TY - CONF A1 - Heuser, Lina A1 - Agudo Jácome, Leonardo A1 - Pauli, Jutta A1 - Nofz, Marianne A1 - Müller, Ralf T1 - Silver in low-melting alkali zinc borate glasses N2 - Ein aktuelles Forschungsziel ist die Substitution von Bleioxid in niedrig schmelzenden Gläsern z.B. zur Anwendung in Silber-Metallisationspasten. Im Fokus steht hier die Untersuchung der Silberdiffusion in Alkali-Zink-Boratgläsern (X2O-ZnO-B2O3, X = Li, Na, K, Rb). Zudem wird der Redoxzustand des Silbers (Ag) und somit die Art der diffundierenden Silberspezies bestimmt. Hierzu wurde eine metallische Silberschicht mittels Sputterns auf Glaswürfel aufgebracht. Die Wärmebehandlung erfolgte nahe der Glasübergangstemperatur bei 470 °C über 2 h unter Luft und Stickstoffatmosphäre. Die Schichtdicke der Silberbeschichtung betrug 1.8 µm nach der Wärmebehandlung, gemessen mittels Weißlicht-Interferometer. Die Silberdiffusionsprofile wurden mittels Sekundär-Neutral-Teilchen-Massenspektrometrie gemessen. Die Diffusionskoeffizienten des Silbers liegen in der Größenordnung von ~10-14 cm2/s und unterscheiden sich nur gering in Abhängigkeit des Alkali-Ions im Glas. Mittels Fluoreszenz-Spektroskopie ließen sich gelöste Ag+-Ionen und [Agm]n+-Cluster nach der Wärmebehandlung unterscheiden. Zusätzlich konnten ausgeschiedene metallische Silber-Partikel im Natrium-enthaltenden Glas mittels Transmissionselektronenmikroskopie beobachtet werden. Diese haben einen mittleren Durchmesser von ~6 nm. N2 - Substitution of lead oxide in low-melting glasses, e.g., for application in silver metallization pastes, is a current research goal. This work is focused on the investigation of silver diffusion in alkali zinc borate glasses (X2O-ZnO-B2O3, X = Li, Na, K, Rb). In addition, the redox state of silver (Ag) and thus the type of diffusing silver species were studied. For this purpose, a metallic silver coating was applied on glass cubes by means of sputtering. Heat treatment of the samples was performed close to the glass transition temperatures at 470 °C for 2 h under air and nitrogen atmosphere. Coating thickness was 1.8 µm after heat treatment, measured by a white light interferometer. Silver diffusion profiles were measured by means of secondary neutral mass spectrometry. The silver diffusion coefficients are in the range of ~10-14 cm2/s and indicate no significant differences depending on the type of alkali ions in the glass. Dissolved Ag+-ions and [Agm]n+-clusters in the glasses were differentiated using fluorescence spectroscopy. Precipitated metallic silver particles in the sodium containing glass were observed by means of transmission electron microcopy. Their mean particle diameter was ~6 nm. T2 - Living Glass Surfaces XI - Year of Glass CY - Ilmenau, Germany DA - 14.09.2022 KW - Alkali zinc borate glasses KW - Silver diffusion KW - Transmission electron microscopy KW - Fluorescence spectroscopy KW - Silver cluster PY - 2022 AN - OPUS4-55736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander A1 - Sprengel, Maximilian A1 - Ulbricht, Alexander A1 - Kromm, Arne A1 - Werner, Tiago A1 - Sommer, Konstantin A1 - Kelleher, Joe A1 - Mishurova, Tatiana A1 - Serrano Munoz, Itziar A1 - Fritsch, Tobias A1 - Schröder, Jakob A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - Manufacturing a safer world: Diffraction based residual stress analysis for metal additive manufacturing N2 - Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, with associated potential gains in performance and efficiency. However, high magnitude residual stresses (RS) are often a product of the rapid thermal cycles typical of the layerwise process. Therefore, a deep understanding of the formation of RS, the influence of process parameters on their magnitude and the impact on mechanical performance is crucial for widespread application. The experimental characterisation of these RS is essential for safety related engineering application and supports the development of reliable numerical models. Diffraction-based methods for RS analysis using neutrons and high energy X-rays enable non-destructive spatially resolved characterisation of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys as a function of process parameters. In addition, the challenges posed by the textured and hierarchical microstructures of LPBF materials on diffraction-based RS analysis in AM materials will be discussed. This will include the question of the d0 reference lattice spacing and the appropriate choice of the diffraction elastic constants (DECs) to calculate the level of RS in LPBF manufactured alloys. T2 - 11th INternational Conference on Residual Stress (ICRS11) CY - Online meeting DA - 28.03.2021 KW - Residual stress analysis KW - Neutron diffraction KW - X-ray diffraction KW - Additive manufacturing KW - Laser powder bed fusion KW - AGIL PY - 2022 AN - OPUS4-54676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Roohbakhshan, Farshad A1 - Nolze, Gert A1 - Fedelich, Bernard A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Cyclic Operation Performance of 9-12% Cr Ferritic-Martensitic Steels. Part 2: Microstructural Evolution during Cyclic Loading and its Representation in a Physically-based Micromechanical Model N2 - The current trend towards cyclic, “flexible” operation of fossil-fueled power plants constitutes a major issue regarding lifetime and operational safety of the respective installations and their components, as was outlined in our complementary contribution (Part 1). The present contribution reports on the investigation of the microstructure evolution in cyclically loaded ferritic-martensitic steels and its representation in a physically-based micromechanical model. For this purpose, specimens of P92 steel grade from the mechanical test programme outlined in our companion contribution (Part 1) were analyzed by scanning electron microscopy (SEM), including backscattered diffraction (EBSD) mapping, and transmission electron microscopy (TEM). A novel method was implemented to improve angular resolution of EBSD scans. Additionally, a correlative microscopy approach was developed and used to correlate EBSD and TEM measurements on the same locations of thick regions of electron transparent specimens. By applying these techniques, a detailed quantitative microstructure description of the as-received material condition, namely in terms of subgrain morphology and dislocation density/distributions, was established. Comparisons of as-received and cyclically loaded conditions from tests interrupted at different stages of lifetime indicate a rapid redistribution of in-grain dislocations with a strong interaction between mobile dislocations and low angle grain boundaries (LABs). The proposed micromechanical model is formulated in a viscoplastic self-consistent (VPSC) scheme, which is a mean-field approach that allows us to include the crystal details at the level of slip systems while avoiding the considerable computational costs of full-field approaches (such as the classical crystal plasticity finite element analysis). Being physically-based, the model uses dislocation densities and includes the interaction between dislocations, e.g. annihilation of mobile dislocations, and evolution of microstructure, e.g. the grain coarsening. Particularly, the constitutive laws for dislocation evolution and interaction between dislocations and low angle boundaries are calibrated based on two-dimensional discrete dislocation dynamic (2D DDD) simulations, which are performed at a micro-/meso-scale. The results of the beforementioned EBSD experiments are considered as a direct input, involving e.g. the amount of geometrically necessary dislocations, average misorientations and grain characteristics. T2 - 45th MPA-Seminar 2019 CY - Leinfelden-Echterdingen, Germany DA - 01.10.2019 KW - Tempered martensite ferritic steel KW - Dislocation KW - Electron backscattered diffraction (EBSD) KW - Transmission electron microscopy (TEM) KW - Microstructure KW - Physically based material model PY - 2019 AN - OPUS4-49346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - López-Galilea, I. A1 - Ruttert, B. A1 - Theisen, W. A1 - Agudo Jácome, Leonardo T1 - Microstructural characterization of the AlMo 0.5 NbTa 0.5 ZrTi refractory complex concentrated 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 and the AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. The AlMo0.5NbTa0.5TiZr rCCA was studied by SEM, EDX, EBSD and TEM, showing the presence of a nanoscopic basket-wave structure inside the grains, with two BCC phases. Additionally, thermodynamic calculations on the AlMo0.5NbTa0.5TiZr alloy were done with two different proprietary databases that anticipate two BCC-disordered phases with distinct constitutions as well as an HCP phase. T2 - Symposium on Advanced Mechanical and Microstructural Characterization of High-Entropy Alloys CY - Bochum, Germany DA - 03.02.2020 KW - High Entropy Alloy KW - EBSD KW - Microstructure Characterization PY - 2020 AN - OPUS4-50729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Manzoni, Anna Maria A1 - Mohring, W. A1 - Karafiludis, Stephanos A1 - Schneider, M. A1 - Haas, S. A1 - Hagen, S. A1 - Glatzel, U. A1 - Laplanche, G. A1 - Stephan-Scherb, C. T1 - Corrosion in the Co-Cr-Fe-Ni high entropy alloy family N2 - While a lage amount of research on high entropy alloys is oriented towards mechanical properties and the microstructural improvement it is also necessary to keep an eye on the environment that potential application materials will be submitted to. The Co-Cr-Fe-Ni based high entropy family has shown great potential over the years of high entropy research and some candidate alloys are chosen for an insight into their corrosion behaviour. Several atmospheres are studied, i.e. O2, H2O, SO2 and a mix thereof in argon as well as synthetic air. Just as for classic alloys, the chromium is the most important element in terms of protection agains further corrosion. The addition of manganese, as in case of the “Cantor alloy” CrMnFeCoNi, overpasses Cr when it comes to oxygen affinity and thus counteracts the layer formation of Cr2O3. Even without Mn, a temperature chosen too high will also affect the formation of the chromium oxide layer and spall it off, annulling its protective potential. We can also observe how trace elements influence the layer formation. These effects and their mechanisms will be discussed for the alloys CrFeNi, CoCrNi, CrMnFeCoNi and variations of Al10Co25Cr8Fe15Ni36Ti6 using a combination of electron microscopy, thermodynamic calculations and x-ray diffraction. T2 - MRS-T International Conference CY - Hsinchu, Taiwan DA - 17.11.2023 KW - Corrosion KW - Scanning electron microscopy KW - Mixed gas atmosphere PY - 2023 AN - OPUS4-58980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weinel, Kristina A1 - Gonzalez-Martinez, I. A1 - Agudo Jacome, Leonardo T1 - Damage induced by electric field of microparticles in the electron microscope N2 - Damage induced by electric field (DIEF) that happens in the transmission electron microscope (TEM) when converging the electron beam (e-beam) on microparticles (MPs) can be used to synthesis new nanomaterial and nanomaterial compositions. The research questions are to clarify the limits and possibilities of the method regarding materials that can be produced, systems to which it is applicable and working beam parameters. Synthesis of nano-objects from microparticles using DIEF in TEM could be shown for different materials. Additionally, DIEF using the e-beam in a scanning electron microscope (SEM) can also be used to synthesis nano-objects. A deeper material analysis of this nano-objects was done using TEM and shows that the material of the nanoparticles (NPs) can be gold or/and silicon. Furthermore, the size of the NPs depends on the distance to the center of DIEF whereby the larger NPs are closer to the center. The areas of gold NPs are promising candidates for plasmonic or photonic devices for energy storage or transport. T2 - PhD-Day 2022 CY - Berlin, Germany DA - 06.09.2022 KW - Electron microscopy KW - Electron beam induced modification KW - Gold nanoparticles PY - 2022 AN - OPUS4-58264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Goedecke, Caroline A1 - Altmann, Korinna A1 - Bannick, C. G. A1 - Kober, E. A1 - Ricking, M. A1 - Schmitt, T. A1 - Braun, Ulrike T1 - Detection of polymers in treated waste water using TED-GC-MS N2 - The presence of large quantities of plastic waste and its fragmentation in various environmental compartments are an important subject of current research. In the environment, (photo ) oxidation processes and mechanical abrasion lead to the formation of microplastics. However, until now, there are no established quality assurance concepts for the analysis of microplastic (<5 mm) in environmental compartments, including sampling, processing and analysis. The aim of the present work is the development of suitable examination methods and protocols (sampling, sample preparation and detection) to qualify and quantify microplastic in urbane water management systems. At first a fractional filtration system for sampling and the analytical tool, the so-called TED-GC-MS (thermal desorption gas chromatography mass spectrometry) were developed. The TED-GC-MS method is a two-step analytical procedure which consists of a thermal extraction where the sample is annealed and characteristic decomposition products of the polymers are collected on a solid phase. Afterwards these products are analysed using GC-MS. The developed fractional filtration for sampling and the TED-GC-MS for detection were used for quantitative analysis to screen the waste water influent and effluent of a Berlin waste water treatment plant for the most relevant polymers, polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA). The results of the study revealed that the polymeres PE, PS and PP were detected in the effluent, and PE and PS were find in the raw waste water of the sewage treatment plant in Ruhleben, Berlin. Differences in polymer types and amounts were detected at different sampling dates and within different sieve fractions. Much higher amounts of polymers were observed in the raw waste water. The peak areas of the decomposition products, used for quantification of the polymers, were adjusted using so-called response factors since the TED-GC-MS method is more sensitive for PP and PS than for PE. It has been shown that PE is the most dominant polymer in the samples. Comparing the masses of polymers in the effluent and in the raw sewage, a removal of 99 % of the polymers in the water treatment plant can be assumed. These results are consistent with the literature where removal rates between 98-99 % were described. T2 - SETAC Europe CY - Rom, Italy DA - 13.05.2018 KW - Microplastics KW - Thermogravimetry KW - Waste water KW - Chromatography PY - 2018 AN - OPUS4-44968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günster, Jens A1 - Zocca, Andrea T1 - Dense Powder Beds for the Additive Manufacturing of Ceramics N2 - Regarding feedstocks for the additive manufacturing (AM) of ceramics, two features are most critical in classical powder based AM processes: a high particle packing density (typically >50% TD) must be achieved with very fine particles (typically submicron) in order to ensure sufficient sintering activity. Three innovative approaches will be introduced to overcome this problem: 1. Layer wise slurry deposition: The use of water based ceramic slurries as feedstock for the additive manufacture of ceramics has many advantages which are not fully exploit yet. In the layerwise slurry deposition (LSD) process a slurry with no or low organic content is repetitively spread as thin layers on each other by means of a doctor blade. During the deposition, the ceramic particles settle on the previously deposited and dried material to form thin layers with a high packing density (55-60%). The LSD therefore shares aspects both of tape casting and slip casting. The LSD differentiates from the classical powder-based AM layer deposition, which typically achieves with a flowable coarse grained powder a low packing density (35-50%) only, consequently hindering the ability of sintering ceramic parts to full density. The LSD is coupled with the principles of selective laser sintering (SLS) or binder jetting, to generate novel processes which take advantage of the possibility of achieving a highly dense powder-bed. 2. Laser induced slip casting: Contrary to the LSD process, which requires drying of each individual layer, the direct interaction of ceramic slurries with intense laser radiation, for the laser induced slip casting (LIS), is a promising approach for the additive manufacture of voluminous parts. 3. Gas flow assisted powder deposition: By the application of a vacuum pump a gas flow is realized throughout the powder bed. This gas flow stabilizes the powder bed and results into an enhanced flowability and packing density of the powder during layer deposition. The presentation will provide a detailed discussion of potentialities and issues connected to the mentioned technologies and will describe the most recent developments in their application to technical ceramics. T2 - SmatMade 2022 CY - Osaka, Japan DA - 25.10.2022 KW - Additive Manufacturing KW - Advanced ceramics PY - 2022 AN - OPUS4-59886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günster, Jens T1 - Binder Jetting of Advanced Ceramics N2 - The Binder Jetting BJ process is one of the most versatile additive manufacturing technologies in use. In this process a binder is locally jetted into a powder bed for the consolidation of a 3D structure, layer by layer. Basically, all materials which can be provided as a flowable powder and, thus, spreadable to a thin layer, can be processed. Metals, ceramics and polymers are processable, but also materials from nature, such as sand, wood sawdust and insect frass. Moreover, the BJ technology is adapted to large building volumes of some cubic meters easily. Besides these striking advantages, the manufacture of ceramic parts by BJ is still challenging, as the packing density of the powder bed is generally too low and the particle size of a flowable powder too large for a successful densification of printed parts in a subsequent sintering step to an advanced ceramic product. After an introduction of binder jetting in general and highlighting some examples, strategies for obtaining dense ceramic parts by BJ will be introduced. T2 - yCAM 2022 CY - Barcelona, Spain DA - 08.11.2022 KW - Additive Manufacturing KW - Ceramics PY - 2022 AN - OPUS4-59887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günster, Jens A1 - Sänger, Johanna T1 - Tailoring powder properties for the light based volumetric additive manufacture of Ceramics N2 - In order to be able to manipulate ceramic powder compacts and ceramic suspensions (slurries) within their volume with light, a minimum transparency of the materials is required. Compared to polymers and metals, ceramic materials are characterized by the fact that they have a wide electronic band gap and therefore a wide optical window of transparency. The optical window generally ranges from less than 0.3 µm to 5 µm wavelength. In order to focus light into the volume of a ceramic powder compact, its light scattering properties must therefore be tailored. In this study, we present the physical background and material development strategies for the application of two-photon polymerization (2PP) and selective volumetric sintering for the additive manufacturing of structures in the volume of ceramic slips and green compacts. T2 - SmartMade 2024 CY - Osaka, Japan DA - 10.04.2024 KW - Additive Manufacturing KW - Two Photon Polymerization KW - Advanced ceramics PY - 2024 AN - OPUS4-59888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -