TY - CONF A1 - Miliūtė, Aistė A1 - George, Janine A1 - Mieller, Björn A1 - Stawski, Tomasz T1 - ZrV2O7 negative thermal expansion (NTE) material N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material that exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). Therefore, it can be used to create composites with controllable expansion coefficients and prevent thermal stress, fatigue, cracking, and deformation at interfaces. We implement interdisciplinary research to analyze such material. We study the influence of the synthesis methods and their parameters on the sample's purity, crystallinity, and homogeneity. Moreover, we implement ab initio-based vibrational computations with partially treated anharmonicity in combination with experimental methods to follow temperature-induced structural changes and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder. T2 - SALSA Make and Measure Conference CY - Berlin, Germany DA - 13.09.2023 KW - NTE KW - Composites KW - TEM PY - 2023 AN - OPUS4-58367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Narsabadi, Hossein A1 - Vafaeenezhad, H. A1 - Klotz, U.E. A1 - Tiberto, D. A1 - Hosseinabadi, F. A1 - Mishurova, Tatiana A1 - Bruno, Giovanni A1 - Skrotzki, Birgit T1 - XCT-assisted micromechanical modeling of the effect of pores on the plastic deformation and mechanical characteristics of PBF-LB/M-produced copper alloys N2 - Due to the low absorption of fiber laser by copper particles, the laser-based powder bed fusion (PBF-LB/M) processing of copper components is accompanied by the development of different types of porosities within the printed samples. This research aims to assess the consequences of various process-induced pores on the me chanical characteristics and deformation of PBF-LB/M-produced copper alloys. Several copper alloys were processed using metal-coated particles and varied laser intensities, yielding samples with different types and amounts of porosities. For instance, CuCrZr alloys processed at 325 J/mm³ and 257 J/mm³ had 0.009 % and 1.117 % porosities, dominated by keyhole and lack-of-fusion pores, respectively. Moreover, PBF-LB/M pro cessing of Cr- and Nb-coated CuNi3SiCr particles accompanied by the generation of 0.004 % and 1.861 % porosities within the samples, predominantly featuring metallurgical and oxidation pores, respectively. Compression and nanoindentation tests revealed that the CuNi3SiCr alloy exhibited superior mechanical properties compared to the CuCrZr sample (nanoindentation hardness values 2.2 GPa and 1.4 GPa, respectively), while the presence of lack-of-fusion pores notably diminished their mechanical performance. X-ray computed tomography (XCT) reconstruction slices and scanning electron microscopy (SEM) images were then used for developing the representative volume elements (RVEs) based micromechanical models. The micromechanical simulations established a structure-property correlation that can simulate the compressive deformation and mechanical characteristics of PBF-LB/M-produced copper alloys as a function of their incorporated pore characteristics. Due to the closure of the pores at the first stages of deformation, samples with minimal keyhole and metallurgical porosities exhibited homogeneous plastic deformation. On the other side, based on the JohnsonCook model, strain concentration and crack propagation around the lack-of-fusion pores lead to damage initi ation in the printed samples at a strain level of 5 % KW - X-ray Computed tomography KW - Defects KW - Copper alloys KW - PBF-LB/M KW - Micromechanics PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624004 DO - https://doi.org/10.1016/j.msea.2025.147836 SN - 0921-5093 VL - 924 PB - Elsevier B.V. AN - OPUS4-62400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Han, Ying A1 - Fritsch, Tobias A1 - Hejazi, Bardia A1 - Ulbricht, Alexander A1 - Skrotzki, Birgit A1 - Bruno, Giovanni T1 - X-ray computed tomography quantifies primary phases and reveals crack morphology in high-cycle fatigue of aluminum alloy EN AW-2618A N2 - Since the introduction of high-strength aluminum alloys understanding their fatigue behavior is of high interest for the structural integrity of engineering components, in this context, the alloy EN AW-2618A gains its high strength from both nanometer size precipitates and micrometer size primary phases. The latter phases are often identified as crack initiation sites. In this study, it uses a combination of synchrotron and laboratory-based X-ray computed tomography to image and quantify such primary phases and the fatigue cracks appearing in interrupted tests. Based on the gray-level differences in the synchrotron X-ray computed tomography scans, this study is able to distinguish low- and high-absorbing particles. The dominant (volume fraction >99%) high absorbing primary phase can be quantified in good agreement with results of Thermo-Calc calculations. To image the fatigue crack, laboratory X-ray computed tomography scans are performed at different tensile loads to open the crack. The results show that with an appropriate crack opening tensile load, the fatigue crack morphology can be reliably revealed. Based on these results, the influence of the primary phases on the fatigue crack initiation and propagation are discussed. KW - X-ray computed tomography KW - Fatigue KW - Aluminum KW - Primary phases PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632724 DO - https://doi.org/10.1002/adem.202500235 SN - 1527-2648 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-63272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - Workflow generation, management, and semantic description for Self-Driving Labs N2 - The software backend that controls the robotic hardware and runs the synthesis workflows is a very important component of any Self-Driving Lab (SDL). On the one hand, it has to deal with orchestrating and managing complex and task-specific hardware through low-level communication protocols and plan and use the available resources as efficiently as possible while executing (parallelized) workflows, on the other hand, it is the interface the users use to communicate with this highly complex platform, and as such, it needs to be as helpful and user-friendly as possible. This includes the AI-aided experimental design in which the system helps the user to decide which experiment to run next, providing automated data analysis from characterization measurements, and offering easy to understand tools and graphical user interfaces for generating the workflows that are executed on the platform. Lastly, the specificity of the workflows and their dependence on the hardware and software of the SDLs necessitates a common description or ontology for making them easily interchangeable and interoperable between different platforms and labs. In this contribution, we present several key aspects of “Minerva-OS”, the central backend that orchestrates the syntheses workflows of our SDL for Nano- and Advanced Materials Syntheses [1]. One key feature is the resource management or “traffic control” for scheduling and executing parallel reactions in a multi-threaded environment. Another is the interface with data analysis algorithms from in-line, at-line, and off-line measurements. Here, we will give examples of how automatic image segmentation of electron microscopy images with the help of AI [2] can be used for reducing the “data analysis bottleneck” from an off-line measurement. We will also discuss, compare, and show benchmarks of various machine learning (ML) algorithms that are currently implemented in the backend and can be used for ML-guided, closed-loop material optimization in our SDL. Lastly, we will show our recent efforts [3] in making the workflow generation on SDLs more user-friendly by using large language models to generate executable workflows automatically from synthesis procedures given in natural language and user-friendly graphical user interfaces based on node editors that also allow for knowledge graph extraction from the workflows. In this context, we are currently also working on an ontology for representing the process steps of the workflows, which will greatly facilitate the semantic description and interoperability of workflows between different SDL hardware and software platforms. T2 - Accelerate 2025 CY - Toronto, Canada DA - 11.08.2025 KW - Nanomaterials KW - Advanced Materials KW - Workflows KW - Machine Learning KW - SDL PY - 2025 AN - OPUS4-63936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hajian, A. A1 - Konegger, T. A1 - Bielecki, K. A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Schwarz, S. A1 - Zellner, C. A1 - Schmid, U. T1 - Wet chemical porosification with phosphate buffer solutions for permittivity reduction of LTCC substrates N2 - The wireless high-frequency technology requires a robust, cost-effective, and highly integrated substrate technology offering the capability for areas of tailored permittivity. The wet-chemical porosification of low temperature co-fired ceramics (LTCC) substrates offers such an approach by locally embedding air. Porosification of LTCC in both extremely acidic and alkaline media has been investigated in previous works. However, for improving the available knowledge on the porosification of LTCC with H3PO4 as a standard and a widely used etching solution, the impact of solution concentration was systematically investigated and a substantial improvement in the etching performance was achieved. Moreover, in the present study, for the first time, the intermediate pH values, and the impact of pH as a key parameter on the etching process have been investigated. For this purpose, the applicability of phosphate buffer solution (PBS) as a prospective novel etchant mixture for the porosification of a commercially available LTCC tape (Ceramtape GC) was explored. Valuable information about surface morphology, crystalline composition, and the pore structure of the etched LTCCs was gathered employing scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and mercury porosimetry measurements. Based on these findings, the performance of PBS-based etchant systems towards the generation of porous LTCCs combining high depths of porosification with acceptable surface characteristics for subsequent metallization is demonstrated. Based on the obtained results, by application of a 0.2 mol L−1 solution of PBS, the effective relative permittivity of test samples with a thickness of approximately 600 µm and a porosification depth of 186 µm from each side, could be reduced up to 10% of its initial “as fired” value. Also, based on the measurement results and by measuring the depth of porosification, the permittivity of the etched layer was estimated to show a reduction of up to 22% compared to the initial “as fired” value. KW - LTCC KW - Porosification KW - Wet chemical etching KW - Permittivity reduction PY - 2020 DO - https://doi.org/10.1016/j.jallcom.2020.158059 SN - 0925-8388 VL - 863 SP - 158059 PB - Elsevier B.V. AN - OPUS4-51800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Manzoni, Anna Maria A1 - Schneider, M. A1 - Laplanche, G. T1 - Welding of high-entropy alloys and compositionally complex alloys - an overview N2 - High-entropy alloys (HEAs) and compositionally complex alloys (CCAs) represent new classes of materials containing five or more alloying elements (concentration of each element ranging from 5 to 35 at. %). In the present study, HEAs are defined as single-phase solid solutions; CCAs contain at least two phases. The alloy concept of HEAs/CCAs is fundamentally different from most conventional alloys and promises interesting properties for industrial applications (e.g., to overcome the strength-ductility trade-off). To date, little attention has been paid to the weldability of HEAs/CCAs encompassing effects on the welding metallurgy. It remains open whether welding of HEAs/CCAs may lead to the formation of brittle intermetallics and promote elemental segregation at crystalline defects. The effect on the weld joint properties (strength, corrosion resistance) must be investigated. The weld metal and heat-affected zone in conventional alloys are characterized by non-equilibrium microstructural evolutions that most probably occur in HEAs/CCAs. The corresponding weldability has not yet been studied in detail in the literature, and the existing information is not documented in a comprehensive way. Therefore, this study summarizes the most important results on the welding of HEAs/CCAs and their weld joint properties, classified by HEA/CCA type (focused on CoCrFeMnNi and AlxCoCrCuyFeNi system) and welding process. KW - High-entropy alloy KW - Compositionally complex alloy KW - Welding KW - Properties KW - Review PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527068 DO - https://doi.org/10.1007/s40194-021-01110-6 SP - 1 EP - 15 PB - Springer Nature AN - OPUS4-52706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Welding of high-entropy alloys - New material concept vs. old challenges N2 - HEAs represent a relatively new class of materials. The the alloy concept is fundamentally different from the most conventional materials and alloys that are used today. Recently, the focus of HEA designs is more application-based. For that purpose, the elements of interest are carefully selected and multiple phases as well as micro-structures are deliberately adjusted. Currently, only limited attention has been paid to weldability of HEA. This encompasses possible effects on metallurgy and its influence on the desired properties. It remains open if welding causes e.g. considerable number of intermetallic phases or segregations and their effect on weld joint properties. For that reason, the scope of this study is to summarize already available studies on welding of HEAs with respect to the HEA-type, the applied welding process and its influence on the weld joint properties. T2 - IIW Annual Assembly, Meeting of Commission II-A CY - Online meeting DA - 20.07.2020 KW - High-entropy alloy KW - Welding KW - Review PY - 2020 AN - OPUS4-51116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zocca, Andrea T1 - Water-based additive manufacturing of ceramics by Laser-Induced Slip Casting (LIS) N2 - The Laser-Induced Slip Casting is an additive manufacturing technology specifically developed for ceramic materials using water-based ceramic slurries. The process takes place layer-by-layer in a similar fashion as top-down vat photopolymerization, selectively consolidating each layer by means of a laser energy source positioned on the top. Contrary to vat photopolymerization, in which the consolidation is achieved by selectively cross-linking a ceramic-filled resin, LIS uses water-based slurries with a low amount of organic additives (typically < 5 wt%) as feedstocks. In LIS, a green body is formed by local evaporation of water which causes the suspension to collapse forming a cast, following a mechanism similar to slip casting. Only a small content of organic additives is needed to effectively disperse the ceramic particles and to increase the green strength. The technology is very versatile and can be applied to all ceramic systems that can be dispersed in water. One of the main advantages is that even dark materials such as silicon carbide can be processed without issues related to light scattering and absorption. The presentation will discuss strengths and limitations of LIS compared to other AM technologies and will highlight the latest results for alumina and for silicon carbide ceramics. T2 - 48th International Conference and Expo on Advanced Ceramics and Composites (ICACC2024) CY - Daytona, FL, USA DA - 28.01.2024 KW - Additive Manufacturing KW - Ceramic KW - Water-based KW - Slurry KW - Laser PY - 2024 AN - OPUS4-60054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balzer, R. A1 - Behrens, H. A1 - Waurischk, Tina A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Kiefer, P. A1 - Deubener, J. A1 - Fechtelkord, M. T1 - Water in Alkali Aluminosilicate Glasses N2 - To understand the influence of water and alkalis on aluminosilicate glasses, three polymerized glasses with varying ratios of Na/K were synthesized [(22. 5-x)Na2O-xK2O-22.5 Al2O3-55 SiO2 with x = 0, 7.5, and 11.25]. Subsequently, these glasses were hydrated (up to 8 wt% H2O) in an internally heated gas pressure vessel. The density of hydrous glasses linearly decreased with water content above 1 wt%, consistent with the partial molar volume of H2O of 12 cm3/mol. Near-infrared spectroscopy revealed that hydroxyl groups are the dominant species at water content of <4 wt%, and molecular water becomes dominating at water content of >5 wt%. The fraction of OH is particularly high in the pure Na-bearing glass compared to the mixed alkali glasses. 27Al magic angle spinning-NMR spectroscopy shows that aluminum is exclusively fourfold coordinated with some variations in the local geometry. It appears that the local structure around Al becomes more ordered with increasing K/Na ratio. The incorporation of H2O reinforces this effect. The differential thermal analysis of hydrous glasses shows a significant mass loss in the range of glass transition already during the first upscan, implying the high mobility of water in the glasses. This observation can be explained by the open structure of the aluminosilicate network and by the low dissociation enthalpy of H2O in the glasses (≈ 8 kJ/mol). The effect of the dissolved H2O on the glass transition temperature is less pronounced than for other aluminosilicate glasses, probably because of the large fraction of Al in the glasses. KW - NMR spectroscopy KW - Alkali aluminosilicate glasses KW - Water speciation KW - Glass transition KW - Infrared spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509497 DO - https://doi.org/10.3389/fmats.2020.00085 VL - 7 SP - 85 AN - OPUS4-50949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gibson, N. A1 - Kuchenbecker, Petra A1 - Rasmussen, K. A1 - Hodoroaba, Vasile-Dan A1 - Rauscher, H. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A.G. T1 - Volume-specific surface area by gas adsorption analysis with the BET method N2 - This chapter first gives an introduction to the concepts of SSA and volume-specific surface area (VSSA) and an outline of the BET method. It continues with a discussion of the relationship between particle size, shape, and the VSSA, followed by an overview of instrumentation, experimental methods, and standards. Finally, sections on the use of the VSSA as a tool to identify nanomaterials and non-nanomaterials and its role in a regulatory context provide some insight on the importance of VSSA in the current Regulation of nanomaterials. KW - Nanomaterials KW - Volume specific surface area PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00017-1 SP - 265 EP - 293 PB - Elsevier CY - Amsterdam AN - OPUS4-49572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -