TY - JOUR A1 - Weber, Kathrin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Stephan-Scherb, Christiane T1 - A µ‐XANES study of the combined oxidation/sulfidation of Fe–Cr model alloys N2 - The precise analysis of cation diffusion profiles through corrosion scales is an important aspect to evaluate corrosion phenomena under multicomponent chemical load, as during high‐temperature corrosion under deposits and salts. The present study shows a comprehensive analysis of cation diffusion profiles by electron microprobe analysis and microbeam X‐ray absorption near edge structure (µ‐XANES) spectroscopy in mixed oxide/sulfide scales grown on Fe–Cr model alloys after exposing them to 0.5% SO2. The results presented here correspond to depth‐dependent phase identification of oxides and sulfides in the corrosion scales by µ‐XANES and the description of oxidation‐state‐dependent diffusion profiles. Scales grown on low‐ and high‐alloyed materials show both a well‐pronounced diffusion profile with a high concentration of Fe3+ at the gas and a high concentration of Fe2+ at the alloy interface. The distribution of the cations within a close‐packed oxide lattice is strongly influencing the lattice diffusion phenomena due to their different oxidation states and therefore different crystal‐field preference energies. This issue is discussed based on the results obtained by µ‐XANES analysis. KW - X-ray absorption spectroscopy KW - Oxidation KW - Sulfidation PY - 2019 DO - https://doi.org/10.1002/maco.201810644 VL - 70 IS - 8 SP - 1360 EP - 1370 PB - Wiley VCH-Verlag AN - OPUS4-47934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prasetiadi, A. E. A1 - Jost, M. A1 - Schulz, Baerbel A1 - Quibeldey, M. A1 - Rabe, Torsten A1 - Follmann, R. A1 - Jakoby, R. T1 - Liquid-crystal-based amplitude tuner and tunable SIW filter fabricated in LTCC technology N2 - Tunable microwave devices will play an important role in future wireless systems, in which high-frequency bands, e.g. millimeter waves, will become promising, due to its huge spectrum availability. At such frequency bands, liquid crystals (LCs) exhibit low microwave loss, which is excellent compared with the other tuning elements. In this paper, LC-based microwave components are fabricated by using low temperature co-fired ceramic technology, allowing the integration of the LC into microwave structures. The first component, the Amplitude tuner, controls the signal’s amplitude by using the interference concept, which exhibits a tunable attenuation range from 11 dB to 30 dB at 30 GHz. The second component is a 3-pole tunable bandpass filter, which is realized by using a substrate integrated waveguide topology, enabling a device with comparatively high-quality factors (Q-factors). The measurement results show Q-factors in the range of 68 to 100 for a frequency tuning of 29.4–30.1 GHz, i.e. a tuning range of 700 MHz, accompanied by an insertion loss 2 dB to 4 dB. KW - Passive components and circuits KW - Filters KW - Microwave technology PY - 2018 DO - https://doi.org/10.1017/S1759078718000600 SN - 1759-0787 VL - 10 IS - 5-6 SP - 674 EP - 681 PB - Cambridge University Press AN - OPUS4-46985 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 - JOUR A1 - Scholz, Philipp A1 - Wachtendorf, Volker A1 - Elert, Anna Maria A1 - Falkenhagen, Jana A1 - Becker, Roland A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Tschiche, Harald A1 - Reinsch, Stefan A1 - Weidner, Steffen ED - Scholz, Philipp T1 - Analytical toolset to characterize polyurethanes after exposure to artificial weathering under systematically varied moisture conditions N2 - Polyether and -ester urethanes (PU) were exposed to artificial weathering at 40 °C and artificial UV radiation in a weathering chamber. In 3 parallel exposures, humidity was varied between dry, humid, and wet conditions. Material alteration was investigated by various analytical techniques like size exclusion chromatography (SEC), liquid chromatography-infrared spectroscopy (LC-FTIR), thermal-desorption gas chromatography-mass spectrometry (TD-GC-MS), fluorescence mapping and dynamic mechanical analysis (DMA). Our results show that depending on the weathering conditions, different degradation effects can be observed. By means of SEC an initial strong decrease of the molar masses and a broadening of the mass distributions was found. After a material dependent time span this was followed by a plateau where molar mass changes were less significant. A minor moisture-dependent degradation effect was only found for polyester PU. Fluorescence measurements on two materials revealed an increase in the luminescence intensity upon weathering process reaching a saturation level after about 500 h. The changes in the optical properties observed after different exposure conditions and times were very similar. The TD-GC-MS data showed the fate of the stabilizers and antioxidant in the course of weathering. LC-FTIR measurements revealed a change in peak intensities and the ratio of urethane and carbonyl bands. KW - Polyurethane KW - Artificial weathering KW - Moisture KW - Crosslinking KW - Degradation PY - 2019 UR - https://www.sciencedirect.com/science/article/pii/S0142941819303708 DO - https://doi.org/10.1016/j.polymertesting.2019.105996 SN - 0142-9418 VL - 78 SP - 105996, 1 EP - 9 PB - Elsevier CY - Amsterdam AN - OPUS4-48625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Reith, F. A1 - Etschmann, B. A1 - Kilburn, M. R. A1 - Brugger, J. T1 - Unravelling the formation histories of placer gold and platinum-group mineral particles from Corrego Bom Successo, Brazil: A window into noble metal cycling N2 - Gold and platinum-group-metals (PGM) are cycled through Earth's environments by interwoven geological, physical, chemical and biological processes leading to the trans/neoformation of metallic particles in placers. The placer deposit at Corrego Bom Successo (CBS, Brazil) is one of the few localities worldwide containing secondary gold- and PGM-particles. Placer gold consists of detrital particles from nearby hydrothermal deposits that were transformed in the surface environment. Processes that have affected these particles include shortdistance transport, chemical de-alloying of the primary Gold silver, and (bio)geochemical dissolution/reprecipitation of Gold leading to the formation of pure, secondary gold and the Dispersion of gold nanoparticles. The latter processes are likely mediated by non-living organic matter (OM) and bacterial biofilms residing on the particles. The biofilms are largely composed of metallophillic β- and γ-Proteobacteria. Abundant mobile gold and platinum nanoparticles were detected in surface waters, suggesting similar mobilities of these metals. Earlier hydrothermal processes have led to the formation of coarsely-crystalline, arborescent dendritic potarite (PdHg). On potarite surfaces, biogeochemical processes have then led to the formation of platinum- and palladium-rich micro-crystalline layers, which make up the botryoidal platinum palladium aggregates. Subsequently potarite was dissolved from the core of many aggregates leaving voids now often filled by secondary anatase (TiO2) containing biophilic elements. The presence of fungal structures associated with the anatase suggests that fungi may have contributed to ist formation. For the first time a primary magmatic PGM-particle comprising a mono-crystalline platinum palladium-alloy with platinum iridium osmium inclusions was described from this locality, finally defining a possible primary source for the PGM mineralisation. In conclusion, the formation of modern-day placer gold- and PGM-particles at CBS began 100s ofmillions of years ago bymagmatic and hydrothermal processes. These provided the metal sources for more recent biogeochemical cycling of PGEs and gold that led to the trans/neoformation of gold- and PGM-particles. KW - Gold KW - Platinum-group-metals KW - Biogeochemical cycling KW - Magmatic and hydrothermal processes KW - Biomineralisation PY - 2019 DO - https://doi.org/10.1016/j.gr.2019.07.003 SN - 1342-937X VL - 76 SP - 246 EP - 259 PB - Elsevier AN - OPUS4-48657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf A1 - Poologasundarampilai, G. A1 - Brauer, D. S. T1 - Sintering and concomitant crystallization of bioactive glasses N2 - The sintering of bioactive glasses allows for the preparation of complex structures, such as three‐dimensional porous scaffolds. Such 3D constructs are particularly interesting for clinical applications of bioactive glasses in bone regeneration, as the scaffolds can act as a guide for in‐growing bone cells, allowing for good Integration with existing and newly formed tissue while the scaffold slowly degrades. Owing to the pronounced tendency of many bioactive glasses to crystallize upon heat treatment, 3D scaffolds have not been much exploited commercially. Here, we investigate the influence of crystallization on the sintering behavior of several bioactive glasses. In a series of mixed‐alkali glasses an increased CaO/alkali metal oxide Ratio improved sintering compared to Bioglass 45S5, where dense sintering was inhibited. Addition of small amounts of calcium fluoride helped to keep melting and sintering temperatures low. Unlike glass 13‐93, these new glasses crystallized during sintering but this did not prevent densification. Variation in bioactive glass particle size allowed for fine‐tuning the microporosity resulting from the sintering process. KW - Bioactive glass KW - Crystallization KW - Scaffolds KW - Sintering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485458 DO - https://doi.org/10.1111/ijag.13477 SN - 2041-1286 VL - 10 IS - 4 SP - 449 EP - 462 PB - Wiley AN - OPUS4-48545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Lima, P. A1 - Diener, S. A1 - Katsikis, N. A1 - Günster, Jens T1 - Additive manufacturing of SiSiC by layerwise slurry deposition and binder jetting (LSD-print) N2 - The current work presents for the first time results on the Additive Manufacturing of SiSiC complex parts based on the Layerwise Slurry Deposition (LSD) process. This technology allows to deposit highly packed powder layers by spreading a ceramic slurry and drying. The capillary forces acting during the process are responsible for the dense powder packing and the good joining between layers. The LSD process can be combined with binder jetting to print 2D cross-sections of an object in each successive layer, thus forming a 3D part. This process is named LSD-print. By LSD-print and silicon infiltration, SiSiC parts with complex geometries and features down to 1mm and an aspect ratio up to 4:1 could be demonstrated. The density and morphology were investigated for a large number of samples. Furthermore, the density and the mechanical properties, measured by ball-on-three-balls method, were in all three building directions close to isostatic pressed references. KW - Silicon Carbide KW - Additive Manufacturing KW - 3D printing KW - Layerwise slurry deposition KW - LSD print PY - 2019 DO - https://doi.org/10.1016/j.jeurceramsoc.2019.05.009 VL - 2019 IS - 39 SP - 3527 EP - 3533 PB - Elsevier Ltd. AN - OPUS4-48546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knauer, S A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Jaeger, P T1 - Contact angle and corrosion of a Water – CO2 system on X70 and S41500 at 278 K and pressures up to 20 MPa N2 - Interfacial properties related to wettability and corrosion in CO2 transport pipelines are experimentally determined by the sessile and the pendant drop methods. The contact angle of a water drop in a compressed CO2 atmosphere is analyzed on an X70 pipeline carbon steel and compared to that on a martensitic steel S41500 to elucidate the effect of corrosion process on active wetting behaviour. The measurements are performed with liquid CO2 at 278 K and pressures ranging from 5 to 20 MPa. The results show that the contact angle (CA) increases with pressure from 132 ° to 143 ° for S41500 and from 117 ° to 137 ° for X70 and decreases with drop age by 20 ° to 24 ° regardless of the pressure and of the fact that corrosion only occurs on X70, which is confirmed by scanning electron microscopy, element mapping and energy dispersive x-ray spectrometry (EDS) analysis. At higher pressure, the contact angles on both materials converge. Further, related properties like density and interfacial tension were determined. CO2 - saturated water has a higher density than pure water: At 5 MPa saturated water reaches a density of 1017 kg⋅m^(-3) and at 20 MPa 1026 kg⋅m^(-3) compared to pure water with a density of 1002 kg⋅m^(-3) and 1009 kg⋅m^(-3), respectively. In this pressure range the IFT drops from 33 mN⋅m^(-1)at 5 MPa to 23 mN⋅m^(-1) at 20 MPa. KW - Carbon capture KW - Utilization, and storage (CCUS) technology KW - Contact angle KW - Wetting KW - Corrosion KW - Condensate KW - Impurities KW - Carbon steel PY - 2019 UR - https://www.sciencedirect.com/science/article/pii/S1750583618309472?dgcid=author DO - https://doi.org/10.1016/j.ijggc.2019.06.021 SN - 1750-5836 SN - 1878-0148 VL - 89 SP - 33 EP - 39 PB - Elsevier, ScienceDirect AN - OPUS4-48601 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 - JOUR A1 - Munzke, Dorit A1 - Kraus, David A1 - Eisermann, René A1 - Kübler, Stefan A1 - Schukar, Marcus A1 - Nagel, Lukas A1 - Hickmann, Stefan A1 - Trappe, Volker T1 - Distributed fiber-optic strain sensing with millimeter spatial resolution for the structural health monitoring of multiaxial loaded GFRP tube specimens N2 - Due to their high strength-to-weight ratio and excellent fatigue resistance, glass fiber reinforced polymers (GFRP) are used as a construction material in a variety of applications including composite high-pressure gas storage vessels. Thus, an early damage detection of the composite material is of great importance. Material degradation can be determined via measuring the distributed strain profile of the GFRP structures. In this article, swept wavelength interferometry based distributed strain sensing (DSS) was applied for structural health monitoring of internal pressure loaded GFRP tube specimens. Measured strain profiles were compared to theoretical calculation considering Classical Lamination Theory. Reliable strain measurements with millimeter resolution were executed even at elongations of up to 3% in the radial direction caused by high internal pressure load. Material fatigue was localized by damaged-induced strain changes during operation, and detected already at 40% of burst pressure. KW - GFRP KW - Swept wavelength interferometry KW - Distributed fiber optic sensing KW - Material degradation KW - Structural health monitoring PY - 2019 DO - https://doi.org/10.1016/j.polymertesting.2019.106085 SN - 0142-9418 VL - 80 SP - 106085 PB - Elsevier Ltd. AN - OPUS4-48950 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 - 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 - Schartel, Bernhard A1 - Humphrey, J.K. A1 - Gibson, A.G. A1 - Hörold, Andreas A1 - Trappe, Volker A1 - Gettwert, V. T1 - Assessing the structural integrity of carbon-fibre sandwich panels in fire: Bench-scale approach N2 - The fire resistance of lightweight sandwich panels (SW) with carbon fibre/epoxy skins and a poly(methacryl imide) (PMI) foam core is investigated in compression under direct application of a severe flame (heat flux=200 kW m−2). A bench-scale test procedure was used, with the sample held vertically. The epoxy decomposition temperature was quickly exceeded, with rapid flash-over and progressive core softening and decomposition. There is a change in failure mode depending on whether the load is greater or less than 50% of the unexposed failure load, or in other words if one or two skins carry the load. At high loads, failure involved both skins with a single clear linear separation across each face. There is an inflection in the failure time relationship in the ∼50% load region, corresponding to the time taken for heat to be transmitted to the rear face, along with a change in the rear skin failure mode from separation to the formation of a plastic hinge. The integrity of the carbon front face, even with the resin burnt out, and the low thermal diffusivity of the core, both play key roles in prolonging rear face integrity, something to be borne in mind for future panel design. Intumescent coatings prolong the period before failure occurs. The ratio of times to failure with and without protection is proposed as a measure of their effectiveness. Apart from insulation properties, their adhesion and stability under severe fire impact play a key role. KW - Carbon fibres KW - Sandwich KW - Structural composites KW - Fracture KW - High-temperature properties KW - Surface treatments PY - 2019 DO - https://doi.org/10.1016/j.compositesb.2018.11.077 SN - 1359-8368 VL - 164 SP - 82 EP - 89 PB - Elsevier AN - OPUS4-46908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zerbst, Uwe A1 - Madia, Mauro A1 - Klinger, Christian A1 - Bettge, Dirk A1 - Murakami, Y. T1 - Defects as a root cause of fatigue failure of metallic components. II: Non-metallic inclusions N2 - This second part of the review on defects as root cause of fatigue failure comprises the origin, the nature and the effects of non-metallic inclusions. Topics addressed are the different kinds of inclusions formed during the manufacturing process, various types of mis-match causing local stresses and, as a consequence, fatigue crack initiation, and effects of characteristics such as size, morphology, localization, spatial distribution and orientation of the defects on the fatigue behavior. Methods for inclusion counting and sizing are discussed along with statistical aspects necessary to be considered when evaluating structural components. KW - Non-metallic inclusions KW - Mis-match KW - Inclusion size KW - Inclusion cluster KW - Statistics PY - 2019 DO - https://doi.org/10.1016/j.engfailanal.2019.01.054 SN - 1350-6307 VL - 98 SP - 228 EP - 239 PB - Elsevier Ltd. AN - OPUS4-47459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chandra, K. A1 - Dörfel, Ilona A1 - Wollschläger, N. A1 - Kranzmann, Axel T1 - Microstructural investigation using advanced TEM techniques of inner ocide layers formed on T92 steel in oxyfuel environment N2 - T92 steel was oxidized at 650 °C for 1000 h in dry and wet oxyfuel gases. The microstructure of inner oxide layer was investigated using scanning transmission electron microscopy and energy dispersive spectroscopy on thin lamellas of oxide cross-sections. The oxides were composed of fine equiaxed grains and separated into Fe-rich and Cr-rich regions. Fe-rich regions were wustite and iron sulphide while Cr-rich regions consisted of Fe-Cr spinel with different stoichiometries. Precipitates of (W,Mo)-rich oxides were formed within the oxide scale and beneath the oxide/alloy interface. Often iron sulphide and (W,Mo)-rich oxide were surrounded by Cr-rich spinel. KW - Steel KW - STEM KW - High temperature corrosion KW - Oxidation KW - Internal oxidation PY - 2019 DO - https://doi.org/10.1016/j.corsci.2018.12.008 SN - 0010-938X SN - 1879-0496 VL - 148 SP - 94 EP - 109 PB - Elsevier AN - OPUS4-47423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falk, Florian A1 - Menneken, M. A1 - Stephan-Scherb, Christiane T1 - Real-time observation of high- temperature gas corrosion in dry and wet SO2-containing atmosphere N2 - Sulfur and water have a fundamental impact on the corrosion rate and potential failure of materials. It is therefore necessary to understand the mechanisms, rates, and potential means of transport, as well as the reactions of these elements with an alloy. This paper investigates the effect of water vapor in the initial stages of SO2 corrosion of an Fe-9Cr-0.5Mn model alloy at 650°C in situ under laboratory conditions using energy-dispersive x-ray diffraction analysis. Two separate experiments were run, one with a 99.5% Ar + 0.5% SO2 atmosphere and one with a 69.5% Ar + 0.5% SO2 + 30% H2O atmosphere. With a wet atmosphere, the alloy formed a scale with decreasing oxygen content towards the scale–alloy interface. Sulfides were identified above and below a (Fe, Cr)3O4 layer in the inner corrosion zone. In contrast to this, the overall scale growth was slower in a dry SO2 atmosphere. KW - Early oxidation KW - Early sulfidation KW - Ferritic steels PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472844 UR - https://link.springer.com/article/10.1007/s11837-019-03335-9#enumeration DO - https://doi.org/10.1007/s11837-019-03335-9 SN - 1047-4838 SN - 1543-1851 VL - 71 SP - 1 EP - 6 PB - Springer CY - New York AN - OPUS4-47284 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 - 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 - JOUR A1 - Thiede, Tobias A1 - Cabeza, S. A1 - Mishurova, Tatiana A1 - Nadammal, N. A1 - Kromm, Arne A1 - Bode, Johannes A1 - Haberland, C. A1 - Bruno, Giovanni T1 - Residual stress in selective laser melted Inconel 718: Influence of the removal from base plate and deposition hatch length N2 - The residual stress distribution in IN718 elongated prisms produced by Selective Laser Melting was studied by means of neutron (bulk) and laboratory X-ray (surface) diffraction. Two deposition hatch lengths were considered. A horizontal plane near the top surface (perpendicular to the building direction) and a vertical plane near the lateral surface (parallel to the building direction) were investigated. Samples both in as-built (AB) condition and removed (RE) from the base plate were characterized. While surface stress fields seem constant for AB condition, X-ray diffraction shows stress gradients along the hatch direction in the RE condition. The stress profiles correlate with the distortion maps obtained by tactile probe measurements. Neutron diffraction shows bulk stress gradients for all principal components along the main sample directions. We correlate the observed stress patterns with the hatch length, i.e. with its effect on temperature gradients and heat flow. The bulk stress gradients partially disappear after removal from the baseplate. KW - Residual stress KW - Additive manufacturing KW - Neutron diffraction KW - Selective laser melting KW - Laboratory X-ray diffraction KW - Coordinate measurement machine KW - IN718 PY - 2018 DO - https://doi.org/10.1520/MPC20170119 SN - 2379-1365 VL - 7 IS - 4 SP - 717 EP - 735 PB - ASTM International CY - USA, West Conshohocken AN - OPUS4-46673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jürgens, Maria A1 - Olbricht, Jürgen A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - Low Cycle Fatigue and Relaxation Performance of Ferritic–Martensitic Grade P92 Steel N2 - Due to their excellent creep resistance and good oxidation resistance, 9–12% Cr ferritic–martensitic stainless steels are widely used as high temperature construction materials in power plants. However, the mutual combination of different loadings (e.g., creep and fatigue), due to a “flexible” operation of power plants, may seriously reduce the lifetimes of the respective components. In the present study, low cycle fatigue (LCF) and relaxation fatigue (RF) tests performed on grade P92 helped to understand the behavior of ferritic–martensitic steels under a combined loading. The softening and lifetime behavior strongly depend on the temperature and total strain range. Especially at small strain amplitudes, the lifetime is seriously reduced when adding a hold time which indicates the importance of considering technically relevant small strains. KW - Ferritic–martensitic steel KW - P92 KW - Low cycle fatigue KW - Relaxation fatigue KW - Cyclic softening PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473905 DO - https://doi.org/10.3390/met9010099 VL - 9 IS - 1 SP - 99, 1 EP - 25 PB - MDPI AN - OPUS4-47390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Bettge, Dirk T1 - On the corrosion mechanism of CO2 transport pipeline steel caused by condensate: Synergistic effects of NO2 and SO2 N2 - To study the effects of condensed acid liquid, hereafter referred to as condensate, on the CO2 transport pipeline steels, gas mixtures containing a varying concentration of H2O, O2, NO2, and SO2, were proposed and resulted in the condensate containing H2SO4 and HNO3 with the pH ranging from 0.5 to 2.5. By exposing the pipeline steel to the synthetic condensate with different concentration of acidic components, the corrosion kinetic is significantly changed. Reaction kinetic was studied using electrochemical methods coupled with water analysis and compared with surface analysis (scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffractometry (XRD)) of corroded coupons. The results showed that, although the condensation of NO2 in the form of HNO3 causes faster general corrosion rate, it is the condensation of SO2 in the form of H2SO4 or the combination of SO2 and NO2 that may cause much more severe problems in the form of localized and pitting corrosions. The resulting corrosion forms were depended on the chemical nature of acids and their concentration at the same investigated pH. The effects of changing CO2 flow rate and renewing condensate on pitting corrosion were further studied. KW - Carbon capture, utilization and storage technology KW - CCUS KW - Corrosion KW - Condensate KW - Electrochemical characterisation KW - Pitting corrosion KW - Impurities KW - Carbon steel PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473685 UR - https://www.mdpi.com/1996-1944/12/3/364 DO - https://doi.org/10.3390/ma12030364 SN - 1996-1944 VL - 12 IS - 3 SP - 364, 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-47368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Böhning, Martin A1 - Niebergall, Ute T1 - Physical and chemical effects of biodiesel storage on high-density polyethylene: Evidence of co-oxidation N2 - The physical and chemical effects of diesel and biodiesel fuels on two high-density polyethylene (PE-HD) types were investigated. Both semi-crystalline PE-HD are common thermoplastic materials for container and storage tank applications. Biodiesel, a composition of unsaturated fatty acid esters from renewable resources, was chosen as it is regarded a possible green alternative to fossil fuels. The study aims at identifying significant differences between biodiesel and conventional diesel fuels based on the differences in the chemical nature of the two. The physical effects of the fuels on the polymer at first comprises the sorption behavior, i.e. kinetics and final equilibrium concentration. Not only are both fuels absorbed by the amorphous phase of the semi-crystalline PE-HD, they also induce a plasticization effect that modifies the molecular mobility and therefore also the characteristic yielding properties, manifest in the obtained stress-strain curves. The chemical effects related to degradation phenomena is investigated by a long-term storage scenario using partially immersed tensile test specimens in diesel and biodiesel. We were able to confirm the proposed co-oxidation mechanism by Richaud et al. for polyethylene-unsaturated penetrant systems on a larger scale based on practical tensile tests. One of the investigated polyethylene grades subjected to tensile drawing showed a significant loss of plastic deformation and the onset of premature failure after 150 days of storage in biodiesel. Further biodiesel storage showed a systematically reduced elongation at break before necking. None of these effects were observed in diesel. Oxidation of fuels and polymer after progressing storage times were analyzed by the evolution of carbonyl species in FT-IR/ATR spectroscopy. KW - Biodiesel KW - Degradation KW - Long-term storage KW - Sorption KW - Diesel PY - 2019 DO - https://doi.org/10.1016/j.polymdegradstab.2019.01.018 SN - 0141-3910 VL - 161 IS - 1 SP - 139 EP - 149 PB - Elsevier CY - Amsterdam AN - OPUS4-47268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gili, A. A1 - Bischoff, B. A1 - Simon, U. A1 - Schmidt, Franziska A1 - Kober, D. A1 - Görke, O. A1 - Bekheet, M. A1 - Gurlo, A. T1 - Ceria-based dual-phase membranes for high-temperature Carbon dioxide separation: Effect of iron doping and pore generation with MgO template N2 - Dual-phase membranes for high-temperature carbon dioxide Separation have emerged as promising technology to mitigate anthropogenic greenhouse gases emissions, especially as a pre- and post-combustion separation technique in coal burning power plants. To implement These membranes industrially, the carbon dioxide permeability must be improved. In this study, Ce_(0.8) Sm_(0.2) O_(2-d) (SDC) and Ce_(0.8)Sm_(0.19)Fe_(0.01)O_(2-d) (FSDC) ceramic powders were used to form the skeleton in dual-Phase membranes. The use of MgO as an environmentally friendly pore generator allows control over the membrane porosity and microstructure in order to compare the effect of the membrane’s ceramic phase. The ceramic powders and the resulting membranes were characterized using ICP-OES, HSM, gravimetric analysis, SEM/EDX, and XRD, and the carbon dioxide flux density was quantified using a high-temperature membrane permeation setup. The carbon dioxide permeability slightly increases with the addition of iron in the FSDC membranes compared to the SDC membranes mainly due to the reported scavenging effect of iron with the siliceous impurities, with an additional potential contribution of an increased crystallite size due to viscous flow sintering. The increased permeability of the FSDC system and the proper microstructure control by MgO can be further extended to optimize carbon dioxide permeability in this membrane system. KW - Samarium doped ceria KW - SDC KW - FSDC KW - CO2 separation membranes KW - Scavenging effect of iron KW - Permeability PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488612 DO - https://doi.org/10.3390/membranes9090108 SN - 2077-0375 VL - 9 IS - 9 SP - 108, 1 EP - 15 PB - MDPI AN - OPUS4-48861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Palantöken, Sinam A1 - Bethke, K. A1 - Zivanovic, V. A1 - Kneipp, Janina A1 - Rademann, Klaus A1 - Kalinka, Gerhard T1 - Cellulose hydrogels physically crosslinked by glycine: Synthesis, characterization, thermal and mechanical properties N2 - Biopolymers are very efficient for significant applications ranging from tissue engineering, biological devices to water purification. There is a tremendous potential value of cellulose because of ist being the most abundant biopolymer on earth, swellability, and functional groups to be modified. A novel, highly efficient route for the fabrication of mechanically stable and natural hydrogels is described in which cellulose and glycine are dissolved in an alkaline solution of NaOH and neutralized in an acidic solution. The dissolving temperature and the glycine amount are essential parameters for the self-assembly of cellulose chains and for Tuning the morphology and the aggregate structures of the resulting hydrogels. Glycine plays the role of a physical crosslinker based on the Information obtained from FTIR and Raman spectra. Among the prepared set of hydrogels, CL5Gly30 hydrogels have the highest capacity to absorb water. The prepared CL5Gly30 gels can absorb up to seven times their dry weight due to its porous 3-D network structure. CL5Gly10 hydrogel exhibits 80% deformation under 21 N force executed. The method developed in this article can contribute to the application of heavy metal adsorption in aqueous solutions for water purification and waste management. KW - Biopolymer KW - Cellulose KW - Hydrogel KW - Natural KW - Synthesis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486845 DO - https://doi.org/10.1002/APP.48380 SN - 1097-4628 SN - 0021-8995 VL - 136 SP - 48380, 1 EP - 11 PB - Wiley CY - USA AN - OPUS4-48684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hilgenberg, Kai A1 - Daum, Werner A1 - Maierhofer, Christiane A1 - Altenburg, Simon A1 - Bruno, Giovanni A1 - Heckel, Thomas A1 - Skrotzki, Birgit A1 - Zerbst, Uwe A1 - Kranzmann, Axel A1 - Bettge, Dirk A1 - Sommer, Konstantin A1 - Seeger, Stefan A1 - Nitsche, Michael A1 - Günster, Jens A1 - Evans, Alexander T1 - Additive manufacturing at the BAM: We focus on Safety N2 - In Germany, the Federal Institute for Materials Research and Testing (BAM) is addressing challenges in the implementation of additive manufacturing on the industrial landscape for safety-critical applications. KW - Process development KW - Additive Manufacturing KW - In-situ Process Monitoring KW - Non-destructive Materials KW - Characterisation KW - Safety KW - Fatigue KW - Environment KW - Standardisation PY - 2019 UR - https://static.asminternational.org/amp/201910/22/ SN - 0882-7958 VL - 177 IS - 7 SP - 22 EP - 26 PB - ASM International CY - Materials Park, OH, USA AN - OPUS4-49780 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 - Kindrachuk, Vitaliy A1 - Titscher, Thomas A1 - Hirthammer, Volker A1 - Unger, Jörg F. ED - Meschke, G. ED - Pichler, B. ED - Rots, J.G. T1 - A continuum damage model for the simulation of concrete under cyclic loading N2 - Lifetime aspects including fatigue failure of concrete structures were traditionally only of minor importance. Because of the growing interest in maxing out the capacities of concrete, its fatigue failure under compression has become an issue. A variety of interacting phenomena such as e.g. loss of prestress, degradation due to chemical reactions or creep and shrinkage influence the fatigue resistance. Failure due to cyclic loads is generally not instantaneous, but characterized by a steady damage accumulation. Therefore, a reliable numerical model to predict the performance of concrete over its lifetime is required, which accurately captures order effects and full three-dimensional stress states. Many constitutive models for concrete are currently available, which are applicable for specific loading regimes, different time scales and different resolution scales. However, a key limitation of those models is that they generally do not address issues related to fatigue on a structural level. Very few models can be found in the literature that reproduce deterioration of concrete under repeated loading-unloading cycles. This is due to the computational effort necessary to explicitly resolve every cycle which exceeds the currently available computational resources. The limitation can only be overcome by the application of multiscale methods in time. The objective of the paper is the development of numerical methods for the simulation of concrete under fatigue loading using temporal multiscale methods. First, a continuum damage model for concrete is developed with a focus on fatigue under compressive stresses [1]. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from static tests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level. Second, a multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach [2]. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed. Finally, the developed methods will be validated and compared to experimental data. [1] Vitaliy Kindrachuk, Marc Thiele, Jörg F. Unger. Constitutive modeling of creep-fatigue interaction for normal strength concrete under compression, International Journal of Fatigue, 78:81-94, 2015 [2] Vitaliy Kindrachuk, Jörg F. Unger. A Fourier transformation-based temporal integration scheme for viscoplastic solids subjected to fatigue deterioration, International Journal of Fatigue, 100:215-228, 2017 T2 - Conference on Computational Modelling of concrete and concrete structures (EURO_C 2018') CY - Bad Hofgastein, Austria DA - 26.02.2018 KW - Fatigue KW - Concrete KW - Damage PY - 2018 SN - 978-1-138-74117-1 DO - https://doi.org/10.1201/9781315182964-19 SP - 155 EP - 164 PB - CRC Press, Taylor & Francis Group CY - Boca Raton, Lodon, New York, Leiden AN - OPUS4-47999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Elert, Anna Maria A1 - Hodoroaba, Vasile-Dan A1 - Agudo Jácome, Leonardo A1 - Altmann, Korinna A1 - Silbernagl, Dorothee A1 - Sturm, Heinz T1 - Short- and long-range mechanical and chemical interphases caused by interaction of Boehmite (γ-AlOOH) with anhydride-cured epoxy resins N2 - Understanding the interaction between boehmite and epoxy and the formation of their interphases with different mechanical and chemical structures is crucial to predict and optimize the properties of epoxy-boehmite nanocomposites. Probing the interfacial properties with atomic force microscopy (AFM)-based methods, especially particle-matrix long-range interactions, is challenging. This is due to size limitations of various analytical methods in resolving nanoparticles and their interphases, the overlap of interphases, and the effect of buried particles that prevent the accurate interphase property measurement. Here, we develop a layered model system in which the epoxy is cured in contact with a thin layer of hydrothermally synthesized boehmite. Different microscopy methods are employed to evaluate the interfacial properties. With intermodulation atomic force microscopy (ImAFM) and amplitude dependence force spectroscopy (ADFS), which contain information about stiffness, electrostatic, and van der Waals forces, a soft interphase was detected between the epoxy and boehmite. Surface potential maps obtained by scanning Kelvin probe microscopy (SKPM) revealed another interphase about one order of magnitude larger than the mechanical interphase. The AFM-infrared spectroscopy (AFM-IR) technique reveals that the soft interphase consists of unreacted curing agent. The long-range electrical interphase is attributed to the chemical alteration of the bulk epoxy and the formation of new absorption bands. KW - Nanocomposites KW - Interphase KW - Intermodulation AFM KW - Electron microscopy KW - Infrared nano AFM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483672 UR - https://www.mdpi.com/2079-4991/9/6/853/htm DO - https://doi.org/10.3390/nano9060853 SN - 2079-4991 VL - 9 IS - 6 SP - 853, 1 EP - 20 PB - MDPI AN - OPUS4-48367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kindrachuk, Vitaliy A1 - Titscher, Thomas A1 - Unger, Jörg F. T1 - A Fourier transformation-based method for gradient-enhanced modeling of fatigue N2 - A key limitation of the most constitutive models that reproduce a Degradation of quasi-brittle materials is that they generally do not address issues related to fatigue. One reason is the huge computational costs to resolve each load cycle on the structural level. The goal of this paper is the development of a temporal Integration scheme, which significantly increases the computational efficiency of the finite element method in comparison to conventional temporal integrations. The essential constituent of the fatigue model is an implicit gradient-enhanced formulation of the damage rate. The evolution of the field variables is computed as amultiscale Fourier series in time.On a microchronological scale attributed to single cycles, the initial boundary value problem is approximated by linear BVPs with respect to the Fourier coefficients. Using the adaptive cycle jump concept, the obtained damage rates are transferred to a coarsermacrochronological scale associated with the duration of material deterioration. The performance of the developedmethod is hence improved due to an efficient numerical treatment of the microchronological problem in combination with the cycle jump technique on the macrochronological scale. Validation examples demonstrate the convergence of the obtained solutions to the reference simulations while significantly reducing the computational costs. KW - Accelerated temporal integration KW - Fourier series KW - Gradient-enhanced fatigue model PY - 2018 DO - https://doi.org/10.1002/nme.5740 SN - 1097-0207 SN - 0029-5981 VL - 114 IS - 2 SP - 196 EP - 214 PB - Wiley AN - OPUS4-44008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Comprehensive study of deuterium-induced effects in in austenitic stainless steel AISI 304L N2 - The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed. To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place. By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules. KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Deuterium KW - Martensite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477540 DO - https://doi.org/10.1016/j.ijhydene.2019.03.058 SN - 0360-3199 SN - 1879-3487 VL - 44 IS - 23 SP - 12228 EP - 12238 PB - Elsevier Ltd. AN - OPUS4-47754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sänger, Johanna C. A1 - Riechers, Birte A1 - Pauw, Brian R. A1 - Maaß, Robert A1 - Günster, Jens T1 - Microplastic response of 2PP‐printed ceramics N2 - AbstractTwo‐photon polymerization (2PP) additive manufacturing (AM) utilizes feedstocks of ceramic nanoparticles of a few nanometers in diameter, enabling the fabrication of highly accurate technical ceramic design with structural details as small as 500 nm. The performance of these materials is expected to differ from conventional AM ceramics, as nanoparticles and three‐dimensional printing at high resolution introduce new microstructural aspects. This study applies 2PP‐AM of yttria‐stabilized zirconia to investigate the mechanical response behavior under compressive load, probing the influence of smallest structural units induced by the line packing during the printing process, design of sintered microblocks, and sintering temperature and thereby microstructure. We find a dissipative mechanical response enhanced by sintering at lower temperatures than conventional. The pursued 2PP‐AM approach yields a microstructured material with an increased number of grain boundaries that proposedly play a major role in facilitating energy dissipation within the here printed ceramic material. This microplastic response is further triggered by the filigree structures induced by hollow line packing at the order of the critical defect size of ceramics. Together, these unique aspects made accessible by the 2PP‐AM approach contribute to a heterogeneous nano‐ and microstructure, and hint toward opportunities for tailoring the mechanical response in future ceramic applications. KW - Additive manufacturing KW - Ceramic KW - Microplasticity PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608897 DO - https://doi.org/10.1111/jace.19849 VL - 107 IS - 10 SP - 6636 EP - 6645 PB - Wiley AN - OPUS4-60889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Schönauer-Kamin, D. A1 - Moos, R. A1 - Reimann, T. A1 - Giovannelli, F. A1 - Rabe, Torsten T1 - Influence of pressure and dwell time on pressure‐assisted sintering of calcium cobaltite N2 - Calcium cobaltite Ca3Co4O9, abbreviated Co349, is a promising thermoelectric material for high‐temperature applications in air. Its anisotropic properties can be assigned to polycrystalline parts by texturing. Tape casting and pressure‐assisted sintering (PAS) are a possible future way for a cost‐effective mass‐production of thermoelectric generators. This study examines the influence of pressure and dwell time during PAS at 900°C of tape‐cast Co349 on texture and thermoelectric properties. Tape casting aligns lentoid Co349. PAS results in a textured Co349 microstructure with the thermoelectrically favorable ab‐direction perpendicular to the pressing direction. By pressure variation during sintering, the microstructure of Co349 can be tailored either toward a maximum figure of merit as required for energy harvesting or toward a maximum power factor as required for energy harvesting. Moderate pressure of 2.5 MPa results in 25% porosity and a textured microstructure with a figure of merit of 0.13 at 700°C, two times higher than the dry‐pressed, pressureless‐sintered reference. A pressure of 7.5 MPa leads to 94% density and a high power factor of 326 µW/mK2 at 800°C, which is 11 times higher than the dry‐pressed reference (30 MPa) from the same powder. KW - Hot pressing KW - Texture KW - Thermoelectric properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515973 DO - https://doi.org/https://doi.org/10.1111/jace.17541 SN - 0002-7820 VL - 104 IS - 2 SP - 917 EP - 927 PB - Wiley Periodicals LLC AN - OPUS4-51597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Mrkwitschka, Paul A1 - Moos, R. A1 - Rabe, Torsten T1 - Glass-ceramic composites as insulation material for thermoelectric oxide multilayer generators N2 - Thermoelectric generators can be used as energy harvesters for sensor applications. Adapting the ceramic multilayer technology, their production can be highly automated. In such multilayer thermoelectric generators, the electrical insulation material, which separates the thermoelectric legs, is crucial for the performance of the device. The insulationmaterial should be adapted to the thermoelectric regarding its averaged coefficient of thermal expansion α and its sintering temperature while maintaining a high resistivity. In this study, starting from theoretical calculations, a glass-ceramic Composite material adapted for multilayer generators fromcalciummanganate and Calcium cobaltite is developed. The material is optimized towards an α of 11 × 10−6 K−1 (20–500◦C), a sintering temperature of 900◦C, and a high resistivity up to 800◦C. Calculated and measured α are in good agreement. The chosen glass-ceramic composite with 45 vol.% quartz has a resistivity of 1 × 107 Ωcm and an open porosity of <3%. Sintered multilayer samples from tape-cast thermoelectric oxides and screen-printed insulation show only small reaction layers. It can be concluded that glass-ceramic composites are a well-suited material class for insulation layers as their physical properties can be tuned by varying glass composition or dispersion phases. KW - Electrical insulators KW - Glass-ceramics KW - Multilayers KW - Thermal expansion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538898 DO - https://doi.org/10.1111/jace.18235 SN - 0002-7820 SP - 1 EP - 10 PB - Wiley Online Library AN - OPUS4-53889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belli, R. A1 - Hurle, K. A1 - Schürrlein, J. A1 - Petschelt, A. A1 - Werbach, K. A1 - Peterlik, H. A1 - Rabe, Torsten A1 - Mieller, Björn A1 - Lohbauer, U. T1 - Relationships between fracture toughness, Y2O3 fraction and phase content in modern dental Yttria-doped zirconias N2 - The relationship between fracture toughness and Yttria content in modern zirconia ceramics was revised. For that purpose, we evaluated here 10 modern Y2O3-stabilized zirconia (YSZ) materials currently used in biomedical applications, namely prosthetic and implant dentistry. The most relevant range between 2-5 mol% Y2O3 was addressed by selecting from conventional opaque 3 mol% YSZ up to more translucent compositions (4-5 mol% YSZs). A technical 2YSZ was used to extend the range of our evaluation. The bulk mol% Y2O3 concentration was measured by X-Ray Fluorescence Spectroscopy. Phase quantification by Rietveld refinement considered two tetragonal phases or an additional cubic phase. A first-account of the fracture toughness (KIc) of the pre-sintered blocks is given, which amounted to 0.4 – 0.7 MPa√m. In the fully-densified state, an inverse power-law behavior was obtained between KIc and bulk mol% Y2O3 content, whether using only our measurements or including literature data, challenging some established relationships. A linear relationship between KIc and the fraction of the transformable t-phase was established within the range of 30–70 vol%. KW - Ceramics KW - Dental KW - Zirconia KW - Fracture toughness KW - X-ray-diffraction KW - Power law PY - 2021 DO - https://doi.org/10.1016/j.jeurceramsoc.2021.08.003 VL - 41 IS - 15 SP - 7771 EP - 7782 PB - Elsevier Ltd. AN - OPUS4-53107 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 - 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 - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Schönauer-Kamin, D. A1 - Moos, R. A1 - Giovanelli, F. A1 - Rabe, Torsten T1 - Influence of pressure assisted sintering and reaction sintering on microstructure and thermoelectric properties of bi-doped and undoped calcium cobaltite N2 - Calcium cobaltite (Ca3Co4O9) is considered as one of the most promising thermoelectric p-type oxides for energy harvesting applications at temperatures above 500 °C. It is challenging to sinter this material as its stability is limited to 920 °C. To facilitate a practicable and scalable production of Ca3Co4O9 for multilayer generators, a systematic study of the influence of powder calcination, Bi-doping, reaction sintering, and pressure-assisted sintering (PAS) on microstructure and thermoelectric properties is presented. Batches of doped, undoped, calcined, and not calcined powders were prepared, tape-cast, and sintered with and without uniaxial pressure at 900 °C. The resulting phase compositions, microstructures and thermoelectric properties were analysed. It is shown that the beneficial effect of Bi-doping observed on pressureless sintered samples cannot be transferred to PAS. Liquid phase formation induces distortions and abnormal grain growth. Although the Seebeck coefficient is increased to 139 µV/K by Bi-doping, the power factor is low due to poor electrical conductivity. The best results were achieved by PAS of calcined powder. The dense and textured microstructure exhibits a high power factor of 326 µW/mK² at 800 °C but adversely high thermal conductivity in the relevant direction. The figure of merit is higher than 0.08 at 700 °C. KW - Ceramics KW - Calcium cobaltite KW - Thermoelectric properties KW - Calcination KW - Pressure-assisted sintering PY - 2019 DO - https://doi.org/10.1063/1.5107476 SN - 0021-8979 VL - 126 IS - 7 SP - 075102-1 EP - 075102-11 PB - AIP Publishing CY - Melville AN - OPUS4-48708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn T1 - Influence of test procedure on dielectric breakdown strength of alumina N2 - Dielectric strength testing of ceramics can be performed with various setups and parameters. Comparisons of results from different sources are often not meaningful, because the results are strongly dependent on the actual testing procedure. The aim of this study is to quantify the influence of voltage ramp rate, electrode size, electrode conditioning, and sample thickness on the measured AC dielectric strength of a commercial alumina. Mean values, Weibull moduli, and failure probabilities determined in standardized short time tests are evaluated and related to withstand voltage tests. Dielectric strength values in the range from 21.6 to 33.2 kV/mm were obtained for the same material using different testing procedures. Short time tests resulted in small standard deviations (< 2 kV/mm) and high Weibull moduli around 30, while withstand tests at voltage levels with low and virtual zero failure probability in short time tests resulted in large scatter of withstand time and Weibull moduli < 1. The strong decrease in Weibull moduli is attributed to progressive damage from partial discharge and depolarization during AC testing. These findings emphasize the necessity of a thorough documentation of testing procedure and highlight the importance of withstand voltage tests for a comprehensive material characterization. KW - Ceramic KW - High-voltage testing KW - Dielectric breakdown KW - Alumina PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483852 DO - https://doi.org/10.1007/s40145-018-0310-4 SN - 2226-4108 SN - 2227-8508 VL - 8 IS - 2 SP - 247 EP - 255 PB - Springer AN - OPUS4-48385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hajian, A. A1 - Konegger, T. A1 - Bielecki, K. A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Schwarz, S. A1 - Zellner, C. A1 - Schmid, U. T1 - Wet chemical porosification with phosphate buffer solutions for permittivity reduction of LTCC substrates N2 - The wireless high-frequency technology requires a robust, cost-effective, and highly integrated substrate technology offering the capability for areas of tailored permittivity. The wet-chemical porosification of low temperature co-fired ceramics (LTCC) substrates offers such an approach by locally embedding air. Porosification of LTCC in both extremely acidic and alkaline media has been investigated in previous works. However, for improving the available knowledge on the porosification of LTCC with H3PO4 as a standard and a widely used etching solution, the impact of solution concentration was systematically investigated and a substantial improvement in the etching performance was achieved. Moreover, in the present study, for the first time, the intermediate pH values, and the impact of pH as a key parameter on the etching process have been investigated. For this purpose, the applicability of phosphate buffer solution (PBS) as a prospective novel etchant mixture for the porosification of a commercially available LTCC tape (Ceramtape GC) was explored. Valuable information about surface morphology, crystalline composition, and the pore structure of the etched LTCCs was gathered employing scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and mercury porosimetry measurements. Based on these findings, the performance of PBS-based etchant systems towards the generation of porous LTCCs combining high depths of porosification with acceptable surface characteristics for subsequent metallization is demonstrated. Based on the obtained results, by application of a 0.2 mol L−1 solution of PBS, the effective relative permittivity of test samples with a thickness of approximately 600 µm and a porosification depth of 186 µm from each side, could be reduced up to 10% of its initial “as fired” value. Also, based on the measurement results and by measuring the depth of porosification, the permittivity of the etched layer was estimated to show a reduction of up to 22% compared to the initial “as fired” value. KW - LTCC KW - Porosification KW - Wet chemical etching KW - Permittivity reduction PY - 2020 DO - https://doi.org/10.1016/j.jallcom.2020.158059 SN - 0925-8388 VL - 863 SP - 158059 PB - Elsevier B.V. AN - OPUS4-51800 LA - eng 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 - 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 - JOUR A1 - Paulus, Daniel A1 - Bresch, Sophie A1 - Moos, Ralf A1 - Schönauer-Kamin, Daniela T1 - Powder aerosol deposited calcium cobaltite as textured P-type thermoelectric material with power factors approaching single crystal values N2 - In this work, the thermoelectric material calcium cobaltite Ca3Co4O9 (CCO), a promising p-type conducting thermoelectric oxide with anisotropic properties, was processed by the powder aerosol deposition method (PAD) to form a dense ceramic CCO film with a thickness in the µm range. The prepared films were characterized regarding their microstructure and thermoelectric properties between room temperature and 900 °C. After heat treatment at 900 °C, the CCO PAD film in-plane shows excellent properties in terms of electrical conductivity (280 S/cm at 900 °C) and Seebeck coefficient (220 µV/K at 900 °C). The calculated power factor in-plane (ab) reaches with 1125 µW/(m K2) 40 % of the single crystal value, surpassing the known-properties of CCO bulk ceramics. Examination of the microstructure shows a strong fiber texture of the film as well as a strong coarsening of the grains during the first heat treatment up to 900 °C. KW - thermoelectrics KW - calcium cobaltite KW - thermoelectric oxide KW - aerosol deposition method (ADM) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606246 DO - https://doi.org/10.1016/j.jeurceramsoc.2024.116717 SN - 0955-2219 VL - 44 IS - 15 SP - 1 EP - 8 PB - Elsevier BV AN - OPUS4-60624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Stargardt, Patrick A1 - Moos, Ralf A1 - Mieller, Björn T1 - Co‐Fired Multilayer Thermoelectric Generators Based on Textured Calcium Cobaltite N2 - Thermoelectric generators are very attractive devices for waste heat energy harvesting as they transform a temperature difference into electrical power. However, commercially available generators show poor power density and limited operation temperatures. Research focuses on high‐temperature materials and innovative generator designs. Finding the optimal design for a given material system is challenging. Here, a theoretical framework is provided that allows appropriate generator design selection based on the particular material properties. For high‐temperature thermoelectric oxides, it can be clearly deduced that unileg multilayer generators have the highest potential for effective energy harvesting. Based on these considerations, prototype unileg multilayer generators from the currently best thermoelectric oxide Ca3Co4O9 are manufactured for the first time by industrially established ceramic multilayer technology. These generators exhibit a power density of 2.2 mW/cm² at a temperature difference of 260 K, matching simulated values and confirming the suitability of the technology. Further design improvements increase the power density by a factor of 22 to facilitate practicable power output at temperature differences as low as 7 K. This work demonstrates that reasonable energy harvesting at elevated temperatures is possible with oxide materials and appropriate multilayer design. KW - Optical and Magnetic Materials KW - Electronic PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596306 DO - https://doi.org/10.1002/aelm.202300636 SN - 2199-160X VL - 10 IS - 3 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-59630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stargardt, Patrick A1 - Bresch, Sophie A1 - Falkenberg, Rainer A1 - Mieller, Björn T1 - Effect of Reaction Layers on Internal Stresses in Co‐Fired Multilayers of Calcium Manganate and Calcium Cobaltite N2 - A widespread recovery of waste heat requires a cost‐effective production of thermoelectric generators. Thermoelectric oxides are predestined for use at high temperatures. For manufacturing reasons, a multilayer generator design will be easily scalable and cost‐effective. To evaluate the potential of ceramic multilayer technology for that purpose, a multilayer of the promising thermoelectric oxides calcium cobaltite (Ca3Co4O9), calcium manganate (CMO, CaMnO3), and glass–ceramic insulation layers is fabricated. Cracks and reaction layers at the interfaces are observed in the microstructure. The compositions of these reaction layers are identified by energy‐dispersive X‐ray spectroscopy and X‐ray diffraction. Mechanical and thermal properties of all layers are compiled from literature or determined by purposeful sample preparation and testing. Based on this data set, the internal stresses in the multilayer after co‐firing are calculated numerically. It is shown that tensile stresses in the range of 50 MPa occur in the CMO layers. The reaction layers have only a minor influence on the level of these residual stresses. Herein, it is proven that the material system is basically suitable for multilayer generator production, but that the co‐firing process and the layer structure must be adapted to improve densification and reduce the tensile stresses in the CMO. KW - Ceramic multilayers KW - Co-firings KW - Internal stresses PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601626 DO - https://doi.org/10.1002/pssa.202300956 SP - 1 EP - 9 PB - Wiley VHC-Verlag AN - OPUS4-60162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, R. A1 - Rabe, Torsten T1 - Lowering the sintering temperature of calcium manganate for thermoelectric applications N2 - This study combines three different approaches to lower the sintering temperature of Sm-doped CaMnO3 to save energy in production and facilitate co-firing with other low-firing oxides or metallization. The surface energy of the powder was increased by fine milling, sintering kinetics were enhanced by additives, and uniaxial pressure during sintering was applied. The shrinkage, density, microstructure, and thermoelectric properties were evaluated. Compared to micro-sized powder, the use of finely ground powder allows us to lower the sintering temperature by 150 K without reduction of the power factor. By screening the effect of various common additives on linear shrinkage of CaMnO3 after sintering at 1100 ○C for 2 h, CuO is identified as the most effective additive. Densification at sintering temperatures below 1000 ○C can be significantly increased by pressure-assisted sintering. The power factor at room temperature of CaMnO3 nano-powder sintered at 1250 ○C was 445 μW/(m K2). Sintering at 1100 ○C reduced the power factor to 130 μW/(m K2) for CaMnO3 nano-powder, while addition of 4 wt.% CuO to the same powder led to ∼290 μW/(m K2). The combination of fine milling, CuO addition, and pressureassisted sintering at 950 ○C resulted in a power factor of ∼130 μW/(m K2). These results show that nano-sized powder and CuO addition are successful and recommendable strategies to produce CaMnO3 with competitive properties at significantly reduced temperatures and dwell times. KW - Sintering additive KW - Liquid phase sintering KW - Pressure assisted sintering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555467 DO - https://doi.org/10.1063/5.0098015 SN - 2158-3226 VL - 12 IS - 8 SP - 1 EP - 9 PB - American Institute of Physics (AIP) CY - New York, NY AN - OPUS4-55546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pereira, Raíssa Monteiro A1 - Lohbauer, Ulrich A1 - Schulbert, Christian A1 - Göken, Mathias A1 - Wurmshuber, Michael A1 - Campos, Tiago Bastos Moreira A1 - Thim, Gilmar Patrocínio A1 - Mieller, Björn A1 - Belli, Renan T1 - Instantiations of Multiscale Kinship in Pressing‐Defect Distributions in Yttria‐Stabilized Zirconias by Powder Partitioning N2 - Modern dry pressing of ceramic powders using spray‐dried granulates cannot avoid the occurrence of defects related to persisting inter‐ and intra‐granulate interstitial voids. These constitute the parent defect size population limiting the application of polycrystalline ceramics in high‐stress conditions. The mitigation of such defects could widen the range of application in technical and biomedical engineering, reduce the safety range for design, and extend the lifetime of components. Herein, the Weibull size‐effect on strength in size‐partitioned Yttria‐stabilized zirconias (YSZ) feedstocks is used to explore the viability of changing the density distribution of granulate sizes as an effective strategy to obtain a denser particle packing that could reduce the size distribution of strength‐limiting pressing defects. In a direct assessment of critical defect size using multiscale strength testing with a dataset of ≈1300 values, the success of such an approach in increasing the strength reliability for small volume components is demonstrated, along with its ultimate failure in altering the defect size distribution in sintered YSZ ceramics across several length scales. Finally, it is shown that granule morphology (spherical or dimpled) fails to affect the defect density and size distribution in YSZ ceramics. KW - Zirconia KW - Strength KW - Toughness KW - Weibull distribution KW - Defect population PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602697 DO - https://doi.org/10.1002/adem.202400139 SN - 1438-1656 SP - 1 EP - 17 PB - Wiley VHC-Verlag AN - OPUS4-60269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn A1 - Valavi, Masood A1 - Caldeira Rêgo, Celso Ricardo T1 - An Automatized Simulation Workflow for Powder Pressing Simulations Using SimStack N2 - Automated computational workflows are a powerful concept that can improve the usability and reproducibility of simulation and data processing approaches. Although used very successfully in bioinformatics, workflow environments in materials science are currently commonly applied in the field of atomistic simulations. This work showcases the integration of a discrete element method (DEM) simulation of powder pressing in the convenient SimStack workflow environment. For this purpose, a Workflow active Node (WaNo) was developed to generate input scripts for the DEM solver using LIGGGHTS Open Source Discrete Element Method Particle Simulation code. Combining different WaNos in the SimStack framework makes it possible to build workflows and loop over different simulation or evaluation conditions. The functionality of the workflows is explained, and the added user value is discussed. The procedure presented here is an example and template for many other simulation methods and issues in materials science and engineering. KW - Simulation workflow KW - Discrete element method PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604791 DO - https://doi.org/10.1002/adem.202400872 SP - 1 EP - 7 PB - Wiley AN - OPUS4-60479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, T. A1 - Kalinka, Gerhard A1 - Mieller, Björn T1 - Manufacturing and deformation behavior of alumina and zirconia helical springs at room temperature N2 - Ceramic helical springs with identical dimensions were produced by hard machining from alumina, alumina toughened zirconia (ATZ), and tetragonal zirconia polycrystals (TZP) stabilized with different oxides. According to the results of the spring constant determination under deformation rates of 3 mm/min, the deformation behavior of all ceramic springs obeys to Hook’s law. However, variation of the deformation rate, tests under constant load, and spring recovery behavior revealed differences in the deformation behavior of alumina, TZP, and ATZ springs. Alumina springs exhibited time-independent deformation in all tests. In contrast, anelastic deformation at room temperature was demonstrated in all springs containing TZP. This deformation is completely reversible over a period of several days. Anelastic behavior is particularly pronounced in Y-TZP springs, whereas Ce-TZP springs exhibit comparatively very low but still reliably detectable anelasticity. Oxygen vacancies in the TZP ceramic are considered the most likely explanation for the anelastic behavior of TZP springs at room temperature. KW - Alumina KW - Creep KW - Elastic properties KW - Zirconia PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571858 DO - https://doi.org/10.1111/jace.19085 SN - 0002-7820 SP - 1 EP - 14 PB - Wiley-Blackwell CY - Oxford [u.a.] AN - OPUS4-57185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Advancing spray granulation by ultrasound atomization N2 - The influence of the atomization technique on the suitability of granules for dry pressing is the focus of the presented investigations. Therefore, destabilized alumina, zirconia, and zirconia toughened alumina (ZTA) slurries were spray dried and the obtained granules were used to fabricate green and finally sintered bodies for evaluation. Granules made in a laboratory spray dryer with a two-fluid nozzle served as a reference. An ultrasonic atomizer was integrated into the same spray dryer and the influence on the granule properties was evaluated. Untapped bulk density, granule size distribution, and flowability are among the evaluated granule-related properties as well as the granule yield which is used as an indicator of the process efficiency. Yield and flowability as most important granule properties are clearly improved when atomization is realized with ultrasound. The investigated sinter body properties include porosity, sinter body density, and biaxial strength and are as well positively affected by switching the atomization technique to ultrasound. Therefore, the Approach to improve the compressibility of granules by ultrasonic atomization, which leads to an improved microstructure, density, and strength of sintered bodies, has proven to be successful for single-component ceramics (alumina and zirconia) as well as for the multicomponent ceramic ZTA. KW - Alumina KW - Granules KW - Spray drying KW - Ultrasound KW - Zirconia KW - Zirconia-toughened alumina PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510696 DO - https://doi.org/10.1111/ijac.13534 VL - 17 IS - 5 SP - 2212 EP - 2219 AN - OPUS4-51069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kindrachuk, Vitaliy ED - Titscher, Thomas ED - Hirthammer, Volker ED - Unger, Jörg F. T1 - A continuum damage model for the simulation of concrete under cyclic loading N2 - A continuum damage model for concrete is developed with a focus on fatigue under compressive stresses. This includes the possibility to model stress redistributions and capture size effects. In contrast to cycle based approaches, where damage is accumulated based on the number of full stress cycles, a strain based approach is developed that can capture cyclic degradation under variable loading cycles including different amplitudes and loading frequencies. The model is designed to represent failure under static loading as a particular case of fatigue failure after a single loading cycle. As a consequence, most of the material parameters can be deduced from statictests. Only a limit set of additional constitutive parameters is required to accurately describe the evolution under fatigue loading. Another advantage of the proposed model is the possibility to directly incorporate other multi-physics effects such as creep and shrinkage or thermal loading on the constitutive level. A multiscale approach in time is presented to enable structural computations of fatigue failure with a reduced computational effort. The damage rate within the short time scale corresponding to a single cycle is computed based on a Fourier based approach. This evolution equation is then solved on the long time scale using different implicit and explicit time integration schemes. Their performance and some limitations for specific loading regimes is discussed. T2 - Euro-C, March 1st 2018 CY - Bad Hofgastein, Austria DA - 26.02.2018 KW - Continnum damage model KW - Simulation of concrete KW - Under cyclic loading PY - 2018 UR - https://euro-c.tuwien.ac.at/home/ SN - 978-1-315-18296-4 SN - 978-1-138-74117-1 VL - 2018 SP - 155 EP - 164 PB - CRC Press, Taylor & Francis Group CY - Leiden, The Netherland AN - OPUS4-48400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -