TY - JOUR A1 - Villajos Collado, José Antonio A1 - Balderas‐Xicohténcatl, Rafael A1 - Al Shakhs, Ali N. A1 - Berenguer‐Murcia, Ángel A1 - Buckley, Craig E. A1 - Cazorla‐Amorós, Diego A1 - Charalambopoulou, Georgia A1 - Couturas, Fabrice A1 - Cuevas, Fermin A1 - Fairen‐Jimenez, David A1 - Heinselman, Karen N. A1 - Humphries, Terry D. A1 - Kaskel, Stefan A1 - Kim, Hyunlim A1 - Marco‐Lozar, Juan P. A1 - Oh, Hyunchul A1 - Parilla, Philip A. A1 - Paskevicius, Mark A1 - Senkovska, Irena A1 - Shulda, Sarah A1 - Silvestre‐Albero, Joaquin A1 - Steriotis, Theodore A1 - Tampaxis, Christos A1 - Hirscher, Michael A1 - Maiwald, Michael T1 - Establishing ZIF‐8 as a reference material for hydrogen cryoadsorption: An interlaboratory study N2 - AbstractHydrogen storage by cryoadsorption on porous materials has the advantages of low material cost, safety, fast kinetics, and high cyclic stability. The further development of this technology requires reliable data on the H2 uptake of the adsorbents, however, even for activated carbons the values between different laboratories show sometimes large discrepancies. So far no reference material for hydrogen cryoadsorption is available. The metal‐organic framework ZIF‐8 is an ideal material possessing high thermal, chemical, and mechanical stability that reduces degradation during handling and activation. Here, we distributed ZIF‐8 pellets synthesized by extrusion to 9 laboratories equipped with 15 different experimental setups including gravimetric and volumetric analyzers. The gravimetric H2 uptake of the pellets was measured at 77 K and up to 100 bar showing a high reproducibility between the different laboratories, with a small relative standard deviation of 3–4 % between pressures of 10–100 bar. The effect of operating variables like the amount of sample or analysis temperature was evaluated, remarking the calibration of devices and other correction procedures as the most significant deviation sources. Overall, the reproducible hydrogen cryoadsorption measurements indicate the robustness of the ZIF‐8 pellets, which we want to propose as a reference material. KW - Physical and theoretical chemistry KW - Atomic and molecular physics, and optics PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594788 DO - https://doi.org/10.1002/cphc.202300794 SN - 1439-7641 SP - 1 EP - 7 PB - Wiley CY - Weinheim AN - OPUS4-59478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaytsev, D. A1 - Funk, Alexander T1 - On the crack evolutional in human dentin under uniaxial compression imaged by high resolution tomography N2 - An observation of the fracture process in front of the crack tip inside a dentin sample by means of ex-situ X-ray computed tomography after uniaxial compression at different deformation values was carried out in this work. This ex-situ approach allowed the microstructure and fracturing process of human dentin to be observed during loading. No cracks are observed up to the middle part of the irreversible deformation in the samples at least visible at 0.4μm resolution. First cracks appeared before the mechanical stress reached the compression strength. The growth of the cracks is realized by connecting the main cracks with satellite cracks that lie ahead of the main crack tip and parallel its trajectory. When under the stress load the deformation in the sample exceeds the deformation at the compression strength of dentin, an appearance of micro-cracks in front of the main cracks is observed. The micro-cracks are inclined (~60°) to the trajectory of the main cracks. The further growth of the main cracks is not realized due to the junction with the micro-cracks; we assume that the micro-cracks dissipate the energy of the main crack and suppressed its growth. These micro-cracks serve as additional stress accommodations, therefore the samples do not break apart after the compression test, as it is usually observed under bending and tension tests. KW - Dentin KW - Crack evolution KW - Compression strength KW - Mechanical properties KW - Microstructure KW - Ex-situ X-ray computed tomography PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594810 DO - https://doi.org/10.18149/MPM.5152023_5 SN - 1605-8119 VL - 51 IS - 5 SP - 38 EP - 51 PB - Advanced Study Center CY - St. Petersburg AN - OPUS4-59481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prabitz, Konstantin Manuel A1 - Antretter, Thomas A1 - Rethmeier, Michael A1 - El-Sari, Bassel A1 - Schubert, Holger A1 - Hilpert, Benjamin A1 - Gruber, Martin A1 - Sierlinger, Robert A1 - Ecker, Werner T1 - Numerical and experimental assessment of liquid metal embrittlement in externally loaded spot welds N2 - Zinc-based surface coatings are widely applied with high-strength steels in automotive industry. Some of these base materials show an increased brittle cracking risk during loading. It is necessary to examine electrogalvanized and uncoated samples of a high strength steel susceptible to liquid metal embrittlement during spot welding with applied external load. Therefore, a newly developed tensile test method with a simultaneously applied spot weld is conducted. A fully coupled 3D electrical, thermal, metallurgical and mechanical finite element model depicting the resistant spot welding process combined with the tensile test conducted is mandatory to correct geometric influences of the sample geometry and provides insights into the sample’s time dependent local loading. With increasing external loads, the morphology of the brittle cracks formed is affected more than the crack depth. The validated finite element model applies newly developed damage indicators to predict and explain the liquid metal embrittlement cracking onset and development as well as even ductile failure. KW - Resistance spot welding KW - Finite element simulation KW - Advanced high-strength steel KW - Liquid metal embrittlement KW - Damage prediction KW - Tensile resistance spot welding experiment PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594848 DO - https://doi.org/10.1007/s40194-024-01696-7 SN - 0043-2288 SP - 1 EP - 10 PB - Springer Science and Business Media LLC AN - OPUS4-59484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asna Ashari, Parsa A1 - Blind, Knut T1 - The effects of hydrogen research and innovation on international hydrogen trade N2 - Climate change and the pressure to decarbonize, as well as energy security concerns, have drawn the attention of policymakers and the industry to hydrogen energy. To ad-vance the hydrogen economy at a global scale, research and innovation progress is of significant importance, among others. However, previous studies have provided only lim-ited quantitative evidence of the effects of research and innovation on the formation of a global hydrogen market. Instead, they postulate rather than empirically support this rela-tionship. Therefore, this study analyzes the effects of research and innovation measured by scientific publications, patents, and standards on bilateral hydrogen trade flows for 32 countries between 1995 and 2019 in a gravity model of trade, using regression analyses and Poisson Pseudo Maximum Likelihood (PPML) estimation. The main results of the PPML estimation show that research and innovation progress is indeed associated with increased trade, especially with patenting and (international) standardization enhancing hydrogen export volumes. As policy implications, we derive that increased public R&D funding can help increase the competitiveness of hydrogen energy and boost market growth, along with infrastructure support and harmonized standards and regulations. KW - Hydrogen supply KW - Global hydrogen market KW - Research and innovation KW - Push and pull effects KW - Hydrogen policies PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594875 DO - https://doi.org/10.1016/j.enpol.2023.113974 SN - 0301-4215 VL - 186 SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-59487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sordello, F. A1 - Prozzi, M. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg A1 - Pellegrino, F. T1 - Increasing the HER efficiency of photodeposited metal nanoparticles over TiO2 using controlled periodic illumination N2 - Although the use of noble metal catalysts can increase the efficiency of hydrogen evolution reaction, the process is still limited by the characteristics of the metal-hydrogen (M−H) bond, which can be too strong or too weak, depending on the metal employed. Studies revealed that the hydrogen affinity for the metal surface (i.e. H absorption/desorption) is regulated also by the potential at the metal nanoparticles. Through controlled periodic illumination (CPI) of a series of metal/TiO2 suspensions, here we demonstrated that an increase of the HER efficiency is possible for those photodeposited metals which have a Tafel slope below 125 mV. Two possible explanations are here reported, in both of them the M−H interaction and the metal covering level play a prominent role, which also depend on the prevailing HER mechanism (Volmer-Heyrovsky or Volmer-Tafel). KW - Controlled periodic illumination KW - Hydrogen evolution reaction KW - Titanium dioxide KW - Photoreforming KW - Volcano plot KW - Sabatier KW - Nanoparticles PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589875 DO - https://doi.org/10.1016/j.jcat.2023.115215 VL - 429 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-58987 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Kai A1 - Mirabella, Francesca A1 - Knigge, Xenia A1 - Mezera, Marek A1 - Weise, Matthias A1 - Sahre, Mario A1 - Wasmuth, Karsten A1 - Voss, Heike A1 - Hertwig, Andreas A1 - Krüger, Jörg A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Bonse, Jörn T1 - Chemical and topographical changes upon sub-100-nm laser-induced periodic surface structure formation on titanium alloy: the influence of laser pulse repetition rate and number of over-scans N2 - Titanium and its alloys are known to allow the straightforward laser-based manufacturing of ordered surface nanostructures, so-called high spatial frequency laser-induced periodic surface structures (HSFL). These structures exhibit sub-100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi-method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near-surface chemical analyses hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (ToF-SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non-ablative laser-induced near-surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat-accumulation effects. T2 - 2023 E-MRS Spring Meeting, Symposium L "Making light matter: lasers in material sciences and photonics" CY - Strasbourg, France DA - 29.05.2023 KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses KW - Laser processing KW - Hard X-ray photoelectron spectroscopy (HAXPES) KW - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589902 UR - https://onlinelibrary.wiley.com/doi/full/10.1002/pssa.202300719 DO - https://doi.org/10.1002/pssa.202300719 SN - 1862-6319 VL - 221 IS - 15 SP - 1 EP - 12 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-58990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jablonka, Kevin Maik A1 - Ai, Qianxiang A1 - Al-Feghali, Alexander A1 - Badhwar, Shruti A1 - Bocarsly, Joshua D. A1 - Bran, Andres M. A1 - Bringuier, Stefan A1 - Brinson, L. Catherine A1 - Choudhary, Kamal A1 - Circi, Defne A1 - Cox, Sam A1 - de Jong, Wibe A. A1 - Evans, Matthew L. A1 - Gastellu, Nicolas A1 - Genzling, Jerome A1 - Gil, María Victoria A1 - Gupta, Ankur K. A1 - Hong, Zhi A1 - Imran, Alishba A1 - Kruschwitz, Sabine A1 - Labarre, Anne A1 - Lála, Jakub A1 - Liu, Tao A1 - Ma, Steven A1 - Majumdar, Sauradeep A1 - Merz, Garrett W. A1 - Moitessier, Nicolas A1 - Moubarak, Elias A1 - Mouriño, Beatriz A1 - Pelkie, Brenden A1 - Pieler, Michael A1 - Ramos, Mayk Caldas A1 - Ranković, Bojana A1 - Rodriques, Samuel G. A1 - Sanders, Jacob N. A1 - Schwaller, Philippe A1 - Schwarting, Marcus A1 - Shi, Jiale A1 - Smit, Berend A1 - Smith, Ben E. A1 - Van Herck, Joren A1 - Völker, Christoph A1 - Ward, Logan A1 - Warren, Sean A1 - Weiser, Benjamin A1 - Zhang, Sylvester A1 - Zhang, Xiaoqi A1 - Zia, Ghezal Ahmad A1 - Scourtas, Aristana A1 - Schmidt, K. J. A1 - Foster, Ian A1 - White, Andrew D. A1 - Blaiszik, Ben T1 - 14 examples of how LLMs can transform materials science and chemistry: a reflection on a large language model hackathon N2 - Large-language models (LLMs) such as GPT-4 caught the interest of many scientists. Recent studies suggested that these models could be useful in chemistry and materials science. To explore these possibilities, we organized a hackathon. This article chronicles the projects built as part of this hackathon. Participants employed LLMs for various applications, including predicting properties of molecules and materials, designing novel interfaces for tools, extracting knowledge from unstructured data, and developing new educational applications. The diverse topics and the fact that working prototypes could be generated in less than two days highlight that LLMs will profoundly impact the future of our fields. The rich collection of ideas and projects also indicates that the applications of LLMs are not limited to materials science and chemistry but offer potential benefits to a wide range of scientific disciplines. KW - Large Language model KW - Hackathon KW - Concrete KW - Prediction KW - Inverse Design KW - Orchestration PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589961 DO - https://doi.org/10.1039/d3dd00113j VL - 2 IS - 5 SP - 1233 EP - 1250 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Torres, Benjamin Moreno A1 - Völker, Christoph A1 - Firdous, Rafia T1 - Concreting a sustainable future: A dataset of alkali-activated concrete and its properties N2 - This data article introduces a dataset comprising 1630 alkali-activated concrete (AAC) mixes, compiled from 106 literature sources. The dataset underwent extensive curation to address feature redundancy, transcription errors, and duplicate data, yielding refined data ready for further data-driven science in the field of AAC, where this effort constitutes a novelty. The carbon footprint associated with each material used in the AAC mixes, as well as the corresponding CO2 footprint of every mix, were approximated using two published articles. Serving as a foundation for future expansions and rigorous data applications, this dataset enables the characterization of AAC properties through machine learning algorithms or as a benchmark for performance comparison among different formulations. In summary, the dataset provides a resource for researchers focusing on AAC and related materials and offers insights into the environmental benefits of substituting traditional Portland concrete with AAC. KW - Multidisciplinary KW - Data Set KW - Alkali Activated Concrete KW - Data driven design PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589974 DO - https://doi.org/10.1016/j.dib.2023.109525 SN - 2352-3409 VL - 50 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-58997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Christoph A1 - Moreno Torres, Benjami A1 - Zia, Ghezal Ahmad A1 - Rug, Tehseen A1 - Firdous, Rafia A1 - Böhmer, Felix A1 - Stephan, Dietmar A1 - Kruschwitz, Sabine T1 - Presenting SLAMD – A Sequential Learning Based Software for the Inverse Design of Sustainable Cementitious Materials N2 - In recent decades, the number of components in concrete has grown, particularly in formulations aimed at reducing carbon footprints. Innovations include diverse binders, supplementary cementitious materials, activators, concrete admixtures, and recycled aggregates. These developments target not only the enhancement of material properties but also the mitigation of the ecological and economic impacts of concrete — the most extensively used material by humankind. However, these advancements also introduce a greater variability in the composition of raw materials. The material’s behavior is significantly influenced by its nanoscale properties, which can pose challenges in accurate characterization. Consequently, there’s an increasing need for experimental tuning of formulations. This is accompanied by a more inconsistent composition of raw materials, which makes an experimental tuning of formulations more and more necessary. However, the increased complexity in composition presents a challenge in finding the ideal formulation through trial and error. Inverse design (ID) techniques offer a solution to this challenge by allowing for a comprehensive search of the entire design space to create new and improved concrete formulations. In this publication, we introduce the concept of ID and demonstrate how our open-source app “SLAMD” provides all necessary steps of the workflow to adapt it in the laboratory, lowering the application barriers. The intelligent screening process, guided by a predictive model, leads to a more efficient and effective data-driven material design process resulting in reduced carbon footprint and improved material quality while considering socio-economic factors in the materials design. KW - Sustainable concrete KW - Machine learning optimization KW - Inverse design techniques KW - Scientific software KW - Data-driven material design PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589993 DO - https://doi.org/10.17756/nwj.2023-s2-032 VL - 9 SP - 180 EP - 187 AN - OPUS4-58999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabo Rios, Alberto A1 - Mishurova, Tatiana A1 - Cordova, Laura A1 - Persson, Mats A1 - Bruno, Giovanni A1 - Olevsky, Eugene A1 - Hryha, Eduard T1 - Ex-situ characterization and simulation of density fluctuations evolution during sintering of binder jetted 316L N2 - Efficient density evolution during sintering of the as-printed component is vital to reach full densification and required properties of binder jet (BJT) components. However, due to the high porosity and brittle nature of the green compact, analysis of the microstructure development during sintering is very difficult, resulting in lack of understanding of the densification process. Density development from green state (57 ± 1.6 %) up to full density (99 ± 0.3 %) was characterized by high-resolution synchrotron X-Ray computed tomography (SXCT) on BJT 316L samples from ex-situ interrupted sintering tests. Periodicity of density fluctuations along the building direction was revealed for the first time and was related to the layer thickness of ~ 42 μm during printing that decreased down to ~ 33 μm during sintering. Sintering simulations, utilizing a continuum sintering model developed for BJT, allowed to replicate the density evolution during sintering with a mean error of 2 % and its fluctuation evolution from green (1.66 %) to sintered (0.56 %) state. Additionally, simulation of extreme particle size segregation (1 μm to 130 μm) suggested that non-optimized printing could lead to undesirable density fluctuation amplitude rapid increase (~10 %) during sintering. This might trigger the nucleation of defects (e.g., layer delamination, cracking, or excessive residual porosity) during the sintering process. KW - Additive manufacturing KW - Synchrotron X-ray CT KW - Binder Jetting KW - Sintering KW - FEM Simulation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594389 DO - https://doi.org/10.1016/j.matdes.2024.112690 SN - 0264-1275 VL - 238 SP - 1 EP - 18 PB - Elsevier AN - OPUS4-59438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jovičević-Klug, Matic A1 - Souza Filho, Isnaldi R. A1 - Springer, Hauke A1 - Adam, Christian A1 - Raabe, Dierk T1 - Green steel from red mud through climate-neutral hydrogen plasma reduction N2 - AbstractRed mud is the waste of bauxite refinement into alumina, the feedstock for aluminium production1. With about 180 million tonnes produced per year1, red mud has amassed to one of the largest environmentally hazardous waste products, with the staggering amount of 4 billion tonnes accumulated on a global scale1. Here we present how this red mud can be turned into valuable and sustainable feedstock for ironmaking using fossil-free hydrogen-plasma-based reduction, thus mitigating a part of the steel-related carbon dioxide emissions by making it available for the production of several hundred million tonnes of green steel. The process proceeds through rapid liquid-state reduction, chemical partitioning, as well as density-driven and viscosity-driven separation between metal and oxides. We show the underlying chemical reactions, pH-neutralization processes and phase transformations during this surprisingly simple and fast reduction method. The approach establishes a sustainable toxic-waste treatment from aluminium production through using red mud as feedstock to mitigate greenhouse gas emissions from steelmaking. KW - Multidisciplinary PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594424 DO - https://doi.org/10.1038/s41586-023-06901-z SN - 0028-0836 VL - 625 IS - 7996 SP - 703 EP - 709 PB - Springer Science and Business Media LLC AN - OPUS4-59442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Vinzenz A1 - Fasselt, Janek Maria A1 - Kruse, Tobias A1 - Klötzer, Christian A1 - Kleba-Ehrhardt, Rafael A1 - Choma, Tomasz A1 - Biegler, Max A1 - Rethmeier, Michael T1 - Using ultrasonic atomization to recycle aluminium bronze chips for additive laser directed energy deposition N2 - Abstract In the post-processing of large maritime components, a considerable amount of waste in the form of milling and grinding chips is produced. At the same time, additive manufacturing technologies have shown great potential in producing high-volume parts for maritime applications, allowing novel design approaches and short lead times. In this context, this study presents a sustainable approach to recycle and use aluminium bronze waste material, generated during post-processing of large cast ship propellers, as feedstock for laser-powder directed energy deposition. The recycling technology used to produce powder batches is inductive re-melting in combination with ultrasonic atomization. The derived metal powders are characterized using digital image analysis, powder flowability tests, scanning electron microscopy as well as energy dispersive X-ray spectroscopy. Compared to conventional metal powders produced by gas atomization, the recycled material shows excellent sphericity and a powder size distribution with a higher content of finer and coarser particles. Metallographic sections of deposited additively produced specimens show an increased hardness and reduced ductility, but also competitive densities and higher yield and ultimate tensile strength compared to cast material. The process chain shows high potential for the maritime sector to enable circular and sustainable manufacturing. KW - Industrial and Manufacturing Engineering PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594444 DO - https://doi.org/10.1088/1757-899X/1296/1/012036 VL - 1296 IS - 1 SP - 1 EP - 11 PB - IOP Publishing AN - OPUS4-59444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kornev, Roman A1 - Gornushkin, Igor B. A1 - Shabarova, Lubov A1 - Kadomtseva, Alena A1 - Mochalov, Georgy A1 - Rekunov, Nikita A1 - Romanov, Sergey A1 - Medov, Vitaly A1 - Belousova, Darya A1 - Maleev, Nikita T1 - Plasma-Chemical Disposal of Silicon and Germanium Tetrachlorides Waste by Hydrogen Reduction N2 - The processes of hydrogen reduction of silicon and germanium chlorides under the conditions of high-frequency (40.68 MHz) counteracted arc discharge stabilized between two rod electrodes are investigated. The main gas-phase and solid products of plasma-chemical transformations are determined. Thermodynamic analysis of SiCl4 + H2 and GeCl4 + H2 systems for optimal process parameters was carried out. Using the example of hydrogen reduction of SiCl4 by the method of numerical modeling, gas-dynamic and thermal processes for this type of discharge are investigated. The impurity composition of gas-phase and solid reaction products is investigated. The possibility of single-stage production of high-purity Si and Ge mainly in the form of compact ingots, as well as high-purity chlorosilanes and trichlorogermane, is shown. KW - High-frequency arc discharge KW - Hydrogen reduction KW - Silicon chlorides KW - Germanium chlorides PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594454 DO - https://doi.org/10.3390/sci6010001 VL - 6 IS - 1 SP - 1 EP - 12 PB - MDPI AG AN - OPUS4-59445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esparza-Mora, M. Alejandra A1 - Mazumdar, Tilottama A1 - Jiang, Shixiong A1 - Radek, Renate A1 - Thiem, Julian N. A1 - Feng, Linshan A1 - Petrašiūnaitė, Vesta A1 - Banasiak, Ronald A1 - Golian, Marek A1 - Gleske, Melanie A1 - Christophe, Lucas A1 - Springer, Andreas A1 - Buellesbach, Jan A1 - McMahon, Dino T1 - Defensive behavior is linked to altered surface chemistry following infection in a termite society N2 - The care-kill response determines whether a sick individual will be treated or eliminated from an insect society, but little is known about the physiological underpinnings of this process. We exploited the stepwise infection dynamics of an entomopathogenic fungus in a termite to explore how care-kill transitions occur, and identify the chemical cues behind these shifts. We found collective responses towards pathogen-injected individuals to vary according to severity and timing of pathogen challenge, with elimination, via cannibalism, occurring sooner in response to a severe active infection. However, injection with inactivated fungal blastospores also resulted in increased albeit delayed cannibalism, even though it did not universally cause host death. This indicates that the decision to eliminate an individual is triggered before pathogen viability or terminal disease status has been established. We then compared the surface chemistry of differently challenged individuals, finding increased amounts of long-chained methyl-branched alkanes with similar branching patterns in individuals injected with both dead and viable fungal blastospores, with the latter showing the largest increase. This coincided with the highest amounts of observed cannibalism as well as signs of severe moribundity. Our study provides new mechanistic insight into the emergent collective behaviors involved in the disease defense of a termite society. KW - Termite KW - Social Immunity KW - CHC KW - Pathogen PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594468 DO - https://doi.org/10.1038/s41598-023-42947-9 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 16 PB - Macmillan Publishers Limited, part of Springer Nature CY - London AN - OPUS4-59446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böllinghaus, Thomas A1 - Cross, Carl T1 - Obituary: Prof. Dr.-Ing. Hans Hoffmeister N2 - On November 3, 2023, our dear colleague, Prof. Dr.-Ing. Hans Hoffmeister, born in 1932 in Kassel, Germany, passed away in Ahrensburg, near Hamburg, Germany. KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594160 DO - https://doi.org/10.1007/s40194-023-01675-4 SP - 1 EP - 2 PB - Springer Science and Business Media LLC AN - OPUS4-59416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohring, W. A1 - Karafiludis, Stephanos A1 - Manzoni, Anna M. A1 - Laplanche, G. A1 - Schneider, M. A1 - Stephan-Scherb, C. T1 - High-Temperature Corrosion of High- and Medium-Entropy Alloys CrMnFeCoNi and CrCoNi Exposed to a Multi-Oxidant Atmosphere H2O–O2–SO2 N2 - AbstractThe high-temperature corrosion behaviors of the equimolar CrCoNi medium-entropy alloy and CrMnFeCoNi high-entropy alloy were studied in a gas atmosphere consisting of a volumetric mixture of 10% H2O, 2% O2, 0.5% SO2, and 87.5% Ar at 800 °C for up to 96 h. Both alloys were initially single-phase fcc with a mean grain size of ~ 50 μm and a homogeneous chemical composition. The oxide layer thickness of CrMnFeCoNi increased linearly with exposure time while it remained constant at ~ 1 μm for CrCoNi. A Cr2O3 layer and minor amounts of (Co,Ni)Cr2O4 developed on the latter while three oxide layers were detected on the former, i.e., a thin and continuous chromium rich oxide layer at the oxide/alloy interface, a dense (Mn,Cr)3O4 layer in the center and a thick and porous layer of Mn3O4 and MnSO4 at the gas/oxide interface. Additionally, a few metal sulfides were observed in the CrMnFeCoNi matrix. These results were found to be in reasonable agreement with thermodynamic calculations. KW - high entropy alloys KW - corrosion KW - oxidation KW - scanning electron microscopy KW - sulfidation KW - CrMnFeCoNi PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594189 DO - https://doi.org/10.1007/s44210-023-00026-8 SP - 1 EP - 17 PB - Springer Science and Business Media LLC AN - OPUS4-59418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emamverdi, Farnaz A1 - Huang, J. A1 - Mosane Razavi, Negar A1 - Bojdys, M. J. A1 - Forster, A. B. A1 - Budd, P. M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Mobility and Gas Transport Properties of Mixed Matrix Membranes Based on PIM‑1 and a Phosphinine Containing Covalent Organic Framework N2 - Polymers with intrinsic microporosity (PIMs) are gaining attention as gas separation membranes. Nevertheless, they face limitations due to pronounced physical aging. In this study a covalent organic framework containing λ5-phosphinine moieties, CPSF-EtO were incorporated as a nanofiller (concentration range 0-10 wt%) into a PIM-1 matrix forming dense films with a thickness of ca. 100 μm. The aim of the investigation was to investigate possible enhancements of gas transport properties and mitigating effects on physical aging. The incorporation of the nanofiller occurred on aggregate level with domains up to 100 nm as observed by T-SEM and confirmed by X-ray scattering. Moreover, the X-ray data show that the structure of the microporous network of the PIM-1 matrix is changed by the nanofiller. As the molecular mobility is fundamental for gas transport as well as for physical aging, the study includes dielectric investigations of pure PIM-1 and PIM-1/CPSF-EtO mixed matrix membranes to establish a correlation between the molecular mobility and the gas transport properties. Using the time-lag method the gas permeability and the permselectivity were determined for N2, O2, CH4 and CO2 for samples with variation in filler content. A significant increase in the permeability of CH4 and CO2 (50 % increase compared to pure PIM-1) was observed for a concentration of 5 wt% of the nanofiller. Furthermore, the most pronounced change in the permselectivity was found for the gas pair CO2/N2 at a filler concentration of 7 wt%. KW - Polymers of Intrinsic Microporosity KW - Nanocomposites PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595031 DO - https://doi.org/10.1021/acs.macromol.3c02419 SN - 0024-9297 VL - 57 IS - 4 SP - 1829 EP - 1845 PB - ACS Publications AN - OPUS4-59503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pérez Blanes, H. A1 - Ghiasi, P. A1 - Sandkühler, J. A1 - Yesilcicek, Yasemin A1 - Pentzien, Simone A1 - Conradi, Andrea A1 - Prinz, Carsten A1 - Al-Sabbagh, Dominik A1 - Thünemann, Andreas A1 - Ozcan, Ozlem A1 - Witt, Julia T1 - High CO2 reduction activity on AlCrCoCuFeNi multi-principal element alloy nanoparticle electrocatalysts prepared by means of pulsed laser ablation N2 - Noble metal-free nanoparticles (NPs) based on multi-principal element alloys (MPEAs) were synthesized using a one-step pulsed laser ablation in liquids (PLALs) method for the electrochemical reduction of CO2. Laser ablation was performed in pure water or poly-(diallyldimethylammonium chloride) (PDADMAC)-containing an aqueous solution of Al8Cr17Co17Cu8Fe17Ni33 MPEA targets. Transmission electron microscopy (TEM) measurements combined with energy dispersive X-ray (EDX) mapping were used to characterize the structure and composition of the laser-generated MPEA nanoparticles (MPEA-NPs). These results confirmed the presence of a characteristic elemental distribution of a core-shell phase structure as the predominant NP species. The electrocatalytic performance of the laser-generated MPEA-NPs was characterized by linear sweep voltammetry (LSV) demonstrating an enhanced electrocatalytic CO2 activity for PDADMAC-stabilized NPs. The findings of these investigations indicate that MPEAs have great potential to replace conventional, expensive noble metal electrocatalysts. KW - Multi-principal element alloys KW - Chemically Complex Materials KW - CCMat KW - Electrocatalysis KW - Carbon dioxide reduction KW - Pulsed laser ablation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594018 DO - https://doi.org/10.1016/j.jmrt.2023.05.143 VL - 24 SP - 9434 EP - 9440 PB - Elsevier BV AN - OPUS4-59401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Maack, Stefan A1 - Strangfeld, Christoph T1 - Fluidic Ultrasound Generation for Non‐Destructive Testing N2 - AbstractAir‐coupled ultrasonic testing (ACU) is a pioneering technique in non‐destructive testing (NDT). While contact testing and fluid immersion testing are standard methods in many applications, the adoption of ACU is progressing slowly, especially in the low ultrasonic frequency range. A main reason for this development is the difficulty of generating high amplitude ultrasonic bursts with equipment that is robust enough to be applied outside a laboratory environment. This paper presents the fluidic ultrasonic transducer as a solution to this challenge. This novel aeroacoustic source uses the flow instability of a sonic jet in a bistable fluidic switch to generate ultrasonic bursts up to 60 kHz with a mean peak pressure of 320 Pa. The robust design allows operation in adverse environments, independent of the operating fluid. Non‐contact through‐transmission experiments are conducted on four materials and compared with the results of conventional transducers. For the first time, it is shown that the novel fluidic ultrasonic transducer provides a suitable acoustic signal for NDT tasks and has potential of furthering the implementation of ACU in industrial applications.This article is protected by copyright. All rights reserved KW - Aeroacoustics KW - Air-coupled ultrasound KW - Fluidics KW - Harsh environment KW - Laser Doppler vibrometer KW - Non-destructive testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594273 DO - https://doi.org/10.1002/adma.202311724 SN - 0935-9648 SP - 1 EP - 14 PB - Wiley AN - OPUS4-59427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Maack, Stefan T1 - Improving onset picking in ultrasonic testing by using a spectral entropy criterion N2 - In ultrasonic testing, material and structural properties of a specimen can be derived from the time-of-flight (ToF). Using signal features, such as the first peak or envelope maximum, to calculate the ToF is error-prone in multipath arrangements or dispersive and attenuating materials, which is not the case for the signal onset. Borrowing from seismology, researchers used the Akaike information criterion (AIC) picker to automatically determine onset times. The most commonly used formulation, Maeda's AIC picker, is reassessed and found to be based on inappropriate assumptions for signals often used in ultrasonic testing and dependent on arbitrary parameters. Consequently, an onset picker for ultrasonic through-transmission measurements is proposed, based on a spectral entropy criterion (SEC) to model the signal using the AIC framework. This SEC picker takes into account the spectral properties of the ultrasonic signal and is virtually free of arbitrary parameters. Synthetic and experimental data are used to compare the performance of SEC and AIC pickers. It is shown that the accuracy of onset picking is improved for densely sampled data. KW - Akaike information criterion picker KW - Nondestructive testing KW - Ultrasound KW - Time of flight PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594284 UR - https://pubs.aip.org/asa/jasa/article/155/1/544/3061576/Improving-onset-picking-in-ultrasonic-testing-by DO - https://doi.org/10.1121/10.0024337 SN - 0001-4966 VL - 155 IS - 1 SP - 544 EP - 554 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-59428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Z. A1 - Raab, A. A1 - Kolmangadi, Mohamed Aejaz A1 - Busch, M. A1 - Grunwald, M. A1 - Demel, F. A1 - Bertram, F. A1 - Kityk, A. V. A1 - Schönhals, Andreas A1 - Laschat, S. A1 - Huber, P. T1 - Self-Assembly of Ionic Superdiscs in Nanopores N2 - Discotic ionic liquid crystals (DILCs) consist of self-assembled superdiscs of cations and anions that spontaneously stack in linear columns with high one-dimensional ionic and electronic charge mobility, making them prominent model systems for functional soft matter. Compared to classical nonionic discotic liquid crystals, many liquid crystalline structures with a combination of electronic and ionic conductivity have been reported, which are of interest for separation membranes, artificial ion/proton conducting membranes, and optoelectronics. Unfortunately, a homogeneous alignment of the DILCs on the macroscale is often not achievable, which significantly limits the applicability of DILCs. Infiltration into nanoporous solid scaffolds can, in principle, overcome this drawback. However, due to the experimental challenges to scrutinize liquid crystalline order in extreme spatial confinement, little is known about the structures of DILCs in nanopores. Here, we present temperaturedependent high-resolution optical birefringence measurement and 3D reciprocal space mapping based on synchrotron X-ray scattering to investigate the thermotropic phase behavior of dopamine-based ionic liquid crystals confined in cylindrical channels of 180 nm diameter in macroscopic anodic aluminum oxide membranes. As a function of the membranes’ hydrophilicity and thus the molecular anchoring to the pore walls (edge-on or face-on) and the variation of the hydrophilic−hydrophobic balance between the aromatic cores and the alkyl side chain motifs of the superdiscs by tailored chemical synthesis, we find a particularly rich phase behavior, which is not present in the bulk state. It is governed by a complex interplay of liquid crystalline elastic energies (bending and splay deformations), polar interactions, and pure geometric confinement and includes textural transitions between radial and axial alignment of the columns with respect to the long nanochannel axis. Furthermore, confinement-induced continuous order formation is observed in contrast to discontinuous first-order phase transitions, which can be quantitatively described by Landau-de Gennes free energy models for liquid crystalline order transitions in confinement. Our observations suggest that the infiltration of DILCs into nanoporous solids allows tailoring their nanoscale texture and ion channel formation and thus their electrical and optical functionalities over an even wider range than in the bulk state in a homogeneous manner on the centimeter scale as controlled by the monolithic nanoporous scaffolds. KW - Ionic Liquid Crystals KW - Nanopropous materials KW - Landau de-Gennes analysis KW - X-ray scattering KW - Optical birefringence PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600797 DO - https://doi.org/10.1021/acsnano.4c01062 SN - 1936-0851 VL - 18 IS - 22 SP - 14414 EP - 14426 PB - ACS AN - OPUS4-60079 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kingsbery, P. A1 - Manzoni, Anna M. A1 - Suárez Ocano, Patricia A1 - Többens, D. M. A1 - Stephan‐Scherb, C. T1 - High‐temperature KCl‐induced corrosion of high Cr and Ni alloys investigated by in‐situ diffraction N2 - High‐temperature KCl‐induced corrosion in laboratory air was observed in situ utilizing X‐ray diffraction. High Cr‐containing model alloys (Fe‐13Cr, Fe‐18Cr‐12Ni, and Fe‐25Cr‐20Ni) were coated with KCl and exposed to dry air at 560°C. KCl‐free alloys were studied in the equivalent atmosphere as a reference. After exposure to KCl‐free environments, all alloys showed the formation of very thin oxide layers, indicating good corrosion resistance. In contrast, KCl‐bearing alloys showed distinct damage after exposure. KW - Corrosion KW - In-situ diffraction KW - High-temperature corrosion PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600831 DO - https://doi.org/10.1002/maco.202314224 SN - 0947-5117 SP - 1 EP - 10 PB - Wiley VHC-Verlag AN - OPUS4-60083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Christian A1 - Thore, Johannes A1 - Clozel, Mélanie A1 - Günster, Jens A1 - Wilbig, Janka A1 - Meyer, Andreas T1 - Additive manufacturing of metallic glass from powder in space N2 - Additive manufacturing of metals – and in particular building with laser-based powder bed fusion – is highly flexible and allows high-resolution features and feedstock savings. Meanwhile, though space stations in low Earth orbit are established, a set of visits to the Moon have been performed, and humankind can send out rovers to explore Venus and Mars, none of these milestone missions is equipped with technology to manufacture functional metallic parts or tools in space. In order to advance space exploration to long-term missions beyond low Earth orbit, it will be crucial to develop and employ technology for in-space manufacturing (ISM) and in-situ resource utilisation (ISRU). To use the advantages of laser-based powder bed fusion in these endeavours, the challenge of powder handling in microgravity must be met. Here we present a device capable of building parts using metallic powders in microgravity. This was proven on several sounding rocket flights, on which occasions Zr-based metallic glass parts produced by additive manufacturing in space were built. The findings of this work demonstrate that building parts using powder feedstock, which is more compact to transport into space than wire, is possible in microgravity environments. This thus significantly advances ISRU and ISM and paves the way for future tests in prolonged microgravity settings. KW - Metallic Glass KW - Additive Manufacturing KW - Space PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600667 DO - https://doi.org/10.1038/s41526-023-00327-7 VL - 9 SP - 1 EP - 9 PB - Springer Nature AN - OPUS4-60066 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 - 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 - 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 - Eberwein, Robert A1 - Hajhariri, Aliasghar A1 - Davide, Camplese A1 - Giordano, Emrys Scarponi A1 - Valerio, Cozzani A1 - Frank, Otremba T1 - Experimental investigation on the behavior of thermal super insulation materials for cryogenic storage tanks in fire incidents N2 - The number of vehicles using or transporting cryogenic fuels such as Liquefied Hydrogen (LH2) or Liquefied Natural Gas (LNG) increases fast in the land transportation sector. Does this also entail new risks? The storage of cryogenic fuels requires tanks with Thermal Super Insulations (TSI) to keep the fluid cold and limit the formation of boil-off gas. TSI has proven itself in some applications since the middle of the 20th century, but in the land transport sector they are still quite new, where accidents involving fires, collisions, and their combination are to be expected. This work focuses on investigating the behavior of different types of TSI while exposed to a heat source representing a fire. To this aim, a High-Temperature Thermal Vacuum Chamber (HTTVC) was applied, which allows the thermal loading of a thermal insulation material in a vacuum and measuring the heat flow transported through the TSI in parallel. In this study, the results of 6 samples are presented regarding 3 types of MLI, rock wool, perlites, and microspheres. The thermal exposure caused different effects on the samples. In practice, this can be connected to the rapid release of flammable gases as well as to a Boiling Liquid Expanding Vapour Explosion (BLEVE). These results are relevant for reducing the risks to people and infrastructures in the progressive establishment of tanks for cryogenic fluids in our industry and society. The data presented in the study can be used to improve the design of tanks and TSIs, the assessment of accident scenarios, and the development of measures for first responders. KW - Liquefied hydrogen KW - Liquefied natural gas KW - Tanks KW - Fire KW - Insulation KW - MLI KW - Perlite KW - Rock wool KW - Microspheres PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599947 DO - https://doi.org/10.1016/j.psep.2024.04.131 SN - 0957-5820 VL - 187 SP - 240 EP - 248 PB - Elsevier AN - OPUS4-59994 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 - Elert, Anna Maria A1 - Chen, Yong-Cin A1 - Smales, Glen J. A1 - Topolniak, Ievgeniia A1 - Sturm, Heinz A1 - Schönhals, Andreas A1 - Szymoniak, Paulina T1 - Effects of the charge density of nanopapers based on carboxymethylated cellulose nanofibrils investigated by complementary techniques N2 - Cellulose nanofibrils (CNFs) with different charge densities were prepared and investigated by a combination of different complementary techniques sensitive to the structure and molecular dynamics of the system. The morphology of the materials was investigated by scanning electron microscopy (SEM) and X-ray scattering (SAXS/WAXS). The latter measurements were quantitatively analyzed yielding to molecular parameters in dependence of the charge density like the diameter of the fibrils, the distance between the fibrils, and the dimension of bundles of nanofibrils, including pores. The influence of water on the properties and the charge density is studied by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and broadband dielectric spectroscopy. The TGA measurements reveal two mass loss processes. The one at lower temperatures was related to the loss of water, and the second process at higher temperatures was related to the chemical decomposition. The resulting char yield could be correlated to the distance between the microfibrils. The DSC investigation for hydrated CNFs revealed three glass transitions due to the cellulose segments surrounded by water molecules in different states. In the second heating scan, only one broad glass transition is observed. The dielectric spectra reveal two relaxation processes. At low temperatures or higher frequencies, the β-relaxation is observed, which is assigned to localized fluctuation of the glycosidic linkage. At higher temperatures and lower frequencies, the α-relaxation takes places. This relaxation is due to cooperative fluctuations in the cellulose segments. Both processes were quantitatively analyzed. The obtained parameters such as the relaxation rates were related to both the morphological data, the charge density, and the content of water for the first time. KW - Cellulose nanofibrils PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600528 DO - https://doi.org/https://doi.org/10.1021/acsomega.4c00255 SN - 2470-1343 VL - 9 SP - 20152 EP - 20166 PB - ACS AN - OPUS4-60052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silbernagl, Dorothee A1 - Szymoniak, Paulina A1 - Tavasolyzadeh, Zeynab A1 - Sturm, Heinz A1 - Topolniak, Ievgeniia T1 - Multiphoton lithography of interpenetrating polymer networks for tailored microstructure thermal and micromechanical properties N2 - Multiphoton lithography (MPL), an emerging truly 3D microfabrication technique, exhibits substantial potential in biomedical applications, including drug delivery and tissue engineering. Fabricated micro-objects are often expected to undergo shape morphing or bending of the entire structure or its parts. Furthermore, ensuring precise property tuning is detrimental to the realization of the functionality of MPL microstructures. Herein, novel MPL materials based on interpenetrating polymer networks (IPNs) are presented that effectively combine the advantages of acrylate and epoxy systems. IPNs with varying component ratios are investigated for their microfabrication performance and structural integrity with respect to thermal and micromechanical properties. A variety of high-resolution techniques is applied to comprehensively evaluate IPN properties at the bulk, micron, and segmental levels. This study shows that the MPL laser scanning velocity and power, photoinitiator content, and multi-step exposure can be used to tune the morphology and properties of the IPN. As a result, a library of 3D MPL IPN microstructures with high 3D structural stability and tailored thermal and micromechanical properties is achieved. New IPN microstructures with Young’s moduli of 3–4 MPa demonstrate high-to-fully elastic responses to deformations, making them promising for applications in morphable microsystems, soft micro-robotics, and cell engineering. KW - Interpenetrating polymer network KW - Multiphoton lithography KW - Atomic force microscopy KW - Intermodulation AFM KW - Fast scanning calorimetry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600593 DO - https://doi.org/10.1002/smll.202310580 SN - 1613-6810 SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-60059 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 - Feng, W. A1 - Gemming, T. A1 - Giebeler, L. A1 - Qu, J. A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, B. A1 - Gonzalez-Martinez, I. T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as ‘‘electron beam-induced fragmentation’’ or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field 𝐵 = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. 𝐵 = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy KW - Electron beam-induced charging PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600170 DO - https://doi.org/10.1016/j.ultramic.2024.113978 VL - 262 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-60017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ratkovac, Mirjana A1 - Gerards-Wünsche, Paul A1 - Thiele, Marc A1 - Brackrock, Daniel A1 - Stamm, Michael T1 - Detection and monitoring of the fatigue crack growth on welds – Application-oriented use of NDT methods N2 - Early detection of fatigue cracks and accurate measurements of the crack growth play an important role in the maintenance and repair strategies of steel structures exposed to cyclic loads during their service life. Observation of welded connections is especially of high relevance due to their higher susceptibility to fatigue damage. The aim of this contribution was to monitor fatigue crack growth in thick welded specimens during fatigue tests as holistically as possible, by implementing multiple NDT methods simultaneously in order to record the crack initiation and propagation until the final fracture. In addition to well-known methods such as strain gauges, thermography, and ultrasound, the crack luminescence method developed at the Bundesanstalt für Materialforschung und -prüfung (BAM), which makes cracks on the surface particularly visible, was also used. For data acquisition, a first data fusion concept was developed and applied in order to synchronize the data of the different methods and to evaluate them to a large extent automatically. The resulting database can ultimately also be used to access, view, and analyze the experimental data for various NDT methods. During the conducted fatigue tests, the simultaneous measurements of the same cracking process enabled a comprehensive comparison of the methods, highlighting their individual strengths and limitations. More importantly, they showed how a synergetic combination of different NDT methods can be beneficial for implementation in large-scale fatigue testing but also in monitoring and inspection programs of in-service structures - such as the support structures of offshore wind turbines. T2 - Fatigue Design 2023 (FatDes 2023) CY - Senlis, France DA - 29.11.2023 KW - Fatigue KW - Welded KW - NDT KW - Crack growth PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600238 DO - https://doi.org/10.1016/j.prostr.2024.03.062 VL - 57 SP - 560 EP - 568 PB - Elsevier B.V. AN - OPUS4-60023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, Wen A1 - Gemming, Thomas A1 - Giebeler, Lars A1 - Qu, Jiang A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, Bernd A1 - González-Martínez, Ignacio T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600247 DO - https://doi.org/10.1016/j.ultramic.2024.113978 SN - 0304-3991 VL - 262 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-60024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zia, Ghezal Ahmad Jan A1 - Hanke, Thomas A1 - Skrotzki, Birgit A1 - Völker, Christoph A1 - Bayerlein, Bernd T1 - Enhancing Reproducibility in Precipitate Analysis: A FAIR Approach with Automated Dark-Field Transmission Electron Microscope Image Processing N2 - AbstractHigh-strength aluminum alloys used in aerospace and automotive applications obtain their strength through precipitation hardening. Achieving the desired mechanical properties requires precise control over the nanometer-sized precipitates. However, the microstructure of these alloys changes over time due to aging, leading to a deterioration in strength. Typically, the size, number, and distribution of precipitates for a quantitative assessment of microstructural changes are determined by manual analysis, which is subjective and time-consuming. In our work, we introduce a progressive and automatable approach that enables a more efficient, objective, and reproducible analysis of precipitates. The method involves several sequential steps using an image repository containing dark-field transmission electron microscopy (DF-TEM) images depicting various aging states of an aluminum alloy. During the process, precipitation contours are generated and quantitatively evaluated, and the results are comprehensibly transferred into semantic data structures. The use and deployment of Jupyter Notebooks, along with the beneficial implementation of Semantic Web technologies, significantly enhances the reproducibility and comparability of the findings. This work serves as an exemplar of FAIR image and research data management. KW - Industrial and Manufacturing Engineering KW - General Materials Science KW - Automated image analysis KW - FAIR research data management KW - Reproducibility KW - microstructural changes PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593905 DO - https://doi.org/10.1007/s40192-023-00331-5 SN - 2193-9772 SP - 1 EP - 15 PB - Springer Science and Business Media LLC CY - Heidelberg AN - OPUS4-59390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieg, Holger A1 - Schaar, Caroline A1 - Fouquet, Nicole A1 - Böhmert, Linda A1 - Thünemann, Andreas A1 - Braeuning, Albert T1 - Particulate iron oxide food colorants (E 172) during artificial digestion and their uptake and impact on intestinal cells N2 - Iron oxide of various structures is frequently used as food colorant (E 172). The spectrum of colors ranges from yellow over orange, red, and brown to black, depending on the chemical structure of the material. E 172 is mostly sold as solid powder. Recent studies have demonstrated the presence of nanoscaled particles in E 172 samples, often to a very high extent. This makes it necessary to investigate the fate of these particles after oral uptake. In this study, 7 differently structured commercially available E 172 food colorants (2 x Yellow FeO(OH), 2 x Red Fe2O3, 1 x Orange Fe2O3 + FeO(OH) and 2 x Black Fe3O4) were investigated for particle dissolution, ion release, cellular uptake, crossing of the intestinal barrier and toxicological impact on intestinal cells. Dissolution was analyzed in water, cell culture medium and artificial digestion fluids. Small-angle X-ray scattering (SAXS) was employed for determination of the specific surface area of the colorants in the digestion fluids. Cellular uptake, transport and toxicological effects were studied using human differentiated Caco-2 cells as an in vitro model of the intestinal barrier. For all materials, a strong interaction with the intestinal cells was observed, albeit there was only a limited dissolution, and no toxic in vitro effects on human cells were recorded. KW - Toxicology KW - Nanoparticles KW - Small-angle X-ray scattering KW - SAXS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593935 DO - https://doi.org/10.1016/j.tiv.2024.105772 VL - 96 SP - 1 EP - 12 PB - Elsevier BV AN - OPUS4-59393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Maxi B. A1 - Böhmert, Linda A1 - Thünemann, Andreas A1 - Loeschner, Katrin A1 - Givelet, Lucas A1 - Fahrenson, Christoph A1 - Braeuning, Albert A1 - Sieg, Holger T1 - Influence of artificial digestion on characteristics and intestinal cellular effects of micro-, submicro- and nanoplastics N2 - The production of plastics is rising since they have been invented. Micro, submicro- and nanoplastics are produced intentionally or generated by environmental processes, and constitute ubiquitous contaminants which are ingested orally by consumers. Reported health concerns include intestinal translocation, inflammatory response, oxidative stress and cytotoxicity. Every digestive milieu in the gastrointestinal tract does have an influence on the properties of particles and can cause changes in their effect on biological systems. In this study, we subjected plastic particles of different materials (polylactic acid, polymethylmethacrylate, melamine formaldehyde) and sizes (micro- to nano-range) to a complex artificial digestion model consisting of three intestinal fluid simulants (saliva, gastric and intestinal juice). We monitored the impact of the digestion process on the particles by performing Dynamic Light Scattering, Scanning Electron Microscopy and Asymmetric Flow Field-Flow Fractionation. An in vitro model of the intestinal epithelial barrier was used to monitor cellular effects and translocation behavior of (un)digested particles. In conclusion, artificial digestion decreased cellular interaction and slightly increased transport of all particles across the intestinal barrier. The interaction with organic matter resulted in clear differences in the agglomeration behavior. Moreover, we provide evidence for polymer-, size- and surface-dependent cellular effects of the test particles. KW - Toxicology KW - Nanoparticles KW - Dynamic Light Scattering KW - Nanoplastics KW - Microplastics KW - Reference Method KW - Reference Material PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593947 DO - https://doi.org/10.1016/j.fct.2023.114423 VL - 184 SP - 1 EP - 16 PB - Elsevier BV AN - OPUS4-59394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ginés-Palomares, J.-C. A1 - Fateri, M. A1 - Schubert, T. A1 - de Peindray d’Ambelle, L. A1 - Simon, Sebastian A1 - Gluth, Gregor A1 - Günster, Jens A1 - Zocca, Andrea T1 - Material aspects of sintering of EAC-1A lunar regolith simulant N2 - Future lunar exploration will be based on in-situ resource utilization (ISRU) techniques. The most abundant raw material on the Moon is lunar regolith, which, however, is very scarce on Earth, making the study of simulants a necessity. The objective of this study is to characterize and investigate the sintering behavior of EAC-1A lunar regolith simulant. The characterization of the simulant included the determination of the phase assemblage, characteristic temperatures determination and water content analysis. The results are discussed in the context of sintering experiments of EAC-1A simulant, which showed that the material can be sintered to a relative density close to 90%, but only within a very narrow range of temperatures (20–30 °C). Sintering experiments were performed for sieved and unsieved, as well as for dried and non-dried specimens of EAC-1A. In addition, an analysis of the densification and mechanical properties of the sintered specimens was done. The sintering experiments at different temperatures showed that the finest fraction of sieved simulant can reach a higher maximum sintering temperature, and consequently a higher densification and biaxial strength. The non-dried powder exhibited higher densification and biaxial strength after sintering compared to the dried specimen. This difference was explained with a higher green density of the non-dried powder during pressing, rather than due to an actual influence on the sintering mechanism. Nevertheless, drying the powder prior to sintering is important to avoid the overestimation of the strength of specimens to be fabricated on the Moon. KW - Lunar regolith KW - Ceramics KW - Microstructure KW - Sintering KW - Softening temperature PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-592668 DO - https://doi.org/10.1038/s41598-023-50391-y SN - 2045-2322 VL - 13 SP - 1 EP - 14 PB - Springer Nature AN - OPUS4-59266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieger, Philip A1 - Magnall, Joseph M. A1 - Gleeson, Sarah A. A1 - Oelze, Marcus T1 - Pyrite chemistry records a multistage ore forming system at the Proterozoic George Fisher massive sulfide Zn-Pb-Ag deposit, Mount Isa, Australia N2 - Trace element (TE) analysis of pyrite via LA-ICP-MS can be used to reconstruct the conditions of pyrite formation in complex mineral systems. The Carpentaria province in northern Australia is host to some of the world’s highest value Zn-Pb (+Ag, Cu) deposits. The genesis of many of these deposits is controversial, with competing models of single-vs. multi-stage ore formation. In this study, LA-ICP-MS data of paragenetically constrained pyrite from the George Fisher Zn-Pb-Ag deposit has been analysed to investigate the chemistry of different stages of ore formation. Pyrite from correlative unmineralized host rocks has also been analysed to investigate evidence of distal hydrothermal anomalism. All LA-ICP-MS data have been statistically evaluated (principal component analysis) and interpreted together with whole rock lithogeochemical data of the same samples. Pre-ore diagenetic pyrite is compositionally similar to other Proterozoic diagenetic pyrite, with some evidence of minor hydrothermal anomalism that with further analysis could help define distal alteration. Pyrite from the different ore stages are compositionally distinct, consistent with a multi-stage system. Ore stage 1 pyrite exceeds background contents of Co, Cu, Zn, As, Ag, Sb, Tl, and Pb and has elevated Co/Ni ratios, whereas only Ni and Co are above background abundances in ore stage 2 and 3 pyrite, of which only ore stage 3 pyrite has high Co/Ni ratios. Ore stage 1 pyrite has a similar composition to hydrothermal pyrite in the undeformed northern Carpentaria CD-type deposits and was likely syn-diagenesis. Ore stage 2 was syn-deformation, and resulted in replacement and recrystallization of pre-existing pyrite, and the expulsion of incompatible TEs. Ore stage 3 formed via a later Cu-Zn-Pb mineralizing event that resulted in a new geochemically distinct generation of Co-rich pyrite. Overall, this study demonstrates the value of paragenetically-constrained pyrite TE data for refining genetic models in complex sediment hosted mineral systems. KW - General Earth and Planetary Sciences PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590407 DO - https://doi.org/10.3389/feart.2023.892759 VL - 11 SP - 1 EP - 19 PB - Frontiers Media SA AN - OPUS4-59040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Schraut, Katharina ED - Adamczyk, Burkart ED - Adam, Christian ED - Stephan, D. ED - Simon, Sebastian ED - von Werder, Julia ED - Meng, Birgit T1 - Production of a hydraulic material from post treated steelmaking slags N2 - Steelmaking slag is a by-product of steel production, of which 4.5 Mt were produced in 2020 in Germany alone. It is mainly used in road construction, earthwork and hydraulic engineering. A smaller part is returned to the metallurgical cycle, used as fertiliser or landfilled. With this use, iron oxides still contained in steelmaking slag are lost. In addition, the possibility of producing higher-grade products from steelmaking slag is foregone. In recent decades, many researchers have investigated the production of Portland cement clinker and crude iron from basic oxygen furnace slags (BOFS) via a reductive treatment. Carbothermal treatment of liquid BOFS causes a reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density. Simultaneously, the chemical composition of the reduced slag is adapted to that of Portland cement clinker. In this study, German BOFS was reduced in a small-scale electric arc furnace using petrol coke as a reducing agent. The resulting low-iron mineral product has a similar chemical composition to Portland cement clinker and was rich in the tricalcium silicate solid solution alite (Ca3SiO5). Based on its chemical and mineralogical composition, similar to that of Portland cement clinker, the reduced BOFS has the potential to react comparably. In our study, the reduced BOFS produced less hydration heat than OPC, and its hydraulic reaction was delayed. However, adding gypsum has shown to accelerate the hydration rate of the reduced BOFS compared to that known from the calcium silicates of Portland cement clinker. Further research to improve the hydraulic properties of the reduced slag is essential. If successful, producing a hydraulic binder and crude iron from BOFS has economic and ecological benefits for both the cement and steel industries. T2 - The 16th International Congress on the Chemistry of Cement 2023 (ICCC2023) CY - Bangkok, Thailand DA - 18.09.2023 KW - Steelmaking slag KW - Alite KW - Clinker substitute KW - Hydraulic reactivity PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590522 UR - https://www.iccc-online.org/archive/ SP - 432 EP - 436 CY - Bangkok AN - OPUS4-59052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knabe, Christine A1 - Adel-Khattab, Doaa A1 - Rezk, Mohamed A1 - Cheng, Jia A1 - Berger, Georg A1 - Gildenhaar, Renate A1 - Wilbig, Janka A1 - Günster, Jens A1 - Rack, Alexander A1 - Heiland, Max A1 - Knauf, Tom A1 - Stiller, Michael T1 - Osteogenic Effect of a Bioactive Calcium Alkali Phosphate Bone Substitute in Humans N2 - (1) Background: The desire to avoid autograft harvesting in implant dentistry has prompted an ever-increasing quest for bioceramic bone substitutes, which stimulate osteogenesis while resorbing in a timely fashion. Consequently, a highly bioactive silicon containing calcium alkali orthophosphate (Si-CAP) material was created, which previously was shown to induce greater bone cell maturation and bone neo-formation than β-tricalcium phosphate (β-TCP) in vivo as well as in vitro. Our study tested the hypothesis that the enhanced effect on bone cell function in vitro and in sheep in vivo would lead to more copious bone neoformation in patients following sinus floor augmentation (SFA) employing Si-CAP when compared to β-TCP. (2) Methods: The effects of Si-CAP on osteogenesis and Si-CAP resorbability were evaluated in biopsies harvested from 38 patients six months after SFA in comparison to β-TCP employing undecalcified histology, histomorphometry, and immunohistochemical analysis of osteogenic marker expression. (3) Results: Si-CAP as well as β-TCP supported matrix mineralization and bone formation. Apically furthest away from the original bone tissue, Si-CAP induced significantly higher bone formation, bone-bonding (bone-bioceramic contact), and granule resorption than β-TCP. This was in conjunction with a higher expression of osteogenic markers. (4) Conclusions: Si-CAP induced higher and more advanced bone formation and resorbability than β-TCP, while β-TCP’s remarkable osteoconductivity has been widely demonstrated. Hence, Si-CAP constitutes a well-suited bioactive graft choice for SFA in the clinical arena. KW - Silicon release KW - Bioceramics KW - Calcium alkali orthophosphate materials KW - Bioactive bone grafting material KW - Bioactivity KW - Osteogenesis KW - Bone regeneration KW - Sinus floor augmentation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591015 DO - https://doi.org/10.3390/bioengineering10121408 VL - 10 IS - 12 SP - 1 EP - 15 PB - MDPI AN - OPUS4-59101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosen, Andrew S. A1 - Gallant, Max A1 - George, Janine A1 - Riebesell, Janosh A1 - Sahasrabuddhe, Hrushikesh A1 - Shen, Jimmy-Xuan A1 - Wen, Mingjian A1 - Evans, Matthew L. A1 - Petretto, Guido A1 - Waroquiers, David A1 - Rignanese, Gian-Marco A1 - Persson, Kristin A. A1 - Jain, Anubhav A1 - Ganose, Alex M. T1 - Jobflow: Computational Workflows Made Simple N2 - We present Jobflow, a domain-agnostic Python package for writing computational workflows tailored for high-throughput computing applications. With its simple decorator-based approach, functions and class methods can be transformed into compute jobs that can be stitched together into complex workflows. Jobflow fully supports dynamic workflows where the full acyclic graph of compute jobs is not known until runtime, such as compute jobs that launch other jobs based on the results of previous steps in the workflow. The results of all Jobflow compute jobs can be easily stored in a variety of filesystem- and cloud-based databases without the data storage process being part of the underlying workflow logic itself. Jobflow has been intentionally designed to be fully independent of the choice of workflow manager used to dispatch the calculations on remote computing resources. At the time of writing, Jobflow workflows can be executed either locally or across distributed compute environments via an adapter to the FireWorks package, and Jobflow fully supports the integration of additional workflow execution adapters in the future. KW - Automation KW - Workflow KW - Computational Materials Science KW - Computations KW - Software PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593104 DO - https://doi.org/10.21105/joss.05995 VL - 9 IS - 93 SP - 1 EP - 7 PB - The Open Journal AN - OPUS4-59310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hildebrandt, R. A1 - Seifert, M. A1 - George, Janine A1 - Blaurock, S. A1 - Botti, S. A1 - Krautscheid, H. A1 - Grundmann, M. A1 - Sturm, C. T1 - Determination of acoustic phonon anharmonicities via second-order Raman scattering in CuI N2 - We demonstrate the determination of anharmonic acoustic phonon properties via second-order Raman scattering exemplarily on copper iodide single crystals. The origin of multi-phonon features from the second-order Raman spectra was assigned by the support of the calculated 2-phonon density of states. In this way, the temperature dependence of acoustic phonons was determined down to 10 K. To determine independently the harmonic contributions of respective acoustic phonons, density functional theory in quasi-harmonic approximation was used. Finally, the anharmonic contributions were determined. The results are in agreement with earlier publications and extend CuI’s determined acoustic phonon properties to lower temperatures with higher accuracy. This approach demonstrates that it is possible to characterize the acoustic anharmonicities via Raman scattering down to zero-temperature renormalization constants of at least 0.1 cm⁻¹. KW - Thermoelectrics KW - Thermal transport KW - Phonon interactions KW - Density functional theory KW - Phonons PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593164 DO - https://doi.org/10.1088/1367-2630/ad1141 SN - 1367-2630 VL - 25 IS - 12 SP - 1 EP - 12 PB - IOP Publishing CY - London AN - OPUS4-59316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hupp, Vitus A1 - Schartel, Bernhard A1 - Flothmeier, K. A1 - Hartwig, A. T1 - Fire Behavior of Pressure-sensitive Adhesive Tapes and Bonded Materials N2 - Pressure-sensitive adhesive tapes are used in several industrial applications such as con-struction, railway vehicles and the automotive sector,where the burning behavior is ofcrucial importance. Flame retarded adhesivetapes are developed and provided, however,often without considering the interaction of adhesive tapes and the bonded materialsduring burning nor the contribution of the tapes to fire protection goal of the bondedcomponents in distinct fire tests. This publication delivers an empirical comprehensiveknowledge how adhesive tapes and their flame retardancy effect the burning behaviorof bonded materials. With a special focus on the interaction between the single compo-nents, one flame retarded tape and one tapewithout flame retardant are examined inscenarios of emerging and developing fires, along with their bonds with the commonmaterials wood, zinc-plated steel, mineral wool, polycarbonate, and polymethylmethacry-late. The flame retardant significantly improved the flame retardancy of the tape as afree-standing object and yielded a V-2 rating in UL 94 vertical test and raised the OxygenIndex by 5 vol.%. In bonds, or rather laminates, the investigations prove that the choiceof carrier and substrates are the factors with the greatest impact on the fire propertiesand can change the peak of heat release rate and the maximum average rate of heatemission up to 25%. This research yielded a good empirical overall understanding of thefire behavior of adhesive tapes and bonded materials. Thus, it serves as a guide for tapemanufacturers and applicants to develop tapes and bonds more substrate specific. KW - Adhesives KW - Cone calorimeter KW - Flame retardancy KW - Laminates KW - Phosphorus flame retardants KW - Pressure-sensitive adhesive KW - Tapes PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593207 DO - https://doi.org/10.1002/fam.3171 SN - 0308-0501 SN - 1099-1018 VL - 48 IS - 1 SP - 114 EP - 127 PB - Wiley CY - New York, NY AN - OPUS4-59320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kindrachuk, Vitaliy A1 - Darvishi Kamachali, Reza T1 - Mean-field modeling and phase-field simulation of grain growth under directional driving forces N2 - Directional grain growth is a common phenomenon in the synthetic and natural evolution of various polycrystals. It occurs in the presence of an external driving force, such as a temperature gradient, along which grains show a preferred, yet competitive, growth. Novel additive manufacturing processes, with intense, localized energy deposition, are prominent examples of when directional grain growth can occur, beneath the melting pool. In this work, we derive a phenomenological mean-field model and perform 3D phase-field simulations to investigate the directional grain growth and its underlying physical mechanisms. The effect of the intensity of driving force is simulated and systematically analyzed at the evolving growth front as well as various cross-sections perpendicular to the direction of the driving force. We found that although the directional growth significantly deviates from normal grain growth, it is still governed by a power law relation α tⁿ with an exponent n ~ 0.6–0.7. The exponent n exhibits a nontrivial dependence on the magnitude of the directional driving force, such that the lowest growth exponent is observed for intermediate driving forces. We elaborate that this can originate from the fact that the forces at grain boundary junctions evolve out of balance under the influence of the directional driving force. With increasing the driving forces, the growth exponent asymptotically approaches a value of n ≈ 0.63, imposed by the largest possible grain aspect ratio for given grain boundary energies. The current combined mean-field and phase-field framework pave the way for future exploration in broader contexts such as the evolution of complex additively manufactured microstructures. KW - Additive manufacturing KW - Phase-field simulation KW - Grain growth KW - Mean-field modelling KW - Directional grain growth PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593210 DO - https://doi.org/10.1016/j.mtla.2023.101989 SN - 2589-1529 VL - 33 SP - 1 EP - 10 PB - Elsevier AN - OPUS4-59321 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Nietzke, Jonathan A1 - Kannengießer, Thomas T1 - In situ measurement of hydrogen concentration in steel using laser‑induced breakdown spectroscopy (LIBS) N2 - The ISO 3690 standard “Determination of hydrogen content in arc weld metal” requires a thermal activation of the diffusible hydrogen in a piece of weld metal for the subsequent ex situ concentration measurement by carrier gas hot extraction CGHE or thermal desorption spectroscopy (TCD). Laser-induced breakdown spectroscopy (LIBS) offers a time and spatially resolved, almost non-destructive, in situ measurement of hydrogen at surfaces without sample preparation. We measured hydrogen in steels, which were charged either electrochemically or by high-pressure hydrogen gas, and compared the results. Further, the feasibility of quantitative hydrogen line scan measurements with LIBS was demonstrated by measuring hydrogen at water jet cut surfaces. The hydrogen concentrations measured with the help of LIBS were compared with CGHE measurements. It was observed that hydrogen can be reliably measured with LIBS for concentrations larger than 2 wt.-ppm. The maximum hydrogen concentration achieved using electrochemical charging was 85.1 ppm. The results show that LIBS is a promising technique for time- and spatially resolved measurements of hydrogen in steels. T2 - IIW Annual Assembly 2023 CY - Singapore KW - LIBS KW - Hydrogen measurement KW - Welding KW - Stainless steel KW - Diffusible hydrogen PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593664 DO - https://doi.org/10.1007/s40194-023-01677-2 SP - 1 EP - 9 PB - Springer AN - OPUS4-59366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roesch, Philipp A1 - Schinnen, Andrea A1 - Riedel, Maren A1 - Sommerfeld, Thomas A1 - Sawal, G. A1 - Bandow, N. A1 - Vogel, Christian A1 - Kalbe, Ute A1 - Simon, Franz-Georg T1 - Investigation of pH-dependent extraction methods for PFAS in (fluoropolymer-based) consumer products: A comparative study between targeted and sum parameter analysis N2 - Here, we report a comparative study of different sum parameter analysis methods for the extraction of per- and polyfluoroalkyl substances (PFAS) from manufactured consumer products, which can be measured by combustion ion chromatography (CIC). Therefore, a hydrolysis-based extraction method was further developed, which accounts for the addition of hydrolyzable covalently bound polyfluoroalkylated side-chain polymers (SFPs) to the extractable organic fluorine portion of the mass balance proposed as "hydrolyzable organically bound fluorine" (HOF). To test this hypothesis, the method was applied to 39 different consumer products containing fluoropolymers or monomeric PFAS taken from four different categories: outdoor textiles, paper packaging, carpeting, and permanent baking sheets. We also evaluated the method's efficiency by extracting four synthesized fluorotelomer polyacrylate reference compounds. The total fluorine (TF) and extractable organically bound fluorine (EOF) values were measured through CIC using established protocols. The TF values ranged from sub-ppb to %-levels, depending on the compound class. All samples showed results for hydrolyzed organofluorine (HOF) between 0.03 and 76.3 μg/g, while most EOF values were lower (