TY - JOUR A1 - Darvishi Kamachali, Reza T1 - A model for grain boundary thermodynamics JF - RSC Advances N2 - Systematic microstructure design requires reliable thermodynamic descriptions of each and all microstructure elements. While such descriptions are well established for most bulk phases, thermodynamic assessment of microstructure defects is challenging because of their individualistic nature. In this paper, a model is devised for assessing grain boundary thermodynamics based on available bulk thermodynamic data. We propose a continuous relative atomic density field and its spatial gradients to describe the grain boundary region with reference to the homogeneous bulk and derive the grain boundary Gibbs free energy functional. The grain boundary segregation isotherm and phase diagram are computed for a regular binary solid solution, and qualitatively benchmarked for the Pt–Au system. The relationships between the grain boundary's atomic density, excess free volume, and misorientation angle are discussed. Combining the current density-based model with available bulk thermodynamic databases enables constructing databases, phase diagrams, and segregation isotherms for grain boundaries, opening possibilities for studying and designing heterogeneous microstructures. KW - Phase Diagram KW - Thermodynamics KW - Grain boundary PY - 2020 VL - 10 IS - 45 SP - 26728 EP - 26741 AN - OPUS4-51268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, A. T1 - About the reliability of EBSD measurements: Data enhancement JF - Materials Science and Engineering N2 - An extensive set of information about the diffracting volume is carried by EBSD patterns: the crystal lattice, the reciprocal lattice, the crystal structure, the crystal symmetry, the mean periodic number of the diffracting phase, the source point from where it has been projected (projection centre), the crystal orientation, the sample topography (local tilt), the (preparation) quality of defect density of the crystal, and possible pattern overlaps. Some of this information is used regularly in conventional EBSD analyses software while others are still waiting for a more widespread application. Despite the wealth of information available, the accuracy and precision of the data that are presently extracted from conventional EBSD patterns are often well below the actual physical limits. Using a selection of example applications, we will demonstrate the gain in angular resolution possible using relatively low-resolution patterns of approximately 20k pixels in combination with pattern matching (PM) approaches. In this way, fine details in a microstructure can be revealed which would otherwise be hidden in the orientation noise. KW - EBSD KW - Orientation precision KW - Disorientation KW - Grain boundary KW - Phase transformation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521618 DO - https://doi.org/10.1088/1757-899X/891/1/012018 VL - 891 SP - 012018 PB - IOP Science AN - OPUS4-52161 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 JF - International Journal of Applied Ceramic Technology 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 - Stephan-Scherb, Christiane T1 - Applied Crystallography as a tool for a better understanding of Fundamental Questions of high temperature corrosion phenomena N2 - Corrosion Science Meets X-Rays, Neutrons and Electrons. The presentation gives an overview on current research activities applying in-situ X-ray diffraction and spectroscopy for a better understanding of fundamental mechanisms of high temperature corrosion. Additionally the knowledge gain by applying neutron powder diffraction and EBSD analysis is presented. T2 - Joint meeting of german and polish crystallographic association 2020 CY - Wroclaw, Poland DA - 24.02.2020 KW - Corrosion KW - Oxidation KW - In situ KW - Diffraction PY - 2020 AN - OPUS4-50483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cios, G. A1 - Nolze, Gert A1 - Winkelmann, A. A1 - Tokarski, T. A1 - Hielscher, R. A1 - Strzalka, R. A1 - Buganski, I. A1 - Wolny, J. A1 - Bala, P. T1 - Approximant-based orientation determination of quasicrystals using electron backscatter diffraction JF - Ultramicroscopy N2 - Orientation mapping of quasicrystalline materials is demonstrated using crystalline approximant structures in the technique of electron backscatter diffraction (EBSD). The approximant-based orientations are symmetrised according to the rotational point group of the quasicrystal, including the visualization of orientation maps using proper colour keys for quasicrystal symmetries. Alternatively, approximant-based orientation data can also be treated using pseudosymmetry post-processing options in the EBSD system software, which enables basic grain size estimations. Approximant-based orientation analyses are demonstrated for icosahedral and decagonal quasicrystals. KW - EBSD KW - Quasicrystal KW - Approximant KW - Chrystal orientation KW - Data processing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514221 DO - https://doi.org/10.1016/j.ultramic.2020.113093 VL - 218 SP - 113093 PB - Elsevier B.V. AN - OPUS4-51422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila, Luis A1 - Rehmer, Birgit A1 - Graf, B. A1 - Ulbricht, Alexander A1 - Skrotzki, Birgit A1 - Rethmeier, Michael T1 - Assessing the low cycle fatigue behaviour of additively manufactured Ti-6Al-4V: Challenges and first results N2 - The understanding of process-microstructure-property-performance (PMPP) relationships in additive manufacturing (AM) of metals is highly necessary to achieve wide-spread industrial application and replace conventionally manufactured parts, especially regarding safety-relevant applications. To achieve this understanding, reliable data and knowledge regarding material’s microstructure-property relationships (e.g. the role of defects) is needed, since it represents the base for future more targeted process optimizations and more reliable calculations of performance. However, producing reliable material data and assessing the AM material behaviour is not an easy task: big challenges are e.g. the actual lack of standard testing methods for AM materials and the occasional difficulties in finding one-to-one comparable material data for the conventional counterpart. This work aims to contribute to end this lack of reliable material data and knowledge for the low cycle fatigue behaviour of the most used titanium alloy in aerospace applications (Ti-6Al-4V). For this purpose, two sets of test specimens were investigated. The first set was manufactured from cylindrical rods produced by an optimized DED-L process and the second was manufactured from a hot formed round bar. The test specimens were cyclically loaded until failure in the low-cycle-fatigue (LCF) regime. The tests were carried out according to ISO 12106 between 0.3 to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behaviour is described and compared between materials and with literature values based on cyclic deformation curves and strain-based fatigue life curves. Besides, the parameters of Manson-Coffin-Basquin relationship were calculated. The microstructures (initial and after failure) and fracture surfaces were comparative characterized. Thereby, the focus lied on understanding the role of grain morphology and defects on the failure mechanisms and fatigue lifetimes. For this latter characterization, optical microscopy (OM), scanning electron microscopy (SEM) and micro computed tomography (µCT) were used. T2 - 4th International Symposium on Fatigue Design and Material Defects CY - Online meeting DA - 26.05.2020 KW - Ti-6Al-4V KW - Additive manufacturing KW - Low cycle fatigue KW - Micro computed tomography KW - Microstructure PY - 2020 AN - OPUS4-50893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kiefer, P. A1 - Maiwald, M. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf T1 - Automated Analysis of Slow Crack Growth in Hydrous Soda-Lime Silicate Glasses JF - Frontiers in Materials N2 - To explore the impact of ambient and structural water on static fatigue, the initiation and growth of 3279 Vickers induced median radial cracks were automatically recorded and analyzed. We find that humidity is more efficient in initiating cracks and promoting their growth than water, which is dissolved in the glass structure. In particular for slow crack growth (< 3x10-6 m s-1), tests in dry nitrogen showed a considerable decrease in the crack growth exponent with increasing water content of the glasses. On the other hand, if tests were performed in humid air, the crack growth exponent was independent of the water content of the hydrous glasses, while stress intensity decreased slightly. These observations indicate that water promotes the processes at the crack-tip regardless of its origin. However, ambient water is more efficient. KW - Indentation fracture toughness KW - Slow crack growth KW - Automated analysis KW - Hydrous glass KW - Vickers indentation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513085 DO - https://doi.org/10.3389/fmats.2020.00268 VL - 7 SP - 268 AN - OPUS4-51308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maaß, Robert T1 - Beyond Serrated Flow in Bulk Metallic Glasses: What Comes Next? JF - Innovations in high entropy alloys and bulk metallic glasses N2 - This manuscript is based on an oral contribution to the TMS 2020 annual meeting and is dedicated to Prof. Peter Liaw, who for decades has shown great interest in serrated plastic flow. Here we will focus on the case of bulk metallic glasses, and begin with briefly summarizing some aspects of serrated and non-serrated inhomogeneous flow—a phenomenon that has perplexed materials scientists for decades. Four directions of research are identified that emerged out of the desire to fundamentally understand the intermittent inhomogeneous flow response. These research directions gear away from the phenomenological stress–strain behavior but put the underlying shear defect into focus. Unsolved problems and future research topics are discussed. KW - Non-serrated inhomogeneous flow PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513106 DO - https://doi.org/10.1007/s11661-020-05985-w SN - 1073-5623 SP - 1 EP - 11 PB - Springer Nature AN - OPUS4-51310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matz, R. A1 - Rabe, Torsten A1 - Töpfer, J. A1 - Ziesche, S. T1 - Circuit-Board-Integrated Transformers Design and Manufacture JF - Journal of Ceramic Science and Technology N2 - Transformers couple two sections of a circuit by electromagnetic induction. They are widely used to either transform alternating voltage levels or to transmit power or signals across galvanic isolation. Both of these functions are essential for the operation of sensors and controllers. Covering all aspects from idea to circuit performance and from design to manufacture, this paper presents the first comprehensive description of the making of miniaturized, rugged, up-to-100W transformers for embedding into multilayer circuit boards. For circular coils, the well-manageable Ampere-Laplace law is shown to yield reliable designs, predicting correctly the performance of manufactured hardware. This enables fast design without lengthy finite element modelling. In the low-power linear regime, basic relations describe how the device’s characteristics evolve from the material properties and device structure. While scattering Parameters are useful for the analysis of isolated transformers with their intrinsic parasitics, the interaction with the components of the final circuit and the aspects of power and efficiency are addressed by chain matrixes. While these design rules are similar for multilayer boards of different material (like epoxy, Teflon, ceramics), the manufacturing of ceramic board transformers is considered here in detail. Low-temperature-cofired ceramic (LTCC) boards being sintered at 900 °C are particularly suited for harsh environments with chemical or thermal stress as frequently found at sensor positions. The transformer performance usually benefits from or even requires an integrated ceramic core of higher permeability, a ferrite, to shape the magnetic flux. Methods to sinter ferrites inside a dielectric ceramic multilayerandto measure their performance are therefore described in detail.Asthe sintering behaviour of dielectricandmagnetic ceramics differs considerably, their simultaneous sintering is challenging.However, the sintering temperatures of the usefulMnZnand NiZnCu ferrites can be lowered to that of the dielectric material with only moderate loss of permeability by glass additives. Furthermore, thermal mismatch between materials causes catastrophic failure or at least stress and loss of magnetic performance during cooling to room temperature after sintering. This is avoidable by either adjusting the thermal expansion coefficient of the ferrite or by enclosing the ferrite between stressreleasing separation layers.We present the state of the art in materials development according to the first approach as well as fully functional devices made with the second technique. Other applications not directly addressed but well related to this work are characterized by low load resistance in relation to the coil resistance of the transformer. Efficient power transmission then requires that technological solutions are applied to achieve the lowest possible resistive loss inside the coils by an enlarged conductor cross-section. As this is particularly challenging for LTCC boards, a technique is discussed to fabricate conductor traces with a thickness larger than their width. KW - Multilayer ceramic technology KW - LTCC KW - Transformer PY - 2020 DO - https://doi.org/10.4416/JCST2019-00071 SN - 2190-9385 VL - 11 IS - 1 SP - 44 EP - 61 PB - Göller Verlag CY - Baden-Baden AN - OPUS4-50751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karl, D. A1 - Duminy, T. A1 - Lima, P. A1 - Kamutzki, F. A1 - Gili, A. A1 - Zocca, Andrea A1 - Günster, Jens A1 - Gurlo, A. T1 - Clay in situ resource utilization with Mars global simulant slurries for additive manufacturing and traditional shaping of unfired green bodies JF - Acta Astronautica N2 - The wet processing of regolith simulant for clay in situ resource utilization (ISRU) on Mars is presented. The two raw materials from the Mars global simulant family, one without clay (MGS-1) and one with clay - sodium montmorillonite smectite - (MGS-1C) were milled and mixed to produce a simulant with small particle size and reduced clay content (MGS-1C/8). All three simulants and the pure clay raw material were extensively characterized using XRF, synchrotron XRD, gas adsorption and gas pycnometry methods. In a straightforward processing approach, MGS-1C/8 was mixed with water and different dispersant approaches were investigated, all of which gave stable slurries. Particle size distribution, rheology, ion concentration, pH and electrical conductivity of these slurries were characterized. The slurry systems can easily be adapted to fit all typical ceramic shaping routes and here parts of varying complexity from slip casting, throwing on a potter's wheel and additive manufacturing, including material extrusion (robocasting) and binder jetting (powder bed 3D printing) were produced. The unique properties of the sodium montmorillonite clay, which is readily accessible in conjunction with magnesium sulfate on the Martian surface, acted as a natural nanosized binder and produced high strength green bodies (unfired ceramic body) with compressive strength from 3.3 to 7.5 MPa. The most elaborate additive manufacturing technique layerwise slurry deposition (LSD) produced water-resistant green bodies with a compressive strength of 30.8 ± 2.5 MPa by employing a polymeric binder, which is similar or higher than the strength of standard concrete. The unfired green bodies show sufficient strength to be used for remote Habitat building on Mars using additive manufacturing without humans being present. KW - Mars KW - Smectite KW - Clay ISRU KW - MGS-1 regolith simulant KW - 3D printing KW - Additive manufacturing PY - 2020 DO - https://doi.org/10.1016/j.actaastro.2020.04.064 VL - 174 SP - 241 EP - 253 PB - Elsevier Ltd. AN - OPUS4-50870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Bettge, Dirk A1 - Knauer, S. A1 - Yevtushenko, O. T1 - CO2-stream impurities and their effects on corrosion susceptibility of materials to be used in CCUS systems N2 - Carbon Capture Utilization and Storage (CCUS) is a promising technology to reach the target for reduction of CO2 emissions. Crucial points for a sustainable and future-proof CCUS system are reliability and cost efficiency of the whole process chain, including separation of CO2 from the source, compression of CO2, its subsequent transportation to the injection site and injection into geological formations, e.g. aquifers. Recent studies have shown that even at a very low concentration of impurities, condensation of sulfuric and nitric acids in dense phase CO2 are possible and observable. Thus, impact of impure CO2 stream toward corrosion susceptibility of materials to be used in CCUS system need to be considered. In this talk, basing on results achieved from two German long-term projects (COORAL and CLUSTER), the dominating impurities of the CO2 stream and corrosion mechanisms are addressed. Investigations cover the whole CCUS process chain and provide a material recommendation for certain parts. T2 - Corrosion in Low-Carbon Energies - IFPEN-Lyon CY - Online meeting DA - 03.11.2020 KW - Corrosion KW - CCUS KW - Carbon dioxide PY - 2020 AN - OPUS4-51509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Manzoni, Anna Maria A1 - Yesilcicek, Yasemin A1 - Demir, E. A1 - Haas, S. A1 - Glatzel, U. T1 - Combining trace elements for microstructural optimization in the Al10Co25Cr8Fe15Ni36Ti6 compositionally complex alloy N2 - Trace elements W and Hf have different influence on the microstructure and the mechanical properties when added to the Al10Co25Cr8Fe15Ni36Ti6 compositionally complex alloy. The addition of both can thus merge both element’s beneficial influences when combined with the appropriate heat treatment: Hf enhances the cubicity of the γ’ particles in the γ matrix while the W reduces the negative influence of the Heusler phase: this phase can be completely dissolved when W is present in the alloy. T2 - ICHEM 2020 CY - Berlin, Germany DA - 27.09.2020 KW - High entropy alloys KW - Transmission electron microscopy KW - Lattice misfit KW - X-ray diffraction KW - Scanning electron microscopy PY - 2020 AN - OPUS4-51370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Composite materials - focus polymer matrix composites (PMC) N2 - Lecture about polymer matrix composites as part of the first trainings event GW4SHM, properties, production, basic theory, testing. T2 - 1. Training GW4SHM-Project CY - BAM, Berlin, Germany DA - 23.11.2020 KW - Polymer matrix composites KW - Composite testing KW - NDT PY - 2020 AN - OPUS4-51868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph A1 - Yevtushenko, O. A1 - Le, Quynh Hoa A1 - Bettge, Dirk T1 - Corrosive CO2-stream components, challenging for materials to be used in CC(U)S applications N2 - This contribution provides current findings regarding materials susceptibility for CCUS applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2 stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide the following recommendations for certain parts. Commercially available carbon steels are suitable for compression and pipelines as long as moisture content and impurities are limited (water 50 to 100 ppmv, SO2 and NO2 ca. 100 ppmv). Corrosion rates increase with increasing water content (0.2 – 20 mm/a). Condensation of acids and therefore droplet formation is always possible, even at low water contents. A low SO2 content within the CO2-stream might be more important than a low water content. Cr13-steels showed a general susceptibility to shallow pitting and pitting. So, they seem to be not suitable for CCUS applications. Low alloyed steels showed better corrosion behavior (predictable uniform corrosion). For direct contact with saline aquifer fluids only high alloyed steels shall be used. T2 - WCO Webinar on the occasion of Corrosion Awareness Day - Corrosion and Low-Carbon Energies CY - Frankfurt, Germany DA - 24.04.2020 KW - CO2-corrosion KW - CCUS KW - Pipeline KW - Carbon Capture PY - 2020 AN - OPUS4-50699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Kiefer, P. A1 - Deubener, J. A1 - Balzer, R. A1 - Behrens, H. T1 - Crack Growth in Hydrous Soda-Lime Silicate Glass JF - Frontiers in Materials N2 - Stable crack growth was measured for nominal dry and water-bearing (6 wt%) soda-lime silicate glasses in double cantilever beam geometry and combined with DMA studies on the effects of dissolved water on internal friction and glass transition, respectively. In vacuum, a decreased slope of logarithmic crack growth velocity versus stress intensity factor is evident for the hydrous glass in line with an increase of b-relaxation intensity indicating more energy Dissipation during fracture. Further, inert crack growth in hydrous glass is found to be divided into sections of different slope, which indicates different water related crack propagation mechanism. In ambient air, a largely extended region II is observed for the hydrous glass, which indicates that crack growth is more sensitive to ambient water. KW - Internal friction KW - Soda-lime silicate glass KW - Water content KW - Stable crack growth KW - DCB geometry KW - Stress intensity factor PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506829 DO - https://doi.org/10.3389/fmats.2020.00066 VL - 7 SP - Articel 66 AN - OPUS4-50682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis Alexander A1 - Rehmer, Birgit A1 - Schriever, Sina A1 - Ulbricht, Alexander A1 - Agudo Jácome, Leonardo A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Skrotzki, Birgit T1 - Creep and fracture behavior of conventionally and additively manufactured stainless steel 316L N2 - A critical task within the frame of establishing process-structure-property-performance relationships in additive manufacturing (AM) of metals is producing reliable and well-documented material behavior’s data and knowledge regarding the structure-property correlation, including the role of defects. After all, it represents the basis for developing more targeted process optimizations and more reliable predictions of performance in the future. Within this context, this contribution aims to close the actual gap of limited historical data and knowledge concerning the creep behavior of the widely used austenitic stainless steel 316L, manufactured by Laser-Powder-Bed-Fusion (L-PBF). To address this objective, specimens from conventional hot-rolled and AM material were tested under application-relevant conditions according to existing standards for conventional material, and microstructurally characterized before and after failure. The test specimens were machined from single blocks from the AM material. The blocks were manufactured using a standard scan and build-up strategy and were subsequently heat-treated. The creep behavior is described and comparatively assessed based on the creep lifetime and selected creep curves and characteristic values. The effect of defects and microstructure on the material’s behavior is analyzed based on destructive and non-destructive evaluations on selected specimens. The AM material shows shorter creep lives, reaches the secondary creep stage much faster and at a lower strain, and features lower creep ductility compared to its conventional counterpart. The creep damage behavior of the AM material is more microstructure than defect controlled and is characterized by the formation and accumulation of single intergranular damage along the whole volume. Critical features identified are the grain morphology and the grain-boundary as well as the dislocation’s density. Micro-computed tomography (µCT) proves to be an alternative to metallography to analyze the creep damage. T2 - ASTM International Conference on Additive Manufacturing 2020 CY - Online meeting DA - 16.11.2020 KW - 316L KW - Creep behavior KW - Laser powder bed fusion KW - Additive manufacturing KW - Microstructure PY - 2020 AN - OPUS4-51823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Thieme, C. A1 - Rüssel, C. T1 - Crystal growth velocities of a highly anisotropic phase obtained via surface and volume crystallization of barium–strontium–zinc silicate glasses JF - Journal of Materials Science N2 - In the past few years, a new phase, Ba0.5Sr0.5Zn2Si2O7 with negative thermal expansion has been described in the literature. Some excess of SiO2 is necessary to produce glasses from which the Ba0.5Sr0.5Zn2Si2O7 phase can be crystallized. Unfortunately, in such glasses usually surface crystallization occurs; however, the addition of nucleating agents such as trace quantities of platinum or relatively high quantities of ZrO2 is necessary to achieve bulk nucleation. These additional components also affect the crystal growth velocity, which furthermore is different for crystal growth from the surface and in the bulk. In this paper, three different chemical compositions containing different ZrO2 concentrations, where one composition additionally contains 100 ppm platinum, are studied with respect to their crystallization behaviour. Although the compositions do not differ much, the crystallization behaviour and also the Crystal growth velocities are surprisingly different. KW - Glass ceramic KW - Crystal growth velocity KW - Low expansion PY - 2020 DO - https://doi.org/10.1007/s10853-020-04773-6 SN - 0022-2461 VL - 55 SP - 10364 EP - 10374 PB - Springer AN - OPUS4-50853 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghafafian, Carineh A1 - Popiela, Bartosz A1 - Trappe, Volker T1 - Damage Mechanisms of Scarf Joint Repairs for Wind Turbine Rotor Blade Shell Applications N2 - Wind turbine rotor blades, made of fiber reinforced polymers (FRP), often fail before their projected 20-year lifespan, largely due to defects that originate during manufacturing and are propagated by operational fatigue and environmental conditions. The cost-intensive replacement outcomes lead to a high loss of earnings, and are one of the inhibitors of wind turbine production [1]. A potential repair alternative is to locally patch these areas of the blades with adhesively bonded structural repairs. However, the effects of such repair methods of the outer shell region on the structural integrity of the rotor blades are still largely unknown, and are thus investigated in this project. The shell components of rotor blades are made of FRP composite material sandwiching a lightweight core, often a rigid foam or Balsa wood. The repair methods involve replacing the lost load path with a new material that is joined to the parent structure [2]. Repairs in this project focus on the scarf method, which allow for a smoother load distribution across the joint, aiming to study the damage mechanism of glass FRP scarf repairs for wind turbine blade shell applications. Namely, the source and path of the damage initiation and propagation, role of the interface between parent and patch material, and the role of the fiber orientation mismatch at this interface are examined. Biaxial ±45° and 0/90° FRP specimens are produced with the vacuum-assisted resin infusion (VARI) process using E-glass non-crimp fabric. The patch layers are then joined using VARI with a scarf ratio of 1:50, using glass FRP fabric with half the areal weight of the parent side to allow for better drapability. The methods and practices in specimen production are based on common industry practice in rotor blade shell manufacturing and repairs. The specimens are tested under uniaxial tensile load, during which they are periodically monitored for damage onset. A comparison of the ±45° and 0/90° specimens allows for an understanding of the role of a highly mismatching fiber orientation in the transition zone between parent and patch material on the failure mechanism of the scarf joint. Although failure in both orientations begins as delamination at the joint edge, the difference in the mechanisms at play in the two different specimen types leads ultimately to different fracture paths. Namely, in the inter fiber failure mechanism of the ±45° specimens, the higher interlaminar strength compared to the intralaminar strength of the laminate leads to intralaminar failure of the ±45° scarf joint specimens. Alternatively, the competition in the 0/90° specimens lies between the interlaminar strength and fiber failure strength, and here we experience failure primarily across the scarf joint length. The scarf joint in the 0/90° specimens disrupts the continuity of the load-carrying 0° layers, directing the failure path to remain primarily along the scarf joint. Experimental results are compared to finite element analyses of scarf patch repairs on glass FRP sandwich specimens with the same respective layup orientations, where the damage initiation regions are identified and correlated to fiber orientation, serving as a bridge to future work which will experimentally examine the scarf repair patches on sandwich shell specimens. T2 - Joint Event: ICCS23 - 23rd International Conference on Composite Structures & MECHCOMP6 - 6th International Conference on Mechanics of Composites CY - Online meeting DA - 01.09.2020 KW - Wind turbine blade shells KW - Glass fiber reinforced polymers KW - Scarf repairs PY - 2020 AN - OPUS4-51175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilbig, Janka A1 - Borges de Oliveira, F. A1 - Obaton, A.-F. A1 - Schwentenwein, M. A1 - Rübner, Katrin A1 - Günster, Jens T1 - Defect detection in additively manufactured lattices JF - Open Ceramics N2 - This paper investigates fast and inexpensive measurement methods for defect detection in parts produced by Additive Manufacturing (AM) with special focus on lattice parts made of ceramics. By Lithography-based Ceramic Manufacturing, parts were built both without defects and with typical defects intentionally introduced. These defects were investigated and confirmed by industrial X-ray Computed Tomography. Alternative inexpensive methods were applied afterwards on the parts such as weighing, volume determination by Archimedes method and gas permeability measurement. The results showed, that defects resulting in around 20% of change in volume and mass could be separated from parts free of defects by determination of mass or volume. Minor defects were not detectable as they were in the range of process-related fluctuations. Permeability measurement did not allow to safely identify parts with defects. The measurement methods investigated can be easily integrated in AM process chains to support quality control. KW - Additive manufacturing KW - Quality assurance KW - Defect detection KW - Lattices KW - Ceramics PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513547 DO - https://doi.org/10.1016/j.oceram.2020.100020 VL - 3 SP - 100020 PB - Elsevier Ltd. AN - OPUS4-51354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Butz, Adam A1 - Fedelich, Bernard A1 - Rehmer, Birgit A1 - Mäde, L. T1 - Detection and prediction of high temperature fatigue crack growth around notches in polycrystalline nickel base alloy N2 - Im Rahmen eines Vorhabens wurden Methoden zur Reduktion des Versuchsaufwandes bei der Modellerstellung für LCF-Lebensdauervorhersage untersucht. Einige dieser Methoden sind hier kurz vorgestellt. N2 - Methods for reducing the experimental effort necessary for the development of LCF life time prediction models were investigated. Some of these methods are briefly presented here. T2 - 4th International Symposium for Fatigue Design and Material Defects CY - Online meeting DA - 26.05.2020 KW - LCF KW - Mechanistic Modelling KW - Fatigue KW - Data Fusion PY - 2020 AN - OPUS4-50904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kling, I. C. S. A1 - Pauw, Brian Richard A1 - Agudo Jácome, Leonardo A1 - Archanjo, B. S. A1 - Simão, R. A. T1 - Development and characterization of starch film and the incorporation of silver nanoparticles N2 - Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties. T2 - Semana MetalMat & Painal PEMM 2020 CY - Online meeting DA - 23.11.2020 KW - Biofilm KW - Starch KW - Starch nanoparticle KW - Silver nanoparticle PY - 2020 AN - OPUS4-51828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cornelsen Sampaio Kling, I. A1 - Pauw, Brian Richard A1 - Jacome, Leonardo A. A1 - Archanjo, B. S. A1 - Simão, R. A. T1 - Development and characterization of starch film and the incorporation of silver nanoparticles T2 - Semana MetalMat & Painal PEMM 2020 N2 - Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties. T2 - Semana MetalMat & Painal PEMM 2020 CY - Online meeting DA - 23.11.2020 KW - Biofilm KW - Silver nanoparticle KW - Starch KW - Starch nanoparticle PY - 2020 SP - 1 EP - 2 AN - OPUS4-51940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xu, F. A1 - Ren, H. A1 - Zheng, M. A1 - Shao, X. A1 - Dai, T. A1 - Wu, Y. A1 - Tian, L. A1 - Liu, Y. A1 - Liu, B. A1 - Günster, Jens A1 - Liu, Y. A1 - Liu, Y. T1 - Development of biodegradable bioactive glass ceramics by DLP printed containing EPCs/BMSCs for bone tissue engineering of rabbit mandible defects JF - Journal of the Mechanical Behavior of Biomedical Materials N2 - Bioactive glass ceramics have excellent biocompatibility and osteoconductivity; and can form direct chemical bonds with human bones; thus, these ceramic are considered as “Smart” materials. In this study, we develop a new type of bioactive glass ceramic (AP40mod) as a scaffold containing Endothelial progenitor cells (EPCs) and Mesenchymal stem cells (BMSCs) to repair critical-sized bone defects in rabbit mandibles. For in vitro experiments: AP40mod was prepared by Dgital light processing (DLP) system and the optimal ratio of EPCs/BMSCs was screened by analyzing cell proliferation and ALP activity, as well as the influence of genes related to osteogenesis and angiogenesis by direct inoculation into scaffolds. The scaffold showed suitable mechanical properties, with a Bending strength 52.7 MPa and a good biological activity. Additionally, when EPCs/BMSCs ratio were combined at a ratio of 2:1 with AP40mod, the ALP activity, osteogenesis and angiogenesis were significantly increased. For in vivo experiments: application of AP40mod/EPCs/BMSCs (after 7 days of in vitro spin culture) to repair and reconstruct critical-sized mandible defect in rabbit showed that all scaffolds were successfully accurately implanted into the defect area. As revealed by macroscopically and CT at the end of 9 months, defects in the AP40mod/EPCs/BMSCs group were nearly completely covered by normal bone and the degradation rate was 29.9% compared to 20.1% in the AP40mod group by the 3D reconstruction. As revealed by HE and Masson staining analyses, newly formed blood vessels, bone marrow and collagen maturity were significantly increased in the AP40mod/EPCs/BMSCs group compared to those in the AP40mod group. We directly inoculated cells on the novel material to screen for the best inoculation ratio. It is concluded that the AP40mod combination of EPCs/BMSCs is a promising approach for repairing and reconstructing large load bearing bone defect. KW - Three-dimensional Bone tissue engineering KW - Endothelial progenitor cell KW - Bone marrow-derived mesenchymal stem cell KW - Bioactive glass scaffold PY - 2020 DO - https://doi.org/10.1016/j.jmbbm.2019.103532 SN - 1751-6161 VL - 103 SP - 103532 EP - 103532 PB - Elsevier Ltd. AN - OPUS4-50491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kratzig, A. A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Menneken, M. A1 - Bäßler, Ralph T1 - Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature JF - Processes N2 - The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products. KW - Corrosion KW - CCUS KW - In-situ ED-XRD KW - CO2 pipeline transport KW - Oxyfuel KW - Carbon steel KW - Impurities PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506303 DO - https://doi.org/10.3390/pr8040421 SN - 2227-9717 VL - 8 IS - 4 SP - 421-1 EP - 421-19 PB - MDPI CY - Basel AN - OPUS4-50630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, A. A1 - Cios, G. A1 - Tokarski, T. A1 - Nolze, Gert A1 - Hielscher, R. A1 - Koziel, T. T1 - EBSD orientation analysis based on experimental Kikuchi reference patterns JF - Acta Materialia N2 - Orientation determination does not necessarily require complete knowledge of the local atomic arrangement in a crystalline phase. We present a method for microstructural phase discrimination and orientation analysis of phases for which there is only limited crystallographic information available. In this method, experimental Kikuchi diffraction patterns are utilized to generate a self-consistent master reference for use in the technique of Electron Backscatter Diffraction (EBSD). The experimentally derived master data serves as an application-specific reference in EBSD pattern matching approaches. As application examples, we map the locally varying orientations in samples of icosahedral quasicrystals observed in a Ti40Zr40Ni20 alloy, and we analyse AlNiCo decagonal quasicrystals. KW - EBSD KW - Quasicrystal KW - Crystal orientation KW - Pattern matching PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507611 DO - https://doi.org/10.1016/j.actamat.2020.01.053 VL - 188 SP - 376 EP - 385 PB - Elsevier Ltd. AN - OPUS4-50761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane A1 - Schulz, Wencke A1 - Karafiludis, Stephanos A1 - Schneider, Mike A1 - Laplanche, Guillaume T1 - Effect of a mixed atmosphere H2O-O2-SO2 on the oxidation kinetics and phase formation on CrMnFeCoNi and CrCoNi N2 - The high-entropy alloy (HEA) CrMnFeCoNi and the medium-entropy alloy (MEA) CrCoNi with a face-centered cubic (fcc) structure have excellent mechanical properties and are considered for high-temperature applications. Both materials were exposed under several oxidized atmospheres in a wide temperature range/regime. Mn-oxide (Mn3O4, Mn2O3) was mainly formed on the HEA and Cr2O3 on the MEA. The fast diffusion of manganese prevents the formation of a continuous chromia layer on CrMnFeCoNi in Ar-O2, Ar-H2O and Ar-SO2 at 800°C. The Cantor alloy and his ternary subsystem CrCoNi were exposed in Ar-O2-H2O-SO2 at 800°C up to 96 h to clarify their oxidation behavior in a mixed atmosphere. The oxidized samples were analyzed by weight measurement, scanning electron microscopy (SEM), and X-ray diffraction analysis (XRD). It was found that mass gain of all samples increased with increasing exposure time. The oxidation rate of the Cantor alloy is significantly higher than that of the ternary alloy system. T2 - International Conference on High Entropy Materials CY - Berlin, Germany DA - 27.09.2020 KW - High Entropy Alloys KW - Medium Entropy Alloys KW - High temperature corrosion KW - Oxidation KW - Sulfidation PY - 2020 AN - OPUS4-51488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Famy, A. A1 - Agudo Jácome, Leonardo A1 - Schönhals, Andreas T1 - Effect of Silver Nanoparticles on the Dielectric Properties and the Homogeneity of Plasma Poly(acrylic acid) Thin Films JF - The Journal of Physical Chemistry C N2 - For the first time, structure−electrochemical relationships of thin films of a plasma-polymerized acrylic acid/carbon dioxide AA/CO2 (75/25%) copolymer modified by implanted silver nanoparticles are discussed. The pulsed plasma polymerization of AA/CO2 was utilized and adjusted to obtain a maximal amount of COOH Groups forming an almost uncross-linked polymer structure. The prepared polymer layer is rinsed by a silver nitrate solution to impregnate Ag+ ions. This step is followed by its reduction of Ag+ with NaBH4 as a chemical route in comparison to the reduction by sunlight as an ecofriendly photoreduction method. The chemical composition and morphology of the topmost surface layer of the AA/CO2 polymer thin film were investigated by X-ray photoelectron spectroscopy and atomic force microscopy. Moreover, the molecular mobility, conductivity, and thermal stability of the polymer layer were analyzed using broadband dielectric spectroscopy. The dielectric properties of the AA/ CO2 polymer thin film were studied in the presence of Ag+ ions or Ag0. It was found that a cross-linked polymer layer with a smooth surface and high conductivity was obtained in the presence of Ag+/ Ag0. KW - Nanoparticles PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c06712 SN - 1932-7447 VL - 124 IS - 41 SP - 22817 EP - 22826 PB - ACS AN - OPUS4-51468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheuerlein, C. A1 - Andrieux, J. A1 - Michels, M. A1 - Lackner, F. A1 - Chiriac, R. A1 - Hagner, M. A1 - Di Michiel, M. A1 - Meyer, Christian A1 - Toche, F. ED - Foley, C. P. T1 - Effect of the fabrication route on the phase and volume changes during the reaction heat treatment of Nb3Sn superconducting wires JF - Superconductor Science and Technology N2 - Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation. KW - Nb3Sn KW - Microstructure KW - Phase transformations KW - Volume changes KW - X-ray diffraction KW - Differential scanning calorimetry KW - Synchrotron micro-tomography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505128 DO - https://doi.org/10.1088/1361-6668/ab627c VL - 33 IS - 3 SP - 034004 PB - IOP Publishing CY - Bristol (UK) AN - OPUS4-50512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Theissen, W. A1 - Agudo Jácome, Leonardo T1 - Effect of the heat treatment in the microstructure of a refractory chemically complex alloy N2 - A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community. The AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. After a two-stage heat treatment, this rCCA morphologically resembles the typical a two-phase microstructure of the latter. The objective of this work consists in determining the effect of the two stages of the heat treatment on the microstructure of the AlMo0.5NbTa0.5TiZr alloy to eventually improve it in terms of homogeneity and porosity. T2 - Third International Conference on High Entropy Materials (2020) CY - Berlin, Germany DA - 27.09.2020 KW - Annealing KW - Hot isostatic pressing KW - Refractory chemically complex alloy KW - Microstructure PY - 2020 AN - OPUS4-53386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Weber, Kathrin A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Elucidation of orientation relations between Fe-Cr alloys and corrosionproducts after high temperature SO2 corrosion JF - Corrosion Science N2 - The early stages of corrosion of Fe-Cr-model alloys (2 and 9 % Cr) were investigated after exposure at 650 °C in0.5 % SO2containing gas by electron backscattered diffraction (EBSD) and transmission electron microscopy(TEM). The impact of the grain orientation of the base alloy on the orientation relations of the corrosion productsis presented. After 2 min–5 min exposure the formation of a multi-layered corrosion zone was discovered. Aclear orientation relationship between ferrite and the (Fe,Cr)3O4 spinel could be demonstrated. The obtainedresults show the importance of the grain orientation on oxidation resistance. KW - Iron KW - TEM KW - SEM KW - High temperature corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508911 DO - https://doi.org/10.1016/j.corsci.2020.108809 VL - 174 SP - 1 EP - 11 PB - Elsevier AN - OPUS4-50891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Schilling, Markus T1 - Environmental Stress Cracking (ESC) and Slow Crack Growth (SCG) of PE-HD induced by external fluids N2 - High-density polyethylene (PE-HD) is widely used as a packaging material. Typical applications are pipes and containers for storage and transport of dangerous goods. For these applications, the understanding of the craze-crack damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC) is of importance. Since these mechanisms are considered to be the major causes of failure, their understanding is essential for inspection and release of those materials. A well-established test method for the assessment of these damage mechanisms is the full-notch creep test (FNCT). It is used in this study for a detailed investigation of crack propagation phenomena in PE-HD container materials under the influence of different fluids such as air, water and aqueous detergent solutions (Arkopal N 100) as well as biodiesel and diesel. Based on the results of the FNCT, a classification scheme of different fluids is proposed, which allows for an assignment of the respective damage mechanisms. Hereby, it is differentiated between (i) inert, (ii) purely surface-active and (iii) additionally sorptive, bulk-active fluids with respect to SCG. If the test fluid changes the intrinsic properties (at the surface or in the bulk), the damage mechanism is addressed to ESC behavior. In FNCT investigations, stress, temperature and specimen geometry were varied systematically. In addition to the time to failure as common measure for the resistance of a PE-HD type against crack propagation, specimen elongation was considered in detail. Several imaging techniques were applied for fracture surface analysis of specimens tested in FNCT to gain novel information on SCG and ESC behavior. From height profiles obtained by laser scanning microscopy (LSM) and information on surface structures from scanning electron microscopy (SEM), indicators for the differentiation of the crack propagation mechanisms could be derived. Based on the LSM data, an algorithm for the distinction between ductile shear deformation and brittle crack growth as dominating failure mechanism was developed. Imaging techniques were also used for determination of crack propagation rates, which were related to time-resolved FNCT elongation data. From the time-resolved determination of crack lengths of partly damaged FNCT specimens, an increasing length of craze zone with a progressively propagating crack was revealed for the first time. This relation of crack and craze zones was specified by fracture mechanical considerations. N2 - Polyethylen hoher Dichte (PE-HD) wird als Werkstoff für Rohre und Behälter für den Transport und zur Lagerung von Gefahrgütern verwendet. Für die Beurteilung und technische Freigabe dieser Materialien ist das Verständnis der beiden Schädigungsmechanismen „langsames Risswachstum“ (engl.: „slow crack growth“, SCG) und „umgebungsbedingter Spannungsriss“ (engl.: „environmental stress cracking“, ESC) essentiell. Eine etablierte Prüfmethode zur Bewertung dieser Schädigungsmechanismen ist der Full-Notch Creep Test (FNCT), der in dieser Arbeit zur systematischen Untersuchung des Risswachstums in PE-HD Behältermaterialien unter Einwirkung von Luft, Wasser und wässrigen Netzmittellösungen (Arkopal N 100) sowie Biodiesel und Diesel verwendet wird. Aus den Ergebnissen des FNCT wird ein Klassifikationsschema für Fluide vorgeschlagen, welches ebenfalls eine Zuordnung zu den Schädigungsmechanismen erlaubt. Hierbei wird in (i) inerte, (ii) rein oberflächen-aktive und (iii) zusätzliche sorptive, volumen-aktive Fluide hinsichtlich des langsamen Risswachstums (SCG) unterschieden. Wenn ein Fluid lokal die intrinsischen Materialeigenschaften des Polymers verändert, wird der Schädigungsmechanismus dem umgebungsbedingten Spannungsriss (ESC) zugeordnet. Bei den FNCT-Untersuchungen wurden die mechanische Spannung, die Temperatur und die Prüfkörpergeometrie systematisch variiert. Zusätzlich zur Standzeit wurde die Prüfkörperdehnung zeitabhängig erfasst. Aus einer erweiterten Bruchflächenanalyse konnten neuartige Informationen über SCG und ESC erhalten werden. Hierzu wurden verschiedene Bildgebungsverfahren verwendet. Insbesondere wurden mit Laserscanningmikroskopie (LSM) Höhenprofile und mit Rasterelektronenmikroskopie (REM) Oberflächeninformationen zur Charakterisierung der Rissfortschrittsmechanismen erhalten. Auf Basis der LSM wurde unter Zuhilfenahme von Höhenprofildaten ein Algorithmus zur Unterscheidung zwischen duktiler Scherverformung und sprödem Risswachstum als dominierende Schädigungsmechanismen entwickelt. Die aus den bildgebenden Verfahren ermittelten Rissfortschrittsraten konnten mit den Daten der während des FNCT erfassten Dehnung der Prüfkörper in Beziehung gesetzt werden. Weiterhin wurde mithilfe von zeitaufgelösten Risslängendaten erstmals eine direkte Korrelation der Risslänge zu vorgeschädigten, fibrillierten Bereichen (Crazes) im PE-HD Prüfkörper während des FNCT nachgewiesen. Demnach vergrößert sich die Craze-Länge linear mit zunehmender Risslänge. Dieser Zusammenhang zwischen Riss- und Craze-Längen wurde auf mathematisch, bruchmechanischer Grundlage bestätigt. KW - High-density polyethylene (PE-HD) KW - Full-Notch Creep Test (FNCT) KW - Slow crack growth (SCG) KW - Environmental Stress Cracking (ESC) KW - Biodiesel KW - Diesel KW - Crack propagation analysis KW - Fracture Surface Analysis KW - Test Improvement KW - Imaging PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:tuda-tuprints-115443 DO - https://doi.org/10.25534/tuprints-00011544 SP - 1 EP - 212 CY - Darmstadt AN - OPUS4-50941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Niebergall, Ute A1 - Wachtendorf, Volker A1 - Böhning, Martin T1 - Evaluation of UV-induced embrittlement of PE-HD by Charpy impact test JF - Journal of Applied Polymer Science N2 - The impact fracture behavior of two common high-density polyethylene grades for container applications were intensively studied by the instrumented Charpy impact test after well-defined exposure to UV-irradiation. Individual stages of the impact event, such as crack initiation and crack propagation energy as well as maximum impact load, were investigated from the recorded load–deflection curves. UV-induced material property changes were further investigated by infrared spectroscopy, differential scanning calorimetry, and dynamic-mechanical analysis as well as density measurements. Based on the results of the Charpy impact test, three indicators were identified to describe the extend of photooxidation on high-density polyethylene: (a) a reduced Charpy impact strength—at least to half of its initial value for a distinctly brittle impact fracture, (b) a marked decrease in the crack propagation contribution to the impact strength, and (c) an increase of the brittle features of the fracture surface. KW - Degradation KW - Mechanical properties KW - Packaging KW - Polyolefins KW - Polyethylene PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509130 DO - https://doi.org/10.1002/APP.49069 SN - 0021-8995 VL - 137 IS - 36 SP - 49069 PB - Wiley AN - OPUS4-50913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and rotor blades of wind turbines are basically made of fiber reinforced plastics (FRP). Their failure heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in-situ non-destructive testing techniques. Here, we report on in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics (CFRP) due to inter fiber failure. An in-house designed compact-tensile testing machine with a load range up to 15 kN was integrated into the beam path. Since conventional radiographs do not reveal sufficient contrast to distinct cracks due to inter fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging technique (DEI) is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. In the laboratory, scanning X-ray refraction topography of CFRP has been applied long before but it comes along with several disadvantages: the long total measuring time hampers real time (in-situ) measurements and the required small beam size hinders end-to-end imaging. The introduced technique overcomes both drawbacks. Imaging and tensile test rig are run unsynchronized at the greatest possible frame rate (0.7 s-1 at 28.8 µm pixel size) and smallest possible strain rate (5.5∙10-4 s-1). For 0°/90° non-crimped fabrics (ncf) the first inter fiber cracks occurred at 380 MPa (strain 0.7 %). Prior to failure at about 760 MPa (strain 2.0 %) we observe the evolution of a nearly equidistant 1 mm grid of cracks running across the entire sample in the fully damaged state before total failure. T2 - 41st Risø International Symposium on Materials Science - Materials and Design for Next Generation Wind Turbine Blades CY - Online meeting DA - 07.09.2020 KW - X-ray refraction KW - Diffraction Enhanced Imaging KW - Carbon Fiber Reinforced Plastics KW - In situ tensile test KW - Crack evolution PY - 2020 AN - OPUS4-51223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging JF - IOP conference series: Materials science and engineering N2 - Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. Imaging and the tensile test are run at the highest possible frame rate (0.7 s-1 ) and the lowest possible strain rate (5.5∙10-4 s -1 ). For 0°/90° non-crimp fabrics, the first inter-fiber cracks occur at 380 MPa (strain 0.8 %). Prior to failure at about 760 MPa (strain 2.0 %), we observe the evolution of nearly equidistant (1 mm distance) cracks running across the entire sample in the fully damaged state. KW - X-ray refraction KW - Diffraction Enhanced Imaging KW - Carbon Fiber Reinforced Plastics KW - In situ tensile test KW - Crack evolution PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515060 DO - https://doi.org/10.1088/1757-899X/942/1/012035 SN - 1757-8981 SN - 1757-899X VL - 942 SP - 012035-1 EP - 012035-9 PB - IOP publishing CY - Bristol, UK AN - OPUS4-51506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in-situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. T2 - 12th BESSY@HZB User Meeting 2020 CY - Online meeting DA - 10.12.2020 KW - Carbon Fiber Reinforced Plastics KW - Crack evolution KW - Diffraction Enhanced Imaging KW - In situ tensile test KW - X-ray refraction PY - 2020 AN - OPUS4-51802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüders, C. A1 - Kalinka, Gerhard A1 - Li, Wei A1 - Sinapius, M. A1 - Wille, T. T1 - Experimental and numerical multiscale approach to thermally cycled FRP JF - Composite Structures N2 - Due to the different thermal expansion of the constituent materials, cyclic thermal loading of FRP induces alternating stresses in the material at two scales: at the micro scale (level of fibre–matrix-interaction) and at the macro scale (level of the multidirectional laminate). Especially the micro scale effect is not comprehensively investigated yet. Additionally, computational investigations mostly neglect this effect due to the homogenous modelling of the composite material. As this effect is assumed to significantly contribute to the fatigue of FRP at thermal loads, the present paper suggests an experimental and numerical multiscale approach including Experiments at the different involved material scales to separately observe the effects acting at these scales. The approach also includes numerical modelling for each scale to complement the knowledge gained from the Experiments and to create a basis for the consideration of the micro effect even in macroscopic fatigue models treating homogeneous modelled composites. The main focus of the contribution is to bring the overall Approach up for discussion, rather than to present the multiscale modelling details. KW - Fatigue KW - Thermal cycling KW - Fibre reinforced plastic KW - Cryogenic KW - Carbon Fibre KW - Epoxy Resin PY - 2020 DO - https://doi.org/10.1016/j.compstruct.2020.112303 SN - 0263-8223 VL - 244 SP - 112303 PB - Elsevier Ltd. CY - Niederlande AN - OPUS4-50844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Kuchenbecker, Petra A1 - Würth, Christian A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan T1 - Fine iron oxide nanoparticles as a candidate reference material for reliable measurement of particle size N2 - Background, Motivation and Objective Nanomaterials are at the core of some of the 21st century’s most promising technologies. In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important. Furthermore, the European Commission has taken measures via the REACH Regulations to control the classification of nanomaterials. REACH Annexes which entered into force in January 2020 require manufacturers to register nanomaterials that are traded in larger quantities (at least 1 ton). Every powder or dispersion where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as a nanomaterial. This creates a need for both industrial manufacturers and research and analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is working on developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution, but also targeting other key parameters such as shape, structure (including porosity) and functional properties. Thus, candidate materials are considered to complement the already available spherical and monodisperse silica, Au and polystyrene reference nanoparticles, e.g. iron oxide and titanium oxide, with an average atomic number between those of silica and gold. Particularly for the imaging by electron microscopies, new nanoparticles of well-defined size in the range of 10 nm are decisive for the accurate particle segmentation by setting precise thresholds. Statement of Contribution/Methods Synthesis: Highly monodisperse iron oxide nanoparticles can be synthesized in large quantities by thermal decomposition of iron oleate or iron acetylacetonate precursors in high boiling solvents such as octadecene or dioctyl ether in the presence of oleic acid and oleylamine as capping agents. Scanning Electron Microscope: An SEM of type Supra 40 from Zeiss has been used including the dedicated measurement mode transmission in SEM (STEM-in-SEM) with a superior material contrast for the nanoparticle analysis. The software package ImageJ has been used for the analysis of the STEM-in-SEM images and to determine the particle size distribution. Dynamic Light scattering (DLS): Particles in suspension were measured in comparison by means of Zetasizer Nano (Malvern Panalytical; cumulants analysis) and NanoFlex (Microtrac; frequency power spectrum). Results/Discussion In this study iron oxide nanoparticles synthesized at BAM and pre-characterized by DLS, SEM (including the transmission mode STEM-in-SEM) are presented. The particles are spherical and highly monodisperse with sizes slightly larger than 10 nm. T2 - Nanosafe 2020 CY - Online meeting DA - 16.11.2020 KW - Reference nanomaterials KW - Imaging techniques KW - Size and size distribution KW - Reliable characterization KW - Iron oxide nanoparticles PY - 2020 AN - OPUS4-51767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sänger, Johanna Christiane A1 - Pauw, Brian Richard A1 - Sturm, Heinz A1 - Günster, Jens T1 - First time additively manufactured advanced ceramics by using two-photon polymerization for powder processing JF - Open Ceramics N2 - Methods and materials are presented here, which enable the manufacturing of fine structures using a 3D-printing method known as two-photon polymerization (2PP). As traditional photolithography methods for structuring ceramic slurries do not function with 2PP, due to light scattering on ceramic particles, a novel water-based photoresist with high ceramic loading of extremely well dispersed ceramic nano particles was developed. This photoresist is basically a ceramic slurry containing a photocurable agent and a photoinitiator to be crosslinkable with the 780 nm wavelength femtosecond laser light source of the 2PP machine. It is demonstrated that it is possible to gain a highly transparent and low viscous slurry suitable for 2PP processing. This work shows the development of the slurry, first printing results and the post-printing processes required to form three dimensional ceramic microstructures consisting of alumina toughened zirconia (ATZ). KW - 3D-printing KW - Two-photon polymerization KW - 2PP KW - Ceramic nano particles KW - Slurry KW - Alumina toughened zirconia KW - ATZ KW - Additive manufacturing KW - SchwarzP cells KW - Nano-ceramic-additive-manufacturing photoresin KW - NanoCAM PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517441 DO - https://doi.org/10.1016/j.oceram.2020.100040 VL - 4 SP - 100040 PB - Elsevier Ltd. AN - OPUS4-51744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Focused ion beam techniques beyond the ordinary - Methodological developments within ADVENT N2 - This poster presents the focused ion beam preparation methodologies developed within the framework of the EU funded EURAMET project ADVENT (Advanced Energy-Saving Technology). It summarises the key breakthroughs achieved for various in situ investigation techniques, e.g. in situ experiments at the Synchrotron facility BESSY II (IR-SNOM and XRS), TEM and SMM instrumentation. The created experimental devices from diverse thin-film semiconductor materials paved the way to dynamic structural studies bearing the potential to determine nanoscale correlations between strain and electric fields and, moreover, for the fundamental development of new in situ capabilities. N2 - Dieses Poster zeigt die FIB Präparationstechniquen, die im Rahmen des EU-finanzierten EURAMET-Projekts ADVENT (Advanced Energy Saving Technology) entwickelt wurden. Es fasst die wichtigsten Errungenschaften zusammen, die für verschiedene in situ Untersuchungstechniken erzielt wurden, z.B. situ-Experimente in dem Synchrotronring BESSY II (IR-SNOM und XRS), in situ TEM Experimente und für die SMM Technik. Die experimentellen Probenstrukturen, die aus verschiedenen Dünnschicht-Halbleitermaterialien erzeugt wurden, ebneten den Weg für dynamische Strukturstudien, die das Potenzial haben, nanoskalige Korrelationen zwischen Dehnung und elektrischen Feldern zu bestimmen und darüber hinaus neue in situ Messmethoden zu entwickeln. T2 - Final Meeting CY - Online Meeting DA - 30.06.2020 KW - FIB KW - Sample preparation KW - In situ KW - TEM KW - AFM PY - 2020 AN - OPUS4-51606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chinellato, Fabio A1 - Wilbig, Janka A1 - Al-Sabbagh, Dominik A1 - Colombo, P. A1 - Günster, Jens T1 - Gas flow assisted powder deposition for enhanced flowability of fine powders: 3D printing of alpha-tricalcium phosphate JF - Open Ceramics N2 - The possibility of creating patient-specific individual implants makes Additive Manufacturing technologies of special interest for the medical sector. For substitution of bone defects, powder based Additive Manufacturing by Binder Jetting is a suitable method to produce complex scaffold-like structures made of bioceramics with easily adapted geometries and controlled porosity. The process inherent residual porosity in the printed part, even though desired as it supports bone ingrowth, also leads to limited mechanical strength. Currently, bioceramic scaffolds made by Binder Jetting feature suitable biocompatible and biodegradable properties, while a sufficient mechanical stability is rather challenging. The purpose of this work is to apply the gas flow assisted powder deposition introduced in 2014 by Zocca et al., to the powder bed during printing of bioceramic tablets and scaffolds using α-TCP powder as feedstock. This enables exploiting the advantages of an increased powder bed density, thereby improving the mechanical properties of the printed parts. KW - Additive Manufacturing KW - Binder Jetting KW - Gas flow assisted powder deposition KW - Alpha-tricalcium phosphate KW - Scaffold PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510138 DO - https://doi.org/10.1016/j.oceram.2020.100003 SN - 2666-5395 VL - 1 SP - 100003 PB - Elsevier Ltd. AN - OPUS4-51013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, L. A1 - Darvishi Kamachali, Reza A1 - Li, Z. A1 - Zhang, Z. T1 - Grain boundary energy effect on grain boundary segregation in an equiatomic high-entropy alloy JF - Physical Review Materials N2 - Grain boundary (GB) Segregation has a substantial effect on the microstructure evolution and properties of polycrystalline alloys. The mechanism of nanoscale segregation at the various GBs in multicomponent alloys is of great challenge to reveal and remains elusive so far. To address this issue, we studied the GB segregation in a representative equiatomic FeMnNiCoCr high-entropy alloy (HEA) aged at 450 °C. By combining transmission Kikuchi diffraction, atom probe tomography analysis and a density-based thermodynamics modeling, we uncover the nanoscale segregation behavior at a series of well-characterized GBs of different characters. No segregation occurs at coherent twin boundaries; only slight nanoscale segregation of Ni takes place at the low-angle GBs and vicinal \Sigma 29b coincidence site lattice GBs. Ni and Mn show cosegregation of high levels at the general high-angle GBs with a strong depletion in Fe, Cr, and Co. Our density-based thermodynamic model reveals that the highly negative energy of mixing Ni and Mn is the main driving force for nanoscale cosegregation to the GBs. This is further assisted by the opposite segregation of Ni and Cr atoms with a positive enthalpy of mixing. It is also found that GBs of higher interfacial energy, possessing lower atomic densities (higher disorder and free volume), show higher segregation levels. By clarifying the origins of GB segregations in the FeMnNiCoCr HEA, the current work provides fundamental ideas on nanoscale segregation at crystal defects in multicomponent alloys. KW - Thermodynamics KW - High-Entropy Alloys KW - Grain Boundary Segregation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508827 DO - https://doi.org/10.1103/PhysRevMaterials.4.053603 VL - 4 IS - 5 SP - 053603 PB - American Physical Society AN - OPUS4-50882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Wencke A1 - Stephan-Scherb, Christiane A1 - Laplanche, Guillaume T1 - High temperature corrosion phenomena of HEAs and MEAs N2 - High- and medium-entropy alloys (HEAs and MEAs) constitute a new class of materials. Those with a face-centered cubic (fcc) structure from the Cr-Mn-Fe-Co-Ni system have excellent mechanical properties and are considered for high-temperature applications since diffusion in these alloys was reported to be sluggish. However, their corrosion resistance at high temperatures must still be evaluated to further qualify them for such kinds of applications. Various groups studied the oxidation behavior of HEAs and MEAs under (dry) laboratory and artificial air as well as CO2/CO mixtures in different temperature ranges. CrCoNi exhibits the best corrosion resistance at 800 °C due to the formation of a protective Cr2O3 layer. The matrix below the oxide scale was reported to be correspondingly depleted in Cr. It was further shown that the addition of Mn and Fe to CrCoNi changes the phase composition of the oxide scale at 800 °C. A Mn2O3 layer was grown during oxidation on CrMnCoNi and CrMnFeCoNi and a Cr2O3 scale was formed at the matrix/oxide scale interface. Beneath these oxide layers, Mn- and Cr-depleted zones were detected. These phase morphologies demonstrate the inward diffusion of oxygen and outward diffusion of Cr and Mn resulting in the formation of Cr2O3 and Mn2O3. In the present study, the corrosion resistance of CrMnFeCoNi and CrCoNi were confirmed and additionally characterized under further oxidizing atmospheres at 800 °C including Ar-2 Vol.% O2, Ar-2 Vol.% H20, and Ar-2 Vol.% SO2 mixtures. T2 - Symposium on Advanced Mechanical and Microstructural Characterization of High-Entropy Alloys CY - Ruhr-Universität Bochum, Germany DA - 03.02.2020 KW - Mn3O4 KW - High-entropy alloy KW - Medium-entropy alloy KW - High-temperature corrosion KW - Chromia PY - 2020 AN - OPUS4-50984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Manzoni, Anna Maria A1 - Glatzel, U. ED - Buschow, K.H.J. ED - Flemings, M.C. ED - Kramer, E.J. ED - Veyssière, P. ED - Cahn, R.W. ED - Ilschner, B. ED - Mahajan, S. T1 - High-Entropy Alloys: Balancing Strength and Ductility at Room Temperature T2 - Encyclopedia of Materials: Science and Technology N2 - A new race for high performance structural materials has started since the discovery of high entropy alloys at the beginning of the 21st century. The possible combination of several elements in an, until then, unknown composition space opened the ground for discovering new materials. Solid solution strengthening remains the most prominent mechanisms that is active in this family of materials, but it is supported by all other strengthening mechanism on the path to better and better performing materials. Chemical, thermal and mechanical approaches are combined to optimize these alloys. Optimum performances can be reached by using a high number of different strengthening mechanisms, induced both by composition and processing. The most prominent with composition induced mechanism is precipitation hardening, and on the processing side it is cold working such as cold-rolling, torsion or extrusion. The contribution uses tensile test data at room temperature solely for comparison – high temperature and cryogenic data are omitted because it would lead beyond the scope of this manuscript. KW - High entropy alloys KW - Compositionally complex alloys PY - 2020 DO - https://doi.org/10.1016/B978-0-12-803581-8.11774-6 PB - Elsevier Inc. AN - OPUS4-50575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Schulz, Wencke A1 - Schneider, M. A1 - Karafiludis, Stephanos A1 - Laplanche, G. T1 - High-Temperature Oxidation in Dry and Humid Atmospheres of the Equiatomic CrMnFeCoNi and CrCoNi High- and Medium-Entropy Alloys JF - Oxidation of Metals N2 - Surface degradation phenomena of two model equiatomic alloys from the CrMnFeCoNi alloy system were investigated in 2% O2 and 10% H2O (pO2 = 0.02 and 10−7 atm, respectively) at 800 °C for times up to 96 h. The crystallographic structures, morphologies, and chemical compositions of the corrosion layers developing on CrMnFeCoNi and CrCoNi were comparatively analyzed by mass gain analysis, X-ray diffraction, and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy and electron backscatter diffraction. The oxidation resistance of CrMnFeCoNi is relatively poor due to the fast growth of porous Mnoxide(s). CrCoNi forms an external chromia layer that is dense and continuous in a dry 2% O2 atmosphere. This layer buckles and spalls off after exposure to 10% H2O atmosphere. Beneath the chromia layer, a Cr-depleted zone forms in the CrCoNi alloy in both environments. As the oxide scale spalls off in the H2O-containing atmosphere, a secondary chromia layer was observed and correspondingly enlarges the Cr-depleted zone. In contrast, as the chromia layer remains without significant spallation when CrCoNi is exposed to a dry oxidizing atmosphere, the region depleted in Cr is narrower. KW - High temperature oxidation KW - High entropy alloys KW - Medium entropy alloys KW - CrMnFeCoNi KW - CrCoNi KW - Mn-oxides PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517859 DO - https://doi.org/10.1007/s11085-020-10014-7 SN - 0030-770X VL - 95 IS - 1-2 SP - 105 EP - 133 PB - Springer AN - OPUS4-51785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Welter, T. A1 - Müller, Ralf A1 - Deubener, J. A1 - Marzok, Ulrich A1 - Reinsch, Stefan T1 - Hydrogen Permeation Through Glass JF - Frontiers in Materials N2 - Physical storage of gaseous hydrogen under high-pressure in glassy micro-containers such as spheres and capillaries is a promising concept for enhancing safety and the volumetric capacity of mobile hydrogen storage systems. As very low permeation through the container wall is required for storage of compressed hydrogen, development of glasses of minimal hydrogen permeability is needed. For this purpose, one has to understand better the dependence of hydrogen permeability on glass structure. The paper points out that minimizing the accessible free volume is as one strategy to minimize hydrogen permeability. Based on previously measured and comprehensive literature data, it is shown that permeation is independently controlled by ionic porosity and network modifier content. Thus, ionic porosity in modified and fully polymerized networks can be decreased equally to the lowest hydrogen permeability among the glasses under study. Applying this concept, a drop of up to 30,000 with respect to the permeation of hydrogen molecules through silica glass is attainable. KW - Ionic porosity KW - hydrogen storage KW - Glass KW - Permeability KW - Solubility KW - Diffusivity PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513927 DO - https://doi.org/10.3389/fmats.2019.00342 VL - 6 SP - Article 342 AN - OPUS4-51392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, Ralf A1 - Rabe, Torsten T1 - Improved thermoelectric properties of CaMnO3 and Ca3Co4O9 by increasing the driving force for sintering N2 - Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (Ca3Co4O9, p-type) and calcium manganate (CaMnO3, n-type) are two of the most promising oxide thermoelectric materials. The performance of these materials is evaluated by the power factor PF = S²∙σ and the figure of merit ZT = (PF ∙ T) / κ, demanding high Seebeck coefficient S, high electrical conductivity σ and low thermal conductivity κ. The latter two are increasing with increasing relative sinter density. According to theory, the relative density of ceramics can be improved by increasing the driving force for sintering. This study investigates different approaches to increase the driving force for sintering of Ca3Co4O9 and CaMnO3 to improve densities and thermoelectric properties. The following approaches were applied: minimizing the energy input during powder synthesis by calcination, fine milling of the powder, using reaction-sintering without a powder synthesis step, and adding a transient liquid phase by sinter additives. All different approaches led to an increased densification and thus higher electrical conductivity and higher PF. Thermal conductivity increased as well but not to the same extent. E.g. reaction-sintering increased the densification of Ca3Co4O9 (p-type) and CaMnO3 (n-type). Consequently, the electrical conductivities improved by about 100 % for both oxides leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Although the thermal conductivity increased as well by 8 %, the figures of merit (ZT) were significantly higher compared to conventionally sintered bars. The addition of 4 wt% CuO as a sinter additive to CaMnO3 lowers the sinter temperature from above 1250 °C to below 1100 °C and increases the relative density. Due to the increased density, both electrical conductivity and PF increased by more than 200 % even though the sintering temperature was 150 K lower. T2 - Electroceramics XVII CY - Online meeting DA - 24.08.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives PY - 2020 AN - OPUS4-51163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koclega, Damian A1 - Radziszewska, A. A1 - Dymek, S. A1 - Morgiel, J. A1 - Maj, L. A1 - Kranzmann, Axel T1 - Improvement of Corrosion Resistance of 13CrMo4-5 Steel by Ni-Based Laser Cladding Coatings JF - Journal of Materials Engineering and Performance N2 - The 13CrMo4-5 ferritic steel is commonly used in power plants, due to its favorable mechanical properties. According to EN 10028-2, this steel can be used at temperatures up to 570°C because of its creep behavior. The inefficient corrosion resistance limits the application of this steel to lower temperatures depending on the gas temperature and slag formation. Therefore, the application of a highly resistant Ni-based coating is proposed to extend the corrosion resistance of elements made of ferritic steel. The corrosion test was performed in an environment containing a mixture of gases, like O2, COx, and SOx, and deposited ashes with elements, e.g., Na, Cl, Ca, Si, C, Fe, and Al. The exposure time was, respectively, 240 h, 1000 h and 4500 h at a temperature of 600°C. The oxide scale formed on the 13CrMo4-5 steel was significantly thicker than on the IN686 coating. The microstructure and chemical and phase compositions of the oxide scale were investigated using light optical microscopy together with scanning and transmission electron microscopy techniques. Energy dispersive x-ray analyses were performed when appropriate. KW - Aggressive environments KW - Corrosion resistance KW - High - temperature KW - Inconel 686 KW - Laser cladding PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514289 DO - https://doi.org/10.1007/s11665-020-04867-x SN - 1059-9495 VL - 29 IS - 6 SP - 3702 EP - 3713 PB - Springer AN - OPUS4-51428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Hänninen, H. A1 - Böllinghaus, Thomas T1 - In-situ ToF-SIMS analyses of deuterium re-distribution in austenitic steel AISI 304L under mechanical load JF - Scientific Reports N2 - Hydrocarbons fuel our economy. Furthermore, intermediate goods and consumer products are often hydrocarbon-based. Beside all the progress they made possible, hydrogen-containing substances can have severe detrimental effects on materials exposed to them. Hydrogen-assisted failure of iron alloys has been recognised more than a century ago. The present study aims to providing further insight into the degradation of the austenitic stainless steel AISI 304L (EN 1.4307) exposed to hydrogen. To this end, samples were electrochemically charged with the hydrogen isotope deuterium (2H, D) and analysed by scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). It was found that deuterium caused a phase transformation from the original γ austenite into ε- and α’-martensite. Despite their low solubility for hydrogen, viz. deuterium, the newly formed phases showed high deuterium concentration which was attributed to the increased density of traps. Information about the behaviour of deuterium in the material subjected to external mechanical load was gathered. A four-point-bending device was developed for this purpose. This allowed to analyse in-situ pre-charged samples in the ToF-SIMS during the application of external mechanical load. The results indicate a movement of deuterium towards the regions of highest stress. KW - ToF-SIMS KW - Hydrogen KW - Deuterium KW - AISI 304L KW - EBSD PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505142 DO - https://doi.org/10.1038/s41598-020-60370-2 VL - 10 IS - 1 SP - 3611 PB - Nature AN - OPUS4-50514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taketa, I. A1 - Kalinka, Gerhard A1 - Gorbatikh, L. A1 - Lomov, S. A1 - Verpoest, I. T1 - Influence of cooling rate on the properties of carbon fiber unidirectional composites with polypropylene, polyamide 6, and polyphenylene sulfide matrices JF - Advanced composite materials N2 - The longitudinal and transverse strength of three unidirectional thermoplastic prepreg systems: carbon fiber/polypropylene (CF/PP), polyamide 6 (CF/PA6), and polyphenylene sulfide (CF/PPS) are studied and analytical formulas are proposed for the estimation of matrix and fiber/matrix interface properties from composites properties. Since the matrices are semi-crystalline thermoplastics, the influence of cooling rate on the strength is statistically evaluated. While the 0° tensile strength is found to be independent of the cooling rate, the 90° tensile strength is strongly influenced by the matrix type and cooling rate. The matrix modulus increases as the cooling rate is decreased; the degree of crystallinity also increases. The matrix residual stress, interfacial shear strength, and mode II interlaminar fracture toughness are also found to depend on the cooling rate, with the trends different for different matrices. KW - Matrix residual stress KW - Thermoplastic prepreg KW - Unidirectional composites KW - Cooling rate KW - Interfacial strength PY - 2020 DO - https://doi.org/10.1080/09243046.2019.1651083 SN - 0924-3046 SN - 1568-5519 N1 - Die originale japanische Version des Artikels erschien in: Journal of the Japan Society for Composite Materials, Jg. 44, Nr. 4 (2018), S. 123-128. - The original Japanese version of the article was published in: Journal of the Japan Society for Composite Materials, vol. 44, no. 4 (2018), pp. 123-128. VL - 29 IS - 1 SP - 101 EP - 113 PB - Taylor & Francis CY - London AN - OPUS4-45433 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 JF - Journal of the American Ceramic Society 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 -