TY - JOUR A1 - Fantin, Andrea A1 - Manzoni, Anna Maria A1 - Springer, H. A1 - Darvishi Kamachali, Reza A1 - Maaß, Robert T1 - Local lattice distortions and chemical short-range order in MoNbTaW N2 - Extended X-ray absorption fine structure (EXAFS) conducted on an equiatomic MoNbTaW bcc medium-entropy alloy that was annealed at 2273 K reveals unexpectedly small 1st and 2nd shell element-specific lattice distortions. An experimental size-mismatch parameter, δexp, is determined to be ca. 50% lower than the corresponding calculated value. Around W, short-range order (SRO) preferring 4d elements in the 1st and 2nd shells persists. A Nb-W ordering is found, which is reminiscent of ordering emerging at lower temperatures in the B2(Mo,W;Ta,Nb)- and B32(Nb,W)-phases. With high-temperature ordering preferences in fcc also foreshadowing low-temperature phase, these findings suggest a general feature of high-temperature SRO. KW - High Entropy Alloys KW - Short-range order KW - Lattice distortions KW - EXAFS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598164 DO - https://doi.org/10.1080/21663831.2024.2326014 SN - 2166-3831 VL - 12 IS - 5 SP - 346 EP - 354 PB - Taylor & Francis AN - OPUS4-59816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darvishi Kamachali, Reza A1 - Wallis, Theophilius A1 - Ikeda, Yuki A1 - Saikia, U. A1 - Ahmadian, A. A1 - Liebscher, C. A1 - Hickel, Tilmann A1 - Maaß, Robert T1 - Giant segregation transition as origin of liquid metal embrittlement in the Fe-Zn system N2 - A giant Zn segregation transition is revealed using CALPHAD-integrated density-based modeling of segregation into Fe grain boundaries (GBs). The results show that above a threshold of only a few atomic percent Zn in the alloy, a substantial amount of up to 60 at.% Zn can segregate to the GB. We found that the amount of segregation abruptly increases with decreasing temperature, while the Zn content in the alloy required for triggering the segregation transition decreases. Direct evidence of the Zn segregation transition is obtained using high-resolution scanning transmission electron microscopy. Base on the model, we trace the origin of the segregation transition back to the low cohesive energy of Zn and a miscibility gap in Fe-Zn GB, arising from the magnetic ordering effect, which is confirmed by ab-initio calculations. We also show that the massive Zn segregation resulting from the segregation transition greatly assists with liquid wetting and reduces the work of separation along the GB. The current predictions suggest that control over Zn segregation, by both alloy design and optimizing the galvanization and welding processes, may offer preventive strategies against liquid metal embrittlement. KW - CALPHAD KW - Microstructure Design KW - Grain boundary engineering KW - Steels KW - Density-based Model KW - Segregation Engineering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584292 DO - https://doi.org/10.1016/j.scriptamat.2023.115758 SN - 1359-6462 SN - 1872-8456 VL - 238 SP - 1 EP - 5 PB - Elsevier CY - Amsterdam AN - OPUS4-58429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Polycondensation of poly(L-lactide) alkyl esters combined with disproportionation and symproportionation of the chain lengths N2 - Ring-opening polymerizations (ROPs) of l-lactide (LA) were performed with ethyl l-lactate or 11-bromoundecanol as initiators (In) and tin(II) ethyl hexanoate (SnOct2) as catalyst (Cat) using four different LA/In ratios (20/1, 40/1, 60/1, and 100/1). One series of ROPs was conducted in bulk at 120 °C, yielding PLAs with low dispersities (Ð ~ 1.2–1.4), and a second series was conducted in bulk at 160 °C, yielding higher dispersities (Ð ~ 1.3–1.9). Samples from both series were annealed for 1 or 14 days at 140 °C in the presence of SnOct2. Both polycondensation and disproportionation reactions occurred, so that all four samples tended to form the same type of molar mass distribution below 10,000 Da, regardless of their initially different number average molar masses (Mn). Both initiators gave nearly identical results. The thermodynamic control of all reversible transesterification processes favored the formation of crystallites composed of chains with a Mn around 3500–3700, corresponding to a crystal thickness of 10–13 nm. KW - Polylactide KW - MALDI-TOF MS KW - Crystalinity PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600081 DO - https://doi.org/10.1002/pol.20240118 SN - 2642-4150 SP - 1 EP - 12 PB - Wiley AN - OPUS4-60008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Schilling, Markus A1 - von Hartrott, Philipp A1 - Waitelonis, Jörg T1 - Semantic integration of diverse data in materials science: Assessing Orowan strengthening N2 - AbstractThis study applies Semantic Web technologies to advance Materials Science and Engineering (MSE) through the integration of diverse datasets. Focusing on a 2000 series age-hardenable aluminum alloy, we correlate mechanical and microstructural properties derived from tensile tests and dark-field transmission electron microscopy across varied aging times. An expandable knowledge graph, constructed using the Tensile Test and Precipitate Geometry Ontologies aligned with the PMD Core Ontology, facilitates this integration. This approach adheres to FAIR principles and enables sophisticated analysis via SPARQL queries, revealing correlations consistent with the Orowan mechanism. The study highlights the potential of semantic data integration in MSE, offering a new approach for data-centric research and enhanced analytical capabilities. KW - Semantic Interoperability KW - Knowledge Graph KW - Orowan Mechanism KW - Aluminum Alloy Aging KW - Ontology KW - Semantic Data Integration PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599780 DO - https://doi.org/10.1038/s41597-024-03169-4 VL - 11 IS - 1 SP - 1 EP - 12 PB - Springer Science and Business Media LLC AN - OPUS4-59978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Temgoua, Ranil C.T. A1 - Dontsi, Fabiola T. A1 - Lebègue, Estelle A1 - Thobie-Gautier, Christine A1 - Tonlé, Ignas K. A1 - Boujtita, Mohammed T1 - Understanding the behavior of phenylurazole-tyrosine-click electrochemical reaction using hybrid electroanalytical techniques N2 - In this work, the electrochemical behavior of 4-phenylurazole (Ph-Ur) was studied and the latter was used as a molecular anchor for the electrochemical bioconjugation of tyrosine (Y). Cyclic voltammetry (CV) and controlled potential coulometry (CPC) allowed the in-situ generation of the PTAD (4-phenyl-3 H-1,2,4-triazole-3,5(4 H)-dione) species from phenylurazole on demand for tyrosine electrolabeling. The chemoselectivity of the reaction was studied with another amino acid (lysine, Lys) and no changes in Lys were observed. To evaluate the performance of tyrosine electrolabeling, coulometric analyses at controlled potentials were performed on solutions of phenylurazole and the phenylurazole-tyrosine mixture in different proportions (2:1, 1:1, and 1:2). The electrolysis of the phenylurazole-tyrosine mixture in the ratio (1:2) produced a charge of 2.07 C, very close to the theoretical value (1.93 C), with high reaction kinetics, a result obtained here for the first time. The products obtained were identified and characterized by liquid chromatography coupled to high-resolution electrospray ionization mass spectrometry (LC-HRMS and LC- HRMS2). Two products were formed from the click reactions, one of which was the majority. Another part of this work was to study the electrochemical degradation of the molecular anchor 4-phenylazole (Ph-Ur). Four stable degradation products of phenylurazole were identified (C7H9N2O, C6H8N, C6H8NO, C14H13N4O2) based on chromatographic profiles and mass spectrometry results. The charge generated during the electrolysis of phenylurazole (two-electron process) (2.85 C) is inconsistent with the theoretical or calculated charge (1.93 C), indicating that secondary/parasitic reactions occurred during the electrolysis of the latter. In conclusion, the electrochemically promoted click phenylurazole-tyrosine reactions give rise to click products with high reaction kinetics and yields in the (1:2) phenylurazole-tyrosine ratios, and the presence of side reactions is likely to affect the yield of the click phenylurazole-tyrosine reaction. KW - Clinical Biochemistry KW - Spectroscopy KW - Drug Discovery KW - Pharmaceutical Science KW - Analytical Chemistry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599267 DO - https://doi.org/10.1016/j.jpba.2024.116147 VL - 245 SP - 1 EP - 8 PB - Elsevier BV AN - OPUS4-59926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strobl, Dominic A1 - Unger, Jörg F. A1 - Ghnatios, C. A1 - Klawoon, Alexander A1 - Pittner, Andreas A1 - Rethmeier, Michael A1 - Robens-Radermacher, Annika T1 - Efficient bead-on-plate weld model for parameter estimation towards effective wire arc additive manufacturing simulation N2 - Despite the advances in hardware and software techniques, standard numerical methods fail in providing real-time simulations, especially for complex processes such as additive manufacturing applications. A real-time simulation enables process control through the combination of process monitoring and automated feedback, which increases the flexibility and quality of a process. Typically, before producing a whole additive manufacturing structure, a simplified experiment in the form of a beadon-plate experiment is performed to get a first insight into the process and to set parameters suitably. In this work, a reduced order model for the transient thermal problem of the bead-on-plate weld simulation is developed, allowing an efficient model calibration and control of the process. The proposed approach applies the proper generalized decomposition (PGD) method, a popular model order reduction technique, to decrease the computational effort of each model evaluation required multiple times in parameter estimation, control, and optimization. The welding torch is modeled by a moving heat source, which leads to difficulties separating space and time, a key ingredient in PGD simulations. A novel approach for separating space and time is applied and extended to 3D problems allowing the derivation of an efficient separated representation of the temperature. The results are verified against a standard finite element model showing excellent agreement. The reduced order model is also leveraged in a Bayesian model parameter estimation setup, speeding up calibrations and ultimately leading to an optimized real-time simulation approach for welding experiment using synthetic as well as real measurement data. KW - Proper generalized decomposition KW - Model order reduction KW - Hardly separable problem KW - Additive manufacturing KW - Model calibration KW - Wire arc additive manufacturing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596502 DO - https://doi.org/10.1007/s40194-024-01700-0 SN - 0043-2288 SP - 1 EP - 18 PB - Springer AN - OPUS4-59650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strobl, Dominic A1 - Unger, Jörg F. A1 - Ghnatios, C. A1 - Robens-Radermacher, Annika T1 - PGD in thermal transient problems with a moving heat source: A sensitivity study on factors affecting accuracy and efficiency N2 - Thermal transient problems, essential for modeling applications like welding and additive metal manufacturing, are characterized by a dynamic evolution of temperature. Accurately simulating these phenomena is often computationally expensive, thus limiting their applications, for example for model parameter estimation or online process control. Model order reduction, a solution to preserve the accuracy while reducing the computation time, is explored. This article addresses challenges in developing reduced order models using the proper generalized decomposition (PGD) for transient thermal problems with a specific treatment of the moving heat source within the reduced model. Factors affecting accuracy, convergence, and computational cost, such as discretization methods (finite element and finite difference), a dimensionless formulation, the size of the heat source, and the inclusion of material parameters as additional PGD variables are examined across progressively complex examples. The results demonstrate the influence of these factors on the PGD model’s performance and emphasize the importance of their consideration when implementing such models. For thermal example, it is demonstrated that a PGD model with a finite difference discretization in time, a dimensionless representation, a mapping for a moving heat source, and a spatial domain non-separation yields the best approximation to the full order model. KW - Additive manufacturing KW - Mapping for unseparable load KW - Model order reduction (MOR) KW - Thermal transient problem KW - Sensitivity analysis KW - Proper generalized decomposition (PGD) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598001 DO - https://doi.org/10.1002/eng2.12887 IS - e12887 SP - 1 EP - 22 PB - John Wiley & Sons Ltd. CY - Berlin AN - OPUS4-59800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herter, Sven-Oliver A1 - Koch, Matthias A1 - Haase, Hajo T1 - First Synthesis of Ergotamine-13CD3 and Ergotaminine-13CD3 from Unlabeled Ergotamine N2 - Ergot alkaloids (EAs) formed by Claviceps fungi are one of the most common food contaminants worldwide, affecting cereals such as rye, wheat, and barley. To accurately determine the level of contamination and to monitor EAs maximum levels set by the European Union, the six most common EAs (so-called priority EAs) and their corresponding epimers are quantified using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The quantification of EAs in complex food matrices without appropriate internal tandards is challenging but currently carried out in the standard method EN 7425:2021 due to their commercial unavailability. To address the need for isotopically labeled EAs, we focus on two semi-synthetic approaches for the synthesis of these reference standards. Therefore, we investigate the feasibility of the N6-demethylation of native ergotamine to yield norergotamine, which can subsequently be remethylated with an isotopically labeled methylating reagent, such as iodomethane (13CD3-I), to yield isotopically labeled ergotamine and its C8-epimer ergotaminine. Testing the isotopically labeled ergotamine/-inine against native ergotamine/-inine with HPLC coupled to high-resolution HR-MS/MS proved the structure of ergotamine-13CD3 and ergotaminine-13CD3. Thus, for the first time, we can describe their synthesis from unlabeled, native ergotamine. Furthermore, this approach is promising as a universal way to synthesize other isotopically labeled EAs. KW - Reference Material KW - HPLC-MS/MS KW - Mycotoxins KW - Standards KW - Organic Synthesis KW - Isotope PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600167 DO - https://doi.org/10.3390/toxins16040199 VL - 16 IS - 4 SP - 1 EP - 12 PB - MDPI AN - OPUS4-60016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dalgic, Mete-Sungur A1 - Weidner, Steffen T1 - Solvent-free sample preparation for matrix-assisted laserdesorption/ionization time-of-flight mass spectrometry ofpolymer blends N2 - Solvent-free sample preparation offers some advantages over solvent-based techniques, such as improved accuracy, reproducibility and sensitivity, for matrix-assisted laser desorption/ionization (MALDI) analysis. However, little or no information is available on the application of solvent-free techniques for the MALDI analysis of polymer blends. Solvent-free sample preparation by ball milling was applied with varying sample-to-matrix ratios for MALDI time-of-flight mass spectrometry analysis of various polymers, including polystyrenes, poly(methyl methacrylate)s and poly(ethylene glycol)s. The peak intensity ratios were compared with those obtained after using the conventional dried droplet sample preparation method. In addition, solvent-assisted milling was also applied to improve sample homogeneities. Depending on the sample preparation method used, different peak intensity ratios were found, showing varying degrees of suppression of the signal intensities of higher mass polymers. Ball milling for up to 30 min was required to achieve constant intensity ratios indicating homogeneous mixtures. The use of wet-assisted grinding to improve the homogeneity of the blends was found to be disadvantageous as it caused partial degradation and mass-dependent segregation of the polymers in the vials.The results clearly show that solvent-free sample preparation must be carefully considered when applied to synthetic polymer blends, as it may cause additional problems with regard to homogeneity and stability of the blends. KW - MALDI TOF MS KW - Sample preparation KW - Polymer blends KW - Solvent-free PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598570 DO - https://doi.org/10.1002/rcm.9756 SN - 0951-4198 VL - 38 IS - 12 SP - 1 EP - 9 PB - Wiley online library AN - OPUS4-59857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von Törne, Wipert Jannik A1 - Steinhäuser, Lorin A1 - Klyk-Seitz, Urszula-Anna A1 - Piechotta, Christian T1 - High-resolution mass spectrometric elucidation of electron ionization induced fragmentation pathways of methylated warfarin and selected hydroxylated species N2 - The plant secondary metabolite families of coumarin and 4-hydroxy coumarin have a broad pharmacological spectrum ranging from antibacterial to anticancer properties. One prominent member of this substance class is the synthetic but naturally inspired anticoagulant drug and rodenticide warfarin (coumadin). A vast number of publications focus on the identification of warfarin and its major cytochrome P450-mediated phase I metabolites by liquid chromatography (LC) with mass spectrometry (MS) and tandem mass spectrometric (MS/MS) detection techniques. For the first time, electron ionization (EI) induced high-resolution quadrupole time-of-flight mass spectrometric (HR-qToF-MS) data of in-liner derivatized warfarin and selected hydroxylated species is provided in this study as an alternative to LC-MS/MS approaches. Furthermore, the characteristic fragments and fragmentation pathways of the analyzed methyl ethers are concluded. The obtained data of analytical standards, specific deuterated and 13C-labeled compounds prove inductive cleavage of the acyl or acetonyl side chain, methyl migration, and H-migration, along with consequential inductive cleavage as predominant fragmentation routes. Based on the HR-spectral data, commonalities and differences between the analyzed compounds and fragment groups were evaluated with future applicability in structure elucidation and spectra prediction of related compounds. KW - High-resolution mass spectrometry KW - Warfarin KW - Hydroxy warfarin KW - Fragmentation pathway PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596025 DO - https://doi.org/10.1016/j.ijms.2024.117220 SN - 1387-3806 VL - 499 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-59602 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Bayerlein, Bernd A1 - von Hartrott, Philipp A1 - Waitelonis, Jörg A1 - Birkholz, Henk A1 - Portella, Pedro Dolabella A1 - Skrotzki, Birgit T1 - FAIR and Structured Data: A Domain Ontology Aligned with Standard‐Compliant Tensile Testing N2 - The digitalization of materials science and engineering (MSE) is currently leading to remarkable advancements in materials research, design, and optimization, fueled by computer‐driven simulations, artificial intelligence, and machine learning. While these developments promise to accelerate materials innovation, challenges in quality assurance, data interoperability, and data management have to be addressed. In response, the adoption of semantic web technologies has emerged as a powerful solution in MSE. Ontologies provide structured and machine‐actionable knowledge representations that enable data integration, harmonization, and improved research collaboration. This study focuses on the tensile test ontology (TTO), which semantically represents the mechanical tensile test method and is developed within the project Plattform MaterialDigital (PMD) in connection with the PMD Core Ontology. Based on ISO 6892‐1, the test standard‐compliant TTO offers a structured vocabulary for tensile test data, ensuring data interoperability, transparency, and reproducibility. By categorizing measurement data and metadata, it facilitates comprehensive data analysis, interpretation, and systematic search in databases. The path from developing an ontology in accordance with an associated test standard, converting selected tensile test data into the interoperable resource description framework format, up to connecting the ontology and data is presented. Such a semantic connection using a data mapping procedure leads to an enhanced ability of querying. The TTO provides a valuable resource for materials researchers and engineers, promoting data and metadata standardization and sharing. Its usage ensures the generation of finable, accessible, interoperable, and reusable data while maintaining both human and machine actionability. KW - Data Interoperability KW - Domain Ontology Development KW - FAIR Data Management KW - Knowledge Representation KW - Tensile Test Ontology KW - Semantic Web Technologies PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598142 DO - https://doi.org/10.1002/adem.202400138 SN - 1438-1656 SP - 1 EP - 19 PB - Wiley VHC-Verlag AN - OPUS4-59814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fardan, Ahmed A1 - Fazi, Andrea A1 - Peng, Ru Lin A1 - Mishurova, Tatiana A1 - Thuvander, Mattias A1 - Bruno, Giovanni A1 - Brodin, Håkan A1 - Hryha, Eduard T1 - Fine-Tuning Melt Pools and Microstructures: Taming Cracks in Powder Bed Fusion—Laser Beam of a non-weldable Ni-base Superalloy N2 - Powder Bed Fusion – Laser Beam (PBF-LB) of high γ’ strengthened Ni-base superalloys, such as CM247LC, is of great interest for high temperature applications in gas turbines. However, PBF-LB of CM247LC is challenging due to the high cracking susceptibility during PBF-LB processing (solidification cracking) and heat treatment (strain age cracking, mostly caused by residual stresses). This study focuses on understanding the impact of process parameters on microstructure, residual stresses and solidification cracking. Laser power (P), speed (v) and hatch spacing (h) were varied while the layer thickness (t) was fixed. The melt pool size and shape were found to be key factors in minimizing solidification cracking. Narrower and shallower melt pools, achieved using a low line energy density (LED = P/v ≤ 0.1 J/mm), gave low crack densities (0.7 mm/mm2). A tight hatch spacing (h = 0.03 mm) resulted in reduced lack of fusion porosity. Electron backscatter diffraction investigations revealed that parameters giving finer microstructure with 〈100〉crystallographic texture had low crack densities provided they were processed with a low LED. Atom probe tomography elucidated early stages of spinodal decomposition in the as-built condition, where Cr and Al cluster separately. The extent of spinodal decomposition was found to be affected by the LED and the hatch spacing. Samples with low LED and small hatch spacing showed higher degrees of spinodal decomposition. X-ray diffraction residual stress investigations revealed that the residual stress is proportional to the volumetric energy density (VED = P/(v. h. t)). Although low residual stresses can be achieved by using low VED, there is a high risk of lack of fusion. Hence, other parameters such as modified scan strategy, build plate pre-heating and pulsed laser mode, must be further explored to minimize the residual stresses to reduce the strain age cracking susceptibility. KW - Additive manufacturing KW - X-ray CT KW - Non-weldable superalloy KW - Solidification cracking PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597340 DO - https://doi.org/10.1016/j.mtla.2024.102059 SN - 2589-1529 VL - 34 IS - 102059 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-59734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Moritz A1 - Stawarczyk, Bogna A1 - Günster, Jens A1 - Zocca, Andrea T1 - Influence of additives and binder on the physical properties of dental silicate glass-ceramic feedstock for additive manufacturing N2 - Objectives The aim of the study was to investigate the impact of organic additives (binder, plasticizer, and the cross-linking ink) in the formulation of water-based feedstocks on the properties of a dental feldspathic glass-ceramic material developed for the slurry-based additive manufacturing technology “LSD-print.” Material and methods Three water-based feldspathic feedstocks were produced to study the effects of polyvinyl alcohol (AC1) and poly (sodium 4-styrenesulfonate) (AC2) as binder systems. A feedstock without organic additives was tested as the control group (CG). Disc-shaped (n = 15) and bar (n = 7) specimens were slip-cast and characterized in the green and fired states. In the green state, density and flexural strength were measured. In the fired state, density, shrinkage, flexural strength (FS), Weibull modulus, fracture toughness (KIC), Martens parameters, and microstructure were analyzed. Disc-shaped and bar specimens were also cut from commercially available CAD/CAM blocks and used as a target reference (TR) for the fired state. Results In the green state, CG showed the highest bulk density but the lowest FS, while the highest FS in the green state was achieved with the addition of a cross-linking ink. After firing, no significant differences in density and a similar microstructure were observed for all slip-cast groups, indicating that almost complete densification could be achieved. The CAD/CAM specimens showed the highest mean FS, Weibull modulus, and KIC, with significant differences between some of the slip-cast groups. Significance These results suggest that the investigated feedstocks are promising candidates for the slurry-based additive manufacturing of restorations meeting the class 1a requirements according to DIN EN ISO 6871:2019–01. KW - Firing KW - 3D-printing KW - Silicate glass-ceramics KW - Debinding PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600516 DO - https://doi.org/10.1016/j.jmbbm.2024.106563 SN - 1751-6161 VL - 155 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-60051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fareed, Adnan A1 - Rosalie, Julian M. A1 - Kar, Satyakam A1 - Fähler, Sebastian A1 - Maaß, Robert T1 - Small-scale functional fatigue of a Ni-Mn-Ga Heusler alloy N2 - Functional fatigue of shape-memory alloys is a considerable threat to the reliable service of actuation devices. Here, we demonstrate the essentially degradation-free cyclic phase-transformation behavior of Ni-Mn-Ga microcrystals up to one million stress-driven superelastic cycles. Cyclic dissipation amounts to about 1/5 of the bulk counterpart and remains unaffected during cycling, even after the introduction of dislocation structures via plastic straining. Plastic yielding and the transformation stress largely exceed the known bulk values. However, the transformation-stress is found to depend on plastic pre-straining, which suggests that the size-affected transformation stress is sensitive to the initial defect structure and that it can be tuned by a targeted introduction of dislocations. These findings demonstrate the high suitability of Ni-Mn-Ga as a robust shape-memory alloy in small-scale functional device engineering. KW - Superelasticity KW - Shape-memory alloys KW - Functional fatigue KW - Ni-Mn-Ga PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600695 DO - https://doi.org/10.1016/j.actamat.2024.119988 VL - 274 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-60069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Yi A1 - Danischewski, Julia A1 - Molnar, Brian A1 - Riedel, Jens A1 - Shelley, Jacob T1 - Manipulation of Gaseous Ions with Acoustic Fields at Atmospheric Pressure N2 - The ability to controllably move gaseous ions is an essential aspect of ion-based spectrometry (e.g., mass spectrometry and ion mobility spectrometry) as well as materials processing. At higher pressures, ion motion is largely governed by diffusion and multiple collisions with neutral gas molecules. Thus, high-pressure ion optics based on electrostatics require large fields, radio frequency drives, complicated geometries, and/or partially transmissive grids that become contaminated. Here, we demonstrate that low-power standing acoustic waves can be used to guide, block, focus, and separate beams of ions akin to electrostatic ion optics. Ions preferentially travel through the static-pressure regions (“nodes”) while neutral gas does not appear to be impacted by the acoustic field structure and continues along a straight trajectory. This acoustic ion manipulation (AIM) approach has broad implications for ion manipulation techniques at high pressure, while expanding our fundamental understanding of the behavior of ions in gases. KW - Ion mobility spectrometry KW - Acoustic KW - Mass spectrometry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600704 DO - https://doi.org/10.1021/jacs.4c01224 SP - 1 EP - 6 PB - ACS Publications AN - OPUS4-60070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maulas, Kryzzyl M. A1 - Paredes, Charla S. A1 - Tabelin, Carlito Baltazar A1 - Jose, Mark Anthony A1 - Opiso, Einstine M. A1 - Arima, Takahiko A1 - Park, Ilhwan A1 - Mufalo, Walubita A1 - Ito, Mayumi A1 - Igarashi, Toshifumi A1 - Phengsaart, Theerayut A1 - Villas, Edrhea A1 - Dagondon, Sheila L. A1 - Metillo, Ephrime B. A1 - Uy, Mylene M. A1 - Manua, Al James A. A1 - Villacorte-Tabelin, Mylah T1 - Isolation and Characterization of Indigenous Ureolytic Bacteria from Mindanao, Philippines: Prospects for Microbially Induced Carbonate Precipitation (MICP) N2 - Microbially induced carbonate precipitation (MICP), a widespread phenomenon in nature, is gaining attention as a low-carbon alternative to ordinary Portland cement (OPC) in geotechnical engineering and the construction industry for sustainable development. In the Philippines, however, very few works have been conducted to isolate and identify indigenous, urease-producing (ureolytic) bacteria suitable for MICP. In this study, we isolated seven, ureolytic and potentially useful bacteria for MICP from marine sediments in Iligan City. DNA barcoding using 16s rDNA identified six of them as Pseudomonas stutzeri, Pseudomonas pseudoalcaligenes, Bacillus paralicheniformis, Bacillus altitudinis, Bacillus aryabhattai, and Stutzerimonas stutzeri but the seventh was not identified since it was a bacterial consortium. Bio-cementation assay experiments showed negligible precipitation in the control (without bacteria) at pH 7, 8, and 9. However, precipitates were formed in all seven bacterial isolates, especially between pH 7 and 8 (0.7–4 g). Among the six identified bacterial species, more extensive precipitation (2.3–4 g) and higher final pH were observed in S. stutzeri, and B. aryabhattai, which indicate better urease production and decomposition, higher CO2 generation, and more favorable CaCO3 formation. Characterization of the precipitates by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) and attenuated total reflectance Fourier transform spectroscopy (ATR-FTIR) confirmed the formation of three carbonate minerals: calcite, aragonite, and vaterite. Based on these results, all six identified indigenous, ureolytic bacterial species from Iligan City are suitable for MICP provided that the pH is controlled between 7 and 8. To the best of our knowledge, this is the first report of the urease-producing ability and potential for MICP of P. stutzeri, P. pseudoalcaligenes, S. stutzeri, and B. aryabhattai. KW - Calcium carbonate KW - Microbially induced carbonate precipitation (MICP) KW - Ureolytic bacteria PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600888 DO - https://doi.org/10.3390/min14040339 VL - 14 IS - 4 SP - 1 EP - 15 PB - MDPI AN - OPUS4-60088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hartwig, Philipp A1 - Bakir, Nasim A1 - Gumenyuk, Andrey A1 - Scheunemann, Lisa A1 - Schröder, Jörg A1 - Rethmeier, Michael T1 - A Physically Motivated Heat Source Model for Laser Beam Welding N2 - In this contribution, we present a physically motivated heat source model for the numerical modeling of laser beam welding processes. Since the calibration of existing heat source models, such as the conic or Goldak model, is difficult, the representation of the heat source using so-called Lamé curves has been established, relying on prior Computational Fluid Dynamics (CFD) simulations. Lamé curves, which describe the melting isotherm, are used in a subsequent finite-element (FE) simulation to define a moving Dirichlet boundary condition, which prescribes a constant temperature in the melt pool. As an alternative to this approach, we developed a physically motivated heat source model, which prescribes the heat input as a body load directly. The new model also relies on prior CFD simulations to identify the melting isotherm. We demonstrate numerical results of the new heat source model on boundary-value problems from the field of laser beam welding and compare it with the prior CFD simulation and the results of the Lamé curve model and experimental data. KW - Welding simulation KW - Heat source models KW - Laser beam welding KW - Thermal analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600899 DO - https://doi.org/10.3390/met14040430 VL - 14 IS - 4 SP - 1 EP - 26 PB - MDPI CY - Basel AN - OPUS4-60089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlögl, Johanna A1 - Goldammer, Ole A1 - Bader, Julia A1 - Emmerling, Franziska A1 - Riedel, Sebastian T1 - Introducing AFS ([Al(SO3F)3]x) – a thermally stable, readily available, and catalytically active solid Lewis superacid N2 - This paper introduces the thermally stable, solid Lewis superacid aluminium tris(fluorosulfate) (AFS), that is easy-to-synthesize from commercially available starting materials. Its applicability, e.g. in catalytic C–F bond activations, is shown. KW - Lewis Acid KW - C-F activation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601001 DO - https://doi.org/10.1039/D4SC01753F SN - 2041-6520 SP - 1 EP - 7 PB - Royal Society of Chemistry (RSC) AN - OPUS4-60100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fiedler, Saskia A1 - Frenzel, Florian A1 - Würth, Christian A1 - Tavernaro, Isabella A1 - Grüne, M. A1 - Schweizer, S. A1 - Engel, A. A1 - Resch-Genger, Ute T1 - Interlaboratory Comparison on Absolute Photoluminescence Quantum Yield Measurements of Solid Light Converting Phosphors with Three Commercial Integrating Sphere Setups N2 - Scattering luminescent materials dispersed in liquid and solid matrices and luminescent powders are increasingly relevant for fundamental research and industry. Examples are luminescent nano- and microparticles and phosphors of different compositions in various matrices or incorporated into ceramics with applications in energy conversion, solid-state lighting, medical diagnostics, and security barcoding. The key parameter to characterize the performance of these materials is the photoluminescence/fluorescence quantum yield (Φf), i.e., the number of emitted photons per number of absorbed photons. To identify and quantify the sources of uncertainty of absolute measurements of Φf of scattering samples, the first interlaboratory comparison (ILC) of three laboratories from academia and industry was performed by following identical measurement protocols. Thereby, two types ofcommercial stand-alone integrating sphere setups with different illumination and detection geometries were utilized for measuring the Φf of transparent and scattering dye solutions and solid phosphors, namely, YAG:Ce optoceramics of varying surface roughness, used as converter materials for blue light emitting diodes. Special emphasis was dedicated to the influence of the measurement geometry, the optical properties of the blank utilized to determine the number of photons of the incident excitation light absorbed by the sample, and the sample-specific surface roughness. While the Φf values of the liquid samples matched between instruments, Φf measurements of the optoceramics with different blanks revealed substantial differences. The ILC results underline the importance of the measurement geometry, sample position, and blank for reliable Φf data of scattering the YAG:Ce optoceramics, with the blank’s optical properties accounting for uncertainties exceeding 20%. KW - Nano KW - Fluorescence KW - Reference material KW - Luminescence KW - Quantitative spectroscopy KW - Particle KW - Quantum yield KW - Quality assurance KW - Phosphor KW - Converter material KW - Lifetime KW - Interlaboratory comparison KW - Method KW - Uncertainty PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600945 DO - https://doi.org/10.1021/acs.analchem.4c00372 SN - 0003-2700 SP - 6730 EP - 6737 PB - ACS Publications AN - OPUS4-60094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Camplese, Davide A1 - Scarponi, Giordano Emrys A1 - Chianese, Carmela A1 - Hajhariri, Aliasghar A1 - Eberwein, Robert A1 - Otremba, Frank A1 - Cozzani, Valerio T1 - Modeling the performance of multilayer insulation in cryogenic tanks undergoing external fire scenarios N2 - Multilayer Insulation (MLI) is frequently used in vacuum conditions for the thermal insulation of cryogenic storage tanks. The severe consequences of the degradation of such materials in engulfing fire scenarios were recently evidenced by several large-scale experimental tests. In the present study, an innovative modelling approach was developed to assess the performance of heat transfer in polyester-based MLI materials for cryogenic applications under fire conditions. A specific layer-by-layer approach was integrated with an apparent kinetic thermal degradation model based on thermogravimetric analysis results. The modeling results provided a realistic simulation of the experimental data obtained by High-Temperature Thermal Vacuum Chamber tests reproducing fire exposure conditions. The model was then applied to assess the behavior of MLI systems for liquid hydrogen tanks in realistic fire scenarios. The results show that in intense fire scenarios degradation occurs rapidly, compromising the thermal insulation performances of the system within a few minutes. KW - Multilayer Insulation KW - Cryogenic Vessels KW - Liquefied Hydrogen KW - Liquefied Natural Gas KW - Safety KW - Fire PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599418 DO - https://doi.org/10.1016/j.psep.2024.04.061 SN - 0957-5820 VL - 186 SP - 1169 EP - 1182 PB - Elsevier B.V. AN - OPUS4-59941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -