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 - THES A1 - Schilling, Markus T1 - Environmental Stress Cracking (ESC) and Slow Crack Growth (SCG) of PE-HD induced by external fluids N2 - High-density polyethylene (PE-HD) is widely used as a packaging material. Typical applications are pipes and containers for storage and transport of dangerous goods. For these applications, the understanding of the craze-crack damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC) is of importance. Since these mechanisms are considered to be the major causes of failure, their understanding is essential for inspection and release of those materials. A well-established test method for the assessment of these damage mechanisms is the full-notch creep test (FNCT). It is used in this study for a detailed investigation of crack propagation phenomena in PE-HD container materials under the influence of different fluids such as air, water and aqueous detergent solutions (Arkopal N 100) as well as biodiesel and diesel. Based on the results of the FNCT, a classification scheme of different fluids is proposed, which allows for an assignment of the respective damage mechanisms. Hereby, it is differentiated between (i) inert, (ii) purely surface-active and (iii) additionally sorptive, bulk-active fluids with respect to SCG. If the test fluid changes the intrinsic properties (at the surface or in the bulk), the damage mechanism is addressed to ESC behavior. In FNCT investigations, stress, temperature and specimen geometry were varied systematically. In addition to the time to failure as common measure for the resistance of a PE-HD type against crack propagation, specimen elongation was considered in detail. Several imaging techniques were applied for fracture surface analysis of specimens tested in FNCT to gain novel information on SCG and ESC behavior. From height profiles obtained by laser scanning microscopy (LSM) and information on surface structures from scanning electron microscopy (SEM), indicators for the differentiation of the crack propagation mechanisms could be derived. Based on the LSM data, an algorithm for the distinction between ductile shear deformation and brittle crack growth as dominating failure mechanism was developed. Imaging techniques were also used for determination of crack propagation rates, which were related to time-resolved FNCT elongation data. From the time-resolved determination of crack lengths of partly damaged FNCT specimens, an increasing length of craze zone with a progressively propagating crack was revealed for the first time. This relation of crack and craze zones was specified by fracture mechanical considerations. N2 - Polyethylen hoher Dichte (PE-HD) wird als Werkstoff für Rohre und Behälter für den Transport und zur Lagerung von Gefahrgütern verwendet. Für die Beurteilung und technische Freigabe dieser Materialien ist das Verständnis der beiden Schädigungsmechanismen „langsames Risswachstum“ (engl.: „slow crack growth“, SCG) und „umgebungsbedingter Spannungsriss“ (engl.: „environmental stress cracking“, ESC) essentiell. Eine etablierte Prüfmethode zur Bewertung dieser Schädigungsmechanismen ist der Full-Notch Creep Test (FNCT), der in dieser Arbeit zur systematischen Untersuchung des Risswachstums in PE-HD Behältermaterialien unter Einwirkung von Luft, Wasser und wässrigen Netzmittellösungen (Arkopal N 100) sowie Biodiesel und Diesel verwendet wird. Aus den Ergebnissen des FNCT wird ein Klassifikationsschema für Fluide vorgeschlagen, welches ebenfalls eine Zuordnung zu den Schädigungsmechanismen erlaubt. Hierbei wird in (i) inerte, (ii) rein oberflächen-aktive und (iii) zusätzliche sorptive, volumen-aktive Fluide hinsichtlich des langsamen Risswachstums (SCG) unterschieden. Wenn ein Fluid lokal die intrinsischen Materialeigenschaften des Polymers verändert, wird der Schädigungsmechanismus dem umgebungsbedingten Spannungsriss (ESC) zugeordnet. Bei den FNCT-Untersuchungen wurden die mechanische Spannung, die Temperatur und die Prüfkörpergeometrie systematisch variiert. Zusätzlich zur Standzeit wurde die Prüfkörperdehnung zeitabhängig erfasst. Aus einer erweiterten Bruchflächenanalyse konnten neuartige Informationen über SCG und ESC erhalten werden. Hierzu wurden verschiedene Bildgebungsverfahren verwendet. Insbesondere wurden mit Laserscanningmikroskopie (LSM) Höhenprofile und mit Rasterelektronenmikroskopie (REM) Oberflächeninformationen zur Charakterisierung der Rissfortschrittsmechanismen erhalten. Auf Basis der LSM wurde unter Zuhilfenahme von Höhenprofildaten ein Algorithmus zur Unterscheidung zwischen duktiler Scherverformung und sprödem Risswachstum als dominierende Schädigungsmechanismen entwickelt. Die aus den bildgebenden Verfahren ermittelten Rissfortschrittsraten konnten mit den Daten der während des FNCT erfassten Dehnung der Prüfkörper in Beziehung gesetzt werden. Weiterhin wurde mithilfe von zeitaufgelösten Risslängendaten erstmals eine direkte Korrelation der Risslänge zu vorgeschädigten, fibrillierten Bereichen (Crazes) im PE-HD Prüfkörper während des FNCT nachgewiesen. Demnach vergrößert sich die Craze-Länge linear mit zunehmender Risslänge. Dieser Zusammenhang zwischen Riss- und Craze-Längen wurde auf mathematisch, bruchmechanischer Grundlage bestätigt. KW - High-density polyethylene (PE-HD) KW - Full-Notch Creep Test (FNCT) KW - Slow crack growth (SCG) KW - Environmental Stress Cracking (ESC) KW - Biodiesel KW - Diesel KW - Crack propagation analysis KW - Fracture Surface Analysis KW - Test Improvement KW - Imaging PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:tuda-tuprints-115443 DO - https://doi.org/10.25534/tuprints-00011544 SP - 1 EP - 212 CY - Darmstadt AN - OPUS4-50941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheuerlein, C. A1 - Andrieux, J. A1 - Michels, M. A1 - Lackner, F. A1 - Chiriac, R. A1 - Hagner, M. A1 - Di Michiel, M. A1 - Meyer, Christian A1 - Toche, F. ED - Foley, C. P. T1 - Effect of the fabrication route on the phase and volume changes during the reaction heat treatment of Nb3Sn superconducting wires N2 - Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation. KW - Nb3Sn KW - Microstructure KW - Phase transformations KW - Volume changes KW - X-ray diffraction KW - Differential scanning calorimetry KW - Synchrotron micro-tomography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505128 DO - https://doi.org/10.1088/1361-6668/ab627c VL - 33 IS - 3 SP - 034004 PB - IOP Publishing CY - Bristol (UK) AN - OPUS4-50512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghafafian, Carineh T1 - Localized repairs for wind turbine rotor blades N2 - The effect of localized repairs on the structural integrity and thus the lifespan of wind turbine rotor blade shells is examined. T2 - SAMPE Symposium 2020 CY - Kassel, Germany DA - 17.02.2020 KW - GFRP KW - Wind turbine blade shells KW - Scarf joint repairs KW - Sandwich PY - 2020 AN - OPUS4-50480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Applied Crystallography as a tool for a better understanding of Fundamental Questions of high temperature corrosion phenomena N2 - Corrosion Science Meets X-Rays, Neutrons and Electrons. The presentation gives an overview on current research activities applying in-situ X-ray diffraction and spectroscopy for a better understanding of fundamental mechanisms of high temperature corrosion. Additionally the knowledge gain by applying neutron powder diffraction and EBSD analysis is presented. T2 - Joint meeting of german and polish crystallographic association 2020 CY - Wroclaw, Poland DA - 24.02.2020 KW - Corrosion KW - Oxidation KW - In situ KW - Diffraction PY - 2020 AN - OPUS4-50483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Cios, G. A1 - Winkelmann, A. T1 - Manual measurement of angles in backscattered and transmission Kikuchi diffraction patterns N2 - A historical tool for crystallographic analysis is provided by the Hilton net, which can be used for manually surveying the crystal lattice as it is manifested by the Kikuchi bands in a gnomonic projection. For a quantitative analysis using the Hilton net, the projection centre as the relative position of the signal source with respect to the detector plane needs to be known. Interplanar angles are accessible with a precision and accuracy which is estimated to be ≤0.3o. Angles between any directions, e.g. zone axes, are directly readable. Finally, for the rare case of an unknown projection-centre position, its determination is demonstrated by adapting an old approach developed for photogrammetric applications. It requires the indexing of four zone axes [uvw]i in a backscattered Kikuchi diffraction pattern of a known phase collected under comparable geometric conditions. KW - Electron backscatter diffraction KW - EBSD KW - Angle measurement KW - Gnomonic projections KW - Kikuchi patterns PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507625 DO - https://doi.org/10.1107/S1600576720000692 VL - 53 SP - 435 EP - 443 AN - OPUS4-50762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matz, R. A1 - Rabe, Torsten A1 - Töpfer, J. A1 - Ziesche, S. T1 - Circuit-Board-Integrated Transformers Design and Manufacture N2 - Transformers couple two sections of a circuit by electromagnetic induction. They are widely used to either transform alternating voltage levels or to transmit power or signals across galvanic isolation. Both of these functions are essential for the operation of sensors and controllers. Covering all aspects from idea to circuit performance and from design to manufacture, this paper presents the first comprehensive description of the making of miniaturized, rugged, up-to-100W transformers for embedding into multilayer circuit boards. For circular coils, the well-manageable Ampere-Laplace law is shown to yield reliable designs, predicting correctly the performance of manufactured hardware. This enables fast design without lengthy finite element modelling. In the low-power linear regime, basic relations describe how the device’s characteristics evolve from the material properties and device structure. While scattering Parameters are useful for the analysis of isolated transformers with their intrinsic parasitics, the interaction with the components of the final circuit and the aspects of power and efficiency are addressed by chain matrixes. While these design rules are similar for multilayer boards of different material (like epoxy, Teflon, ceramics), the manufacturing of ceramic board transformers is considered here in detail. Low-temperature-cofired ceramic (LTCC) boards being sintered at 900 °C are particularly suited for harsh environments with chemical or thermal stress as frequently found at sensor positions. The transformer performance usually benefits from or even requires an integrated ceramic core of higher permeability, a ferrite, to shape the magnetic flux. Methods to sinter ferrites inside a dielectric ceramic multilayerandto measure their performance are therefore described in detail.Asthe sintering behaviour of dielectricandmagnetic ceramics differs considerably, their simultaneous sintering is challenging.However, the sintering temperatures of the usefulMnZnand NiZnCu ferrites can be lowered to that of the dielectric material with only moderate loss of permeability by glass additives. Furthermore, thermal mismatch between materials causes catastrophic failure or at least stress and loss of magnetic performance during cooling to room temperature after sintering. This is avoidable by either adjusting the thermal expansion coefficient of the ferrite or by enclosing the ferrite between stressreleasing separation layers.We present the state of the art in materials development according to the first approach as well as fully functional devices made with the second technique. Other applications not directly addressed but well related to this work are characterized by low load resistance in relation to the coil resistance of the transformer. Efficient power transmission then requires that technological solutions are applied to achieve the lowest possible resistive loss inside the coils by an enlarged conductor cross-section. As this is particularly challenging for LTCC boards, a technique is discussed to fabricate conductor traces with a thickness larger than their width. KW - Multilayer ceramic technology KW - LTCC KW - Transformer PY - 2020 DO - https://doi.org/10.4416/JCST2019-00071 SN - 2190-9385 VL - 11 IS - 1 SP - 44 EP - 61 PB - Göller Verlag CY - Baden-Baden AN - OPUS4-50751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, A. A1 - Cios, G. A1 - Tokarski, T. A1 - Nolze, Gert A1 - Hielscher, R. A1 - Koziel, T. T1 - EBSD orientation analysis based on experimental Kikuchi reference patterns N2 - Orientation determination does not necessarily require complete knowledge of the local atomic arrangement in a crystalline phase. We present a method for microstructural phase discrimination and orientation analysis of phases for which there is only limited crystallographic information available. In this method, experimental Kikuchi diffraction patterns are utilized to generate a self-consistent master reference for use in the technique of Electron Backscatter Diffraction (EBSD). The experimentally derived master data serves as an application-specific reference in EBSD pattern matching approaches. As application examples, we map the locally varying orientations in samples of icosahedral quasicrystals observed in a Ti40Zr40Ni20 alloy, and we analyse AlNiCo decagonal quasicrystals. KW - EBSD KW - Quasicrystal KW - Crystal orientation KW - Pattern matching PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507611 DO - https://doi.org/10.1016/j.actamat.2020.01.053 VL - 188 SP - 376 EP - 385 PB - Elsevier Ltd. AN - OPUS4-50761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina A1 - Sobek, P. T1 - Sintering of silver-alkali zinc borate glass composites N2 - High conductive silver-glass-metallization-pastes are key components in photovoltaics and advanced microelectronics. However, the underlying mechanisms of liquid phase sintering as silver dissolution, diffusion and reprecipitation are poorly understood so far. In the current work, the influence of different network modifier in alkali-zinc-borate paste-glasses on liquid phase sintering of silver-glass-composites was studied. Therefore, silver-glass-composites containing 30 vol% glass were prepared, using low melting X2O-ZnO-B2O3 glasses with X = Na, Li, and Rb (NZB, LZB, and RZB). Glass transition temperature, viscosity, glass-silver wetting, crystallization and sintering behavior was studied by means of thermal analysis, dilatometry, heating microscopy and microscopy. Similar glass transition temperatures of 450 °C (RZB), 460 °C (LZB) and 465 °C (NZB) were found by means of thermal analysis for glasses under study. Also, all glasses have a similar crystallization onset at about 550 °C, even though exhibiting with a different degree of crystallization. Despite these similarities, however, the sintering behavior, measured in terms of area shrinkage, significantly differs for the composites. This finding indicates a different degree of silver dissolution. Assuming that dissolved silver reduces the viscosity, this effect could explain why glass crystallization starts at lower temperature in the composites. For example, the crystallization peak of LZB at 629 °C measured for pure glass powder compacts was decreased to 586 °C for the composite. Confirmatively, microstructure analyses indicate different degrees of silver dissolution, as e.g. revealed by different amount of silver precipitates within the residual glass phase, and reprecipitation. Best silver dissolution appeared for the RZB glass. Nevertheless, the final densification of RZB was retarded probably due to swelling and crystallization. T2 - XRM Workshop CY - Halle, Germany DA - 03.03.2020 KW - Silver-glass-metallization-paste KW - Sintering KW - Alkali ions PY - 2020 AN - OPUS4-51243 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 -