TY - JOUR A1 - Dmitriev, A. I. A1 - Nikonov, A. Y. A1 - Österle, Werner T1 - Molecular dynamics modeling of the sliding performance of an amorphous silica nano-layer - The impact of chosen interatomic potentials N2 - The sliding behavior of an amorphous silica sample between two rigid surfaces is in the focus of the present paper. Molecular Dynamics using a classical Tersoff’s potential and a recently developed ReaxFF potential was applied for simulating sliding within a thin film corresponding to a tribofilm formed from silica nanoparticles. The simulations were performed at different temperatures corresponding to moderate and severe tribological stressing conditions. Simulations with both potentials revealed the need of considering different temperatures in order to obtain a sound interpretation of experimental findings. The results show the striking differences between the two potentials not only in terms of magnitude of the resistance stress (about one order of magnitude) but also in terms of friction mechanisms. The expected smooth sliding regime under high temperature conditions was predicted by both simulations, although with Tersoff’s potential smooth sliding was obtained only at the highest temperature. On the other hand, at room temperature Tersoff-style calculations demonstrate stick-slip behavior, which corresponds qualitatively with our experimental findings. Nevertheless, comparison with a macroscopic coefficient of friction is not possible because simulated resistance stresses do not depend on the applied normal pressure. KW - Molecular dynamics KW - Thin tribofilm KW - Resistance stress KW - Sliding simulation KW - Amorphous silica PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-449366 DO - https://doi.org/10.3390/lubricants6020043 SN - 2075-4442 VL - 6 IS - 2 SP - 43, 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-44936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nofz, Marianne A1 - Dörfel, Ilona A1 - Sojref, Regine A1 - Wollschläger, Nicole A1 - Mosquera Feijoo, Maria A1 - Schulz, Wencke A1 - Kranzmann, Axel T1 - Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C N2 - Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far. KW - Steel KW - Oxide coatings KW - High-temperature corrosion KW - TEM KW - SEM PY - 2018 DO - https://doi.org/10.1007/s11085-017-9799-0 SN - 0030-770X SN - 1573-4889 VL - 89 IS - 3-4 SP - 453 EP - 470 PB - Springer AN - OPUS4-44472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böllinghaus, Thomas A1 - Lüders, V. A1 - Nolze, Gert T1 - Microstructural insights into natural silver wires N2 - Due to the increasing global demand for pure silver, native wire silver aggregates in very high purities are gaining more industrial attention. Up to the present, no substantial metallurgical Investigation of natural wire silver exists in the accessible literature. To convey urgently needed cross-disciplinary fundamental knowledge for geoscientists and metallurgical engineers, twenty natural wire silver specimens from eight different ore deposits have been investigated in detail for the first time by EBSD (Electron Back Scattering Diffraction), supported by light microscopy and micro-probe analyses. The improved understanding of the natural silver wire microstructure provides additional Information regarding the growth of natural silver aggregates in comparison to undesired artificial growth on electronic devices. Clear evidence is provided that natural silver curls and hairs exhibit a polycrystalline face-centered cubic microstructure associated with significant twinning. Although the investigated natural wire silver samples have relatively high purity (Ag > 99.7 wt.-%), they contain a variety of trace elements such as, S, Cu, Mn, Ni, Zn, Co and Bi, As and Sb. Additionally, Vickers micro-hardness measurements are provided for the first time which revealed that natural silver wires and curls are softer than it might be expected from conversion of the general Mohs hardness of 2.7. KW - Natural silver wires PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-451655 UR - http://www.nature.com/articles/s41598-018-27159-w DO - https://doi.org/10.1038/s41598-018-27159-w SN - 2045-2322 VL - 8 IS - 1 SP - Article 9053, 1 EP - 9 PB - nature publishing group CY - London, United Kingdom AN - OPUS4-45165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Chyrkin, A. A1 - Nolze, Gert A1 - Midtlyng, Jan A1 - Mayer, H. M. A1 - Petrushin, N. A1 - Reimers, W. T1 - Interdiffusion in the Face-Centered Cubic Phase of the Co-Al-W-Ta System Between 1090 and 1240 °C N2 - Interdiffusion of Al, W, Ta and Co in a Co-base alloy at temperatures between 1090 and 1240 °C has been investigated. The interdiffusion coefficients were found to be close to those reported for these elements in Ni-base alloys. Combining the diffusion simulation software DICTRA with the Ni-base diffusion databases TCNi5 and MobNi3, the interdiffusion profiles of Co, Al W, and Ta were modeled for Co9Al8W2Ta/Co diffusion couples annealed at different temperatures and for different times. The results show that interdiffusion in the Co-Al-W-Ta alloys can be modeled reasonably well using the available commercial databases for thermodynamics and kinetics of Ni-base systems. KW - Alloys KW - Interdiffusion KW - Modeling PY - 2018 DO - https://doi.org/10.1007/s11669-018-0620-9 VL - 39 IS - 2 SP - 176 EP - 185 PB - Springer AN - OPUS4-44463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Nofz, Marianne A1 - Dörfel, Ilona A1 - Schulz, Wencke A1 - Sojref, Regine A1 - Kranzmann, Axel T1 - Exposition of sol-gel alumina-coated P92 steel to flue gas: Time-resolved microstructure evolution, defect tolerance, and repairing of the coating N2 - Technically relevant P92 steel (9% Cr) was coated with a micron-thick porous alumina layer prepared by sol-gel technique and treated with flue gas (60 CO2-30 H2O-2 O2-1 SO2-7 N2 (mole fraction in %)) at 650 ° to mimic an oxyfuelcombustion process. Local defects in the coating were marked using focused ion beam (FIB) technique and were inspected after exposition to hot flue gas atmosphere at 300, 800, and 1300 h, respectively. Local defects like agglomerated alumina sol particles tend to spall off from the coating uncovering the underlying dense chromia scale. Re-coating was found to restore the protection ability from oxidation when repeatedly treated with hot flue gas. Cracks and voids did not promote the local oxidation due to the formation of crystalline Mn/S/O species within and on top of the coating. The protective character of the steel-coating system is a result of (i) the fast formation of a dense chromia scale at the surface of sol-gel alumina-coated P92 steel bars in combination with (ii) the porous alumina coating acting as diffusion barrier, but also as diffusion partner in addition with (iii) fast Mn outward diffusion capturing the S species from flue gas. KW - Alumina coatings KW - Oxyfuel KW - Steel P92 KW - High temperature corrosion PY - 2018 DO - https://doi.org/10.1002/maco.201709712 SN - 1521-4176 SN - 0947-5117 SN - 0043-2822 VL - 69 IS - 4 SP - 492 EP - 502 PB - Wiley-VCH Verlag GmbH&Co. KGaA CY - Weinheim AN - OPUS4-45300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nützmann, Kathrin A1 - Wollschläger, Nicole A1 - Rockenhäuser, Christian A1 - Kranzmann, Axel A1 - Stephan-Scherb, Christiane T1 - Identification and 3D reconstruction of Cr5S6 precipitates along grain boundaries in Fe13Cr N2 - Metal sulfide grain boundary precipitates of a ferrous model alloy with 13 wt.% chromium formed at 650°C under a gas atmosphere containing 0.5% SO2 and 99.5% Ar were investigated after ageing for 3 h, 6 h, and 12 h. The precipitates formed along grain boundaries were identified as Cr5S6 using energy-dispersive x-ray spectroscopy in transmission electron microscopy and electron backscatter diffraction analysis. Serial focused ion beam slicing was conducted followed by three-dimensional reconstruction to determine the number, size, and penetration depth of the precipitates evolved at the different time steps. There was a linear increase in the number of precipitates with time, while their average size increased only for the initial aging time but became constant after 6 h. Based on these results, a model for grain boundary sulfidation of ferritic alloys is discussed. KW - Internal Sulfidation KW - Grain Boundary Corrosion KW - FIB Tomography PY - 2018 DO - https://doi.org/10.1007/s11837-018-2940-y SN - 1047-4838 SN - 1543-1851 VL - 70 IS - 8 SP - 1478 EP - 1483 PB - Springer Science + Business Media CY - New York, NY AN - OPUS4-45090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel A1 - Knauer, S. T1 - Droplet corrosion of CO2 transport pipeline steels N2 - In this work, the focus was set on the corrosion process of condensate as drops on the surface of carbon steels (X52, X70), martensitic steel UNS S41500, and superaustenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the transportation condition in a buried pipeline). Exposure tests were performed at both normal pressure and high pressure where CO2 is supercritical or in dense phase. The drop, 1 ‑ 10 μL in volume, was prepared by dropping CO2 saturated ultra-pure water onto the surface of steel coupons in a one-liter-autoclave. The CO2 gas stream, simulating the oxyfuel flue gas with varying concentration of impurities (SO2 and O2 ), was then pumped into the autoclave to observe the condensation and corrosion impacts of impurities. Comparable exposure tests were carried out with the same gas mixture and the same volume of water as vapor to observe the drop formation and the corrosion process that follows. The wettability and stability of drops on the surface of steel coupons in CO2 supercritical/dense phase environment was evaluated additionally by contact angle measurement. T2 - NACE International Annual Corrosion Conference CY - Phoenix, AZ, USA DA - 15.04.2018 KW - Geothermal KW - Coating KW - SiO2 KW - Polyaniline KW - Corrosion PY - 2018 SP - 10845, 1 EP - 11 PB - Omnipress CY - Houston AN - OPUS4-44917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, A. A1 - Wolf, M. A1 - Kranzmann, Axel T1 - In-situ testing of corrosion and corrosion fatigue behavior of stainless steels in geothermal 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 - 10th International Conference on Chemical, Biological and Environmental Engineering ICBEE 2018 CY - Berlin, Germany DA - 27.09.2018 KW - Adiabatic calorimeter KW - Thermal energy storage KW - Phase change material KW - Salt eutectics PY - 2018 DO - https://doi.org/10.7763/IPCBEE.2018.V103.5 VL - 103 SP - 13 EP - 20 AN - OPUS4-50364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, A. A1 - Simkin, Roman A1 - Kranzmann, Axel T1 - Construction of an adiabatic calorimeter for investigation of high tempertarue salt - based phase change material N2 - The commercial usage of latent thermal energy storages primarily depends on the development of a suitable phase change material (PCM). For industrial high temperature applications above 400 °C multicomponent chloride eutectics are promising and therefore discussed seriously. The profound thermodynamic investigation of such eutectics requires a much greater amount of specimen material than conventional calorimeter can handle. Therefore, a special adiabatic calorimeter was developed and designed. With a specimen mass of > 100 g the typical thermodynamic measurements with a commercial calorimeter can be extended by cycle stability measurements, which are often decisive for practical application of PCM. Furthermore, by implementing corrosion specimens inside the calorimeter high temperature corrosion experiments according to ISO 21608 can be performed inside the calorimeter. Adiabatic measuring conditions can be provided by using two separate heating systems. Therefore, the outer “protective system” follows the temperature curve of the inner “measuring system” minimizing the temperature difference between the heating systems and simultaneously preventing heat losses from the measuring systems. T2 - 10th International Conference on Chemical, Biological and Environmental Engineering ICBEE 2018 CY - Berlin, Germany DA - 27.09.2018 KW - Adiabatic calorimeter KW - Thermal energy storage KW - Phase change material KW - Salt eutectics PY - 2018 DO - https://doi.org/10.7763/IPCBEE.2018.V103.6 VL - 103 SP - 21 EP - 28 AN - OPUS4-50363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, Damian A1 - Radziszewska, A. A1 - Kranzmann, Axel A1 - Marynowski, P. A1 - Wozny, K. T1 - Morphology and chemical composition of inconel 686 after high-temperature corrosion N2 - The work presents the microstructure, chemical composition and mechanical properties of Inconel 686 coatings after high - temperature corrosion in environment of aggressive gases and ashes. To produce the Ni - based coatings the QS Nd:YAG laser cladding process was carried out. As the substrate used 13CrMo4-5 boilers plate steel. Ni - base alloys characterize the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. Formed clad were characterized by high quality of metallurgical bonding with the substrate material and sufficiently low amount of the iron close to the clad layer surface. After corrosion experiment the oxide scale on the substrate and clad created. The scale on 13CrMo4-5 steel had 70 μm thickness while the scale of the clad had less than 10 μm. The microstructure, chemical composition of the obtained clad and scales were investigated by scanning electron microscope (SEM) and electron probe microanalyzer (EPMA) equipped with the EDS detectors. T2 - 27th International conference on metallurgy and materials CY - Brno, Czech Republic DA - 23.05.2018 KW - laser cladding KW - Inconel 686 KW - High - temperature corrosion KW - Aggressive environment KW - Oxide scale PY - 2018 SP - 1010 EP - 1016 AN - OPUS4-49660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Peetz, Christoph A1 - Buggisch, Enrico A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Electrochemical study on wellbore constellations for CO2 injection N2 - Carbon Capture and Storage (CCS) is identified as an excellent technology to reach the target of CO2 reduction. However, the safety issue and cost effectiveness hinder the future of CCS. For the reliability and safety issues of injection wells the corrosion resistance of the materials used needs to be determined. In this study, representative low cost materials including carbon steel 1.8977 and low alloyed steel 1.7225 were embedded in cement to mimic the realistic casing-cement interface. Electrochemical studies were carried out using these metal-cement specimens in comparison with those made of metal only in CO2 saturated synthetic aquifer fluid, at 333 K, to reveal the effect of cement on the steel performance. The results showed the protective effect of cement on the performance of pipeline metals during polarisation process. However, the corrosion current density was high in all cases, with and without cement, indicating that the corrosion resistance of these materials is low. This conclusion was supported by the surface analysis of the polarized specimens, which revealed both homogenous and pitting corrosions. T2 - EUROCORR 2018 CY - Krakow, Poland DA - 09.09.2018 KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Injection KW - Impurities PY - 2018 SP - 1 EP - 4 PB - EFC CY - Krakau, Poland AN - OPUS4-46291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja A1 - Kranzmann, Axel T1 - Impact of saline aquifer water on surface and shallow pit corrosion of martensitic stainless steels during exposure to CO2 environment (CCS) N2 - Pipe steels suitable for carbon capture and storage technology (CCS) require resistance against the corrosive environment of a potential CCS-site, e.g. heat, pressure, salinity of the aquifer, CO2-partial pressure. Samples of different mild and high alloyed stainless injection-pipe steels partially heat treated: 42CrMo4, X20Cr13, X46Cr13, X35CrMo4 as well as X5CrNiCuNb16-4 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CO2-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. Main corrosion products are FeCO3 and FeOOH. Corrosion rates obtained at 100 bar are generally much lower than those measured at ambient pressure. Highest surface corrosion rates are 0.8 mm/year for 42CrMo4 and lowest 0.01 mm/year for X5CrNiCuNb16-4 in the vapour phase at ambient pressure. At 100 bar the highest corrosion rates are 0.01 mm/year for 42CrMo4, X20Cr13 (liquid phase), X46Cr13 and less than 0.01 mm/year for X35CrMo4 and X5CrNiCuNb16-4 after 8000 h of exposure with no regard to atmosphere. Martensitic microstructure offers good corrosion resistance. T2 - 8th International Conference on Future Environment and Energy (ICFEE 2018) CY - Phuket, Thailand DA - 10.01.2018 KW - CCS KW - CO2 corrosion KW - Pipeline PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-465896 DO - https://doi.org/10.1088/1755-1315/150/1/012012 VL - 150 SP - 81 EP - 90 PB - IOP Publ. AN - OPUS4-46589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbricht, Jürgen A1 - Agudo Jácome, Leonardo A1 - Jürgens, Maria A1 - Roohbakhshan, Farshad A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - Cyclic loading performance and related microstructure evolution of ferritic-martensitic 9-12% Cr steels 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. T2 - 44th MPA-Seminar CY - Leinfelden/Stuttgart, Germany DA - 17.10.2018 KW - Ferritic-martensitic steels KW - Cyclic loading KW - Microstructure evolution PY - 2018 SP - 259 EP - 265 AN - OPUS4-47118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, Damian A1 - Radziszewska, A. A1 - Kranzmann, Axel T1 - The influence of the aggressive environments on the Inconel 686 coating in high-temperature corrosion experiments N2 - This work presents the microstructure and chemical composition of oxide scales created on Ni – base coating after corrosion experiments in aggressive gases and ashes. The Inconel 686 coating applied on the low carbon steel 13CrMo4-5 was performed by a CO2 laser cladding process. The experiments were carried out in oxidizing gas atmospheres containing O2, COx, SOx. The second Variation of corrosion experiments were performed in a reducing atmosphere with ashes containing elements such as: Na, Cl, Ca, Si, C, Fe, Al etc. After 240 h and 1.000 h corrosion experiments the oxide scales on the substrate and overlay were created in both cases. The sulfur compounds were found on the top of the coating surface (EPMA) and also higher contents of silica compounds were revealed on specimens covered by ashes during the experiments. The microstructure and chemical composition of the clad and scales were investigated by means of a light microscope and an electron microscope (SEM)equipped with an EDS detector. T2 - 50. Kraftwerkstechnisches Kolloquium CY - Dresden, Germany DA - 23.10.2018 KW - Nickel based coatings KW - Inconel 686 KW - High temperature corrosion PY - 2018 SP - 599 AN - OPUS4-46590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koclega, Damian A1 - Petrzak, P. A1 - Kowalski, K. A1 - Rozmus-Gornikowska, M. A1 - Debowska, A. A1 - Jedrusik, M. T1 - Annealing effect on microstructure and chemical composition of Inconel 625 alloy N2 - Our research focused on Inconel 625 weld overlays on 16Mo3 steel boiler pipes. The Investigation focused on the characterization of changes in the microstructure and chemical composition after annealing. The annealing was performed for ten hours at temperatures from 600 to 1000°C. Changes in the microstructure were observed with a scanning and transmission electron microscope (SEM and TEM). The investigation was supplemented by hardness measurements. KW - Inconel 625 KW - Microsegregation KW - Annealing PY - 2018 DO - https://doi.org/10.7494/mafe.2018.44.2.73 SN - 1230-2325 SN - 0860-6307 SN - 2300-8377 VL - 44 IS - 2 SP - 73 EP - 80 PB - AGH University of Science and Technology Press CY - Cracow AN - OPUS4-49659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stegemann, Robert A1 - Cabeza, Sandra A1 - Pelkner, Matthias A1 - Lyamkin, Viktor A1 - Pittner, Andreas A1 - Werner, Daniel A1 - Wimpory, R. A1 - Boin, M. A1 - Kreutzbruck, Marc A1 - Bruno, Giovanni T1 - Influence of the microstructure on magnetic stray fields of low-carbon steel welds N2 - This study examines the relationship between the magnetic mesostructure with the microstructure of low carbon steel tungsten inert gas welds. Optical microscopy revealed variation in the microstructure of the parent material, in the heat affected and fusion zones, correlating with distinctive changes in the local magnetic stray fields measured with high spatial resolution giant magneto resistance sensors. In the vicinity of the heat affected zone high residual stresses were found using neutron diffraction. Notably, the gradients of von Mises stress and triaxial magnetic stray field modulus follow the same tendency transverse to the weld. In contrast, micro-X-ray fluorescence characterization indicated that local changes in element composition had no independent effect on magnetic stray fields. KW - TIG-welding KW - GMR sensors KW - Magnetic stray field KW - Neutron diffraction KW - Residual stress KW - Microstructure KW - Low carbon steel PY - 2018 DO - https://doi.org/10.1007/s10921-018-0522-0 SN - 0195-9298 SN - 1573-4862 VL - 37 IS - 3 SP - 66,1 EP - 18 PB - Springer US CY - New York AN - OPUS4-45855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eggeler, G. A1 - Wieczorek, N. A1 - Fox, F. A1 - Berglund, S. A1 - Bürger, D. A1 - Dlouhý, A. A1 - Wollgramm, P. A1 - Neuking, K. A1 - Schreuer, J. A1 - Agudo Jácome, Leonardo A1 - Gao, S. A1 - Hartmaier, A. A1 - Laplanche, G. T1 - On shear testing of single crystal Ni-base superalloys N2 - Shear testing can contribute to a better understanding of the plastic deformation of Ni-base superalloy single crystals. In the present study, shear testing is discussed with special emphasis placed on its strengths and weaknesses. Key mechanical and microstructural results which were obtained for the high-temperature (T ≈ 1000 °C) and low-stress (τ ≈ 200 MPa) creep regime are briefly reviewed. New 3D stereo STEM images of dislocation substructures which form during shear creep deformation in this regime are presented. It is then shown which new aspects need to be considered when performing double shear creep testing at lower temperatures (T < 800 °C) and higher stresses (τ > 600 MPa). In this creep regime, the macroscopic crystallographic [11−2](111) shear system deforms significantly faster than the [01−1](111) system. This represents direct mechanical evidence for a new planar fault nucleation scenario, which was recently suggested (Wu et al. in Acta Mater 144:642–655, 2018). The double shear creep specimen geometry inspired a micro-mechanical in-situ shear test specimen. Moreover, the in-situ SEM shear specimen can be FIB micro-machined from prior dendritic and interdendritic regions. Dendritic regions, which have a lower γ′ volume fraction, show a lower critical resolved shear stress. T2 - EuroSuperalloys 2018 CY - Oxford, UK DA - 09.09.2018 KW - Superalloy single crystals KW - Shear testing KW - Creep mechanisms KW - In-situ SEM micro shear deformation KW - Transmission electron microscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-456591 DO - https://doi.org/10.1007/s11661-018-4726-9 SN - 1073-5623 SN - 1543-1940 VL - 49A IS - 9 SP - 3951 EP - 3962 PB - Springer US CY - New York AN - OPUS4-45659 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. T1 - Mapping of local lattice parameter ratios by projective Kikuchi pattern matching N2 - We describe a lattice-based crystallographic approximation for the analysis of distorted crystal structures via Electron Backscatter Diffraction (EBSD) in the scanning electron microscope. EBSD patterns are closely linked to local lattice parameter ratios via Kikuchi bands that indicate geometrical lattice plane projections. Based on the transformation properties of points and lines in the real projective plane, we can obtain continuous estimations of the local lattice distortion based on projectively transformed Kikuchi diffraction simulations for a reference structure. By quantitative image matching to a projective transformation model of the lattice distortion in the full solid angle of possible scattering directions, we enforce a crystallographically consistent approximation in the fitting procedure of distorted simulations to the experimentally observed diffraction patterns. As an application example, we map the locally varying tetragonality in martensite grains of steel. KW - EBSD KW - Scanning electron microscopy KW - Orientation refinement PY - 2018 DO - https://doi.org/10.1103/PhysRevMaterials.2.123803 SN - 2475-9953 VL - 2 IS - 12 SP - 123803, 1 EP - 15 PB - American Physical Society CY - College Park, MD AN - OPUS4-47296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Kranzmann, Axel T1 - Local Corrosion of Martensitic Stainless Steels during Exposure to Saline Aquifer Water and CO2 Environment N2 - Carbon Capture and Storage (CCS) is well acknowledged to mitigate climate change. Therefore, pipe Steels suitable for CCS technology require resistance against the corrosive environment of a potential CCS-site, e.g. heat, pressure, salinity of the aquifer, CO2-partial pressure. Samples of different mild and high alloyed stainless injection-pipe Steels partially heat treated: 42CrMo4, X20Cr13, X46Cr13, X35CrMo4 as well as X5CrNiCuNb16-4 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CO2-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. Main corrosion products analysed on pits are FeCO3 and FeOOH. The carbon content does not show significant influence on the pitting behaviour. Generally, higher chromium Content results in better corrosion resistance. Although X35CrMo17-1 and X5CrNiCuNb16-4 show low surface corrosion rates, their resistance against local corrosion in CCS environment is not significantly better compared to the much less costly Steels X20Cr13 and X46Cr13. KW - Corrosion KW - CCS KW - Carbon storage KW - Aquifer KW - Heat treatment PY - 2018 DO - https://doi.org/10.18178/ijcea.2018.9.1.694 SN - 2010-0221 VL - 9 SP - 26 EP - 31 PB - International Association of Computer Science and Information Technology Press CY - Singapore AN - OPUS4-46627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mujica Roncery, L. A1 - Agudo Jácome, Leonardo A1 - Aghajani, A. A1 - Theisen, W. A1 - Weber, S. T1 - Subsurface characterization of high-strength high-interstitial austenitic steels after impact wear N2 - The microstructure of the subsurface after impact wear of three high-strength high interstitial austenitic steels has been analysed using transmission electron microscopy (TEM) in alloys with C and N as interstitial elements. In all cases, a nanocrystalline region followed by a transition zone and a cold-worked area are present. Additionally, microhardness and nano-scratching tests were conducted to study the wear-related properties of the impact subsurface and the base material. The results of the microstructural analysis reveal that the following mechanisms are involved during impact wear: abrasion (ploughing), microcrack formation associated with contact fatigue, entrapment and adhesion of SiO2 particles. The analysis of the wear-related properties indicates that the subsurface acts as a self-protective layer that prevents the deterioration of the substrate. KW - Impact wear KW - TEM KW - Nano-scratch test KW - High interstitial austenitic steel PY - 2018 DO - https://doi.org/10.1016/j.wear.2018.02.016 SN - 0043-1648 VL - 402-403 SP - 137 EP - 147 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-44290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Nützmann, Kathrin A1 - Kranzmann, Axel A1 - Klaus, M. A1 - Genzel, C. T1 - Real time observation of high temperature oxidation and sulfidation of Fe-Cr model alloys N2 - Insights into early damage mechanisms during high-temperature gas corrosion provide important aspects for the prediction of the long-term stability of hightemperature materials exposed to a hot and corrosive environment. The current work presents a real time study concerning the combined oxidation and sulfidation of ferritic model alloys in a hot SO2 containing atmosphere using energy dispersive X-ray diffraction. The applied high temperature reactor allows the transmittance of high energetic X-rays in order to collect X-ray diffraction pattern of the sample surface in situ during the reaction with the reactive environment. The results revealed that the first phases crystallizing on iron with 2 wt% chromium and with 9 wt% chromium are oxides. The aging experiments at T = 650° C with 0.5% SO2 and 99.5% Ar were followed in situ and caused an external mixed oxide-sulfide layer on top of iron with 2 wt% chromium. On the higher alloyed material the external scale consists of iron oxides and the inner scale of mixed (Fe,Cr)-oxides and chromium-sulfides. The oxide content continuously increases parallel to an increase of the sulfide amount. Thus, the initially formed (Fe,Cr)-oxides do not have a protective character and support the transport of sulfur through the growing oxide scale. KW - High temperature corrosion KW - In situ diffraction KW - Sulfidation PY - 2018 DO - https://doi.org/10.1002/maco.201709892 SN - 0947-5117 VL - 69 IS - 6 SP - 678 EP - 689 PB - Wiley VCH Verlag AN - OPUS4-44776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agudo Jácome, Leonardo A1 - Pöthkow, K. A1 - Paetsch, O. A1 - Hege, H.-C. T1 - Three-dimensional reconstruction and quantification of dislocation substructures from transmission electron microscopy stereo pairs N2 - A great amount of material properties is strongly influenced by dislocations, the carriers of plastic deformation. It is therefore paramount to have appropriate tools to quantify dislocation substructures with regard to their features, e.g., dislocation density, Burgers vectors or line direction. While the transmission electron microscope (TEM) has been the most widely-used equipment implemented to investigate dislocations, it usually is limited to the two-dimensional (2D) observation of three-dimensional (3D) structures. We reconstruct, visualize and quantify 3D dislocation substructure models from only two TEM images (stereo pairs) and assess the results. The reconstruction is based on the manual interactive tracing of filiform objects on both images of the stereo pair. The reconstruction and quantification method are demonstrated on dark field (DF) scanning (S)TEM micrographs of dislocation substructures imaged under diffraction contrast conditions. For this purpose, thick regions (> 300 nm) of TEM foils are analyzed, which are extracted from a Ni-base superalloy single crystal after high temperature creep deformation. It is shown how the method allows 3D quantification from stereo pairs in a wide range of tilt conditions, achieving line length and orientation uncertainties of 3% and 7°, respectively. Parameters that affect the quality of such reconstructions are discussed. KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) KW - Stereoscopy KW - Visualization PY - 2018 DO - https://doi.org/10.1016/j.ultramic.2018.08.015 SN - 0304-3991 VL - 195 SP - 157 EP - 170 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-46355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Jürgens, Maria A1 - Olbricht, Jürgen A1 - Winkelmann, Aimo T1 - Improving the precision of orientation measurements from technical materials via EBSD pattern matching N2 - We use pattern matching of experimental and dynamically simulated backscattered Kikuchi diffraction (BKD) patterns to increase the orientation precision of electron backscatter diffraction (EBSD) measurements. In order to quantify the improvement in orientation precision, we analyze the experimental distribution of the kernel average misorientation (KAM) angles. We find that for the same raw data, i.e. the same EBSD data acquisition time budget, the pattern matching approach improves the KAM resolution by an order of magnitude compared to orientation data delivered from the conventional Hough-transform based data analysis. This quantitative improvement enables us to interpret small orientation changes in plastically deformed materials which are hidden in noisy orientation data delivered from the reference EBSD system. As an application example, we analyze a ferritic-martensitic steel (P92) sample before and after low-cycle fatigue (LCF) loading (±0.3% strain) at 620 °C. Whereas the low precision of the EBSD orientation data from the manufacturer software does not allow a reliable discrimination of the gradually changing microstructure, we find very clear systematic differences of the local microstructure after the pattern matching orientation refinement of the initial, raw pattern data. For the investigated P92 sample, the KAM-angle histograms are well described by two log-normal distributions indicating the already tempered and the remaining and mostly untempered martensite. KW - Misorientation KW - Thermo-mechanical loading KW - Martensite KW - Log-normal distribution KW - Bimodal distribution PY - 2018 DO - https://doi.org/10.1016/j.actamat.2018.08.028 VL - 159 SP - 408 EP - 415 PB - Elsevier Ltd. AN - OPUS4-46454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Han, M. A1 - Chen, C. A1 - Zhao, G. A1 - Li, L. A1 - Yo, B. A1 - Huang, X. A1 - Zhu, Y. T1 - Blind lattice-parameter determination of cubic and tetragonal phases with high accuracy using a single EBSD pattern N2 - The Bravais lattices and their lattice parameters are blindly determined using electron backscatter diffraction (EBSD) patterns of materials with cubic or tetragonal crystal structures. Since the geometric relationships in a single EBSD pattern are overdetermined, the relative errors of determining the lattice parameters as well as the axial ratios are confined to about 0.7 ± 0.4% and 0.07 ± 0.03%, respectively, for ideal simulated EBSD patterns. The accuracy of the crystal orientation determination reaches about 0.06 ± 0.03°. With careful manual band detection, the accuracy of determining lattice parameters from experimental patterns can be as good as from simulated patterns, although the results from simulated patterns are often better than expermental patterns, which are lower quality and contain uncertain systematic errors. The reasonably high accuracy is obtained primarily because the detection of the diffracting-plane traces and zone axes is relatively accurate. The results here demonstrate that the developed procedure based on the EBSD technique presents a reliable tool for crystallographic characterization of the Bravais lattices of unknown phases. KW - EBSD KW - Bravais lattice KW - Lattice parameters KW - Kikuchi pattern PY - 2018 DO - https://doi.org/10.1107/S2053273318010963 SN - 2053-2733 VL - 74 IS - 6 SP - 630 EP - 639 PB - International Union of Crystallography AN - OPUS4-46455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Laser ablation in liquid KW - Nanoparticles KW - Titanium oxide KW - Particle morphology PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electron-microscopy-and-xray-diffraction-analysis-of-titanium-oxide-nanoparticles-synthesized-by-pulsed-laser-ablation-in-liquid/AE368446FAC70E08C514F9AEABFD131B DO - https://doi.org/10.1017/S1431927618009030 VL - 24 IS - S1 (August) SP - 1710 EP - 1711 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-45949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reith, F. A1 - Rea, M.A.D. A1 - Sawley, P. A1 - Zammit, C.M. A1 - Nolze, Gert A1 - Reith, T. A1 - Rantanen, K. A1 - Bissett, A. T1 - Biogeochemical cycling of gold: Transforming gold particles from arctic Finland N2 - (Bio)geochemical cycling of gold (Au) has been demonstrated in present-day (semi)-arid, (sub)-tropical and temperate environment. Hereby biofilms on Au-bearing mineral- and Au-particle surfaces drive Au dispersion and reconcentration, thereby (trans)forming the particles. However, it is unknown if biogeochemical cycling of Au occurs in polar environments, where air temperatures can reach −40 °C and soils remain frozen for much of the year. Therefore, placer Au-particles, soils and waters were collected at two placer mining districts in arctic Finland, i.e., the Ivalojoki and Lemmenjoki goldfields. Sites were chosen based on contrasting settings ((glacio)-fluvial vs. glacial-till deposits) and depths (surface to 5m below current surface). Gold particles were studied using a combination of tagged 16S rRNA gene next generation sequencing and electron microscopic/microanalytical techniques. Across all sites a range of Au-particle morphologies were observed, including morphotypes indicative of Au dissolution and aggregation. Elevated Au concentrations indicative of Au mobility were detected in placer particle bearing soils at both districts. Typically Au-particles were coated by polymorphic biofilm layers composed of living and dead cells embedded in extracellular polymeric substances. Intermixed were biominerals, clays and iron-sulfides/oxides and abundant secondary Au morphotypes, i.e., nano-particles, microcrystals, sheet-like Au, branched Au networks and overgrowths and secondary rims. Biofilms communities were composed of Acidobacteria (18.3%), Bacteroidetes (15.1%) and Proteobacteria (47.1%), with β-Proteobacteria (19.5%) being the most abundant proteobacterial group. Functionally, biofilms were composed of taxa contributing to biofilm establishment, exopolymer production and nutrient cycling, abundant taxa capable of Au mobilization, detoxification and biomineralization, among them Cupriavidus metallidurans, Acinetobacter spp. and Pseudomonas spp., were detected. In conclusion, these results demonstrate that placer Au-particle transformation and Au dispersion occur in cold, arctic environments. This corroborates the existence of biogeochemical Au cycling in present-day cold environments. KW - Gold KW - Bacteria KW - Biogeochemistry KW - Mobility KW - Finland KW - Cupriavidus metallidurans KW - NGS PY - 2018 DO - https://doi.org/10.1016/j.chemgeo.2018.03.021 SN - 0009-2541 VL - 483 SP - 511 EP - 529 PB - Elsevier AN - OPUS4-44805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, A. A1 - Kranzmann, Axel T1 - Degradation of AISI 630 exposed to CO2-saturated saline aquifer at ambient pressure and 100 bar N2 - In general high alloyed steels are suitable as pipe steels for carbon capture and storage technology (CCS), because they provide sufficient resistance against the corrosive environment of CO2-saturated saline aquifer which serves as potential CCS-site in Germany. High alloyed martensitic steel AISI 630 has been proven to be sufficient resistant in corrosive environments, e.g. regarding heat, pressure, salinity of the aquifer, CO2-partial pressure), but reveals a distinct corrosion pattern in CCS environment. Therefore coupons of AISI 630 heat treated using usual protocols were kept at T=60 °C and ambient pressure as well as p=100 bar up to 8000 h in an a) water saturated supercritical CO2 and b) CO2-saturated synthetic aquifer environment similar to on-shore CCS-sites in the Northern German Basin. AISI 630 precipitates a discontinuous ellipsoidal corrosion layer after being exposed for more than 4000 hours. Best corrosion resistance in the CO2-saturated synthetic aquifer environment phase is achieved via normalizing prior to exposure. In water saturated supercritical CO2 tempering at medium temperatures after hardening gives lowest corrosion rates. Corrosion fatigue via push-pull tests with a series of 30 specimens was evaluated at stress amplitudes between 150 MPa and 500 MPa (sinusoidal dynamic test loads, R=-1; resonant frequency ~ 30 Hz). The endurance limit of AISI 630 is reduced by more than 50% when exposed to CCS environment (maximum number of cycles (10 x 106) at a stress amplitude of 150 MPa). KW - Corrosion Fatigue KW - High Cycle Fatigue KW - Steel KW - Ccs KW - Co2-Storage PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503783 DO - https://doi.org/10.22587/jasr.2018.14.6.3 SN - 1819-544X SN - 1816-157X SP - 11 EP - 17 PB - INSInet Publications CY - Faisalabad AN - OPUS4-50378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Knauer, S A1 - Jaeger, P A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Droplet corrosion of CO2 transport pipeline steels in simulated oxyfuel flue gas N2 - The research focus of this study was set on the corrosion process of condensate as droplets on the surface of carbon steels (X52, X70) martensitic steel UNS S41500, and super austenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the offshore transportation condition in a buried pipeline). The possibility of dew/droplet formation on the steel surface and wetting behavior of corresponding materials were evaluated by contact angle measurement in dense CO2 at 278 K. To observe the effect of impurities (SO2 and O2) on droplet corrosion process, exposure tests were carried out in the mixed atmosphere with a drop, 1 ‑ 10 µL in volume, of CO2 saturated ultra-pure water on steel surface. Comparable exposure tests were carried out with the same gas mixture and the same volume of water, as vapor, to observe the droplet formation and the corrosion process that follows. Effects of surface roughness on the droplet formation and its corrosion process were further studied and showed no significant role upon long time exposure. The results from droplet experiments were compared to those from the bulk electrolyte for the further recommendation on the quality control of gas stream along with the use of carbon steels as transport pipelines in CCS - Carbon Capture and Storage system. KW - CCUS, supercritical/dense phase CO2, carbon steels, martensitic steel, superaustenite steel, droplet corrosion PY - 2018 UR - http://corrosionjournal.com/doi/abs/10.5006/2927 DO - https://doi.org/10.5006/2927 SN - 0010-9312 SN - 1938-159X VL - 74 IS - 12 SP - 1406 EP - 1420 PB - NACE International CY - Houston, Texas, USA AN - OPUS4-46903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hinrichs, R. A1 - Zen Vasconcellos, M.A. A1 - Österle, Werner A1 - Prietzel, C. T1 - Amorphization of graphite flakes in gray cast iron under tribological load N2 - A gray cast iron disc, which had been submitted to a heavy duty automotive brake test, was examined with energy filtered transmission electron microscopy. A graphite flake in a convenient angular position showed the shear interaction of graphite layers with the iron matrix in nano-scale resolution. Atomic layers of graphite were wedged into the ferritic bulk, allowing the entrance of oxygen and the subsequent formation of magnetite. The exfoliated few-layer graphene batches deformed heavily when forced into the matrix. When Raman spectra from the disc surface, which show distinctive carbonaceous bands, were compared with Raman spectra from graphite subjected to deformation in a shaker mill with different milling times, it could be seen that the shear stress on the brake surface was much more effective to induce disorder than the milling, where compressive and impact forces had been additionally exerted on the sample. During shear load the high anisotropy of elastic modulus in the graphite crystalline structure and the low adhesion between graphite basal planes allowed the exfoliation of wrinkled few-layer grapheme batches, causing the formation of more defect related Raman bands than the mechanical stress during high-energy milling. KW - Graphite KW - Shear load KW - Amorphization KW - EFTEM KW - Raman spectroscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-469227 DO - https://doi.org/10.1590/1980-5373-MR-2017-1000 SN - 1516-1439 SN - 1980-5373 VL - 21 IS - 4 SP - e20171000, 1 EP - 6 PB - Universidade Federal de São Carlos CY - São Carlos AN - OPUS4-46922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclęga, Damian A1 - Radziszewska, A. A1 - Kranzmann, Axel A1 - Dymek, S. T1 - Microstructure characterization of the Inconel 686 clad layer after high-temperature corrosion tests in aggressive gases and ashes N2 - The Ni-Cr-Mo-W alloy is characterized by the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. To protect the surface of the substrate 13CrMo4-5 steel against aggressive environments the Inconel 686 as clad layer was used. The corrosion process was performed in oxidizing mixture of gases like O2, COx, SOx. The second part of corrosion Experiment concerned the corrosion test of the coating in reducing atmosphere of the specified gases with ashes, which contained e.g. Na, Cl, Ca, Si, C, Fe, Al. T2 - Junior EUROMAT 2018 CY - Budapest, Hungary DA - 08.07.2018 KW - Laser Cladding KW - Inconel 686 KW - High temperature corrosion KW - Aggressive environement KW - Material oxidation PY - 2018 AN - OPUS4-45627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koclega, Damian A1 - Radziszewska, Agnieszka A1 - Kranzmann, Axel A1 - Dymek, Stanislaw T1 - The microstructure characterization of the oxide scale created on Inconel 686 clad N2 - The Ni-Cr-Mo-W alloy is characterized by the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. To protect the surface of the substrate 13CrMo4-5 steel against aggressive environments the Inconel 686 as clad layer was used. The corrosion process was performed in oxidizing mixture of gases like O2, COx, SOx. The second part of corrosion Experiment concerned the corrosion test of the coating in reducing atmosphere of the specified gases with ashes, which contained e.g. Na, Cl, Ca, Si, C, Fe, Al. T2 - EUROCORR 2018 CY - Crocow, Poland DA - 09.09.2018 KW - Laser cladding KW - Inconel 686 coating KW - High-temperature corrosion KW - Aggressive gases PY - 2018 AN - OPUS4-47393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Donėlienė1, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Nanoparticles KW - Titanium oxide KW - Laser ablation in liquid KW - Electron microscopy KW - XRD PY - 2018 AN - OPUS4-46502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Pöthkow, K. A1 - Paetsch, O. A1 - Hege, H.-C. T1 - 3D reconstruction and quantification of dislocation substructures from TEM stereo pairs N2 - Dislocations are the carriers of plastic deformation. As such, their characterization offers important information on the properties they affect. In this contribution, a new tool is presented, which is incorporated in Amira ZIB Edition and allows for three-dimensional (3D) imaging and quantification of dislocations substructures from thick regions an electron-transparent specimen. In the tool, the dislocation segments are traced on diffraction contrast images that are obtained in the transmission electron microscope (TEM). The uncertainties related to the experimental setup and to the proposed method are discussed on the base of a tilt series. T2 - AVIZO / AMIRA User Meeting CY - Berlin, Germany DA - 14.11.2018 KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) PY - 2018 AN - OPUS4-47394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zerbst, Uwe A1 - Klinger, Christian A1 - Bettge, Dirk T1 - Defects as a root cause for fatigue failure of metallic components N2 - The Topic of the presentationis a discussion on defects which can cause failure in cyclically loaded metallic components. Although also touching Features such as material defects such as pores or micro-shrinkages, etc. and geometric defects such as surface roughness and secondary notches (which are not considered in the design process) which origin in manufacturing, and others the presentation concentrates on non-metallic inclusions. It is prefaced by an introduction to the life cycle of a fatigue crack from initiation up to fracture. Special emphasis is put on the fact that only cracks which are not arrested during one of their distinct Propagation stages can grow to a critical size. T2 - VIII. International Conference on Engineering Failure Analysis CY - Budapest, Ungarn DA - 08.06.2018 KW - Metallic components KW - Material defects KW - Micro-shrinkages PY - 2018 AN - OPUS4-46875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk A1 - Kratzig, Andreas A1 - Peetz, Christoph A1 - Kranzmann, Axel T1 - Interaction of Oxidizing and Reductive Impurities in CO2 Streams with Transport Pipeline Steel N2 - A main goal of CLUSTER CCS project at BAM was to study the corrosion behaviour of pipeline steel with dense phase carbon dioxide containing impurities. Depending on the kind of impurities specific corrosion mechanisms and corrosion rates were determined. T2 - CO2 and H2 Technologies for the Energy Transition CY - BAM, Berlin, Germany DA - 28.11.2018 KW - Carbon capture KW - Carbon dioxide KW - Corrosion KW - CCS PY - 2018 AN - OPUS4-47016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Knauer, S A1 - Bäßler, Ralph A1 - Peetz, Christoph A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel A1 - Jaeger, P A1 - Schulz, S T1 - Impact of acid condensation on wetting and corrosion behavior of CO2 transport-pipeline steel N2 - Es ist allgemein akzeptiert, das Korrosion in CO2-Transport-Pipelines vernach¬lässigbar ist, solange der Wassergehalt des CO2-Stroms deutlich unter der maximal löslichen Menge liegt. Bisher gibt es keinen allgemeinen Konsens darüber, welcher maximale Wassergehalt in zu transportierendem CO2 zugelassen werden sollte. Bei einem Druck von 100 bar und im Temperaturbereich von 277 K bis 298 K beträgt die Löslichkeit von Wasser in CO2 ca. 1.900 bis 3.200 ppmv, aber die Korrosionsrate von Stählen steigt schon ab einem Wassergehalt von 500 ppmv deutlich an. Bei Anwesenheit von Begleitstoffen wie SO2, NO2 und O2, können sich HNO3, H2SO3 und H2SO4 bilden. Menge und Zusammensetzung von kondensierter Säure sind von der Gaszusammensetzung abhängig, und der Korrosionsmechanismus und die Korrosionsform sind vom Kondensationsverhalten abhängig. T2 - CLUSTER Symposium: CO2 and H2 Technologies for the Energy Transition CY - BAM, Berlin, Germany DA - 28.11.2018 KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Droplet corrosion PY - 2018 AN - OPUS4-46907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Peetz, Christoph A1 - Buggisch, Enrico A1 - Bettge, Dirk A1 - Kranzmann, Axel T1 - Electrochemical study on wellbore constellations for CO2 injection N2 - Carbon Capture and Storage (CCS) is identified as an excellent technology to reach the target of CO2 reduction. However, the safety issue and cost effectiveness hinder the future of CCS. For the reliability and safety issues of injection wells the corrosion resistance of the materials used needs to be determined. In this study, representative low cost materials including carbon steel 1.8977 and low alloyed steel 1.7225 were embedded in cement to mimic the realistic casing-cement interface. Electrochemical studies were carried out using these metal-cement specimens in comparison with those made of metal only in CO2 saturated synthetic aquifer fluid, at 333 K, to reveal the effect of cement on the steel performance. The results showed the protective effect of cement on the performance of pipeline metals during polarisation process. However, the corrosion current density was high in all cases, with and without cement, indicating that the corrosion resistance of these materials is low. This conclusion was supported by the surface analysis of the polarized specimens, which revealed both homogenous and pitting corrosions. Furthermore, to reveal the possible protective performance of FeCO3, the pipeline steels were pre-carbonated and then tested in the same condition as freshly polished specimens. T2 - EUROCORR 2018 CY - Krakow, Poland DA - 09.09.2018 KW - CCUS KW - Supercritical/dense phase CO2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Injection KW - Impurities PY - 2018 AN - OPUS4-46279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded A1 - Röhsler, Andreas A1 - Nolze, Gert A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Sputtering derived artefacts in austenitic steel during Time-of-Flight Secondary Ion Mass Spectrometry analyses N2 - Among the very few techniques to localize hydrogen (H) at the microscale in steels, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. The necessity to detect hydrogen stems from its deleterious effects in metals, that are often used as structural components and to obtain better understanding of the underlying metallurgical mechanisms of hydrogen embrittlement (HE) which are still unclear. Austenitic stainless steels are nowadays commonly used in a wide variety of application, from hydrogen transport and storage facilities to petrochemical and offshore applications where they are exposed to aggressive environments and therefore prone to HE. One of the greater risks in the austenitic class is the embrittlement of the material due to the instability of the γ austenite and its transformation into a brittle α martensitic phase. This transformation takes place due to the local stresses that are induced by the uptake of hydrogen during service. Nonetheless, it was shown that this transformation can occur as an artefact during SIMS analysis itself where Cs-sputtering is necessary not only to remove surface contaminations but mainly to enhance H/D secondary ion yield. In the following contribution we show the influence of different sputtering conditions on AISI 304L austenitic stainless steel in order to distinguish the artefact from the hydrogen induced transformation. The material was charged electrochemically in a deuterium based electrolyte. Deuterium (D) must be in these experiments as a replacement for hydrogen which cannot be used because adsorbed hydrogen superimposes hydrogen originating from charging the sample in the SIMS images. ToF-SIMS analyses were conducted by ToF SIMS IV (IONTOF GmbH, Münster, Germany). The experiments were carried out on deuterium charged and non-charged samples. The structural characterization was carried out by SEM and EBSD examinations before and after charging, both with a Leo Gemeni 1530VP field-emission scanning electron microscope and a Zeiss Supra 40 instrument (Carl Zeiss Microscopy GmbH, Oberkochen, Germany). The results showed that the use of 1keV Cs+ beam induces stacking faults while higher sputter beam energies results in γ→α transformation. T2 - SIMS Europe 2018 CY - Münster, Germany DA - 16.09.2018 KW - Austenitic steel KW - Hydrogen KW - ToF-SIMS KW - Artefact PY - 2018 AN - OPUS4-46701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Peetz, Andreas A1 - Kranzmann, Axel T1 - Interaction of Reactive Components in CO2 Streams with Transport Pipeline Steel X70 N2 - In context of CLUSTER project, impacts of impurities (SO2, NO2, O2, CO, H2S, H2, N2, Ar and H2O) in CO2 streams captured from different sources in a regional cluster on transport, injection and storage were investigated. Corrosion studies of oxidizing, reductive or mixed atmospheres towards transport pipeline steel X70 were carried out applying high pressure (10 MPa) at low temperatures (278 K or 313 K). T2 - GHGT-14 Conference CY - Melbourne, Australia DA - 22.10.2018 KW - Carbon capture KW - CCS KW - Carbon dioxide KW - Corrosion PY - 2018 AN - OPUS4-47017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falk, Florian A1 - Menneken, Martina A1 - Stephan-Scherb, Christiane T1 - Early oxidation and sulfidation of high temperature model alloys: An EDXRD in situ study N2 - The fundamental impact of sulfur and water on corrosion rates and potential failure of the exposed material is well known. However, the access to the related corrosion mechanism causing material degradation is often a problem to solve. This study investigates the effect of SO2 and water vapor in the initial stages of corrosion of an Fe9Cr0.5Mn model alloy at 650 °C in situ. The analysis was carried out under laboratory conditions using energy-dispersive X-ray diffraction (EDXRD). T2 - Dechema EFC Workshop CY - Frankfurt am Main, Germany DA - 26.09.2018 KW - Sulfidation KW - Model alloy KW - Oxidation PY - 2018 AN - OPUS4-46134 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Menneken, Martina A1 - Falk, Florian A1 - Stephan-Scherb, Christiane T1 - Early stages of corrosion in hot, aggressive environments N2 - We investigated the effect of water vapor in the initial stages of SO2 corrosion of an Fe-9Cr-0.5Mn model alloy at 650 °C. Two separate experiments were run, one with 99.5%-Ar + 0.5%-SO2 and one with 69.5%-Ar + 0.5%-SO2 with 30%-H2O atmosphere. During the experiment the scale growth was observed in-situ, using energy dispersive X-ray diffraction (EDXRD). Our results confirm an increased speed of oxygen transport into the material, with the addition of water, while the transport of sulfur appears to be less affected. T2 - Sektionstreffen der DMG Sektionen "Angewandte Mineralogie in Umwelt & Technik" und "Chemie, Physik und Kristallographie der Minerale" CY - Bad Windsheim, Germany DA - 28.02.2018 KW - Corrosion KW - In-situ KW - EDXRD PY - 2018 AN - OPUS4-45369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Kratzig, Andreas A1 - Bettge, Dirk A1 - Kranzmann, Axel A1 - Knauer, S. T1 - Droplet corrosion of CO2 transport pipeline steels N2 - In this work, the focus was set on the corrosion process of condensate as drops on the surface of carbon steels (X52, X70), martensitic steel UNS S41500, and superaustenite UNS 08031 in CO2 atmosphere with impurities at 278 K (to simulate the transportation condition in a buried pipeline). Exposure tests were performed at both normal pressure and high pressure where CO2 is supercritical or in dense phase. The drop, 1 ‑ 10 µL in volume, was prepared by dropping CO2 saturated ultra-pure water onto the surface of steel coupons in a one-liter-autoclave. The CO2 gas stream, simulating the oxyfuel flue gas with varying concentration of impurities (SO2 and O2), was then pumped into the autoclave to observe the condensation and corrosion impacts of impurities. Comparable exposure tests were carried out with the same gas mixture and the same volume of water as vapor to observe the drop formation and the corrosion process that follows. The wettability and stability of drops on the surface of steel coupons in CO2 supercritical/dense phase environment was evaluated additionally by contact angle measurement. T2 - NACE International Annual Corrosion Conference CY - Phoenix, AZ, USA DA - 15.04.2018 KW - CCUS KW - Supercritical/dense phase CO 2 KW - Carbon steels KW - Martensitic steel KW - Superaustenite steel KW - Droplet corrosion PY - 2018 AN - OPUS4-44922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Nolze, Gert A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - In-situ observation of the hydrogen behaviour in austenitic stainless steel by time-of-flight secondary ion mass spectrometry during mechanical loading N2 - The reduction of harmful emissions to the environment is one of the most urgent challenges of our time. To achieve this goal, it is inevitable to shift from using fossil fuels to renewable energy sources. Within this transition, hydrogen can play a key role serving as fuel in transportation and as means for energy storage. The storage and transport of hydrogen using austenitic stainless steels as the infrastructure, as well as the use of these grades in hydrogen containing aggressive environments, remains problematic. The degradation of the mechanical properties and the possibility of phase transformation by ingress and accumulation of hydrogen are the main drawbacks. Advanced studies of the behaviour of hydrogen in austenite is necessary to fully understand the occurring damage processes. This knowledge is crucial for the safe use of components in industry and transportation facilities of hydrogen. A powerful tool for depicting the distribution of hydrogen in steels, with high accuracy and resolution, is time-of-flight secondary ion mass spectrometry (ToF-SIMS). We here present a comprehensive research on the hydrogen degradation processes in AISI 304L based on electrochemical charging and subsequent ToF-SIMS experiments. To obtain furthermore information about the structural composition and cracking behaviour, electron-backscattered diffraction (EBSD) and scanning electron microscopy (SEM) were performed afterwards. All the gathered data was treated employing data fusion, thus creating a thorough portrait of hydrogen diffusion and its damaging effects in AISI 304L. Specimens were charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and traces existing in the material or adsorbed from the rest gas in the analysis chamber. Similar diffusion and permeation behaviour, as well as solubility, allow nonetheless to draw onclusions from the experiments. T2 - International Conference on Metals and Hydrogen; Steely Hydrogen 2018 CY - Ghent, Belgium DA - 29.05.2018 KW - Hydrogen KW - Deuterium KW - ToF-SIMS KW - AISI 304L PY - 2018 AN - OPUS4-45079 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Nolze, Gert A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Use of time-of-flight secondary ion mass spectrometry for the investigation of hydrogen-induced effects in austenitic steel AISI 304L N2 - During the energy transformation from fossil fuels to renewable energy sources, the use of hydrogen as fuel and energy storage can play a key role. This presents new challenges to industry and the scientific community alike. The storage and transport of hydrogen, which is nowadays mainly realized by austenitic stainless steels, remains problematic, which is due to the degradation of mechanical properties and the possibility of phase transformation by hydrogen diffusion and accumulation. The development of materials and technologies requires a fundamental understanding of these degradation processes. Therefore, studying the behavior of hydrogen in austenitic steel contributes to an understanding of the damage processes, which is crucial for both life assessment and safe use of components in industry and transportation. As one of the few tools that is capable of depicting the distribution of hydrogen in steels, time-of-flight secondary ion mass spectrometry was conducted after electrochemical charging. To obtain further information about the structural composition and cracking behavior, electron-backscattered diffraction and scanning electron microscopy were performed. Gathered data of chemical composition and topography were treated employing data fusion, thus creating a comprehensive portrait of hydrogen-induced effects in the austenite grade AISI 304L. Specimens were electrochemically charged with deuterium instead of hydrogen. This arises from the difficulties to distinguish between artificially charged hydrogen and traces existing in the material or the rest gas in the analysis chamber. Similar diffusion and permeation behavior, as well as solubility, allow nonetheless to draw conclusions from the experiments. T2 - 21st International Conference on Secondary Ion Mass Spectrometry CY - Kraków, Poland DA - 10.09.2017 KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Austenitic stainless steel PY - 2018 DO - https://doi.org/10.1116/1.5013931 SN - 1071-1023 VL - 36 IS - 3 SP - Article 03F103, 1 EP - 6 PB - American Vacuum Society (AVS) AN - OPUS4-44840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Goedecke, Caroline A1 - Altmann, Korinna A1 - Bannick, C. G. A1 - Kober, E. A1 - Ricking, M. A1 - Schmitt, T. A1 - Braun, Ulrike T1 - Detection of polymers in treated waste water using TED-GC-MS N2 - The presence of large quantities of plastic waste and its fragmentation in various environmental compartments are an important subject of current research. In the environment, (photo ) oxidation processes and mechanical abrasion lead to the formation of microplastics. However, until now, there are no established quality assurance concepts for the analysis of microplastic (<5 mm) in environmental compartments, including sampling, processing and analysis. The aim of the present work is the development of suitable examination methods and protocols (sampling, sample preparation and detection) to qualify and quantify microplastic in urbane water management systems. At first a fractional filtration system for sampling and the analytical tool, the so-called TED-GC-MS (thermal desorption gas chromatography mass spectrometry) were developed. The TED-GC-MS method is a two-step analytical procedure which consists of a thermal extraction where the sample is annealed and characteristic decomposition products of the polymers are collected on a solid phase. Afterwards these products are analysed using GC-MS. The developed fractional filtration for sampling and the TED-GC-MS for detection were used for quantitative analysis to screen the waste water influent and effluent of a Berlin waste water treatment plant for the most relevant polymers, polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA). The results of the study revealed that the polymeres PE, PS and PP were detected in the effluent, and PE and PS were find in the raw waste water of the sewage treatment plant in Ruhleben, Berlin. Differences in polymer types and amounts were detected at different sampling dates and within different sieve fractions. Much higher amounts of polymers were observed in the raw waste water. The peak areas of the decomposition products, used for quantification of the polymers, were adjusted using so-called response factors since the TED-GC-MS method is more sensitive for PP and PS than for PE. It has been shown that PE is the most dominant polymer in the samples. Comparing the masses of polymers in the effluent and in the raw sewage, a removal of 99 % of the polymers in the water treatment plant can be assumed. These results are consistent with the literature where removal rates between 98-99 % were described. T2 - SETAC Europe CY - Rom, Italy DA - 13.05.2018 KW - Microplastics KW - Thermogravimetry KW - Waste water KW - Chromatography PY - 2018 AN - OPUS4-44968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Goedecke, Caroline A1 - Bannick, C.G. A1 - Ricking, M. A1 - Kober, E. A1 - Schmitt, T. A1 - Braun, Ulrike T1 - Detektion von Polymeren im Abwasser eines Klärwerks mittels TED-GC_MS N2 - In den Umweltmedien Wasser, Boden und Luft wird Mikroplastik (MP) gefunden. Mögliche Eintragspfade, besonders Einträge über den Klarlauf kommunaler Klärwerke, sind unklar. Dazu wurde das Klärwerk Ruhleben in Berlin an jeweils vier Tagen im Sommer- und Winterbetrieb beprobt. Es wurde jeweils 1 m3 Klarlauf fraktioniert filtriert (500, 100 und 50 µm Siebe). Weiterhin wurde Rohabwasser exemplarisch untersucht. Als Analyse-methoden wurden die TED-GC-MS und die FTIR Mikroskopie verwendet. Bei der TED-GC-MS wird die Probe zunächst thermisch extrahiert, bevor die charakteristischen Zersetzungsgase mittels einer GC-Säule getrennt und im MS detektiert werden [1,2]. Es ist hier erstmals gelungen, nicht nur das MP zu identi-fizieren, sondern auch eine Massenbilanz zu erstellen und so eine quantitative Auswertung vorzunehmen. Es wurde PE, PS ganzjährig und PP im Sommer gefunden. Das Klärwerk Ruhleben hat einen Rückhalt an MP von 99%. T2 - Wasser 2018 CY - Papenburg, Germany DA - 07.05.2018 KW - Mikroplastik KW - Abwasser KW - TED-GC-MS KW - Bilanzierung PY - 2018 AN - OPUS4-44889 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mair, Georg A1 - Becker, B. A1 - Gesell, Stephan A1 - Wang, Bin T1 - Monte-Carlo-analysis of minimum load cycle requirements for composite cylinders for hydrogen N2 - Hydrogen is an attractive energy carrier that requires high effort for safe storage. For ensuring safety, storage cylinders must undergo a challenging approval process. Relevant standards and regulations for composite cylinders used for the transport of hydrogen and for its onboard storage are currently based on deterministic (e.g. ISO 11119-3) or to some respect semi-probabilistic criteria (UN GTR No. 13; with respect to burst strength). This paper provides a systematic analysis of the load cycle properties resulting from these regulations and standards. Their characteristics are compared with the probabilistic approach of the Federal Institute for Materials Research and Testing BAM. The most important aspect of comparing different concepts is the rate for accepting designs with potentially unsafe or critical safety properties. This acceptance rate is analysed by operating Monte-Carlo simulations over the available range of production properties. T2 - ICHS 2017 CY - Hamburg, Germany DA - 11.09.2017 KW - Safety assessment KW - Failure rate KW - Ageing KW - Degradation KW - End of life KW - Production scatter PY - 2018 DO - https://doi.org/10.1016/j.ijhydene.2018.09.185 SN - 0360-3199 VL - 44 IS - 17 SP - 8833 EP - 8841 PB - Elsevier Ltd AN - OPUS4-46341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas A1 - Braun, Ulrike A1 - Becker, Roland A1 - Maiwald, Michael A1 - Paul, Andrea T1 - Mikroplastikanalyse: Nahinfrarotspektroskopie und chemometrische Auswertung N2 - Für die Erfassung der Verbreitung von Mikroplastik (MP) in der Umwelt ist die zeit- und kostenaufwendige Analysestrategie und der damit verbundene geringe Probendurchsatz eine limitierende Größe. Eine große Zahl verschiedener Studien dokumentriet das Auftreten von MP über den gesamten Globus. Meist sind die Studien aufgrund des großen analytischen Aufwands auf exemplarische, stichpunktartige Untersuchungen kleiner Umweltaliquoten und zahlenmäßig kleiner Probenumfänge begrenzt. Um die Verbreitung, die Eintragspfade und den Verbleib von MP in der Umwelt besser zu verstehen und effektive Vermeidungsstrategien abzuleiten, ist es jedoch notwendig, analytisch mehr Proben erfassen zu können. Bildgebende mikro-spektroskopische Methoden wie das Raman- und FTIR-Imaging ermöglichen eine zeitaufwendige, umfassende Charakterisierung kleiner Umweltaliquoten. Neben der Partikelanzahl sind zusätzlich Informationen zu Partikelgröße, Größenverteilung und Oberflächenmorphologie zugänglich. Chemische und thermische Extraktionsverfahren sind bereits deutlich schneller und können diese Informationen durch eine Massenbilanz vervollständigen. Die analysierbare Probenmenge ist jedoch auf Milligramm Mengen beschränkt. Wir schlagen daher vor, die Analyse von Proben auf MP durch ein vorangestelltes Screening mit der Nahinfrarot-Spektroskopie (NIRS) zur komplementieren. In diesem wird bereits eine erste Einschätzung über die Präsenz von MP in einer Probe gefällt und dadurch die wertvolle Messzeit anderer Methoden effizienter genutzt. NIR zur Analyse von Polymeren wird seit langem eingesetzt, jedoch bisher lediglich im Rahmen einer Studie zur Mikroplastikuntersuchung mittels Hyperspektraler Bildgebung beschrieben. Der NIR Spektralbereich findet sich zwischen dem sichtbaren Licht und dem mittleren Infrarot (MIR). MIR Spektren sind durch klar definierte Banden charakterisiert, welche mehrheitlich von den Grundschwingungen der Moleküle stammen. Die höheren Energien im nahen Infrarot regen hingegen Kombinations- und Oberschwingungen der Streck und Biegeschwingungen an. Die resultierenden Absorptionsbanden sind oft breit und relativ unspezifisch. Erst mit Hilfe einer computergestützten Datenauswertung lassen sich aus diesen Spektren nützliche Informationen gewinnen. Dies erklärt die steigende Popularität der NIR-Spektroskopie in der jüngeren Vergangenheit mit einem Schwerpunkt als prozessanalytische Methode. NIR Spektrometer für das industrielle Prozessmonitoring zeichnen sich durch eine kompakte und robuste Konstruktionsweise aus. Die verfügbaren faseroptischen Reflexionssonden eignen sich gut um pulverförmige Proben zu untersuchen. Der räumlich erfassbare Messbereich kann durch die Sondengeometrie variiert werden. Sind die untersuchten Partikel im Verhältnis zur abgetasteten Fläche klein, wird als spektrale Information die Summe der Absorption aller Partikel im Sichtfeld erfasst. Die Methode ist deshalb nicht für Detailuntersuchungen von MP geeignet, erlaubt es jedoch innerhalb weniger Minuten eine Einschätzung über das Vorkommen von Mikroplastik in einer Probe zu treffen. Exemplarisch wurden für diese Untersuchungen vier der am weitesten verbreiteten Kunststoffe Polyethylen (PE), Polyethylenterephthalat (PET), Polypropylen (PP) und Polystyrol (PS) gewählt. Aus den additivfreien Polymeren wurden nach einer Kryo-vermahlung und anschließender Siebung (< 125 µm) Modellproben generiert. Die Polymere wurden dafür zu einem Massenanteil von 1 % mit einem Standardboden (LUFA2.3, gesiebt < 125 µm) vermischt. Die Gesamtmenge von 1 g je Probe wurde in Aluminiumbehältern präpariert und 8 Messungen an unterschiedlichen, zufällig gewählten Positionen vorgenommen. Die erhaltenen Spektren wurden zur Kalibrierung chemometrischer Modelle genutzt. In einem hierarchischen Ansatz wurde anhand der NIR-Spektren eine Klassifizierung vorgenommen: 1. Bestimmung ob eine Probe MP enthält (Ja/Nein). 2. Identifikation der Polymere in der Probe. Eine aussagekräftige Klassifizierung beruht auf einer Vorbehandlung der Spektren. Hierdurch werden die Unterschiede zwischen den einzelnen Polymerbanden hervorgehoben. Die Eignung der so erstellten Modelle wurde anhand eines Referenzmaterials und am Beispiel von Realproben erfolgreich getestet. Dabei zeigte sich, dass nicht nur in den erstellten Polymer-Bodenmischungen, sondern auch in den Rückständen von fermentiertem Bioabfall und in Filterrückständen einer Waschmaschine, MP richtig erkannt wurde. Weiterhin zeigten Tests mit Mikroplastik-freien Bodenproben unterschiedlicher Herkunft, dass keine falsch-positive Resultate erzeugt wurden. Alle vier untersuchten Polymere, d.h. PE, PET, PS und PP mit einem Massenanteil von 1 % in einer Bodenmatrix werden auch bei einer gemischten Polymerzusammensetzung mit der NIR-Spektroskopie erkannt. Der kombinierte Einsatz von NIRS und Chemometrie ermöglicht die Entscheidung über ein potenzielles Vorkommen sowie die Zuordnung des Materials der enthaltenen Polymerpartikel für eine Massefraktion ≥ 1 % in einer (trockenen) Probenmenge von 1 g innerhalb von 10–15 min. Der zeitaufwendige Schritt der Methode liegt hier in der Erstellung geeigneter chemometrischer Modelle sowie deren Validierung. Wesentliche Voraussetzung ist dabei, dass bei der Kalibrierung die Varianz der zu erwartenden Partikel und der Matrix realistisch abgebildet wird. T2 - GDCh Jahrestagung der Wasserchemischen Gesellschaft CY - Papenburg, Ems, Germany DA - 07.05.2018 KW - Mikroplastik KW - Nahinfrarotspektroskopie KW - Chemometrie KW - Boden PY - 2018 AN - OPUS4-44887 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Wander, Lukas A1 - Becker, Roland A1 - Goedecke, Caroline A1 - Braun, Ulrike T1 - High-throughput NIR spectroscopic (NIRS) detection of microplastics in soil N2 - The increasing pollution of terrestrial and aquatic ecosystems with plastic debris leads to the accumulation of microscopic plastic particles of still unknown amount. To monitor the degree of contamination analytical methods are urgently needed, which help to quantify microplastics (MP). Currently, time-costly purified materials enriched on filters are investigated both by micro-infrared spectroscopy and/or micro-Raman. Although yielding precise results, these techniques are time consuming, and are restricted to the analysis of a small part of the sample in the order of few micrograms. To overcome these problems, here we tested a macroscopic dimensioned NIR process-spectroscopic method in combination with chemometrics. For calibration, artificial MP/soil mixtures containing defined ratios of polyethylene, polyethylene terephthalate, polypropylene, and polystyrene with diameters < 125 µm were prepared and measured by a process FT-NIR spectrometer equipped with a fiber optic reflection probe. The resulting spectra were processed by chemometric models including support vector machine regression (SVR), and partial least squares discriminant analysis (PLS-DA). Validation of models by MP mixtures, MP-free soils and real-world samples, e.g. and fermenter residue, suggest a reliable detection and a possible classification of MP at levels above 0.5 to 1.0 mass% depending on the polymer. The benefit of the combined NIRS chemometric approach lies in the rapid assessment whether soil contains MP, without any chemical pre-treatment. The method can be used with larger sample volumes and even allows for an online prediction and thus meets the demand of a high-throughput method. KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA KW - Support vector machines KW - Near Infrared Spectroscopy PY - 2018 DO - https://doi.org/10.1007/s11356-018-2180-2 SN - 1614-7499 SN - 0944-1344 VL - 26 IS - 8 SP - 7364 EP - 7374 PB - Springer AN - OPUS4-45405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Usmani, Shirin A1 - Stephan, Ina A1 - Huebert, Thomas A1 - Kemnitz, E. T1 - Nano metal fluorides for wood protection against fungi N2 - Wood treated with nano metal fluorides is found to resist fungal decay. Sol−gel synthesis was used to synthesize MgF2 and CaF2 nanoparticles. Electron microscopy images confirmed the localization of MgF2 and CaF2 nanoparticles in wood. Efficacy of nano metal fluoride-treated wood was tested against brown-rot fungi Coniophora puteana and Rhodonia placenta. Untreated wood specimens had higher mass losses (∼30%) compared to treated specimens, which had average mass loss of 2% against C. puteana and 14% against R. placenta, respectively. Nano metal fluorides provide a viable alternative to current wood preservatives. KW - Brown-rot fungi KW - Coniophora puteana KW - Fluoride nanoparticles KW - Fluorolytic sol−gel KW - Rhodonia placenta KW - SEM wood characterization KW - Wood protection PY - 2018 DO - https://doi.org/10.1021/acsanm.8b00144 SN - 2574-0970 VL - 2018 SP - 1 EP - 6 PB - American Chemical Society (ACS) CY - Washington DC, US AN - OPUS4-44730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schmidt, Wolfram A1 - Ramirez Caro, Alejandra A1 - Sojref, Regine A1 - Mota Gassó, Berta ED - Greim, M. ED - Kusterle, W. ED - Teubert, O. T1 - Contribution of the coarse aggregates to rheology - effects of flow coefficient, particle size distribution, and volume fraction N2 - In order to observe the effect of the aggregate phases between 2 mm and 16 mm without overlap with rheological effects induced by the cement hy-dration and without interactions with a threshold fine sand particle size that affects both, paste and aggregates, rheological experiments were conducted on a limestone filler based paste mixed with aggregates up to 16 mm. Vari-ous aggregate fractions were blended and mixed with the replacement paste in different volumetric ratios. The dry aggregates’ flow coefficients were determined and compared to yield stress and plastic viscosity values at different aggregate volume fractions. The results indicated that the flow coefficient is not a suitable parameter to predict the performance of the aggregates in the paste. It was shown that the yield stress of pastes is largely determined by the blend of different aggregate fractions, while the plastic viscosity to large extend depends upon the coars-est aggregate fraction. Based on the results, ideal aggregate composition ranges for minimised yield stress are presented. For the plastic viscosity no such grading curves to achieve minimum values could be found, but high viscosity curves are identified. KW - Rheology KW - Flow Coefficient KW - Particle Size Distribution KW - Volume Fraction KW - Cement KW - Concrete KW - Reference Material KW - Limestone Filler PY - 2018 SN - 978-3-7469-1878-5 SP - 96 EP - 108 PB - tredition GmbH CY - Hamburg AN - OPUS4-44434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich A1 - Braun, Ulrike A1 - Schartel, Bernhard A1 - Weidner, Steffen A1 - Rurack, Knut A1 - Thünemann, Andreas A1 - Sturm, Heinz T1 - Polymerwissenschaften@BAM - Sicherheit macht Märkte N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine Ressortforschungseinrichtung, die zum Schutz von Mensch, Umwelt und Sachgüter, forscht, prüft und berät. Im Fokus aller Tätigkeiten in der Materialwissenschaft, der Werkstofftechnik und der Chemie steht dabei die technische Sicherheit von Produkten und Prozessen. Dazu werden Substanzen, Werkstoffe, Bauteile, Komponenten und Anlagen sowie natürliche und technische Systeme erforscht und auf sicheren Umgang oder Betrieb geprüft und bewertet. Schwerpunkt des Vortrages sind multimodale Polymeranalytik, nanoskalige Sensormaterialien und die Charakterisierung von technischen Eigenschaften von Polymeren sowie ihre Alterung und Umweltrelevanz. T2 - Institutsvortrag CY - Fraunhofer IAP, Potsdam, Germany DA - 18.05.2018 KW - Polymerwissenschaften PY - 2018 AN - OPUS4-45243 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kirner, Sabrina V. A1 - Slachciak, Nadine A1 - Elert, Anna Maria A1 - Griepentrog, Michael A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Sahre, Mario A1 - Dörfel, Ilona A1 - Sturm, Heinz A1 - Pentzien, Simone A1 - Koter, Robert A1 - Spaltmann, Dirk A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Tribological performance of titanium samples oxidized by fs-laser radiation, thermal heating, or electrochemical anodization N2 - Commercial grade-1 titanium samples (Ti, 99.6%) were treated using three alternative methods, (i) femtosecond laser processing, (ii) thermal heat treatment, and (iii) electrochemical anodization, respectively, resulting in the formation of differently conditioned superficial titanium oxide layers. The laser processing (i) was carried out by a Ti:sapphire laser (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz) in a regime of generating laser-induced periodic surface structures (LIPSS). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning setup for the processing of several square-millimeters large surface areas covered homogeneously by these nanostructures. The differently oxidized titanium surfaces were characterized by optical microscopy, micro Raman spectroscopy, variable angle spectroscopic ellipsometry, and instrumented indentation testing. The tribological performance was characterized in the regime of mixed friction by reciprocating sliding tests against a sphere of hardened steel in fully formulated engine oil as lubricant. The specific tribological performance of the differently treated surfaces is discussed with respect to possible physical and chemical mechanisms. KW - Femtosecond laser KW - Titanium KW - Oxidation KW - Friction PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-445609 DO - https://doi.org/10.1007/s00339-018-1745-8 SN - 0947-8396 SN - 1432-0630 VL - 124 IS - 4 SP - 326, 1 EP - 10 PB - Springer-Verlag AN - OPUS4-44560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Selleng, Christian A1 - Stöcker, T. A1 - Moos, R. A1 - Rabe, Torsten T1 - Influence of the calcination procedure on the thermoelectric properties of calcium cobaltite Ca3Co4O9 N2 - Calcium cobaltite is one of the most promising oxide p-type thermoelectric materials. The solid-state reaction (or calcination, respectively), which is well known for large-scale powder synthesis of functional materials, can also be used for the synthesis of thermoelectric oxides. There are various calcination routines in literature for Ca3Co4O9 powder synthesis, but no systematic study has been done on the influence of calcination procedure on thermoelectric properties. Therefore, the influence of calcination conditions on the Seebeck coefficient and the electrical conductivity was studied by modifying calcination temperature, dwell time, particle size of raw materials and number of calcination cycles. This study shows that elevated temperatures, longer dwell times, or repeated calcinations during powder synthesis do not improve but deteriorate the thermoelectric properties of calcium cobaltite. Diffusion during calcination leads to idiomorphic grain growth, which lowers the driving force for sintering of the calcined powder. A lower driving force for sintering reduces the densification. The electrical conductivity increases linearly with densification. The calcination procedure barely influences the Seebeck coefficient. The calcination procedure has no influence on the phase formation of the sintered specimens. KW - Thermoelectrics KW - Calcination KW - Calcium Cobaltite KW - Solid-State-Synthesis KW - Reaction-sintering PY - 2018 DO - https://doi.org/10.1007/s10832-018-0124-3 SN - 1385-3449 SN - 1573-8663 VL - 40 IS - 3 SP - 225 EP - 234 PB - Springer AN - OPUS4-44336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, Ralf A1 - Rabe, Torsten T1 - Niedrigsinterndes CaMnO3 für thermoelektrische Anwendungen N2 - Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (p-type) and calcium manganate (n-type) are two of the most promising oxide thermoelectric materials. The development of cost-effective multilayer thermoelectric generators requires the co-firing of these materials and therefore the adjustment of sintering temperatures. Calcium manganate is conventionally sintered between 1200 °C and 1350 °C. Calcium cobaltite exhibits an undesired phase transition at 926 °C but can be sintered to high relative density of 95 % at 900 °C under axial pressure of 7.5 MPa. Hence, co-firing at 900 °C would be favourable. Therefore, strategies for lowering the sintering temperature of calcium manganate have been investigated. Basically, two approaches are common: i) addition of low melting additives like Bi2O3-ZnO-B2O3-SiO2 (BBSZ) glass or Bi2O3, and ii) addition of additives that form low-melting eutectics with the base material, for example CuO. In this study, several low melting additives including BBSZ glass and Bi2O3, as well as CuO were tested regarding their effect on calcium manganate densification. Bi2O3 did not improve the densification, whereas BBSZ glass led to 10 % higher relative density at 1200 °C. An addition of 4 wt% CuO decreases the temperature of maximum sinter rate from above 1200 °C to 1040 °C. By reducing the particle size of the raw materials from 2 μm to 0.7 μm the maximum sinter rate could be further shifted 20 K towards lower temperatures and the sinter begin decreased from 920 °C to 740 °C. It is shown that eutectic phase formation is more effective in lowering sintering temperature and accelerating densification than low-melting additives. N2 - Thermoelektrische Materialien können durch die Nutzung des Seebeckeffektes einen Temperaturunterschied direkt in eine Spannung umwandeln. Calciumcobaltit (p-typ) und Calciummanagant (n-typ) sind 2 der vielversprechendsten oxidischen thermoelektrischen Materialien. Für die Entwicklung von kostengünstigen Multilayergeneratoren ist das Co-sintern dieser beiden Materialien notwendig und deshalb eine Anpassung der Sintertemperatur nötig. Calciummangant wird herkömmlicherweise zwischen 1200°C und 1350°C gesintert. Calciumcobaltit erfährt einen ungewünschte Phasenumwandlung bei 926°C, es kann allerding bei 900°C unter 7.5MPa zu 95% dicht gesintert werden. Demzufolge, ist eine Co-sintertemperatur von 900°C anzustreben. Aus diesem Grund wurden mehrere Strategien zur Absenkung der Sintertemperatur von Calciummanaganat untersucht. Zum einen die Zugabe niedrigschmelzender Additive, zum anderen die Zugabe von Additiven, die eine eutektische Schmelze bilden. Es konnte gezeigt werden, dass für Calciummanganat die Verwendung von eutektischen Schmelzen besser geeignet ist als die Verwendung von niedrigschmelzenden Additiven um die Sintertemperatur zu senken.“ T2 - Seminar des Lehrstuhls für Funktionsmaterialien CY - Universität Bayreuth, Bayreuth, Germany DA - 22.06.2018 KW - Thermoelectrics KW - Sinter additive PY - 2018 AN - OPUS4-45281 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, R. A1 - Rabe, Torsten T1 - Lowering the sintering temperature of calcium manganate CaMnO3 for thermoelectric applications N2 - Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (p-type) and calcium manganate (n-type) are two of the most promising oxide thermoelectric materials. The development of cost-effective multilayer thermoelectric generators requires the co-firing of these materials and therefore the adjustment of sintering temperatures. Calcium manganate is conventionally sintered between 1200 °C and 1350 °C. Calcium cobaltite exhibits an undesired phase transition at 926 °C but can be sintered to high relative density of 95 % at 900 °C under axial pressure of 7.5 MPa. Hence, co-firing at 900 °C would be favourable. Therefore, strategies for lowering the sintering temperature of calcium manganate have been investigated. Basically, two approaches are common: i) addition of low melting additives like Bi2O3-ZnO-B2O3-SiO2 (BBSZ) glass or Bi2O3, and ii) addition of additives that form low-melting eutectics with the base material, for example CuO. In this study, several low melting additives including BBSZ glass and Bi2O3, as well as CuO were tested regarding their effect on calcium manganate densification. Bi2O3 did not improve the densification, whereas BBSZ glass led to 10 % higher relative density at 1200 °C. An addition of 4 wt% CuO decreases the temperature of maximum sinter rate from above 1200 °C to 1040 °C. By reducing the particle size of the raw materials from 2 μm to 0.7 μm the maximum sinter rate could be further shifted 20 K towards lower temperatures and the sinter begin decreased from 920 °C to 740 °C. It is shown that eutectic phase formation is more effective in lowering sintering temperature and accelerating densification than low-melting additives. T2 - 93. DKG-Jahrestagung und Symposium Hochleistungskeramik 2018 CY - Munich, Germany DA - 10.04.2018 KW - Thermoelectrics KW - Sinter additive PY - 2018 AN - OPUS4-44818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, Ralf A1 - Rabe, Torsten T1 - Pressure-assisted sintering of tape cast calcium cobaltite for thermoelectric applications N2 - Thermoelectric materials can convert waste heat directly into electrical power by using the Seebeck effect. Calcium cobaltite Ca3Co4O9 is a promising p-type oxide thermoelectric material for applications between 600 °C and 900 °C in air. The properties and morphology of Ca3Co4O9 are strongly anisotropic because of its crystal structure of alternating layers of CoO2 and Ca2CoO3. By aligning the plate-like grains, the anisotropic properties can be assigned to the component. Pressure-assisted sintering (PAS), as known from large-scale production of low temperature co-fired ceramics, was used to sinter multilayers of Ca3Co4O9 green tape at 900 °C with different pressures and dwell times. In-situ shrinkage measurements, microstructural investigations and electric measurements were performed. Pressure-less sintered multilayers have a 2.5 times higher electrical conductivity at room temperature than dry pressed test bars with randomly oriented particles. The combination of tape casting and PAS induces a pronounced alignment of the anisotropic grains. Relative density increases from 57 % after free sintering for 24 h to 94 % after 2 h of PAS with 10 MPa axial load. By applying a uniaxial pressure of 10 MPa during sintering, the electrical conductivity (at 25°C) improves by a factor of 15 compared to test bars with randomly oriented particles. The high temperature thermoelectric properties show the same dependencies. The smaller the applied axial load, the lower the relative densities, and the lower the electrical conductivity. Longer dwell times may increase the density and the electrical conductivity significantly if the microstructure is less densified as in the case of a small axial load like 2 MPa. At higher applied pressures the dwell time has no significant influence on the thermoelectric properties. This study shows that PAS is a proper technique to produce dense Ca3Co4O9 panels with good thermoelectric properties similar to hot-pressed tablets, even in large-scale production. T2 - Electroceramics XVI CY - Hasselt, Belgium DA - 09.07.2018 KW - Texturation KW - Hot Press KW - Calcination KW - Multilayer PY - 2018 AN - OPUS4-45491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Delorme, F. A1 - Chen, C. A1 - Bektas, M. A1 - Moos, R. A1 - Rabe, Torsten T1 - Influence of Reaction-Sintering and Calcination Conditions on Thermoelectric Properties of Sm-doped Calcium Manganate CaMnO3 N2 - A wide range of solid-state synthesis routes for calcium manganate is reported in the literature, but there is no systematic study about the influence of the solid-state synthesis conditions on thermoelectric properties. Therefore, this study examined the influence of calcination temperature and calcination cycles on the Seebeck coefficient, electrical conductivity, and thermal conductivity. Higher calcination temperatures and repeated calcination cycles minimized the driving force for sintering of the synthesized powder, leading to smaller shrinkage and lower densities of the sintered specimens. As the electrical conductivity increased monotonously with increasing density, a higher energy input during calcination caused deterioration of electrical conductivity. Phase composition and Seebeck coefficient of sintered calcium manganate were not influenced by the calcination procedure. The highest thermoelectric properties with the highest power factors and figures of merit were obtained by means of reaction-sintering of uncalcined powder. KW - Thermoelectric oxides KW - Calcination KW - Solid-state-synthesis KW - Power factor KW - Reaction-sintering PY - 2018 DO - https://doi.org/10.4416/JCST2018-00017 SN - 2190-9385 VL - 9 IS - 3 SP - 289 EP - 300 PB - Göller Verlag AN - OPUS4-46224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik A1 - Ziegler, Mathias A1 - Ahmadi, Samim A1 - Portella, Pedro Dolabella T1 - Structured heating in active thermography by using laser arrays N2 - Lock-in- and flash thermography are standard methods in active thermography. They are widely used in industrial inspection tasks e.g. for the detection of delaminations, cracks or pores. The requirements for the light sources of these two methods are substantially different. While lock-in thermography requires sources that can be easily and above all fast modulated, the use of flash thermography requires sources that release a very high optical energy in the very short time. By introducing high-power vertical cavity surface emitting lasers (VCSELs) arrays to the field of thermography a source is now available that covers these two areas. VCSEL arrays combine the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination range of flash lamps or LEDs and can thus potentially replace all conventional light sources of thermography. However, the main advantage of this laser technology lies in the independent control of individual array areas. It is therefore possible to heat not only in terms of time, but also in terms of space. This new degree of freedom allows the development of new NDT methods. We demonstrate this approach using a test problem that can only be solved to a limited extent in active thermography, namely the detection of very thin, hidden defects in metallic materials that are aligned vertically to the surface. For this purpose, we generate destructively interfering thermal wave fields, which make it possible to detect defects within the range of the thermal wave field high sensitivity. This is done without pre-treatment of the surface and without using a reference area to depths beyond the usual thermographic rule of thumb. T2 - ConaEnd&Iev 2018 CY - Sao Paulo, Brazil DA - 27.08.2018 KW - VCSEL KW - Active thermography KW - Laser KW - Structured heating KW - Subsurface defects PY - 2018 AN - OPUS4-45851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Slurry development for spray granulation of ceramic multicomponent batches N2 - The granules commonly yielded by spray drying procedures exhibit a hard shell and an irregular, dimpled shape, which is often described as donut-like morphology. Sintered parts produced from such granules suffer from microstructural defects and reduced mechanical properties resulting from these disadvantageous granule properties. Using the example of alumina, zirconia and zirconia-toughened alumina (ZTA) batches, this paper shows that the morphology of the granules can be tuned by adjusting slurry stability. High zeta potential is essential to optimally disperse the particles. But to achieve spherical and soft granules the electrostatic repulsion forces between the particles should be reduced before spray granulation. Electrostatic repulsion forces were changed with the addition of nitric acid. Measurements of zeta potential and viscosity, as well as sedimentation investigations with an optical centrifuge were used for precise slurry assessment as a major precondition for optimal and reproducible adjustment of slurries before spray drying. Sedimentation analysis using an optical centrifuge was performed to investigate different influences like that of additive composition, solids content or pH-value on the sedimentation behavior. Adequately flocculated slurries lead to homogeneous, soft granules that can be easily deformed and pressed. The fraction of donut-shaped particles and the rigidity of granules were reduced. Consequently, the sintered parts produced from these granulates show improvements regarding porosity, pore size distribution, sintered density and biaxial strength. KW - Slurry optimization KW - Optical centrifugation KW - Destabilization KW - Spray drying KW - Biaxial strength PY - 2018 DO - https://doi.org/10.4416/JCST2018-00022 SN - 2190-9385 VL - 9 IS - 3 SP - 327 EP - 336 PB - Göller Verlag AN - OPUS4-46225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Mieller, Björn ED - Kollenberg, W. T1 - Sintern N2 - Unter Sintern versteht man allgemein die Überführung eines aus Pulver geformten Rohlings in ein Formteil mit angestrebter Mikrostruktur bzw. gewünschten Gebrauchseigenschaften durch thermische Prozesse. In diesem Kapitel werden die Grundlagen zu Triebkräften und Kinetik sowie die prinzipiellen Mechanismen für Stofftransport und Verdichtung vorgestellt. Die verschiedenen Sintermechanismen Festphasensintern, Flüssigphasensintern und Reaktionssintern werden erläutert und mit einem Überblick über Drucksinterverfahren ergänzt. Abschließend wird ein Überblick über technologische Einflussfaktoren auf die Sinterung gegeben. KW - Technische Keramik KW - Sintermechanismen PY - 2018 SN - 978-3-8027-2986-7 SN - 978-3-8027-3081-8 SP - Kap. 4.6, 510 EP - 525 PB - Vulkan Verlag GmbH CY - Essen ET - 3 AN - OPUS4-43656 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, T. A1 - Reimann, T. A1 - Bochmann, A. A1 - Vogel, A. A1 - Capraro, B. A1 - Mieller, Björn A1 - Teichert, S. A1 - Töpfer, J. T1 - Sintering behavior, microstructure and thermoelectric properties of calcium cobaltite thickfilms for transversal thermoelectric multilayer generators N2 - The sintering behavior and the thermoelectric performance of Ca3Co4O9 multilayer laminates were studied, and a multilayer thermoelectric generator was fabricated. Compacts and multilayer samples with anisotropic microstructure and residual porosity were obtained after conventional sintering at 920 °C, whereas dense and isotropic multilayer samples were prepared by firing at 1200 °C and reoxidation at 900 °C. A hot-pressed sample has a dense and anisotropic microstructure. Samples sintered at 920 °C exhibit low electrical conductivity due to the low density, whereas the Seebeck coefficient is not sensitive to preparation conditions. However, thermal conductivity of multilayers is very low, and, hence acceptable ZT values are obtained. A ransversal multilayer thermoelectric generator (TMLTEG) was fabricated by stacking layers of Ca3Co4O9 green tapes, AgPd conductor printing, and co-firing at 920 °C. The TMLTEG has a power output of 3 mW at ΔT =200 K in the temperature interval of 25 °C to 300 °C. KW - Thermoelectric oxide KW - Calcium cobaltite KW - Pressure-assisted sintering KW - Multilayer PY - 2018 DO - https://doi.org/10.1016/j.jeurceramsoc.2017.11.017 SN - 0955-2219 SN - 1873-619X VL - 38 IS - 4 SP - 1600 EP - 1607 PB - Elsevier Ltd. AN - OPUS4-43983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn A1 - Bresch, Sophie A1 - Marucha, P. A1 - Moos, R. A1 - Rabe, Torsten T1 - Sintering and interconnecting thermoelectric oxides for energy applications N2 - Today, more than 12% of the primary energy is lost in the form of waste heat. Thermoelectric generators (TEGs) can convert waste heat directly into electrical power by utilizing the Seebeck effect. The performance of such a generator is defined by a dimensionless figure of merit ZT of the thermoelectric pairs and the resistance R of the metallic contacts between these pairs. The figure of merit of thermoelectric oxides is considerably smaller compared to semiconductors. Still, thermoelectric oxides like calcium cobaltite (Ca3Co4O9) are attractive for applications at elevated temperatures in air. In contrast to the established π-type architecture of common TEGs, tape casting and multilayer technology may be applied for cost-effective manufacturing of oxide TEGs. Promising demonstrations of multilayer TEGs have been published in the last years. Still, the development of reliable and scalable manufacturing processes and proper material combinations is necessary. The aim of our project is to evaluate the feasibility of low temperature co-fired ceramics (LTCC) technology for a practical manufacturing of oxide multilayer TEGs of Ca3Co4O9 (p-type) and calcium manganate (CaMnO3, n-type). Ca3Co4O9 exhibits an undesired phase decomposition at 926 °C. Because of that, the application of sintering strategies and interconnect concepts well known from LTCC technology is a promising approach. We present results of pressure-assisted sintering of Ca3Co4O9 multilayer at 900 °C and axial pressures of up to 7.5 MPa. Ca3Co4O9 was produced by solid state reaction of CaCO3 and cobalt(II,III)oxide at 900 °C. Green tapes were prepared by a doctor-blade process, manually stacked and laminated by uniaxial thermocompression. Sintering was conducted in a LTCC sintering press between SiC setter plates. The thickness shrinkage was recorded by an in-situ technique. After sintering under 7.5 MPa, the microstructure of the single phase material shows a high density of 95 % and an advantageous alignment of the platelet grains. This results in good electrical conductivity and a comparatively high ZT of 0.018 at room temperature. However, the lowering of CaMnO3 sintering temperature from above 1200 °C to below 920 °C remains a challenge. To select a proper metal paste for interconnections of an oxide TEG, several pastes have been investigated regarding contact resistance of internal and external (soldered) connections in a preliminary study. Commercial pastes containing Ag, Au, Au/Pt, Ag/Pd, and Ag/Pd/Bi were manually applied and post-fired on sintered test bars of Ca3Co4O9 and CaMnO3 at 900 °C for 2 h. All tested pastes formed mechanically stable metallization after firing. For resistance measurement, 4-wire method and a custom-made probe head were used. The contacts on Ca3Co4O9 exhibit significantly (2-sample t-test, α = 5%) higher resistance compared to contacts on CaMnO3. Pure silver paste exhibits the lowest resistance for internal contacts on both materials, lower than 5 mΩ on CaMnO3. Ag/Pd/Bi paste resulted in conspicuously high variance of resistance. EDX analyses clarified an enrichment of Bi in the thermoelectric material near the interface and thereby the formation of an oxide layer with probably high electrical resistance. The thickness of that layer varies with the thickness of metallization. In conclusion, the use of Bi containing pastes is not advisable. Pure Ag paste shows the best results regarding resistance and solderability. T2 - CICMT 2018 CY - Aveiro, Portugal DA - 18.04.2018 KW - Thermoelectric oxide KW - Thermoelectric generator KW - Multilayer technology KW - Pressure-assisted sintering PY - 2018 AN - OPUS4-44740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon A1 - Maierhofer, Christiane A1 - Hilgenberg, Kai A1 - Mohr, Gunther A1 - Gumenyuk, Andrey A1 - Straße, Anne A1 - Pittner, Andreas A1 - Günster, Jens A1 - Gornushkin, Igor B. A1 - Pelkner, Matthias A1 - Ehlers, Henrik A1 - Heckel, Thomas A1 - Zscherpel, Uwe A1 - Seeger, Stefan A1 - Bruno, Giovanni T1 - ProMoAM - Verfahrensentwicklung für das Prozessmonitoring in der additiven Fertigung N2 - Verfahren zum in-situ Monitoring der Prozess- und Bauteilparameter sollen Fehlstellen und Inhomogenitäten bereits während der Fertigung nachweisen und zukünftig auch die Regelung der Prozessparameter ermöglichen. T2 - Challenges in Additive Manufacturing: Innovative Materials and Quality Control, Berlin Partner Workshop CY - Berlin, Germany DA - 12.09.2018 KW - Additive Fertigung KW - Prozessmonitoring KW - ProMoAM PY - 2018 AN - OPUS4-46300 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mueller, Axel A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Simon, Franz-Georg A1 - Braun, Ulrike T1 - The effect of polymer aging on the uptake of fuel aromatics and ethers by microplastics N2 - Microplastics are increasingly entering marine, limnic and terrestrial ecosystems worldwide, where they sorb hydrophobic organic contaminants. Here, the sorption behavior of the fuel-related water contaminants benzene, toluene, ethyl benzene and xylene (BTEX) and four tertiary butyl ethers to virgin and via UV radiation aged polypropylene (PP) and polystyrene (PS) pellets was investigated. Changes in material properties due to aging were recorded using appropriate polymer characterization methods, such as differential scanning calorimetry, Fourier transform infrared spectroscopy, gel permeation chromatography, X-ray photoelectron spectroscopy, and microscopy. Pellets were exposed to water containing BTEX and the ethers at 130-190 mg/L for up to two weeks. Aqueous sorbate concentrations were determined by headspace gas chromatography. Sorption to the polymers was correlated with the sorbate's Kow and was significant for BTEX and marginal for the ethers. Due to substantially lower glass transition temperatures, PP showed higher sorption than PS. Aging had no effect on the sorption behavior of PP. PS sorbed less BTEX after aging due to an oxidized surface layer. KW - BTEX KW - Polypropylene KW - Polystyrene KW - Sorption KW - Degradation PY - 2018 DO - https://doi.org/10.1016/j.envpol.2018.04.127 SN - 0269-7491 VL - 240 SP - 639 EP - 646 PB - Elsevier CY - Amsterdam AN - OPUS4-44990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Skrotzki, Birgit A1 - Stegemann, Robert A1 - Löwe, Peter A1 - Kreutzbruck, M. T1 - The role of surface topography on deformation-induced magnetization under inhomogeneous elastic-plastic deformation N2 - It is widely accepted that the magnetic state of a ferromagnetic material may be irreversibly altered by mechanical loading due to magnetoelastic effects. A novel standardized nondestructive testing (NDT) technique uses weak magnetic stray fields, which are assumed to arise from inhomogeneous deformation, for structural health monitoring (i.e., for detection and assessment of damage). However, the mechanical and microstructural complexity of damage has hitherto only been insufficiently considered. The aim of this study is to discuss the phenomenon of inhomogeneous “self-magnetization” of a polycrystalline ferromagnetic material under inhomogeneous deformation experimentally and with stronger material-mechanical focus. To this end, notched specimens were elastically and plastically deformed. Surface magnetic states were measured by a three-axis giant magnetoresistant (GMR) sensor and were compared with strain field (digital image correlation) and optical topography measurements. It is demonstrated that the stray fields do not solely form due to magnetoelastic effects. Instead, inhomogeneous plastic deformation causes topography, which is one of the main origins for the magnetic stray field formation. Additionally, if not considered, topography may falsify the magnetic signals due to variable lift-off values. The correlation of magnetic vector components with mechanical tensors, particularly for multiaxial stress/strain states and inhomogeneous elastic-plastic deformations remains an issue. KW - Magnetic stray fields KW - Magnetomechanical effect KW - Damage KW - Topography KW - Multiaxial deformation KW - Notch KW - Plastic deformation KW - Metal magnetic memory KW - Digital image correlation KW - Structural steel PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-457878 DO - https://doi.org/10.3390/ma11091518 SN - 1996-1944 VL - 11 IS - 9 SP - 1518, 1 EP - 26 PB - MDPI CY - Basel, Switzerland AN - OPUS4-45787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Cabeza, S. A1 - Kuntner, M. A1 - Mishurova, Tatiana A1 - Klaus, M. A1 - Kling e Silva, L. A1 - Skrotzki, Birgit A1 - Genzel, Ch. A1 - Bruno, Giovanni T1 - Visualisation of deformation gradients in structural steel by macroscopic magnetic domain distribution imaging (Bitter technique) N2 - Abstract While classically used to visualise the magnetic microstructure of functional materials (e.g., for magnetic applications), in this study, the Bitter technique was applied for the first time to visualise macroscopic deformation gradients in a polycrystalline low-carbon steel. Spherical indentation was chosen to produce a multiaxial elastic–plastic deformation state. After removing the residual imprint, the Bitter technique was applied, and macroscopic contrast differences were captured in optical microscopy. To verify this novel characterisation technique, characteristic “hemispherical” deformation zones evolving during indentation were identified using an analytical model from the field of contact mechanics. In addition, near-surface residual stresses were determined experimentally using synchrotron radiation diffraction. It is established that the magnetic domain distribution contrast provides deformation-related information: regions of different domain wall densities correspond to different “hemispherical” deformation zones (i.e., to hydrostatic core, plastic zone and elastic zone, respectively). Moreover, the transitions between these three zones correlate with characteristic features of the residual stress profiles (sign changes in the radial and local extrema in the hoop stress). These results indicate the potential of magnetic domain distribution imaging: visualising macroscopic deformation gradients in fine-grained ferromagnetic material with a significantly improved spatial resolution as compared to integral, mean value-based measurement methods. KW - Bitter technique KW - Deformation KW - Expanding cavity model KW - Indentation KW - Magnetic domain distribution KW - Residual stress PY - 2018 DO - https://doi.org/10.1111/str.12296 SN - 1475-1305 VL - 54 IS - 6 SP - e12296, 1 EP - 15 PB - Wiley AN - OPUS4-46569 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Nützmann, Kathrin A1 - Falk, Florian A1 - de Oliveira Guilherme Buzanich, Ana A1 - Witte, Steffen A1 - Radtke, Martin T1 - Early stages of high temperature oxidation/sulfidation studied by synchrotron x-ray diffraction and spectroscopy N2 - Ferritic high temperature alloys are widely used as boiler tube and heat exchanger materials in coal, biomass and co-fired power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres that lead to a change of the material properties and a further degradation of the material. Material changes caused by aging in highly corrosive and toxic gases such as SO2 are mainly studied ex situ after the reaction is finished. The solid material is deposited in the atmosphere for a certain period of time, and material changes are then examined by various microscopic techniques such as optical microscopy (OM), electron microprobe analysis (EMPA), scanning electron microscopy (SEM and TEM) and X-ray diffraction (XRD). Nevertheless, extensive efforts were made to study material changes of high temperature alloys under oxidizing and reducing atmospheres by environmental scanning electron microscopy or in situ TEM techniques However, the possibilities of microscopic in situ techniques are very limited for the use of highly corrosive and toxic gases such as SO2. Since Sulfur induced corrosion at temperatures relevant for coal and biomass fired power plants, which is causing breakaway oxidation and sulfide precipitation at grain boundaries, is still of scientific interest, the current work focuses on the effect of SO2 in an initial stage of corrosion of ferritic alloys. For the analysis of early stages of combined oxidation and sulphidation processes of Fe-Cr model alloys the usage of a light furnace to conduct a rapid reactive annealing experiment is feasible. Previous studies presented distinct results of the influence of chromium on early high temperature corrosion by SO2 by this technique and subsequent classical metallographic analyses. However, it is still not possible to trace the corrosion mechanism in real time by conducting single aging experiments. The current work introduces two different approaches to study the initial stages of high temperature oxidation processes by applying above state of the art X-ray diffraction and spectroscopy methods. One part focuses on the real time observation of the formation of corrosion products such as oxides and sulfides by energy dispersive X-ray diffraction (EDXRD). The potential of this technique to study crystallization and growth processes of thin films in a reactive environment in real time was previously shown for different compound semiconductors. This approach was now applied to follow oxidation and sulphidation processes of ferritic model alloys in SO2 and SO2/H2O environments. The diffraction signals of the X-rays were detected during the corrosion process and the peak area and positions were analyzed as a function of time. This procedure enables monitoring external oxide growth and material loss in real time in an early stage of corrosion. The other part of the current work presents the possibilities of X-ray absorption near edge structure spectroscopy (XANES) to characterize oxide scales and their growth mechanisms. Precise phase identification and quantification of corrosion products in a multi-phase oxide/sulfide scale is a pre-requisite to understand diffusion paths of metal ions and gas components. It is a challenging task to distinguish structurally similar reaction products such as Fe3O4 and FeCr2O4 especially in thin films with texture effects by diffraction. To illustrate for example Cr-out diffusion of an alloy throughout an inner and external oxide scale the differentiation of Fe3O4 and FeCr2O4 is indispensable. XANES uses the photoionization effect at the metal absorption edge in an aging product and accesses by this structural and chemical information. The current work uses XANES at the Fe-K and Cr-K absorption edge to identify various aging products grown as thin layers on alloys after short time aging experiments. A reaction chamber for combining high temperature oxidation experiments with surface sensitive X-ray absorption near edge structure spectroscopy will be introduced and first results of XANES on scales at high temperatures will be presented. T2 - ISHOC 2018 CY - Matsue, Japan DA - 22.10.2018 KW - Corrosion KW - Sulfidation KW - In situ KW - Diffraction KW - XANES PY - 2018 AN - OPUS4-47278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Umgebungsinduzierte Spannungsrissbildung (ESC) von PE-HD induziert durch äußerliche Einwirkung organischer Flüssigkeiten N2 - Polyethylen hoher Dichte (PE-HD) wird als Werkstoff für Rohre und Behälter für den Transport und zur Lagerung von Gefahrgütern verwendet. Für die Beurteilung und technische Freigabe dieser Materialien ist insbesondere das Verständnis des Schädigungsmechanismus des langsamen, umgebungsbedingten Spannungsrisses (engl.: „environmental stress cracking“, ESC) essentiell. ESC tritt bei relativ geringen auf einen Werkstoff einwirkenden mechanischen Spannungen auf. An lokalen Fehlstellen (z.B. Defekte, Inhomogenitäten, Kerben) beginnend wächst ein Riss langsam durch das Material und führt nach gewisser Zeit zu einem charakteristischen, pseudo-spröden Bruch. Dabei wird das Risswachstum durch äußere Medieneinwirkung zusätzlich entscheidend beeinflusst. Dieses langsame Risswachstum wird als Hauptursache für das plötzliche und unerwartete Versagen von Polymerwerkstoffen angesehen. Eine etablierte Prüfmethode zur Bewertung des Materialverhaltens gegenüber dieses Schädigungsmechanismus ist der Full-Notch Creep Test (FNCT), der für PE-HD Behältermaterialien üblicherweise unter Verwendung von wässrigen Netzmittellösungen (Arkopal N 100) durchgeführt wird. Die aus dem FNCT erhaltene Standzeit dient dabei als Bewertungskriterium für verschiedene PE-HD-Werkstoffe. In einer Studie wurden neben einer typischen Arkopal-N-100-Netzmittellösung praktisch relevante, organische Flüssigkeiten wie Biodiesel und Diesel als Testmedien verwendet, um deren Einfluss auf das ESC-Verhalten von PE-HD-Behältermaterialien zu charakterisieren. Neben der klassischen Standzeit-Auswertung erfolgte eine erweiterte Bruchflächenanalyse mittels Licht- (LM), Laserscanning- (LSM) und Rasterelektronenmikroskopie (REM). Insbesondere die LSM erlaubt eine schnelle und einfache Unterscheidung pseudo-spröder und duktiler Bruchbilder, die zur Beurteilung der Repräsentativität des FNCT für das dem Spannungsriss zugrundeliegenden langsamen Risswachstum von Bedeutung ist. T2 - Polymer Service GmbH Merseburg - "Lebensdauerabschätzung von Polymerwerkstoffen - Möglichkeiten und Grenzen" CY - Merseburg, Germany DA - 27.03.2019 KW - Environmental Stress Cracking (ESC) KW - Slow Crack Growth (SCG) KW - Spannungsriss KW - Polyethylen hoher Dichte KW - Full-Notch Creep Test (FNCT) KW - Bruchflächenanalyse KW - Laserscanningmikroskopie (LSM) PY - 2019 AN - OPUS4-52947 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balzer, R. A1 - Behrens, H. A1 - Reinsch, Stefan A1 - Fechtelkord, M. T1 - Structural investigation of hydrous phosphate glasses N2 - Dissolved water has major impact on the physical and chemical properties of phosphate glasses. In the present study we have investigated the structural response to water incorporation for glasses in the system Li2O–MgO–Al2O3–P2O5. Glasses containing 0–8 wt% H2O were synthesised at 500 MPa confining pressure in internally heated gas pressure vessels at 1323 K (LMP, Al-poor glass) and 1423 K (LMAP, Al-enriched glass). Water contents of glasses were determined by pyrolysis and subsequent Karl-Fischer titration (KFT) and/or by infrared spectroscopy. Density varies nonlinearly with water content implying large structural changes when adding up to 2 wt% H2O to the dry glass. Glass Transition temperatures measured by differential thermal analysis (DTA) continuously decrease with water content. The trend can be explained by depolymerisation of the phosphate network. Near-infrared spectroscopy shows that even in Al poor glasses only a minority of dissolved water is present as H2O molecules, but the largest amount is present as OH Groups formed by hydrolysis of P–O–P bonds. The network is stabilised by aluminium which is predominantly six-coordinated in these glasses as shown by 27Al MAS NMR spectroscopy. With increase of Al in the glasses, breaking up of the Phosphate network through hydrolysis is depressed, i.e. much lower OH Contents are formed at same total water content. Network depolymerisation upon addition of H2O is evident also from 31P MAS NMR spectroscopy. While Phosphate tetraheda are crosslinked by two to three bridging oxygen in dry glasses, diphosphate Groups are dominant in glasses containing 8 wt% H2O. T2 - 2. INT. CONF. ON PHOSPHATE GLASSES CY - Oxford, UK DA - 26.07.2017 KW - water speciation KW - phosphate glasses KW - infrared spectroscopy KW - NMR spectroscopy KW - high pressure PY - 2019 DO - https://doi.org/10.13036/17533562.60.2.041 SN - 1753-3562 VL - 60 IS - 2 SP - 49 EP - 61 PB - Society of Glass Technology CY - Sheffield AN - OPUS4-48122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Charmi, Amir A1 - Falkenberg, Rainer A1 - Skrotzki, Birgit T1 - Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts N2 - This work aims for a yield function description of additively manufactured parts of S316L steel at the continuum-mechanical macro-scale by means of so-called virtual experiments using a crystal plasticity (CP) model at meso-scale. Additively manufactured parts require the consideration of the specific process-related microstructure, which prevents this material to be macroscopically treated as isotropic, because of crystallographic as well as topological textures. From virtual experiments, yield loci under various loading conditions are simulated. The scale bridging from meso- to macro-scale is realised by the identification of the simulated yield loci as a modified anisotropic Barlat-type yield model representation. T2 - Workshop on Additive Manufacturing, BAM CY - Berlin, Germany DA - 13.05.2019 KW - Virtual experiments KW - Additive manufacturing KW - Anisotropy KW - Crystal plasticity KW - Scale-bridging PY - 2019 AN - OPUS4-48064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra A1 - Lindemann, Franziska A1 - Hodoroaba, Vasile-Dan T1 - Nano Powder - a Challenge for Granulometry N2 - If the particle size decreases, the ratio of surface area to volume increases considerably. This provides benefits for all surface-driven processes that run faster or at lower temperatures than larger particles. However, handling and characterization of the nanopowders are much more difficult. Particularly polydisperse powders with irregular shape, as grinding products, represent a challenge. Granulometry in the submicron and nanoscale often leads to incorrect results without knowledge of particle morphology. This presentation demonstrates potentials of using the volume-specific surface area (SV or VSSA) in the granulometric characterization of nanopowders, for instance, correlations between the volume-specific surface area and the median particle size are discussed considering the particle morphology and the model of the logarithmic normal distribution. Moreover, the presentation deals with the optimal dispersion of nanopowders during sample preparation. Indirect ultrasound device with defined cooling was developed to prevent both contamination by sonotrode abrasion and sample changes by heat. Successful granulometric characterization of nanopowders demands both improved dispersion technology and very often an effective combination of two or more measurement methods. T2 - Jahrestagung der Deutschen Keramischen Gesellschaft CY - Leoben, Austria DA - 06.05.2019 KW - Nano screening KW - VSSA KW - Nano particle KW - Particle size PY - 2019 AN - OPUS4-47976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Partikelgrößenverteilung mittels Zentrifugen-Sedimentationsverfahren nach ISO 13318-2 (Küvette) N2 - Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Nach einem Vergleich der Ergebnisse mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet. T2 - Rheologie und Stabilität von dispersen Systemen CY - Potsdam, Germany DA - 03.06.2019 KW - Nanomaterial KW - Partikelgrößenverteilung KW - Analytische Zentrifuge PY - 2019 AN - OPUS4-48286 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Höhne, Patrick A1 - Kuchenbecker, Petra A1 - Rabe, Torsten T1 - Superior granule properties by spray drying controlled destabilized slurries with ultrasound N2 - Homogeneous introduction of organic additives is a key of ceramic powder processing. Addition of organics to ceramic slurries holds advantages compared to dry processing like organic content reduction and a more homogeneous additive distribution on the particle surface. Investigations of the alumina slurries were primarily based on zeta potential measurements and sedimentation analysis by optical centrifugation. Both methods were combined to determine a suitable additive type, amount and composition, whereas the spray drying suitability has been ensured by viscosity measurements. Granules, yielded by spray drying of such ideally dispersed alumina slurries, are mostly hollow and possess a hard shell. Those granules cannot easily be processed and can only hardly be destroyed in the following shaping step, leading to sinter bodies with many defects and poor strength and density. The precise slurry destabilization, carried out after ideally dispersing the ceramic powder, shows a strong influence on the drying behavior of the granules and hence on the granule properties. A promising degree of destabilization and partial flocculation was quantified by optical centrifugation and resulted in improved granule properties. Spray drying the destabilized alumina slurries yielded homogeneous “non-hollow” granules without the above mentioned hard shell. Sample bodies produced of these granules exhibited a reduction of defect size and number, leading to better results for sinter body density and strength. The positive effect of the slurry destabilization has been further improved, by exchanging the atomizing unit from a two-fluid one to an ultrasound atomizer with only minor slurry adjustments necessary. The controlled destabilization and ultrasound atomization of the ceramic slurry show excellent transferability for zirconia and even ZTA (zirconia toughened alumina) composite materials. T2 - Partec 2019 CY - Nuremberg, Germany DA - 09.04.2019 KW - Destabilization KW - Slurry KW - Ultrasound KW - Atomization PY - 2019 AN - OPUS4-48291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghafafian, Carineh A1 - Popiela, Bartosz A1 - Nielow, Dustin A1 - Trappe, Volker T1 - Restoration of structural integrity – a comparison of various repair concepts for wind turbine rotor blade shells N2 - Localized patches are a cost- and time-effective method for repairing fiber-reinforced polymer (FRP) sandwich wind turbine rotor blade shells. To increase the understanding of their effect on the fatigue of the blades, this study examines the effect of various layup methods of localized repair patches on the structural integrity of composite sandwich structures. Manufactured with the vacuum-assisted resin infusion (VARI) process, the shell test specimens are produced as a curved structure with glass fiber reinforced polymer (GFRP) sandwiching a polyvinyl chloride (PVC) foam core. Patch repairs are then introduced with varying layup techniques, and material properties are examined with cyclic fatigue tests. The transition region between patch and parent material is studied in greater detail with finite element method (FEM) simulations, with a focus on the effect of fiber orientation mismatch. Damage onset, crack development, and eventual failure are monitored with in-situ non-destructive testing methods to develop a robust understanding of the effects of repair concepts on material stiffness and strength. T2 - SMAR 2019 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.2019 KW - Lightweight materials KW - Glass fiber reinforced polymers KW - Sandwich KW - Wind turbine blades PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-482170 SP - 1 EP - 8 PB - German Society for Non-Destructive Testing (DGZfP e.V.) AN - OPUS4-48217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Agea-Blanco, Boris A1 - Blaeß, Carsten A1 - Waurischk, Tina T1 - Sintering and foaming of silicate glass powders N2 - Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites, glass bonded ceramics or pastes. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface. T2 - IMAPS/ACerS 15th International Conference and Exhibition on Ceramic Interconnect and Ceramic Microsystems Technologies (CICMT 2019) CY - Shanghai, China DA - 16.04.2019 KW - Glass powder KW - Sintering KW - Foaming PY - 2019 AN - OPUS4-48196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan A1 - Tielemann, Christopher A1 - Busch, R. A1 - Patzig, C. A1 - Müller, Ralf A1 - Höche, T. T1 - Oriented surface crystallization in 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glasses N2 - Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. The vast majority of previous work does not consider possible effects of surface preparation and surrounding atmosphere. Moreover, very few observations of surface crystal orientation were made on separately grown crystals. The aim of our project is to advance the basic understanding of oriented surface crystallization, e.g. whether preferred orientation of surface crystals results from oriented nucleation or reorientation mechanisms during early crystal growth. In both cases, crystal orientation may reflect the orientation of the glass surface or that of anisotropic active surface nucleation sites. Therefore, we focus on orientation of surface crystals separately growing under controlled conditions. First results on diopside (MgCaSi2O6) and walstromite (BaCa2Si3O9) crystals growing from 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glass surfaces, respectively, indicate that different orientation mechanisms may occur. Neighbored walstromite crystals were found to gradually reorient themselves when they are going to impinge each other during stepwise isothermal treatments (log η = 4,5 Pa*s) of polished glass samples. Nevertheless, no preferred crystal orientation was evident for separate crystals. For diopside crystals growing from polished glass surfaces (1 μm diamond lapping foil), strong preferred orientation was observed for 3.5 to 85 min annealing at 850 °C. Electron Backscatter Diffraction (EBSD) studies showed that the c-axis of surface crystals is oriented parallel to the glass surface and that separated diopside crystals as small as 600 nm are already oriented. Studies on glass surfaces, polished with diamond lapping foils starting from 16 μm down to 1 μm grain, revealed that crystal orientation may scatter arround this preferential orientation and that this scatter progressively decreases with decreasing polishing grain size. T2 - 93rd Annual Meeting of the German Society of Glass Technology (DGG) in conjunction with the French Union for Science and Glass Technology (USTV) Annual Meeting CY - Nuremberg, Germany DA - 13.05.2019 KW - Surface crystallization KW - Orientation KW - Glass KW - Diopside PY - 2019 AN - OPUS4-48198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. A1 - Niebergall, Ute A1 - Böhning, Martin A1 - Bruno, Giovanni ED - Erdmann, Maren T1 - Diesel-induced transparency of plastically deformed high-density polyethylene N2 - High-density polyethylene becomes optically transparent during tensile drawing when previously saturated with diesel fuel. This unusual phenomenon is investigated as it might allow conclusions with respect to the material behavior. Microscopy, differential scanning calorimetry, density measurements are applied together with two scanning X-ray scattering techniques: wide angle X-ray scattering (WAXS) and X-ray refraction, able to extract the spatially resolved crystal orientation and internal surface, respectively. The sorbed diesel softens the material and significantly alters the yielding characteristics. Although the crystallinity among stretched regions is similar, a virgin reference sample exhibits strain whitening during stretching, while the diesel-saturated sample becomes transparent. The WAXS results reveal a pronounced fiber texture in the tensile direction in the stretched region and an isotropic orientation in the unstretched region. This texture implies the formation of fibrils in the stretched region, while spherulites remain intact in the unstretched parts of the specimens. X-ray refraction reveals a preferred orientation of internal surfaces along the tensile direction in the stretched region of virgin samples, while the sample stretched in the diesel-saturated state shows no internal surfaces at all. Besides from stretching saturated samples, optical transparency is also obtained from sorbing samples in diesel after stretching. KW - PE-HD Sorption KW - Cavitation KW - Diesel Fuel KW - X-ray refraction KW - WAXS KW - Internal Surfaces KW - Crystal Texture PY - 2019 DO - https://doi.org/10.1007/s10853-019-03700-8 SN - 1573-4803 SN - 0022-2461 VL - 54 IS - 17 SP - 11739 EP - 11755 PB - Springer US CY - US AN - OPUS4-48226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Addressing ESC using FNCT enhanced by optical fracture surface analysis N2 - During their lifetime, polymer components subjected to mechanical loads and environmental influences show a loss of their mechanical properties required for their specific applications. In this respect, the craze-crack damage mechanism slow crack growth (SCG) is relevant for PE-HD components used in high-performance applications such as pipes and containers for the storage and transport of dangerous goods. SCG is considered to be the major failure mechanism in polyolefins and it typically occurs suddenly and unexpectedly. Due to the fields of application, SCG is a safety relevant issue. To test for the resistance of PE-HD pipe and container materials against SCG, the full-notch creep test (FNCT) is widely applied in Europe. In this study, SCG phenomena in PE-HD are investigated in detail based on an improved FNCT, especially including the consideration of the influence of environmental liquids effecting the damage mechanism. Using an enhanced fracture surface and a crack propagation analysis with imaging techniques such as light microscopy (LM), laser scanning microscopy (LSM), X-ray computed tomography (CT-scan) and scanning electron microscopy (SEM), detailed data concerning SCG are obtained. The combined application of FNCT and such imaging techniques is explicitly advantageous and recommended to gain important information on damage occurring to PE-HD induced by mechanical stress and the influence of environmental liquids, which is essential within the Fourth Industry Revolution. T2 - PPS Europe-Africa 2019 Regional Conference (PPS 2019) CY - Pretoria, South Africa DA - 18.11.2019 KW - Polyethylene, PE-HD KW - Full-Notch Creep Test (FNCT) KW - Fracture surface analysis KW - Slow crack growth KW - Environmental stress cracking KW - Laser Scanning Microscopy (LSM) KW - Scanning Electron Microscopy (SEM) PY - 2019 AN - OPUS4-50939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus A1 - Marschall, Niklas A1 - Niebergall, Ute A1 - Böhning, Martin T1 - An optical criterion for the assessment of Full-Notch Creep Test (FNCT) fracture surfaces N2 - The full-notch creep test (FNCT) is a common method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD) 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 specimens mechanically loaded in a well-defined liquid environment. Since the craze-crack damage mechanism underlying the ESC process is associated with brittle failure, the occurrence of globally brittle fracture surfaces is a prerequisite to consider an FNCT measurement as representative for ESC . Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. Due to the experimental setup, an inevitable increase of the true mechanical stress and the associated appearance of small ductile parts on fracture surfaces is induced in any case. Hence, an FNCT experiment is considered as 'valid', if the corresponding fracture surface is predominantly brittle . Based on laser scanning microscopy (LSM) height data of FNCT fracture surfaces , a universal and easy-to-use phenomenological criterion was developed to assess the validity of distinct FNCT experiments. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing. T2 - PPS Europe-Africa 2019 Regional Conference (PPS 2019) CY - Pretoria, South Africa DA - 18.11.2019 KW - Full-Notch Creep Test (FNCT) KW - Polyethylene, PE-HD KW - Fracture surface analysis KW - Environmental stress cracking (ESC) KW - Optical criterion KW - Brittle fracture PY - 2019 AN - OPUS4-50940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grun, Benthe Birger A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen ED - Christ, Hans-Jürgen T1 - Charakterisierung von Hochtemperaturwerkstoffen durch Zug- und Ermüdungsversuche an Kleinproben T1 - Characterization of high-temperature materials by tensile and fatigue tests on small specimens N2 - Die Verwendung von miniaturisierten Probengeometrien in der mechanischen Prüfung ermöglicht die Entnahme des Probenmaterials direkt aus kritischen Bereichen wie Fügeverbindungen und ermöglicht die Prüfung von kleinen Bauteilen wie additiv gefertigten Strukturen. In der vorliegenden Arbeit werden exemplarisch die Ergebnisse von vergleichenden Zug- und niederzyklischen Schwing-versuchen (LCF) an dem austenitischen Stahl AISI 316L und der Nickelbasislegierung IN718 vorgestellt. Die Prüfergebnisse der Kleinproben aus AISI 316L weisen die charakteristischen Eigenschaften des Werkstoffs auf, und die Analyse der Zug- und Ermüdungsdaten führt zu Werten, die den Literaturdaten weitgehend entsprechen. Der direkte Vergleich mit Standardprobendaten zeigt jedoch systematische Abweichungen bei Zugfestigkeit, Dehngrenze und Gleichmaßdehnung, die in diesem Beitrag diskutiert werden. N2 - The use of miniaturized specimen geometries in mechanical testing allows to extract speci-men material directly from critical areas such as weldments and to test small structures such as additively manufactured components. In the present paper, example results of comparative tensile and low-cyclic fatigue tests (LCF) on the austenitic steel AISI 316L and the nickel-based alloy IN718 are presented. The test results of the small specimens on AISI 316L show the characteristic properties of the material, and the analysis of the tensile and fatigue tests leads to values which largely correspond to literature data. However, the direct comparison with standard sample data shows systematic deviations in tensile strength, yield strength and uniform elongation, which are discussed in this paper. T2 - Werkstoffprüfung 2019 CY - Neu-Ulm, Germany DA - 03.12.2019 KW - Kleinprobenprüfung KW - Probengrößeneffekt KW - Low Cycle Fatigue KW - Zugversuch KW - AISI 316L KW - IN 718 PY - 2019 SP - 329 EP - 334 AN - OPUS4-50220 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grun, Benthe Birger A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit A1 - Avila, Luis A1 - Charmi, Amir T1 - Charakterisierung von Hochtemperaturwerkstoffen durch Zug- und Ermüdungsversuche an Kleinproben N2 - Die Verwendung von miniaturisierten Probengeometrien in der mechanischen Prüfung ermöglicht die Entnahme des Probenmaterials direkt aus kritischen Bereichen wie Fügeverbindungen und ermöglicht die Prüfung von kleinen Bauteilen wie additiv gefertigten Strukturen. In der vorliegenden Arbeit werden exemplarisch die Ergebnisse von vergleichenden Zug- und niederzyklischen Schwingversuchen (LCF) an dem austenitischen Stahl AISI 316L und der Nickelbasislegierung IN718 vorgestellt. Die Prüfergebnisse der Kleinproben aus AISI 316L weisen die charakteristischen Eigenschaften des Werkstoffs auf, und die Analyse der Zug- und Ermüdungsdaten führt zu Werten, die den Literaturdaten weitgehend entsprechen. Der direkte Vergleich mit Standardprobendaten zeigt jedoch systematische Abweichungen bei Zugfestigkeit, Dehngrenze und Gleichmaßdehnung, die in diesem Beitrag diskutiert werden. T2 - Werkstoffprüfung 2019 CY - Neu-Ulm, Germany DA - 03.12.2019 KW - Kleinprobenprüfung KW - Probengrößeneffekt KW - Low Cycle Fatigue KW - Zugversuch KW - AISI 316L KW - IN 718 PY - 2019 AN - OPUS4-50221 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Faserkunststoffverbunde (FKV) in Forschung und Anwendung N2 - Der Fachbereich Mechanik der Polymerwerkstoffe befasst sich mit der Charakterisierung der mechanischen Eigenschaften und der Degradation von Polymeren und Faserverbundwerkstoffen, die in hochbeanspruchten, sicherheitsrelevanten Konstruktionen wie jenen des Flugzeugbaus, des Automobilbaus und der Windenergie-Industrie eingesetzt werden. Auch die Analyse der chemischen und physikalischen Eigenschaften von Polymeren zählt zu unserem Aufgabenbereich. Das Spektrum reicht von der statischen Festigkeit über die Betriebsfestigkeit, die Messung bruchmechanischer und viskoelastischer Parameter bis hin zur Formulierung molekularer Schädigungsmechanismen. T2 - VDI Arbeitskreis Kunststofftechnik, BAM, Unter den Eichen 87 CY - Berlin, Germany DA - 14.08.2019 KW - Faserkunststoffverbunde KW - Werkstoffprüfung KW - Normung PY - 2019 AN - OPUS4-50128 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Effective composite testing – from specimen size to component scale N2 - Even for the basic measurements of material data for design and engineering of composite structures there is a need to upgrade standards. With a new shear frame test rig more precise values can be obtained. With advanced methods in the research on the fatigue behaviour of FRP it was found a load level of infinite life for GFRP and CFRP. This is in the range of typical strain values of airliners and rotor blades in normal operation. Statistically the mean time between damage events on rotor blades is 6 years (Deutscher Windenergie Report 2006). Due to imperfection in the production the shell structures get cracks after a few years fare before the designed life time. A shell test rig was built at BAM for efficient research on the effects of defects in production. Test blades of ~10m are an efficient way for SHM research and evaluation of NDT-methods and blade geometry. T2 - colloquium genesis-puc CY - Rio de Janeiro, Brazil DA - 01.11.2019 KW - Polymer matrix composites KW - Nondestructive testing KW - New standards PY - 2019 AN - OPUS4-50129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Polymer matrix composites investigated with NDT at BAM N2 - Statistically the mean time between damage events on rotor blades is 6 years (Deutscher Windenergie Report 2006). Due to imperfection in the production the shell structures get cracks after a few years fare before the designed life time. A shell test rig was built at BAM for efficient research on the effects of defects in production. In-situ and ex-situ NDT give a better understanding from degradation processes in composite materials. With advanced methods in the research on the fatigue behaviour of FRP it was found a load level of infinite life for GFRP and CFRP. This is in the range of typical strain values of airliners and rotor blades in normal operation. Due to the fibre-composite nature NDT techniques have to be suitable to a wide length scale to image micro cracking as well as bigger defects. Therefore different techniques have to be applied and developed. T2 - Colloquium Abendi CY - São Paulo, Brazil DA - 05.11.2019 KW - Polymer matrix composites KW - Non-destructive testing PY - 2019 AN - OPUS4-50130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Fatigue life evaluation and certification according to CS22 N2 - The common fatigue life certification of aircrafts according to the certification Standards 23 and 25 follows a building block approach. Static tests at room temperature as well in humid and high temperature conditions are done on the coupon level. Additionally, a full-scale static and fatigue test must be performed on the complete airframe (minimum on the fuselage together with the wing). For each type-certificate the complete building block approach test program must be performed. Traditionally in Germany, the certification of sailplanes (Certification Standard 22) follows rather a family concept. A shared data base was created over the last 50 years based upon a large number of material testing. In addition to static tests at room temperature and hot-humid conditions, fatigue tests are also done on the coupon level. Additional static and fatigue tests were done on complex structures such as spar-beams, fuselages and full-scale wing structures. However, for each type-certificate, only static tests should be performed in full-scale. This concept is determined by the certification memorandum CM-S-006 “Composite Lightweight Aircraft” 2017. The presentation was given as an introduction to the discussion about the future expectations and developments of the EASA concerning the type-certification of lightweight aircrafts according to CS22 at the OSTIVE Sailplane Development Panel Meeting at the EASA in Cologne on the 11th of October 2019. T2 - OSTIV Sailplane Development Panel Meeting 2019, Europäische Agentur für Flugsicherheit (EASA) CY - Cologne, Germany DA - 11.10.2019 KW - Certification Standard 22 KW - EASA KW - Sailplane Development Panel KW - Fatigue Life Evaluation PY - 2019 AN - OPUS4-50147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zemke, F. A1 - Schölch, V. A1 - Bekheet, M.F. A1 - Schmidt, Franziska T1 - Surfactant-assisted sol–gel synthesis of mesoporous bioactive glass microspheres N2 - Spherical mesoporous bioactive glasses in the silicon dioxide (SiO2)-phosphorus pentoxide (P2O5)–calcium oxide (CaO) system with a high specific surface area of up to 300m2/g and a medium pore radius of 4 nm were synthesized by using a simple one-pot surfactant-assisted sol–gel synthesis method followed by calcination at 500–700°C. The authors were able to control the particle properties by varying synthesis parameters to achieve microscale powders with spherical morphology and a particle size of around 5–10 mm by employing one structure-directing agent. Due to a high Calcium oxide content of 33·6mol% and a phosphorus pentoxide content of 4·0mol%, the powder showed very good bioactivity up to 7 d of immersion in simulated Body fluid. The resulting microspheres are promising materials for a variety of life science applications, as further processing – for example, granulation – is unnecessary. Microspheres can be applied as materials for powder-based additive manufacturing or in stable suspensions for drug release, in bone cements or fillers. KW - bioactive KW - biomaterials KW - bone PY - 2019 DO - https://doi.org/10.1680/jnaen.18.00020 SN - 2045-9831 SN - 2045-984X VL - 8 IS - 2 SP - 126 EP - 134 PB - ICE Publishing CY - London AN - OPUS4-50148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, X. A1 - Schmidt, Franziska A1 - Gurlo, A. T1 - Fabrication of polymer-derived ceramics with hierarchical porosities by freeze casting assisted by thiol-ene click chemistry and HF etching N2 - The freeze casting technique assisted with cryo thiol-ene photopolymerization is successfully employed for the fabrication of macroporous polymer-derived silicon oxycarbide with highly aligned porosity. It is demonstrated that the free radical initiated thiol-ene click reaction effectively cross-linked the vinyl-containing liquid polysiloxanes into infusible thermosets even at low temperatures. Furthermore, mixed solution- and suspension-based freeze casting is employed by adding silica nanopowders. SiOC/SiO2 foams with almost perfect cylindrical shapes are obtained, demonstrating that the presence of nano-SiO2 does not restrict the complete photoinduced cross-linking. The post-pyrolysis HF acid treatments of produced SiOC monoliths yields hierarchical porosities, with SiOC/SiO2 nanocomposites after etching demonstrating the highest specific surface area of 494 m2/g and pore sizes across the macro-, meso- and micropores ranges. The newly developed approach gives a versatile solution for the fabrication of bulk polymer-derived ceramics with controlled porosity. KW - Freeze casting KW - Preceramic polymer KW - Hierarchical porosities KW - Thiol-ene click chemistry KW - Frozen state photopolymerization PY - 2019 DO - https://doi.org/10.1016/j.jeurceramsoc.2019.09.038 SN - 0955-2219 VL - 40 IS - 2 SP - 315 EP - 323 PB - Elsevier AN - OPUS4-49172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zocca, Andrea A1 - Lüchtenborg, Jörg A1 - Lima, P. A1 - Diener, S. A1 - Katsikis, N. A1 - Günster, Jens T1 - Additive Manufacturing of Silicon Carbide by LSD-print N2 - The layerwise slurry deposition (LSD) has been established in the recent years as a method for the deposition of ceramic powder layers. The LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade; each layer is sequentially deposited and dried to achieve a highly packed powder layer. The combination of binder jetting and LSD was introduced as a novel technology named LSD-print. The LSD-print takes advantage of the speed of binder jetting to print large areas, parallel to the flexibility of the LSD, which allows the deposition of highly packed powder layers with a variety of ceramic materials. The working principle and history of the LSD technology will be shortly discussed. A theoretical background will be also discussed, highlighting advantages and drawbacks of the LSD compared to the deposition of a dry powder. The last part of the talk will be dedicated to highlight recent results on the LSD-print of SiSiC of geometrically complex components, in collaboration between BAM and HC Starck Ceramics GmbH. Density, microstructure and mechanical properties of LSD-printed and isostatic pressed samples will be discussed and compared. T2 - XVI ECerS CONFERENCE CY - Torino, Italy DA - 16.06.2019 KW - Additive Manufacturing KW - Silicon Carbide KW - 3D printing KW - Layerwise Slurry Deposition PY - 2019 AN - OPUS4-49220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zocca, Andrea A1 - Mühler, T. A1 - Lima, P. A1 - Günster, Jens A1 - Lüchtenborg, Jörg T1 - Advanced ceramics by powder bed 3D printing N2 - Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability. However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive. This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions. In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles. T2 - Smart Made CY - Osaka, Japan DA - 01.09.2019 KW - Additive Manufacturing KW - Ceramic KW - Powder KW - Layerwise slurry deposition KW - 3D printing PY - 2019 AN - OPUS4-49221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilbig, Janka A1 - Borges de Oliveira, F. A1 - Schwentenwein, M. A1 - Günster, Jens T1 - Quality Aspects of Additively Manufactured Medical Implants - Defect Detection in Lattice Parts N2 - Additive Manufacturing technologies are developing fast to enable a rapid and flexible production of parts. Tailoring products to individual needs is a big advantage of this technology, which makes it of special interest for the medical device industry and the direct manufacturing of final products. Due to the fast development, standards to assure reliability of the AM process and quality of the printed products are often lacking. The EU project Metrology for Additively Manufactured Medical Implants (MetAMMI) is aiming to fill this gap by investigating alternative and cost efficient non-destructive measurement methods. T2 - yCAM Forum CY - Mons, Belgium DA - 03.03.2019 KW - Additive Manufacturing KW - Metrology PY - 2019 AN - OPUS4-49141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hlavacek, Petr A1 - Gluth, Gregor A1 - Lüchtenborg, Jörg A1 - Sturm, Patrick A1 - Mühler, T. A1 - Kühne, Hans-Carsten A1 - Günster, Jens T1 - A Novel Approach to Additive Manufacturing of Alkali-activated Materials: Laser-induced Slip Casting (LIS) of Lithium Aluminate/Silica Slurries N2 - Additive manufacturing of alkali-activated materials currently attracts a lot of attention, because of the possibility to produce customized high-performance elements for a range of applications, potentially being more resource-efficient than conventionally produced parts. Here, we describe a new additive manufacturing process for alkali-activated materials that is based on selective laser-heating of lithium aluminate/microsilica slurries. The new process-material combination allows to manufacture elements with complex geometries at high building rates and high accuracy. The process is versatile and transferrable to structures of sizes differing by orders of magnitude. The mechanical strength of the obtained materials was in the range of values reported for conventional metakaolin-based geopolymers, and superior to what has been hitherto reported for alkali-activated materials produced by additive manufacturing. This mechanical performance was obtained despite the fact that the degree of reaction of the lithium aluminate and the microsilica was low, suggesting that significant reactions took place only at the surface of the microsilica particles. KW - Laser-induced slip casting KW - Alkali-activated materials KW - Additive manufacturing PY - 2019 DO - https://doi.org/10.29272/cmt.2018.0011 SN - 2612-4882 VL - 1 IS - 2 SP - 138 EP - 144 PB - Techna Group AN - OPUS4-49142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fleck, M. A1 - Tielemann, Christopher A1 - Scheffler, F. A1 - Brauer, D. S. A1 - Müller, Ralf T1 - Surface crystallization of BT0.75S (fresnoite) glass in different atmosphere N2 - Fresnoite glass with excess SiO2 exhibits oriented surface crystallization, in contrast to the stoichiometric glass composition. Recent EBSD studies documented that the crystals in BTS (2BaO-TiO2-xSiO2, x=0-3) can occur in a distinct [101]-orientation perpendicular to the surface and claimed that this orientation is not a result of growth selection. During these previous studies, however, the effect of surface preparation and surrounding atmosphere during the crystallization experiments were not considered. As these parameters may influence crystal orientation, we studied the surface crystallization of a BTS glass (2BaO-TiO2–2.75SiO2) under controlled conditions with the help of light, electron and polarisation microscopy as well as EBSD. Heat treatments for one hour at 840°C of fractured BTS glass surfaces in air resulted in a large number of not-separable surface crystals. This large number of crystals can be caused by dust particles, which act as nucleation agents. As crystal growth velocity could further be influenced by humidity, our experiments are performed in a filtered and dried air atmosphere. The crystal morphology and orientation will be analysed in dependence of the sample preparation and a differing surrounding atmosphere. T2 - 93rd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meeting of French Union for Science and Glass Technology (USTV) CY - Nuremberg, Germany DA - 13.05.2019 KW - BTS KW - Fresnoit KW - Glass ceramic KW - Glass-ceramic KW - Glass PY - 2019 AN - OPUS4-49294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Busch, R. A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Patzig, C. A1 - Höche, T. A1 - Müller, Ralf T1 - Characterization of early crystallization stages in surface-crystallized diopside glass-ceramics N2 - Structure formation in glass-ceramics by means of surface crystallization is a challenging open question and remains elusive to definite answers. In several glass-ceramic systems, oriented crystal layers have been observed at the immediate surface, including diopside and some fresnoite systems. However, it is still open to debate, whether oriented surface crystallization is the result of oriented nucleation or growth selection effects. In the same vein, there is still discussion whether surface nucleation is governed by surface chemistry effects or by defects serving as active nucleation sites. In order to help answer these questions, annealing experiments at 850°C have been performed on a MgO·CaO·2SiO2 glass, leading to the crystallization of diopside at the surface. Different annealing durations and surface treatment protocols (i.a. lapping with diamond slurries between 16 µm and 1 µm grain size) have been applied. Particular focus has been put on earliest crystallization stages, with crystal sizes down to about 200 nm. The resultant microstructure has been analyzed by electron backscatter diffraction (EBSD) and two different kinds of textures have been observed, with the a- or b-axis being perpendicular to the sample surface and the c-axis lying in the sample plane. Even at shortest annealing durations, a clear texture was present in the samples. Additionally, selected samples have been investigated with energy-dispersive x-ray spectroscopy in the scanning transmission electron microscope (STEM-EDX). The diopside crystals have been found to exhibit distinguished submicron structure variations and the glass around the crystals was shown to be depleted of Mg. T2 - 93rd Annual Meeting of the German Society of Glass Technology in Conjunction with the Annual Meeting of French Union for Science and Glass Technology (USTV) CY - Nuremberg, Germany DA - 13.05.2019 KW - Glass KW - Crystallization KW - Diopside KW - EBSD KW - Orientation PY - 2019 AN - OPUS4-49296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Villajos Collado, José Antonio A1 - Jagorel, Noëmie A1 - Reinsch, Stefan T1 - Increasing Exposed Metal Site Accessibility in a Co-MOF-74 Material With Induced Structure-Defects N2 - Metal-organic frameworks (MOFs) are promising nanoporous materials with many practical applications. This owes largely to their remarkable porosity and the presence of specific chemical functionalities, such as exposed metal sites (EMS). The MOF-74 structure is known for exhibiting one of the highest EMS densities among porous materials. Moreover, the inclusion of structural defects has been proposed to enhance activity further. This was previously achieved by mixing the original linker together with a second one, having lower topology. The presence of structural defects was evidenced by the resulting crystalline properties and thermal stability. In this work, different mixtures of tetratopic 2,5-dihydroxyterephthalic acid with up to 60% of the tritopic hydroxyterephtalic acid were used to synthesize crystalline Co-MOF-74-like materials. Materials synthesized from higher proportions than 30% of hydroxyterephtalic acid in the synthesis media collapse upon partial removal of the solvent molecules. This indicates the presence of structural defects and the importance of the solvent molecules in stabilizing the crystalline structures. Electron microscope images show that crystal size reduces with inclusion of hydroxyterephtalic acid as the second linker. The presence of coordinated solvent molecules at the EMS was evaluated by Fourier-transform infrared spectra (FTIR) spectroscopy, so that a higher degree of solvent-exchange was observed during washing for defective structures. Furthermore, TG analysis suggests defective structures exhibit lower desolvation temperatures than the defect-free structures. Finally, N2 adsorption-desorption analyses at −196°C showed an enhanced accessibility of the gas to the inner porosity of the defective structures and therefore, the EMS of the material. All these finding make this pathway interesting to enhance the potential interest of these materials for an industrial application because of both a facilitated activation and a better access to the active sites. KW - MOF-74 KW - Structural defects KW - Mixed-linkers KW - Exposed metal sites KW - Facilitated activation PY - 2019 DO - https://doi.org/10.3389/fmats.2019.00230 VL - 6 SP - 230 PB - Frontiers Media CY - Lausanne AN - OPUS4-49256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waurischk, Tina A1 - Balzer, R. A1 - Kiefer, P. A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. A1 - Deubener, J. T1 - Subcritical crack growth in hydrous silicate glass N2 - Ambient water influences sub-critical crack growth (SCCG) from microscopic surface flaws, leading to stress corrosion at the crack tip. The complex influence of humidity accelerating slow crack propagation (region I) is well studied only for dry commercial NCS glass (< 1000 ppm water). To shed light on this influence, the effect of water is mimicked by studying SCCG water-bearing glasses. For this purpose, water-bearing silicate glasses of 8 wt% total water were synthesized at 0.5 GPa and compared to dry glasses. SCCG was measured in double cantilever beam geometry. For dry glasses, 3 trends in crack velocity vs. stress intensity, KI, curve were found. The slope in region I increases in the order NCS < NBS < BaCS < NZnS < NAS glass. The velocity range of region II, reflecting the transition between corrosion affected and inert crack growth (region III), varies within one order of magnitude among these glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam0.5. For hydrous glasses, it is found that water strongly decreases Tg, form a new sub-Tg internal friction peak caused by molecular water, and makes the glasses more prone to SCCG. The observed trends will be discussed in terms of the effects of Youngs Modulus on the strain energy release rate and energy dissipation related to mechanical glass relaxation phenomena. T2 - 25th International Congress on Glass (ICG2019) CY - Boston, MA, USA DA - 09.06.2019 KW - Internal friction KW - Soda-lime silicate glass KW - Crack growth KW - Water content KW - DCB PY - 2019 AN - OPUS4-49536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kiefer, P. A1 - Deubener, J. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Behrens, H. A1 - Balzer, R. T1 - Density, microhardness and elastic moduli of hydrous soda-lime silicate glasses N2 - The effect of structural water on density, elastic constants and microhardness of water-bearing soda-lime-silica glasses of up to 21.5 mol% total water is studied. T2 - 25th International Congress on Glass (ICG2019) CY - Boston, MA, USA DA - 09.06.2019 KW - Elastic constants KW - Soda-lime-silica glass KW - Water content KW - Microhardness PY - 2019 AN - OPUS4-49537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Charmi, Amir A1 - Falkenberg, Rainer A1 - Skrotzki, Birgit A1 - Ávila, Luis A1 - Sommer, Konstantin T1 - Virtual-lab-based determination of a macroscopic yield function for additively manufactured parts N2 - This work aims for an yield function description of additively manufactured (AM) parts of S316L steel at the continuum-mechanical macro-scale by means of so-called virtual experiments using a crystal plasticity (CP) model at meso-scale. Additively manufactured parts require the consideration of the specific process-related microstructure, which prevents this material to be macroscopically treated as isotropic, because of crystallographic as well as topological textures. EBSD/CT-Scans from in-house additively manufactured specimen extract the unique microstructural topology which is converted to a representative volume element (RVE) with grain structure and crystal orientations. Crystal plasticity model parameters on this RVE are calibrated and validated by means of mechanical testing under different texture angles. From virtual experiments on this RVE, yield loci under various loading conditions are simulated. The scale bridging from meso- to macro-scale is realised by the identification of the simulated yield loci as a modified anisotropic Barlat-type yield model representation. T2 - The First European Conference on Structural Integrity of Additively Manufactured Materials (ESIAM19) CY - Trondheim, Norway DA - 09.09.2019 KW - Virtual experiments KW - Additive manufacturing KW - Anisotropy KW - Crystal plasticity KW - Scale-bridging PY - 2019 AN - OPUS4-49376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trappe, Volker T1 - Fatigue life evaluation of composite wing spar cap materials N2 - An effective method for evaluating the fatigue strength of thick unidirectional composite laminates of wing spar caps has been presented here. A typical width-tapered bending specimen has been developed for a four-point loading set up. Static and fatigue loading was performed at a load ratio R = -1. The complex stress state has been investigated numerically by finite element analysis. Finally, the concept is proven experimentally on specimens made of pultruded fibre rods. The fatigue behavior of the continuously tapered width by water Jet cutting has been compared to discrete tapering via rod-drop. The new method enables a screening of material fatigue behavior caused by normal and shear loading. KW - Fatigue Testing KW - Pultruded fiber rods KW - CFRP KW - Four-point bending test KW - Spar cap design PY - 2019 DO - https://doi.org/10.3139/120.111431 SN - 0025-5300 VL - 61 IS - 12 SP - 1135 EP - 1139 PB - Carl Hanser Verlag CY - München AN - OPUS4-50090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Trappe, Volker A1 - Spancken, D. A1 - Zeiser, A. A1 - Kose, K. A1 - DeMonte, M. T1 - Kurzfaserverstärkte Thermoplaste - Zug-Druck-Schubprüfung mit einem Rohrprobekörper unter schwingender Beanspruchung N2 - Diese DIN SPEC legt ein Verfahren für die Prüfung von unverstärkten und partikel- und kurzfaserverstärkten Kunststoffen mittels Zug-Druck-Schubprüfung fest. Dieses Verfahren findet Anwendung zur Bestimmung der Schwingfestigkeit im Bereich von 103 bis 107 Schwingspielen und der Nachgiebigkeiten unter statischer Belastung sowie der Zugfestigkeit. Alle Beanspruchungen und berechneten Größen sind nennspannungs-basiert. Grundsätzlich besteht bei Rohrprobekörpern auch die Möglichkeit eine Beanspruchung in Längs- und in Umfangsrichtung durch Innendruck zu erzeugen. Dies wird in dieser Spezifikation nicht berücksichtigt, um die Anwendung überschaubar zu halten. Bei Rohrproben mit ausgeprägter Querschnittsverkleinerung (z. B. der Prüfkörper Typ B), entsteht eine Umfangsspannung auch aufgrund einer Zugkraft (siehe Anhang C). Die Umfangsspannung muss dann mittels FEA lokal berechnet werden. Das Verfahren gilt für rohrförmige Prüfkörper deren spezifische Form den Anforderungen der Werkstoff-prüfung und bei Kurzfaserverstärkung einer hohen Vorzugsausrichtung in Probenlängsrichtung genügen. Diese DIN SPEC gilt nicht für endlosfaserverstärkte Kunststoffe. Wegen der vollkommen unterschiedlichen Fertigungstechnologien und der zu erwartenden hohen Prüflasten, sind hier die Anforderungen an die Prüfkörpergeometrie gesondert zu betrachten. Es wird nicht zielführend sein, beide Werkstoffklassen in einer Norm zu behandeln. KW - Kurzfaser-verstärkte Thermoplaste KW - Zug-Druck-Schubprüfung KW - Betriebsfestigkeit KW - Rohrprobekörper PY - 2019 DO - https://doi.org/10.31030/3085076 IS - DIN SPEC 16457:2019-12 SP - 1 EP - 58 PB - Beuth CY - Berlin AN - OPUS4-50092 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -