingbrüche treten nach einer Periode unbemerkten Risswachstums oft ohne Vorwarnung und ohne makroskopische Verformung auf. Im Falle von sicherheitsrelevanten Komponenten wie Rahmen, Gabeln, Lenkern, Sattelstützen, Kurbelarmen oder Pedalen kann dies zu erheblichen Personenschäden führen, die den Wert des ursächlichen Bauteilschadens weit überschreiten. Über einen langjährigen Zeitraum wurden gebrochene Komponenten aus dem Alltag und aus Gerichtsverfahren analysiert. Das Hauptaugenmerk lag hierbei auf der fraktographischen Analyse, teilweise wurden die zu Grunde liegenden Schadensursachen ermittelt. Einflussfaktoren sind beispielsweise konstruktive Kerben an ungünstigen Stellen, aber auch Werkstoffwahl und Fertigungsqualität spielen eine Rolle. In den meisten Fällen wurde jedoch die konstruktive Lebensdauer überschritten. Diese wird praktisch nie mitgeteilt, und eine wiederkehrende Prüfung sicherheitsrelevanter Bauteile findet nicht statt. Im Sinne der Vermeidung von Schäden und Unfällen könnte darauf hingewirkt werden, für sicherheitsrelevante Komponenten Lebensdauern besser abzuschätzen und von der Laufleistung abhängige Sichtprüfungen zu empfehlen. T2 - DGM Tagung Werkstoffprüfung CY - Dresden, Germany DA - 26.10.2022 KW - Fraktographie KW - Fahrrad KW - Lebensdauer KW - Öffentliche Sicherheit KW - Schadensanalyse KW - Schadensprävention PY - 2022 AN - OPUS4-56122 LA - deu 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 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 - Nasr Esfahani, M. A1 - Zare Pakzad, S. A1 - Li, T. A1 - Li, X. A1 - Tasdemir, Z. A1 - Wollschläger, Nicole A1 - Leblebici, Y. A1 - Erdem Alaca, B. T1 - Effect of Native Oxide on Stress in Silicon Nanowires: Implications for Nanoelectromechanical Systems N2 - Understanding the origins of intrinsic stress in Si nanowires (NWs) is crucial for their successful utilization as transducer building blocks in next-generation, miniaturized sensors based on anoelectromechanical systems (NEMS). With their small size leading to ultrahigh-resonance frequencies and extreme surface-to-volume ratios, silicon NWs raise new opportunities regarding sensitivity, precision, and speed in both physical and biochemical sensing. With silicon optoelectromechanical properties strongly dependent on the level of NW intrinsic stress, various studies have been devoted to the measurement of such stresses generated, for example, as a result of harsh fabrication processes. However, due to enormous NW surface area, even the native oxide that is conventionally considered as a benign surface condition can cause significant stresses. To address this issue, a combination of nanomechanical characterization and atomistic simulation approaches is developed. Relying only on low-temperature processes, the fabrication approach yields monolithic NWs with optimum boundary conditions, where NWs and support architecture are etched within the same silicon crystal. Resulting NWs are characterized by transmission electron microscopy and micro-Raman spectroscopy. The interpretation of results is carried out through molecular dynamics simulations with ReaxFF potential facilitating the incorporation of humidity and temperature, thereby providing a close replica of the actual oxidation environment - in contrast to previous dry oxidation or self-limiting thermal oxidation studies. As a result, consensus on significant intrinsic tensile stresses on the order of 100 MPa to 1 GPa was achieved as a function of NW critical dimension and aspect ratio. The understanding developed herein regarding the role of native oxide played in the generation of NW intrinsic stresses is important for the design and development of silicon-based NEMS. KW - Nanoelectromechanical systems (NEMS) KW - Silicon nanowires KW - Native oxide KW - Intrinsic stress KW - Raman spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560471 DO - https://doi.org/10.1021/acsanm.2c02983 SN - 2574-0970 VL - 5 SP - 13276 EP - 13285 PB - ACS Publ. CY - Washington, DC AN - OPUS4-56047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, M. A1 - Bettge, Dirk A1 - Hilgenberg, Kai A1 - Binder, M. A1 - Dollmeier, K. A1 - Dreyer, M. A1 - Klöden, B. A1 - Schlingmann, T. A1 - Schmidt, J. T1 - Reproducibility and Scattering in Additive Manufacturing: Results from a Round Robin on PBF-LB/M AlSi10Mg Alloy T1 - Reproduzierbarkeit und Streuung bei der additiven Fertigung: Ergebnisse eines Ringversuchs mit einer PBF-LB/M AlSi10Mg-Legierung N2 - The round robin test investigated the reliability users can expect for AlSi10Mg additive manufactured specimens by laser powder bed fusion through examining powder quality, process parameter, microstructure defects, strength and fatigue. Besides for one outlier, expected static material properties could be found. Optical microstructure inspection was beneficial to determine true porosity and porosity types to explain the occurring scatter in properties. Fractographic analyses reveal that the fatigue crack propagation starts at the rough as-built surface for all specimens. Statistical analysis of the scatter in fatigue using statistical derived safety factors concludes that at a stress of 36.87 MPa the fatigue limit of 107 cycles could be reached for all specimen with a survival probability of 99.999 %. N2 - Im Rahmen eines Ringversuchs wurde durch die Untersuchung der Pulverqualität, der Prozessparameter, der Gefügefehler, der Festigkeit und der Ermüdung die Zuverlässigkeit bestimmt, die Nutzer von AlSi10Mg-Proben erwarten können, die mit pulverbettbasiertes Schmelzen mittels Laser (engl. Laser Powder Bed Fusion) gefertigt worden sind. Abgesehen von einem Ausreißer wurden die erwarteten statischen Materialeigenschaften erreicht. Eine optische Gefügeprüfung diente dazu, die tatsächliche Porosität und Arten von Porosität zu ermitteln, um die bei den Eigenschaften auftretende Streuung zu erklären. Fraktographische Unterschungen zeigen eine bei allen Proben von der rauen Oberfläche im As-built-Zustand ausgehende Ermüdungsrissausbreitung. Aus der statistischen Analyse der Streuung bezüglich der Ermüdung unter Anwendung von statistischen abgeleiteten Sicherheitsfaktoren geht hervor, dass alle Proben die Dauerfestigkeit von 107 Zyklen bei einer Spannung von 36,87 MPa mit einer Überlebenswahrscheinlichkeit von 99,999 % erreichten. KW - Additive manufacturing KW - Reproducibility KW - Reliability PY - 2022 DO - https://doi.org/10.1515/pm-2022-1018 SN - 2195-8599 VL - 59 IS - 10 SP - 580 EP - 614 PB - De Gruyter AN - OPUS4-55935 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hemmleb, M. T1 - Integrated topographic SEM imaging for software assisted fractography N2 - The aim of a fractographic investigation is the evaluation of macroscopic and microscopic fracture surface characteristics and, as a result, the determination of the fracture mechanism of a component from a failure case. The basis for such evaluations of fracture characteristics comes from actual comparative mechanical testing and from the literature. A fractographic analysis can be very complex and, in any case, requires considerable experience. Machine learning methods enables the quantitative determination of fracture characteristics and fracture mechanisms utilizing digitized expert knowledge [1]. Although the application of SE images provides promising results, additional information is required to obtain reliable solutions. As expected, BSE and 3D information helps to improve the classification (Fig. 1). But only a fast, widely integrated, and automated topography measurement can provide the required amount of referenced surface data for the application of machine learning methods. To fulfil these requirements, topographical data are obtained from a BSE detector with four symmetric segments (4Q-BSE) using shape-from-shading technology [2]. Surface height calculation is performed live during image acquisition and provides immediate feedback in three dimensions. All available signals (SE, BSE and more if applicable) are recorded simultaneously together with the surface topography and stored in a multichannel data file. This guaranties the same geometrical reference for all data, which is required for further analysis (Fig. 2). When applying machine learning methods to topographic data together with SEM images, topographic information must be provided as depth image. Consequently, a unique height scale is required for all applied data with different magnifications. This requires a calibrated height measurement, which is ensured with the integrated 3D calibration of the topographic acquisition and a dedicated calibration sample. Thus, a large number of data sets from different fracture samples was generated and used as training data for machine learning. T2 - 16th Multinational Congress on Microscopy CY - Brno, Czech Republic DA - 04.09.2022 KW - Fractography KW - Machine Learning KW - Topography PY - 2022 AN - OPUS4-55937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmies, Lennart T1 - Using Machine Learning and Topographic SEM Imaging for Software Assisted Fractography N2 - The aim of a fractographic investigation is the evaluation of macroscopic and microscopic fracture surface characteristics and, as a result, the determination of the fracture mechanism of a component from a failure case. The basis for such evaluations of fracture characteristics comes from actual comparative mechanical testing and from the literature. A fractographic analysis can be very complex and, in any case, requires considerable experience. In the IGF project "iFrakto", software is being developed that quantitatively determines fracture characteristics and fracture mechanisms utilizing digitized expert knowledge, machine learning, and standard 2D and topographical data from SEM imaging. Topographical data are obtained from 4QBSE detector using shape-from-shading technology. In the medium term, a software tool should provide knowledge-based suggestions for the evaluation of fracture surfaces in real time during SEM work or at subsequent evaluation. As a basis for this, round robins were carried out among fractographers in order to create a knowledge base, to query the practice-relevant requirements for such tools and to carry out first practical tests. Actual results are presented and the relevance of the evaluation strategy is evaluated. T2 - Material Science and Engineering 2022 CY - Darmstadt, Germany DA - 27.9.2022 KW - Fractography KW - Machine Learning KW - Topography PY - 2022 AN - OPUS4-55938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sonntag, U. T1 - Softwaregestützte Bestimmung von Bruchmechanismen und Bruchflächenmerkmalen mittels Machine Learning und Topographie-Informationen N2 - Ziel von fraktographischen Untersuchungen ist die Auswertung von makroskopischen und mikroskopischen Bruchflächenmerkmalen und daraus resultierend die Bestimmung des Bruchmechanismus eines Bauteils aus einem Schadensfall. Die Grundlage für die Bewertung von Bruchmerkmalen stammt dabei aus zuvor durchgeführten eigenen Vergleichsversuchen und aus der Literatur. Eine fraktographische Analyse kann sehr aufwändig sein und setzt in jedem Fall erhebliches Erfahrungswissen voraus. Im IGF-Vorhaben „iFrakto“ wird Software entwickelt, die auf Basis von digitalisiertem Expertenwissen, Machine Learning und unter Zuhilfenahme von Topographie-Daten anhand von REM-Aufnahmen Bruchmerkmale und Bruchmechanismen quantitativ bestimmt, s. Abbildung. Solche Software soll mittelfristig direkt am REM oder bei der nachfolgenden Auswertung wissensbasierte Vorschläge für die Bewertung von Bruchflächen liefern. Als Grundlage hierfür wurden Ringversuche unter Fraktograph/inn/en durchgeführt, um die Wissensbasis zu schaffen, die praxisrelevanten Anforderungen an solche Software abzufragen und erste Praxistests durchzuführen. Die bisherigen Ergebnisse werden vorgestellt und die Relevanz der Auswertestrategie und unterschiedlicher Sensordaten bewertet. T2 - 56. Metallographie-Tagung CY - Saarbrücken, Germany DA - 21.9.2022 KW - Fraktographie KW - Machine Learning KW - Topographie PY - 2022 AN - OPUS4-55939 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Langer, Carlotta A1 - Georgie, Yasmin Kim A1 - Porohovoj, Ilja A1 - Hafner, Verena Vanessa A1 - Ay, Nihat T1 - Analyzing Multimodal Integration in the Variational Autoencoder from an Information-Theoretic Perspective N2 - Human perception is inherently multimodal. We integrate, for instance, visual, proprioceptive and tactile information into one experience. Hence, multimodal learning is of importance for building robotic systems that aim at robustly interacting with the real world. One potential model that has been proposed for multimodal integration is the multimodal variational autoencoder. A variational autoencoder (VAE) consists of two networks, an encoder that maps the data to a stochastic latent space and a decoder that reconstruct this data from an element of this latent space. The multimodal VAE integrates inputs from different modalities at two points in time in the latent space and can thereby be used as a controller for a robotic agent. Here we use this architecture and introduce information-theoretic measures in order to analyze how important the integration of the different modalities are for the reconstruction of the input data. Therefore we calculate two different types of measures, the first type is called single modality error and assesses how important the information from a single modality is for the reconstruction of this modality or all modalities. Secondly, the measures named loss of precision calculate the impact that missing information from only one modality has on the reconstruction of this modality or the whole vector. The VAE is trained via the evidence lower bound, which can be written as a sum of two different terms, namely the reconstruction and the latent loss. The impact of the latent loss can be weighted via an additional variable, which has been introduced to combat posterior collapse. Here we train networks with four different weighting schedules and analyze them with respect to their capabilities for multimodal integration. KW - Multimodal Integration KW - Variational Autoencoder KW - Information Theory KW - Posterior Collapse PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616420 DO - https://doi.org/10.48550/arXiv.2411.00522 SP - 1 EP - 17 PB - Cornell University CY - Ithaca, NY AN - OPUS4-61642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cios, G. A1 - Winkelmann, A. A1 - Nolze, Gert A1 - Tokarski, T. A1 - Jany, B. R. A1 - Bala, P. T1 - EBSD and TKD analyses using inverted contrast Kikuchi diffraction patterns and alternative measurement geometries N2 - Electron backscatter diffraction (EBSD) patterns can exhibit Kikuchi bands with inverted contrast due to anomalous absorption. This can be observed, for example, on samples with nanoscale topography, in case of a low tilt backscattering geometry, or for transmission Kikuchi diffraction (TKD) on thicker samples. Three examples are discussed where contrast-inverted physics-based simulated master patterns have been applied to find the correct crystal orientation. As first EBSD example, self-assembled gold nanostructures made of Au fcc and Au hcp phases on single-crystal germanium were investigated. Gold covered about 12% of the mapped area, with only two thirds being successfully interpreted using standard Hough-based indexing. The remaining third was solved by brute force indexing using a contrast-inverted master pattern. The second EBSD example deals with maps collected at a non-tilted surface instead of the commonly used 70◦ tilted one. As TKD example, a jet-polished foil made of duplex stainless steel 2205 was examined. The thin part close to the hole edge producing normal-contrast patterns were standard indexed. The areas of the foil that become thicker with increasing distance from the edge of the hole produce contrast-inverted patterns. They covered three times the evaluable area and were successfully processed using the contrast-inverted master pattern. In the last example, inverted patterns collected at a non-tiled sample were mathematically inverted to normal contrast, and Hough/Radon-based indexing was successfully applied. KW - EBSD KW - TKD KW - Contrast inversion KW - Topography KW - Kikuchi diffraction PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613862 VL - 267 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-61386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Mohring, Wencke A1 - Wolf, Marcus T1 - The insignificant improvement of corrosion and corrosion fatigue behavior in geothermal environment applying Boehmit coatings on high alloyed steels N2 - The efficacy of alumina-sol based coatings in a water-free atmosphere at high temperatures suggests a potential solution for enhancing the corrosion resistance of high-alloyed steels in Carbon Capture and Storage (CCS) environments. In this study, coupons of X20Cr13, designed for use as injection pipes with 13% Chromium and 0.20% Carbon (1.4021, AISI 420), were sol-gel coated with water and ethanol-based alumina. These coated coupons were then exposed to CO2-saturated saline aquifer water, simulating conditions in the Northern German Basin, for 1000 h at ambient pressure and 60 °C. Corrosion fatigue experiments were also conducted using specimens of X5CrNiMoCuNb16-4 (1.4542, AISI 630), a suitable candidate for geothermal applications, to assess the impact of the ethanol-based coating on the number of cycles to failure at different stress amplitudes. Unfortunately, the coating exhibited early spallation, resulting in corrosion kinetics and corrosion fatigue data identical to those of uncoated specimens. Consequently, the initially promising Boehmit coating is deemed unsuitable for CCS applications and further research therefore not advisable. KW - Alumina coating KW - High alloyed steel KW - Pitting KW - Surface corrosion KW - CO2 KW - Pipeline KW - Corrosion KW - CCS KW - CO2-storage PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623786 DO - https://doi.org/10.3390/app14041575 SN - 2076-3417 VL - 14 IS - 4 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-62378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, A. A1 - Simkin, Roman T1 - Identifying the initial corrosion fatigue failure based on dropping electrochemical potential N2 - The corrosion fatigue of duplex stainless-steel X2CrNiMoN22-5-3 can be determined by purely alternating axial cyclic load to failure using hour-glass shaped specimens. The experimental setup comprises a corrosion chamber allowing for the circulation of an aquifer electrolyte heated to 369 K simulating a carbon capture and storage as well as geothermal power plant environment. During engineering of a carbon storage site or geothermal power plant, it may be crucial to determine the failure onset of a component beforehand. Therefore, an algorithm with 93.3% reliability was established based on splitting the measured potential values into ten time series with a capacity of ten values. The failure of corrosion fatigue specimens in a geothermal environment correlates to the drop of the curves of the electrochemical potential which is measured simultaneously within the corrosion chamber. Crack initiation was, therefore, successfully derived from the electrochemical potential. KW - Corrosion fatigue KW - Surface corrosion KW - CO2 KW - Crack initiation KW - Geothermal energy production PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629310 DO - https://doi.org/10.3390/app15010403 SN - 2076-3417 VL - 15 IS - 1 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-62931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Werner, Tiago T1 - Short fatigue crack propagation in L-PBF 316L stainless steel N2 - Fracture mechanics is a key to fatigue assessment in AM metal components. Short fatigue cracks are initiated at defects and pronounced surface roughness intrinsic to AM. The subsequent crack-propagation is strongly influenced by microstructural interactions and the build-up of crack-closure. The aim of the present study is to give an insight into short-crack propagation in AM-metals. Fatigue crack propagation resistance curves were determined experimentally for AISI 316L manufactured by Laser Powder Bed Fusion (L-PBF) which was heat treated at three different temperatures. Differences in the build-up of the fatigue-crack propagation threshold in between the L-PBF specimens and compared to wrought material are due to the residual stress states, a pronounced roughness of the crack-faces in the L-PBF specimens and phase transformation in the vicinity of the crack-tip, resulting in increased crack-closure. This, together with crack-branching found along the crack path, enhances the resistance to the propagation of fatigue cracks. T2 - ASTM International Conference on Additive Manufacturing 2020 CY - Online meeting DA - 16.11.2020 KW - Additive Manufacturing KW - Cyclic R-Curve KW - Component assessment KW - L-PBF KW - 316L KW - Residual Stress KW - Fatigue Crack Growth PY - 2020 AN - OPUS4-51585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kumar, Sumit A1 - Swaminathan, Srinivasan A1 - Hesse, Rene A1 - Goldbeck, Hennig A1 - Ding, Wenjin A1 - Bonk, Alexander A1 - Bauer, Thomas T1 - Understanding the effect of oxide ions on Solar Salt chemistry and corrosion mechanism of 316L stainless steel at 600 °C N2 - Solar Salt (60 wt% NaNO3, 40 wt% KNO3), used in Concentrated Solar Power (CSP) Thermal Energy Storage (TES) technology, can decompose into various products at elevated temperatures, with oxide ions being one of the known corrosive byproducts. The study mimics Solar Salt aging by intentionally adding sodium peroxide (Na2O2) and sodium oxide (Na2O) at concentrations of 0.005–0.33 wt% to investigate their role in the corrosion of austenitic stainless steel at 600 °C in typical operating conditions. Salt chemistry (nitrite, nitrate, oxide ions, and metal cations) was analyzed every 24 h, and steel corrosion after 168 h was assessed by weight change, corrosion rate, phase analysis, and cross-sectional morphology. Results reveal that at or above 0.135 wt% added Na2O2/Na2O leads to a quasi-steady-state equilibrium of oxide ions in the salt. Interestingly, at these concentrations, the presence of steel further decreases oxide ion concentration. Furthermore, above 0.135 wt%, the corrosion rate increases significantly, along with increased spallation, porosity and disintegration of the corrosion layer, forming a non-protective layer. This study highlights the critical role of oxide ions in the corrosion process. KW - Solar Salt KW - High temperature corrosion KW - Thermal Energy Storage KW - Alkali oxides KW - Austenitic stainless steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628463 DO - https://doi.org/10.1016/j.corsci.2025.112849 SN - 1879-0496 VL - 249 SP - 1 EP - 17 PB - Elsevier Ltd. AN - OPUS4-62846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa T1 - Licht- und Elektronenoptische 3D-Verfahren zur Analyse von Bruchflächen N2 - Die Analyse von Bruchflächen wird in der Schadensanalyse meist auf der Basis von Erfahrungswissen vorgenommen, welches aus vorliegenden Untersuchungen, eigenen Vergleichsversuchen und aus der Literatur stammt. Durch Vergleiche mit bereits vorliegenden Bildern werden qualitativ Bruchmechanismen ermittelt. Grundlage sind zumeist zweidimensionale Bilder aus licht- und elekt-ronenoptischen Verfahren. Quantitative Aussagen beziehen sich bislang beispielsweise auf makroskopische Anteile von Bruchmechanismen oder die Ausmessung von Schwingstreifen. In jüngerer Zeit gibt es vermehrt Ansätze, Computer-Algorithmen einzusetzen, die in der Lage sind, unterschiedlich strukturierte Bruchmerkmale zu finden und zu klassifizieren. Im hier vorgestellten IGF-Vorhaben „iFrakto“, IGF Vorhaben Nr.: 21477 N, werden licht- und elektronenoptisch Topographie-Bilder erzeugt und die gewonnenen 3D-Informationen zusammen mit den klassischen 2D-Bildern ausgewertet. T2 - Treffen der AG Fraktographie im Gemeinschaftsausschuss Rasterelektronenmikroskopie in der Materialprüfung CY - Online meeting DA - 19.11.2021 KW - 3D REM KW - Fraktographie KW - Bruchflächen PY - 2021 UR - https://dgm.inventum.de/widget/preview/45d8c33d-622b-43e2-8459-ba783394a723/611d133ebdac0611d133ebdac1 AN - OPUS4-53800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Wencke T1 - High temperature corrosion of high (HEA) and medium (MEA) entropy alloys N2 - The high-temperature corrosion behavior of the medium-entropy alloy Cr33Co33Ni33 (MEA) and the high-entropy alloy Fe20Cr20Co20Ni20Mn20 (HEA) in a mixed gas atmosphere of 10% H2O-2% O2 -0.5% SO2 + Ar as carrier gas [Vol.%] at 800 °C with duration times of t = 24h, 48h and 96h was investigated. Both alloys have a single-phase fcc microstructure. The oxidation kinetics of the HEA-CrMnFeCoNi roughly followed a linear rate law and a slow oxide growth was observable for the MEA-CrCoNi. The scale thickness of the corrosion layer in the quinary alloy increased with exposure time, while the scale thickness in the ternary alloy remained constant at around 1 µm. The MEA-CrCoNi developed a protective Cr2O3 layer with minor buckled parts. Co,Ni-chromite (Co,Ni)Cr2O4 was detected by XRD in minor amounts. The scale on HEA-CrMnFeCoNi displayed a triplex structure of a thin, continuous, inner Cr2O3 layer, a dense, intermediate Mn3O4 layer, and a thick, outer, porous layer consisting of Mn3O4 and MnSO4. Sulphides were only identified in the matrix of HEA-CrMnFeCoNi. Thermodynamic equilibrium calculations with FactSage (Log(S2) vs. Log(O2), ΔG of reactions) are in good agreement with these observations. The intense diffusion of Cr in the ternary alloy leads to an immediate formation of a protective Cr2O3 layer. The fast diffusion of Mn through the bulk HEA material and through the formed Cr2O3 layer compared to the other alloying elements is considered as the rate-limiting process. T2 - DMG Sektionstreffen Angewandte Mineralogie und Kristallographie CY - Online meeting DA - 25.02.2021 KW - Cr2O3 KW - High-Temperature Corrosion KW - HEA KW - MEA PY - 2021 AN - OPUS4-52164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Wolf, M. A1 - Kranzmann, Axel T1 - Corrosion and Corrosion Fatigue of Steels in Downhole CCS Environment—A Summary N2 - Static immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4, and X5CrNiCuNb16-4 at T = 60°C and ambient pressure, as well as p = 100 bar were performed for 700–8000 h in a CO2-saturated synthetic aquifer environment similar to CCS sites in the Northern German Basin (NGB). Corrosion rates at 100 bar are generally lower than at ambient pressure. The main corrosion products are FeCO3 and FeOOH with surface and local corrosion phenomena directly related to the alloy composition and microstructure. The appropriate heat treatment enhances corrosion resistance. The lifetime reduction of X46Cr13, X5CrNiCuNb16-4, and duplex stainless steel X2CrNiMoN22-5-3 in a CCS environment is demonstrated in the in situ corrosion fatigue CF experiments (axial push-pull and rotation bending load, 60°C , brine: Stuttgart Aquifer and NGB, flowing CO2: 30 L/h, +/- applied potential). Insulating the test setup is necessary to gain reliable data. S-N plots, micrographic-, phase-, fractographic-, and surface analysis prove that the life expectancy of X2CrNiMoN22-5-3 in the axial cyclic load to failure is clearly related to the surface finish, applied stress amplitude, and stress mode. The horizontal grain attack within corrosion pit cavities, multiple fatigue cracks, and preferable deterioration of austenitic phase mainly cause fatigue failure. The CF life range increases significantly when a protective potential is applied. KW - Carbon capture and storage KW - Steel KW - High alloyed steel KW - Corrosion KW - Corrosion fatigue KW - CCS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523948 DO - https://doi.org/10.3390/pr9040594 VL - 9 IS - 4 SP - 594 PB - MDPI CY - Basel, Switzerland AN - OPUS4-52394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Botsch, B T1 - Classification of fracture surface types based on SEM images N2 - The following work deals with the quantitative fracture surface evaluation in damage analysis. So far, fracture surfaces have almost exclusively been evaluated qualitatively, i.e. the presence of fracture features is documented and their surface proportions are estimated, if necessary. Many years of experience are required, as well as an intensive comparison with defined comparative images from the literature. The aim of this work is the development of classifiers which can recognize fracture mechanisms or fracture features in scanning electron microscope images (SEM). The basis is 46 SEM images, which have been evaluated by fractography experts with regard to fracture features. The existing data set of images is expanded using augmentation methods in order to increase the variability of the data and counteract overfitting. Only convolutional neural networks (CNN) are used to create the classifiers. Various network configurations are tested, with the SegNet achieving the best results. T2 - Materialsweek 2021 CY - Online meeting DA - 07.09.2021 KW - Fractography KW - Fracture surface KW - Deep learning KW - SEM PY - 2021 AN - OPUS4-53418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Schulz, Wencke A1 - Schneider, M. A1 - Karafiludis, Stephanos A1 - Laplanche, G. T1 - High-Temperature Oxidation in Dry and Humid Atmospheres of the Equiatomic CrMnFeCoNi and CrCoNi High- and Medium-Entropy Alloys N2 - Surface degradation phenomena of two model equiatomic alloys from the CrMnFeCoNi alloy system were investigated in 2% O2 and 10% H2O (pO2 = 0.02 and 10−7 atm, respectively) at 800 °C for times up to 96 h. The crystallographic structures, morphologies, and chemical compositions of the corrosion layers developing on CrMnFeCoNi and CrCoNi were comparatively analyzed by mass gain analysis, X-ray diffraction, and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy and electron backscatter diffraction. The oxidation resistance of CrMnFeCoNi is relatively poor due to the fast growth of porous Mnoxide(s). CrCoNi forms an external chromia layer that is dense and continuous in a dry 2% O2 atmosphere. This layer buckles and spalls off after exposure to 10% H2O atmosphere. Beneath the chromia layer, a Cr-depleted zone forms in the CrCoNi alloy in both environments. As the oxide scale spalls off in the H2O-containing atmosphere, a secondary chromia layer was observed and correspondingly enlarges the Cr-depleted zone. In contrast, as the chromia layer remains without significant spallation when CrCoNi is exposed to a dry oxidizing atmosphere, the region depleted in Cr is narrower. KW - High temperature oxidation KW - High entropy alloys KW - Medium entropy alloys KW - CrMnFeCoNi KW - CrCoNi KW - Mn-oxides PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517859 DO - https://doi.org/10.1007/s11085-020-10014-7 SN - 0030-770X VL - 95 IS - 1-2 SP - 105 EP - 133 PB - Springer AN - OPUS4-51785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaminathan, Srinivasan A1 - Kumar, S. A1 - Kranzmann, Axel A1 - Hesse, Rene A1 - Goldbeck, Hennig A1 - Fantin, Andrea T1 - Corrosion characteristics of 316L stainless steel in oxide-rich molten solar salt at 600◦C N2 - An attempt has been made in this work, to observe the influence on alloy aging by the sodium oxide (Na2O) in solar salt (60 wt% NaNO3 + 40 wt% KNO3). The accelerated aging was established by adding Na2O (0.005, 0.07, 0.135 and 0.2 wt%) to the solar salt and their effect on corrosion of 316L stainless steel (SS) at 600 ◦C in that oxide-rich solar salts for 168 h in synthetic air was investigated. Corrosion is significantly more in oxide-rich solar salt compared to pure solar salt. Strikingly, the oxide scale-base metal interface is wavy in solar salt containing 0.005 % Na2O clearly shows the oxide addition to salt melt influences Cr-rich inner oxide layer formation and its selective dissolution at early stage that leads to non-uniform corrosion. Interestingly, with increase of Na2O to 0.07 %, steel corrosion proceeded uniformly by accelerated disintegration of Cr-rich inner layer and subsequent dissolution. Severe scale spallation and weight loss in nitrate melt containing 0.2 % Na2O fostering more rapid corrosion, alarming that substantial tolerance of oxide content in solar salt is ≥ 0.135 % for an acceptable corrosion of 316L SS. Despite preferential dissolution of Cr and scale degradation/spallation with increased oxide content in solar salt, the corrosion layer in all cases comprised of sodium ferrite, and Cr-rich Cr-Fe mixed oxides with the Ni enrichment at the scale-metal interface. Competing processes between oxide scale growth, degradation and dissolution or even spallation has been discussed with an emphasis of Na2O addition to solar salt. KW - Molten salt corrosion KW - Solar salt KW - Thermal energy storage KW - Stainless steel KW - Concentrating solar power PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610819 DO - https://doi.org/10.1016/j.solmat.2024.113176 VL - 278 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-61081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Kalady, Mohammed Fayis A1 - Schultz, Johannes A1 - Weinel, Kristina A1 - Wolf, Daniel A1 - Lubk, Axel T1 - Localization of Hybridized Surface Plasmon Modes on Random Gold Nanoparticle Assemblies N2 - Assemblies of plasmonic nanoparticles (NPs) support hybridized modes of localized surface plasmons (LSPs), which delocalize in geometrically well-ordered arrangements. Here, the hybridization behavior of LSPs in geometrically completely disordered arrangements of Au NPs fabricated by an e-beam synthesis method is studied. Employing electron energy loss spectroscopy in a scanning transmission electron microscope in combination with numerical simulations, the disorder-driven spatial and spectral localization of the coupled LSP modes that depend on the NP thickness is revealed. Below 0.4nm sample thickness (flat NPs), localization increases towards higher hybridized LSP mode energies. In comparison, above 10nm thickness, a decrease of localization (an increase of delocalization) with higher mode energies is observed. In the intermediate thickness regime, a transition of the energy dependence of the localization between the two limiting cases, exhibiting a transition mode energy with minimal localization, is observed. This behavior is mainly driven by the energy and thickness dependence of the polarizability of the individual NPs. KW - Plasmonics KW - Electron-Energy Loss Spectroscopy KW - Discrete Dipole Approximation KW - Nanoparticles PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618323 DO - https://doi.org/10.48550/arXiv.2410.10514 SP - 1 EP - 8 PB - Cornell University CY - Ithaca, NY AN - OPUS4-61832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Wencke T1 - High temperature corrosion phenomena of HEAs and MEAs N2 - High- and medium-entropy alloys (HEAs and MEAs) constitute a new class of materials. Those with a face-centered cubic (fcc) structure from the Cr-Mn-Fe-Co-Ni system have excellent mechanical properties and are considered for high-temperature applications since diffusion in these alloys was reported to be sluggish. However, their corrosion resistance at high temperatures must still be evaluated to further qualify them for such kinds of applications. Various groups studied the oxidation behavior of HEAs and MEAs under (dry) laboratory and artificial air as well as CO2/CO mixtures in different temperature ranges. CrCoNi exhibits the best corrosion resistance at 800 °C due to the formation of a protective Cr2O3 layer. The matrix below the oxide scale was reported to be correspondingly depleted in Cr. It was further shown that the addition of Mn and Fe to CrCoNi changes the phase composition of the oxide scale at 800 °C. A Mn2O3 layer was grown during oxidation on CrMnCoNi and CrMnFeCoNi and a Cr2O3 scale was formed at the matrix/oxide scale interface. Beneath these oxide layers, Mn- and Cr-depleted zones were detected. These phase morphologies demonstrate the inward diffusion of oxygen and outward diffusion of Cr and Mn resulting in the formation of Cr2O3 and Mn2O3. In the present study, the corrosion resistance of CrMnFeCoNi and CrCoNi were confirmed and additionally characterized under further oxidizing atmospheres at 800 °C including Ar-2 Vol.% O2, Ar-2 Vol.% H20, and Ar-2 Vol.% SO2 mixtures. T2 - Symposium on Advanced Mechanical and Microstructural Characterization of High-Entropy Alloys CY - Ruhr-Universität Bochum, Germany DA - 03.02.2020 KW - Mn3O4 KW - High-entropy alloy KW - Medium-entropy alloy KW - High-temperature corrosion KW - Chromia PY - 2020 AN - OPUS4-50984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Effect of a mixed atmosphere H2O-O2-SO2 on the oxidation kinetics and phase formation on CrMnFeCoNi and CrCoNi N2 - The high-entropy alloy (HEA) CrMnFeCoNi and the medium-entropy alloy (MEA) CrCoNi with a face-centered cubic (fcc) structure have excellent mechanical properties and are considered for high-temperature applications. Both materials were exposed under several oxidized atmospheres in a wide temperature range/regime. Mn-oxide (Mn3O4, Mn2O3) was mainly formed on the HEA and Cr2O3 on the MEA. The fast diffusion of manganese prevents the formation of a continuous chromia layer on CrMnFeCoNi in Ar-O2, Ar-H2O and Ar-SO2 at 800°C. The Cantor alloy and his ternary subsystem CrCoNi were exposed in Ar-O2-H2O-SO2 at 800°C up to 96 h to clarify their oxidation behavior in a mixed atmosphere. The oxidized samples were analyzed by weight measurement, scanning electron microscopy (SEM), and X-ray diffraction analysis (XRD). It was found that mass gain of all samples increased with increasing exposure time. The oxidation rate of the Cantor alloy is significantly higher than that of the ternary alloy system. T2 - International Conference on High Entropy Materials CY - Berlin, Germany DA - 27.09.2020 KW - High Entropy Alloys KW - Medium Entropy Alloys KW - High temperature corrosion KW - Oxidation KW - Sulfidation PY - 2020 AN - OPUS4-51488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klinger, Christian T1 - Systematische Schadensanalyse: Vergleich und Anwendung von Richtlinien und Prozeduren N2 - Recherche verschiedener jeweils nationaler/internationaler Regelwerke und Prozeduren für die Systematische Schadensanalyse • Literaturrecherche zu Methoden der systematischen interdisziplinären Schadensanalyse • Vergleich der Regelwerke VDI 3822, ASTM, ASM sowie der Methoden • Anwendung der Regelwerke/Prozeduren und Methoden am Beispiel T2 - 46. VDI Jahrestagung: Schadensanalyse in der Energietechnik CY - Online meeting DA - 06.10.2020 KW - Regelwerke KW - Systematische Schadensanalysen, Prozeduren PY - 2020 AN - OPUS4-51401 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Werner, Tiago A1 - Teske, Tanita A1 - Hilgenberg, Kai A1 - Mauro, Madia A1 - Nielsen, S. A1 - Gärtner, F. A1 - Klassen, T. T1 - Untersuchung des Potenzials von Kaltgasspritzen für die Reparatur zyklisch belasteter Bauteile T1 - Investigation on the capability of cold-spray for repair of cyclically loaded components N2 - Die Reparatur mittels Kaltgasspritzen ist eine vielversprechende Alternative zum teuren Austausch fehlerbehafteter Bauteile in der Luft- und Raumfahrt. Im Rahmen dieser Arbeit wurde das Potential des Verfahrens an der hochfesten Aluminiumlegierungen Al6061-T6 unter Anwendung von Stickstoff als kostengünstiges Prozessgas untersucht. Es wurden quasi-statische Zugversuche und einachsige Zeitfestigkeitsversuche mit besonderem Fokus auf das in-situ Kugelstrahlen zur Verbesserung der mechanischen Eigenschaften durchgeführt. Im Ergebnis wurde die Verbesserung der Adhäsion zwischen Substrat und aufgebautem Werkstoff als entscheidendes Kriterium für eine Anwendbarkeit ermittelt. Die Laserstrukturierung von Substratoberflächen ist hierfür vielversprechend und wurde im Rahmen der Arbeit mittels Adhäsionsversuchen untersucht. N2 - Repair by cold-spray is a promising alternative to the costly replacement of flawed components in aerospace applications. In the present work this process was investigated on the high-strength aluminum alloy Al6061-T6. For the cold-spray process, inexpensive Nitrogen was used as process-gas. Quasi-static tensile and highcycle- fatigue tests (HCF) were performed, focusing on in-situ shot peening to improve the mechanical properties of the repaired part. An improved adhesion between substrate and built-up material was identified as a key-factor for the applicability of the process. Under this respect laser-structuring of the substrate surface was applied and its effect on the mechanical performance of the restored samples were examined by adhesion tests. T2 - 9. Tagung des DVM-Arbeitskreises Additiv gefertigte Bauteile und Strukturen CY - Stuttgart, Germany DA - 06.11.2024 KW - Kaltgasspritzen KW - cold-spray KW - Reparatur KW - Repair KW - Ermüdungsfestigkeit KW - Fatigue KW - Luft- und Raumfahrt KW - Aerospace KW - Substratvorbehandlung KW - Substrate pre-treatment PY - 2024 DO - https://doi.org/10.48447/ADD-2024-BB VL - 409 SP - 67 EP - 79 AN - OPUS4-63182 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Was, G.S. A1 - Bahn, C.-B. A1 - Busby, J. A1 - Cui, B. A1 - Farkas, D. A1 - Gussev, M. A1 - Rigen He, M. A1 - Hesterberg, J. A1 - Jiao, Z. A1 - Johnson, D. A1 - Kuang, W. A1 - McMurtrey, M. A1 - Robertson, I. A1 - Sinjlawi, A. A1 - Song, M. A1 - Stephenson, K. A1 - Sun, K. A1 - Swaminathan, Srinivasan A1 - Wang, M. A1 - West, E. T1 - How irradiation promotes intergranular stress corrosion crack initiation N2 - Irradiation assisted stress corrosion cracking (IASCC) is a form of intergranular stress corrosion cracking that occurs in irradiated austenitic alloys. It requires an irradiated microstructure along with high temperature water and stress. The process is ubiquitous in that it occurs in a wide range of austenitic alloys and water chemistries, but only when the alloy is irradiated. Despite evidence of this degradation mode that dates back to the 1960s, the mechanism by which it occurs has remained elusive. Here, using high resolution electron backscattering detection to analyze local stress-strain states, high resolution transmission electron microscopy to identify grain boundary phases at crack tips, and decoupling the roles of stress and grain boundary oxidation, we are able to unfold the complexities of the phenomenon to reveal the mechanism by which IASCC occurs. The significance of the findings impacts the mechanical integrity of core components of both current and advanced nuclear reactor designs worldwide. KW - Irradiation KW - Stress corrosion cracking KW - Grain boundaries KW - Oxidation KW - Austenitic alloys PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595748 DO - https://doi.org/10.1016/j.pmatsci.2024.101255 SN - 0079-6425 VL - 143 SP - 1 EP - 15 PB - Elsevier AN - OPUS4-59574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weinel, Kristina T1 - Plasmonic Behavior in Assemblies of Disordered Gold Nanoparticles N2 - Plasmons are collective oscillations of the free electron density in metals which can be described by an electromagnetic field. Surface plasmons are longitudinal waves propagating at the surface of the metallic material coupled to an external field. Localized surface plasmons on a nanoparticle reveal the behavior of standing waves with discrete resonance frequencies whose dominating mode is called dipole mode. Coupling of nanoparticles leads eventually to a hybridization of those dipole modes and therefore to spectral and spatial delocalization which was already investigated in ordered systems. In disordered systems, there are a lot of open questions regarding the propagation behavior which changes from delocalization to localization for instance due to the disorder. This phenomenon is then called Anderson localization. To investigate the propagation behavior of plasmonic waves in an assembly of disordered gold NPs, we combine experimental results of electron energy loss spectroscopy in a scanning transmission microscope with simulation results of the self-consistent dipole modelling. We indeed find experimentally localization of plasmon modes and with the simulation we could exclude other localization mechanism such as life-time damping or retardation. In conclusion, we could found Anderson localization of surface plasmons in assemblies of disordered gold nanoparticles which will enhance the understanding of this kind of vector waves to the Anderson localization as a general wave behavior in disordered systems. T2 - PhD seminar Leipniz Institut for solid state and material research (IFW Dresden) CY - Dresden, Germany DA - 19.06.2024 KW - Plasmonic KW - EELS in STEM KW - Self-consistent dipole model KW - Assemblies of gold nanoparticles PY - 2024 AN - OPUS4-60945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wojciak, K. A1 - Tokarski, T. A1 - Cios, G. A1 - Nolze, Gert T1 - Precision and accuracy during standard-less mapping of local lattice distortions using ebsd and calm technique N2 - Electron Back Scatter Diffraction (EBSD) is a very versatile analytical technique allowing for the characterization of material structure. Historically, diffraction images (Kikuchi patterns) registered during EBSD analysis were solved using Hough/Radon transformation. The last decade brought several novel techniques of experimental pattern analysis, focusing entirely on image analysis routines such as pattern matching, or various variants of High-Resolution EBSD. However, all the above-mentioned techniques require prior knowledge of the material structure to perform orientation analysis. The recently presented algorithm employed in Crystallographic Analysis of Lattice Metric (CALM) software, effectively removes this limitation enabling a standard-less analytical approach in EBSD systems. At its core, the CALM technique couples accurate detection of the Kikuchi bands position, with a rigid construction of reciprocal lattice resulting from translational crystal symmetry. A unique characteristic of the methodology also gives an opportunity for application in the analysis of continuous lattice changes, for example tetragonality mapping. During mapping, however, the geometry of the gnomonic projection (represented by the projection center) is continuously altered decreasing overall algorithm efficiency. The work presents an analysis of the projection center in terms of precision and accuracy. T2 - Oxford User Meeting 2024 CY - Krakow, Poland DA - 14.05.2024 KW - EBSD KW - Kikuchi KW - Lattice parameters KW - Ratio refinement PY - 2024 AN - OPUS4-60087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tokarski, T. A1 - Nolze, Gert T1 - Exploring Unconventional Uses of Kikuchi Pattern Analysis N2 - The characterization of really unknown phases typically uses 70 to 150 reflectors for lattice metric calculation. The determination of the lattice parameters follows with 4% accuracy. Including a Z correction up to 1% can be reached. The precision of the lattice parameters ratios (a:b:c) is, however, better than 0.1%. T2 - Oxford Users Meeting 2024 CY - Krakow, Poland DA - 14.05.2024 KW - EBSD KW - Kikuchi KW - Lattice parameters KW - Ratio refinement PY - 2024 AN - OPUS4-60086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Wencke T1 - Effect of corrosive atmosphere on the oxidation behavior of CrMnFeCoNi and CrCoNi alloys N2 - High- and medium-entropy alloys (HEAs and MEAs) constitute a new class of materials. Those with a face-centered cubic (fcc) structure from the Cr-Mn-Fe-Co-Ni system have excellent mechanical properties and are considered for high-temperature applications since diffusion in these alloys was reported to be sluggish. However, their corrosion resistance at high temperatures must still be evaluated to further qualify them for such kinds of applications. Various groups studied the oxidation behavior of HEAs and MEAs under (dry) laboratory and artificial air as well as CO2/CO mixtures in different temperature ranges. Adomako et al. carried out oxidation tests in dry air between 800 °C and 1000 °C for 24 h in equiatomic CrCoNi, CrMnCoNi, and CrMnFeCoNi alloys. The authors showed that CrCoNi exhibits the best corrosion resistance at 800 °C due to the formation of a protective Cr2O3 layer. The matrix below the oxide scale was reported to be correspondingly depleted in Cr. It was further shown that the addition of Mn and Fe to CrCoNi changes the phase composition of the oxide scale at 800 °C. A Mn2O3 layer was grown during oxidation on CrMnCoNi and CrMnFeCoNi and a Cr2O3 scale was formed at the matrix/oxide scale interface. Beneath these oxide layers, Mn- and Cr-depleted zones were detected. These phase morphologies demonstrate the inward diffusion of oxygen and outward diffusion of Cr and Mn resulting in the formation of Cr2O3 and Mn2O3. In the present study, the corrosion resistance of CrMnFeCoNi and CrCoNi were confirmed and additionally characterized under further oxidizing atmospheres at 800 °C including Ar-2 Vol.% O2, Ar-2 Vol.% H20, and Ar-2 Vol.% SO2 mixtures. T2 - 10th International Symposium on High-Temperature Corrosion and Protection of Materials CY - Online meeting DA - 28.03.2021 KW - High-entropy alloys KW - High-temperature corrosion KW - Chromium oxide KW - Manganese oxide PY - 2021 AN - OPUS4-53143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk T1 - Merkmale von alltäglichen Brüchen und wie wir daraus lernen können N2 - Schadensfälle aus dem Alltag erscheinen oft simpel, sind im Detail aber meist komplexer als erwartet und eröffnen die Möglichkeit, Merkmale zu studieren, Aufnahmetechniken und Bildbearbeitung zu optimieren und die Erfahrungen am Ende ohne Restriktionen weiter zu vermitteln. Beispielsweise verändern sich die mikroskopischen Merkmale von Schwingrissen über ihren Verlauf oft deutlich. Dies hängt von der Art des Werkstoffs und von den Beanspruchungsbedingungen ab. Die Bruchmerkmale werden schließlich systematisch dargestellt und ein Datensatz für die Fraktographische online-Datenbank der DVM/DGM AG Fraktographie erstellt, die fachöffentlich einsehbar ist. T2 - Metallographietagung 2024 CY - Berlin, Germany DA - 18.09.2024 KW - Fraktographie KW - Schadensanalyse PY - 2024 AN - OPUS4-61239 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Junge, Paul A1 - Rupprecht, Christian A1 - Sänger, Johanna A1 - Oedinghofen, Frank T1 - Thermisch gespritzte Schichten auf keramischen Hitzeschutzschilden für den Einsatz regenerativer Brennstoffe in stationäre Gasturbinen T1 - Thermally sprayed coatings on ceramic heat shields for the utilisation of regenerative fuels in stationary gas turbines N2 - Die Entwicklung zukünftiger Generationenvon stationären Gasturbinen verfolgt das Hauptziel, den thermischen Wirkungsgrad zu erhöhen, bei gleichzeitiger Reduktion der CO2-Emissionen. Ein mögliches Lösungskonzept besteht darin, bestehende Turbinenkonzepte auf nachhaltig erzeugten Wasserstoff umzustellen. Durch den Betrieb mit Wasserstoff entsteht eine erhöhte Belastung für konventionelle thermische Hitzeschutzkomponenten. Daher ist die Entwicklung von sogenannte Environmental Barrier Coatings (EBC) oder Materialkonzepten, die eine thermodynamische Stabilität in heißer Gasumgebung aufweisen, erforderlich. N2 - The development of future generations of stationary gas turbines is pursuing the main objective of increasing the thermal efficiency, with a simultaneous reduction in the CO2 emissions. One possible solution concept consists of converting existing turbine concepts to sustainably produced hydrogen. The operation with hydrogen results in increased loads for conventional thermal heat protection components. Therefore, it is necessary to develop so-called environmental barrier coatings (EBCs) or material concepts which exhibit thermodynamic stability in a hot gas environment KW - Keramischen Hitzeschutzschilden KW - Thermische Spritzschichten KW - Gasturbine PY - 2024 UR - https://www.thermal-spray-bulletin.info/en/article/thermisch-gespritzte-schichten-auf-keramischen-hitzeschutzschilden-fuer-den-einsatz-regenerativer-brennstoffe-in-stationaeren-gasturbinen IS - 2 SP - 100 EP - 103 PB - DVS Media AN - OPUS4-61066 LA - mul 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 - Lemiasheuski, Anton A1 - Wehrkamp, F. A1 - Bajer, Evgenia A1 - Sonnenburg, Elke A1 - Göbel, Artur A1 - Porohovoj, Ilja A1 - Bettge, Dirk A1 - Pfennig, Anja T1 - Practical application of an automated 3D metallography system for the reconstruction and microstructural analysis of porosity in a sintered steel N2 - In the 3D microstructural analysis of a digital twin of porosity in the sintered steel Astaloy CrA, pore shape, average pore size as well as pore distribution will be analyzed. Porosity plays a major role in powder-metallurgical materials since it greatly impacts the mechanical properties of these materials and therefore represents a key parameter in their characterization. Based on the robot-assisted automated serial sectioning and imaging (RASI) system of the Federal Institute for Materials Research and Testing (BAM, Bundesanstalt für Materialforschung und Prüfung) in Berlin, the technique of metallographic serial sectioning will be used to image the microstructure and reconstruct a digital 3D twin from the stack of images obtained. Compared with an individual 2D microsection, the quantitative microstructural analysis of this 3D twin will enable more accurate conclusions on the shape, size and distribution of pores. This paper will detail the key steps in 3D microstructural analysis, including the metallographic preparation routine, the imaging technique, image alignment as well as the segmentation of pores. After the methodology has been described, the results of the quantitative microstructural analysis will be presented and the validity of quantitative parameters of 3D and 2D images will be compared and discussed. The analysis of more than 10,000 pores revealed a correlation between pore shape and pore size. It was also found that a 2D representation of the material surface is insufficient for a precise quantitative characterization of porosity. N2 - In der 3D-Gefügeanalyse eines digitalen Zwillings von Poren in einem Sinterstahl des Typs Astaloy CrA werden sowohl die Porenform als auch die durchschnittliche Porengröße und -verteilung analysiert. Die Porosität spielt in pulvermetallurgischen Werkstoffen eine große Rolle, da sie erheblich die mechanischen Eigenschaften beeinflusst und daher bei der Charakterisierung dieser Werkstoffe ein wichtiger Parameter ist. Basierend auf der Verwendung des Robot-Assisted Automated Serial-Sectioning and Imaging (RASI)-Systems der Bundesanstalt für Materialforschung und Prüfung (BAM) in Berlin, wird das metallographische Serienschnittverfahren genutzt, um das Gefüge aufzunehmen und aus dem Bildstapel einen digitalen 3D-Zwilling zu rekonstruieren. Verglichen zu einem 2D-Einzelschliff ermöglicht die quantitative Gefügeanalyse dieses 3D-Zwillings präzisere Aussagen zu Porenform, -größe und -verteilung. Diese Arbeit beschreibt die wesentlichen Schritte, die für eine 3D-Gefügeanalyse nötig sind, darunter die metallografische Präparationsroutine, das Bildgebungs-Verfahren, das Alignment der Bilder sowie die Segmentierung der Poren. Im Anschluss an die methodische Darstellung werden die Ergebnisse der quantitativen Gefügeanalyse präsentiert und ein Vergleich zwischen der Aussagekraft der quantitativen Parameter von 3D- und 2D-Abbildungen diskutiert. Bei der Analyse von über 10.000 Poren konnte eine Korrelation zwischen der Form und der Porengröße aufgezeigt werden. Weiterhin konnte aufgezeigt werden, dass eine 2D-Abbildung der Werkstoffoberfläche nicht ausreichend für eine eindeutige quantitative Beschreibung der Porosität ist. KW - 3D Metallographie KW - RASI KW - Porenstruktur PY - 2025 DO - https://doi.org/10.1515/pm-2025-0049 SN - 2195-8599 VL - 62 IS - 8 SP - 516 EP - 535 PB - De Gruyter Brill AN - OPUS4-63930 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk T1 - Fraktographie mit Hilfe von klassischen Methoden und Machine Learning – bisherige Erfahrungen und Anwendung auf weitere Fragestellungen N2 - In der Schadensanalyse und bei der Bewertung von mechanischen Experimenten liefert die Fraktographie Informationen über die vorliegenden Bruchmerkmale und den Bruchmechanismus eines Bauteils oder einer Probe. Im Rahmen des DGM AK Fraktographie werden an metallischen Werkstoffen Vergleichsexperimente durchgeführt und die Ergebnisse in einer Datenbank zur Verfügung gestellt. In einem Vorhaben wurde die Analyse von Bruchmerkmalen mittels Topographie-Daten und Machine Learning erprobt. Die gewonnenen Erfahrungen könnten auf weitere Anwendungsfälle wie z.B. Schweißverbindungen angewendet werden. T2 - Erfahrungsaustausch Werkstoff- und Bauteilprüfung CY - Halle, Germany DA - 04.09.2025 KW - Fraktographie KW - Machine Learning KW - Schadensanalyse KW - Schweißverbindungen PY - 2025 AN - OPUS4-64032 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehmusto, Juho T1 - Initial oxidation of the refractory high-entropy superalloy AlMo0.5NbTa0.5TiZr N2 - In contrast to traditional alloys, which are typically based on a single dominant element, high-entropy alloys (HEAs) consist of five or more principal elements in roughly equal proportions. These complex alloys often exhibit superior characteristics compared to conventional alloys, including enhanced strength and hardness, exceptional wear resistance, high structural stability, and strong resistance to oxidation. Despite these promising characteristics, the vast compositional space of HEAs means that only a limited number have been thoroughly investigated for their mechanical and chemical behavior. One notable example is the refractory high-entropy superalloy AlMo0.5NbTa0.5TiZr, which represents a newly emerging class of materials. This alloy features a nanoscale microstructure composed of B2 and bcc phases, resulting in compressive strength at elevated temperatures that surpasses that of conventional Ni-based superalloys. Such performance offers potential benefits for improving turbine efficiency in aerospace and energy generation applications. However, the alloy’s microstructure is known to be sensitive to annealing. Specifically, its mechanical properties deteriorate when intragranular hexagonal Al-Zr-based intermetallic compounds form, likely due to issues with phase stability. On the other hand, the inclusion of Al has been shown to enhance oxidation resistance. Nevertheless, HEAs are also known to develop pronounced internal aging zones caused by diffusion during oxidation processes. These findings indicate a need for further investigation into the thermodynamic stability of this alloy. In addition, its oxidation behavior—both at the surface and within the material—remains incompletely understood. This ongoing research explores the oxidation behavior of the AlMo0.5NbTa0.5TiZr alloy at temperatures ranging from 800 °C to 1000 °C. The influence of water vapor on the oxidation process is also examined. Ultimately, the goal is to integrate insights into the alloy’s structural, mechanical, and chemical characteristics at high temperatures. T2 - Gordon Research Conference - High Temperature Corrosion CY - New London, United States DA - 16.07.2023 KW - High-Entropy superalloy KW - Phase stability KW - Microstructural evolution KW - Oxidation behavior KW - High-Temperature Performance PY - 2023 AN - OPUS4-63851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madia, Mauro T1 - Damage Tolerant Approach in Additively Manufactured Metallic Materials N2 - Damage tolerance counts as one of the most widespread approach to fatigue assessment and surely as one of the most promising in understanding the process-structure-property-performance relationships in additively manufactured metallic materials. Manufacturing defects, surface roughness, microstructural features, short and long crack fatigue propagation, residual stresses and applied loads can be taken into consideration in a fracture mechanics-based fatigue assessment. Many aspects are crucial to the reliable component life prediction. Among those a prominent role is played by an accurate measurement and modelling of the short crack fatigue behavior, and reliable statistical characterization of defects and residual stresses. This work aims at addressing the issues related to both experimental testing, fatigue and fatigue crack propagation, and fracture mechanics-based modelling of fatigue lives. Examples will be provided on an additively manufactured AISI 316 L. T2 - TMS2021 VIRTUAL CY - Online meeting DA - 15.03.2021 KW - AISI 316L KW - Additive Manufacturing KW - Damage Tolerance KW - Microstructure KW - Defects KW - Residual Stress PY - 2021 AN - OPUS4-52293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohr, Gunther A1 - Sommer, Konstantin A1 - Knobloch, Tim A1 - Altenburg, Simon A1 - Recknagel, Sebastian A1 - Bettge, Dirk A1 - Hilgenberg, Kai T1 - Process Induced Preheating in Laser Powder Bed Fusion Monitored by Thermography and Its Influence on the Microstructure of 316L Stainless Steel Parts N2 - Undetected and undesired microstructural variations in components produced by laser powder bed fusion are a major challenge, especially for safety-critical components. In this study, an in-depth analysis of the microstructural features of 316L specimens produced by laser powder bed fusion at different levels of volumetric energy density and different levels of inter layer time is reported. The study has been conducted on specimens with an application relevant build height (>100 mm). Furthermore, the evolution of the intrinsic preheating temperature during the build-up of specimens was monitored using a thermographic in-situ monitoring set-up. By applying recently determined emissivity values of 316L powder layers, real temperatures could be quantified. Heat accumulation led to preheating temperatures of up to about 600 °C. Significant differences in the preheating temperatures were discussed with respect to the individual process parameter combinations, including the build height. A strong effect of the inter layer time on the heat accumulation was observed. A shorter inter layer time resulted in an increase of the preheating temperature by more than a factor of 2 in the upper part of the specimens compared to longer inter layer times. This, in turn, resulted in heterogeneity of the microstructure and differences in material properties within individual specimens. The resulting differences in the microstructure were analyzed using electron back scatter diffraction and scanning electron microscopy. Results from chemical analysis as well as electron back scatter diffraction measurements indicated stable conditions in terms of chemical alloy composition and austenite phase content for the used set of parameter combinations. However, an increase of the average grain size by more than a factor of 2.5 could be revealed within individual specimens. Additionally, differences in feature size of the solidification cellular substructure were examined and a trend of increasing cell sizes was observed. This trend was attributed to differences in solidification rate and thermal gradients induced by differences in scanning velocity and preheating temperature. A change of the thermal history due to intrinsic preheating could be identified as the main cause of this heterogeneity. It was induced by critical combinations of the energy input and differences in heat transfer conditions by variations of the inter layer time. The microstructural variations were directly correlated to differences in hardness. KW - Additive manufacturing KW - Laser powder bed fusion KW - In-situ process monitoring KW - Thermography KW - Heat accumulation KW - Inter layer time KW - Cellular substructure PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529240 DO - https://doi.org/10.3390/met11071063 VL - 11 IS - 7 SP - 1063 PB - MDPI CY - Basel, Schweiz AN - OPUS4-52924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Manzoni, Anna Maria A1 - Schneider, M. A1 - Laplanche, G. T1 - Welding of high-entropy alloys and compositionally complex alloys - an overview N2 - High-entropy alloys (HEAs) and compositionally complex alloys (CCAs) represent new classes of materials containing five or more alloying elements (concentration of each element ranging from 5 to 35 at. %). In the present study, HEAs are defined as single-phase solid solutions; CCAs contain at least two phases. The alloy concept of HEAs/CCAs is fundamentally different from most conventional alloys and promises interesting properties for industrial applications (e.g., to overcome the strength-ductility trade-off). To date, little attention has been paid to the weldability of HEAs/CCAs encompassing effects on the welding metallurgy. It remains open whether welding of HEAs/CCAs may lead to the formation of brittle intermetallics and promote elemental segregation at crystalline defects. The effect on the weld joint properties (strength, corrosion resistance) must be investigated. The weld metal and heat-affected zone in conventional alloys are characterized by non-equilibrium microstructural evolutions that most probably occur in HEAs/CCAs. The corresponding weldability has not yet been studied in detail in the literature, and the existing information is not documented in a comprehensive way. Therefore, this study summarizes the most important results on the welding of HEAs/CCAs and their weld joint properties, classified by HEA/CCA type (focused on CoCrFeMnNi and AlxCoCrCuyFeNi system) and welding process. KW - High-entropy alloy KW - Compositionally complex alloy KW - Welding KW - Properties KW - Review PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527068 DO - https://doi.org/10.1007/s40194-021-01110-6 SP - 1 EP - 15 PB - Springer Nature AN - OPUS4-52706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, M. A1 - Diercks, P. A1 - Manzoni, Anna Maria A1 - Čížek, J. A1 - Ramamurty, U. A1 - Banhart, J. T1 - Positron annihilation investigation of thermal cycling induced martensitic transformation in NiTi shape memory alloy N2 - Thermal cycling of a Ni-excess NiTi alloy was conducted between 50 °C and liquid nitrogen temperature to induce martensitic transformations and to reverse them after. The starting point was an annealed and slowly cooled state, the end point a sample thermally cycled 1500 times. Positron annihilation lifetime spectra and Coincidence Doppler Broadening profiles were obtained in various states and at various tem- peratures. It was found that the initial state was low in defects with positron lifetimes close to that of bulk NiTi. Cycling lead to a continuous build-up of a defect structure up to 20 0 −50 0 cycles after which saturation was reached. Two types of defects created during cycling were identified, namely pure dislo- cations and vacancies attached to dislocations. KW - Shape memory alloy KW - Thermal Cycling KW - Defects KW - Positron annihilation spectroscopy KW - Austenite-to-martensite phase transformation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533641 DO - https://doi.org/10.1016/j.actamat.2021.117298 VL - 220 SP - 117298 PB - Elsevier Ltd. AN - OPUS4-53364 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 - Yesilcicek, Yasemin A1 - Haas, S. A1 - Suárez Ocano, Patricia A1 - Zaiser, E. A1 - Hesse, René A1 - Többens, D. M. A1 - Glatzel, U. A1 - Manzoni, Anna Maria T1 - Controlling Lattice Misfit and Creep Rate Through the γ' Cube Shapes in the Al10Co25Cr8Fe15Ni36Ti6 Compositionally Complex Alloy with Hf and W Additions N2 - Trace elements play an important role in the fine-tuning of complex material properties. This study focuses on the correlation of microstructure, lattice misfit and creep properties. The compositionally complex alloy Al10Co25Cr8Fe15Ni36Ti6 (in at. %) was tuned with high melting trace elements Hf and W. The microstructure consists of a γ matrix, γ' precipitates and the Heusler phase and it is accompanied by good mechanical properties for high temperature applications. The addition of 0.5 at.% Hf to the Al10Co25Cr8Fe15Ni36Ti6 alloy resulted in more sharp-edged cubic γ′ precipitates and an increase in the Heusler phase amount. The addition of 1 at.% W led to more rounded γ′ precipitates and the dissolution of the Heusler phase. The shapes of the γ' precipitates of the alloys Al9.25Co25Cr8Fe15Ni36Ti6Hf0.25W0.5 and Al9.25Co25Cr8Fe15Ni36Ti6Hf0.5W0.25, that are the alloys of interest in this paper, create a transition from the well-rounded precipitates in the alloy with 1% W containing alloy to the sharp angular particles in the alloy with 0.5% Hf. While the lattice misfit has a direct correlation to the γ' precipitates shape, the creep rate is also related to the amount of the Heusler phase. The lattice misfit increases with decreasing corner radius of the γ' precipitates. So does the creep rate, but it also increases with the amount of Heusler phase. The microstructures were investigated by SEM and TEM, the lattice misfit was calculated from the lattice parameters obtained by synchrotron radiation measurements. KW - High entropy alloy KW - Lattice misfit KW - Creep KW - Transmission electron microscopy KW - X-ray diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565655 DO - https://doi.org/10.1007/s44210-022-00009-1 SP - 1 EP - 9 PB - Springer AN - OPUS4-56565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haas, S. A1 - Manzoni, Anna Maria A1 - Holzinger, M. A1 - Glatzel, U. T1 - Influence of high melting elements on microstructure, tensile strength and creep resistance of the compositionally complex alloy Al10Co25Cr8Fe15Ni36Ti6 N2 - Due to its matrix/γ′ structure, the compositionally complex alloy (CCA) Al10Co25Cr8Fe15Ni36Ti6 has excellent properties that fulfill the requirements for a high-temperature material. This base alloy is alloyed with small amounts of high melting elements to a further improvement of its properties, which results in different shapes, fractions and sizes of the two phases γ′ and Heusler after various homogenization and annealing steps. By correlating this microstructure with time independent and dependent mechanical properties, conclusions can be drawn about the effects of the individual phases. The needle-shaped Heusler-phase leads to bad mechanical behavior if its phase fraction is too high. A fraction below 3 vol% is not critical in tensile tests, but it reduces the creep resistance compared to a purely two-phase matrix/γ′-alloy. Sharp-edged cubic γ′-particles and a coarse Heusler-phase without sharp edges in case of the base alloy with 0.5 at.% hafnium lead to the best tensile and creep properties in the high temperature range. At 750 °C, the Hf-containing alloy clearly outperforms two commercially used alloys in the targeted area of application when it comes to creep resistance. KW - High entropy alloy KW - Creep KW - Microstructure PY - 2021 DO - https://doi.org/10.1016/j.matchemphys.2021.125163 SN - 0254-0584 VL - 274 SP - 1 EP - 10 PB - Elsevier CY - Amsterdam AN - OPUS4-53175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -