TY - CONF A1 - Sommer, Konstantin A1 - Bettge, Dirk A1 - Nolze, Gert T1 - Microstructure analysis in AM 316L N2 - Additive manufacturing (AM) offers diverse advantages compared to conventional manufacturing. In this work the microstructure of austenitic steel 316L, manufactured with Selective Laser Melting (SLM), was analyzed and compared to microstructure of 316L hot rolled material. Methods used for analysis are microprobe, optical microscopy and electron backscatter diffraction. T2 - BAM workshop on Additive Manufacturing CY - Berlin, Germany DA - 13.05.2019 KW - 316L KW - selective laser melting KW - microstructure analysis PY - 2019 AN - OPUS4-49880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sommer, Konstantin A1 - Bettge, Dirk A1 - Nolze, Gert T1 - Microstructure Characterization of Additively Manufactured Austenitic Steel 316L N2 - Additive manufacturing processes (AM) offer different advantages compared to conventional manufacturing processes. In this work the microstructure of austenitic steel 316L, manufactured with Selective Laser Melting (SLM), and the powder, used for the process, were investigated. T2 - BAM workshop on Additive Manufacturing CY - Berlin, Germany DA - 13.05.2019 KW - 316L KW - Selective laser melting KW - Microstructure analysis KW - Metal powder characterization PY - 2019 AN - OPUS4-49884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kranzmann, Axel A1 - Midtlyng, Jan A1 - Schlitte, I.-V. A1 - Escoda de Pablo, S. T1 - Corrosion of VM12 SHC in Salt melt N2 - Alkali and alkaline earth chlorides are discussed as heat storage media and are characterized by their low price and high availability. Disadvantages are a high corrosion rate and formation of Cr6+ ions in the melt, as observed in various binary chlorine salt melts. In our work the system NaCl-KCl-MgCl2 is considered. The storage capacity in this salt system is between 2 and 3 MWh per 10 t salt, depending on composition, melting temperature and working temperature. At the same time the system offers a eutectic line, which allows a high variance of the composition and possibly different corrosion rates can be observed. Corrosion tests in melts were carried out and the corrosion layers investigated. The tests with chloride melts on 12% Cr steel show an inner corrosion zone of up to 40 µm depth after 96 hours. The corrosion mechanisms and potential solutions are discussed. T2 - EUROCORR 2019 CY - Sevilla, Spain DA - 09.09.2019 KW - Salt melt KW - Corrosion KW - VM12 SHC PY - 2019 AN - OPUS4-50759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Probenpräparation für AFM-basierte Untersuchungsverfahren N2 - Adapted and advanced sample preparation of semiconductor layer systems with the focused ion beam for AFM-based test methods N2 - Der vorliegende Vortrag gibt einen Überblick über Probenpräparationen mit der Focused Ion Beam (FIB) für AFM-basierte Untersuchungsverfahren. Anhand zweier Beispiele wird gezeigt, wie ionenstrahlpolierte Lamellen aus Halbleiter-Schichtsystemen elektrisch leitfähig auf Substrate platziert werden, so dass in-situ und in-operando Messungen mit Scanning Microwave Microscope (SMM) bzw. Spectroscopic infrared scanning near-field optical microscope (IR-SNOM) durchgeführt werden können. T2 - 15. Berlin-Brandenburger Präparatorentreffen CY - Potsdam/Golm, Germany DA - 11.04.2019 KW - Focused Ion Beam KW - AFM based test methods KW - Sample preparation KW - Semiconductor materials KW - Layer system PY - 2019 AN - OPUS4-47784 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph A1 - Le, Quynh Hoa A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Knauer, S. T1 - Factors Influencing Droplet Corrosion in Dense Phase CO2 N2 - This work examined the factors that influence the droplet corrosion of CO2 pipeline steels caused by oxyfuel flue gases in dense phase CO2 at 278 K, simulating the underground transport conditions. The wetting properties were studied by contact angle measurement, revealing pH and time dependency on the reactive wetting behaviors of carbon steel X70. Exposure tests with CO2 saturated water droplet on steel surface showed that the impurities (220 ppmv SO2 and 6700 ppmv O2) diffused into the droplet and then reacted with metal surfaces in dense phase condition, forming the corrosion products. The corrosion rate was confirmed strongly depending on the droplet volume as well as the SO2 concentration. Condensation experiments carried out on freshly polished coupons in CO2 with 200 ppmv H2O, 220 ppmv SO2 and 6700 ppmv O2, showed that the formation and aggregation of droplets is time and temperature dependent. At 278 K, condensation happened stronger and the corrosion products, mainly consisted of dense hydrated FeSO3/FeSO4. While at 288 K, more fluffy corrosion products consisting of iron oxide/hydroxide and hydrated FeSO3/FeSO4 were found. Further exposure tests on carbon steel coupons with different surface roughness did not reveal the difference in weight loss/gain and therefore the corrosion rate. T2 - NACE International Corrosion Conference 2019 CY - Nashville, TN, USA DA - 24.03.2019 KW - Carbon Capture, Utilization and Storage (CCUS) KW - Supercritical/dense phase CO2 KW - Carbon steel KW - Droplet corrosion KW - Condensation PY - 2019 AN - OPUS4-47916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph A1 - Le, Quynh Hoa A1 - Yevtushenko, Oleksandra A1 - Bettge, Dirk T1 - Corrosion Aspects for Materials to be Used in CC(U)S Applications N2 - This contribution provides current findings regarding materials susceptibility for carbon capture, utilization and storage (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 material recommendations for certain parts. T2 - 1st International Conference on Corrosion Protection and Application CY - Chongqing, China DA - 09.09.2019 KW - Carbon KW - Capture KW - Storage KW - Utilization KW - CCS KW - CCU KW - CO2 KW - Corrosion PY - 2019 AN - OPUS4-49302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Roohbakhshan, Farshad A1 - Nolze, Gert A1 - Fedelich, Bernard A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Cyclic Operation Performance of 9-12% Cr Ferritic-Martensitic Steels. Part 2: Microstructural Evolution during Cyclic Loading and its Representation in a Physically-based Micromechanical Model N2 - The current trend towards cyclic, “flexible” operation of fossil-fueled power plants constitutes a major issue regarding lifetime and operational safety of the respective installations and their components, as was outlined in our complementary contribution (Part 1). The present contribution reports on the investigation of the microstructure evolution in cyclically loaded ferritic-martensitic steels and its representation in a physically-based micromechanical model. For this purpose, specimens of P92 steel grade from the mechanical test programme outlined in our companion contribution (Part 1) were analyzed by scanning electron microscopy (SEM), including backscattered diffraction (EBSD) mapping, and transmission electron microscopy (TEM). A novel method was implemented to improve angular resolution of EBSD scans. Additionally, a correlative microscopy approach was developed and used to correlate EBSD and TEM measurements on the same locations of thick regions of electron transparent specimens. By applying these techniques, a detailed quantitative microstructure description of the as-received material condition, namely in terms of subgrain morphology and dislocation density/distributions, was established. Comparisons of as-received and cyclically loaded conditions from tests interrupted at different stages of lifetime indicate a rapid redistribution of in-grain dislocations with a strong interaction between mobile dislocations and low angle grain boundaries (LABs). The proposed micromechanical model is formulated in a viscoplastic self-consistent (VPSC) scheme, which is a mean-field approach that allows us to include the crystal details at the level of slip systems while avoiding the considerable computational costs of full-field approaches (such as the classical crystal plasticity finite element analysis). Being physically-based, the model uses dislocation densities and includes the interaction between dislocations, e.g. annihilation of mobile dislocations, and evolution of microstructure, e.g. the grain coarsening. Particularly, the constitutive laws for dislocation evolution and interaction between dislocations and low angle boundaries are calibrated based on two-dimensional discrete dislocation dynamic (2D DDD) simulations, which are performed at a micro-/meso-scale. The results of the beforementioned EBSD experiments are considered as a direct input, involving e.g. the amount of geometrically necessary dislocations, average misorientations and grain characteristics. T2 - 45th MPA-Seminar 2019 CY - Leinfelden-Echterdingen, Germany DA - 01.10.2019 KW - Tempered martensite ferritic steel KW - Dislocation KW - Electron backscattered diffraction (EBSD) KW - Transmission electron microscopy (TEM) KW - Microstructure KW - Physically based material model PY - 2019 AN - OPUS4-49346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Wachtendorf, Volker A1 - Elert, Anna Maria A1 - Falkenhagen, Jana A1 - Becker, Roland A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Tschiche, Harald A1 - Reinsch, Stefan A1 - Weidner, Steffen ED - Scholz, Philipp T1 - Analytical toolset to characterize polyurethanes after exposure to artificial weathering under systematically varied moisture conditions N2 - Polyether and -ester urethanes (PU) were exposed to artificial weathering at 40 °C and artificial UV radiation in a weathering chamber. In 3 parallel exposures, humidity was varied between dry, humid, and wet conditions. Material alteration was investigated by various analytical techniques like size exclusion chromatography (SEC), liquid chromatography-infrared spectroscopy (LC-FTIR), thermal-desorption gas chromatography-mass spectrometry (TD-GC-MS), fluorescence mapping and dynamic mechanical analysis (DMA). Our results show that depending on the weathering conditions, different degradation effects can be observed. By means of SEC an initial strong decrease of the molar masses and a broadening of the mass distributions was found. After a material dependent time span this was followed by a plateau where molar mass changes were less significant. A minor moisture-dependent degradation effect was only found for polyester PU. Fluorescence measurements on two materials revealed an increase in the luminescence intensity upon weathering process reaching a saturation level after about 500 h. The changes in the optical properties observed after different exposure conditions and times were very similar. The TD-GC-MS data showed the fate of the stabilizers and antioxidant in the course of weathering. LC-FTIR measurements revealed a change in peak intensities and the ratio of urethane and carbonyl bands. KW - Polyurethane KW - Artificial weathering KW - Moisture KW - Crosslinking KW - Degradation PY - 2019 UR - https://www.sciencedirect.com/science/article/pii/S0142941819303708 DO - https://doi.org/10.1016/j.polymertesting.2019.105996 SN - 0142-9418 VL - 78 SP - 105996, 1 EP - 9 PB - Elsevier CY - Amsterdam AN - OPUS4-48625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Humphrey, J.K. A1 - Gibson, A.G. A1 - Hörold, Andreas A1 - Trappe, Volker A1 - Gettwert, V. T1 - Assessing the structural integrity of carbon-fibre sandwich panels in fire: Bench-scale approach N2 - The fire resistance of lightweight sandwich panels (SW) with carbon fibre/epoxy skins and a poly(methacryl imide) (PMI) foam core is investigated in compression under direct application of a severe flame (heat flux=200 kW m−2). A bench-scale test procedure was used, with the sample held vertically. The epoxy decomposition temperature was quickly exceeded, with rapid flash-over and progressive core softening and decomposition. There is a change in failure mode depending on whether the load is greater or less than 50% of the unexposed failure load, or in other words if one or two skins carry the load. At high loads, failure involved both skins with a single clear linear separation across each face. There is an inflection in the failure time relationship in the ∼50% load region, corresponding to the time taken for heat to be transmitted to the rear face, along with a change in the rear skin failure mode from separation to the formation of a plastic hinge. The integrity of the carbon front face, even with the resin burnt out, and the low thermal diffusivity of the core, both play key roles in prolonging rear face integrity, something to be borne in mind for future panel design. Intumescent coatings prolong the period before failure occurs. The ratio of times to failure with and without protection is proposed as a measure of their effectiveness. Apart from insulation properties, their adhesion and stability under severe fire impact play a key role. KW - Carbon fibres KW - Sandwich KW - Structural composites KW - Fracture KW - High-temperature properties KW - Surface treatments PY - 2019 DO - https://doi.org/10.1016/j.compositesb.2018.11.077 SN - 1359-8368 VL - 164 SP - 82 EP - 89 PB - Elsevier AN - OPUS4-46908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baesso, Ilaria A1 - Altenburg, Simon A1 - Günster, Jens T1 - Co-axial online monitoring of Laser Beam Melting (LBM) N2 - Within the perspective of increasing reliability of AM processes, real-time monitoring allows part inspection while it is built and simultaneous defect detection. Further developments of real-time monitoring can also bring to self-regulating process controls. Key points to reach such a goal are the extensive research and knowledge of correlations between sensor signals and their causes in the process. T2 - BAM workshop on Additive Manufacturing CY - BAM, Berlin, Germany DA - 13.05.2019 KW - Laser Beam Melting KW - Process Monitoring KW - Co-axial monitoring KW - 3D imaging PY - 2019 AN - OPUS4-48517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Elert, Anna Maria A1 - Hodoroaba, Vasile-Dan A1 - Agudo Jácome, Leonardo A1 - Altmann, Korinna A1 - Silbernagl, Dorothee A1 - Sturm, Heinz T1 - Short- and long-range mechanical and chemical interphases caused by interaction of Boehmite (γ-AlOOH) with anhydride-cured epoxy resins N2 - Understanding the interaction between boehmite and epoxy and the formation of their interphases with different mechanical and chemical structures is crucial to predict and optimize the properties of epoxy-boehmite nanocomposites. Probing the interfacial properties with atomic force microscopy (AFM)-based methods, especially particle-matrix long-range interactions, is challenging. This is due to size limitations of various analytical methods in resolving nanoparticles and their interphases, the overlap of interphases, and the effect of buried particles that prevent the accurate interphase property measurement. Here, we develop a layered model system in which the epoxy is cured in contact with a thin layer of hydrothermally synthesized boehmite. Different microscopy methods are employed to evaluate the interfacial properties. With intermodulation atomic force microscopy (ImAFM) and amplitude dependence force spectroscopy (ADFS), which contain information about stiffness, electrostatic, and van der Waals forces, a soft interphase was detected between the epoxy and boehmite. Surface potential maps obtained by scanning Kelvin probe microscopy (SKPM) revealed another interphase about one order of magnitude larger than the mechanical interphase. The AFM-infrared spectroscopy (AFM-IR) technique reveals that the soft interphase consists of unreacted curing agent. The long-range electrical interphase is attributed to the chemical alteration of the bulk epoxy and the formation of new absorption bands. KW - Nanocomposites KW - Interphase KW - Intermodulation AFM KW - Electron microscopy KW - Infrared nano AFM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483672 UR - https://www.mdpi.com/2079-4991/9/6/853/htm DO - https://doi.org/10.3390/nano9060853 SN - 2079-4991 VL - 9 IS - 6 SP - 853, 1 EP - 20 PB - MDPI AN - OPUS4-48367 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 - Giovanelli, F. A1 - Rabe, Torsten T1 - Influence of pressure assisted sintering and reaction sintering on microstructure and thermoelectric properties of bi-doped and undoped calcium cobaltite N2 - Calcium cobaltite (Ca3Co4O9) is considered as one of the most promising thermoelectric p-type oxides for energy harvesting applications at temperatures above 500 °C. It is challenging to sinter this material as its stability is limited to 920 °C. To facilitate a practicable and scalable production of Ca3Co4O9 for multilayer generators, a systematic study of the influence of powder calcination, Bi-doping, reaction sintering, and pressure-assisted sintering (PAS) on microstructure and thermoelectric properties is presented. Batches of doped, undoped, calcined, and not calcined powders were prepared, tape-cast, and sintered with and without uniaxial pressure at 900 °C. The resulting phase compositions, microstructures and thermoelectric properties were analysed. It is shown that the beneficial effect of Bi-doping observed on pressureless sintered samples cannot be transferred to PAS. Liquid phase formation induces distortions and abnormal grain growth. Although the Seebeck coefficient is increased to 139 µV/K by Bi-doping, the power factor is low due to poor electrical conductivity. The best results were achieved by PAS of calcined powder. The dense and textured microstructure exhibits a high power factor of 326 µW/mK² at 800 °C but adversely high thermal conductivity in the relevant direction. The figure of merit is higher than 0.08 at 700 °C. KW - Ceramics KW - Calcium cobaltite KW - Thermoelectric properties KW - Calcination KW - Pressure-assisted sintering PY - 2019 DO - https://doi.org/10.1063/1.5107476 SN - 0021-8979 VL - 126 IS - 7 SP - 075102-1 EP - 075102-11 PB - AIP Publishing CY - Melville AN - OPUS4-48708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Small batch preparation of ready-to-press powder for systematic studies N2 - Efficient studies of scarce or expensive materials require material saving processes. Therefore, a high yield concept for small batch preparation of ready-to-press powder is exemplarily presented for yttria stabilized nano-zirconia (d50 < 50 nm). The concept involves small batch preparation in an ultrasound resonator, dispersant selection based on zeta potential measurements, evaluation of slurry stability using an analytical centrifuge, and preparation of ready-to-press powder by freeze drying. Freeze drying offers key advantages. Process efficiency and high yield above 95 % are independent of sample size. The dried product does not require further mechanical treatment like milling or grinding. Side effects like migration of additives are avoided. An optimized freeze drying process tolerates slurries with moderate stability. Thus, efforts for slurry development can be reduced. Generally, identifying a suitable dispersing agent requires only 3-5 zeta potential measurements. Slurry stability is rechecked using an analytical centrifuge, which also accounts for steric stabilization. An ultrasound resonator is used to disperse the powder without contamination, which becomes critical for small batches. The described route is exemplarily presented for the development of an additive recipe for nano-sized zirconia powder, targeting for good pressing behavior and high green density. Therefore, a variety of binding and lubricating agents were tested. Following the presented route, 80 g zirconia powder were sufficient to conduct a study including slurry development and five sample sets with varying composition, each set comprising five discs (d = 20 mm and h = 2 mm). T2 - 94. DKG Jahrestagung CY - Leoben, Austria DA - 05.05.2019 KW - Fine Powder KW - Slurry KW - Freeze Drying PY - 2019 AN - OPUS4-48293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geyler, Paul A1 - Rabe, Torsten A1 - Mieller, Björn A1 - Léonard, Fabien T1 - Machine learning assisted evaluation of the shape of VIAs in a LTCC multilayer N2 - The introduction of the 5G technology and automotive radar applications moving into higher frequency ranges trigger further miniaturization of LTCC technology (low temperature co-fired ceramics). To assess dimensional tolerances of inner metal structures of an industrially produced LTCC multilayer, computer tomography (CT) scans were evaluated by machine learning segmentation. The tested multilayer consists of several layers of a glass ceramic substrate with low resistance silver-based vertical interconnect access (VIA). The VIAs are punched into the LTCC green tape and then filled with silver-based pastes before stacking and sintering. These geometries must abide by strict tolerance requirements to ensure the high frequency properties. This poster presents a method to extract shape and size specific data from these VIAs. For this purpose, 4 measurements, each containing 3 to 4 samples, were segmented using the trainable WEKA segmentation, a non-commercial machine learning tool. The dimensional stability of the VIA can be evaluated regarding the edge-displacement as well as the cross-sectional area. Deviation from the ideal tubular shape is best measured by aspect ratio of each individual layer. The herein described method allows for a fast and semi-automatic analysis of considerable amount of structural data. This data can then be quantified by shape descriptors to illustrate 3-dimensional information in a concise manner. Inter alia, a 45 % periodical change of cross-sectional area is demonstrated. T2 - DKG Jahrestagung 2019 CY - Leoben, Austria DA - 06.05.2019 KW - Machine Learning KW - LTCC multilayer KW - 5G PY - 2019 AN - OPUS4-48289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Electrode area dependence of dielectric breakdown strength N2 - Dielectric breakdown of ceramics is widely believed to originate from microstructural defects. Still, there is no commonly accepted model for the origin and process of dielectric failure that covers all observed phenomena and dependencies. In analogy to mechanical strength, the Weibull distribution is commonly used to evaluate dielectric strength data. This works well for a given group of specimens with constant geometry. But unlike mechanical strength, dielectric strength scales with the inverse square root of sample thickness. This cannot be explained by the classic Weibull concept. The Griffith type energy release rate model of dielectric breakdown proposed by Schneider is based on space charge injection and conducting filaments from the sample surface. This model incorporates the distinct thickness dependence and the pronounced influence of surface defects. Based on this model and the classic Weibull probability of failure, Schneider’s group theoretically derived a probability of breakdown that predicts an increase of failure probability with increasing electrode area. In our study we tested this model with dielectric strength data measured on dense alumina samples using different electrode areas. Weibull modulus and characteristic dielectric strength (scale parameter) were determined for a set of measurements using small electrodes. These values were used to calculate the failure probability under large electrodes according to the model. The calculated data excellently fits the measured values. Thus, our experiments substantiate the assumptions made in the breakdown model and the significance of surface defects for dielectric failure. T2 - 94. DKG Jahrestagung CY - Leoben, Austria DA - 05.05.2019 KW - Dielectric strength KW - Breakdown strength KW - Ceramics PY - 2019 AN - OPUS4-48015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Evaluation of a multi-purpose measurement cell for standardized volume resistivity measurements at high temperatures N2 - The ProboStat is a multi-purpose measurement cell suitable for various electrical and physical measurements under different atmospheres and at high temperatures. Disc and bar shaped samples are sandwiched between platinum electrodes at the top of the tubular cell. The gas tight assembly can be inserted into a furnace. Different gases can be flushed through the tube. For this study, a ProboStat was adapted to measure volume resistivity of ceramic insulators at high temperatures according to standards. The standardized measurement of volume resistivity of ceramic insulators requires the consideration of many specifications including sample diameter, thickness, electrode design, and the proportion of these characteristics. Measurements are ideally performed in a state of dielectric equilibrium. The time-related slope of resistivity of a specific sample follows a power function. Thus, care must be taken when choosing a charge time or defining the duration of a measurement. As fringing of the guarded electrode occurs under high voltage, the effective electrode area for evaluation of the results should be corrected with respect to sample thickness and electrode design. The demands of effective standards on sample geometry and electrode design are stricter for room temperature measurements than for high temperature measurements. To perform high temperature measurements on ceramic samples that also fulfill the demands on room temperature measurements, a ProboStat was equipped with a dedicated large sample setup for discs with diameters of up to 60 mm. The volume resistivity of different alumina samples was first measured at room temperature in a standard test fixture and then compared to results obtained with the ProboStat. All measurements were performed for at least 100 min using a 26 mm guarded electrode. High temperature measurements at 500 °C were performed using the same samples. Room temperature values obtained with the standard test fixture are in the order of 10^17 Ohm·cm. The quantitative effect of electrode area correction is presented. Practical issues related to the use of the multi-purpose cell are addressed. These include electrode material selection, application of electrodes, and compensation of leakage currents. High temperature results of volume resistivity of the different alumina samples are presented. The validity is discussed with respect to the suitability of the multi-purpose cell for such measurements. T2 - XVI Conference and Exhibition of the European Ceramic Society (ECerS 2019) CY - Torino, Italy DA - 16.06.2019 KW - ceramics KW - alumina KW - volume resistivity PY - 2019 AN - OPUS4-48270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, Kathrin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Stephan-Scherb, Christiane T1 - A µ‐XANES study of the combined oxidation/sulfidation of Fe–Cr model alloys N2 - The precise analysis of cation diffusion profiles through corrosion scales is an important aspect to evaluate corrosion phenomena under multicomponent chemical load, as during high‐temperature corrosion under deposits and salts. The present study shows a comprehensive analysis of cation diffusion profiles by electron microprobe analysis and microbeam X‐ray absorption near edge structure (µ‐XANES) spectroscopy in mixed oxide/sulfide scales grown on Fe–Cr model alloys after exposing them to 0.5% SO2. The results presented here correspond to depth‐dependent phase identification of oxides and sulfides in the corrosion scales by µ‐XANES and the description of oxidation‐state‐dependent diffusion profiles. Scales grown on low‐ and high‐alloyed materials show both a well‐pronounced diffusion profile with a high concentration of Fe3+ at the gas and a high concentration of Fe2+ at the alloy interface. The distribution of the cations within a close‐packed oxide lattice is strongly influencing the lattice diffusion phenomena due to their different oxidation states and therefore different crystal‐field preference energies. This issue is discussed based on the results obtained by µ‐XANES analysis. KW - X-ray absorption spectroscopy KW - Oxidation KW - Sulfidation PY - 2019 DO - https://doi.org/10.1002/maco.201810644 VL - 70 IS - 8 SP - 1360 EP - 1370 PB - Wiley VCH-Verlag AN - OPUS4-47934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jürgens, Maria A1 - Sonntag, Nadja A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Cyclic operation performance of 9-12% Cr ferritic-martensitic steels part 1: Cyclic mechanical behavior under fatigue and creep-fatigue loading N2 - The current competitive situation on electricity markets forces power plants into cyclic operation regimes with frequent load shifts and starts/shutdowns. In the present work, the cyclic mechanical behavior of ferritic-martensitic 9-12 % Cr steels under isothermal and thermomechanical loading was investigated for the example of grade P92 material. A continuous softening was observed under all loading conditions. The introduction of hold periods to the applied cycles reduced material lifetime, with most prominent effects at technologically relevant small strain levels. The microstructural characterization reveals a coarsening of the original “martensitic” lath-type microstructure to a structure with polygonal subgrains and reduced dislocation density. The microstructural data forms the input for a physically-based modelling approach, both of which are presented in “Part 2: Microstructural Evolution during Cyclic Loading and its Representation in a Physically-based Micromechanical Model“. T2 - 45. MPA-Seminar CY - Leinfelden-Echterdingen, Germany DA - 01.10.2019 KW - Tempered Martensite Ferritic Steels KW - P92 KW - Low Cycle Fatigue KW - Thermo-Mechanical Fatigue KW - Creep-Fatigue PY - 2019 SP - 75 EP - 79 PB - MPA (Materialprüfungsanstalt Universität Stuttgart) CY - Stuttgart AN - OPUS4-50051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander A1 - Mohr, Gunther A1 - Hilgenberg, Kai A1 - Straße, Anne A1 - Gumenyuk, Andrey A1 - Winterkorn, René A1 - Pittner, Andreas A1 - Sommer, Konstantin A1 - Bettge, Dirk A1 - Kranzmann, Axel A1 - Nolze, Gert A1 - Avila, Luis A1 - Rehmer, Birgit A1 - Charmi, Amir A1 - Falkenberg, Rainer A1 - Skrotzki, Birgit A1 - Werner, Tiago A1 - Madia, Mauro A1 - Zerbst, Uwe A1 - Ulbricht, Alexander A1 - Sprengel, Maximilian A1 - Kromm, Arne A1 - Thiede, Tobias A1 - Bruno, Giovanni T1 - Ageing in additively manufactured metallic components: from powder to mechanical failure” an overview of the project agil N2 - An overview of the BAM funed Focus Area Materials Project "AGIL" will be presented. AGIL focussed on the stdiy of the ageing characteristics of additively manufactured austenitic stainless steel with a "powder to mechanical failure" Approach. Recent Highlights are presented and a perspective for future studies. T2 - Workshop on Additive Manufacturing CY - BAM, Berlin, Germany DA - 13.05.2019 KW - Residual stress KW - Additive Manufacturing KW - Non-destructive testing KW - Microstructure characterisation KW - Tensile testing KW - Fatigue KW - Crystal Plasticity Modelling KW - Crack propagation PY - 2019 AN - OPUS4-49823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Jürgens, Maria A1 - Sonntag, Nadja A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Cyclic operation performance of 9 -12% cr ferritic martensitic steels part 1: cyclic mechanical behavior under fatigue and creep fatigue loading N2 - 9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in fossil fueled power plants due to their excellent creep and oxidation resistance, but changes in electricity markets during the last two decades have considerably changed the typical working conditions of these facilities. The growing share of renewable energy sources in power generation forces most of these plants into flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue, raising the question which fundamental processes govern the reaction of ferritic-martensitic steels to cyclic load and temperature variations. The present contribution reports on current findings obtained in a multidisciplinary project funded by German Ministry of Education and Research (BMBF) which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses and related micromechanical modeling. In the present first part of our contribution, an overview will be given on the results obtained in the mechanical testing programme of the project. Mechanical analyses were carried out on P91 and (mainly) P92 steel grades, particularly looking at softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods. For this purpose, cylindrical specimens were extracted from thick-walled steam pipes, orthogonal to the pipe axis, and subjected to strain controlled cyclic loading (± 0.2 to ±0.5 % mechanical strain) to different degrees of softening at temperatures up to 620 °C. The test results will be presented and discussed with a focus on the impact of hold periods (i.e. combined creep-fatigue conditions) on mechanical softening, lifetime and crack formation. Details on the microstructural evolution and their representation in a micromechanical model will be given in a second, complementary contribution to this conference. T2 - 45. MPA-Seminar CY - Stuttgart, Germany DA - 01.10.2019 KW - Tempered Martensite Ferritic Steels KW - Low Cycle Fatigue KW - Creep-Fatigue KW - Thermo-Mechanical Fatigue KW - P92 PY - 2019 AN - OPUS4-50050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -