TY - CONF A1 - Mieller, Björn T1 - Practical breakdown voltage calculations using dielectric breakdown strength reference values N2 - Dielectric breakdown is a catastrophic failure of ceramic substrates and insulators. The use of dielectric breakdown strength (DBS) reference values for the dimensioning of such components is not straightforward, as the DBS depends on sample thickness and electrode area. This fact also hampers a valid comparison of data taken from different literature sources. Based on the empirically confirmed proportionality of DBS to the reciprocal square root of sample thickness and an approach to account for the influence of electrode area on the failure probability, a practical equation is derived to calculate the breakdown voltage for arbitrary sample thickness and electrode area from one set of DBS reference data. To validate the equation, the AC DBS of commercial alumina substrates with thicknesses ranging from 0.3 mm to 1.0 mm was performed using different printed electrodes with varying areas. The breakdown voltages comprise a range from 18 kV for thick samples to 8.5 kV for thin samples, resulting in DBS values from 17 kV/mm for 1.0 mm thick samples to 29 kV/mm for 0.3 mm thin samples, all made from the same material. The influence of electrode area is comparatively smaller. The results calculated with the proposed equation are in reasonable accordance with the measured data. Thus, the equation can be applied for a proper comparison of literature DBS data measured in different setups and for a reasonable estimation of breakdown voltages in DBS tests and applications based on reference data. T2 - Electroceramics Conference XVII CY - Online meeting DA - 24.08.2020 KW - Ceramics KW - Dielectric breakdown KW - Weibull distribution PY - 2020 AN - OPUS4-51151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Machine learning assisted characterization of a Low Temperature Co-fired Ceramic (LTCC) module measured by synchrotron computed tomography. N2 - The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed. T2 - 54. Metallographie Tagung CY - Online meeting DA - 16.09.2020 KW - Machine Learning KW - LTCC KW - Synchrotron Tomography PY - 2020 AN - OPUS4-51299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Schönauer-Kamin, D. A1 - Moos, R. A1 - Reimann, T. A1 - Giovannelli, F. A1 - Rabe, Torsten T1 - Influence of pressure and dwell time on pressure‐assisted sintering of calcium cobaltite N2 - Calcium cobaltite Ca3Co4O9, abbreviated Co349, is a promising thermoelectric material for high‐temperature applications in air. Its anisotropic properties can be assigned to polycrystalline parts by texturing. Tape casting and pressure‐assisted sintering (PAS) are a possible future way for a cost‐effective mass‐production of thermoelectric generators. This study examines the influence of pressure and dwell time during PAS at 900°C of tape‐cast Co349 on texture and thermoelectric properties. Tape casting aligns lentoid Co349. PAS results in a textured Co349 microstructure with the thermoelectrically favorable ab‐direction perpendicular to the pressing direction. By pressure variation during sintering, the microstructure of Co349 can be tailored either toward a maximum figure of merit as required for energy harvesting or toward a maximum power factor as required for energy harvesting. Moderate pressure of 2.5 MPa results in 25% porosity and a textured microstructure with a figure of merit of 0.13 at 700°C, two times higher than the dry‐pressed, pressureless‐sintered reference. A pressure of 7.5 MPa leads to 94% density and a high power factor of 326 µW/mK2 at 800°C, which is 11 times higher than the dry‐pressed reference (30 MPa) from the same powder. KW - Hot pressing KW - Texture KW - Thermoelectric properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515973 DO - https://doi.org/https://doi.org/10.1111/jace.17541 SN - 0002-7820 VL - 104 IS - 2 SP - 917 EP - 927 PB - Wiley Periodicals LLC AN - OPUS4-51597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Altenburg, Simon A1 - Sprengel, Maximilian A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Fritsch, Tobias A1 - Mishurova, Tatiana A1 - Serrano-Munoz, Itziar A1 - Evans, Alexander A1 - Hofmann, M. A1 - Bruno, Giovanni T1 - Separation of the Formation Mechanisms of Residual Stresses in LPBF 316L N2 - Rapid cooling rates and steep temperature gradients are characteristic of additively manufactured parts and important factors for the residual stress formation. This study examined the influence of heat accumulation on the distribution of residual stress in two prisms produced by Laser Powder Bed Fusion (LPBF) of austenitic stainless steel 316L. The layers of the prisms were exposed using two different border fill scan strategies: one scanned from the centre to the perimeter and the other from the perimeter to the centre. The goal was to reveal the effect of different heat inputs on samples featuring the same solidification shrinkage. Residual stress was characterised in one plane perpendicular to the building direction at the mid height using Neutron and Lab X-ray diffraction. Thermography data obtained during the build process were analysed in order to correlate the cooling rates and apparent surface temperatures with the residual stress results. Optical microscopy and micro computed tomography were used to correlate defect populations with the residual stress distribution. The two scanning strategies led to residual stress distributions that were typical for additively manufactured components: compressive stresses in the bulk and tensile stresses at the surface. However, due to the different heat accumulation, the maximum residual stress levels differed. We concluded that solidification shrinkage plays a major role in determining the shape of the residual stress distribution, while the temperature gradient mechanism appears to determine the magnitude of peak residual stresses. KW - Additive Manufacturing KW - Laser Powder Bed Fusion KW - LPBF KW - AISI 316L KW - Online Process Monitoring KW - Thermography KW - Residual Stress KW - Neutron Diffraction KW - X-ray Diffraction KW - Computed Tomography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512903 DO - https://doi.org/10.3390/met10091234 VL - 10 IS - 9 PB - MDPI CY - Basel AN - OPUS4-51290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Advancing spray granulation by ultrasound atomization N2 - The influence of the atomization technique on the suitability of granules for dry pressing is the focus of the presented investigations. Therefore, destabilized alumina, zirconia, and zirconia toughened alumina (ZTA) slurries were spray dried and the obtained granules were used to fabricate green and finally sintered bodies for evaluation. Granules made in a laboratory spray dryer with a two-fluid nozzle served as a reference. An ultrasonic atomizer was integrated into the same spray dryer and the influence on the granule properties was evaluated. Untapped bulk density, granule size distribution, and flowability are among the evaluated granule-related properties as well as the granule yield which is used as an indicator of the process efficiency. Yield and flowability as most important granule properties are clearly improved when atomization is realized with ultrasound. The investigated sinter body properties include porosity, sinter body density, and biaxial strength and are as well positively affected by switching the atomization technique to ultrasound. Therefore, the Approach to improve the compressibility of granules by ultrasonic atomization, which leads to an improved microstructure, density, and strength of sintered bodies, has proven to be successful for single-component ceramics (alumina and zirconia) as well as for the multicomponent ceramic ZTA. KW - Alumina KW - Granules KW - Spray drying KW - Ultrasound KW - Zirconia KW - Zirconia-toughened alumina PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510696 DO - https://doi.org/10.1111/ijac.13534 VL - 17 IS - 5 SP - 2212 EP - 2219 AN - OPUS4-51069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. Imaging and the tensile test are run at the highest possible frame rate (0.7 s-1 ) and the lowest possible strain rate (5.5∙10-4 s -1 ). For 0°/90° non-crimp fabrics, the first inter-fiber cracks occur at 380 MPa (strain 0.8 %). Prior to failure at about 760 MPa (strain 2.0 %), we observe the evolution of nearly equidistant (1 mm distance) cracks running across the entire sample in the fully damaged state. KW - X-ray refraction KW - Diffraction Enhanced Imaging KW - Carbon Fiber Reinforced Plastics KW - In situ tensile test KW - Crack evolution PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515060 DO - https://doi.org/10.1088/1757-899X/942/1/012035 SN - 1757-8981 SN - 1757-899X VL - 942 SP - 012035-1 EP - 012035-9 PB - IOP publishing CY - Bristol, UK AN - OPUS4-51506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Creep and fracture behavior of conventionally and additively manufactured stainless steel 316L N2 - A critical task within the frame of establishing process-structure-property-performance relationships in additive manufacturing (AM) of metals is producing reliable and well-documented material behavior’s data and knowledge regarding the structure-property correlation, including the role of defects. After all, it represents the basis for developing more targeted process optimizations and more reliable predictions of performance in the future. Within this context, this contribution aims to close the actual gap of limited historical data and knowledge concerning the creep behavior of the widely used austenitic stainless steel 316L, manufactured by Laser-Powder-Bed-Fusion (L-PBF). To address this objective, specimens from conventional hot-rolled and AM material were tested under application-relevant conditions according to existing standards for conventional material, and microstructurally characterized before and after failure. The test specimens were machined from single blocks from the AM material. The blocks were manufactured using a standard scan and build-up strategy and were subsequently heat-treated. The creep behavior is described and comparatively assessed based on the creep lifetime and selected creep curves and characteristic values. The effect of defects and microstructure on the material’s behavior is analyzed based on destructive and non-destructive evaluations on selected specimens. The AM material shows shorter creep lives, reaches the secondary creep stage much faster and at a lower strain, and features lower creep ductility compared to its conventional counterpart. The creep damage behavior of the AM material is more microstructure than defect controlled and is characterized by the formation and accumulation of single intergranular damage along the whole volume. Critical features identified are the grain morphology and the grain-boundary as well as the dislocation’s density. Micro-computed tomography (µCT) proves to be an alternative to metallography to analyze the creep damage. T2 - ASTM International Conference on Additive Manufacturing 2020 CY - Online meeting DA - 16.11.2020 KW - 316L KW - Creep behavior KW - Laser powder bed fusion KW - Additive manufacturing KW - Microstructure PY - 2020 AN - OPUS4-51823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Assessing the low cycle fatigue behaviour of additively manufactured Ti-6Al-4V: Challenges and first results N2 - The understanding of process-microstructure-property-performance (PMPP) relationships in additive manufacturing (AM) of metals is highly necessary to achieve wide-spread industrial application and replace conventionally manufactured parts, especially regarding safety-relevant applications. To achieve this understanding, reliable data and knowledge regarding material’s microstructure-property relationships (e.g. the role of defects) is needed, since it represents the base for future more targeted process optimizations and more reliable calculations of performance. However, producing reliable material data and assessing the AM material behaviour is not an easy task: big challenges are e.g. the actual lack of standard testing methods for AM materials and the occasional difficulties in finding one-to-one comparable material data for the conventional counterpart. This work aims to contribute to end this lack of reliable material data and knowledge for the low cycle fatigue behaviour of the most used titanium alloy in aerospace applications (Ti-6Al-4V). For this purpose, two sets of test specimens were investigated. The first set was manufactured from cylindrical rods produced by an optimized DED-L process and the second was manufactured from a hot formed round bar. The test specimens were cyclically loaded until failure in the low-cycle-fatigue (LCF) regime. The tests were carried out according to ISO 12106 between 0.3 to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behaviour is described and compared between materials and with literature values based on cyclic deformation curves and strain-based fatigue life curves. Besides, the parameters of Manson-Coffin-Basquin relationship were calculated. The microstructures (initial and after failure) and fracture surfaces were comparative characterized. Thereby, the focus lied on understanding the role of grain morphology and defects on the failure mechanisms and fatigue lifetimes. For this latter characterization, optical microscopy (OM), scanning electron microscopy (SEM) and micro computed tomography (µCT) were used. T2 - 4th International Symposium on Fatigue Design and Material Defects CY - Online meeting DA - 26.05.2020 KW - Ti-6Al-4V KW - Additive manufacturing KW - Low cycle fatigue KW - Micro computed tomography KW - Microstructure PY - 2020 AN - OPUS4-50893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Czichos, Horst A1 - Skrotzki, Birgit ED - Hennecke, Manfred ED - Skrotzki, Birgit T1 - Anforderungen, Eigenschaften und Verhalten von Werkstoffen N2 - Die Eigenschaften verschiedener Werkstoffe werden behandelt und typische Werkstoffkennwerte angegeben. Es werden Arten der Beanspruchung von Bauteilen und Werkstoffen vorgestellt, die diese in technischen Anwendungen unterworfen sind. Im Betrieb von Bauteilen kann Materialschädigung und unter Umständen auch Versagen eintreten. Mögliche Mechanismen und Ursachen werden erläutert und Einblicke in die Methodik der Schadensanalyse gegeben. KW - Beanspruchung KW - Werkstoffkennwerte KW - Mechanische Eigenschaften KW - Thermophysikalische Eigenschaften KW - Schadenskunde KW - Alterung KW - Bruch KW - Korrosion KW - Tribologie KW - Werkstoffauswahl PY - 2020 DO - https://doi.org/10.1007/978-3-662-57492-8_29-1 SP - 1 EP - 45 PB - Springer-Verlag GmbH Deutschland AN - OPUS4-51286 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Portella, Pedro Dolabella A1 - Skrotzki, Birgit A1 - Muth, Thilo T1 - Die Digitalisierung der Materialwissenschaft und Werkstofftechnik - ein Überblick N2 - Die Bereitstellung von zuverlässigen Werkstoffdaten stand für die Werkstoffprüfung seit dem 19. Jahrhundert in zentraler Stelle. Mit der zunehmender Digitalisierung unserer Gesellschaft gewinnt das Datenmanagement insbesondere im Hinblick auf die Modellierungs- und Simulationsaktivitäten an Bedeutung. In unserem Beitrag beschreiben wir die gegenwärtigen Aktivitäten in Deutschland – insbesondere die NFDI-MatWerk und die BMBF-Initiative MaterialDigital – sowie in Europa und Übersee. Abschließend heben wir die Auswirkungen auf die technische und akademische Aus- und Weiterbildung. T2 - DVM - Tagung Werkstoffprüfung CY - Online meeting DA - 03.12.2020 KW - Werkstoffdaten KW - Digitalisierung KW - Materialwissenschaft PY - 2020 AN - OPUS4-52044 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Fine iron oxide nanoparticles as a candidate reference material for reliable measurement of particle size N2 - Background, Motivation and Objective Nanomaterials are at the core of some of the 21st century’s most promising technologies. In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important. Furthermore, the European Commission has taken measures via the REACH Regulations to control the classification of nanomaterials. REACH Annexes which entered into force in January 2020 require manufacturers to register nanomaterials that are traded in larger quantities (at least 1 ton). Every powder or dispersion where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as a nanomaterial. This creates a need for both industrial manufacturers and research and analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is working on developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution, but also targeting other key parameters such as shape, structure (including porosity) and functional properties. Thus, candidate materials are considered to complement the already available spherical and monodisperse silica, Au and polystyrene reference nanoparticles, e.g. iron oxide and titanium oxide, with an average atomic number between those of silica and gold. Particularly for the imaging by electron microscopies, new nanoparticles of well-defined size in the range of 10 nm are decisive for the accurate particle segmentation by setting precise thresholds. Statement of Contribution/Methods Synthesis: Highly monodisperse iron oxide nanoparticles can be synthesized in large quantities by thermal decomposition of iron oleate or iron acetylacetonate precursors in high boiling solvents such as octadecene or dioctyl ether in the presence of oleic acid and oleylamine as capping agents. Scanning Electron Microscope: An SEM of type Supra 40 from Zeiss has been used including the dedicated measurement mode transmission in SEM (STEM-in-SEM) with a superior material contrast for the nanoparticle analysis. The software package ImageJ has been used for the analysis of the STEM-in-SEM images and to determine the particle size distribution. Dynamic Light scattering (DLS): Particles in suspension were measured in comparison by means of Zetasizer Nano (Malvern Panalytical; cumulants analysis) and NanoFlex (Microtrac; frequency power spectrum). Results/Discussion In this study iron oxide nanoparticles synthesized at BAM and pre-characterized by DLS, SEM (including the transmission mode STEM-in-SEM) are presented. The particles are spherical and highly monodisperse with sizes slightly larger than 10 nm. T2 - Nanosafe 2020 CY - Online meeting DA - 16.11.2020 KW - Reference nanomaterials KW - Imaging techniques KW - Size and size distribution KW - Reliable characterization KW - Iron oxide nanoparticles PY - 2020 AN - OPUS4-51767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Jürgens, Maria T1 - Verhalten des hochwarmfesten Stahles P92 unter zyklischen thermo-mechanischen Bedingungen in lastflexiblen Dampfkraftwerken N2 - Die Erzeugung von Erneuerbaren Energien unterliegt starken Schwankungen, die von konventionellen Kraftwerken ausgeglichen werden müssen, um das Stromnetz stabil zu halten. Für die konventionellen Kraftwerke bedeutet dies eine zunehmend zyklische Fahrweise, die zu häufigeren Last- und Temperaturwechseln führt. Von den eingesetzten Werkstoffen fehlen Daten zum Verhalten unter zyklischer Fahrweise. Ziel dieser Arbeit ist es daher, für P92, einen als Rohrleitungswerkstoff eingesetzten hochwarmfesten Stahl, zu untersuchen, welche Auswirkungen zyklische Fahrweisen auf die Schädigungsprozesse und Lebensdauern haben. Da durch den zyklischen Betrieb eine verstärkte Schädigung durch Ermüdungsprozesse zu erwarten ist, wurden dehnungskontrollierte isotherme (LCF) und nicht-isotherme (TMF) Ermüdungsversuche mit und ohne Haltezeit bei verschiedenen Temperaturen bzw. Temperaturintervallen durchgeführt. Mit den Haltezeitversuchen soll dabei das Kriech-Ermüdungs-Verhalten untersucht werden. Bei den TMF-Versuchen wurde zusätzlich die Temperaturrate variiert, um näher an den realen Lastwechselgeschwindigkeiten zu prüfen. Schließlich wurden auf Basis der durchgeführten LCF- und TMF-Versuche betriebsnahe Versuchsprozeduren entwickelt, um unterschiedliche Betriebsmodi in einem Versuch abzubilden. Die durchgeführten mechanischen Versuche stellen eine umfangreiche Basis zu Ermüdungsdaten an P92 dar. Neben der Abhängigkeit der Lebensdauer von Temperatur, Temperaturintervall und –rate, sowie Dehnung und Haltezeit, konnte auch das Entfestigungsverhalten genauer charakterisiert werden. Sowohl Haltezeiten als auch das Reduzieren der Temperaturrate können die Lebensdauer erheblich verringern. Dabei kommt es gerade bei vermeintlich kleinen Dehnungen, bei denen die Streckgrenze nur leicht überschritten wird, zu einer Lebensdauerreduzierung. Haltezeiten verstärken zudem die zyklische Entfestigung. Die fraktographische Analyse der Proben hat ergeben, dass es keinen direkten Zusammenhang zwischen der Entfestigung und der Bildung von Nebenrissen gibt. Stattdessen zeigen EBSD- und TEM-Untersuchungen, dass es zur Bildung einer Subkornstruktur kommt und die Entfestigung auf dem Verschwinden von Kleinwinkelkorngrenzen beruht. Während bei den LCF-Proben eine reine Ermüdungsschädigung vorliegt, konnte bei einigen TMF-Proben eine kriechdominierende Schädigung nachgewiesen werden. Die betriebsnahen Zyklen zeigen, dass sich mit den durchgeführten Versuchen das reale Betriebsverhalten gut abschätzen lässt. Da es jedoch auch Parameterkombinationen gibt, bei denen keine Änderung des Entfestigungs- und Lebensdauerverhaltens auftritt, sollte genau bekannt sein, welche Belastungen in einem Bauteil auftreten. KW - P92 KW - LCF KW - TMF KW - Energiewende KW - Kriechermüdung KW - Energy transition KW - Creep-fatigue PY - 2020 DO - https://doi.org/10.14279/depositonce-10538 SP - 1 EP - 144 CY - Berlin AN - OPUS4-51571 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Melo Bernardino, Raphael A1 - Valentino, S. A1 - Franchin, G. A1 - Günster, Jens A1 - Zocca, Andrea T1 - Manufacturing of ceramic components with internal channels by a novel additive/subtractive hybridizazion process N2 - A new approach for fabrication of ceramic components with inner channels is proposed, as a result of the combination of two additive and one subtractive manufacturing processes. In this project, porcelain parts are manufactured by the Layerwise Slurry Deposition (LSD) process, meanwhile end milling and Direct Ink Writing (DIW) are applied to create channels on the surface of the deposited ceramic. Unique to the LSD process is the Formation of a freestanding powder bed with a mechanical strength comparable to conventional slip casted ceramic green bodies. Combining these three processes allows the manufacturing of ceramic objects containing an internal path of ink, which in this case was a graphite-based ink that can be further eliminated by heat treatment to obtain a porcelain object embedded with channels. The results show the capabilities of this method and its potential to fabricate not only parts with inner channels, but also multi-material and multi-functional components (such as integrated electronic circuits). KW - Additive Manufacturing KW - Layerwise Slurry Deposition KW - Hybrid Manufacturing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510012 UR - https://www.sciencedirect.com/science/article/pii/S2666539520300109?via%3Dihub DO - https://doi.org/10.1016/j.oceram.2020.100010 VL - 2 SP - 100010 PB - Elsevier Ltd. AN - OPUS4-51001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilbig, Janka A1 - Borges de Oliveira, F. A1 - Obaton, A.-F. A1 - Schwentenwein, M. A1 - Rübner, Katrin A1 - Günster, Jens T1 - Defect detection in additively manufactured lattices N2 - This paper investigates fast and inexpensive measurement methods for defect detection in parts produced by Additive Manufacturing (AM) with special focus on lattice parts made of ceramics. By Lithography-based Ceramic Manufacturing, parts were built both without defects and with typical defects intentionally introduced. These defects were investigated and confirmed by industrial X-ray Computed Tomography. Alternative inexpensive methods were applied afterwards on the parts such as weighing, volume determination by Archimedes method and gas permeability measurement. The results showed, that defects resulting in around 20% of change in volume and mass could be separated from parts free of defects by determination of mass or volume. Minor defects were not detectable as they were in the range of process-related fluctuations. Permeability measurement did not allow to safely identify parts with defects. The measurement methods investigated can be easily integrated in AM process chains to support quality control. KW - Additive manufacturing KW - Quality assurance KW - Defect detection KW - Lattices KW - Ceramics PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513547 DO - https://doi.org/10.1016/j.oceram.2020.100020 VL - 3 SP - 100020 PB - Elsevier Ltd. AN - OPUS4-51354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kratzig, A. A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Menneken, M. A1 - Bäßler, Ralph T1 - Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature N2 - The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products. KW - Corrosion KW - CCUS KW - In-situ ED-XRD KW - CO2 pipeline transport KW - Oxyfuel KW - Carbon steel KW - Impurities PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506303 DO - https://doi.org/10.3390/pr8040421 SN - 2227-9717 VL - 8 IS - 4 SP - 421-1 EP - 421-19 PB - MDPI CY - Basel AN - OPUS4-50630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Orlov, Nikolai A1 - Kiseleva, A. K. A1 - Milkini, P. A. A1 - Evdokimov, P. V. A1 - Putlayev, V. I. A1 - Günster, Jens T1 - Potentialities of Reaction Sintering in the Fabrication of High-Strength Macroporous Ceramics Based on Substituted Calcium Phosphate N2 - Calcium alkali metal (potassium and sodium) double and triple phosphates have been synthesized in different ways. Was for the first time used reaction sintering to produce ceramics based on calcium alkali metal mixed phosphates and investigated the densification behavior of mixed phosphate-based multiphase materials during sintering by this method. Was presented the microstructure of polished surfaces of sintered samples differing in phase composition and determined the density of ceramics prepared using reaction mixtures differing in composition. The effect of reaction sintering on the porosity of the ceramics has been assessed. Using stereolithographic printing and reaction sintering, was produced macroporous mixed Calcium phosphate-based ceramic implants. Their compressive strength has been determined to be 0.78 ± 0.21 MPa for two-phase samples and 1.02 ± 0.13 MPa for three-phase samples. KW - Reaction Sintering KW - Bio Ceramics PY - 2020 DO - https://doi.org/10.1134/s0020168520120146 VL - 56 IS - 12 SP - 1298 EP - 1306 PB - Pleiades Publishing LTD AN - OPUS4-52004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maaß, Robert T1 - Structural dynamics in metallic glasses due to Thermal and Mechanical Stress N2 - This talk addresses aging induced property changes of metallic glasses. Priority is given thermally and mechanically induced structural changes, of which the time-dependent dynamics is tracked using coherent scattering. Strong intermittency is observed and accelerated transport is seen at the smallest applied stresses. These findings have significant implications for how metallic glass components respond in realistic service conditions. T2 - Seminar Universität Münster 2020 CY - Münster, Germany DA - 01.12.2020 KW - Metallic glasses KW - Structure PY - 2020 AN - OPUS4-60714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karl, D. A1 - Duminy, T. A1 - Lima, P. A1 - Kamutzki, F. A1 - Gili, A. A1 - Zocca, Andrea A1 - Günster, Jens A1 - Gurlo, A. T1 - Clay in situ resource utilization with Mars global simulant slurries for additive manufacturing and traditional shaping of unfired green bodies N2 - The wet processing of regolith simulant for clay in situ resource utilization (ISRU) on Mars is presented. The two raw materials from the Mars global simulant family, one without clay (MGS-1) and one with clay - sodium montmorillonite smectite - (MGS-1C) were milled and mixed to produce a simulant with small particle size and reduced clay content (MGS-1C/8). All three simulants and the pure clay raw material were extensively characterized using XRF, synchrotron XRD, gas adsorption and gas pycnometry methods. In a straightforward processing approach, MGS-1C/8 was mixed with water and different dispersant approaches were investigated, all of which gave stable slurries. Particle size distribution, rheology, ion concentration, pH and electrical conductivity of these slurries were characterized. The slurry systems can easily be adapted to fit all typical ceramic shaping routes and here parts of varying complexity from slip casting, throwing on a potter's wheel and additive manufacturing, including material extrusion (robocasting) and binder jetting (powder bed 3D printing) were produced. The unique properties of the sodium montmorillonite clay, which is readily accessible in conjunction with magnesium sulfate on the Martian surface, acted as a natural nanosized binder and produced high strength green bodies (unfired ceramic body) with compressive strength from 3.3 to 7.5 MPa. The most elaborate additive manufacturing technique layerwise slurry deposition (LSD) produced water-resistant green bodies with a compressive strength of 30.8 ± 2.5 MPa by employing a polymeric binder, which is similar or higher than the strength of standard concrete. The unfired green bodies show sufficient strength to be used for remote Habitat building on Mars using additive manufacturing without humans being present. KW - Mars KW - Smectite KW - Clay ISRU KW - MGS-1 regolith simulant KW - 3D printing KW - Additive manufacturing PY - 2020 DO - https://doi.org/10.1016/j.actaastro.2020.04.064 VL - 174 SP - 241 EP - 253 PB - Elsevier Ltd. AN - OPUS4-50870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chinellato, Fabio A1 - Wilbig, Janka A1 - Al-Sabbagh, Dominik A1 - Colombo, P. A1 - Günster, Jens T1 - Gas flow assisted powder deposition for enhanced flowability of fine powders: 3D printing of alpha-tricalcium phosphate N2 - The possibility of creating patient-specific individual implants makes Additive Manufacturing technologies of special interest for the medical sector. For substitution of bone defects, powder based Additive Manufacturing by Binder Jetting is a suitable method to produce complex scaffold-like structures made of bioceramics with easily adapted geometries and controlled porosity. The process inherent residual porosity in the printed part, even though desired as it supports bone ingrowth, also leads to limited mechanical strength. Currently, bioceramic scaffolds made by Binder Jetting feature suitable biocompatible and biodegradable properties, while a sufficient mechanical stability is rather challenging. The purpose of this work is to apply the gas flow assisted powder deposition introduced in 2014 by Zocca et al., to the powder bed during printing of bioceramic tablets and scaffolds using α-TCP powder as feedstock. This enables exploiting the advantages of an increased powder bed density, thereby improving the mechanical properties of the printed parts. KW - Additive Manufacturing KW - Binder Jetting KW - Gas flow assisted powder deposition KW - Alpha-tricalcium phosphate KW - Scaffold PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510138 DO - https://doi.org/10.1016/j.oceram.2020.100003 SN - 2666-5395 VL - 1 SP - 100003 PB - Elsevier Ltd. AN - OPUS4-51013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maaß, Robert T1 - Temperature-dependent intermittent plasticity of Nb microcrystals N2 - Intermittent microplasticity via dislocation avalanches indicates scale-invariance, which is a paradigm shift away from traditional bulk deformation. Recently, we have developed an experimental method to trace the spatiotemporal dynamics of correlated dislocation activity (dislocation avalanches) in microcrystals (Phys. Rev. Mat. 2 (2018) 120601; Phys. Rev. Mat. 3 (2019) 080601). Here we exploit the temperature sensitive deformation of bcc metals. A marked change of the slip-size distribution is observed in the studied microcrystals, with increasingly small event-sizes dominating with decreasing temperature. This shows how a reduction in thermal energy increasingly suppresses the length-scale of dislocation avalanches, indicating how long-range correlations become gradually limited to the scale of the lattice. Our results further show that the stress-strain response is composed of strain-increments that are either thermally activated or essentially athermal. Temperature-dependent small-scale testing in combination with state-of-the-art discrete dislocation dynamics (DDD) simulations of Nb microcrystals are used to reveal these insights. T2 - MS&T20 Virtual CY - Online meeting DA - 02.11.2020 KW - Microcrystals PY - 2020 AN - OPUS4-60700 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maaß, Robert T1 - Tracing structural dynamics in metallic glasses during cryogenic cycling N2 - Highly unrelaxed structural states of metallic glasses have often advantageous mechanical properties. Since metallic glasses continuously relax with time (age) or inherently are well relaxed after processing, methods to uniformly rejuvenate the material are needed. One approach that has received attention is the so-called cryogenic-cycling method, during which a metallic glass is repeatedly immersed into liquid nitrogen. In some cases, cryogenic cycling is truly efficient in increasing the stored excess enthalpy of metallic glasses, but it does not seem to be universally applicable to all alloys and structural states. The origins for these differences remain unclear due to our limited understanding of the underlying structural evolution. In order to shed more light onto the fundamental structural processes of cryogenic cycling, we pursue in-situ x-ray photon correlation spectroscopy (XPCS) to trace the atomic-scale structural dynamics of a Zr-based metallic glass in two different structural states (ribbon and bulk metallic glass). This method allows calculating the relaxation times as a function of time throughout the thermal cycling. It is found that the investigated glasses exhibit heterogeneous structural dynamics at 300 K, which changes to monotonic aging at 78 K. Cryogenic cycling homogenizes the relaxation time distribution for both structural states. This effect is much more pronounced in the ribbon, which is the only structural state that rejuvenates upon cycling. We furthermore reveal how fast atomic-scale dynamics is correlated with long-time average structural relaxation times irrespective of the state, and that the ribbon exhibits unexpected additional fast atomic-scale relaxation in comparison to the plate material. Overall, a picture emerges that points towards heterogeneities in fictive temperature as a requirement for cryogenic energy storage. T2 - MRS Fall 2020 - Invited Talk CY - Boston, MA, USA DA - 27.11.2020 KW - Relaxation metallic glasses PY - 2020 AN - OPUS4-59542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Das, A. A1 - Dufresne, E.M. A1 - Maaß, Robert T1 - Structural dynamics and rejuvenation during cryogenic cycling in a Zr-based metallic glass N2 - Subjecting metallic glasses repeatedly to liquid nitrogen temperature has become a popular method to homogeneously rejuvenate the material. Here we reveal the atomic-scale structural dynamics using in- situ x-ray photon correlation spectroscopy (XPCS) during and after cryogenic cycling of a Zr-based metallic glass in two structural states (plate and ribbon). Heterogeneous structural dynamics is observed at 300 K that changes to monotonic aging at 78 K. It is found that cryogenic cycling homogenizes the relaxation time distribution. This effect is much more pronounced in the ribbon, which is the only structural state that rejuvenates upon cycling. We furthermore reveal how fast atomic-scale dynamics is correlated with longtime structural relaxation times irrespective of the structural state, and that the ribbon exhibits unexpected additional fast atomic-scale relaxation in comparison to the plate material. A structural picture emerges that points towards heterogeneities in the fictive temperature as a requirement for cryogenic energy storage. KW - Structural dynamics KW - Metallic glass KW - Relaxation KW - Rejuvenation KW - Cryogenic cycling PY - 2020 DO - https://doi.org/10.1016/j.actamat.2020.06.063 SN - 1359-6454 VL - 196 SP - 723 EP - 732 PB - Elsevier Ltd. AN - OPUS4-51311 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Honrao, S. J. A1 - Rizzardi, Q. A1 - Maaß, Robert A1 - Trinkle, D. R. A1 - Hennig, R. G. T1 - Split-vacancy defect complexes of oxygen in hcp and fcc cobalt N2 - One of the most ubiquitous and important defects in solids is oxygen. Knowledge about the solubility and diffusivity of oxygen in materials is crucial to understand a number of important technological processes, such as oxidation, corrosion, and heterogeneous catalysis. Density-functional theory calculations of the thermodynamics and kinetics of oxygen in cobalt show that oxygen diffusing into the two close-packed phases, namely α (hcp) and β (fcc), strongly interacts with vacancies.We observe the formation of oxygen split-vacancy centers (V-Oi-V) in both phases, and we show that this defect complex exhibits a similar migration energy barrier to the vacancy and oxygen interstitials. In contrast to the vacancy and oxygen interstitials, the oxygen split-vacancy centers exhibit an anisotropic strain field that couples to applied stress, making it possible to observe them through an internal friction experiment on quenched cobalt. KW - Split-vacancy defect complexes PY - 2020 DO - https://doi.org/10.1103/PhysRevMaterials.4.103608 VL - 4 IS - 10 SP - 103608-1 EP - 103608-9 PB - American Physical Society AN - OPUS4-51582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maaß, Robert T1 - Beyond Serrated Flow in Bulk Metallic Glasses: What Comes Next? N2 - This manuscript is based on an oral contribution to the TMS 2020 annual meeting and is dedicated to Prof. Peter Liaw, who for decades has shown great interest in serrated plastic flow. Here we will focus on the case of bulk metallic glasses, and begin with briefly summarizing some aspects of serrated and non-serrated inhomogeneous flow—a phenomenon that has perplexed materials scientists for decades. Four directions of research are identified that emerged out of the desire to fundamentally understand the intermittent inhomogeneous flow response. These research directions gear away from the phenomenological stress–strain behavior but put the underlying shear defect into focus. Unsolved problems and future research topics are discussed. KW - Non-serrated inhomogeneous flow PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513106 DO - https://doi.org/10.1007/s11661-020-05985-w SN - 1073-5623 SP - 1 EP - 11 PB - Springer Nature AN - OPUS4-51310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Gojani, Ardian A1 - Völker, Tobias A1 - Günther, Tobias A1 - Gornushkin, Igor B. A1 - Wilsch, Gerd A1 - Günster, Jens T1 - Investigation of grain sizes in cement-based materials and their influence on laser-induced plasmas by shadowgraphy and plasma imaging N2 - The effect of particle grain sizes in different cement-based mixtures on the laser-induced plasma evolution is studied using two experimental methods: (i) temporal and spatial evolution of the laser-induced shock wave is investigated using shadowgraphy and two-dimensional plasma imaging, and (ii) temporal and spatial distribution of elements in the plasma is investigated using two-dimensional spectral imaging. This study is motivated by the interest in applying laser-induced breakdown spectroscopy (LIBS) for chemical analysis of concrete, and subsequently obtain information related to damage assessment of structures like bridges and parking decks. The distribution of grain sizes is of major interest in civil engineering as for making concrete different aggregate grain sizes defined by a sieving curve (64mm to 0.125 mm) are needed. Aggregates up to a size of 180 μm can be excluded from the data set, therefore only the amount of small aggregates with a grain size below 180 μm must be considered with LIBS. All components of the concrete with a grain size smaller than 0.125mm are related to the flour grain content. Tested samples consisted of dry and hardened cement paste (water-cement ratio w/z=0.5), which served as a reference. Aggregate mixtures were made by adding flour grains (size 40 μm) and silica fume (size 0.1 μm) in different ratios to cement: 10%, 30%, 50% and 60%, all combined to the remaining percentage of dry or hydrated cement. The visualization results show that a dependance in the evolution of the plasma as a function of sample grain size can be detected only in the initial stages of the plasma formation, that is, at the initial 3 μs of the plasma life. Spectral information reveals the elemental distribution of the silicon and calcium in plasma, in both neutral and ionized form. Here also, a significant effect is observed in the first 1 μs of the plasma lifetime. KW - LIBS KW - Cement-based materials KW - Particle size KW - Shadowgraphy KW - Plasma imaging PY - 2020 DO - https://doi.org/10.1016/j.sab.2020.105772 VL - 165 SP - 105772 PB - Elsevier B.V. AN - OPUS4-50319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Campbell, C. G. A1 - Jordon Astorga, D. A1 - Dümichen, Erik A1 - Celina, M. T1 - Thermoset materials characterization by thermal desorption or pyrolysis based gas chromatography-mass spectrometry methods N2 - Thermoset materials characterization is often limited to solid state analytical techniques such as IR, NMR, DSC, TGA and mechanical testing. Alternatively, their off-gassing behavior can also be evaluated using GC based techniques such as TD-GC-MS, allowing this method to be applied to thermoset materials analyses such as identification, aging characterization, and formulation optimization. As an overview, common thermoset materials were evaluated by analyzing their gaseous degradation products via TGA-based pyrolysis and subsequent TD-GC-MS for the identification of representative volatile signatures. It is thereby possible to distinguish different classes of phenolic materials or cured epoxy resins, as well as their amine or anhydride curatives. Additionally, this method enabled quantification of a volatile fragment (bisphenol A, BPA) which is associated with oxidation of epoxy/amine thermoset materials. The amount of evolved BPA increased linearly with aging time and this trend exhibits linear Arrhenius behavior over the temperature range (80–125 °C) studied, in agreement with oxidation sensitivies based on oxygen consumption data. Further, TD-GC-MS was used to explore how off-gassing of residual anhydride curative from an epoxy/anhydride material depends on formulation stoichiometry. Even in formulations that theoretically contained enough epoxy to consume all anhydride (1:1 stoichiometry), an imperfect final cure state resulted in residual anhydride which could evolve from the material. For such materials, a slightly epoxy-rich formulation is required to ensure that the material contains no residual unreacted anhydride. Analysis of volatiles generated by thermal exposure is an attractive characterization approach enabling compositional analysis as well as complementary diagnostics for materials degradation. KW - Polymer analysis/characterization KW - Thermal desorption mass spectrometry KW - Thermoset composition KW - Volatiles from thermosets KW - Degradation signatures PY - 2020 DO - https://doi.org/10.1016/j.polymdegradstab.2019.109032 VL - 174 SP - 109032 PB - Elsevier Ltd. AN - OPUS4-50435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sänger, Johanna Christiane A1 - Pauw, Brian Richard A1 - Sturm, Heinz A1 - Günster, Jens T1 - First time additively manufactured advanced ceramics by using two-photon polymerization for powder processing N2 - Methods and materials are presented here, which enable the manufacturing of fine structures using a 3D-printing method known as two-photon polymerization (2PP). As traditional photolithography methods for structuring ceramic slurries do not function with 2PP, due to light scattering on ceramic particles, a novel water-based photoresist with high ceramic loading of extremely well dispersed ceramic nano particles was developed. This photoresist is basically a ceramic slurry containing a photocurable agent and a photoinitiator to be crosslinkable with the 780 nm wavelength femtosecond laser light source of the 2PP machine. It is demonstrated that it is possible to gain a highly transparent and low viscous slurry suitable for 2PP processing. This work shows the development of the slurry, first printing results and the post-printing processes required to form three dimensional ceramic microstructures consisting of alumina toughened zirconia (ATZ). KW - 3D-printing KW - Two-photon polymerization KW - 2PP KW - Ceramic nano particles KW - Slurry KW - Alumina toughened zirconia KW - ATZ KW - Additive manufacturing KW - SchwarzP cells KW - Nano-ceramic-additive-manufacturing photoresin KW - NanoCAM PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517441 DO - https://doi.org/10.1016/j.oceram.2020.100040 VL - 4 SP - 100040 PB - Elsevier Ltd. AN - OPUS4-51744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Fateri, M. A1 - Al-Sabbagh, Dominik A1 - Günster, Jens T1 - Investigation of the sintering and melting of JSC-2A lunar regolith simulant N2 - Future lunar exploration can benefit greatly from In-Situ Resource Utilization. Accordingly, the in-Situ Resource Utilization approach highlights the need for detailed analysis of lunar regolith. In this study, JSC-2A Simulant was studied regarding its sintering and melting behaviour using Differential Thermal Analysis under ambient and inert conditions. The minerals at the crystalline peaks were determined using X-Ray Diffraction analysis. Moreover, melting droplet shape and wetting behaviour of pressed regolith samples of different particle size distributions were studied by Hot Stage Microscopy technique. Hot Stage Microscopy experiments were performed at different heating rates under ambient conditions. Bloating effects within the solidified samples were then qualitatively examined by X-ray tomography. Lastly, the optimization of processing strategies for the Additive Manufacturing of lunar regolith is discussed. KW - Lunar regolith KW - Sintering KW - Melting KW - Hot stage microscopy PY - 2020 DO - https://doi.org/10.1016/j.ceramint.2020.02.212 VL - 46 IS - 9 SP - 14097 EP - 14104 PB - Elsevier Ltd. AN - OPUS4-50869 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph T1 - Corrosive CO2-stream components, challenging for materials to be used in CC(U)S applications N2 - This contribution provides current findings regarding materials susceptibility for CCUS applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2 stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide the following recommendations for certain parts. Commercially available carbon steels are suitable for compression and pipelines as long as moisture content and impurities are limited (water 50 to 100 ppmv, SO2 and NO2 ca. 100 ppmv). Corrosion rates increase with increasing water content (0.2 – 20 mm/a). Condensation of acids and therefore droplet formation is always possible, even at low water contents. A low SO2 content within the CO2-stream might be more important than a low water content. Cr13-steels showed a general susceptibility to shallow pitting and pitting. So, they seem to be not suitable for CCUS applications. Low alloyed steels showed better corrosion behavior (predictable uniform corrosion). For direct contact with saline aquifer fluids only high alloyed steels shall be used. T2 - WCO Webinar on the occasion of Corrosion Awareness Day - Corrosion and Low-Carbon Energies CY - Frankfurt, Germany DA - 24.04.2020 KW - CO2-corrosion KW - CCUS KW - Pipeline KW - Carbon Capture PY - 2020 AN - OPUS4-50699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa T1 - CO2-stream impurities and their effects on corrosion susceptibility of materials to be used in CCUS systems N2 - Carbon Capture Utilization and Storage (CCUS) is a promising technology to reach the target for reduction of CO2 emissions. Crucial points for a sustainable and future-proof CCUS system are reliability and cost efficiency of the whole process chain, including separation of CO2 from the source, compression of CO2, its subsequent transportation to the injection site and injection into geological formations, e.g. aquifers. Recent studies have shown that even at a very low concentration of impurities, condensation of sulfuric and nitric acids in dense phase CO2 are possible and observable. Thus, impact of impure CO2 stream toward corrosion susceptibility of materials to be used in CCUS system need to be considered. In this talk, basing on results achieved from two German long-term projects (COORAL and CLUSTER), the dominating impurities of the CO2 stream and corrosion mechanisms are addressed. Investigations cover the whole CCUS process chain and provide a material recommendation for certain parts. T2 - Corrosion in Low-Carbon Energies - IFPEN-Lyon CY - Online meeting DA - 03.11.2020 KW - Corrosion KW - CCUS KW - Carbon dioxide PY - 2020 AN - OPUS4-51509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abram, Sarah-Luise T1 - Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements N2 - In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles. The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum. 1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties. 2. Iron oxide nanoparticles are under development as new candidate reference material at BAM. 3. Narrow particle size distribution confirmed by light scattering and electron microscopy. T2 - Nanosafety 2020 CY - Online meeting DA - 05.10.2020 KW - Iron oxide nanoparticles KW - Reference material KW - Particle size KW - Electron microscopy KW - Nanoplattform PY - 2020 AN - OPUS4-52774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Lei A1 - Hoyt, J. J. T1 - Layering misalignment and negative temperature dependence of interfacial free energy of B2-liquid interfaces in a glass forming system N2 - From molecular dynamics simulations and the capillary fluctuation method, the solid-liquid interfacial free energy has been computed for the B2-liquid interface in the Cu-Zr system. Consistent with previous results for the FCC-liquid interface in Cu-Zr and Al-Sm but atypical of most alloys, was found to increase as the temperature is lowered. In addition, the temperature dependence was obtained for model Lennard-Jones B2-liquid alloys. In all cases the unusual temperature dependence of is correlated with an atomic structure of the interfacial region characterized by a misalignment of the number density peaks between solvents and solutes. In cases where the number density peaks are aligned, the typical temperature dependence is observed. The results are discussed in terms of the Gibbs theory of the thermodynamics of interfaces. It is proposed that the unique interfacial structure and the atypical temperature dependence of are hallmarks of an easy glass forming alloy. KW - Atomistic simulations KW - Interfacial free energy KW - Layering misalignment KW - Glass forming PY - 2021 DO - https://doi.org/10.1016/j.actamat.2021.117259 SN - 1359-6454 VL - 219 SP - 117259 PB - Elsevier Ltd. AN - OPUS4-53650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - 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 - Gebhardt, M. A1 - Malolakis, I. A1 - Kalinka, Gerhard A1 - Deubener, J. A1 - Chakraborty, S. A1 - Meiners, D. T1 - Re-use potential of carbon fibre fabric recovered from infusible thermoplastic CFRPs in 2nd generation thermosetting-matrix composites N2 - The research presented here attempts to assess the potential for re-using carbon fibre (CF) fabrics recovered from recycling infusible acrylic thermoplastic carbon fibre reinforced polymer composites (CFRPs) in a universal manner, i.e. by combining with a wide variety of matrices to manufacture 2nd generation composite laminates by resin infusion. The 2nd generation composites have been compared in terms of bulk and interfacial properties against counteparts processed with virgin carbon fibre fabric infused with the same matrices. Generally, an increase in damping (tanδ) was observed in all 2nd generation composites, which can be attributed to a residual thin thermoplastic layer present on the recovered fibres. The interfacial adhesion of the 2nd generation Composites was investigated by shear tests and scanning electron micsoscopy, and also appears to be less influenced by the type of matrix. KW - Composite recycling KW - Thermoplastic matrix KW - Thermosetting resin KW - Fibre/matrix bonding PY - 2021 DO - https://doi.org/10.1016/j.coco.2021.100974 VL - 28 SP - 100974 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-53639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kalinka, Gerhard T1 - Optische Beobachtungen der Faser-Matrix-Trennung im Pull-out-Versuch N2 - Der Vortrag behandelt Rissentstehung und Ausbreitung an Faser-Matrix-Interfaces, untersucht mit dem optischen Mikroskop. T2 - Composites United, CU-Arbeitsgruppe/n Faser-Matrix-Haftung & Matrices CY - Online meeting DA - 02.12.2021 KW - Faser KW - Matrix KW - Pull-out KW - Interface PY - 2021 AN - OPUS4-53968 LA - deu 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 - JOUR A1 - Agea, Boris A1 - Walzel, S. T1 - 3D Druck unterstütz die Dekarbonisierung N2 - Suspensionsbasiertes Binder Jetting reduziert die Brennzeiten von technischer Keramik im Vergleich zu anderen 3d-druckverfahren signifikant. dabei wird nicht nur Energie beim Betrieb der Brennöfen gespart, sondern auch die Emission von Kohlendioxid beim Brennvorgang selbst gesenkt. KW - Schlickerdeposition PY - 2021 VL - 6 SP - 26 EP - 28 PB - Keramische Zeitschrift AN - OPUS4-53812 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 - CONF A1 - Ghafafian, Carineh T1 - The effect of fiber orientation mismatch on scarf joint damage mechanisms under fatigue load N2 - Wind turbine rotor blades commonly fail before their projected 20-year lifespan largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production. A potential repair alternative to restoring the mechanical properties of such lightweight fiber reinforced polymer (FRP) structures is to locally patch these areas with scarf joints. This type of repair allows for a smoother load distribution across the joint, and is favored especially on structures where minor aerodynamic contour changes are key. The effects of such repairs on the structural integrity, however, is still largely unknown. Building upon an understanding of the static load failure mechanism of GFRP scarf joints, presented at the ICCS23 Joint Event in 2020, the influence of the fiber orientation mismatch between parent and repair materials of 1:50 scarf joints on the failure mechanism of monolithic glass FRP specimens under cyclic fatigue load were examined in this study. Specimens with various layups were produced with the vacuum-assisted resin infusion (VARI) process using biaxial E-glass non-crimp fabric (NCF). The patch layers were then joined directly to the parent structure with the VARI using biaxial E-glass NCF with half the areal weight of the parent side to allow for better drapability. This mimics the soft-to-hard patch style utilized in wind turbine blade shell field repairs. The specimens were tested under uniaxial fatigue load, during which they were periodically monitored for damage onset. A comparison of the +45/-45° and 0/90° layups allowed for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. In addition to the tensile strength and stiffness property recovery assessment, a grayscale analysis using in-situ camera images determined the damage state leading to failure in each region across the scarf joint, which varied in the parent material versus scarf joint region, providing insight to the critical regions in this composite structure under cyclic loading. T2 - ICCS24 - 24th International Conference on Composite Structures CY - Online meeting DA - 14.06.2021 KW - Glass fiber reinforced polymers KW - Scarf repairs KW - Damage mechanisms PY - 2021 AN - OPUS4-52817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Entwicklung thermoelektrischer Multilayergeneratoren auf der Basis von Calciumcobaltit N2 - Thermoelectric generators can be used as energy harvesters for sensor applications. Multilayer thermoelectric generators (ML-TEGs) are a promising alternative to conventional π-type generators due to their high filling factor, high capability of automated production and the texturing potential during the production process. Calcium cobaltite is a promising thermoelectric oxide (p-type) with highly anisotropic properties. The following study shows the development of a textured unileg ML-TEG using ceramic multilayer technology. Tape-casting and pressure assisted sintering are applied to fabricate textured calcium cobaltite. Compared to conventional sintering, pressure assisted sintering increases the strength by the factor 10. Thermoelectric properties can be tuned either towards maximum power factor or towards maximum figure of merit depending on the pressure level. As electrical insulation material, a screen-printable glass-ceramic with high resistivity and adapted coefficient of thermal expansion is developed. From various commercial pastes a metallization with low contact resistance is chosen. The unileg ML-TEG is co-fired in one single step. The demonstrators reach 80% of the simulated output power and the power output is highly reproducible between the different demonstrators (99%). These results provide the first proof-of-concept for fabricating co-fired multilayer generators based on textured calcium cobaltite with high power factor, high density, and high strength. N2 - Thermoelektrische Generatoren können zum „Energy harvesting“ für den autarken Betrieb von bspw. Sensoren eingesetzt werden. Eine interessante Alternative zu den herkömmlichen π-Typ Generatoren sind auf Grund der höheren Leistungsdichte und der guten Automatisierbarkeit thermoelektrische Multilayergeneratoren. Calciumcobaltit ist ein vielsprechendes oxidisches Thermoelektrika (p-Typ) mit stark anisotropen Eigenschaften. Die hier vorgestellte Studie zeigt die Entwicklung von texturierten Unileg-Multilayer-Generatoren mittels keramischer Multilayertechnologie. Calciumcobaltit wird durch Foliengießen und druckunterstützte Sinterung texturiert. Im Vergleich zur konventionellen Sinterung verbessert sich die Festigkeit um den Faktor 10. Die thermoelektrischen Eigenschaften können je nach verwendetem Druckniveau hinsichtlich maximalem Power Factor oder hinsichtlich maximalem Gütefaktor optimiert werden. Ein Glaskeramikkomposit wird als Isolationsmaterial mit hohem Volumenwiderstand und angepasstem Wärmeausdehnungskoeffizienten entwickelt. Der Unileg-Multilayer-Generator wird in einem Schritt co-gesintert. Die hergestellten Demonstratoren erreichen 80% der simulierten Output-Leistung. Diese Ergebnisse stellen den ersten Machbarkeitsnachweis für die Herstellung von co-gesinterten Multilayer-Generatoren aus texturiertem Calciumcobaltit mit hohem Power Factor und hoher Festigkeit dar. T2 - Seminar des Lehrstuhls für Funktionsmaterialien, Universität Bayreuth CY - Online meeting DA - 18.06.2021 KW - Thermoelektrischer Generator KW - Multilayertechnik KW - Energy harvesting PY - 2021 AN - OPUS4-52834 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Plichta, T. A1 - Sirjovona, V. A1 - Zvonek, M. A1 - Kalinka, Gerhard A1 - Cech, V. T1 - The Adhesion of Plasma Nanocoatings Controls the Shear Properties of GF/Polyester Composite N2 - High-performance fibre-reinforced polymer composites are important construction materials based not only on the specific properties of the reinforcing fibres and the flexible polymer Matrix but also on the compatible properties of the composite interphase. First, oxygen-free (a-CSi:H) and oxygen-binding (a-CSiO:H) plasma nanocoatings of different mechanical and tribological properties were deposited on planar silicon dioxide substrates that closely mimic E-glass. The nanoscratch test was used to characterize the nanocoating adhesion expressed in terms of critical normal load and work of adhesion. Next, the same nanocoatings were deposited on E-glass fibres, which were used as reinforcements in the polyester composite to affect its interphase properties. The shear properties of the polymer composite were characterized by macro- and micromechanical tests, namely a short beam shear test to determine the short-beam strength and a single fibre push-out test to determine the interfacial shear strength. The results of the polymer composites showed a strong correlation between the short-beam strength and the interfacial shear strength, proving that both tests are sensitive to changes in fibre-matrix adhesion due to different surface modifications of glass fibres (GF). Finally, a strong correlation between the shear properties of the GF/polyester composite and the adhesion of the plasma nanocoating expressed through the work of adhesion was demonstrated. Thus, increasing the work of adhesion of plasma nanocoatings from 0.8 to 1.5 mJ·m−2 increased the short-beam strength from 23.1 to 45.2 MPa. The results confirmed that the work of adhesion is a more suitable parameter in characterising the level of nanocoating adhesion in comparison with the critical normal load. KW - Mechanical properties KW - Plasma nanocoatings KW - Glass fibre KW - Polymer composite KW - Short-beam strength KW - Interfacial shear strength KW - Work of adhesion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521844 DO - https://doi.org/10.3390/polym13040593 VL - 13 IS - 4 SP - 593 PB - MDPI CY - Basel,Schweiz AN - OPUS4-52184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rabe, Torsten A1 - Eichler, J. A1 - Picht, G. A1 - Rossner, W. A1 - Stelter, M. A1 - Voigt, I. T1 - Digitalisierung der keramischen Fertigung - Herausforderungen und Chancen N2 - Dieses Strategiepapier zielt darauf ab, Akteuren und Entscheidungsträgern den Status der Digitalisierung in der keramischen Fertigung, erfolgreiche Best-Practice-Beispiele aber auch die Herausforderungen nahezubringen, die es nun anzugehen gilt. Es ist die Vision, die Keramikfertigung durchgehend zu digitalisieren und alle Schritte des Produktkreislaufs lückenlos über die gesamte Wertschöpfungs- und Nutzungskette zu vernetzen: also eine Keramikindustrie 4.0 zu etablieren. Das Strategiepapier erfasst zunächst die Spezifität der keramischen Fertigung und nimmt eine Analyse des gegenwärtigen Standes der Digitalisierung in der keramischen Industrie vor, auch anhand einiger ausgewählter Beispiele aus der industriellen Praxis. Auf Basis der wesentlichen Bausteine für eine Fertigungsdigitalisierung werden schließlich die Chancen für Keramikproduzenten sowie der erforderliche Forschungs- und Entwicklungsbedarf aufgezeigt. KW - Datenmanagement KW - Digitalisierung KW - Fertigungsprozess KW - Keramik KW - Sensorik PY - 2021 SP - 1 EP - 39 PB - Deutsche Gesellschaft für Materialkunde (DGM) und Deutsche Keramische Gesellschaft (DKG) CY - Köln ET - 1000 AN - OPUS4-52708 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Rychlowski, L. A1 - Cios, G. A1 - Winkelmann, A. T1 - Crystallographic analysis of the lattice metric (CALM) from single electron backscatter diffraction or transmission Kikuchi diffraction patterns N2 - A new software is presented for the determination of crystal lattice parameters from the positions and widths of Kikuchi bands in a diffraction pattern. Starting with a single wide-angle Kikuchi pattern of arbitrary resolution and unknown phase, the traces of all visibly diffracting lattice planes are manually derived from four initial Kikuchi band traces via an intuitive graphical user interface. A single Kikuchi bandwidth is then used as reference to scale all reciprocal lattice point distances. Kikuchi band detection, via a filtered Funk transformation, and simultaneous display of the band intensity profile helps users to select band positions and widths. Bandwidths are calculated using the first derivative of the band profiles as excess-deficiency effects have minimal influence. From the reciprocal lattice, the metrics of possible Bravais lattice types are derived for all crystal systems. The measured lattice parameters achieve a precision of <1%, even for good quality Kikuchi diffraction patterns of 400 x 300 pixels. This band-edge detection approach has been validated on several hundred experimental diffraction patterns from phases of different symmetries and random orientations. It produces a systematic lattice parameter offset of up to ±4%, which appears to scale with the mean atomic number or the backscatter coefficient. KW - Electron backscatter diffraction KW - Kikuchi patterns KW - Lattice parameters KW - Radon transform PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527076 DO - https://doi.org/10.1107/S1600576721004210 SN - 1600-5767 VL - 54 IS - Pt 3 SP - 1012 EP - 1022 AN - OPUS4-52707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraus, David A1 - Trappe, Volker T1 - Transverse damage in glass fiber reinforced polymer under thermo-mechanical loading N2 - In this study, the thermomechanical damage behavior of a glass fiber reinforced polymer material is investigated. The coefficients of thermal expansion of the composite as well as the matrix are measured in a wide temperature range. Quasi-static experiments with neat resin, unidirectional and multidirectional laminates are performed as well as fatigue experiments in a temperature range from 213 K to 343 K. This study focusses on the matrix damage due to fiber-parallel loading. A correlation between matrix effort, the dilatational strain energy of the matrix and the damage state of the specimen is demonstrated. It is shown that a fatigue life assessment can be performed with the aid of a temperature-independent master fatigue curve. KW - Composite KW - Glass fiber reinforced polymer KW - Thermo-mechanics KW - Fatigue KW - Damage KW - Temperature PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527462 DO - https://doi.org/10.1016/j.jcomc.2021.100147 SN - 2666-6820 VL - 5 SP - 100147 PB - Elsevier B.V. AN - OPUS4-52746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghafafian, Carineh T1 - Restoring lightweight strength - Effect of localized repairs on the mechanical properties of composites sandwich structures N2 - As a type of high-performance composite material, glass-fiber reinforced plastics (GFRP) are favored for the construction of wind turbine rotor blades due to their high specific strength and stiffness properties (Grasse et al, 2010). During the blade manufacturing process, however, imperfections are often introduced, then further propagated due to harsh environmental conditions and a variety of loads (Caminero et al, 2013; Trappe et al, 2018). This leads to failure significantly before their designed lifespan. Since replacement of entire blades can be a costly potential outcome, localized repairs of the damaged region to restore structural integrity and thus lengthen its lifespan can executed in the field by technicians accessing the blades directly by suspended roping. These methods involve replacing the lost load path with a new material that is joined to the parent structure. In recent years, considerable studies have been conducted to investigate the influence of different repair parameters on the stress distribution, ultimate strength, impact behavior, and residual stresses of bonded repaired structures [Caminero et al, 2013; Trappe et al, 2018; Shufeng et al, 2014; Harman and Rider, 2011; Ahn and Springer, 2000; Lekou and Vionis, 2002). However, there currently do not exist any standardized repair procedures for wind turbine rotor blades. Namely, there is a lack of understanding about the effects of the layup of various repair methods, especially on the damage mechanism and fatigue life of the shells of rotor blades (Caminero et al, 2013; Trappe et al, 2018). This work therefore aims to begin to enrich this knowledge gap by testing the influence of different variables among repair patches on the mechanical properties of sandwich composite structures. Manufactured with the vacuum-assisted resin infusion (VARI) process, the test specimens are produced as a GFRP structure to represent the outer shell portion of a wind turbine blade, then repaired with a scarf joint. Scarf repairs are favored as the most efficient of the common structural joints, as the removal of the damaged area with angled walls leads to a nearly uniform shear stress distribution along the bond surface and no eccentricity in the load distribution (Caminero et al, 2013; Lekou and Vionis, 2002; Siener, 1992). The performance of specific layup methods of repair patches, namely a large-to-small versus small-to-large scheme of repair layers, is studied with static and load-controlled fatigue testing, then compared to pristine test specimens as well as to each other in terms of mechanical property restoration. The transition layer between repair and parent material is especially of interest in the performance of the structure. Damage onset, crack development and eventual failure are monitored in-situ with non-destructive testing methods, including thermography with an infrared camera system and a 3D deformation analysis system, to develop a more robust understanding of the effects of these repair concept variables on wind turbine blade shell structures. T2 - Wind Energy Science Conference CY - Online Meeting DA - 25.05.2021 KW - Glass fiber reinforced polymers KW - Wind turbine blade shell structures KW - Scarf joint repair PY - 2021 AN - OPUS4-52687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Höhne, Patrick T1 - Limits of computer tomography aided characterization of different types of porous ceramic materials N2 - Ceramics with open porosity are attractive materials in many fields of applications covering medicine, catalysis, and filtration. Manifold technologies to produce porous ceramics are available, e.g. foaming and replica processes, resulting in various microstructures. Development and manufacturing of new materials is accelerating, while crucial characterization is becoming increasingly difficult and conventional measurements lack the desired speed. Computed tomography (CT) offers the possibility to three-dimensionally characterize entire samples with minimal sample preparation, while its main advantage is that it is non-destructive. Still, the assessment of quantitative results from CT measurements is not trivial. The poster presents CT characterizations of newly developed as well as commercially available openly porous ceramic samples. Properties such as porosity, permeability or pore characteristics were measured conventionally and compared to results calculated from CT-measurements using the commercial software VG StudioMax. The determined differences between measured and calculated values are presented and application areas as well as limits of the CT characterization are evaluated. T2 - Jahrestagung der Deutschen keramischen Gesellschaft 2021 CY - Online Meeting DA - 19.04.2021 KW - Ceramic KW - Porosity PY - 2021 AN - OPUS4-52724 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 - Schilling, Markus T1 - Tensile Test: From Standard to PMD Application Ontology N2 - Data analysis methods play an important role in both the experimental and simulation-based digital description of materials but have so far been poorly structured. The platform Material Digital (PMD) should contribute to a standardized description of data processing methods in materials research. The goal is the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications. Therefore, application ontologies are created to explicitly describe processes and test methods. In this presentation, the first efforts in creating a tensile test application ontology in accordance with the ISO standard 6892-1:2019-11 are shown. Especially, the path of ontology development to be pursued based on standards was focused. T2 - Onboarding Workshop der Plattform Material Digital (PMD) CY - Online meeting DA - 13.04.2021 KW - Ontology KW - Platform MaterialDigital KW - PMD KW - Tensile Test KW - Normung KW - Standardization PY - 2021 AN - OPUS4-52425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stargardt, Patrick T1 - Modeling of the cooling behavior of thermoelectric multilayers N2 - Multilayered designs are an attractive approach towards cost-effective manufacturing of thermoelectric generators. Therefore, efforts are being made to co-fire two promising thermoelectric oxides, namely calcium cobaltite and calcium manganate. In this study, ceramic tapes, multilayer technology, and pressure-assisted sintering (PAS) were used. A major challenge for the PAS of low-sintered calcium manganate was cracking during cooling. A relationship between the properties of the release tape used during PAS and the cracking behavior was experimentally observed. To understand the origin of failure, reaction layers in the multilayer were analyzed and thermal stresses during cooling were estimated by finite element (FE) simulations. Thermal expansion, elastic properties, and biaxial strength of the thermoelectric oxides and selected reaction layers were determined on separately prepared bulk samples. The analysis showed that the reaction layers were not the cause for cracking of calcium manganate. Using the FE model, thermal stresses in different manganate multilayer designs with varying properties of the release tape were studied. The FEM study indicated, and a validation experiment proved that the thickness of the release tape has the main effect on thermal stresses during cooling in separately sintered calcium manganate. T2 - Keramik 2021 / Ceramics 2021 CY - Online Meeting DA - 19.04.2021 KW - Fem KW - Thermoelectric KW - Pressure assisted sintering PY - 2021 AN - OPUS4-52489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Charmi, Amir T1 - Mechanical anisotropy of LPBF 316L: a modeling approach N2 - The underlying cause of mechanical anisotropy in additively manufactured (AM) parts is not yet fully understood and has been attributed to several different factors like microstructural defects, residual stresses, melt pool boundaries, crystallographic and morphological textures. To better understand the main contributing factor to the mechanical anisotropy of AM stainless steel 316L, bulk specimens were fabricated via laser powder bed fusion (LPBF). Tensile specimens were machined from these AM bulk materials for three different inclinations relative to the build plate. Dynamic Young's modulus measurements and tensile tests were used to determine the mechanical anisotropy. Some tensile specimens were also subjected to residual stress measurement via neutron diffraction, porosity determination with X-ray micro-computed tomography, and texture analysis with electron backscatter diffraction (EBSD). A crystal plasticity model was used to analyze the elastic anisotropy and the anisotropic yield behavior of the AM specimens, and it was able to capture and predict the experimental behavior accurately. Overall, it was shown that the mechanical anisotropy of the tested specimens was mainly influenced by the crystallographic texture. T2 - 2. Online-Workshop "In-situ Monitoring and Microstructure Development in Additive Manufactured Alloys " CY - Online meeting DA - 20.04.2021 KW - Anisotropy KW - Crystal plasticity KW - Additive manufacturing PY - 2021 AN - OPUS4-52603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Portella, Pedro Dolabella A1 - Krebber, Katerina T1 - Fiber Optic Sensors for SHM - From Laboratory to Industrial N2 - The paper highlights the research activities in Germany and Europe in the development of distributed fiber optic sensor for structural health monitoring (SHM) like the monitoring of geotechnical and civil infrastructures and presents selected results achieved within these projects. T2 - Conaendi & IEV 2021 CY - Online meeting DA - 09.03.2021 KW - Fiber KW - Optic KW - SHM PY - 2021 AN - OPUS4-52254 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 - CHAP A1 - Stephan-Scherb, Christiane ED - Schorr, S. ED - Weidenthaler, C. T1 - Crystallographic challenges in corrosion research N2 - High-temperature corrosion is a widespread problem in various industries. As soon as a hot and reactive gas (CO2, O2, H2O, SO2, NOx, etc.) is in contact with a solid, physico-chemical processes at the surface and interfaces lead to material degradation. The processes are dynamic and controlled by thermodynamic and kinetic boundary conditions. Whether a reaction product is protective or not depends on various factors, such as chemical composition of the solid and the reactive media, surface treatment as well as diffusion and transport paths of cations and anions. Resulting chemical and structural inhomogeneities with the corrosion layers are characterized by off stoichiometry within cationic and anionic sub lattices. The competitive processes can be studied by various techniques of applied crystallography. This chapter gives an overview on the challenges of chemical-structural Analysis of reaction products by crystallographic methods such as X-ray diffraction and X-ray near-edge structure spectroscopy and scanning electron microscopy electron backscatter diffraction (SEM-EBSD) for corrosion science. KW - High-temperature corrosion KW - Oxidation KW - Diffraction KW - Spectroscopy KW - Oxides PY - 2021 DO - https://doi.org/10.1515/9783110674910-009 SP - 291 PB - De Gruyter ET - 1 AN - OPUS4-52903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Thermo-mechanical fatigue of glass fiber reinforced polymer N2 - Glass fiber reinforced polymer (GFRP) materials in practical applications have to endure cyclic mechanical loading in a wide temperature range (e.g. aircraft applications, automotive, wind turbine blades). In this study the static strength and fatigue behavior of GFRP was investigated in a temperature range from 213 K to 343 K. Therefor the coefficients of thermal expansion of the composite as well as the matrix are measured in this temperature interval. The inverse laminate theory was extended and used to calculate the inter fiber-failure effort for a virtual UD-layer according to the layer wise strength approach. The experimentally determined results are compared with the micro-mechanical model according to Krimmer, which has been enhanced to include the effect of temperature and fiber-perpendicular failure modes. A correlation between matrix effort, the dilatational strain energy of the matrix and the damage state of the specimen is demonstrated. It is shown that a fatigue life assessment can be performed with the aid of a temperature-independent master fatigue curve, as it was similar done for the fatigue behavior of CFRP and GFRP to very high load cycles at room temperature. T2 - ICFC8 - The 8th International Conference on the Fatigue of Composites CY - Online meeting DA - 23.06.2021 KW - Glass fibre reinforced plastics KW - Fatigue KW - Thermo-mechanical-loading PY - 2021 AN - OPUS4-52910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agea Blanco, Boris A1 - Walzel, S. A1 - Chi, J. A1 - Lüchtenborg, J. T1 - Making Binder Jetting Really Work for Technical Ceramics - Additive Manufacturing of Technical Ceramics N2 - As an alternative shaping method to the traditionally used processes, additive manufacturing (AM) can produce economical ceramic components in small lot sizes and/or with complex geometries. Powder-based additive manufacturing processes like binder jetting are popular in the field of metal AM. One reason is the increased productivity compared to other AM technologies. For ceramic materials, powder-based AM technologies result in porous ceramic parts, provided they are not infiltrated. CerAMing GmbH unites the advantages of powder-based processes with the production of dense ceramic by means of the Layerwise Slurry Deposition. By using a suspension, a high packing density of the powder bed is achieved which leads to high green body densities. Due to this advantage the approach overcomes the problems of other powder-based AM technologies. Furthermore, a very economical debinding time allows the production of parts with high wall thicknesses. KW - Additive Manufacturing KW - Binder Jetting KW - Layerwise Slurry Deposition KW - Lithography-based technologies KW - Technical Ceramics PY - 2021 SP - 49 EP - 52 PB - Göller Verlag CY - Baden-Baden AN - OPUS4-52948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus T1 - Tensile Test Ontology used in Platform Material Digital (PMD) N2 - Data analysis methods play an important role in both the experimental and simulation-based digital description of materials but have so far been poorly structured. The platform Material Digital (PMD) is supposed to contribute to a standardized description of data processing methods in materials research. The goal is the quality assurance of the processes and the output data, the acquisition and definition of their accuracy as well as the interoperability between applications. Therefore, application ontologies are created to explicitly describe processes and test methods. In this presentation, the first efforts within the joint project PMD in creating a tensile test application ontology in accordance with the ISO standard 6892-1:2019-11 are shown. Especially, the path of ontology development to be pursued based on standards was focused. Furthermore, the presentation includes a live demonstration of queries possibly performed to query data that was uploaded in the PMD triple store. T2 - Online Workshop: An introduction to the semantic web and ontologies CY - Online meeting DA - 23.04.2021 KW - Ontology KW - Tensile Test KW - Platform Material Digital KW - PMD KW - Knowledge Graphs KW - Semantic Web PY - 2021 AN - OPUS4-52949 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 - CONF A1 - Blaeß, Carsten T1 - Viskose Rissschließung in Gläsern und Glasmatrixkompositen N2 - Um die Langzeitbeständigkeit von Hochtemperatur-Festoxidbrennstoffzellen (SOFC) sicherzustellen, ist das grundlegende Verständnis der viskosen Schließung oder Heilung von Rissen, als Folge wechselnder thermischer oder mechanischer Belastung, in Gläsern und teilkristallinen Materialien ein entscheidender Faktor. In Glas ist die Rissheilung hauptsächlich durch viskoses Fließen bestimmt. In teilkristallinen Schmelzen bewirkt der kristalline Volumenanteil die Erhöhung der effektiven Viskosität. Um die Auswirkungen des kristallinen Volumenanteils auf die Rissheilung zu ergründen, wurden Glasmatrixkomposite mit variierten inerten kristallinen Fülleranteilen, die während der Wärme-behandlung konstant blieben, hergestellt. Verwendet wurde ein kristallisationsträges Natrium-Calcium-Silicatglas und ZrO2 als inerter Füller. Komplexe, reproduzierbare Rissstrukturen wurden durch Vickers-Eindrücke erzeugt und die viskose Rissschließung während isothermer Wärmebehandlungs-schritte mittels Laser-Scanning-Mikroskopie verfolgt. Die Untersuchungen zeigen, dass, verglichen zum füllerfreien Glas, der kristalline Phasenanteil die effektive Viskosität erhöht und dadurch großräumiges Fließen verlangsamt. Dies verzögert das Aufweiten der Risse. Dieser Effekt erschwert die Rissverkürzung und führt oftmals zu großen gerundeten Kavitäten und dadurch zu einer verzögerten Rissschließung. Wird dieses Aufweiten verringert, ist zunächst ein lokales viskoses Fließen der Restglasphase weiterhin gegeben, sodass sich die Risse sogar schneller schließen. Für kristalline Anteile > 27 Vol% bildet sich dann ein stabiles Perkolationsgerüst aus, das die weitere Rissschließung auch lokal unterbindet. Nur innerhalb größerer glasiger Bereiche ist hierbei noch eine Rissschließung zu beobachten. Ein Optimum der Risslängenverkürzung konnte bei 17 Vol% beobachtet werden. T2 - 94. Glastechnische Tagung CY - Online meeting DA - 10.05.2021 KW - Glas KW - Hochtemperaturbrennstoffzelle KW - Glasmatrixkomposit KW - Rissheilung PY - 2021 AN - OPUS4-54245 LA - deu 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 - 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 - Stephan-Scherb, Christiane T1 - Novel insights into high temperature corrosion phenomena by advanced X-ray methods N2 - A variety of materials of technological interest change their properties through contact with reactive media. Solid-gas reactions lead to a variety of reaction products on the surfaces and internal interfaces. The observation of nucleation and growth processes in the environment where they occur (in situ) from a chemical-structural perspective is especially challenging for aggressive atmospheres. The talk presents innovative approaches to study corrosion mechanisms using advanced X-ray methods. Using energy dispersive X-ray diffraction and X-ray absorption spectroscopy in different tailor made environmental reaction chambers, valuable insights into high temperature oxidation and sulfidation processes were gained. Fe-based alloys were exposed to hot and reactive atmospheres containing gases like SO2, H2O and O2 at 650°C. During the gas exposure the tailor made reaction chambers were connected to a high energy diffraction end station at the synchrotron. The crystallization and growth of oxide and sulfide reaction products at the alloy surfaces were monitored by collecting full diffraction pattern every minute. Careful examination of shape and intensity of phase-specific reflections enabled to a detailed view on growth kinetics. These studies showed, oxides are the first phases occurring immediately after experimental start. As soon as reactive gas media enter the chamber, the conditions change and different reaction products, such as sulfides start to grow. A comparison of different gas environments applied, illustrated the differences in the type of reaction products. The in situ observation of high temperature material degradation by corrosion made it possible to study the contribution of phases, which are not stable at room temperature. For instance, wuestite (Fe1-xO), was frequently observed at high temperatures in humid gases on Fe with 2 wt.% and 9 wt.% chromium, but not at room temperature. The strength of the occurrence of this phase additionally explains why, despite a higher Cr content, ferritic alloys with 9 wt.% Cr in a challenging atmosphere prevent the intrinsic formation of protective layers. The in situ observations were supplemented by careful considerations of thermodynamic boundary conditions and detailed post characterization by classical metallographic analysis. Additionally, the structure and chemistry of the dominant oxide layers were evaluated using X-ray absorption near edge structure spectroscopy. The talk will give an overview about chances and challenges for studying high temperature corrosion phenomena by advanced X-ray methods. T2 - MRS Spring Meeting CT08.02.01 CY - Online Meeting DA - 18.04.2021 KW - XRD KW - Spectroscopy KW - Corrosion KW - High temperature KW - In-situ PY - 2021 AN - OPUS4-52486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Sample Preparation of Nano-Powders for Particle Size Determination N2 - The use of increasingly finer starting powders up to nanopowders can also be observed in the field of ceramics. Their advantages consist, for example, in their lower activation energy, an increase in strength or unique optical properties. However, handling and characterization of the powders are much more difficult. The main reason for this is the very high adhesive forces between the particles and between particles and other surfaces, too. Therefore, submicron and even more so nanoparticles tend to agglomerate and their separation into primary particles during sample preparation prior to particle sizing is of particular challenge. A representative measurement sample is only obtained when it no longer contains agglomerates. The evaluation of the dispersion process and a decision on whether it was successful thus increases in importance for the reliability of the measurement results of particle sizing. The presentation uses examples to show possible approaches and provides information on possible sources of error. It is shown that successful granulometric characterisation of fine powders requires both an improved dispersion technique and very often an effective combination of two or more measurement methods. T2 - 96. Jahrestagung der Deutschen Keramischen Gesellschaft CY - Online Meeting DA - 19.04.2021 KW - Agglomerates KW - Nano-powder KW - Dispersion process PY - 2021 AN - OPUS4-52503 LA - eng 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 - CONF A1 - Trappe, Volker T1 - Current and future technological advancement in polymer matrix composites enabled through fundamental discoveries N2 - This presentation is a summary of the work from the past 20 years’ development of PMC-testing at the BAM-FB 5.3 with respect to safety-relevant design of advanced light weight structures in aircraft, wind turbine and automotive applications. The talk begins with wood as an example from nature, and emphasizes that load case, fiber architectural design and the production process and quality have to go hand in hand to generate an advanced light weight structure. Since PMC-relevant basic findings of mankind span across hundreds of years, high-performance composite applications today are based more on long term experiences than on breakthrough inventions of modern days. In the second part of the talk, future plans and projects of FB-5.3 are presented, specifically addressing H2-safety, circular economy, recycling by design and digitalization of PMC-technologies. T2 - Abteilungsseminar CY - Online meeting DA - 07.09.2021 KW - Polymer Matrix Composites KW - Thermo mechanical fatigue PY - 2021 AN - OPUS4-54150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Beschreibung des Ermüdungsverhaltens von Endlos-Faserverstärkten-Kunststoff-Verbunden mit Hilfe mikromechanischer Modelle N2 - Im Rahmen des Vortrags werden die neusten Ergebnisse aus dem Fachbereich 5.3 zur Beschreibung des Ermüdungsverhaltens von FKV mittels Mikromechanischer-Modelle präsentiert. Explizit wird der theoretische Ansatz am Beispiel von GFK unter thermomechanischer Beanspruchung hergeleitet und an Hand von Versuchsergebnissen verifiziert. T2 - Webkonferenz Composites United, Composite Fatigue CY - Online meeting DA - 30.09.2021 KW - Faser-Kunststoff-Verbunde KW - thermomechanische Beanspruchung KW - Materialmodell PY - 2021 AN - OPUS4-54151 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dub, S. A1 - Haftaoglu, Cetin A1 - Kindrachuk, Vitaliy T1 - Estimate of theoretical shear strength of C60 single crystal by nanoindentation N2 - The onset of plasticity in a single crystal C60 fullerite was investigated by nanoindentation on the (111) crystallographic plane. The transition from elastic to plastic deformation in a contact was observed as pop-in events on loading curves. The respective resolved shear stresses were computed for the octahedral slip systems ⟨011¯¯¯⟩{111}, supposing that their activation resulted in the onset of plasticity. A finite element analysis was applied, which reproduced the elastic loading until the first pop-in, using a realistic geometry of the Berkovich indenter blunt tip. The obtained estimate of the C60 theoretical shear strength was about 1/11 of the shear modulus on {111} planes. KW - Finite element analysis KW - Fullerite KW - Nanoindentation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523208 DO - https://doi.org/10.1007/s10853-021-05991-2 VL - 56 IS - 18 SP - 10905 EP - 10914 PB - Springer Nature AN - OPUS4-52320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - JOUR A1 - Hildebrand, G. A1 - Sänger, Johanna Christiane A1 - Schirmer, U. A1 - Mantei, W. A1 - Dupuis, Y. A1 - Houbertz, R. A1 - Liefeith, K. T1 - Process Development for Additive Manufacturing of Alumina Toughened Zirconia for 3D Structures by Means of Two-Photon Absorption Technique N2 - Additive manufacturing is well established for plastics and metals, and it gets more and more implemented in a variety of industrial processes. Beside these well-established material platforms, additive manufacturing processes are highly interesting for ceramics, especially regarding resource conservation and for the production of complex three-dimensional shapes and structures with specific feature sizes in the µm and mm range with high accuracy. The usage of ceramics in 3D printing is, however, just at the beginning of a technical implementation in a continuously and fast rising field of research and development. The flexible fabrication of highly complex and precise 3D structures by means of light-induced photopolymerization that are difficult to realize using traditional ceramic fabrication methods such as casting and machining is of high importance. Generally, slurry-based ceramic 3D printing technologies involve liquid or semi-liquid polymeric systems dispersed with ceramic particles as feedstock (inks or pastes), depending on the solid loading and viscosity of the system. This paper includes all types of photo-curable polymer-ceramic-mixtures (feedstock), while demonstrating our own work on 3D printed alumina toughened zirconia based ceramic slurries with light induced polymerization on the basis of two-photon absorption (TPA) for the first time. As a proven exemplary on cuboids with varying edge length and double pyramids in the µm-range we state that real 3D micro-stereolithographic fabrication of ceramic products will be generally possible in the near future by means of TPA. This technology enables the fabrication of 3D structures with high accuracy in comparison to ceramic technologies that apply single-photon excitation. In sum, our work is intended to contribute to the fundamental development of this technology for the representation of oxide-ceramic components (proof-of-principle) and helps to exploit the high potential of additive processes in the field of bio-ceramics in the medium to long-term future. KW - Additive manufacturing KW - Ceramics 3D printing KW - Two-photon adsorption KW - Polymer-ceramic mixtures KW - Bio-ceramic engineering PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526672 DO - https://doi.org/10.3390/ceramics4020017 VL - 4 IS - 2 SP - 224 EP - 239 PB - MDPI CY - Basel AN - OPUS4-52667 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 - THES A1 - Kraus, David T1 - Ermüdungsverhalten von Glasfaser-Kunststoff-Verbunden unter thermomechanischer Beanspruchung N2 - Die Werkstoffgruppe der Faser-Kunststoff-Verbunde (FKV) hat sich aufgrund ihrer hervorragenden Leichtbaueigenschaften unter anderem im Sportgerätebau, in der Luft- und Raumfahrt und in der Windenergieindustrie etabliert. Die so hergestellten Strukturen sind in der Regel nicht nur mechanischen Belastungen, sondern auch thermischen Lasten in einem breiten Temperaturspektrum ausgesetzt. Dennoch ist die Auswirkung des Temperatureinflusses bei einer Kombination von thermischer und mechanischer Last auf die Lebensdauer von Strukturen aus FKV bisher nur wenig untersucht. Im Rahmen dieser Arbeit wird der Einfluss von Temperaturen zwischen 213 K und 343 K auf einen Glasfaser-Epoxidharz-Verbund experimentell untersucht. Das Material wird in diesem Temperaturbereich eingehend charakterisiert: Es werden sowohl die thermomechanischen Eigenschaften von Faser- und Matrixwerkstoff als auch die des Verbundes ermittelt. In einem weiteren Schritt wird dann der Einfluss der Temperatur auf die Schädigungsentwicklung im quasi-statischen Lastfall sowie unter schwingender Ermüdungsbeanspruchung bei verschiedenen FKV-Mehrschichtverbunden analysiert. Basierend auf den experimentellen Daten wird ein Zusammenhang zwischen der Schädigung und der Anstrengung der Matrix innerhalb der Einzelschicht demonstriert. Die Matrixanstrengung wird mithilfe eines mikromechanischen Modells unter Berücksichtigung der thermomechanischen Eigenspannungen analytisch berechnet. Bei Querzugbeanspruchung kann gezeigt werden, dass eine Vorhersage der Schädigung in Abhängigkeit der Volumenänderungsenergie innerhalb der Matrix getroffen werden kann. Mithilfe des Konzepts der Matrixanstrengung ist eine Vorhersage der Lebensdauer des Werkstoffs unter schwingender Ermüdungsbeanspruchung in Abhängigkeit der Einsatztemperatur möglich. N2 - Due to their superior lightweight properties, fiber reinforced polymer (FRP) materials are well established in various fields, such as sports equipment, aerospace or wind energy structures. These structures are not only subjected to mechanical loads, but also to a broad spectrum of thermal environments. However, the impact of temperature on the fatigue life of thermomechanically loaded FRP structures is barely investigated to-date. In the scope of this work, the influence of temperatures in a range of 213 K to 343 K on a glass fiber reinforced epoxy polymer is experimentally examined. An extensive thermo-mechanical characterization of the static properties of the material is performed. The neat resin and Fiber material are investigated, as well as the composite. In addition, the impact of thermal loads on the damage evolution under quasi-static as well as cyclic fatigue loading is investigated for different multi-angle laminates. Based on the experimental data, a correlation is shown between damage and matrix effort of the unidirectional layer. The matrix effort is calculated according to a micromechanical model considering thermal residual stresses. Particularly under transverse loading, the damage Evolution can be predicted as a function of the dilatational strain energy of the matrix. Using the concept of the matrix effort presented in this work, a prediction of the fatigue life of the investigated material at different ambient temperature conditions can be performed. T3 - BAM Dissertationsreihe - 169 KW - Ermüdung KW - Faser-Kunststoff-Verbund KW - GFK KW - Schädigung KW - Thermomechanik KW - Fatigue KW - Composite KW - Glas fibre reinforced polymer KW - Damage KW - Thermomechanics PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530253 SN - 1613-4249 VL - 169 SP - 1 EP - 164 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-53025 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gebhardt, M. A1 - Manolakis, I. A1 - Chatterjee, A. A1 - Kalinka, Gerhard A1 - Deubener, J. A1 - Pfnür, H. A1 - Chakraborty, S. A1 - Meiners, D. T1 - Reducing the raw material usage for room temperature infusible and polymerisable thermoplastic CFRPs through reuse of recycled waste matrix material N2 - In this work, a closed loop recycling process is investigated, which allows polymerised bulk thermoplastic matrix (Elium 150) from production waste (also referred to as recyclate) to be reused as additive in composite manufacturing by vacuum assisted resin infusion (VARI) of virgin Elium 150 monomer. It is shown that this process can save up to 7.5 wt% of virgin material usage in each processing cycle. At the same time, the thermal stability and stiffness of the composite increases with the proportion of recyclate introduced. Contemporarily, the shear and bending properties have also been observed to improve. Gel permeation chromatography (GPC) showed that the changes observed are due to an increase in molecular weight with the recyclate content. In particular, a correlation between the molecular weight and the shear properties of the composite was discovered using single fibre push-out tests. KW - Mechanical properties KW - Recycling KW - Carbon fibres KW - Fibre/matrix bond PY - 2021 DO - https://doi.org/10.1016/j.compositesb.2021.108877 SN - 1359-8368 VL - 216 SP - 108877 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-52711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kindrachuk, Vitaliy A1 - Klunker, Andre T1 - Phase field modeling of Hertzian cone cracks under spherica indentation N2 - A phase field model of brittle fracture has been developed to simulate the Hertzian crack induced by penetration of a rigid sphere to an isotropic linear-elastic half-space. The fracture formation is regarded as a diffusive field variable, which is zero for the intact material and unity if there is a crack. Crack growth is assumed to be driven by a strain invariant. The numerical implementation is performed with the finite element method and an implicit time integration scheme. The mechanical equilibrium and the phase field equations are solved in a staggered manner, sequentially updating the displacement field and the phase field variable. Numerical examples demonstrate the capability of the model to reproduce the nucleation and growth of the Hertzian cone crack. KW - Hertzian cracks KW - Phase field model KW - Contact mechanics PY - 2021 DO - https://doi.org/10.1007/s11223-021-00251-9 VL - 52 IS - 6 SP - 967 EP - 974 AN - OPUS4-52276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thuy, Maximilian T1 - Influence of molecular orientation on the environmental stress cracking resistance N2 - Molecular orientation has a significant effect on the material properties of polymers. Preferential orientation of the microstructure (polymer chains or crystallites) in a specific direction or plane often enhances the material properties, especially if the high-strength covalent bonds are primarily exposed to loads instead of the weaker van der Waals bonds. However, the orientation-dependent microstructure and its mechanical behavior is in general already well understood by many scientific studies [1-3]. Isotropic materials are frequently required for an intrinsic material characterization without prevailing processing-induced properties, as is the case for Full Notch Creep Test (FNCT) [4] addressing environmental stress cracking (ESC) in high-density polyethylene (PE-HD) [5, 6]. Since ESC is one of the major limiting issues for long-term performance of PE-HD pipes and containers [7], which in contrast have a production-related preferential orientated microstructure due to extrusion or extrusion blow molding, it is important to additionally investigate the ESC resistance of such anisotropic microstructure. Investigations of the slow crack growth (SCG) with respect to the molecular orientation generally obtain a factor of 1.2 up to 4.7 between crack growth perpendicular to the extrusion direction and crack growth parallel to the extrusion direction 8. Based on FNCT investigations with an aqueous detergent solution as environmental medium, hot pressed sheets with isotropic morphology are compared with extruded sheets from which specimens with different orientation angles are taken. However, the time to failure obtained by FNCT is also significantly influenced by the different cooling conditions under which the final morphology is formed. The tendency of the specimen to fail due to ESC is investigated as a function of environmental medium temperature. For a more detailed analysis of the affecting parameters in the manufacturing process, the ESC resistance is discussed considering the differences in crystallinity as revealed by thermal analysis. T2 - 36th International Conference of the Polymer Processing Society CY - Montreal, Canada DA - 26.09.2021 KW - Environmental stress cracking KW - Orientation-dependent microstructure KW - High-density polyethylene KW - Full Notch Creep Test PY - 2021 AN - OPUS4-53399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Busch, R. A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Patzig, C. A1 - Krause, M. A1 - Höche, T. T1 - Sample preparation for analytical scanning electron microscopy using initial notch sectioning N2 - A novel method for broad ion beam based sample sectioning using the concept of initial notches is presented. An adapted sample geometry is utilized in order to create terraces with a well-define d step in erosion depth from the surface. The method consists of milling a notch into the surface, followed by glancing-angle ion beam erosion, which leads to preferential erosion at the notch due to increased local surface elevation. The process of terrace formation can be utilized in sample preparation for analytical scanning electron microscopy in order to get efficient access to the depth-dependent microstructure of a material. It is demonstrated that the method can be applied to both conducting and non-conducting specimens. Furthermore, experimental parameters influencing the preparation success are determined. Finally, as a proof-of-concept, an electron backscatter diffraction study on a surface crystallized diopside glass ceramic is performed, where the method is used to analyze orientation dependent crystal growth phenomena occurring during growth of surface crystals into the bulk. KW - 3D etching KW - Ion beam erosion Sectioning KW - EBSD KW - Sample preparation KW - Analytical scanning electron microscopy KW - SEM KW - Glass Ceramic KW - Glass KW - Diopsid PY - 2021 DO - https://doi.org/10.1016/j.micron.2021.103090 SN - 0968-4328 VL - 150 PB - Elsevier B.V. AN - OPUS4-53075 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 - JOUR A1 - Müller, Ralf A1 - Waurischk, Tina A1 - Behrens, H. A1 - Deubener, J. T1 - Crack growth in borate and silicate glasses: Stress-corrosion susceptibility and hydrolytic resistance N2 - A double cantilever beam technique in air equipped with ultrasound modulation was used to measure the crack velocity v in borate and silicate glasses. In all glasses v and the stress intensity KI followed the empirical correlation v ~ KIn. Indicated by its smallest KI at v = 1 μm s − 1, KI* = 0.27 MPa m0.5, the silicoborate glass containing 70 mol% B2O3 was found most susceptible to stress-corrosion enhanced crack growth. Contrarily, the sodium calcium magnesium silicate glass appeared least susceptible with KI* = 0.57 MPa m0.5. No clear correlation is evident between KI*, reflecting the stress-corrosion susceptibility, and the hydrolytic resistance for all glasses under study, but values of n obtained from the present study and taken from previous literature for 35 glasses tend to decrease with increasing network modifier ion fraction. Energy dissipation during stress-corrosion enhanced crack propagation is assumed to cause this trend. KW - DCB KW - Alkali and alkaline earth silicate and borate glass KW - Crack growth in air KW - Stress-corrosion KW - Stress intensity PY - 2021 DO - https://doi.org/10.1016/j.jnoncrysol.2020.120414 VL - 551 SP - 120414 PB - Elsevier B.V. AN - OPUS4-51393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuchenbecker, Petra T1 - Granulometry of Nano Powders - a Challenge Especially for the Dispersion Process N2 - The use of increasingly finer starting powders up to nanopowders can also be observed in the field of ceramics. Their advantages consist, for example, in their lower activation energy, an increase in strength or unique optical properties. However, handling and characterization of the powders are much more difficult. The main reason for this is the very high adhesive forces between the particles and between particles and other surfaces, too. Therefore, submicron and even more so nanoparticles tend to agglomerate and their separation into primary particles during sample preparation prior to particle sizing is of particular challenge. A representative measurement sample is only obtained when it no longer contains agglomerates. The evaluation of the dispersion process and a decision on whether it was successful thus increases in importance for the reliability of the measurement results of particle sizing. The presentation uses examples to show possible approaches and provides information on possible sources of error. It is shown that successful granulometric characterisation of fine powders requires both an improved dispersion technique and very often an effective combination of two or more measurement methods. KW - Agglomerates KW - Nano-powder KW - Dispersion process PY - 2021 SN - 0173-9913 VL - 98 IS - 2 SP - 47 EP - 54 PB - Göller Verlag GmbH CY - Baden-Baden AN - OPUS4-52504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Marschall, Niklas A1 - Alig, I. A1 - Böhning, Martin T1 - A phenomenological criterion for an optical assessment of PE-HD fracture surfaces obtained from FNCT N2 - The full-notch creep test (FNCT) is a common test method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD), e.g. for container materials. The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of PE-HD specimens under constant mechanical load in a well-defined liquid test environment. Since the craze-crack damage mechanism underlying the ESC phenomenon is associated with brittle failure, the occurrence of a predominantly brittle fracture surface is a prerequisite to consider an FNCT measurement as representative for ESC, i.e. a time to failure dominated by craze-crack propagation. The craze-crack propagation continuously reduces the effective residual cross-sectional area of the specimen during the test, which results in a corresponding increase of the effective mechanical stress. Thus, a transition to ductile shear deformation is inevitable at later stages of the test, leading usually to a pronounced central ligament. Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. An enhanced imaging analysis of FNCT fracture surfaces enables a detailed assessment of craze-crack Propagation during ESC. In this study, laser scanning microscopy (LSM) was employed to evaluate whether FNCT fracture surfaces are representative with respect to craze-crack propagation and ESC. Based on LSM height data, a phenomenological criterion is proposed to assess the validity of distinct FNCT measurements. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing. Its applicability is verified on a sample basis for seven different commercial PE-HD container materials. KW - Environmental stress cracking (ESC) KW - Full notch creep test (FNCT) KW - Laser scanning microscopy (LSM) KW - Fracture surfaces KW - Optical criterion of brittleness PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521012 DO - https://doi.org/10.1016/j.polymertesting.2020.107002 VL - 94 SP - 107002 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-52101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thuy, Maximilian T1 - Umgebungsbedingter Spannungsriss: Gefahr für Kunststoffbauteile unter Medieneinfluss N2 - Polyethylen hoher Dichte (PE-HD) ist ein weit verbreitetes Material für Transportbehälter, die oft für eine längere Nutzungsdauer vorgesehen sind. Insbesondere in diesem Fall können mikroskopische Schäden im Material auch weit unterhalb der Streckgrenze auftreten, die durch eine Spannungskonzentration verursacht werden, deren Ursprung in intrinsischen Materialfehlern oder äußeren Kratzern liegt. Mit fortschreitender Schädigung bilden sich Rissstrukturen, die von verstreckten Fibrillen aufgespannt werden, bis es zum Versagen dieser Fibrillen kommt und sich der Riss ausbreitet. Dieser Schadensmechanismus des langsamen Risswachstums kann durch eine Vielzahl von Umgebungsmedien beschleunigt werden und wird dann als "environmental stress cracking" (ESC) bezeichnet. Eine international normierte Methode zur Validierung der Spannungsrissbeständigkeit von PE-HD Materialien ist der „Full Notch Creep Test“ (FNCT). Anhand von Bruchflächenauswertungen mittels Rasterelektronenmikroskopie und Laser-Scanning-Mikroskopie, werden die typischen Schädigungsstrukturen des ESC sichtbar. Die fibrillierten Strukturen des ESC auf der Bruchfläche von PE-HD ergeben sich besonders bei oberflächenaktiven wässrigen Umgebungsmedien. In Lösungsmittel-Umgebungsmedien, im Zusammenspiel mit PE-HD, kommt es aufgrund der plastifizierenden Wirkung zur Herabsetzung der Streckspannung und Bruchflächen aus dem FNCT veranschaulichen keine signifikanten Anzeichen des Schädigungsmechanismus ESC. T2 - 47. VDI-Jahrestagung Schadensanalyse 2021- Mediale und klimatische Beanspruchung von polymeren Produkten CY - Würzburg, Germany DA - 06.10.2021 KW - Umgebungsbedingter Spannungsriss KW - Polyethylen hoher Dichte KW - Full Notch Creep Test KW - Lösungsmittel KW - Oberflächenaktive wässrige Medien KW - Bruchflächenauswertung PY - 2021 AN - OPUS4-53665 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thuy, Maximilian T1 - Damage progression of environmental stress cracking affected by manufacturing process-induced microstructural orientation N2 - Currently, the Full Notch Creep Test (FNCT) [1] method is used by material suppliers and end users in industry for the approval of container and pipe materials based on high-density polyethylene (PE-HD). The resistance to environmental stress cracking (ESC) of the material is evaluated using the time to failure of the specimen in an aqueous solution of a detergent [2, 3]. Usually specimens made of sheets with isotropic material properties, manufactured by hot pressing, are employed in order to obtain intrinsic properties of the material in terms of ESC failure. In contrast, the processes used in manufacturing to form containers and pipes, such as extrusion blow molding or extrusion, impose anisotropic properties to the material. These are mostly due to a microstructural orientation (polymer chains or crystallites) [4]. Furthermore, the different cooling conditions significantly affect the size distribution of crystallites as well as the overall morphology. It is therefore essential to understand the influence of process-induced material characteristics on failure due to ESC. A large number of studies on material properties as a function of microstructural preferential orientation have already been conducted [5-7]. However, effects on ESC as the major failure mechanism of containers and pipes are still rather unexplored [8, 9]. The most important factor is whether primarily intramolecular high-strength covalent bonds or the substantially weaker intermolecular van der Waals forces are predominantly loaded. In addition to the widely established classification by time to failure, the strain or crack opening displacement (COD) provides valuable information about the evolution and progression of damage as a function of time [10, 11]. Optical strain measurement using digital image correlation allows the differences in COD for isotropic and different angles of orientation of anisotropic specimens to be discussed. Also, a post-fracture surface analysis provides clarification on the craze-crack mechanism of the ESC. These different ESC-related properties of extruded and hot-pressed specimens have been investigated at different environmental medium temperatures and different initial stresses to provide a broad characterization of the fracture behavior of PE-HD. T2 - 36th International Conference of the Polymer Processing Society CY - Montreal, Canada DA - 26.09.2021 KW - Environmental stress cracking KW - High-density polyethylene KW - Fracture behavior KW - Microstructural orientation PY - 2021 AN - OPUS4-53400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghafafian, Carineh A1 - Popiela, Bartosz A1 - Trappe, Volker T1 - Failure Mechanisms of GFRP Scarf Joints under Tensile Load N2 - A potential repair alternative to restoring the mechanical properties of lightweight fiberreinforced polymer (FRP) structures is to locally patch these areas with scarf joints. The effects of such repair methods on the structural integrity, however, are still largely unknown. In this paper, the mechanical property restoration, failure mechanism, and influence of fiber orientation mismatch between parent and repair materials of 1:50 scarf joints are studied on monolithic glass fiber-reinforced polymer (GFRP) specimens under tensile load. Two different parent orientations of [-45/+45]2S and [0/90]2S are exemplarily examined, and control specimens are taken as a baseline for the tensile strength and stiffness property recovery assessment. Using a layer-wise stress analysis with finite element simulations conducted with ANSYS Composite PrepPost to support the experimental investigation, the fiber orientation with respect to load direction is shown to affect the critical regions and thereby failure mechanism of the scarf joint specimens. KW - Scarf joint KW - Glass fiber reinforced polymers KW - Failure mechanisms PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523952 DO - https://doi.org/10.3390/ma14071806 VL - 14 IS - 7 SP - 1806 PB - MDPI CY - Basel, Switzerland AN - OPUS4-52395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tielemann, Christopher A1 - Busch, R. A1 - Reinsch, Stefan A1 - Patzig, C. A1 - Höche, T. A1 - Avramov, I. A1 - Müller, Ralf T1 - Oriented surface nucleation in diopside glass N2 - Es wird die Texturbildung in kristallisierendem Diopsidglas im Zusammenhang mit der Oberflächenbeschaffenheit der unbehandelten Probe untersucht. Zudem wird der diskutiert, dass es sich bei der Texturbildung in Gläsern höchstwahrscheinlich um ein Nukleationsphänomen handelt welches auf die richtungsabhängige Grenzflächenenergie der kristallisierenden Phase zurückzuführen ist. N2 - Oriented surface crystallization on polished diopside glass surfaces has been studied with scanning electron microscopy, electron backscatter diffraction, transmission electron microscopy and laser scanning microscopy. An orientation preference of [001] parallel to the glass surface was detected for separately growing diopside crystals even as small as 700 nm in size. This finding shows that crystal orientation occurs in the outermost surface layer without crystal-crystal interaction and indicates that the crystal orientation is a result of oriented nucleation. Depending on surface preparation, monomodal crystal orientation distributions with [100] perpendicular to the surface or bimodal distributions with [100] and [010] perpendicular to the glass Surface were detected. It was also shown that the degree of crystal orientation increases with decreasing Surface roughness. The observed orientation of diopside crystals could be explained in terms of the interfacial energies of different crystal faces. KW - Surface energy KW - Glass ceramic KW - Glass KW - EBSD KW - Diopsid PY - 2021 UR - https://www.sciencedirect.com/science/article/pii/S002230932100020X DO - https://doi.org/10.1016/j.jnoncrysol.2021.120661 SN - 0022-3093 VL - 562 PB - Elsevier B.V. AN - OPUS4-53073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Rouxel, T. A1 - Behrens, H. A1 - Deubener, J. A1 - Müller, Ralf T1 - Vacuum crack growth in alkali silicate glasses N2 - Crack growth velocity in alkali silicate glasses was measured in vacuum across 10 orders of magnitude with double cantilever beam technique. Measured and literature crack growth data were compared with calculated intrinsic fracture toughness data obtained from Young´s moduli and the theoretical fracture surface energy estimated from chemical bond energies. Data analysis reveals significant deviations from this intrinsic brittle fracture behavior. These deviations do not follow simple compositional trends. Two opposing processes may explain this finding: a decrease in the apparent fracture surface energy due to stress-induced chemical changes at the crack tip and its increase due to energy dissipation during fracture. KW - Silicate glass KW - Brittle fracture KW - Crack growth KW - Calculated intrinsic fracture toughness PY - 2021 DO - https://doi.org/10.1016/j.jnoncrysol.2021.121094 SN - 0022-3093 VL - 572 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-53144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Sintering of silver‑alkali zinc borate glass‑composites N2 - Since decades electric contacts based on silver metallization pastes are key components of photovoltaics and advanced microelectronics. For the metallization of commercial Si solar cells, high conductive silver glass pastes are cost effectively applicated by screen printing. Nevertheless, silver pastes are still one of the most crucial and expensive none Si materials in solar cells. Ever shorter time to market as well as increasing demands on reduced Ag consumption and line width require the targeted development of silver-glass-pastes with increased sinter ability and electrical conductivity. As a main difficulty, however, the liquid phase sintering of silver glass pastes is poorly understood so far. In the present study, the influence of different network modifier in alkali-zinc-borate paste glasses on liquid phase sintering of silver-glass-pastes was investigated. Low melting X2O-ZnO-B2O3 glasses with X = Na, Li and Rb (abbr. LZB, NZB, and RZB) were utilized to prepare silver-glass-composites containing 30 %Vol glass. Shrinkage behavior of the silver-glass-composites compared with that of pure silver and pure glass powder compacts was studied with heating microscopy. The powder compacts were uniaxially pressed and heated at 5 K/min to the glass softening temperature. Glass transformation temperature and viscosity of the glasses were respectively measured with dilatometry and rotational viscometry. The thermal behavior of the pure glasses was analyzed with thermal analysis. Additionally, the contact angle of glass on pure silver foil was determined by means of heating microscopy between room temperature and 830 °C. Thermal analysis of the alkali-zinc-borate-glasses under study has shown transformation temperatures between 450 °C (RZB), 460 °C (LZB) and 465 °C (NZB). For all glasses crystallization was found to start approximately at about 550 °C. However, different peak areas hint on a different degree of crystallization. Conformingly, the sintering behavior, measured in terms of area shrinkage, significantly differed for the silver-pastes under study. For silver-pastes with NZB or LZB-glass, sintering starts at 464 °C for NZB Ag pastes and at 451 °C for LZB Ag pastes and ends at 597 °C for NZB Ag paste and at 594 °C for LZB Ag paste. The sintering of the RZB Ag paste proceeds between 426 °C and 703 °C. The final densification was retarded possibly due to crystallization or swelling. The low sinter onset at 426 °C seems to correlate with the good wetting behavior of the RZB glass. Thus, the lowest apparent contact angle between the just densified powder compact sintered at a silver substrate was found for this glass. Moreover, microstructure analyses of the various composites indicate differences in silver dissolution and reprecipitation. T2 - Technology Crossover Extravaganza, HiTEC/CICMT/APEPS CY - Online meeting DA - 26.04.2021 KW - Silver-glass-metallization-paste KW - Sintering KW - Crystallization KW - Alkali ions KW - Sintering atmosphere PY - 2021 AN - OPUS4-52872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Sintering and Foaming of Silicate Glass Powders N2 - The lecture focuses on the mechanisms of non-desired gas bubble formation and foaming during the sintering of glass powder compacts. It is shown that foaming is driven by carbon gases and that carbonates, encapsulated in micropores or mechaniacally dissolved beneath the glass surface, provide the major foaming source. T2 - Sandanski Workshop Sinter crystallization 27th-29th September 2021 PROJECT “THEORY AND APPLICATIONS OF SINTER-CYSTALLIZATION” DN 19/7 CY - Online meeting DA - 27.10. 2021 KW - Sintering KW - Non-desired foaming PY - 2021 AN - OPUS4-53772 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 - Thuy, Maximilian A1 - Niebergall, Ute A1 - Oehler, H. A1 - Alig, I. A1 - Böhning, Martin T1 - Evaluation of the damaging effect of crop protection formulations on high density polyethylene using the Full Notch Creep Test N2 - Four typical high-density polyethylene container materials were used to investigate damage or stress cracking behavior in contact with model liquids for crop protection products. These model liquids are established in German regulations for the approval of dangerous goods containers and consist of typical admixtures used for crop protection products but without biological active ingredients. This study is performed with the standardized method of Full Notch Creep Test, adapting the media temperature to 40 °C according to the usual conditions where these test liquids are applied. The two model liquids differ into a water-based solution and a composition based on different organic solvents which are absorbed by the material up to significant levels. Therefore, extensive sorption measurements are performed. The fracture surfaces obtained are analyzed in detail not only by light microscopy, but also by laser scanning microscopy as well as scanning electron microscopy. Influence of pre-saturation and applied stress are addressed by respective systematic series of experiments. KW - Polyethylene KW - Full Notch Creep Test KW - Environmental Stress Cracking KW - Fracture PY - 2021 DO - https://doi.org/10.1016/j.polymer.2021.123853 SN - 0032-3861 VL - 228 SP - 123853 PB - Elsevier Ltd. AN - OPUS4-52686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -