TY - JOUR A1 - Reichenauer, F. A1 - Wang, Cui A1 - Förster, C. A1 - Boden, P. A1 - Ugur, N. A1 - Báez-Cruz, R. A1 - Kalmbach, J. A1 - Carrella, L. M. A1 - Rentschler, E. A1 - Ramanan, C. A1 - Niedner-Schatteburg, G. A1 - Gerhards, M. A1 - Seitz, M. A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Strongly Red-Emissive Molecular Ruby [Cr(bpmp)2]3+ Surpasses [Ru(bpy)3]2+ N2 - Gaining chemical control over the thermodynamics and kinetics of photoexcited states is paramount to an efficient and sustainable utilization of photoactive transition metal complexes in a plethora of technologies. In contrast to energies of charge Transfer states described by spatially separated orbitals, the energies of spinflip states cannot straightforwardly be predicted as Pauli Repulsion and the nephelauxetic effect play key roles. Guided by multireference quantum chemical calculations, we report a novel highly luminescent spin-flip emitter with a quantum chemically predicted blue-shifted luminescence. The spin-flip emission band of the chromium complex [Cr(bpmp)2]3+ (bpmp = 2,6-bis(2-pyridylmethyl) pyridine) shifted to higher energy from ca. 780 nm observed for known highly emissive chromium(III) complexes to 709 nm. The photoluminescence quantum yields climb to 20%, and very long excited state lifetimes in the millisecond range are achieved at room temperature in acidic D2O solution. Partial ligand deuteration increases the quantum yield to 25%. The high excited state energy of [Cr(bpmp)2]3+ and its facile reduction to [Cr(bpmp)2]2+ result in a high excited state redox potential. The ligand’s methylene bridge acts as a Brønsted acid quenching the luminescence at high pH. Combined with a pH-insensitive chromium(III) emitter, ratiometric optical pH sensing is achieved with single wavelength excitation. The photophysical and Ground state properties (quantum yield, lifetime, redox potential, and acid/base) of this spin-flip complex incorporating an earth-abundant metal surpass those of the classical precious metal [Ru(α-diimine)3]2+ charge transfer complexes, which are commonly employed in optical sensing and photo(redox) catalysis, underlining the bright future of these molecular ruby analogues. KW - Fluorescence KW - Optical probe KW - Sensor KW - PH KW - Quantum yield KW - Quality assurance KW - Complex KW - Cr(III) KW - Lifetime KW - Ligand KW - Theory PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530548 DO - https://doi.org/10.1021/jacs.1c05971 VL - 143 IS - 30 SP - 11843 EP - 11855 PB - ACS Publications AN - OPUS4-53054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reigl, Selina A1 - Van Driessche, Alexander A1 - Stawski, Tomasz A1 - Koltzenburg, Sebastian A1 - Kunz, Werner A1 - Kellermeier, Matthias T1 - Sustainable Pathways for the Synthesis of Calcium Sulfate Hemihydrate N2 - Calcium sulfate, and especially its hemihydrate form (bassanite), is crucial in the construction industry, primarily used as a hydraulic binder in cements, mortars, and wallboards. Because of the rapid transformation of bassanite into thermodynamically stable gypsum (calcium sulfate dihydrate) upon contact with water, natural deposits are scarce, rendering it one of the most extensively produced inorganic materials worldwide. Currently, bassanite is derived from mined or waste gypsum through a thermal dehydration process, which is energy-intensive and costly. As sustainability has become a key target for industrial processes and products, a series of studies aiming to increase the energy efficiency and reduce the carbon footprint of bassanite production was published recently. Two primary approaches are pursued: conversion of gypsum and direct precipitation of bassanite from solution. In both cases, organic solvents, (specific) additives and/or elevated temperatures have been used to control the activity/availability of water in the reaction medium and thus direct phase selection towards bassanite. This review offers a comprehensive overview of alternative bassanite production methods, critically examining their benefits, potential downsides, and overall impact on the sustainability of industrial-scale use. KW - Calcium sulfate KW - Gypsum KW - Bassanite KW - Recycling PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630657 DO - https://doi.org/10.1002/anie.202415161 SN - 1521-3773 SP - 1 EP - 20 PB - Wiley VHC-Verlag AN - OPUS4-63065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reimann, C. A1 - Brangsch, J. A1 - Kaufmann, Jan Ole A1 - Adams, L. C. A1 - Onthank, D. C. A1 - Thöne-Reineke, C. A1 - Robinson, S. P. A1 - Hamm, B. A1 - Botnar, R. M. A1 - Makowski, M. R. T1 - Dual-probe molecular MRI for the in vivo characterization of atherosclerosis in a mouse model: Simultaneous assessment of plaque inflammation and extracellular matrix remodeling N2 - Molecular MRI is a promising in-vivo modality to detect and quantify morphological and molecular vessel-wall changes in atherosclerosis. The combination of different molecular biomarkers may improve the risk stratification of patients. This study aimed to investigate the feasibility of simultaneous visualization and quantification of plaque-burden and inflammatory activity by dual-probe molecular MRI in a mouse-model of progressive atherosclerosis and in response-to-therapy. Homozygous apolipoprotein E knockout mice (ApoE−/−) were fed a high-fat-diet (HFD) for up to four-months prior to MRI of the brachiocephalic-artery. To assess response-to-therapy, a statin was administered for the same duration. MR imaging was performed before and after administration of an elastin-specific gadolinium-based and a macrophage-specific iron-oxide-based probe. Following in-vivo MRI, samples were analyzed using histology, immunohistochemistry, inductively-coupled-mass-spectrometry and laser-inductively-coupled-mass-spectrometry. In atherosclerotic-plaques, intraplaque expression of elastic-fibers and inflammatory activity were not directly linked. While the elastin-specific probe demonstrated the highest accumulation in advanced atherosclerotic-plaques after four-months of HFD, the iron-oxide-based probe showed highest accumulation in early atherosclerotic-plaques after two months of HFD. In-vivo measurements for the elastin and iron-oxide-probe were in good agreement with ex-vivo histopathology (Elastica-van-Giesson stain: y = 298.2 + 5.8, R2 = 0.83, p < 0.05; Perls‘ Prussian-blue-stain: y = 834.1 + 0.67, R2 = 0.88, p < 0.05). Contrast-to-noise-ratio (CNR) measurements of the elastin probe were in good agreement with ICP-MS (y = 0.11x-11.3, R² = 0.73, p < 0.05). Late stage atherosclerotic-plaques displayed the strongest increase in both CNR and gadolinium concentration (p < 0.05). The gadolinium probe did not affect the visualization of the iron-oxide-probe and vice versa. This study demonstrates the feasibility of simultaneous assessment of plaque-burden. KW - Gadolinium KW - Elastin KW - Probe KW - Iron oxide KW - Ferumoxytol PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497066 DO - https://doi.org/10.1038/s41598-019-50100-8 VL - 9 SP - 13827 PB - Springer Nature AN - OPUS4-49706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Adams, L. C. A1 - Onthank, D. C. A1 - Thöne-Reineke, C. A1 - Robinson, S. P. A1 - Hamm, B. A1 - Botnar, R. M. A1 - Makowski, M. R. T1 - Dual-probe molecular MRI for the in vivo characterization of atherosclerosis in a mouse model: Simultaneous assessment of plaque inflammation and extracellular-matrix remodeling N2 - Molecular MRI is a promising in-vivo modality to detect and quantify morphological and molecular vessel-wall changes in atherosclerosis. The combination of different molecular biomarkers may improve the risk stratification of patients. This study aimed to investigate the feasibility of simultaneous visualization and quantification of plaque-burden and inflammatory activity by dual-probe molecular MRI in a mouse-model of progressive atherosclerosis and in response-to-therapy. Homozygous apolipoprotein E knockout mice (ApoE−/−) were fed a high-fat-diet (HFD) for up to four-months prior to MRI of the brachiocephalic-artery. To assess response-to-therapy, a statin was administered for the same duration. MR imaging was performed before and after administration of an elastin-specific gadolinium-based and a macrophage-specific iron-oxide-based probe. Following in-vivo MRI, samples were analyzed using histology, immunohistochemistry, inductively-coupled-mass-spectrometry and laser-inductively-coupled-mass-spectrometry. In atherosclerotic-plaques, intraplaque expression of elastic-fibers and inflammatory activity were not directly linked. While the elastin-specific probe demonstrated the highest accumulation in advanced atherosclerotic-plaques after four-months of HFD, the iron-oxide-based probe showed highest accumulation in early atherosclerotic-plaques after two-months of HFD. In-vivo measurements for the elastin and iron-oxide-probe were in good agreement with ex-vivo histopathology (Elastica-van-Giesson stain: y = 298.2 + 5.8, R2 = 0.83, p < 0.05; Perls‘ Prussian-blue-stain: y = 834.1 + 0.67, R2 = 0.88, p < 0.05). Contrast-to-noise-ratio (CNR) measurements of the elastin probe were in good agreement with ICP-MS (y = 0.11x-11.3, R² = 0.73, p < 0.05). Late stage atherosclerotic-plaques displayed the strongest increase in both CNR and gadolinium concentration (p < 0.05). The gadolinium probe did not affect the visualization of the iron-oxide-probe and vice versa. This study demonstrates the feasibility of simultaneous assessment of plaque-burden and inflammatory activity by dual-probe molecular MRI of progressive atherosclerosis. The in-vivo detection and quantification of different MR biomarkers in a single scan could be useful to improve characterization of atherosclerotic-lesions. KW - In-vivo KW - Molecular MRI PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492514 DO - https://doi.org/10.1038/s41598-019-50100-8 VL - 9 IS - 1 SP - Article number: 13827 PB - Nature AN - OPUS4-49251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinmuth-Selzle, K. A1 - Bellinghausen, I. A1 - Leifke, A. L. A1 - Backes, A. T. A1 - Bothen, N. A1 - Ziegler, K. A1 - Weller, Michael G. A1 - Saloga, J. A1 - Schuppan, D. A1 - Lucas, K. A1 - Pöschl, U. A1 - Fröhlich-Nowoisky, J. T1 - Chemical modification by peroxynitrite enhances TLR4 activation of the grass pollen allergen Phl p 5 N2 - The chemical modification of aeroallergens by reactive oxygen and nitrogen species (ROS/RNS) may contribute to the growing prevalence of respiratory allergies in industrialized countries. Post-translational modifications can alter the immunological properties of proteins, but the underlying mechanisms and effects are not well understood. In this study, we investigate the Toll-like receptor 4 (TLR4) activation of the major birch and grass pollen allergens Bet v 1 and Phl p 5, and how the physiological oxidant peroxynitrite (ONOO–) changes the TLR4 activation through protein nitration and the formation of protein dimers and higher oligomers. Of the two allergens, Bet v 1 exhibited no TLR4 activation, but we found TLR4 activation of Phl p 5, which increased after modification with ONOO– and may play a role in the sensitization against this grass pollen allergen. We attribute the TLR4 activation mainly to the two-domain structure of Phl p 5 which may promote TLR4 dimerization and activation. The enhanced TLR4 signaling of the modified allergen indicates that the ONOO–-induced modifications affect relevant protein-receptor interactions. This may lead to increased sensitization to the grass pollen allergen and thus contribute to the increasing prevalence of allergies in the Anthropocene, the present era of globally pervasive anthropogenic influence on the environment. KW - Bet v 1 KW - Birch pollen allergen KW - Phl p 5 KW - Grass pollen KW - Phleum pratense KW - Betula pendula KW - Nitration KW - Nitrotyrosine KW - Protein nitration KW - Toll-like receptor 4 KW - Allergy KW - Enhancement KW - Oligomerization KW - Dimerization KW - TLR4 activation KW - Air pollution KW - Nitrogen oxides KW - Inflammation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570298 DO - https://doi.org/10.3389/falgy.2023.1066392 VL - 4 SP - 1 EP - 7 PB - Frontiers Media SA CY - Lausanne, Switzerland AN - OPUS4-57029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinmuth-Selzle, K. A1 - Kampf, C. J. A1 - Lucas, K. A1 - Lang-Yona, N. A1 - Fröhlich-Nowoisky, J. A1 - Shiraiwa, M. A1 - Lakey, P. S. J. A1 - Lai, S. A1 - Liu, F. A1 - Kunert, A. T. A1 - Ziegler, K. A1 - Shen, F. A1 - Sgarbanti, R. A1 - Weber, B. A1 - Bellinghausen, I. A1 - Saloga, J. A1 - Weller, Michael G. A1 - Duschl, A. A1 - Schuppan, D. A1 - Pöschl, U. T1 - Air pollution and climate change effects on allergies in the anthropocene: Abundance, interaction, and modification of allergens and adjuvants N2 - Air pollution and climate change are potential drivers for the increasing burden of allergic diseases. The molecular mechanisms by which air pollutants and climate parameters may influence allergic diseases, however, are complex and elusive. This article provides an overview of physical, chemical and biological interactions between air pollution, climate change, allergens, adjuvants and the immune system, addressing how these interactions may promote the development of allergies. We reviewed and synthesized key findings from atmospheric, climate, and biomedical research. The current state of knowledge, open questions, and future research perspectives are outlined and discussed. The Anthropocene, as the present era of globally pervasive anthropogenic influence on planet Earth and, thus, on the human environment, is characterized by a strong increase of carbon dioxide, ozone, nitrogen oxides, and combustion- or traffic-related particulate matter in the atmosphere. These environmental factors can enhance the abundance and induce chemical modifications of allergens, increase oxidative stress in the human body, and skew the immune system toward allergic reactions. In particular, air pollutants can act as adjuvants and alter the immunogenicity of allergenic proteins, while climate change affects the atmospheric abundance and human exposure to bioaerosols and aeroallergens. To fully understand and effectively mitigate the adverse effects of air pollution and climate change on allergic diseases, several challenges remain to be resolved. Among these are the identification and quantification of immunochemical reaction pathways involving allergens and adjuvants under relevant environmental and physiological conditions. KW - Allergie KW - Klimaveränderung KW - Luftverschmutzung KW - Partikel KW - Ozon KW - Stickoxide KW - Allergene KW - Adjuvantien KW - PALM KW - DAMP PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404531 DO - https://doi.org/10.1021/acs.est.6b04908 SN - 1520-5851 SN - 0013-936X VL - 51 IS - 8 SP - 4119 EP - 4141 PB - American Chemical Society (ACS) CY - Washington AN - OPUS4-40453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinmuth-Selzle, K. A1 - Tchipilov, Teodor A1 - Backes, A. T. A1 - Tscheuschner, Georg A1 - Tang, K. A1 - Ziegler, K. A1 - Lucas, K. A1 - Pöschl, U. A1 - Fröhlich-Nowoisky, J. A1 - Weller, Michael G. T1 - Determination of the protein content of complex samples by aromatic amino acid analysis, liquid chromatography-UV absorbance, and colorimetry N2 - Fast and accurate determination of the protein content of a sample is an important and non-trivial task of many biochemical, biomedical, food chemical, pharmaceutical, and environmental research activities. Different methods of total protein determination are used for a wide range of proteins with highly variable properties in complex matrices. These methods usually work reasonably well for proteins under controlled conditions, but the results for non-standard and complex samples are often questionable. Here, we compare new and well-established methods, including traditional amino acid analysis (AAA), aromatic amino acid analysis (AAAA) based on the amino acids phenylalanine and tyrosine, reversed-phase liquid chromatography of intact proteins with UV absorbance measurements at 220 and 280 nm (LC-220, LC-280), and colorimetric assays like Coomassie Blue G-250 dye-binding assay (Bradford) and bicinchoninic acid (BCA) assay. We investigated different samples, including proteins with challenging properties, chemical modifications, mixtures, and complex matrices like air particulate matter and pollen extracts. All methods yielded accurate and precise results for the protein and matrix used for calibration. AAA, AAAA with fluorescence detection, and the LC-220 method yielded robust results even under more challenging conditions (variable analytes and matrices). These methods turned out to be well-suited for reliable determination of the protein content in a wide range of samples, such as air particulate matter and pollen. KW - Air particulate matter KW - Aromatic amino acid analysis KW - Atmospheric aerosol KW - Chemical protein modification KW - Derivatization KW - Nitration KW - Nitrotyrosine KW - LC-UV absorbance KW - Pollen extract KW - Protein quantification KW - Protein test KW - Kjeldahl KW - Tyrosine KW - Phenylalanine KW - Hydrolysis KW - Bradford KW - BCA test KW - 280 nm KW - Air filter samples KW - Fluorescence KW - HPLC KW - Chromatography KW - Protein content KW - 150th anniversary of BAM KW - Topical collection: Analytical Methods and Applications in the Materials and Life Sciences PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545924 UR - https://pubmed.ncbi.nlm.nih.gov/35320366/ DO - https://doi.org/10.1007/s00216-022-03910-1 SP - 1 EP - 14 PB - Springer Nature Limited CY - New York, Heidelberg AN - OPUS4-54592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinsch, Stefan A1 - Welter, T. A1 - Müller, Ralf A1 - Deubener, J. T1 - Hydrogen Permeability of Tectosilicate Glasses for Tank Barrier Liners N2 - The permeation of hydrogen gas was studied in meta-aluminous (tectosilicate) glass powders of Li2O×Al2O3×SiO2 (LAS), Na2O×Al2O3×SiO2 (NAS) and MgO×Al2O3×SiO2 (MAS) systems by pressure loading and vacuum extraction in the temperatures range 210–310 °C. With this method, both the solubility S and the diffusivity D were determined, while the permeability was given by the product SD. For all glasses, S was found to decrease with temperature, while D increased. Since the activation energy of diffusion of H2 molecules exceeded that of dissolution, permeation increased slightly with temperature. When extrapolated to standard conditions (25 °C), the permeability of tectosilicate glasses was found to be only 10-22–10-24 mol H2 (m s Pa)-1, which is 8–10 magnitudes lower than most polymers. Thin glass liners of these compositions are expected to be the most effective barrier for tanks of pressurised hydrogen. KW - Hydrogen permeation KW - Aluminosilicate glasses KW - Hydrogen storage tank KW - Glass liner PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587284 DO - https://doi.org/10.52825/glass-europe.v1i.425 VL - 1 SP - 1 EP - 11 AN - OPUS4-58728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ren, J. A1 - Weigert, Florian A1 - Weber, F. A1 - Wang, Y. A1 - Choudhury, S. A1 - Xiao, J. A1 - Lauermann, I. A1 - Resch-Genger, Ute A1 - Bande, A. A1 - Petit, T. ED - Petit, Tristan T1 - Influence of surface chemistry on optical, chemical and electronic properties of blue luminescent carbon dots N2 - Carbon dots have attracted much attention due to their unique optical, chemical and electronic properties enabling a wide range of applications. The properties of carbon dots can be effectively adjusted through modifying their chemical composition. However, a major challenge remains in understanding the core and surface contributions to optical and electronic transitions. Here, three blue luminescent carbon dots with carboxyl, amino and hydroxyl groups were comprehensively characterized by UV-vis absorption and emission spectroscopy, synchrotron-based X-ray spectroscopy, and infrared spectroscopy. The influence of the surface functionality on their fluorescence was probed by pH-dependent photoluminescence measurements. Moreover, the hydrogen bonding interactions between water and the surface groups of carbon dots were characterized by infrared spectroscopy. Our results show that both core and surface electronic states of blue luminescent carbon dots contribute to electronic acceptor levels while the chemical nature of the surface groups determines the hydrogen bonding behavior of the carbon dots. This comprehensive spectroscopic study demonstrates that the surface chemistry has a profound influence on the electronic configuration and surface–water interaction of carbon dots, thus affecting their photoluminescence properties. KW - Quantum dots KW - Spectroscopy KW - UV Vis KW - Fluorescence KW - Surface chemistry PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472325 DO - https://doi.org/10.1039/c8nr08595a SN - 2040-3372 VL - 11 IS - 4 SP - 2056 EP - 2064 PB - RSC AN - OPUS4-47232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Brunet, G. A1 - Marin, R. A1 - Monk, Melissa-Jane A1 - Galico, D. A. A1 - Sigoli, F. A. A1 - Suturina, E. A. A1 - Hemmer, E. A1 - Murugesu, M. T1 - Exploring the dual functionality of an Ytterbium complex for luminescence thermometry and slow magnetic relaxation† N2 - We present a comprehensive investigation of the magnetic and optical properties of an ytterbium complex, which combines two desirable and practical features into a single molecular system. Based upon YbIII Ions that promote near-infrared optical activity and a chemical backbone that is ideal for an in-depth understanding of the magnetic behaviour, we have designed a multifunctional opto-magnetic species that operates as a luminescent thermometer and as a single-molecule magnet (SMM). Our magnetic investigations, in conjunction with ab initio calculations, reveal one of the highest energy barriers reported for an YbIII-based complex. Moreover, we correlate this anisotropic barrier with the Emission spectrum of the compound, wherein we provide a complete assignment of the energetic profile of the complex. Such studies lay the foundation for the design of exciting multi-faceted materials that are able to retain information at the single-molecule level and possess built-in thermal self-monitoring capabilities. KW - Magnetic KW - Fluorescence KW - NIR KW - Temperature KW - Dual sensing KW - Sensor KW - Yb(III) complex KW - Lanthanide KW - Quantum yield KW - Quality assurance PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486659 DO - https://doi.org/10.1039/c9sc00343f VL - 10 IS - 28 SP - 6799 EP - 6808 PB - Royal Society of Chemistry AN - OPUS4-48665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Carl, F. A1 - Grauel, Bettina A1 - Pons, Monica A1 - Würth, Christian A1 - Haase, M. T1 - LiYF4:Yb/LiYF4 and LiYF4:Yb,Er/LiYF4 core/shell nanocrystals with luminescence decay times similar to YLF laser crystals and the upconversion quantum yield of the Yb,Er doped nanocrystals N2 - We developed a procedure to prepare luminescent LiYF4:Yb/LiYF4 and LiYF4:Yb,Er/LiYF4 core/shell nanocrystals with a size of approximately 40 nm revealing luminescence decay times of the dopant ions that approach those of high-quality laser crystals of LiYF4:Yb (Yb:YLF) and LiYF4:Yb,Er (Yb,Er:YLF) with identical doping concentrations. As the luminescence decay times of Yb3+ and Er3+ are known to be very sensitive to the presence of quenchers, the long decay times of the core/shell nanocrystals indicate a very low number of defects in the core particles and at the core/shell interfaces. This improvement in the performance was achieved by introducing two important modifications in the commonly used oleic acid based synthesis. First, the shell was prepared via anewly developed method characterized by a very low nucleation rate for particles of pure LiYF4 shell material. Second, anhydrous acetates were used as precursors and additional drying steps were applied to reduce the incorporation of OH− in the crystal lattice, known to quench the emission of Yb3+ ions. Excitation power density (P)-dependent absolute measurements of the upconversion luminescence quantum yield (Φ,UC) of LiYF4:Yb,Er/LiYF4 core/shell particles reveal a maximum value of 1.25% at P of 180 W·cm−2. Although lower than the values reported for NaYF4:18%Yb,2%Er core/shell nanocrystals with comparable sizes, these Φ, UC values are the highest reported so far for LiYF4:18%Yb,2%Er/LiYF4 nanocrystals without additional dopants. Further improvements May nevertheless be possible by optimizing the dopant concentrations in the LiYF4 nanocrystals. KW - Nano KW - Crystal KW - Quantum yield KW - LiYF4 KW - Synthesis KW - Lifetime KW - Fluorescence KW - NIR KW - Photoluminescence KW - Lanthanide KW - Upconversion nanoparticle KW - Nanomaterial PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515395 DO - https://doi.org/10.1007/s12274-020-3116-y SN - 1998-0124 VL - 14 IS - 3 SP - 797 EP - 806 PB - Springer AN - OPUS4-51539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Meermann, Björn A1 - Koch, Matthias A1 - Weller, Michael G. T1 - Editorial: Analytical methods and applications in materials and life sciences N2 - Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials. This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences. However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences. The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - Analysis KW - Life sciences KW - Analytical sciences KW - Quality assurance KW - Reference material KW - Fluorescence KW - Nanoparticle KW - Sensor KW - Material sciences KW - Pollutant KW - Environment KW - Method KW - Limit of detection KW - 150th anniversary KW - ABC KW - BAM KW - Collection KW - Editorial KW - Special issue KW - Bundesanstalt für Materialforschung und -prüfung KW - Jahrestag PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550720 DO - https://doi.org/10.1007/s00216-022-04082-8 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - Topical collection: Analytical methods and applications in the materials and life sciences SP - 4267 EP - 4268 PB - Springer CY - Berlin AN - OPUS4-55072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ressnig, A. A1 - Corbiere, T. A1 - Lunkenbein, T. A1 - Braun, Ulrike A1 - Willinger, M. G. A1 - Antonietti, M. T1 - Decomposition synthesis of tuneable, macroporous carbon foams from crystalline precursors via in situ templating N2 - A flexible, sustainable, one-step thermal decomposition route for the synthesis of hierarchical, heteroatom doped carbon foams is presented. Task-specific semi-organic crystals combine functions for three different purposes: the carbon and heteroatom source, a foaming agent (CO2) and an in situ generable template (NaCl). Insights to the decomposition pathway were gained through FTIR/MS coupled TGA and an ultrafast out-of-furnace heating procedure and the products were analysed with (HR)SEM/TEM, EELS, FTIR, and N2 sorption. The resulting macroporous carbon foams are excellent supports for metallic nanoparticles due to their hierarchical structure, high surface area and tuneable heteroatom contents. This was demonstrated for catalytically active copper or the magnetic CoNi alloy for water purification. KW - macroporous carbon KW - thermal decomposition KW - synthesize heteroatom KW - in situ template (NaCl) PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-318641 DO - https://doi.org/10.1039/c4ta03646h SN - 2050-7496 SN - 2050-7488 VL - 2 IS - 42 SP - 18076 EP - 18081 PB - RSC CY - London [u.a.] AN - OPUS4-31864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Retzmann, Anika A1 - Faßbender, Sebastian A1 - Rosner, M. A1 - von der Au, Marcus A1 - Vogl, Jochen T1 - Performance of second generation ICP-TOFMS for (multi-)isotope ratio analysis: a case study on B, Sr and Pb and their isotope fractionation behavior during the measurements N2 - The performance of second generation ICP-TOFMS, equipped with a micro-channel plate (MCP) enabling multi-isotope detection, in terms of isotope ratio precision and instrumental isotopic fractionation (IIF) for (multi-)isotope ratio analysis was thoroughly assessed for B, Sr and Pb. Experimental isotope ratio precision of 0.14 % for 11B/10B intensity ratio, 0.15 % for 87Sr/86Sr intensity ratio and 0.07% for 208Pb/206Pb intensity ratio were obtained at high signal levels ($500 mg L−1) which is comparable to first generation ICP-TOFMS. The long-term stability of isotope ratios, measured over several hours and expressed as repeatability, is between 0.05 % and 1.8 % for B, Sr and Pb. The observed IIF per mass unit is negative for B (i.e., −11 % for 11B/10B) which is in accordance with measurements using sector field (MC) ICP-MS. But the observed IIF per mass unit is positive for Sr (i.e., 2 % for 87Sr/86Sr) and Pb (i.e., 4.5 % for 208Pb/206Pb) which is not in accordance with measurements using sector field (MC) ICP-MS. Furthermore, different IIFs per mass unit were observed for different isotope pairs of the same isotopic system (i.e., Sr, Pb) and adjacent isotopic systems (i.e., Pb vs. Tl). This and the observations from three-isotope plots for Sr and Pb show that ion formation, ion extraction, ion transmission, ion separation and ion detection in second generation ICP-TOFMS is subject to IIF that does not follow the known mass dependent fractionation laws and is possibly caused by mass independent fractionation and/or multiple (contradictory) fractionation processes with varying contributions. The non-mass dependent IIF behavior observed for second generation ICP TOFMS has profound consequences for the IIF correction of isotope raw data, including application of multi-isotope dilution mass spectrometry (IDMS) using ICP-TOFMS. Hence, only IIF correction models that correct also for mass independent fractionation are applicable to calculate reliable isotope ratios using second generation ICP-TOFMS. In the present study, reliable d11B values, and absolute B, Sr and Pb isotope ratios could be determined using the SSB approach in single-element solutions as well as in a mixture of B, Sr and Pb, where the isotopes were measured simultaneously. KW - ICP-TOFMS KW - Isotope delta value KW - Isotope amount ratio KW - Conventional isotope ratio KW - Instrumental isotope fractionation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582239 DO - https://doi.org/10.1039/d3ja00084b SN - 0267-9477 VL - 38 IS - 10 SP - 2144 EP - 2158 PB - Royal Society of Chemistry AN - OPUS4-58223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Czeskleba, Denis A1 - Fleißner-Rieger, H. A1 - Nietzke, Jonathan A1 - Kannengießer, Thomas T1 - Combined heating rate and restraint condition effect on stress relief cracking during PWHT of thick-walled Cr–Mo-V steel SAW joints N2 - Creep-resistant steels such as 13CrMoV9-10 are utilized in the manufacture of thick-walled pressure vessels and are typically joined by submerged arc welding (SAW). However, these materials are susceptible to stress relief cracking (SRC) if the required post weld heat treatment (PWHT) is not applied correctly. Existing PWHT guidelines, encompassing heating rate and dwell (or holding) time at a given temperature, are derived from a synthesis of empirical knowledge and typically free-shrinkage weld experiments to assess the susceptibility to SRC. Therefore, this study discusses the combined effect of the PWHT heating rate under free-shrinkage compared to restrained shrinkage. Welding experiments were conducted (using plates with a thickness of 25 mm) for both shrinkage conditions for a variety of heating rates and maximum temperatures. In-situ acoustic emission analysis was used to locate propagating SRCs during PWHT. Hardness measurements, mechanical property characterization (Charpy impact strength), and microstructure correlation were used to evaluate the SRC susceptibility. The results suggested that the influence of heating rate could not be directly related to SRC formation and that the initial weld microstructure prior to PWHT was more relevant in terms of very high hardness in the coarse grain heat affected zone, especially that of the last beads in the top layer of the welding sequence. This was seen in the form of random, unexpected SRC occurrence in only one specimen at a heating rate commonly used in welding practice (approximately 100 K/h). In this context, the additional effect of an external shrinkage restraint on SRC must be considered in the form of increasing mechanical loads during welding, which are typically not within the scope of welding practice. To mitigate the probability of SRC during PWHT, it is imperative to reduce the welding heat input and to restrict the structural shrinkage restraint of the weld joint. KW - Component test KW - Stress relief cracking KW - PWHT KW - Creep-resistant steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631439 DO - https://doi.org/10.1007/s40194-025-02062-x SN - 1878-6669 SP - 1 EP - 17 PB - Springer Nature AN - OPUS4-63143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Erxleben, Kjell A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Mente, Tobias A1 - Michael, Thomas T1 - Local mechanical properties of dissimilar metal TIG welded joints of CoCrFeMnNi high entropy alloy and AISI 304 austenitic steel N2 - Multiple principal element alloys encompass the well-known high entropy alloys (HEA). The alloy system represents a new class of materials consisting of at least three alloying elements, each containing 5 to 35 at.%. Thus, this alloying concept differs fundamentally from conventional materials such as steel or nickel alloys. For this purpose, the alloying elements are specifically selected, the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. In particular, conflicting goals, such as the trade-off between strength and ductility in conventional steels, are overcome. However, in the last 20 years, the focus has been on material synthesis. With the increase in available material quantities, the focus is now on processing issues such as joining and welding processes. The weldability of HEAs has received very little attention so far. The experience with dissimilar metal welds is completely lacking but is essential for the application of these materials in combination with conventional materials. The present study presents comprehensive experimental results on the weldability of an equimolar CoCrFeMnNi-HEA in cold-rolled and heat-treated condition, which was joined by tungsten inert gas welding to an austenitic steel AISI 304. The mechanical properties of the dissimilar metal welds were characterized by cross-weld tensile samples, whereas the local deformation in the weld of the different welding zones was measured by digital image correlation. In accordance with the respective initial HEA condition (cold-rolled vs. heat-treated), the local strain behavior was divergent and influenced the global mechanical properties of both DMW types. Nonetheless, the experiments provided proof in principle of the weldability for dissimilar joints of the CoCrFeMnNi-HEA welded to conventional materials like austenitic stainless steels ensuring a corresponding capability for mechanical loading. This allows further considerations on the application of these innovative materials. KW - TIG welding KW - High-entropy alloys KW - Mechanical properties KW - Dissimilar metal weld PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595775 DO - https://doi.org/10.1007/s40194-024-01718-4 SN - 0043-2288 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-59577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Kromm, Arne A1 - Mente, Tobias A1 - Brackrock, Daniel A1 - Czeskleba, Denis A1 - Kannengießer, Thomas T1 - Component test for the assessment of delayed hydrogen-assisted cracking in thick-walled SAW joints for offshore applications N2 - Offshore wind turbines continuously increase in size and weight and demand adequate offshore foundations concepts like monopiles, tripods, or jackets. These components are typically constructed using submerged arc welding (SAW) with high-strength thick steel plates like the S420ML. During welding, the occurrence of delayed hydrogen-assisted cracking (HAC) must be anticipated. HAC is a critical combination of the local hydrogen concentration within a susceptible microstructure under certain mechanical load, i.e., the occurring (welding) residual stresses. The welding sequence of the thick-walled plates complicates the residual stress distribution due to the necessary repeated thermal cycling, i.e., welding seam/layer deposition to fill the joint. For that purpose, SAW with two-wire-technique was used to weld a specially designed and prototype-like mock-up of a real component with a thickness of 50 mm, filled with over 20 passes and a seam length of 1000 mm. Additional welded stiffeners simulated the effect of a high restraint, to achieve critical HAC conditions. The necessity of a minimum waiting time (MWT) before the NDT can be conducted (to exclude HAC) was critically verified by the application of ultrasonic testing of the welded joint at different time-steps of the NDT of up to 48 h after the completion welding. The residual stresses were determined by a robot XRD goniometer. Tensile residual stresses up to the yield limit are found both in the weld metal and in the heat-affected zone. Numerical modeling allowed the qualitative estimation of the hydrogen diffusion in the weld. No noticeable HAC occurrence was identified and confirms the high cracking resistance of the investigated material. Finally, the applicability of the MWT concept should be critically discussed. KW - Hydrogen KW - Cold cracking KW - Minimum Waiting Time KW - Offshore steel grade KW - Component test PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591981 DO - https://doi.org/10.1007/s40194-023-01658-5 SP - 1 EP - 15 PB - Springer Science and Business Media LLC AN - OPUS4-59198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Mente, Tobias T1 - Trapping and diffusion in high-pressure hydrogen charged CoCrFeMnNi high entropy alloy compared to austenitic steel 316L N2 - High entropy alloys (HEAs) have attracted considerable research attention as potential substitute materials for austenitic steels in high-pressure hydrogen environments. The corresponding hydrogen absorption, diffusion and trapping has received less scientific attention. Therefore, the CoCrFeMnNi-HEA was investigated and compared to an austenitic steel AISI 316L. Both were subjected to high-pressure hydrogen charging at 200 bar and 1000 bar. Thermal Desorption Analysis (TDA) was used to clarify the specific desorption behavior and hydrogen trapping. For this purpose, the underlying TDA spectra were analyzed in terms of a reasonable peak deconvolution into a defined number of peaks and the activation energies for the respective and predominant hydrogen trapping sites were then calculated. Both materials show comparable hydrogen diffusivity. However, there were significant differences in the absorbed hydrogen concentrations at both charging pressures. The calculated activation energies suggest strong hydrogen trapping in the CoCrFeMnNi-HEA. KW - High-entropy alloy KW - Hydrogen diffusion KW - Trapping KW - High-pressure charging KW - Thermal desorption analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611901 DO - https://doi.org/10.1016/j.ijhydene.2024.09.393 SN - 0360-3199 VL - 89 IS - 89 SP - 772 EP - 782 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-61190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Mente, Tobias A1 - Richter, Tim A1 - Kannengießer, Thomas T1 - Characterization of Hydrogen Diffusion in Offshore Steel S420G2+M Multi-layer Submerged Arc Welded Joint N2 - As onshore installation capacity is limited, the increase in the number of offshore wind turbines (OWT) is a major goal. In that connection, the OWTs continuously increase in size and weight and demand adequate foundations concepts like monopiles or tripods. These components are typically manufactured from welded mild steel plates with thickness up to 200 mm. The predominant welding technique is submerged arc welding (SAW). In accordance with the standards, the occurrence of hydrogen-assisted cracking is anticipated by either a minimum waiting time (MWT, before non-destructive testing of the welded joint is allowed) at ambient or a hydrogen removal heat treatment (HRHT) at elevated temperatures. The effectiveness of both can be estimated by calculation of the diffusion time, i.e., diffusion coefficients. In this study, these coefficients are obtained for the first time for a thick-walled S420G2+M offshore steel grade and its multi-layer SAW joint. The electrochemical permeation technique at ambient temperature is used for the determination of diffusion coefficients for both the base material and the weld metal. The coefficients are within a range of 1025 to 1024 mm2/s (whereas the weld metal had the lowest) and are used for an analytical and numerical calculation of the hydrogen diffusion and the related MWT. The results showed that long MWT can occur, which would be necessary to significantly decrease the hydrogen concentration. Weld metal diffusion coefficients at elevated temperatures were calculated from hydrogen desorption experiments by carrier gas hot extraction. They are within a range of 1023 mm2/s and used for the characterization of a HRHT dwell-time. The analytical calculation shows the same tendency of long necessary times also at elevated temperatures. That means the necessary time is strongly influenced by the considered plate thickness and the estimation of any MWT/HRHT via diffusion coefficients should be critically discussed. T2 - European Congress and Exhibition on Advanced Materials and Process - Euromat 2021 CY - Online meeting DA - 13.09.2021 KW - Thick-walled KW - Hydrogen diffusion KW - Offshore KW - Steel KW - Submerged arc welding PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544127 DO - https://doi.org/10.1007/s11665-022-06679-7 SN - 1059-9495 SP - 1 EP - 13 PB - Springer Nature AN - OPUS4-54412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Richter, Tim A1 - Mente, Tobias A1 - Mayr, P A1 - Nitsche, A T1 - Hydrogen effect on mechanical properties and cracking of creep‑resistant 9% Cr P92 steel and P91 weld metal N2 - Martensitic 9% Cr steels like P91 and P92 can show an increased susceptibility to delayed hydrogen-assisted cracking. The focus of this study was the microstructure and heat treatment efect on the mechanical properties of P92 base material and P91 multi-layer weld metal in both as-welded and post weld heat treated (PWHT) condition. Tensile tests with hydrogen free reference samples and electrochemically hydrogen charged samples were carried out; the mechanical properties were assessed and supported by detailed fractographic analysis. Finally, a hydrogen and microstructure-dependent fracture criterion is established. All investigated microstructures showed a hydrogen-infuenced degradation of the mechanical properties compared to the hydrogen-free reference samples. The as-welded martensitic P91 weld metal had the highest degree of degradation in the presence of hydrogen. The P91 PWHT weld metal and the P92 base material had comparable properties. From that point of view, a signifcantly increased risk for hydrogen-assisted cold cracking during welding fabrication of P91 weld joints must be considered before any heat treatment is conducted. T2 - IIW Annual Assembly, Meeting of Commission IX-C CY - Tokyo, Japan DA - 16.07.2022 KW - Creep-resisting materials KW - Welding KW - Hydrogen assisted cracking KW - Hydrogen embrittlement KW - Mechanical properties PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564070 DO - https://doi.org/10.1007/s40194-022-01410-5 SN - 0043-2288 SP - 1 EP - 12 PB - Springer Nature CY - Basel (CH) AN - OPUS4-56407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Richter, Tim A1 - Mente, Tobias A1 - Mayr, P. A1 - Nitsche, A. T1 - Thickness and microstructure effect on hydrogen diffusion in creep‑resistant 9% Cr P92 steel and P91 weld metal N2 - Martensitic 9% Cr steels like P91 and P92 show susceptibility to delayed hydrogen assisted cracking depending on their microstructure. In that connection, effective hydrogen diffusion coefficients are used to assess the possible time-delay. Limited data on room temperature diffusion coefficients reported in literature vary widely by several orders of magnitude (mostly attributed to variation in microstructure). Especially P91 weld metal diffusion coefficients are rare so far. For that reason, electrochemical permeation experiments had been conducted using P92 base metal and P91 weld metal (in as-welded and heat-treated condition) with different thicknesses. From the results obtained, diffusion coefficients were calculated using to different methods, time-lag, and inflection point. Results show that, despite microstructural effects, the sample thickness must be considered as it influences the calculated diffusion coefficients. Finally, the comparison of calculated and measured hydrogen concentrations (determined by carrier gas hot extraction) enables the identification of realistic diffusion coefficients. KW - Creep-resistant steel KW - Diffusion KW - Hydrogen assisted cracking KW - Welding KW - Electrochemical permeation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540645 DO - https://doi.org/10.1007/s40194-021-01218-9 SN - 0043-2288 SP - 1 EP - 16 PB - Springer Nature Switzerland AG AN - OPUS4-54064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Anja A1 - Buchberger, G. A1 - Stifter, D. A1 - Duchoslav, J. A1 - Hertwig, Andreas A1 - Bonse, Jörn A1 - Heitz, J. A1 - Schwibbert, Karin T1 - Spatial Period of Laser-Induced Surface Nanoripples on PET Determines Escherichia coli Repellence N2 - Bacterial adhesion and biofilm formation on surfaces are associated with persistent microbial contamination, biofouling, and the emergence of resistance, thus, calling for new strategies to impede bacterial surface colonization. Using ns-UV laser treatment (wavelength 248 nm and a pulse duration of 20 ns), laser-induced periodic surface structures (LIPSS) featuring different submicrometric periods ranging from ~210 to ~610 nm were processed on commercial poly(ethylene terephthalate) (PET) foils. Bacterial adhesion tests revealed that these nanorippled surfaces exhibit a repellence for E. coli that decisively depends on the spatial periods of the LIPSS with the strongest reduction (~91%) in cell adhesion observed for LIPSS periods of 214 nm. Although chemical and structural analyses indicated a moderate laser-induced surface oxidation, a significant influence on the bacterial adhesion was ruled out. Scanning electron microscopy and additional biofilm studies using a pili-deficient E. coli TG1 strain revealed the role of extracellular appendages in the bacterial repellence observed here. KW - Laser-induced periodic surface structures (LIPSS) KW - Laser processing KW - Polyethylene terephthalate KW - Biofilm formation KW - Cell appendages KW - Biomimetic KW - F pili PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537431 DO - https://doi.org/10.3390/nano11113000 VL - 11 IS - 11 SP - 3000 PB - MDPI AN - OPUS4-53743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Anja A1 - Possling, A. A1 - Malysheva, N. A1 - Yousef, K. P. A1 - Herbst, S. A1 - von Kleist, M. A1 - Hengge, R. T1 - Local c-di-GMP signaling in the control of synthesis of the E. coli biofilm exopolysaccharide pEtN-cellulose N2 - In many bacteria, the biofilm-promoting second messenger c-di-GMP is produced and degraded by multiple diguanylate cyclases (DGC) and phosphodiesterases (PDE), respectively. High target specificity of some of these enzymes has led to theoretical concepts of "local" c-di-GMP signaling. In Escherichia coli K-12, which has 12 DGCs and 13 PDEs, a single DGC, DgcC, is specifically required for the biosynthesis of the biofilm exopolysaccharide pEtN-cellulose without affecting the cellular c-di-GMP pool, but the mechanistic basis of this target specificity has remained obscure. DGC activity of membrane-associated DgcC, which is demonstrated in vitro in nanodiscs, is shown to be necessary and sufficient to specifically activate cellulose biosynthesis in vivo. DgcC and a particular PDE, PdeK (encoded right next to the cellulose operon), directly interact with cellulose synthase subunit BcsB and with each other, thus establishing physical proximity between cellulose synthase and a local source and sink of c-di-GMP. This arrangement provides a localized, yet open source of c-di-GMP right next to cellulose synthase subunit BcsA, which needs allosteric activation by c-di-GMP. Through mathematical modeling and simulation, we demonstrate that BcsA binding from the low cytosolic c-di-GMP pool in E. coli is negligible, whereas a single c-di-GMP molecule that is produced and released in direct proximity to cellulose synthase increases the probability of c-di-GMP binding to BcsA several hundred-fold. This local c-di-GMP signaling could provide a blueprint for target-specific second messenger signaling also in other bacteria where multiple second messenger producing and degrading enzymes exist. KW - Biofilm KW - Cellulose synthase KW - Bacterial second messenger KW - C-di-GMP PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511214 DO - https://doi.org/10.1016/j.jmb.2020.06.006 SN - 0022-2836 VL - 432 IS - 16 SP - 4576 EP - 4595 PB - Elsevir Ltd. AN - OPUS4-51121 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Maria A1 - Güttler, Arne A1 - Pauli, Jutta A1 - Vogel, K. A1 - Homann, Christian A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Extending certified spectral fluorescence standards for the calibration and performance validation of fluorescence instruments to the NIR—closing the gap from 750 to 940 nm with two novel NIR dyes N2 - Fluorescence techniques such as fluorescence spectroscopy, microfluorometry, and fluorescence microscopy, providing spectral, intensity, polarization, and lifetime information, are amongst the most broadly utilized analytical methods in the life and materials sciences. However, the measured fluorescence data contain sample- and instrument-specific contributions, which hamper their comparability across instruments and laboratories. Comparable, instrument-independent fluorescence data require the determination of the fluorescence instrument’s wavelength-dependent spectral responsivity, also termed emission correction curve, for the same instrument settings as those used for the fluorescence measurements as a prerequisite for the subsequent correction of the measured instrument-specific data. Such a spectral correction is essential for the performance comparison of different fluorescent labels and reporters, quantitative fluorescence measurements, the determination of the fluorescence quantum yield, and the spectroscopic measure for the fluorescence efficiency of a fluorophore. Simple-to-use tools for obtaining emission correction curves are chromophore-based reference materials (RMs), referred to as fluorescence standards, with precisely known, preferably certified instrument-independent fluorescence spectra. However, for the increasingly used near-infrared (NIR) wavelength region >700 nm, at present, no spectral fluorescence standards are available. To close this gap, we developed two novel spectral fluorescence standards, BAM F007 and BAM-F009, with broad emission bands from about 580 to 940 nm in ethanolic solution. These liquid fluorescence standards currently under certification, which will be released in 2025, will expand the wavelength range of the already available certified Calibration Kit BAM F001b-F005b from about 300–730 to 940 nm. In this research article, we will detail the criteria utilized for dye and matrix selection and the homogeneity and stability tests accompanying dye certification as well as the calculation of the wavelength-dependent uncertainty budgets of the emission spectra BAM F007 and BAM-F009, determined with the traceably calibrated BAM reference spectrofluorometer. These fluorescence standards can provide the basis for comparable fluorescence measurements in the ultraviolet, visible, and NIR for the fluorescence community. KW - Quality assurance KW - Reference material KW - Fluorescence KW - Dye KW - Traceability KW - Metrology KW - Calibration KW - Reference data KW - Reference product KW - Digital certificate KW - NIR KW - Instrument performance validation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626317 DO - https://doi.org/10.1007/s00216-024-05723-w SN - 1618-2650 SP - 1 EP - 15 PB - Springer AN - OPUS4-62631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Matthias A1 - Horn, Wolfgang A1 - Juritsch, Elevtheria A1 - Klinge, A. A1 - Radeljic, L. A1 - Jann, Oliver T1 - Natural building materials for interior fitting and refurbishment - What about indoor emissions? N2 - Indoor air quality can be adversely affected by emissions from building materials, consequently having a negative impact on human health and well-being. In this study, more than 30 natural building materials (earth dry boards and plasters, bio-based insulation materials, and boards made of wood, flax, reed, straw, etc.) used for interior works were investigated as to their emissions of (semi-) volatile organic compounds ((S)VOC), formaldehyde, and radon. The study focused on the emissions from complete wall build-ups as they can be used for internal Partition walls and the internal insulation of external walls. Test chambers were designed, allowing the compounds to release only from the surface of the material facing indoors under testing Parameters that were chosen to simulate model room conditions. The emission test results were evaluated using the AgBB evaluation scheme, a procedure for the health-related evaluation of construction products and currently applied for the approval of specific groups of building materials in Germany. Seventeen out of 19 sample build-ups tested in this study would have passed this scheme since they generally proved to be low-emitting and although the combined emissions of multiple materials were tested, 50% of the measurements could be terminated before half of the total testing time. KW - Bio-based insulation KW - Earthen building materials KW - Volatile organic compounds KW - Semivolatile organic compounds KW - Radon PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519634 DO - https://doi.org/10.3390/ma14010234 VL - 14 IS - 1 (Special issue: Measurement of the environmental impact of materials) SP - 234-1 EP - 234-14 PB - MDPI CY - Basel AN - OPUS4-51963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Matthias A1 - Schühle, Florian T1 - Experimental determination of 7-day uptake rates for diffusive sampling of 86 volatile and semi-volatile organic compounds relevant for indoor air monitoring and investigation on their sensitivity to exposure time and indoor climate N2 - This study aimed to experimentally determine uptake rates for 86 indoor relevant volatile and semi-volatile organic compounds (VOC, SVOC) for the passive sampler type Perkin Elmer/Markes™ with Tenax® TA as sorbent, which was used in the German Environmental Survey on Health (GerES VI) carried out by the German Environmental Agency (UBA) in the years 2023-2024. For this purpose, single reference gas atmospheres of 76 pure VOCs (liquid at room temperature) and a group of 10 SVOCs and VOCs (solid at room temperature) were generated using two generation procedures. By exposing the samplers to individual components, it was ruled out that interactions in a mixture have a influence on the uptake rate. Another aspect was to precisely describe the methodology and the resulting uncertainties, as there are gaps in the literature in this regard. The selection of the compounds was based on the findings of the preceding GerES V study for which data was missing or needed to be verified. In each experiment, a number of six passive samplers was exposed to the test gas atmospheres in dynamically operated exposure chambers for seven days. The sensitivity of the uptake rates of a group of 10 selected VOCs to variations in exposure time, ambient temperature, and air humidity in a multi-component reference gas atmosphere was investigated. Here, a decrease in the uptake rate with the exposure time could be observed stabilising from the fifth day of exposure onwards. A significant effect of temperature and humidity on the uptake rate was not apparent. The determined uptake rates exhibit uncertainties of < 20 % for 71 substances, and < 10 % for 51 substances which are also in good agreement with the literature, if already published elsewhere. The quantity of investigated substances, the detailed description of the methodology used to determine the uptake rates complemented by the respective uncertainties, as well as the compilation of comparative data, contribute to a better assessment of the quality and relevance of such data, which had not been published before. KW - Indoor air quality KW - Volatile organic compounds KW - Uptake rates KW - Passive sampling KW - Tenax TA PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629913 DO - https://doi.org/10.1016/j.indenv.2025.100095 VL - 2 IS - 2 SP - 1 EP - 11 PB - Elsevier AN - OPUS4-62991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, S. A1 - Horstmann, J. A1 - Altmann, Korinna A1 - Braun, U. A1 - Hagendorf, C. T1 - A reference methodology for microplastic particle size distribution analysis: Sampling, filtration, and detection by optical microscopy and image processing N2 - Microplastic (MP) contamination in natural water circulation is a concern for environmental issues and human health. Various types of polymer materials have been identified and were detected in MP analytic test procedures. Beyond MP polymer type, particle size and form play a major role in water analysis due to possible negative toxicologic effects on flora and fauna. However, the correct quantitative measurement of MP size distribution over several orders of magnitude is strongly influenced by sample preparation, filtration materials and processes, and microanalytical techniques, as well as data acquisition and analysis. In this paper, a reference methodology is presented aiming at an improved quantitative analysis of MP particles. An MP analysis workflow is demonstrated including all steps from reference materials to sample preparation, filtration handling, and MP particle size distribution analysis. Background-corrected particle size distributions (1–1000 µm) have been determined for defined polyethylene (PE) and polyethylene terephthalate (PET) reference samples. Microscopically measured particle numbers and errors have been cross-checked with the total initial mass. In particular, defined reference MP samples (PE, PET) are initially characterized and applied to filtration experiments. Optical microscopy imaging on full-area Si filters with subsequent image analysis algorithms is used for statistical particle size distribution analysis. To quantify the effects of handling and filtration, several blind tests with distilled water are carried out to determine the particle background for data evaluation. Particle size distributions of PE and PET reference samples are qualitatively and quantitatively reproduced with respect to symmetry, and maximum and cut-off diameter of the distribution. It is shown that especially MP particles with a radius of >50 µm can be detected and retrieved with high reliability. For particle sizes <50 µm, a significant interference with background contamination is observed. Data from blank samples allows a correction of background contaminations. Furthermore, for enhanced sampling statistics, the recovery of the initial amount of MP will be qualitatively shown. The results are intended as an initial benchmark for MP analytics quality. This quality is based on statistical MP particle distributions and covers the complete analytic workflow starting from sample preparation to filtration and detection. Microscopic particle analysis provides an important supplement for the evaluation of established spectroscopic methods such as Fourier-transform infrared spectroscopy or Raman spectroscopy. KW - Drinking water KW - Filtration KW - Microplastics detection KW - Quality control KW - Statistical particle distribution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567625 DO - https://doi.org/10.1002/appl.202200055 SN - 2702-4288 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke A1 - Roethke, A. A1 - Rienitz, O. A1 - Matschat, Ralf A1 - Schiel, D. A1 - Jaehrling, R. A1 - Goerlitz, V. A1 - Kipphardt, Heinrich T1 - SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods N2 - Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM – 25 years ago – up to latest achievements in the field of inorganic analysis. KW - Metrology KW - SI Traceability KW - CCQM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496080 DO - https://doi.org/10.1088/1681-7575/ab5636 SN - 0026-1394 SN - 1681-7575 SP - 1 EP - 23 PB - IOP CY - Bristol AN - OPUS4-49608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Delgado Arroyo, Diego A1 - Börner, Andreas A1 - Schröpfer, Dirk A1 - Rhode, Michael A1 - Lindner, T. A1 - Löbel, M. A1 - Preuß, B. A1 - Lampke, T. T1 - Ultrasonic assisted milling of a CoCrFeNi medium entropy alloy N2 - Medium and High Entropy Alloys (MEA/HEA) are recently developed material classes, providing manifold applications, e.g., due to extraordinary structural properties. In that connection, the machinability as important issue for the processing of these materials was not in the scientific focus. This study focusses on experimental analysis of milling process conditions including ultrasonic assisted milling (USAM) and their effects on the resulting surface integrity of equiatomic CoCrFeNi-MEA specimens. For that reason, milling parameters (cutting speed, feed per cutting edge) were systematically varied for both conventional milling and USAM. The surface integrity was analyzed in terms of topography, defects, and residual stresses. Especially USAM leads to a decrease of occurring cutting forces and, hence, to an improvement of the surface integrity. Beneficial effects were observed in terms of lower tensile residual stresses at high cutting speed and feed per cutting edge. KW - Medium entropy alloy KW - Ultrasonic Assisted Machining KW - Surface Integrity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554458 DO - https://doi.org/10.1016/j.procir.2022.05.203 VL - 108 SP - 879 EP - 884 PB - Elsevier B.V. AN - OPUS4-55445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Giese, Marcel A1 - Rhode, Michael A1 - Schröpfer, Dirk A1 - Michael, Thomas A1 - Fritsch, Tobias T1 - Influence of Surface Preparation on Cracking Phenomena in TIG-Welded High and Medium Entropy Alloys N2 - Multi-element systems with defined entropy (HEA—high entropy alloy or MEA—medium entropy alloy) are rather new material concepts that are becoming increasingly important in materials research and development. Some HEA systems show significantly improved properties or combinations of properties, e.g., the overcoming of the trade-off between high strength and ductility. Thus, the synthesis, the resulting microstructures, and properties of HEA have been primarily investigated so far. In addition, processing is crucial to achieve a transfer of potential HEA/MEA materials to real applications, e.g., highly stressed components. Since fusion welding is the most important joining process for metals, it is of vital importance to investigate the weldability of these materials. However, this has rarely been the subject of research to date. For that reason, in this work, the weldability depending on the surface preparation of a CoCrFeMnNi HEA and a CoCrNi MEA for TIG welding is investigated. The fusion welding of longer plates is described here for the first time for the CoCrNi alloy. The welds of both materials showed distinct formation of cracks in the heat affected Zone (HAZ). Optical and scanning electron microscopy analysis clearly confirmed an intergranular fracture topography. However, based on the results, the crack mechanism cannot be conclusively identified as either a liquid metal embrittlement (LME) or hot cracking-like liquid film separation. T2 - 2nd International Conference on Advanced Joining Processes CY - Sintra, Portugal DA - 21.10.2021 KW - TIG welding KW - Cracking KW - High entropy alloy KW - Medium entropy alloy KW - Surface preparation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-541697 DO - https://doi.org/10.3390/jmmp6010005 SN - 2504-4494 VL - 6 IS - 5 SP - 1 EP - 13 PB - MDPI CY - Basel (CH) AN - OPUS4-54169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Rhode, Michael T1 - Residual stresses in a high- and a medium-entropy alloy due to TIG and friction stir welding N2 - The new alloying concept of multi-element systems with defined entropy (HEA—high-entropy alloy; MEA—medium-entropy alloy) is gaining increasing importance in materials research. Significantly improved properties or combinations of properties are shown by some HEA/MEA systems. Thus, primarily the production and resulting microstructures of HEA, as well as its properties, have been investigated so far. Furthermore, processing is a main issue in transferring HEA systems from the laboratory to real components. Since welding is the most important joining process for metals, it is crucial to investigate the influence of welding to guarantee component integrity. Welding leads to residual stresses, which significantly affect the component integrity. Hence, the focus of this study is the residual stress formation and distribution in a CoCrFeMnNi HEA and ternary CoCrNi MEA using two different welding processes: tungsten inert gas (TIG) welding and solid-state friction stir welding (FSW). As a pathway for the application of HEA in this investigation, for the first time, residual stress analyses in realistic near-component specimens were performed. The residual stresses were determined by X-ray diffraction (XRD) on the surfaces of top and root weld side. The results were correlated with the local welding microstructures. The results show that both FSW and TIG generate significant tensile residual stresses on the weld surfaces in, and transverse to, the welding direction. In the case of FSW of the CoCrFeMnNi HEA, the longitudinal residual stresses are in the range of the yield strength of approx. 260 MPa in the weld zone. KW - High entropy alloy KW - Welding KW - Residual stresses KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567039 DO - https://doi.org/10.3390/jmmp6060147 SN - 2504-4494 VL - 6 IS - 6 SP - 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-56703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riebesell, Janosh A1 - Goodall, Rhys E. A. A1 - Benner, Philipp A1 - Chiang, Yuan A1 - Deng, Bowen A1 - Ceder, Gerbrand A1 - Asta, Mark A1 - Lee, Alpha A. A1 - Jain, Anubhav A1 - Persson, Kristin A. T1 - A framework to evaluate machine learning crystal stability predictions N2 - The rapid adoption of machine learning in various scientific domains calls for the development of best practices and community agreed-upon benchmarking tasks and metrics. We present Matbench Discovery as an example evaluation framework for machine learning energy models, here applied as pre-filters to first-principles computed data in a high-throughput search for stable inorganic crystals. We address the disconnect between (1) thermodynamic stability and formation energy and (2) retrospective and prospective benchmarking for materials discovery. Alongside this paper, we publish a Python package to aid with future model submissions and a growing online leaderboard with adaptive user-defined weighting of various performance metrics allowing researchers to prioritize the metrics they value most. To answer the question of which machine learning methodology performs best at materials discovery, our initial release includes random forests, graph neural networks, one-shot predictors, iterative Bayesian optimizers and universal interatomic potentials. We highlight a misalignment between commonly used regression metrics and more task-relevant classification metrics for materials discovery. Accurate regressors are susceptible to unexpectedly high false-positive rates if those accurate predictions lie close to the decision boundary at 0 eV per atom above the convex hull. The benchmark results demonstrate that universal interatomic potentials have advanced sufficiently to effectively and cheaply pre-screen thermodynamic stable hypothetical materials in future expansions of high-throughput materials databases. KW - Machine Learning KW - Interatomic Potentials PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637139 DO - https://doi.org/10.1038/s42256-025-01055-1 SN - 2522-5839 VL - 7 IS - 6 SP - 836 EP - 847 PB - Springer Science and Business Media LLC AN - OPUS4-63713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riechers, Birte A1 - Das, Amlan A1 - Dufresne, Eric A1 - Derlet, Peter M. A1 - Maaß, Robert T1 - Intermittent cluster dynamics and temporal fractional diffusion in a bulk metallic glass N2 - Glassy solids evolve towards lower-energy structural states by physical aging. This can be characterized by structural relaxation times, the assessment of which is essential for understanding the glass’ time-dependent property changes. Conducted over short times, a continuous increase of relaxation times with time is seen, suggesting a time-dependent dissipative transport mechanism. By focusing on micro-structural rearrangements at the atomic-scale, we demonstrate the emergence of sub-diffusive anomalous transport and therefore temporal fractional diffusion in a metallic glass, which we track via coherent x-ray scattering conducted over more than 300,000 s. At the longest probed decorrelation times, a transition from classical stretched exponential to a power-law behavior occurs, which in concert with atomistic simulations reveals collective and intermittent atomic motion. Our observations give a physical basis for classical stretched exponential relaxation behavior, uncover a new power-law governed collective transport regime for metallic glasses at long and practically relevant time-scales, and demonstrate a rich and highly non-monotonous aging response in a glassy solid, thereby challenging the common framework of homogeneous aging and atomic scale diffusion. KW - Glassy solids KW - Fractional diffusion KW - Coherent x-ray scattering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608015 DO - https://doi.org/10.1038/s41467-024-50758-3 VL - 15 IS - 1 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-60801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riechers, Birte A1 - Das, Amlan A1 - Rashidi, Reza A1 - Dufresne, Eric A1 - Maaß, Robert T1 - Metallic glasses: Elastically stiff yet flowing at any stress N2 - Crystalline solids have a minimum stress needed to displace atoms or to move defects. This stress defines the true elastic limit and is generally a sizeable share of the macroscopic yield stress. Here we demonstrate that a metallic glass, an amorphous solid with a yield stress in the giga-pascal regime, lacks such a true microscopic elastic limit. Leveraging in-situ coherent x-ray scattering, we uncover a strongly accelerated atomic-scale transport upon the application of a stress as small as 0.005 times the yield stress. With increasing stress levels, the distribution of structural relaxation times changes from compressed exponential to simple exponential form, revealing a stress–temperature equivalence in the time-scale domain. These findings strongly promote a microstructurally heterogeneous picture of metallic glasses, in which a part of the amorphous microstructure controls macroscopic yielding whereas another part admits microplastic flow at any stress. KW - Metallic glasses KW - Microstructure PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624530 DO - https://doi.org/10.1016/j.mattod.2024.11.015 VL - 82 SP - 92 EP - 98 PB - Elsevier B.V. AN - OPUS4-62453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riechers, Birte A1 - Ott, C. A1 - Das, S. M. A1 - Liebscher, C. A1 - Samwer, K. A1 - Derlet, P. M. A1 - Maaß, Robert T1 - On the elastic microstructure of bulk metallic glasses N2 - Metallic glasses (MGs) are known to be structurally heterogeneous at the nanometer (nm) scale. In addition, elastic property mapping has indicated the presence of at least an order-of-magnitude larger length scales, of which the origin continues to remain unknown. Here we demonstrate the existence of an elastic decorrelation length of the order of 100 nm in a Zr-based bulk MG using spatially resolved elastic property mapping via nanoindentation. Since compositional modulations sufficiently large to account for this elastic microstructure were not resolved by analytical scanning-transmission electron microscopy, chemical phase separation such as spinodal decomposition cannot explain their occurrence as previously suggested. Instead, we argue that the revealed long-range elastic modulations stem from structural variations affecting the local density. These emerge during solidification and are strongly influenced by the cooling constraints imposed on bulk MGs during the casting process. KW - Metallic glasses KW - Nanoindentation KW - Elastic microstructure PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573504 DO - https://doi.org/10.1016/j.matdes.2023.111929 SN - 0264-1275 VL - 229 SP - 1 EP - 8 PB - Elsevier Ltd. CY - Amsterdam, Niederlande AN - OPUS4-57350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riechers, Birte A1 - Roed, L. A1 - Mehri, S. A1 - Ingebrigtsen, T. A1 - Hecksher, T. A1 - Dyre, J. A1 - Niss, K. T1 - Predicting nonlinear physical aging of glasses from equilibrium relaxation via the material time N2 - The noncrystalline glassy state of matter plays a role in virtually all fields of materials science and offers complementary properties to those of the crystalline counterpart. The caveat of the glassy state is that it is out of equilibrium and therefore exhibits physical aging, i.e., material properties change over time. For half a century, the physical aging of glasses has been known to be described well by the material-time concept, although the existence of a material time has never been directly validated. We do this here by successfully predicting the aging of the molecular glass 4-vinyl-1,3-dioxolan-2-one from its linear relaxation behavior. This establishes the defining property of the material time. Via the fluctuation-dissipation theorem, our results imply that physical aging can be predicted from thermal-equilibrium fluctuation data, which is confirmed by computer simulations of a binary liquid mixture. KW - Physical aging KW - Equilibrium relaxation KW - Glass PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546015 DO - https://doi.org/10.1126/sciadv.abl9809 SN - 2375-2548 VL - 8 IS - 11 SP - 1 EP - 8 PB - American Association for the Advancement of Science CY - Washington, DC AN - OPUS4-54601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Jens A1 - Hufgard, Josefin A1 - You, Yi T1 - LIBS at high duty-cycles: effect of repetition rate and temporal width on the excitation laser pulses N2 - Laser-induced breakdown spectroscopy (LIBS) is becoming a more mature technology every year with new variants such as laser ablation molecular isotopic spectrometry, reheating by various discharge techniques, and multiple pulse excitation schemes, in which sometimes lasers of different pulse lengths are used. However, lasers with inherent parameters like pulse length and repetition rate are still almost exclusively employed. Recent years have witnessed the advent of novel high-repetition-rate laser concepts for machining processes, like welding, milling, and engraving. Here, a comprehensive study of single-pulse LIBS spectra of a single aluminum target is presented to showcase the applicability of flexible high duty-cycle master oscillator power amplifier (MOPA) lasers. Although traditional flashlamp-pumped Fabry–Pérot lasers only permit a variation in the pulse energy and are operated at very low duty-cycles, MOPA lasers add repetition rate and pulse length as variable parameters. A thorough analysis of the temporal plasma behavior revealed the emission dynamic to closely match the excitation laser pulse pattern. An aluminum sample’s spectral response was shown to be significantly impacted by variations in both rate and length. Although the spectral emission strength of the elemental lines of Al, Sr, and Ca all peaked at slightly different parameter settings, the strongest impact was found on the relative abundance of molecular AlO bands. Unlike in previous laser ablation molecular isotopic spectrometry (LAMIS) publications, the latter could be readily detected with a good intensity and well-resolved spectral features without any temporal gating of the detector. This finding, together with the fact that MOPA lasers are both inexpensive and dependable, makes for a promising combination for future studies including the detection of diatomic band structures. KW - Laser-induced breakdown spectroscopy KW - LIBS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583300 DO - https://doi.org/10.3389/fphy.2023.1241533 SN - 2296-424X VL - 11 SP - 1 EP - 8 AN - OPUS4-58330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Juliane A1 - Recknagel, Sebastian A1 - Sassenroth, Diana A1 - Mauch, Tatjana A1 - Buttler, Sabine A1 - Sommerfeld, Thomas A1 - Penk, Sibylle A1 - Koch, Matthias T1 - Development and certification of a reference material for zearalenone in maize germ oil N2 - Zearalenone (ZEN), an estrogenic mycotoxin produced by several species of Fusarium fungi, is a common contaminant of cereal-based food worldwide. Due to frequent occurrences associated with high levels of ZEN, maize oil is a particular source of exposure. Although a European maximumlevel for ZEN in maize oil exists according to Commission Regulation (EC) No. 1126/2007 along with a newly developed international standard method for analysis, certified reference materials (CRM) are still not available. To overcome this lack, the first CRM for the determination of ZEN in contaminated maize germ oil (ERM®-BC715) was developed in the frame of a European Reference Materials (ERM®) project according to the requirements of ISO Guide 35. The whole process of CRM development including preparation, homogeneity and stability studies, and value assignment is presented. The assignment of the certified mass fraction was based upon an in-house study using high-performance liquid chromatography isotope dilution tandem mass spectrometry. Simultaneously, to support the in-house certification study, an interlaboratory comparison study was conducted with 13 expert laboratories using different analytical methods. The certified mass fraction and expanded uncertainty (k=2) of ERM®-BC715 (362± 22) μg kg−1 ZEN are traceable to the SI. This reference material is intended for analytical quality control and contributes to the improvement of consumer protection and food safety. KW - Fusarium mycotoxin KW - Vegetable edible oil KW - Food analysis KW - European Reference Material KW - Quality assurance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531831 DO - https://doi.org/10.1007/s00216-021-03532-z SN - 1618-2642 SN - 1618-2650 VL - 413 IS - 21 SP - 5483 EP - 5491 PB - Springer CY - Berlin AN - OPUS4-53183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Soraya A1 - Hülagü, Deniz A1 - Bennet, Francesca A1 - Carl, Peter A1 - Flemig, Sabine A1 - Schmid, Thomas A1 - Schenk, J. A. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf T1 - Electrochemical Immunomagnetic Ochratoxin A Sensing: Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine in Amperometric Assays N2 - Electrochemical methods offer great promise in meeting the demand for user-friendly on-site devices for Monitoring important parameters. The food industry often runs own lab procedures, for example, for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with smart technologies. Enzyme-linked immunosorbent assays, with photometric detection of 3,3’,5,5’-tetramethylbenzidine (TMB),form a good basis for sensitive detection. To provide a straightforward approach for the miniaturization of the detectionstep, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry it was found that the TMB electrochemistry is strongly dependent on the pH and the electrode material. A stable electrode response to TMB could be achieved at pH 1 on gold electrodes. We created a smartphonebased, electrochemical, immunomagnetic assay for the detection of ochratoxin A in real samples, providing a solid basis forsensing of further analytes. KW - Ochratoxin A KW - Amperometry KW - Cyclic voltammetry KW - Electrochemistry KW - Immunoassay PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530421 DO - https://doi.org/10.1002/celc.202100446 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. VL - 8 IS - 13 SP - 2597 EP - 2606 AN - OPUS4-53042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Soraya A1 - Jaut, Valerie A1 - Schneider, Rudolf T1 - Ergometrine sensing in rye flour by a magnetic bead-based immunoassay followed by flow injection analysis with amperometric detection N2 - A certain group of mycotoxins, the ergot alkaloids, has caused countless deaths throughout human history. They are found in rye and other cereals and ingesting contaminated foods can cause serious health problems. To identify contaminated food exceeding the legal limits for ergot alkaloids, a portable and cost-effective test system is of great interest to the food industry. Rapid analysis can be achieved by screening for a marker compound, for which we chose ergometrine. We developed a magnetic bead-based immunoassay for ergometrine with amperometric detection in a flow injection system using a handheld potentiostat and a smartphone. With this assay a limit of detection of 3 nM (1 μg/L) was achieved. In spiked rye flour, ergometrine levels from 25 to 250 μg/kg could be quantified. All results could be verified by optical detection. The developed assay offers great promise to meet the demand for on-site ergometrine detection in the food industry. KW - Ergot alkaloids KW - Amperometry KW - Magnetic beads KW - Immunoassay KW - Food analysis KW - Fow injection analysis KW - Mycotoxins PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565906 DO - https://doi.org/10.1016/j.talanta.2022.124172 SN - 0039-9140 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. VL - 254 IS - 124172 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-56590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieder, Philipp A1 - Petrich, Lukas A1 - Serrano-Munoz, Itziar A1 - Mouiya, Mossaab A1 - Markötter, Henning A1 - Huger, Marc A1 - Bruno, Giovanni A1 - Schmidt, Volker T1 - Statistical analysis of grains and pores within polycrystalline Al2TiO5 ceramics, based on X-ray computed tomography N2 - Advanced statistical image analysis workflows were developed to segment and quantitatively evaluate 2D electron-backscatter diffraction (EBSD) maps and 3D synchrotron X-ray computed tomography (SXCT) volumes of a polycrystalline Al2TiO5 refractory composite that contains microcracks and pores. Several size, shape, and further geometric descriptors were determined for both the solid phase (Al2TiO5 grains) and the pore space. The resulting pore-size distribution is distinctly bimodal: coarse pores (tens to hundreds of micrometers), traced to incomplete powder compaction, coexist with fine pores generated during sintering. The two pore populations appear to be correlated with grain growth and crystallographic orientation in different ways. Finally, the descriptors obtained from the 2D EBSD and 3D SXCT data sets are internally consistent but complementary, highlighting the value of characterizations based on EBSD and SXCT in the microstructural study of refractory ceramics. KW - Synchrotron X-ray computed tomography KW - Electron-backscatter diffraction KW - Aluminum titanate KW - Morphological reconstruction KW - Image Segmentation KW - Statistical image analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643918 DO - https://doi.org/10.1016/j.matchar.2025.115602 SN - 1044-5803 VL - 229 SP - 1 EP - 13 PB - Elsevier Inc. AN - OPUS4-64391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieger, J. A1 - Colla, V. A1 - Matino, I. A1 - Branca, T. A. A1 - Stubbe, G. A1 - Panizza, A. A1 - Brondi, C. A1 - Falsafi, M. A1 - Hage, J. A1 - Wang, X. A1 - Voraberger, B. A1 - Fenzl, T. A1 - Masaguer, V. A1 - Faraci, E. L. A1 - di Sante, L. A1 - Cirilli, F. A1 - Loose, Florian A1 - Thaler, C. A1 - Soto, A. A1 - Frittella, P. A1 - Foglio, G. A1 - di Cecca, C. A1 - Tellaroli, M. A1 - Corbella, M. A1 - Guzzon, M. A1 - Malfa, E. A1 - Morillon, A. A1 - Algermissen, D. A1 - Peters, K. A1 - Snaet, D. T1 - Residue Valorization in the Iron and Steel Industries: Sustainable Solutions for a Cleaner and More Competitive Future Europe N2 - The steel industry is an important engine for sustainable growth, added value, and high-quality employment within the European Union. It is committed to reducing its CO2 emissions due to production by up to 50% by 2030 compared to 1990′s level by developing and upscaling the technologies required to contribute to European initiatives, such as the Circular Economy Action Plan (CEAP) and the European Green Deal (EGD). The Clean Steel Partnership (CSP, a public–private partnership), which is led by the European Steel Association (EUROFER) and the European Steel Technology Platform (ESTEP), defined technological CO2 mitigation pathways comprising carbon direct avoidance (CDA), smart carbon usage SCU), and a circular economy (CE). CE ap-proaches ensure competitiveness through increased resource efficiency and sustainability and consist of different issues, such as the valorization of steelmaking residues (dusts, slags, sludge) for internal recycling in the steelmaking process, enhanced steel recycling (scrap use), the use of secondary carbon carriers from non-steel sectors as a reducing agent and energy source in the steelmaking process chain, and CE business models (supply chain analyses). The current paper gives an overview of different technological CE approaches as obtained in a dedicated workshop called “Resi4Future—Residue valorization in iron and steel industry: sustainable solutions for a cleaner and more competitive future Europe” that was organized by ESTEP to focus on future challenges toward the final goal of industrial deployment. KW - Circular economy KW - Steelmaking residues KW - Clean steel PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530350 DO - https://doi.org/10.3390/met11081202 VL - 11 IS - 8 SP - 1202 PB - MDPI AN - OPUS4-53035 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 - JOUR A1 - Rietsch, P. A1 - Sobottka, S. A1 - Hoffmann, K. A1 - Popov, A. A. A1 - Hildebrandt, P. A1 - Sarkar, B. A1 - Resch-Genger, Ute A1 - Eigler, S. T1 - Between Aromatic and Quinoid Structure: A Symmetrical UV to Vis/NIR Benzothiadiazole Redox Switch N2 - Reversibly switching the light absorption of organic molecules by redox processes is of interest for applications in sensors, light harvesting, smart materials, and medical diagnostics. This work presents a symmetrical benzothiadiazole (BTD) derivative with a high fluorescence quantum yield in solution and in the crystalline state and shows by spectroelectrochemical analysis that reversible switching of UV absorption in the neutral state, to broadband Vis/NIR absorption in the 1st oxidized state, to sharp band Vis absorption in the 2nd oxidized state, is possible. For the one-electron oxidized species, formation of a delocalized radical is confirmed by electron paramagnetic resonance spectroelectrochemistry. Furthermore, our results reveal an increasing quinoidal distortion upon the 1st and 2nd oxidation, which can be used as the leitmotif for the development of BTD based redox switches. KW - Dye KW - Electrochemistry KW - Switch KW - Redox KW - Sensor KW - Photophysics KW - Quantum yield KW - photoluminescence PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517222 DO - https://doi.org/10.1002/chem.202004009 VL - 26 IS - 72 SP - 17361 EP - 17365 PB - Wiley-VCH GmbH AN - OPUS4-51722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rietsch, P. A1 - Sobottka, S. A1 - Hoffmann, Katrin A1 - Hildebrandt, P. A1 - Sarkar, B. A1 - Resch-Genger, Ute A1 - Eigler, S. T1 - Identification of the Irreversible Redox Behavior of Highly Fluorescent Benzothiadiazoles N2 - Redox switches are applied in various fields of research, including molecular lifts, electronic devices and sensors. Switching the absorbance between UV and Vis/NIR by redox processes is of interest for applications in light harvesting or biomedicine. Here, we present a series of push-pull benzothiadiazole derivatives with high fluorescence quantum yields in solution and in the crystalline solid state. Spectroelectrochemical analysis reveals the switching of UV-absorption in the neutral state to Vis/NIR absorption in the reduced state. We identify the partial irreversibility of the switching process, which appears to be reversible on the cyclic voltammetry timescale. KW - Redox switch KW - Electrochemistry KW - Dye KW - Fluorescence KW - Absorption KW - Sensor KW - Benzothiadiazole PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520865 DO - https://doi.org/10.1002/cptc.202000050 SN - 2367-0932 VL - 4 IS - 9 SP - 668 EP - 673 PB - Wiley Online Library AN - OPUS4-52086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ringleb, F. A1 - Andree, Stefan A1 - Heidmann, B. A1 - Bonse, Jörn A1 - Eylers, K. A1 - Ernst, O. A1 - Boeck, T. A1 - Schmid, M. A1 - Krüger, Jörg T1 - Femtosecond laser-assisted fabrication of chalcopyrite micro-concentrator photovoltaics N2 - Micro-concentrator solar cells offer an attractive way to further enhance the efficiency of planar-cell technologies while saving absorber material. Here, two laser-based bottom-up processes for the fabrication of regular arrays of CuInSe2 and Cu(In,Ga)Se2 microabsorber islands are presented, namely one approach based on nucleation and one based on laser-induced forward transfer. Additionally, a procedure for processing these microabsorbers to functioning micro solar cells connected in parallel is demonstrated. The resulting cells show up to 2.9% efficiency and a significant efficiency enhancement under concentrated Illumination. KW - Chalcopyrite KW - Femtosecond laser patterning KW - Laser-induced forward transfer KW - Micro-concentrator solar cell KW - Photovoltaics PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-470026 DO - https://doi.org/10.3762/bjnano.9.281 SN - 2190-4286 VL - 9 SP - 3025 EP - 3038 PB - Beilstein-Institut zur Förderung der Chemischen Wissenschaften CY - Frankfurt, M. AN - OPUS4-47002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Risse, Kerstin A1 - Nikiforidis, Constantinos V. A1 - Morris, Imogen A1 - Thünemann, Andreas A1 - Drusch, Stephan T1 - Regulating the heat stability of protein-phospholipid stabilised oil-water emulsions by changing the phospholipid headgroup or fatty acyl chain N2 - Stabilising oil–water emulsions remains a central challenge across food, pharmaceutical and cosmetic applications. β-lactoglobulin (β-LG) and phospholipids (PLs) can act synergistically at oil-water interfaces: PLs adsorb rapidly, while β-LG forms a viscoelastic protein network that enhances long-term stability. However, competitive adsorption between proteins and PLs can disrupt interfacial structure. In addition, for commercial production, emulsions are often exposed to heat treatment during or after manufacture, for instance due to food safety requirements. Yet, the combined effects of PL structure and heat treatment on interfacial organisation and emulsion stability remain poorly understood. Here we show that PL saturation and processing temperature jointly determine interfacial organisation, protein-PL interactions and emulsion stability. Using β-LG-PL emulsions, we combined ζ-potential measurements, small-angle X-ray scattering (SAXS), micro-differential scanning calorimetry (μDSC), X-ray diffraction and confocal laser scanning microscopy (CLSM) to link interfacial composition with functional stability. Below the β-LG denaturation temperature (≤75 °C), saturated PLs promoted partial unfolding of β-LG at the interface without displacement, producing mixed protein-PL networks with enhanced viscoelasticity and stability. Unsaturated PLs displaced β-LG, yielding less elastic interfaces and promoting protein aggregation in the bulk. At ≥75 °C, increased hydrophobicity intensified protein-protein interactions irrespective of PL type. Our findings reveal that saturated PLs shift the β-LG denaturation temperature upward by restricting molecular mobility, without preventing quaternary-level protein-protein interactions. Thermal denaturation, regardless of PL type, promoted interfacial multilayer formation at 90 °C. These results provide a mechanistic framework for tailoring emulsion stability via lipid saturation and processing temperature. KW - Small-angle X-ray scattering KW - SAXS KW - Nanostructure KW - Reference Method KW - Colloid KW - Nanoparticle PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648956 DO - https://doi.org/10.1016/j.jcis.2025.139530 SN - 0021-9797 VL - 705 SP - 1 EP - 25 PB - Elsevier Inc. AN - OPUS4-64895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ritter, B. A1 - Krahl, T. A1 - Rurack, Knut A1 - Kemnitz, E. T1 - Nanoscale CaF2 doped with Eu3+ and Tb3+ through fluorolytic sol-gel synthesis N2 - In this article, the high potential of the fluorolytic sol–gel process to synthesize nanoscopic rare earth-doped calcium fluoride sols is shown. Through a fluorolytic sol–gel process we manage to achieve spherical monodisperse ~5 nm sized nanoparticles using a simple and reproducible one-pot-wet chemical route at room temperature. The as-synthesized clear sols exhibit an intense red and green luminescence under UV excitation at room temperature. A spectroscopic study of the sols revealed the characteristic transitions 5D0 → 7FJ of Eu3+ and 5D4 → 7FJ of Tb3+, with 5D0 → 7F2 (611 nm) of Eu3+ and 5D4 → 7F4 (581 nm) of Tb3+ as the most prominent transitions. This facile synthetic strategy is also valuable for developing other luminescent nanoparticles. KW - Calciumfluorid KW - Europium KW - Lumineszenz KW - Nanopartikel KW - Sol-Gel-Synthese KW - Terbium PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-320120 DO - https://doi.org/10.1039/c4tc01073f SN - 2050-7526 SN - 2050-7534 VL - 2 IS - 40 SP - 8607 EP - 8613 PB - Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-32012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rizzardi, Q. A1 - McElfresh, C. A1 - Sparks, G. A1 - Stauffer, D. A1 - Marian, J. A1 - Maaß, Robert T1 - Mild-to-wild plastic transition is governed by athermal screw dislocation slip in bcc Nb N2 - Plastic deformation in crystals is mediated by the motion of line defects known as dislocations. For decades, dislocation activity has been treated as a homogeneous, smooth continuous process. However, it is now recognized that plasticity can be determined by longrange correlated and intermittent collective dislocation processes, known as avalanches. Here we demonstrate in body-centered cubic Nb how the long-range and scale-free dynamics at room temperature are progressively quenched out with decreasing temperature, eventually revealing intermittency with a characteristic length scale that approaches the Burgers Vector itself. Plasticity is shown to be bimodal across the studied temperature regime, with conventional thermally-activated smooth plastic flow (‘mild’) coexisting with sporadic Bursts (‘wild’) controlled by athermal screw dislocation activity, thereby violating the classical Notion of temperature-dependent screw dislocation motion at low temperatures. An abrupt increase of the athermal avalanche component is identified at the critical temperature of the material. Our results indicate that plasticity at any scale can be understood in terms of the coexistence of these mild and wild modes of deformation, which could help design better alloys by suppressing one of the two modes in desired temperature Windows. KW - Plastic deformation KW - Microplastic stress KW - Intermittent microplasticity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543927 DO - https://doi.org/10.1038/s41467-022-28477-4 VL - 13 IS - 1 SP - 1 EP - 9 PB - Nature AN - OPUS4-54392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Robens-Radermacher, Annika A1 - Held, Felix A1 - Coelho Lima, Isabela A1 - Titscher, Thomas A1 - Unger, Jörg F. T1 - Efficient identification of random fields coupling Bayesian inference and PGD reduced order model for damage localization N2 - One of the main challenges regarding our civil infrastructure is the efficient operation over their complete design lifetime while complying with standards and safety regulations. Thus, costs for maintenance or replacements must be optimized while still ensuring specified safety levels. This requires an accurate estimate of the current state as well as a prognosis for the remaining useful life. Currently, this is often done by regular manual or visual inspections within constant intervals. However, the critical sections are often not directly accessible or impossible to be instrumented at all. Model‐based approaches can be used where a digital twin of the structure is set up. For these approaches, a key challenge is the calibration and validation of the numerical model based on uncertain measurement data. The aim of this contribution is to increase the efficiency of model updating by using the advantage of model reduction (Proper Generalized Decomposition, PGD) and applying the derived method for efficient model identification of a random stiffness field of a real bridge.” KW - Model reduction KW - Model updating KW - Proper generalized decomposition KW - Random field KW - Variational Bayesian Inference PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521275 DO - https://doi.org/10.1002/pamm.202000063 VL - 20 IS - 1 SP - e202000063 PB - Wiley Online Libary AN - OPUS4-52127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Robens-Radermacher, Annika A1 - Kujath, Cezary A1 - Bos, Freek A1 - Mechtcherine, Viktor A1 - Unger, Jörg F. T1 - Mechanical properties of 3D printed concrete: a RILEM TC 304-ADC interlaboratory study-Design and implementation of a database system for querying, sharing, and analyzing experimental data N2 - Interlaboratory studies are essential for implementing standardized test methods for new innovative materials or technologies such as 3D concrete printing, certifying reference materials, and validating methods. They provide the basis for recommendations and design standards. Typically, the collected data are used only for one study and are published in paper form, without open access to the raw data files. However, preserving the collected data and analysis procedures in a shareable and reusable way leads to advantages for further usage. New data with the same structure can be added or the data can be analyzed by a new analysis procedure generating new knowledge. Additionally, resources are saved by avoiding the repetition of the same measurements. In line with the recent digitalization trend in material science and engineering, a database for the interlaboratory study on mechanical properties of 3D printed concrete conducted in RILEM Technical Committee 304-ADC is established. The challenges and experiences from defining the data structure, uploading the data, and using the database for evaluations are discussed. The openBIS software is used to create and fill the database, while an export method to an SQLite format is developed and discussed to generate a shareable and reusable database. With the exported database, querying the data is possible independently of a particular data management system. Additionally, examples of data processing with reusable workflows automating the analysis procedure are demonstrated. KW - Data management KW - Interlaboratory study KW - 3D concrete printing KW - Database KW - Reusability PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634627 DO - https://doi.org/10.1617/s11527-025-02650-9 SN - 1871-6873 VL - 58 IS - 184 SP - 1 EP - 37 PB - Springer Nature AN - OPUS4-63462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Robens-Radermacher, Annika A1 - Schmidt, Wolfram A1 - Unger, Jörg F. A1 - Mezhov, Alexander T1 - Characterization of temperature influence on the structural build-up of 3D printed concrete N2 - 3D concrete printing technologies enhance design freedom while reducing material use and costs without the need for formwork. Thereby, structural build-up is the key property governing stability and early strength evolution of 3D printed concrete after placement. Structural build-up is influenced by various factors, i.e., environmental conditions such as temperature. In this paper, the influence of ambient temperature on structural build-up was investigated through experimental and numerical approaches. Three experimental setups (small amplitude oscillatory shear, constant shear rate, and small amplitude oscillatory extensional tests) were applied to materials of increasing complexity under varying temperature conditions. A common modeling framework based on the maturity approach was developed to capture the time and temperature evolution. A stochastic framework was employed to estimate the unknown model parameters using experimental data. Experimental results demonstrate a significant temperature influence on structural build-up, consistent across all test setups and materials. The calibrated models successfully predict the structural build-up under different temperatures, confirming the applicability of the maturity approach to rheological parameters at early age. Furthermore, the stochastic parameter estimation allows a correct quantification of the uncertainties, enhancing model reliability. The comparison of two time evolution formulations indicates that a model with an additional linear stage is required for predicting the increase of the storage moduli ( $${G}{\prime}$$ G ′ , $${E}{\prime}$$ E ′ ). In conclusion, the study demonstrates that temperature significantly affects the structural build-up, and that the proposed modeling approach allows to predict this behavior. KW - Structural build-up KW - 3D concrete printing KW - Rheology KW - Temperature influence KW - Modeling KW - Green intelligent building PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654138 DO - https://doi.org/10.1617/s11527-025-02931-3 SN - 1359-5997 VL - 59 IS - 2 SP - 1 EP - 20 PB - Springer Science and Business Media LLC AN - OPUS4-65413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Robens-Radermacher, Annika A1 - Unger, Jörg F. T1 - Efficient structural reliability analysis by using a PGD model in an adaptive importance sampling schema N2 - One of the most important goals in civil engineering is to guarantee the safety of the construction. Standards prescribe a required failure probability in the order of 10−4 to 10−6. Generally, it is not possible to compute the failure probability analytically. Therefore, many approximation methods have been developed to estimate the failure probability. Nevertheless, these methods still require a large number of evaluations of the investigated structure, usually finite element (FE) simulations, making full probabilistic design studies not feasible for relevant applications. The aim of this paper is to increase the efficiency of structural reliability analysis by means of reduced order models. The developed method paves the way for using full probabilistic approaches in industrial applications. In the proposed PGD reliability analysis, the solution of the structural computation is directly obtained from evaluating the PGD solution for a specific parameter set without computing a full FE simulation. Additionally, an adaptive importance sampling scheme is used to minimize the total number of required samples. The accuracy of the failure probability depends on the accuracy of the PGD model (mainly influenced on mesh discretization and mode truncation) as well as the number of samples in the sampling algorithm. Therefore, a general iterative PGD reliability procedure is developed to automatically verify the accuracy of the computed failure probability. It is based on a goal-oriented refinement of the PGD model around the adaptively approximated design point. The methodology is applied and evaluated for 1D and 2D examples. The computational savings compared to the method based on a FE model is shown and the influence of the accuracy of the PGD model on the failure probability is studied. KW - Reliability KW - Probability of failure KW - Adaptive importance sampling KW - Reduced order models KW - Proper Generalized Decomposition PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510345 DO - https://doi.org/10.1186/s40323-020-00168-z VL - 7 SP - Article number: 29 PB - SpringerOpen AN - OPUS4-51034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockel, Daniel A1 - Sanchez Olivares, G. A1 - Calderas, F. A1 - Schartel, Bernhard T1 - Two heads are better than one: Aluminum trihydroxide / phosphorous flame retardant combination in natural waste fiber biocomposites N2 - Future polymeric materials that replace fossil fuel-based engineering plastics demand the use of renewable sources as well as the implementation of key properties such as flame retardancy, processing, and mechanical properties. This study focuses on the combination of aluminum trihydroxide (ATH) and phosphorus-based flame retardants in compositable thermoplastic starch reinforced with sustainable multifunctional leather waste fibers. The flame retardants engender different flame-retardant modes of action, improving overall performance when combined. The partial substitution of ATH with phosphorous flame retardant allowed a reduction in flame retardant loading. Materials with 90 phr of ATH reached a limiting oxygen index of 31.5 vol.-% and a UL-94 rating of V-1, whereas the combination of 73 phr ATH and 7 phr of diphenyl ocytyl phosphate achieved a V-0 rating and a slightly reduced peak of heat release rate. This study demonstrates the potential of multicomponent systems implementing waste fiber–reinforced biocomposites. KW - Biocomposites KW - Flame retardancy KW - Phosphorous flame retardants KW - Synergism KW - Sustainability PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639084 DO - https://doi.org/10.1016/j.polymertesting.2025.108938 SN - 0142-9418 SN - 1873-2348 VL - 150 SP - 1 EP - 17 PB - Elsevier Ltd. AN - OPUS4-63908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockel, Daniel A1 - Sanchez Olivares, G. A1 - Schartel, Bernhard T1 - Improving the Flame Retardancy of Aluminium Trihydroxide in Thermoplastic Starch Biocomposites Using Waste Fibers and Silicon-Based Synergists N2 - The synergistic behavior of different silicon compounds is investigated in flame retardant biocomposites with aluminum trihydroxide (ATH) as the main flame retardant. The paper shows a new approach towards sustainable biocomposites through the implementation of thermoplastic starch (TPS), leather fibers from industrial waste streams, and non-hazardous flame retardants and synergists. In these multicomponent systems, the different components address different modes of action in the fire scenario. When ATH is partially substituted by glass frits or layered silicates, fire performance is enhanced without changing the total amount of filler in the polymer. In a biocomposite with 25 phr of fiber and 90 phr of ATH, substituting 5 phr of ATH for layered silicates increased the LOI from 31.5 vol % to 34.8 vol %, decreased the peak of heat release by 20%, and increased the UL 94 rating from V-1 to V-0. KW - Biocomposites KW - Sustainability KW - Waste streams KW - Flame retardancy KW - Synergism KW - Modes of action PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605711 DO - https://doi.org/10.1021/acssusresmgt.4c00053 SN - 2837-1445 VL - 1 IS - 6 SP - 1131 EP - 1145 PB - ACS AN - OPUS4-60571 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockenhäuser, Christian A1 - Rowolt, C. A1 - Milkereit, B. A1 - Darvishi Kamachali, Reza A1 - Kessler, O. A1 - Skrotzki, Birgit T1 - On the long-term aging of S-phase in aluminum alloy 2618A N2 - The aluminum alloy 2618A is applied for engine components such as radial compressor wheels which operate for long time at elevated temperatures. This results in coarsening of the hardening precipitates and degradation in mechanical properties during the long-term operation, which is not taken into account in the current lifetime prediction models due to the lack of quantitative microstructural and mechanical data. To address this issue, a quantitative investigation on the evolution of precipitates during long-term aging at 190 °C for up to 25,000 h was conducted. Detailed transmission electron microscopy (TEM) was combined with Brinell hardness measurements and thorough differential scanning calorimetry (DSC) experiments. The results showthat GPB zones and S-phase Al2CuMg grow up to < 1,000 h during which the GPB zones dissolve and S-phase precipitates form. For longer aging times, only S-phase precipitates coarsen, which can be well described using the Lifshitz–Slyozov Wagner theory of ripening. A thorough understanding of the underlying microstructural processes is a prerequisite to enable the integration of aging behavior into the established lifetime models for components manufactured from alloy 2618A. KW - Long-term aging KW - Transmission electron microscopy (TEM) KW - Differential scanning calorimetry (DSC) KW - Microstructure KW - S-phase KW - Ostwald ripening PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519899 DO - https://doi.org/10.1007/s10853-020-05740-x SN - 0022-2461 VL - 56 IS - 14 SP - 8704 EP - 8716 PB - Springer Nature AN - OPUS4-51989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockenhäuser, Christian A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Brinell-Hardness data (HBW 2.5/62.5) of aluminum alloy EN AW-2618A after different aging times and temperatures N2 - The article covers data on the Brinell hardness of the forged precipitation-hardened aluminum alloy EN AW-2618A in the initial T61 condition (i. e. slightly underaged) and after isothermal aging for up to 25,0 0 0 h at aging temperatures between 160 °C and 350 °C. In addition, the hardness was determined on specimens after creep testing at 190 °C and various stresses. The hardness decreases with increasing ag- ing time due to the microstructural evolution of the harden- ing precipitates. The drop occurs faster the higher the aging temperature. Aging under creep load additionally accelerates the hardness decrease. KW - Aluminum alloy KW - EN AW-2618A KW - Brinell hardness KW - Aging KW - Creep KW - Ostwald ripening KW - Reheating PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567611 DO - https://doi.org/10.1016/j.dib.2022.108830 SN - 2352-3409 VL - 46 PB - Elsevier Inc. AN - OPUS4-56761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodricks, Carol Winnifred A1 - Prockat, Annabell A1 - Kalinka, Gerhard A1 - Trappe, Volker T1 - Novel Recyclable Hierarchical Carbon Fiber/Epoxy Composites: Preserving Fiber Length and Orientation Using Elium N2 - Current recycling methods for polymer matrix composites produce short, unoriented carbon fibers, limiting their use to intermediate‐strength applications. A method is therefore needed to recycle fibers while preserving their original length and orientation, enabling a circular economy for carbon fiber composites. This study proposes a novel hierarchical composite designed to retain fiber length and orientation during recycling. Virgin carbon fibers are encased in an insoluble epoxy matrix to form tapes that act as the primary units of the structure. The primary tape matrix shields the fibers from chemical degradation while preserving their alignment throughout recycling. The tapes are then embedded in a secondary recyclable matrix, Elium, a thermoplastic polymer soluble in acetone with mechanical properties comparable to epoxy. The composite is recycled by dissolving the secondary Elium matrix in acetone and recovering the primary tape units with intact fiber length and orientation. The primary units can then be used to assemble new composites. In this study, hierarchical composite laminates underwent recycling up to three times. Their mechanical properties were assessed after each cycle. Laminates with an Elium secondary matrix retained 60%–90% of the mechanical performance of epoxy‐based laminates. Minimal degradation was observed between cycles, and fiber length, orientation, and volume fraction were fully preserved. Pushout tests confirmed that fibers in the primary tapes were sufficiently shielded during the recycling process. These results validate the feasibility of a hierarchical recyclable composite that combines recyclability with high mechanical performance, serving as a proof of concept and providing opportunities for future development. KW - Review KW - Interface KW - Micromechanics KW - Polymer matrix composites KW - Glass fibre reinforced composites PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655276 DO - https://doi.org/10.1002/pc.70869 SN - 0272-8397 SP - 1 EP - 16 PB - Wiley Periodicals LLC. AN - OPUS4-65527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodriguez, Santiago A1 - Kumanski, Sylvain A1 - Ayed, Zeineb A1 - Fournet, Aurélie A1 - Bouanchaud, Charlène A1 - Sagar, Amin A1 - Allemand, Frédéric A1 - Baulin, Vladimir A. A1 - Resch‐Genger, Ute A1 - Cortés, Juan A1 - Sibille, Nathalie A1 - Chirot, Fabien A1 - Wegner, Karl David A1 - Antoine, Rodolphe A1 - Le Guével, Xavier A1 - Bernadó, Pau T1 - Programming the Optoelectronic Properties of Atomically Precise Gold Nanoclusters Using the Conformational Landscape of Intrinsically Disordered Proteins N2 - The rational design of hybrid nanomaterials with precisely controlled properties remains a central challenge in materials science. While atomically precise gold nanoclusters (Au‐NCs) offer molecule‐like control over a metallic core, tuning their optoelectronic behavior via surface engineering is often empirically driven. Here, we establish a design principle by demonstrating that the conformational landscape of intrinsically disordered proteins (IDP) can be used as a programmable scaffold to rationally modulate the photophysical properties of a covalently bound Au‐NC. We synthesized a series of bioconjugates between Au 25 nanoclusters and bioengineered IDPs containing a variable number of cysteine anchoring points. A combination of mass spectrometry, small‐angle X‐ray scattering, and modeling on the conjugates indicates that increasing the number of covalent anchors systematically restricts the conformational ensemble, inducing a progressively more compact protein shell around nanoclusters. This structural rigidification at the interface directly translates into a 15‐fold enhancement of the Au‐NC near‐infrared photoluminescence and a six‐fold increase in its average lifetime. Our findings demonstrate that the conformational plasticity of IDPs and the capacity to engineer them can be harnessed as a molecular tuning knob, moving to a new regime of programmable soft‐matter control over the properties of quantum‐confined nanomaterials for tailored biotechnological applications. KW - Fluorescence KW - Custer KW - Nano KW - Advanced material KW - Characterization KW - Fluorescence quantum yield KW - Integrating sphere spectroscopy KW - Thiol ligands KW - Gold KW - Surface chemistry KW - SWIR KW - Mass spectrometry KW - Protein PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655086 DO - https://doi.org/10.1002/chem.202502991 SN - 0947-6539 SP - 1 EP - 9 PB - Wiley VHC-Verlag AN - OPUS4-65508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodríguez-Sánchez, Noelia A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska A1 - Prinz, Carsten A1 - Prieto-Laria, P. A1 - Ruiz-Salvador, A.R. A1 - Ballesteros, M. T1 - Engineering a multivariate cobalt metal–organic framework for high photocatalytic activity: the impact of mixed ligands and metal incorporation in a visible light-driven heterogeneous photo-Fenton reaction for water treatment N2 - Metal–organic frameworks (MOFs) have attracted increasing attention for the removal of organic pollutants in wastewater via photocatalysis. Here, we design a multivariate modification of ZIF-9 to tune its electronic properties for use in visible light photocatalysis. A controllable synthesis of ZIF-9 and its multivariate forms with the incorporation of copper and the 2-imidazolecarboxaldehyde (ica) ligand was carried out. The materials are tested for the removal of the model dye methylene blue (MB) by a heterogeneous photo-Fenton-like reaction at neutral pH and room temperature. Cu-ZIF-9-ica (UPO-3) shows high photocatalytic activity under both visible and ultraviolet A (UVA) light, achieving 94% MB degradation in 45 min, compared to 65% MB degradation in 120 min using bare ZIF-9. The study revealed a first-order rate constant of 0.0475 min−1 for Cu-ZIF-9-ica compared to 0.0088 min−1 for ZIF-9 under visible light. The improvement of the catalyst was clearly attributed to the co-incorporation of Cu and the ica ligand in the MOF, which reduces the band gap, in agreement with DFT calculations. Reproducibility and recyclability tests proved that Cu-ZIF-9-ica can be used for at least 3 cycles without a significant loss of efficiency, making it a promising material for the study and application of wastewater treatment. KW - Metal-Organic Framework (MOF) KW - Heterogeneous photo-Fenton KW - ZIF-9 KW - Methylene Blue PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630797 DO - https://doi.org/10.1039/d4na00954a SN - 2516-0230 VL - 7 IS - 8 SP - 2255 EP - 2265 PB - Royal Society of Chemistry AN - OPUS4-63079 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodríguez-Sánchez, Noelia A1 - Domínguez-Santos, J. Enrique A1 - Bhattacharya, Biswajit A1 - Prinz, Carsten A1 - Canosa, Inés A1 - Flores, Amando A1 - Jiménez-Rodríguez, Antonia A1 - Ruiz-Salvador, A. Rabdel A1 - Emmerling, Franziska A1 - Ballesteros, Menta T1 - Mechanochemical synthesis of multivariate UPO-3 (Cu-ZIF-9-ica) MOF for inactivation of antibiotic-resistant bacteria and irrigation-quality water production via heterogeneous photo-Fenton catalysis N2 - Water scarcity and pollution are critical global challenges, particularly in agriculture, the largest consumer of water. The development of sustainable, effective, and environmentally friendly disinfection methods is essential to address the risks posed by antibiotic-resistant bacteria and to ensure safe reuse of water for irrigation. In this study, we report the synthesis of the metal-organic framework (MOF) Universidad Pablo de Olavide-3 (UPO-3) via a mechanochemical approach, a scalable and sustainable method compared to traditional solvothermal synthesis. The resulting UPO-3/H2O2 system exhibits robust photocatalytic properties under visible light, achieving effective and broad-spectrum antibacterial activity. The disinfection efficiency of the catalyst was evaluated against Escherichia coli as a model of microbial pathogen in two saline matrices, considering the key parameters of the heterogeneous photo-Fenton process, including catalyst dosage, initial H2O2 concentration, and light irradiation. Notably, it inactivated two important virulent and antibiotic-resistant bacterial pathogens (Staphylococcus aureus and Pseudomonas aeruginosa). Furthermore, UPO-3 shows exceptional performance under real-world conditions, such as river water disinfection, achieving >5-log reduction of E. coli, fulfilling a critical criterion for Class A water reuse under Regulation (EU) 2020/741. These results highlight UPO-3 as a versatile and sustainable solution for water reuse, addressing water scarcity and advancing efforts to achieve United Nations Sustainable Development Goal 6. KW - Water reuse KW - Antibiotic-resistant bacteria KW - Water disinfection KW - Mechanochemical synthesis KW - Metal organic framework PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639766 DO - https://doi.org/10.1016/j.chemosphere.2025.144610 SN - 0045-6535 VL - 386 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-63976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodríguez-Sánchez, Noelia A1 - Prinz, Carsten A1 - Bienert, Ralf A1 - Ballesteros, Menta A1 - Ruiz Salvador, A. Rabdel A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska T1 - Mechanochemical ZIF-9 formation: in situ analysis and photocatalytic enhancement evaluation N2 - Efficient treatment of persistent pollutants in wastewater is crucial for sustainable water management and environmental protection. This study addresses this challenge by investigating the mechanochemical synthesis and photocatalytic performance of ZIF-9, a cobalt-based zeolitic imidazolate framework. Using synchrotron-based powder X-ray diffraction, we provide real-time insights into the formation dynamics of ZIF-9 during mechanosynthesis. Our results show that mechanochemically synthesised ZIF-9 exhibits superior photocatalytic activity compared to its solvothermally prepared counterpart, achieving a 2-fold increase in methylene blue degradation rate. This research not only advances our understanding of the synthesis and properties of ZIF-9, but also demonstrates the potential of mechanochemical approaches in the development of high-performance, sustainably produced materials for water treatment and other environmental applications. KW - MOFs KW - ZIF KW - Time-resolved in situ investigation KW - Photocatalysis synchrotron X-ray powder diffraction PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641416 DO - https://doi.org/10.1039/D4MR00114A SN - 2976-8683 VL - 2 IS - 1 SP - 116 EP - 126 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-64141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roebben, G. A1 - Kestens, V. A1 - Varga, Z. A1 - Charoud-Got, J. A1 - Ramaye, Y. A1 - Gollwitzer, Christian A1 - Bartczak, D. A1 - Geißler, Daniel A1 - Noble, J.E. A1 - Mazoua, S. A1 - Meeus, N. A1 - Corbisier, P. A1 - Palmai, M. A1 - Mihály, J. A1 - Krumrey, M. A1 - Davies, J. A1 - Resch-Genger, Ute A1 - Kumarswami, N. A1 - Minelli, C. A1 - Sikora, A. A1 - Goenaga-Infante, H. T1 - Reference materials and representative test materials to develop nanoparticle characterization methods: the NanoChOp project case N2 - This paper describes the production and characteristics of the nanoparticle test materials prepared for common use in the collaborative research project NanoChOp (Chemical and optical characterization of nanomaterials in biological systems), in casu suspensions of silica nanoparticles and CdSe/CdS/ZnS quantum dots (QDs). This paper is the first to illustrate how to assess whether nanoparticle test materials meet the requirements of a "reference material" (ISO Guide 30, 2015) or rather those of the recently defined category of "representative test material (RTM)" (ISO/TS 16195, 2013). The NanoChOp test materials were investigated with small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), and centrifugal liquid sedimentation (CLS) to establish whether they complied with the required monomodal particle size distribution. The presence of impurities, aggregates, agglomerates, and viable microorganisms in the suspensions was investigated with DLS, CLS, optical and electron microscopy and via plating on nutrient agar. Suitability of surface functionalization was investigated with attenuated total reflection Fourier transform infrared spectrometry (ATR-FTIR) and via the capacity of the nanoparticles to be fluorescently labeled or to bind antibodies. Between-unit homogeneity and stability were investigated in terms of particle size and zeta potential. This paper shows that only based on the outcome of a detailed characterization process one can raise the status of a test material to RTM or reference material, and how this status depends on its intended use. KW - Nanoparticle KW - Materials characterization KW - Reference material KW - Analytical quality assurance KW - Metrology PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-349644 DO - https://doi.org/10.3389/fchem.2015.00056 SN - 2296-2646 VL - 3 SP - Article 56, 1 EP - 16 PB - Frontiers Media CY - Lausanne AN - OPUS4-34964 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 (C8 (e.g. 580 µg/kg dw PFOS for Soil1), whereas the consumer product samples showed a more uniform distribution with regard to chain lengths from C4 to C8. Independent from quantified PFAS amounts via target analysis, µ-XRF mapping combined with µ-XANES spectroscopy was successfully applied to detect both point-specific concentration maxima and evenly distributed surface coatings of fluorinated organic contaminants in the corresponding samples. KW - PFAS KW - XRF KW - LC-MS/MS KW - XANES KW - Fluoride KW - Soil PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576109 DO - https://doi.org/10.1039/D3EM00107E SN - 2050-7887 SP - 1 EP - 12 PB - Royal Society of Chemistry AN - OPUS4-57610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Romero-Navarrete, José A. A1 - Otremba, Frank T1 - A method to assess the gravity response efficiency of a truck N2 - In spite that transport activities do not represent the biggest contributor of pollutants emissions, their reduction has been a priority as some other externalities are associated to such emissions and to the transport itself. A crucial element to characterize the behavior of the vehicles against the environment are the losses that such vehicles exhibit in a passive way, that is, without any involvement of power conditions. The energy loses due to the rolling, the drag and to the friction in mechanical components, have been assessed so far in terms of the stopping acceleration when the vehicle idles on a ramp. However, such a testing procedure produces some uncertainties due to the dynamic conditions that are considered. To avoid such critical limitations, in this paper a testing procedure and facility are proposed, which are based on static conditions of the vehicle at the initiation and at the ending of the test, which are assumed to provide a better reliability to the testing. Some preliminary theoretical analysis should be made in order to validate the operational principles proposed herein for such testing facility. KW - Road tankers KW - Energy efficiency KW - Environmental assessment KW - Gravity response KW - Transportation energy KW - Rolling resistance KW - Drag resistance PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511530 UR - https://www.iaras.org/iaras/home/caijes/a-method-to-assess-the-gravity-response-efficiency-of-a-truck SN - 2367-8941 VL - 5 SP - 213 EP - 219 PB - IARAS CY - Sofia AN - OPUS4-51153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Romero-Navarrete, José A. A1 - Otremba, Frank A1 - Lozano Guzman, A. A. T1 - Estimation of the effect of the driving style on pollutants emission by heavy trucks N2 - Different approaches have been attempted so far to reduce fuel consumption and linked pollutants, including vehicle equipment and design, with rational driving style being recognized as a potential source of fuel savings. However, no specific methodology had been suggested so far to assess fuel economy of driving other than the fuel consumed itself. In this paper, the Standard deviation of driving acceleration has been found to be directly associated to fuel consumption, so that the less dispersion of the driving acceleration, produces the lower fuel consumptions and emissions. Such metric could be thus used to assess driving style. KW - Driving style KW - Fuel consumption KW - Stored energy KW - GPS data KW - Simulation KW - Particle emissions PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511540 UR - https://www.iaras.org/iaras/home/caijes/estimation-of-the-effect-of-the-driving-style-on-pollutants-emission-by-heavy-trucks SN - 2367-8941 VL - 5 SP - 220 EP - 226 PB - IARAS CY - Sofia AN - OPUS4-51154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosemann, Paul A1 - Müller, C. A1 - Baumann, O. A1 - Modersohn, W. A1 - Halle, T. T1 - Influence of the post-weld surface treatment on the corrosion resistance of the duplex stainless steel 1.4062 N2 - The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polished or blasting depending on the application and the requested corrosion resistance. Blasted surfaces are often used in industrial practice due to the easier and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the different performed corrosion tests (potential measurement, KorroPad-test and pitting potential) on welding seams with different surface treatments. T2 - 19th Chemnitz Seminar on Materials Engineering – 19. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 16.03.2017 KW - Corrosion resistance KW - Welding KW - Duplex stainless steels KW - Pitting corrosion KW - Surface treatment PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395374 DO - https://doi.org/10.1088/1757-899X/181/1/012019 SN - 1757-899X SN - 1757-8981 VL - 181 IS - Conference 1 SP - Article UNSP 012019, 1 EP - 9 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-39537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosemann, Paul A1 - Müller, Christina A1 - Meyer, A. A1 - Halle, T. T1 - Influence of nitrogen on the corrosion resistance of martensitic stainless steels N2 - The corrosion resistance of martensitic stainless steels (MSS) depends strongly on the chemical composition and the applied heat treatment. Both determines the distribution of the alloying elements in the microstructure and the resulting material properties. The addition of nitrogen is known to be beneficial for the pitting corrosion resistance of stainless steels. In case of MSS this effect is not only connected to nitrogen itself because nitrogen can be used to substitute carbon which also influences the result of the heat treatment process. This paper shows the effect of nitrogen on the corrosion resistance in relation to the hardening process of MSS. Therefore the effects of austenitization duration, austenitization temperature and cooling rate on microstructure, hardness and corrosion resistance were studied on the MSS X30CrMoN15 1 and X50CrMoV15. The effect of different cooling rates was studied in the range of > 100 K/s down to 1 K/s using the jominy end quench test. The changes in corrosion resistance were detected with electrochemical potentiodynamic reactivation (EPR) and by the determination of critical pitting potentials. Besides this experimental approach thermodynamic calculations with the software thermocalc will be presented and used for the interpretation of the effect of nitrogen on the corrosion resistance of MSS. T2 - 18th Chemnitz Seminar on Materials Engineering – 18. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany KW - Martensitic stainless steels KW - Corrosion resistance KW - Heat treatment PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366956 DO - https://doi.org/10.1088/1757-899X/118/1/011002 VL - 118 IS - 1 SP - 19 EP - 19 PB - IOP Publishing AN - OPUS4-36695 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 - Rosenbusch, Ivo A1 - Arai, Marylyn Setsuko A1 - Rizzo, Fabio A1 - de Camargo, Andrea S. S. A1 - Ravoo, Bart Jan T1 - A host–guest approach to ratiometric pH sensing using upconversion nanoparticles N2 - A new pH nanosensor based on β-NaYF4:Yb3+/Tm3+ upconversion nanoparticles functionalized with cyclodextrin and a pH-sensitive adamantane-modified nitrobenzoxadiazole dye (NBD-Ad). KW - Host-guest materials KW - Upconversion nanoparticles KW - Ratiometric optical sensors KW - pH sensing PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637722 DO - https://doi.org/10.1039/d5na00145e SN - 2516-0230 VL - 7 IS - 13 SP - 4142 EP - 4151 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenbusch, Sjard Mathis A1 - Balzani, D. A1 - Unger, Jörg F. T1 - Regularization of softening plasticity models for explicit dynamics using a gradient-enhanced modified Johnson–Holmquist model N2 - The behavior of concrete under high strain rates is often described by plasticity models with softening, which is modeled by a reduction of the yield surface as a function of the local equivalent plastic strain. Many of these models are local and therefore produce mesh-dependent results. In this contribution, the gradient-enhancement of such models is investigated to mitigate the mesh-dependency. First, the mesh-dependency of these local formulations based on the analysis with a modified JH2 model as a representative for these constitutive formulations is demonstrated using a one-dimensional benchmark example. In the benchmark, the width of the damaged zone decreases upon mesh-refinement and the dissipated plastic energy tends to zero. It is further shown that a significantly small safety factor for the critical time step is needed in order to achieve accurate results for the benchmark example. The first investigated gradient-enhancement approach replaces the equivalent local plastic strain with its nonlocal counterpart. The enhancement is based on the inclusion of inertia and damping to the additional Helmholtz equation which enables the use of the central difference method as an explicit solver. This method successfully distributes the damage over several elements, however, the local equivalent plastic strain still localizes into one cell. The inclusion of hardening with respect to the local equivalent plastic strain inhibits the localization and the dissipated plastic energy converges with mesh-refinement. This is further confirmed in a two-dimensional wedge-splitting experiment and a four-point bending test where the damage pattern produced by the local model is mesh-dependent as well and the dissipated plastic energy tends to zero with mesh-refinement. The proposed nonlocal model with hardening results in a consistent damage pattern and the dissipated plastic energy converges. Furthermore, the nonlocal model with hardening is less sensitive to time step refinement, such that computational efficiency can be improved compared to the local model. The numerical experiments are implemented using the free open source tool FEniCSx and have been made available on Zenodo. KW - Gradient plasticity KW - Explicit dynamics KW - JH2 model KW - Concrete modeling KW - FEniCS KW - Mesh convergence KW - Time step convergence PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630453 DO - https://doi.org/10.1016/j.ijimpeng.2024.105209 SN - 1879-3509 VL - 198 SP - 1 EP - 18 PB - Elsevier Ltd. CY - Schweiz AN - OPUS4-63045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenbusch, Sjard Mathis A1 - Diercks, Philipp A1 - Kindrachuk, Vitaliy A1 - Unger, Jörg F. T1 - Integrating custom constitutive models into FEniCSx: A versatile approach and case studies N2 - The development and integration of user-defined constitutive relationships into finite element (FE) tools using standardized interfaces play a pivotal role in advancing the capabilities of FE solvers for structural mechanics applications. While commercial FE solvers like Abaqus and Ansys have designed their interfaces to provide custom stresses, tangents, and updated history variables, the open-source solver FEniCSx remains efficient only when the constitutive update has an analytical representation. This restricts the application of FEniCSx for non-linear structural mechanics. Since FEniCSx has become a powerful and popular open-source tool for solving partial differential equations, particularly due to its automatic computation of Hessians, we aim to develop a generalized interface to enhance its capability for constitutive modeling. This approach will address complex constitutive equations that require iterative solutions at the quadrature point level. Specific implementation challenges, such as using return-mapping procedures, can then be managed commonly. The provided interface for custom constitutive models offers a versatile way to implement them in various languages, including C++, Python, Rust, and Fortran. Finally, with UMATs for viscoplastic models as an example, we demonstrate how existing user subroutines can be incorporated into the interface and utilized within the FEniCSx framework. KW - Finite element method KW - Constitutive models KW - FEniCSx KW - UMAT KW - Rust KW - Python KW - C++ PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630439 DO - https://doi.org/10.1016/j.advengsoft.2025.103922 SN - 0965-9978 VL - 206 SP - 1 EP - 11 PB - Elsevier CY - Amsterdam AN - OPUS4-63043 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenkranz, D. A1 - Kriegel, F. L. A1 - Mavrakis, E. A1 - Pergantis, S. A. A1 - Reichardt, P. A1 - Tentschert, J. A1 - Jakubowski, N. A1 - Laux, P. A1 - Panne, Ulrich A1 - Luch, A. T1 - Versatile dual-inlet sample introduction system for multi-mode single particle inductively coupled plasma mass spectrometry N2 - Metal-containing nanoparticles (NP) can be characterized with inductively coupled plasma mass spectrometers (ICP-MS) in terms of their size and number concentration by using the single-particle mode of the instrument (spICP-MS). The accuracy of measurement depends on the setup, operational conditions of the instrument and specific parameters that are set by the user. The transport efficiency of the ICP-MS is crucial for the quantification of the NP and usually requires a reference material with homogenous size distribution and a known particle number concentration. Currently, NP reference materials are available for only a few metals and in limited sizes. If particles are characterized without a reference standard, the results of both size and particle number may be biased. Therefore, a dual-inlet Setup for characterizing nanoparticles with spICP-MS was developed to overcome this problem. This setup is based on a conventional introduction system consisting of a pneumatic nebulizer (PN) for nanoparticle solutions and a microdroplet Generator (μDG) for ionic calibration solutions. A new and flexible interface was developed to facilitate the coupling of μDG, PN and the ICP-MS system. The interface consists of available laboratory components and allows for the calibration, nanoparticle (NP) characterization and cleaning of the arrangement, while the ICP-MS instrument is still running. Three independent analysis modes are available for determining particle size and number concentration. Each mode is based on a different calibration principle. While mode I (counting) and mode III (μDG) are known from the literature, mode II (sensitivity), is used to determine the transport efficiency by inorganic ionic Standard solutions only. It is independent of NP reference materials. The μDG based inlet system described here guarantees superior analyte sensitivities and, therefore, lower detection limits (LOD). The size dependent LODs achieved are less than 15 nm for all NP (Au, Ag, CeO2) investigated. KW - Spectrometer KW - Reference KW - Calibration PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536121 DO - https://doi.org/10.3791/61653 SN - 1940-087X IS - 163 SP - 1 EP - 19 PB - MyJoVE Corporation CY - Cambridge, MA, USA AN - OPUS4-53612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rossi, Andrea A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Development of a one-pot synthesis of rGO in water by optimizing Tour’s method parameters N2 - Since its first synthesis in 2004, graphene has been widely studied and several different synthesis methods has been developed. Solvent exfoliation of graphite and the reduction of graphene oxide previously obtained through graphite oxidation are the most employed. In this work, we exploited synthesis conditions of a method usually employed for obtaining graphene oxide (the Tour’s method) for directly obtaining a very poorly oxidised material with characteristics like reduced graphene oxide. For the first time, a one-pot synthesis of reduced graphene oxide (rGO) is reported avoiding the use of a post-synthesis chemical or thermal reduction of the graphene oxide that requires further reagents, heat and time. KW - Graphene KW - 2D-materials KW - Tour's method KW - rGO KW - One-pot synthesis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611827 DO - https://doi.org/10.1038/s41598-024-73606-2 SN - 2045-2322 VL - 14 SP - 1 EP - 10 PB - Springer Nature CY - London AN - OPUS4-61182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rossi, Andrea A1 - Corrao, Elena A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Yasamin, Nakhli A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Multivariate optimization and characterization of graphene oxide via design of experiments and chemometric analysis N2 - Controlling the structure and properties of graphene oxide (GO) remains a challenge due to the poor reproducibility of conventional synthetic protocols and limited understanding of parameter-property relationships. In this study, we present an integrated analytical framework that combines Design of Experiments (DoE) with chemometric modelling to systematically assess the effects of eight synthesis variables on GO’s physicochemical and functional features. A Plackett–Burman experimental design enabled efficient screening of synthesis conditions, while comprehensive characterization (spanning UV–Vis spectroscopy, XPS, SEM–EDX, TEM–EDX, and XRD) was coupled with multivariate tools (Principal Component Analysis and Multiple Linear Regression) to identify statistically significant correlations between synthetic inputs and material responses. Notably, we demonstrate that UV–Vis spectra can serve as a robust proxy for oxidation state, offering a rapid and accessible alternative to surface-sensitive methods. The approach yields a predictive analytical toolkit for guiding GO synthesis and highlights a generalizable strategy for the rational design of flat nanomaterials. This work supports reproducible, resource-efficient material development aligned with Safe and Sustainable by Design (SSbD) principles. KW - Graphene oxide KW - 2D-materials KW - Design of Experiment KW - Synthesis KW - Chemometric analysis PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652576 DO - https://doi.org/10.1016/j.flatc.2025.100988 SN - 2452-2627 VL - 55 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-65257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roters, F. A1 - Aslam, A. A1 - Bai, Y. A1 - Büschelberger, M. A1 - Bulert, K. A1 - Butz, A. A1 - Hickel, Tilmann A1 - Jogi, T. A1 - Klitschke, S. A1 - Martin, M. A1 - Meyer, L.-P. A1 - Morand, L. A1 - Nahshon, Y. A1 - Radtke, N. A1 - Saikia, Ujjal A1 - Trondl, A. A1 - Wessel, A. A1 - Zierep, P. A1 - Helm, D. T1 - StahlDigital: Ontology-Based Workflows for the Steel Industry N2 - The innovative strength of the steel industry is based on the mastery of microstructure–property relationships. Digital workflows can largely contribute to this aim by making the complexity of workflows reproducible and their execution user independent. In this work, the tools and workflows developed in the project StahlDigital as part of the German MaterialDigital initiative are presented and application examples are provided. A steel ontology builds the foundation for data collection and storage as well as for the semantic description of experimental and simulation data processing workflows. A dataspace powered by the Dataspace Management System (DSMS) digitally represents such workflows and manages data along them in a Findable, Accessible, Interoperable, Reusable manner aiming to derive new knowledge. Experimental data processed via DSMS can be further evaluated and used as input for simulation workflows. The simulations included in such workflows are run by the workflow system pyiron, which has been semantically extended in StahlDigital for this purpose. KW - Steel KW - Rolling KW - Multiscale simulation KW - Ontology KW - Workflow PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627187 DO - https://doi.org/10.1002/adem.202402148 SN - 1527-2648 SP - 1 EP - 13 PB - Wiley VHC-Verlag AN - OPUS4-62718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rothbart, Nick A1 - Maierhofer, Christiane A1 - Goldammer, M. A1 - Hohlstein, F. A1 - Koch, J. A1 - Kryukov, I. A1 - Mahler, G. A1 - Stotter, B. A1 - Oswald-Tranta, B. A1 - Sengebusch, M. T1 - A round robin test of flash thermography of CFRP and metal structures N2 - Within the scope of a DIN INS project, a flash thermography round robin test that evaluates reliability, comparability and efficiency of different testing situations is organized. The results give information about the detectability of defects e.g. by their size and depth, the evaluation method and by the materials used. Besides, the influence of equipment and parameters used by the participants on the results were analysed. All of the quantitative results as well as the feedback given by the participants will be presented in a DIN committee in order to contribute to a flash thermography standard. T2 - 7th International Symposium on NDT in Aerospace CY - Bremen, Germany DA - 16.11.2015 KW - Flash thermography KW - Round robin test KW - Metal KW - Flat bottom holes KW - SNR PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351070 UR - https://www.ndt.net/?id=18921 SN - 1435-4934 VL - 21 IS - 4 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-35107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roveda, Ilaria A1 - Mishurova, Tatiana A1 - Evans, Alexander A1 - Fitch, Andrew N. A1 - Haubrich, Jan A1 - Requena, Guillermo A1 - Bruno, Giovanni A1 - Serrano-Munoz, Itziar T1 - Evolution of interphase stress over a crack propagation plane as a function of stress relief heat treatments in a PBF‐LB/M AlSi10Mg alloy N2 - AbstractIn this study, we compare the residual stress state in a laser powder bed fusion (PBF‐LB/M) AlSi10Mg alloy in the as‐built (AB) condition with that after two different heat treatments (265 °C for 1 h, HT1; and 300 °C for 2 h, HT2). The bulk residual stress (RS) is determined using synchrotron X‐ray diffraction (SXRD), and near‐surface profiles are determined using laboratory energy‐dispersive X‐ray diffraction (EDXRD). The EDXRD results do not reveal any notable difference between the conditions at a depth of 350 μm, suggesting that the machining process yields a comparable residual stress state in the near‐surface regions. On the other hand, the SXRD results show that HT1 is more effective in relieving the bulk RS. It is observed that HT1 reduces the RS state in both the aluminium matrix and the silicon network. In addtion, HT2 does not have a significant impact on relaxing the RS as‐built state of the matrix, although it does induce a reduction in the RS magnitudes of the Si phase. It is concluded that the heat treatment stress relieving is effective as long as the Si‐network is not disaggregated. KW - Interphase residual stress KW - Laboratory energy-dispersive X-ray diffraction (EDXRD) KW - PBFLB/M AlSi10Mg alloy KW - Stress-relief heat-treatments KW - Synchrotron X-ray diffraction (SXRD) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597591 DO - https://doi.org/10.1111/str.12475 VL - 60 IS - 6 SP - 1 EP - 13 PB - John Wiley & Sons Ltd. AN - OPUS4-59759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roveda, Ilaria A1 - Serrano-Munoz, Itziar A1 - Haubrich, Jan A1 - Requena, Guillermo A1 - Madia, Mauro T1 - Investigation on the fatigue strength of AlSi10Mg fabricated by PBF-LB/M and subjected to low temperature heat treatments N2 - This work provides an investigation of the influence of low temperature heat treatments on the fatigue behavior of a PBF-LB AlSi10Mg alloy. Fatigue specimens are produced in form of round bars on a build platform preheated at 200 ◦C. The specimens have been tested in three different conditions: as-built, and after heat treatments at 265 ◦C for 1 h and 300 ◦C for 2 h. Prior to the fatigue testing, the defect distribution is analyzed by means of micro computed tomography. Subsequently, the peak over threshold method is successfully applied to provide a prediction of the size of killer defect. The defect population was of gas porosity type. No clear improvement of the fatigue performance is observed after the heat treatments. The fatigue strength predicted using fracture mechanics-based approaches is in good agreement with the experimental data. Among the studied approaches, short crack models provided the most conservative predictions. KW - PBF-LB/M AlSi10Mg KW - Fatigue strength KW - Defects KW - Kitagawa-Takahashi Diagram KW - Short Crack Models PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607071 DO - https://doi.org/10.1016/j.matdes.2024.113170 SN - 0264-1275 VL - 244 SP - 1 EP - 12 PB - Elsevier Ltd. AN - OPUS4-60707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roveda, Ilaria A1 - Serrano-Munoz, Itziar A1 - Kromm, Arne A1 - Madia, Mauro T1 - Investigation of residual stresses and microstructure effects on the fatigue behaviour of a L-PBF AlSi10Mg alloy N2 - Al-Si alloys produced by Laser Powder Bed Fusion (L-PBF) techniques allow the fabrication of lightweight free-shape components that find space in aerospace, automotive, biomedical and military applications. Due to the high cooling rates occurring during the building process, L-PBF AlSi10Mg alloys exhibit an ultra-fine microstructure that leads to superior mechanical properties in the as-built condition compared to conventional cast Al-Si materials. Nevertheless, L-PBF processing induces high thermal gradients, leading to deleterious residual stress levels that must be considered to avoid part distortion and unpredicted failures. In order to relax detrimental residual stress and to increase the ductility, post-processing stress relief treatments are generally performed. In as-built condition the hypoeutectic AlSi10Mg microstructure consist of fine α-Al cells containing uniformly dispersed silicon nanoparticles, which are, in addition, surrounded by a eutectic Si network. Above 260°C the silicon interconnectivity starts to breakdown into spheroidized particles and to coarsen. At the same time, the heating residual stresses are relieved. The objective of the contribution is to investigate, under different heat treatment conditions, the evolution of microstructure and residual stresses in view of optimizing the fatigue performance of the alloy. To this purpose various heat treatments in a range of temperatures between 265°C and 300°C for a duration between 15 minutes and 2 hours are performed. The microstructure modifications are analysed using a scanning electron microscope and the residual stress state is measured by laboratory X-ray diffraction. T2 - FATIGUE DESIGN 2021 CY - Online meeting DA - 17.11.2021 KW - AlSi10Mg alloy KW - Additive manufacturing KW - L-PBF KW - Residual stress KW - Heat treatment PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544942 DO - https://doi.org/10.1016/j.prostr.2022.03.057 SN - 2452-3216 VL - 38 SP - 564 EP - 571 PB - Elsevier B.V. AN - OPUS4-54494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roveda, Ilaria A1 - Serrano-Munoz, Itziar A1 - Mishurova, Tatiana A1 - Madia, Mauro A1 - Pirling, T. A1 - Evans, Alexander A1 - Klaus, M. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Influence of a 265 °C heat treatment on the residual stress state of a PBF-LB/M AlSi10Mg alloy N2 - Laser Powder Bed Fusion (PBF-LB/M) additive manufacturing (AM) induces high magnitude residual stress (RS) in structures due to the extremely heterogeneous cooling and heating rates. As the RS can be deleterious to the fatigue resistance of engineering components, great efforts are focused on understanding their generation and evolution after post-process heat treatments. In this study, one of the few of its kind, the RS relaxation induced in an as-built PBF-LB/M AlSi10Mg material by a low-temperature heat treatment (265 °C for 1 h) is studied by means of X-ray and neutron diffraction. Since the specimens are manufactured using a baseplate heated up to 200 °C, low RS are found in the as-built condition. After heat treatment a redistribution of the RS is observed, while their magnitude remains constant. It is proposed that the redistribution is induced by a repartition of stresses between the a-aluminium matrix and the silicon phase, as the morphology of the silicon phase is affected by the heat treatment. A considerable scatter is observed in the neutron diffraction RS profiles, which is principally correlated to the presence (or absence) of pockets of porosity developed at the borders of the chessboard pattern. KW - Neutron diffraction KW - Additive manufacturing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565115 DO - https://doi.org/10.1007/s10853-022-07997-w SN - 1573-4803 VL - 57 SP - 22082 EP - 22098 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-56511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rua-Ibarz, Ana A1 - Nakadi, Flávio V. A1 - Bolea-Fernandez, Eduardo A1 - Bazo, Antonio A1 - Battistella, Beatrice A1 - Matiushkina, Anna A1 - Resch-Genger, Ute A1 - Abad Andrade, Carlos Enrique A1 - Resano, Martín T1 - Discrete entity analysis via microwave-induced nitrogen plasma–mass spectrometry in single-event mode N2 - In this work, single-event microwave-induced nitrogen plasma–mass spectrometry (single-event MINP-MS) was evaluated for the first time for the analysis of discrete entities such as nanoparticles, biological cells, and microplastics. Nitrogen (N2) effectively overcomes Ar-based polyatomic interferences, enabling (ultra)trace element determination of Fe and Se using their most abundant isotopes, 56Fe (91.66%) and 80Se (49.82%). Iron oxide nanoparticles (Fe2O3 NPs) ranging from 20 to 70 nm were accurately characterized, with excellent agreement with established sizing techniques, such as transmission electron microscopy (TEM) and dynamic light scattering (DLS). A limit of detection (LoD) of 8.6 ag for Fe─equivalent to an LoDsize of 19 nm for Fe2O3─was achieved, which is significantly lower than recent values reported for high-end quadrupole-based ICP-MS. Selenium nanoparticles (SeNPs) of 150 and 250 nm were also accurately characterized, without the N2-based plasma experiencing issues handling relatively large metallic NPs (linearity, R2 = 0.9994). Se-enriched yeast cells (SELM-1 certified reference material) were successfully analyzed via single-cell MINP-MS using external calibration based on SeNPs and a transport efficiency-independent approach. In addition, 2–3 μm polystyrene (PS) and polytetrafluoroethylene (PTFE) were accurately sized by monitoring 12C+, confirming the method’s suitability for handling micrometer-sized polymeric materials (microplastics). The average duration of individual events (680 ± 160 μs) suggests that the digestion of individual entities in N2-based plasmas is comparable to that in Ar-based plasmas. These results open new avenues for this instrumentation as an alternative to ICP ionization sources, also in the context of discrete entity analysis. KW - Microwave-Induced Nitrogen Plasma KW - Discrete entity analysis KW - Particle/droplet event counting KW - Comparison to SP-ICP-MS methodologies KW - Nitrogen plasma vs. argon ICP trade-offs KW - Trace elemental quantification at the single-entity level KW - Time-resolved mass spectrometry for discrete entities PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643825 DO - https://doi.org/10.1021/acs.analchem.5c04341 SN - 0003-2700 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-64382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudenko, A. A1 - Colombier, J.-P. A1 - Höhm, S. A1 - Rosenfeld, A. A1 - Krüger, Jörg A1 - Bonse, Jörn A1 - Itina, T.E. T1 - Spontaneous periodic ordering on the surface and in the bulk of dielectrics irradiated by ultrafast laser: a shared electromagnetic origin N2 - Periodic self-organization of matter beyond the diffraction limit is a puzzling phenomenon, typical both for surface and bulk ultrashort laser processing. Here we compare the mechanisms of periodic nanostructure formation on the surface and in the bulk of fused silica. We show that volume nanogratings and surface nanoripples having subwavelength periodicity and oriented perpendicular to the laser polarization share the same electromagnetic origin. The nanostructure orientation is defined by the near-field local enhancement in the vicinity of the inhomogeneous scattering centers. The periodicity is attributed to the coherent superposition of the waves scattered at inhomogeneities. Numerical calculations also support the multipulse accumulation nature of nanogratings formation on the surface and inside fused silica. Laser surface processing by multiple laser pulses promotes the transition from the high spatial frequency perpendicularly oriented nanoripples to the low spatial frequency ripples, parallel or perpendicular to the laser polarization. The latter structures also share the electromagnetic origin, but are related to the incident field interference with the scattered far-field of rough non-metallic or transiently metallic surfaces. The characteristic ripple appearances are predicted by combined electromagnetic and thermo-mechanical approaches and supported by SEM images of the final surface morphology and by time-resolved pump-probe diffraction measurements. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser KW - Nanostructures KW - Dielectrics KW - Electromagnetic scattering PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-421747 UR - https://www.nature.com/articles/s41598-017-12502-4 DO - https://doi.org/10.1038/s41598-017-12502-4 SN - 2045-2322 VL - 7 SP - Article 12306, 1 EP - 14 PB - Springer Nature AN - OPUS4-42174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudić, O. A1 - Mittermayr, F. A1 - Gluth, Gregor A1 - Simon, Sebastian A1 - Ukrainczyk, N. A1 - Seyrek, Y. A1 - Freytag, B. A1 - Juhart, J. A1 - Grengg, C. T1 - On the benefits of vegetable oil addition for the pore structure and acid resistance of alkali-activated systems N2 - The impact of high additions of vegetable oil (12 vol%) on the mechanical and microstructural properties of metakaolin-slag-based alkali-activated materials (AAMs) was studied. The addition of oil resulted in a slight decrease in initial polymerization kinetics but did not affect the final degree of reaction. AAM-oil-composite-mortars exhibited approximately ∼30% lower compressive strength primarily due to the entrainment of air voids. Newly formed soap phases significantly reduced the volume of small capillary and gel pores (pore radii <15 nm), leading to a decrease in specific inner surface area by a factor of up to 15. The porosity modification induced by the oil addition greatly enhanced the resistance of AAMs against sulfuric acid attack, shifting the dominant processes from diffusion and cracks to framework-dissolution controlled by the inherent phase stabilities. Following the immersion in sulfuric acid (pHstat = 2) for 8 weeks, the depth of corroded layer decreased by 70% and no cracks due to expansive phases were observed. These promising findings suggest that the incorporation of vegetable oil in AAMs has the potential to address durability concerns associated with diffusion-based corrosion processes, thereby expanding the range of future applications. KW - Alkali-activated materials KW - Acid resistance KW - Pore structure PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581719 DO - https://doi.org/10.1016/j.ceramint.2023.08.036 VL - 49 IS - 20 SP - 33275 EP - 33290 PB - Elsevier Ltd. AN - OPUS4-58171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruehle, Bastian T1 - Natural language processing for automated workflow and knowledge graph generation in self-driving labs N2 - Natural language processing with the help of large language models such as ChatGPT has become ubiquitous in many software applications and allows users to interact even with complex hardware or software in an intuitive way. The recent concepts of Self-Driving Labs and Material Acceleration Platforms stand to benefit greatly from making them more accessible to a broader scientific community through enhanced user-friendliness or even completely automated ways of generating experimental workflows that can be run on the complex hardware of the platform from user input or previously published procedures. Here, two new datasets with over 1.5 million experimental procedures and their (semi)automatic annotations as action graphs, i.e., structured output, were created and used for training two different transformer-based large language models. These models strike a balance between performance, generality, and fitness for purpose and can be hosted and run on standard consumer-grade hardware. Furthermore, the generation of node graphs from these action graphs as a user-friendly and intuitive way of visualizing and modifying synthesis workflows that can be run on the hardware of a Self-Driving Lab or Material Acceleration Platform is explored. Lastly, it is discussed how knowledge graphs – following an ontology imposed by the underlying node setup and software architecture – can be generated from the node graphs. All resources, including the datasets, the fully trained large language models, the node editor, and scripts for querying and visualizing the knowledge graphs are made publicly available. KW - Natural Language Processing KW - Large Language Models KW - Self-Driving Labs KW - Materials Acceleration Platforms KW - Workflows KW - Nanomaterials KW - Advanced Materials PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631947 UR - https://github.com/BAMresearch/MAPz_at_BAM/tree/main/Minerva-Workflow-Generator DO - https://doi.org/10.1039/d5dd00063g SN - 2635-098X SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruibal, C. A1 - Gueidan, C. A1 - Selbmann, L. A1 - Gorbushina, Anna A1 - Crous, P.W. A1 - Groenewald, J.Z. A1 - Muggia, L. A1 - Grube, M. A1 - Isola, D. A1 - Schoch, C.L. A1 - Staley, J.T. A1 - Lutzoni, F. A1 - De Hoog, G.S. T1 - Phylogeny of rock-inhabiting fungi related to Dothideomycetes N2 - The class Dothideomycetes (along with Eurotiomycetes) includes numerous rock-inhabiting fungi (RIF), a group of ascomycetes that tolerates surprisingly well harsh conditions prevailing on rock surfaces. Despite their convergent morphology and physiology, RIF are phylogenetically highly diverse in Dothideomycetes. However, the positions of main groups of RIF in this class remain unclear due to the lack of a strong phylogenetic framework. Moreover, connections between rock-dwelling habit and other lifestyles found in Dothideomycetes such as plant pathogens, saprobes and lichen-forming fungi are still unexplored. Based on multigene phylogenetic analyses, we report that RIF belong to Capnodiales (particularly to the family Teratosphaeriaceae s.l.), Dothideales, Pleosporales, and Myriangiales, as well as some uncharacterised groups with affinities to Dothideomycetes. Moreover, one lineage consisting exclusively of RIF proved to be closely related to Arthoniomycetes, the sister class of Dothideomycetes. The broad phylogenetic amplitude of RIF in Dothideomycetes suggests that total species richness in this class remains underestimated. Composition of some RIF-rich lineages suggests that rock surfaces are reservoirs for plant-associated fungi or saprobes, although other data also agree with rocks as a primary substrate for ancient fungal lineages. According to the current sampling, long distance dispersal seems to be common for RIF. Dothideomycetes lineages comprising lichens also include RIF, suggesting a possible link between rock-dwelling habit and lichenisation. KW - Arthoniomycetes KW - Capnodiales KW - Dothideomycetes KW - Evolution KW - Extremotolerance KW - Multigene phylogeny KW - Rock-inhabiting fungi PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-219821 DO - https://doi.org/10.3114/sim.2009.64.06 SN - 0166-0616 VL - 64 IS - 1 SP - 123 EP - 133 PB - Centraalbureau voor Schimmelcultures CY - Utrecht, The Netherlands AN - OPUS4-21982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rus, J. A1 - Gustschin, A. A1 - Mooshofer, H. A1 - Grager, J.-C. A1 - Bente, Klaas A1 - Gaal, Mate A1 - Pfeiffer, F. A1 - Grosse, C. U. T1 - Qualitative comparison of non-destructive methods for inspection of carbon fiber-reinforced polymer laminates N2 - In the rapidly expanding composite industry, novel inspection methods have been developed in recent years. Particularly promising for air-coupled testing are cellular polypropylene transducers which offer better impedance matching to air than piezoelectric transducers. Furthermore, broadband transmitters (laser-induced ultrasound and thermoacoustic emitters) and receivers (optical microphones) have opened a completely new chapter for advanced contact-free ultra-sound inspection. X-ray dark-field radiography offers a different approach to detect porosity and microcracks, employing small angle X-ray scattering. These innovative ultrasonic and radiographic alternatives were evaluated in comparison with well-established inspection techniques. We applied thirteen different non-destructive methods to inspect the same specimen (a carbon fiber-reinforced polymer laminate with induced impact damage): air-coupled ultrasound testing (using piezoelectric transducers, broadband optical microphones, cellular polypropylene transducers, and a thermoa- coustic emitter), laser-induced ultrasound testing, ultrasonic immersion testing, phased array ultrasonic testing, optically excited lock-in thermography, and X-ray radiography (projectional absorption and dark-field, tomosynthesis, and micro-computed tomography). The inspection methods were qualitatively characterized by comparing the scan results. The conclusions are advantageous for a decision on the optimal method for certain testing constraints. KW - Carbon fiber-reinforced polymer KW - Air-coupled ultrasound KW - Optically excited lock-in thermography KW - X-ray micro-computed tomography KW - X-ray dark-field radiography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509473 DO - https://doi.org/10.1177/0021998320931162 SN - 0021-9983 VL - 54 IS - 27 SP - 4325 EP - 4337 PB - SAGE AN - OPUS4-50947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Russo, Francesco F. A1 - Nowatzky, Yannek A1 - Jaeger, Carsten A1 - Parr, Maria K. A1 - Benner, Philipp A1 - Muth, Thilo A1 - Lisec, Jan T1 - Machine learning methods for compound annotation in non‐targeted mass spectrometry—A brief overview of fingerprinting, in silico fragmentation and de novo methods N2 - Non‐targeted screenings (NTS) are essential tools in different fields, such as forensics, health and environmental sciences. NTSs often employ mass spectrometry (MS) methods due to their high throughput and sensitivity in comparison to, for example, nuclear magnetic resonance–based methods. As the identification of mass spectral signals, called annotation, is labour intensive, it has been used for developing supporting tools based on machine learning (ML). However, both the diversity of mass spectral signals and the sheer quantity of different ML tools developed for compound annotation present a challenge for researchers in maintaining a comprehensive overview of the field.In this work, we illustrate which ML‐based methods are available for compound annotation in non‐targeted MS experiments and provide a nuanced comparison of the ML models used in MS data analysis, unravelling their unique features and performance metrics. Through this overview we support researchers to judiciously apply these tools in their daily research. This review also offers a detailed exploration of methods and datasets to show gaps in current methods, and promising target areas, offering a starting point for developers intending to improve existing methodologies. KW - Mass Spectrometry KW - Spectra annotation KW - Machine learning PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608732 DO - https://doi.org/10.1002/rcm.9876 VL - 38 IS - 20 SP - 1 EP - 15 PB - Wiley AN - OPUS4-60873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruyle, B. A1 - Pickard, H. A1 - Schultes, L. A1 - Fredriksson, F. A1 - Heffernan, A. A1 - Knappe, D. A1 - Lord, H. A1 - Meng, P. A1 - Mills, M. A1 - Ndungu, K. A1 - Roesch, Philipp A1 - Rundberget, J.T. A1 - Tettenhorst, D. A1 - Van Buren, J. A1 - Vogel, Christian A1 - Westerman, D. A1 - Yeung, L. A1 - Sunderland, E. T1 - Interlaboratory Comparison of Extractable Organofluorine Measurements in Groundwater and Eel (Anguilla rostrata): Recommendations for Methods Standardization N2 - Research on per- and polyfluoroalkyl substances (PFAS) frequently incorporates organofluorine measurements, particularly because they could support a class-based approach to regulation. However, standardized methods for organofluorine analysis in a broad suite of matrices are currently unavailable, including a method for extractable organofluorine (EOF) measured using combustion ion chromatography (CIC). Here, we report the results of an international interlaboratory comparison. Seven laboratories representing academia, government, and the private sector measured paired EOF and PFAS concentrations in groundwater and eel (Anguilla rostrata) from a site contaminated by aqueous film-forming foam. Among all laboratories, targeted PFAS could not explain all EOF in groundwater but accounted for most EOF in eel. EOF results from all laboratories for at least one replicate extract fell within one standard deviation of the interlaboratory mean for groundwater and five out of seven laboratories for eel. PFAS spike mixture recoveries for EOF measurements in groundwater and eel were close to the criterion (±30%) for standardized targeted PFAS methods. Instrumental operation of the CIC such as replicate sample injections was a major source of measurement uncertainty. Blank contamination and incomplete inorganic fluorine removal may introduce additional uncertainties. To elucidate the presence of unknown organofluorine using paired EOF and PFAS measurements, we recommend that analysts carefully consider confounding methodological uncertainties such as differences in precision between measurements, data processing steps such as blank subtraction and replicate analyses, and the relative recoveries of PFAS and other fluorine compounds. KW - Extractable organic fluorine KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Combustion ion chromatography (CIC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587726 DO - https://doi.org/10.1021/acs.est.3c04560 SN - 0013-936X VL - 57 IS - 48 SP - 20159 EP - 20168 PB - American Chemical Society (ACS) AN - OPUS4-58772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Hänninen, H. A1 - Böllinghaus, Thomas T1 - In-situ ToF-SIMS analyses of deuterium re-distribution in austenitic steel AISI 304L under mechanical load N2 - Hydrocarbons fuel our economy. Furthermore, intermediate goods and consumer products are often hydrocarbon-based. Beside all the progress they made possible, hydrogen-containing substances can have severe detrimental effects on materials exposed to them. Hydrogen-assisted failure of iron alloys has been recognised more than a century ago. The present study aims to providing further insight into the degradation of the austenitic stainless steel AISI 304L (EN 1.4307) exposed to hydrogen. To this end, samples were electrochemically charged with the hydrogen isotope deuterium (2H, D) and analysed by scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). It was found that deuterium caused a phase transformation from the original γ austenite into ε- and α’-martensite. Despite their low solubility for hydrogen, viz. deuterium, the newly formed phases showed high deuterium concentration which was attributed to the increased density of traps. Information about the behaviour of deuterium in the material subjected to external mechanical load was gathered. A four-point-bending device was developed for this purpose. This allowed to analyse in-situ pre-charged samples in the ToF-SIMS during the application of external mechanical load. The results indicate a movement of deuterium towards the regions of highest stress. KW - ToF-SIMS KW - Hydrogen KW - Deuterium KW - AISI 304L KW - EBSD PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505142 DO - https://doi.org/10.1038/s41598-020-60370-2 VL - 10 IS - 1 SP - 3611 PB - Nature AN - OPUS4-50514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Comprehensive study of deuterium-induced effects in in austenitic stainless steel AISI 304L N2 - The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed. To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place. By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules. KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Deuterium KW - Martensite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477540 DO - https://doi.org/10.1016/j.ijhydene.2019.03.058 SN - 0360-3199 SN - 1879-3487 VL - 44 IS - 23 SP - 12228 EP - 12238 PB - Elsevier Ltd. AN - OPUS4-47754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rösler, Alexander A1 - Weidner, Steffen A1 - Klamroth, Tillmann A1 - Müller, Axel H. E. A1 - Schlaad, Helmut T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents N2 - The kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. KW - MALDI-TOF MS KW - Anionic polymerization KW - β‐myrcene KW - Kinetics KW - Reaction order KW - Activation energy KW - Microstructure KW - Quantum chemical calculations PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630900 DO - https://doi.org/10.1002/pi.6772 SN - 1097-0126 SP - 1 EP - 8 PB - Wiley CY - New York, NY AN - OPUS4-63090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rösler, Alexander A1 - Weidner, Steffen A1 - Klamroth, Tillmann A1 - Müller, Axel HE A1 - Schlaad, Helmut T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. KW - Myrcene KW - Anionic polymerization KW - Reaction order KW - Activation energy KW - Microstructure KW - Quantum chemical calculation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636840 DO - https://doi.org/10.1002/pi.6772 SN - 0959-8103 SP - 1 EP - 8 PB - Wiley AN - OPUS4-63684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rösler, Alexander A1 - Weidner, Steffen A1 - Klamroth, Tillmann A1 - Müller, Axel HE A1 - Schlaad, Helmut T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. KW - Myrcene KW - Anionic polymerization KW - MALDI TOF MS PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649039 DO - https://doi.org/10.1002/pi.6772 SN - 0959-8103 SP - 1 EP - 8 PB - Wiley AN - OPUS4-64903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rühle, Bastian A1 - Krumrey, Julian Frederic A1 - Hodoroaba, Vasile-Dan T1 - Workflow towards automated segmentation of agglomerated, non‑spherical particles from electron microscopy images using artificial neural networks N2 - We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from scanning electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. We compare the segmentation masks obtained with our suggested workflow qualitatively and quantitatively to state-of-the-art methods using various metrics. Finally, we used the segmentation masks for automatically extracting particle size distributions from the SEM images of TiO2 particles, which were in excellent agreement with particle size distributions obtained manually but could be obtained in a fraction of the time. KW - Electron microscopy KW - Neural networks KW - Artificial intelligence KW - Image segmentation KW - Automated image analysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522454 DO - https://doi.org/10.1038/s41598-021-84287-6 VL - 11 IS - 1 SP - 4942 PB - Springer Nature AN - OPUS4-52245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rütters, H. A1 - Fischer, S. A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Bäßler, Ralph A1 - Maßmann, J. A1 - Ostertag-Henning, C. A1 - Wolf, J. L. A1 - Pumpa, M. A1 - Lubenau, U. A1 - Knauer, S. A1 - Jaeger, P. A1 - Neumann, A. A1 - Svensson, K. A1 - Pöllmann, H. A1 - Lempp, C. A1 - Menezes, F. F. A1 - Hagemann, B. T1 - Towards defining reasonable minimum composition thresholds – Impacts of variable CO2 stream compositions on transport, injection and storage N2 - To set up recommendations on how to define “reasonable minimum composition thresholds” for CO2 streams to access CO2 pipeline networks, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the CCS chain. All investigations were based on a generic “CCS cluster scenario” in which CO2 streams captured from a spatial cluster of eleven emitters (seven fossil-fired power plants, two cement plants, one refinery and one steel mill) are collected in a regional pipeline network. The resulting CO2 stream (19.78 Mio t impure CO2 per year) is transported in a trunk line (onshore and offshore) and injected into five generic replicate storage structures (Buntsandstein saline aquifers) offshore. Experimental investigations and modeling of selected impacts revealed beneficial as well as adverse impacts of different impurities and their combinations. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the considered variable compositions and mass flow rates were observed. We recommend to define minimum composition thresholds for each specific CCS project through limiting i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of concentrations of critical impurities, and defining impurity combinations to be avoided. KW - Impurities KW - CO2 quality KW - Pipeline network KW - Whole-chain CCS scenario KW - Recommendations PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543004 DO - https://doi.org/10.1016/j.ijggc.2022.103589 SN - 1750-5836 VL - 114 SP - 1 EP - 14 PB - Elsevier CY - New York, NY AN - OPUS4-54300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, André A1 - Hasenbein, Ines A1 - Hortschansky, Peter A1 - Schmuck, Klaus D. A1 - Maenz, Stefan A1 - Illerhaus, Bernhard A1 - Kuehmstedt, Peter A1 - Ramm, Roland A1 - Huber, René A1 - Kunisch, Elke A1 - Horbert, Victoria A1 - Gunnella, Francesca A1 - Roth, Andreas A1 - Schubert, Harald A1 - Kinne, Raimund W. T1 - BMP-2 (and partially GDF-5) coating significantly accelerates and augments bone formation close to hydroxyapatite/tricalcium-phosphate/brushite implant cylinders for tibial bone defects in senile, osteopenic sheep N2 - Bilateral defects (diameter 8 mm) in the medial tibial head of senile, osteopenic female sheep (n = 48; 9.63 ± 0.10 years; mean ± SEM) were treated with hydroxyapatite (HA)/beta-tricalcium phosphate (β-TCP)/dicalcium phosphate dihydrate (DCPD; brushite) cylinders coated with BMP-2 (25 or 250 micrograms) or growth differentiation factor (GDF)-5 (125 or 1250 micrograms; left side); cylinders without BMP served as controls (right side). Three, 6, and 9 months post-operation (n = 6 each group), bone structure and formation were analyzed in vivo by X-ray and ex vivo by osteodensitometry, histomorphometry, and micro-computed tomography (micro-CT) at 3 and 9 months. Semi-quantitative X-ray evaluation showed significantly increasing bone densities around all implant cylinders over time. High-dose BMP-2-coated cylinders (3 and 9 months) and low-dose GDF-5-coated cylinders (3 and 6 months) demonstrated significantly higher densities than controls (dose-dependent for BMP-2 at 3 months). This was confirmed by osteodensitometry at 9 months for high-dose BMP-2-coated cylinders (and selected GDF-5 groups), and was again dose-dependent for BMP-2. Osteoinduction by BMP-2 was most pronounced in the adjacent bone marrow (dynamic histomorphometry/micro-CT). BMP-2 (and partially GDF-5) significantly increased the bone formation in the vicinity of HA/TCP/DCPD cylinders used to fill tibial bone defects in senile osteopenic sheep and may be suitable for surgical therapy of critical size, non-load-bearing bone defects in cases of failed tibial head fracture or defect healing. KW - Bone morphogenetic protein (BMP) KW - Growth differentiation factor (GDF) KW - Bone replacement material PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623923 DO - https://doi.org/10.1007/s10856-023-06734-2 SN - 1573-4838 VL - 34 IS - 7 SP - 1 EP - 15 PB - Springer Science and Business Media LLC CY - Dordrecht AN - OPUS4-62392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -