TY - JOUR A1 - Abdel-Wakil, W. A1 - Fahmy, Alaa A1 - Kamoun, E. A1 - Hassan, W. A1 - Abdelhai, Q. A1 - Salama, T. T1 - A New Route for Synthesis of Polyurethanevinyl Acetate Acrylate Emulsions as Binders for Pigment Printing of Cotton Fabrics N2 - Herein, two polyurethane oligomers were successfully synthesized using a prepolymer mixing process. The prepolymers were synthesized based on the step-growth addition polymerization of polypropylene glycol, Methylene diphenyl diisocyanate and 2-hydroxyethyl methacrylate or 2-hydroxyethyl acrylate. Isopropanol was functioned as the isocyanate blocking agent. Thereafter, different terpolymer emulsions were prepared by the emulsion graft copolymerization with the vinyl acetate monomer in presence of 2-ethylhexyl acrylate as a vinyl monomer. The chemical structures of the synthesized oligomeric monomers were probed by FTIR spectroscopy and found to vary with the content of acrylic monomer used in the oligomer synthesis phase (i.e.hydroxyethyl acrylate or hydroxyethyl methacrylate). The topography, thermal stability, and particle size of terpolymers were investigated by SEM, TGA, and zeta potential, respectively. The TGA results demonstrated marked enhancement in thermal stability of the synthesized terpolymers up to ca. 600°C, which was concurrent with enhanced surface homogeneity and film properties as evidenced by the SEM images. These terpolymers showed also property enhancement as binders for textile pigment printing in terms of rubbing resistance, color strength and fastness to washing when compared to the commercial binders. These judgments would provide a new competent synthesis route by introducing polyurethane acetate vinyl acrylate as the binder for use in pigment printing of cotton fabrics. KW - Vinyl monomer KW - Polyurethane acetate vinyl acrylate KW - Surface coating KW - Terpolymer KW - Textile binder PY - 2020 DO - https://doi.org/10.21608/ejchem.2020.21712.2292 VL - 63 IS - 3 SP - 1063 EP - 1073 AN - OPUS4-52300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abed, Jehad A1 - Bai, Yanh A1 - Persaud, Daniel A1 - Kim, Jiheon A1 - Witt, Julia A1 - Hattrick.Simpers, Jason A1 - Sargent, Edward T1 - AMPERE: automated modular platform for expedited and reproducible electrochemical testing N2 - Rapid and reliable electrochemical screening is critical to accelerate the development of catalysts for sustainable energy generation and storage. This paper introduces an automated and modular platform for expedited and reproducible electrochemical testing (AMPERE), designed to enhance the efficiency and reliability of multivariate optimization. The platform integrates a liquid-handling robot with custommade modular array reactors, offering sample preparation and electrochemical testing in the same platform. Additionally, we use offline inductively coupled plasma optical emission spectroscopy (ICPOES) to measure metal concentrations in the electrolyte after the reaction, which serves as a proxy for assessing the electrochemical stability. We use the platform to conduct 168 experiments continuously in less than 40 hours to examine the influence of catalyst ink formulation on the performance of Ir, Ru, IrO2, and RuO2 for the oxygen evolution reaction (OER) in acid. We specifically investigate the role of solvent type and concentration, catalyst concentration, and binder content on the performance. We find that Ru/RuO2 catalysts show improvements in activity that are not directly linked to improvements in the electrochemical surface area or inversely correlated to Ru dissolution. This suggests a complex interplay between the catalytic performance of the drop-casted catalyst film and ink formulation. AMPERE simplifies catalyst preparation and testing at large scale, making it faster, more reliable, and accessible for widespread use. KW - Electrochemical screening KW - Automated platform KW - Catalysis KW - Energy generation and storage KW - Oxygen evolution reaction (OER) KW - MAPz@BAM PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614724 DO - https://doi.org/10.1039/d4dd00203b SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-61472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abusafia, A. A1 - Scheid, C. A1 - Meurer, Maren A1 - Altmann, Korinna A1 - Dittmer, U. A1 - Steinmetz, H. T1 - Microplastic sampling strategies in urban drainage systems for quantification of urban emissions based on transport pathways N2 - Tracking waterborne microplastic (MP) in urban areas is a challenging task because of the various sources and transport pathways involved. Since MP occurs in low concentrations in most wastewater and stormwater streams, large sample volumes need to be captured, prepared, and carefully analyzed. The recent research in urban areas focused mainly on MP emissions at wastewater treatment plants (WWTPs), as obvious entry points into receiving waters. However, important transport pathways under wet-weather conditions are yet not been investigated thoroughly. In addition, the lack of comprehensive and comparable sampling strategies complicated the attempts for a deeper understanding of occurrence and sources. The goal of this paper is to (i) introduce and describe sampling strategies for MP at different locations in a municipal catchment area under dry and wet-weather conditions, (ii) quantify MP emissions from the entire catchment and two other smaller ones within the bigger catchment, and (iii) compare the emissions under dry and wet-weather conditions. WWTP has a high removal rate of MP (>96%), with an estimated emission rate of 189 kg/a or 0.94 g/[population equivalents (PEQ · a)], and polyethylene (PE) as the most abundant MP. The specific dry-weather emissions at a subcatchment were ≈30 g/(PEQ · a) higher than in the influent of WWTP with 23 g/(PEQ · a). Specific wet-weather emissions from large sub-catchment with higher traffic and population densities were 1952 g/(ha · a) higher than the emissions from smaller catchment (796 g/[ha · a]) with less population and traffic. The results suggest that wet-weather transport pathways are likely responsible for 2–4 times more MP emissions into receiving waters compared to dry-weather ones due to tire abrasion entered from streets through gullies. However, more investigations of wet-weather MP need to be carried out considering additional catchment attributes and storm event characteristics. KW - Combined sewer system KW - Large volume samplers KW - Microplastic pollution KW - Separate sewer system KW - Stormwater retention tank PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568271 DO - https://doi.org/10.1002/appl.202200056 SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Accorsi, M. A1 - Tiemann, M. A1 - Wehrhan, L. A1 - Finn, Lauren M. A1 - Cruz, R. A1 - Rautenberg, Max A1 - Emmerling, Franziska A1 - Heberle, J. A1 - Keller, B. G. A1 - Rademann, J. T1 - Pentafluorophosphato-Phenylalanines: Amphiphilic Phosphotyrosine Mimetics Displaying Fluorine-Specific Protein Interactions N2 - Phosphotyrosine residues are essential functional switches in health and disease. Thus, phosphotyrosine biomimetics are crucial for the development of chemical tools and drug molecules. We report here the discovery and investigation of pentafluorophosphato amino acids as novel phosphotyrosine biomimetics. A mild acidic pentafluorination protocol was developed and two PF5-amino acids were prepared and employed in peptide synthesis. Their structures, reactivities, and fluorine-specific interactions were studied by NMR and IR spectroscopy, X-ray diffraction, and in bioactivity assays. The mono-anionic PF5 motif displayed an amphiphilic character binding to hydrophobic surfaces, to water molecules, and to protein-binding sites, exploiting charge and H−F-bonding interactions. The novel motifs bind 25- to 30-fold stronger to the phosphotyrosine binding site of the protein tyrosine phosphatase PTP1B than the best current biomimetics, as rationalized by computational methods, including molecular dynamics simulations. KW - Chemical Biology KW - Drug Development KW - Pentafluorophosphates KW - Phosphotyrosine Biomimetics KW - Protein Tyrosine Phosphatases PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549984 DO - https://doi.org/10.1002/anie.202203579 SN - 1433-7851 VL - 134 IS - 25 SP - 1 EP - 6 PB - Wiley-VCH GmbH AN - OPUS4-54998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Acosta-Zepeda, C. A1 - Saavedra, S. A1 - Bonse, Jörn A1 - Haro-Poniatowski, E. T1 - Modelling of single UV nanosecond pulsed laser surface modifications of silicon N2 - Irradiation with a single spatially Gaussian-shaped nanosecond laser pulse in the melting regime can result in a characteristic annular change in the surface morphology of crystalline silicon. This has been verified experimentally in a variety of situations, where dimple-shaped surface topographies are produced. In a recent work we have investigated the induced changes in the surface topography upon exposure to wavelengths in the visible and near infrared spectral region. Irradiation in the UV requires a more detailed analysis due to the enhanced absorption of the material. In the present analysis, we determine under which conditions our previous model can be used and the corresponding results are presented. KW - Laser KW - Silicon KW - Surface modification PY - 2020 DO - https://doi.org/10.1088/1555-6611/ab9b2c SN - 1555-6611 SN - 1054-660X VL - 30 IS - 8 SP - 086003-1 EP - 086003-4 PB - IOP Publishing / Astro Ltd CY - Bristol, United Kingdom AN - OPUS4-51022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adamski, Paweł A1 - Zgrzebnicki, Michał A1 - Albrecht, Aleksander A1 - Jurkowski, Artur A1 - Wojciechowska, Agnieszka A1 - Ekiert, Ewa A1 - Sielicki, Krzysztof A1 - Mijowska, Ewa A1 - Smales, Glen J. A1 - Maximenko, Alexey A1 - Moszyński, Dariusz T1 - Ammonia synthesis over γ-Al2O3 supported Co-Mo catalysts N2 - Novel ammonia synthesis catalysts are sought due to energetic transformation and increasing environmental consciousness. Materials containing cobalt and molybdenum are showing state-of-art activities in ammonia synthesis. The application of γ-alumina support was proposed to enhance the properties of Co-Mo nanoparticles. The wet impregnation of the support was conducted under reduced pressure. The active catalysts were obtained by ammonolysis of precursors. The chemical and phase composition, as well as morphology, porosity, and surface composition of precursors and catalysts, were characterized. The Co-Mo nanoparticles phase composition as well as their size and dispersion were determined using X-ray absorption spectroscopy utilizing synchrotron radiation, electron microscopy, and X-ray scattering. The catalytic activity was tested in the ammonia synthesis process under atmospheric pressure. The activity and stability of the supported catalysts were compared with unsupported cobalt molybdenum nitride Co3Mo3N, revealing the superiority of the present approach. KW - Ammonia synthesis KW - Supported catalyst KW - Cobalt molybdenum nitrides KW - Scattering KW - X-ray scattering KW - Gamma-alumina KW - Stability PY - 2025 DO - https://doi.org/10.1016/j.mcat.2025.114907 SN - 2468-8231 VL - 575 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-64827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adhami, Forogh A1 - Safavi, Maliheh A1 - Ehsani, Maryam A1 - Ardestani, Sussan K. A1 - Emmerling, Franziska A1 - Simyari, Farzaneh T1 - Synthesis, crystal structure, and cytotoxic activity of novel cyclic systems in [1,2,4]thiadiazolo[2,3-a]pyridine benzamide derivatives and their copper(ii) complexes N2 - Three N-(pyridine-2-ylcarbamothioyl)benzamide derivatives were synthesized by the reaction of potassium thiocyanate, benzoyl chloride, and 2-amino pyridine derivatives in one pot. The obtained derivatives were oxidized using copper(II) chloride. During the oxidation, two hydrogen atoms were removed, cyclization of the derivatives occurred, and finally, three new N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives were produced. Coordination of these three new derivative ligands to the copper(II) ion resulted in the formation of three new complexes: dichlorobis(N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide)copper(II), dichlorobis(N-(7-methyl-2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2ylidene)benzamide)copper(II), and dichlorobis(N-(5-methyl-2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide)copper(II). All the synthesized products were characterized by IR, 1H NMR, and 13C NMR spectroscopies. Crystal structures of the obtained N-(pyridine-2-ylcarbamothioyl)benzamide derivatives, N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives, and complexes were determined using X-ray single-crystal diffraction; the positions of atoms, bond lengths, bond angles, and dihedral angles were also determined. In all complexes, the coordination of two large monodentate ligands and two chloride anions to the copper(II) ion resulted in the formation of a stable planar geometry around the central ion. Three N-(pyridine-2-ylcarbamothioyl)benzamide derivatives, three N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives, and three complexes were evaluated for their cytotoxicity against five human cancer cell lines (breast cancer cell line MDA-MB-231, neuroblastoma cell line SK-N-MC, prostate adenocarcinoma cell line LNCap, nasopharyngeal epidermoid carcinoma cell line KB, and liver cancer cell line HEPG-2) using an in vitro analysis. The N-(pyridine-2-ylcarbamothioyl)benzamide derivatives showed no cytotoxic activity, whereas the N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives and their complexes showed significant cytotoxicity, especially against MDA-MB-231 and LNCap cell lines. The complexes demonstrated smaller IC50 values than N-(2H-[1,2,4]thiadiazolo[2,3-a]pyridine-2-ylidene)benzamide derivatives. KW - Copper complexes PY - 2014 DO - https://doi.org/10.1039/c3dt52905c SN - 1477-9226 VL - 43 IS - 21 SP - 7945 EP - 7957 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Afantitis, A. A1 - Melagraki, G. A1 - Isigonis, P. A1 - Tsoumanis, A. A1 - Varsou, D. D. A1 - Valsami-Jones, E. A1 - Papadiamantis, A. A1 - Ellis, L.-J. A. A1 - Sarimveis, H. A1 - Doganis, P. A1 - Karatzas, P. A1 - Tsiros, P. A1 - Liampa, I. A1 - Lobaskin, V. A1 - Greco, D. A1 - Serra, A. A1 - Kinaret, P. A. S. A1 - Saarimäki, L. A. A1 - Grafström, R. A1 - Kohonen, P. A1 - Nymark, P. A1 - Willighagen, E. A1 - Puzyn, T. A1 - Rybinska-Fryca, A. A1 - Lyubartsev, A. A1 - Jensen, K. A. A1 - Brandenburg, J. G. A1 - Lofts, S. A1 - Svendsen, C. A1 - Harrison, S. A1 - Maier, D. A1 - Tamm, K. A1 - Jänes, J. A1 - Sikk, L. A1 - Dusinska, M. A1 - Longhin, E. A1 - Rundén-Pran, E. A1 - Mariussen, E. A1 - El Yamani, N. A1 - Unger, Wolfgang A1 - Radnik, Jörg A1 - Tropsha, A. A1 - Cohen, Y. A1 - Lesczynski, J. A1 - Hendren, C. O. A1 - Wiesner, M. A1 - Winkler, D. A1 - Suzuki, N. A1 - Yoon, T. H. A1 - Choi, J.-S. A1 - Sanabria, N. A1 - Gulumian, M. A1 - Lynch, I. T1 - NanoSolveIT Project: Driving nanoinformatics research to develop innovative and integrated tools for in silico nanosafety assessment N2 - Nanotechnology has enabled the discovery of a multitude of novel materials exhibiting unique physicochemical (PChem) properties compared to their bulk analogues. These properties have led to a rapidly increasing range of commercial applications; this, however, may come at a cost, if an association to long-term health and environmental risks is discovered or even just perceived. Many nanomaterials (NMs) have not yet had their potential adverse biological effects fully assessed, due to costs and time constraints associated with the experimental assessment, frequently involving animals. Here, the available NM libraries are analyzed for their suitability for integration with novel nanoinformatics approaches and for the development of NM specific Integrated Approaches to Testing and Assessment (IATA) for human and environmental risk assessment, all within the NanoSolveIT cloud-platform. These established and well-characterized NM libraries (e.g. NanoMILE, NanoSolutions, NANoREG, NanoFASE, caLIBRAte, NanoTEST and the Nanomaterial Registry (>2000 NMs)) contain physicochemical characterization data as well as data for several relevant biological endpoints, assessed in part using harmonized Organisation for Economic Co-operation and Development (OECD) methods and test guidelines. Integration of such extensive NM information sources with the latest nanoinformatics methods will allow NanoSolveIT to model the relationships between NM structure (morphology), properties and their adverse effects and to predict the effects of other NMs for which less data is available. The project specifically addresses the needs of regulatory agencies and industry to effectively and rapidly evaluate the exposure, NM hazard and risk from nanomaterials and nano-enabled products, enabling implementation of computational ‘safe-by-design’ approaches to facilitate NM commercialization. KW - Nanoinformatics KW - Hazard assessment KW - (Quantitative) Structure-Active Relationships KW - Safe-by-design KW - Predictive modelling PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505952 DO - https://doi.org/10.1016/j.csbj.2020.02.023 VL - 18 SP - 583 EP - 602 PB - Elsevier B.V. AN - OPUS4-50595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agostini, G. A1 - Radnik, Jörg T1 - Spectroscopy in Catalysis N2 - Knowledge-based catalyst development is always an interaction between preparation, analysis and catalytic testing. Only if these three factors fit together can success be expected. For the analytic side of this triangle, spectroscopic methods play a crucial role. Whereas with diffraction, scattering and microscopy, decisive insights into the structure and morphology of the catalysts can be obtained, spectroscopy produces new knowledge about the chemical nature of the catalyst, e.g., its bonding and valence states. KW - Spectroscopy KW - Catalysis KW - Operando KW - In situ PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506507 DO - https://doi.org/10.3390/catal10040408 VL - 10 IS - 4 SP - 408 PB - MDPI CY - Basel AN - OPUS4-50650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmed, R. A1 - Vaishampayan, A. A1 - Cuellar-Camacho, J. L. A1 - Wight, D. J. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang A1 - Grohmann, E. A1 - Haag, R. A1 - Wagner, O. T1 - Multivalent Bacteria Binding by Flexible Polycationic Microsheets Matching Their Surface Charge Density N2 - Aiming at the overall negative surface charge of bacteria, a new strategy of antibacterial agents based on large polymer-modified graphene oxide (GO) sheets is assessed. The presented flexible, polycationic Sheets match the size and charge density of the Escherichia coli surface charge density (2 × 1014 cm−2). These matching parameters create an unspecific but very strong bacteria adsorber by multivalent, electrostatic attraction. Their interaction with bacteria is visualized via atomic force and confocal microscopy and shows that they effectively bind and wrap around E. coli cells, and thereby immobilize them. The incubation of Gram-negative and -positive bacteria (E. coli and methicillin-resistant Staphylococcus aureus, MRSA) with these polycationic sheets leads to the inhibition of proliferation and a reduction of the colony forming bacteria over time. This new type of antibacterial agent acts in a different mode of Action than classical biocides and could potentially be employed in medicinal, technical, or agriculture applications. The presented microsheets and their unspecific binding of cell interfaces could further be employed as adsorber material for bacterial filtration or immobilization for imaging, analysis, or sensor technologies. KW - Surface charge KW - Bacteria KW - Graphene oxide KW - Escherichia coli KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509651 DO - https://doi.org/10.1002/admi.201902066 VL - 7 IS - 15 SP - 1902066 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Waqfi, R. A. A1 - Khan, C. J. A1 - Irving, O. J. A1 - Matthews, Lauren A1 - Albrecht, T. T1 - Crowding Effects during DNA Translocation in Nanopipettes N2 - Quartz nanopipettes are an important emerging class of electric single-molecule sensors for DNA, proteins, their complexes, as well as other biomolecular targets. However, in comparison to other resistive pulse sensors, nanopipettes constitute a highly asymmetric environment and the transport of ions and biopolymers can become strongly directiondependent. For double-stranded DNA, this can include the characteristic translocation time and tertiary structure, but as we show here, nanoconfinement can also unlock capabilities for biophysical and bioanalytical studies at the single-molecule level. To this end, we show how the accumulation of DNA inside the nanochannel leads to crowding effects, and in some cases reversible blocking of DNA entry, and provide a detailed analysis based on a range of different DNA samples and experimental conditions. Moreover, using biotin-functionalized DNA and streptavidinmodified gold nanoparticles as target, we demonstrate in a proof-of-concept study how the crowding effect, and the resulting increased residence time in nanochannel, can be exploited by first injecting the DNA into the nanochannel, followed by incubation with the nanoparticle target and analysis of the complex by reverse translocation. We thereby integrate elements of sample processing and detection into the nanopipette, as an important conceptual advance, and make a case for the wider applicability of this device concept. KW - DNA translocation KW - Transport KW - Resistive-pulse sensing KW - Nanopores KW - Nanopipettes KW - Crowding KW - Confinement PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630448 DO - https://doi.org/10.1021/acsnano.5c01529 SN - 1936-086X VL - 19 IS - 17 SP - 1 EP - 9 PB - ACS Publications AN - OPUS4-63044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Albornoz, Ricardo Valencia A1 - Antypov, Dmytro A1 - Blanke, Gerd A1 - Borges, Itamar A1 - Marulanda Bran, Andres A1 - Cheung, Joshua A1 - Collins, Christopher M. A1 - David, Nicholas A1 - Day, Graeme M. A1 - Deringer, Volker L. A1 - Draxl, Claudia A1 - Eardley-Brunt, Annabel A1 - Evans, Matthew L. A1 - Fairlamb, Ian A1 - Fieseler, Kate A1 - Franklin, Barnabas A. A1 - George, Janine A1 - Grundy, Joanna A1 - Johal, Jay A1 - Kalikadien, Adarsh V. A1 - Kapil, Venkat A1 - Kotopanov, Lyubomir A1 - Kumar, Vishank A1 - Kuttner, Christian A1 - Lederbauer, Magdalena A1 - Ojeda-Porras, Andrea Carolina A1 - Pang, Jiayun A1 - Parkes, Michael A1 - Pemberton, Miles A1 - Ruscic, Branko A1 - Ryder, Matthew R. A1 - Sakaushi, Ken A1 - Saleh, Gabriele A1 - Savoie, Brett M. A1 - Schwaller, Philippe A1 - Skjelstad, Bastian Bjerkem A1 - Sun, Wenhao A1 - Taniguchi, Takuya A1 - Taylor, Christopher R. A1 - Torrisi, Steven A1 - Vishnoi, Shubham A1 - Walsh, Aron A1 - Wu, Ruiqi T1 - Discovering trends in big data: General discussion N2 - This article is a discussion of the paper "Specialising and analysing instruction-tuned and byte-level language models for organic reaction prediction" by Jiayun Pang and Ivan Vulić (Faraday discussions, 2025, 256, 413-433). KW - Automation KW - Big data KW - Machine learning KW - Materials design KW - Chemically complex materials PY - 2025 DO - https://doi.org/10.1039/D4FD90063D SN - 1359-6640 SN - 1364-5498 VL - 256 IS - Themed collection: Data-driven discovery in the chemical sciences SP - 520 EP - 550 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-62652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aliyah, K. A1 - Prehal, C. A1 - Diercks, J. S. A1 - Diklić, N. A1 - Xu, L. A1 - Ünsal, S. A1 - Appel, C. A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Guizar-Sicairos, M. A1 - Herranz, J. A1 - Gubler, L. A1 - Büchi, F. N. A1 - Eller, J. T1 - Quantification of PEFC Catalyst Layer Saturation via In Silico, Ex Situ, and In Situ Small-Angle X-ray Scattering N2 - The complex nature of liquid water saturation of polymer electrolyte fuel cell (PEFC) catalyst layers (CLs) greatly affects the device performance. To investigate this problem, we present a method to quantify the presence of liquid water in a PEFC CL using small-angle X-ray scattering (SAXS). This method leverages the differences in electron densities between the solid catalyst matrix and the liquid water filled pores of the CL under both dry and wet conditions. This approach is validated using ex situ wetting experiments, which aid the study of the transient saturation of a CL in a flow cell configuration in situ. The azimuthally integrated scattering data are fitted using 3D morphology models of the CL under dry conditions. Different wetting scenarios are realized in silico, and the corresponding SAXS data are numerically simulated by a direct 3D Fourier transformation. The simulated SAXS profiles of the different wetting scenarios are used to interpret the measured SAXS data which allows the derivation of the most probable wetting mechanism within a flow cell electrode. KW - Polymer electrolyte fuel cell KW - Water management KW - Catalyst layer KW - Representative morphology modeling KW - Small-angle X-ray scattering KW - MOUSE KW - SAXS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575973 DO - https://doi.org/10.1021/acsami.3c00420 SN - 1944-8244 VL - 15 IS - 22 SP - 26538 EP - 26553 PB - ACS Publications AN - OPUS4-57597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alić, Jasna A1 - Schlegel, Moritz-Caspar A1 - Emmerling, Franziska A1 - Stolar, Tomislav T1 - Meeting the UN Sustainable Development Goals with Mechanochemistry N2 - Chemistry traditionally relies on reactions in solution, but this method is increasingly problematic due to the scale of chemical processes and their economic and environmental impact. Handling residual chemical waste, including solvents, incurs significant costs and environmental pressure. Conversely, novel chemical approaches are needed to address pressing societal issues such as climate change, energy scarcity, food insecurity, and waste pollution. Mechanochemistry, a sustainable chemistry discipline that uses mechanical action to induce chemical reactivity without bulk solvents, is a hot topic in academic research on sustainable and green chemistry. Given its fundamentally different working principles from solution chemistry, mechanochemistry offers more efficient chemical processes and the opportunity to design new chemical reactions. Mechanochemistry has a profound impact on many urgent issues facing our society and it is now necessary to use mechanochemistry to address them. This Minireview aims to provide a guide for using mechanochemistry to meet the United Nations (UN) Sustainable Development Goals (SDGs), thereby contributing to a prosperous society. Detailed analysis shows that mechanochemistry connects with most UN SDGs and offers more cost‐efficiency than other approaches together with a superior environmental performance. KW - Mechanochemistry KW - SDGs PY - 2024 DO - https://doi.org/10.1002/anie.202414745 SP - 1 EP - 3 PB - Wiley AN - OPUS4-61108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Almalla, A. A1 - Hertwig, Andreas A1 - Fischer, Daniel A1 - Özcan Sandikcioglu, Özlem A1 - Witt, Julia T1 - Development of layer-by-layer assembled thin coatings on aluminium alloy AA2024-T3 for high resolution studies of local corrosion processes N2 - The aim of this study is to develop nanometer-thin epoxy-based films on aluminium alloy AA2024-T3 as a model coating system for high resolution corrosion studies. Spin coating was used for the layer-by-layer (LbL) deposition of poly-(ethylenimine) (PEI) and poly([o-cresyl glycidyl ether]-co-formaldehyde) (CNER) bilayers. The film chemistry and the cross-linking process were characterized by means of Fourier-transform infrared spectroscopy (FTIR). Ellipsometric data confirmed the linear increase of film thickness. The potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) results indicate the improvement of the film barrier properties with increasing film thickness. Mapping of the topography and the volta potential was performed by means of scanning Kelvin probe force microscopy (SKPFM). The results indicate the presence of a homogeneous film structure, while the intermetallic phases can still be identified below the coating. The SKPFM Analysis confirmed that the model films are suitable for investigation of corrosion processes at the coating/metal interface. KW - Spectroscopy KW - Coatings KW - Electrochemistry KW - Microscopy KW - Resins PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514627 DO - https://doi.org/10.1002/app.49826 SN - 0021-8995 VL - 137 IS - 48 SP - e49826-1 EP - e49826-9 PB - Wiley CY - New York, NY AN - OPUS4-51462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Almalla, A. A1 - Özcan Sandikcioglu, Özlem A1 - Witt, Julia T1 - In Situ Atomic Force Microscopy Analysis of the Corrosion Processes at the Buried Interface of an Epoxy-like Model Organic Film and AA2024-T3 Aluminum Alloy N2 - The application of characterization methods with high spatial resolution to the analysis of buried coating/metal interfaces requires the design and use of model systems. Herein, an epoxy-like thin film is used as a model coating resembling the epoxy-based coatings and adhesives widely used in technical applications. Spin coating is used for the deposition of a 30 nm-thin bilayer (BL) composed of poly-(ethylenimine) (PEI) and poly[(o-cresyl glycidyl ether)-co-formaldehyde] (CNER). Fourier-transform infrared spectroscopy (FTIR) results confirm that the exposure of coated AA2024-T3 (AA) samples to the corrosive electrolyte solution does not cause the degradation of the polymer layer. In situ atomic force microscopy (AFM) studies are performed to monitor local corrosion processes at the buried interface of the epoxy-like film and the AA2024-T3 aluminum alloy surface in an aqueous electrolyte solution. Hydrogen evolution due to the reduction of water as the cathodic corrosion reaction leads to local blister formation. Based on the results of the complementary energy-dispersive X-ray spectroscopy (EDX) analysis performed at the same region of interest, most of the hydrogen evolved originates at the vicinity of Mg-containing intermetallic particles. KW - Scanning Kelvin probe force microscopy KW - Aluminum alloys KW - Buried interfaces KW - In situ atomic force microscopy KW - Local corrosion PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546932 DO - https://doi.org/10.1002/adem.202101342 SN - 1438-1656 SP - 1 EP - 9 PB - Wiley VHC-Verlag AN - OPUS4-54693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Braun, U. A1 - Herper, D. A1 - Knefel, M. A1 - Bednarz, M. A1 - Bannick, C.-G. T1 - Smart filters for the analysis of microplastic in beverages filled in plastic bottles N2 - The occurrence of microplastic (MP) in food products, such as beverages in plastic bottles, is of high public concern. Existing analytical methods focus on the determination of particle numbers, requiring elaborate sampling tools, laboratory infrastructure and generally time-consuming imaging detection methods. A comprehensive routine analysis of MP in food products is still not possible. In the present work, we present the development of a smart filter crucible as sampling and detection tool. After filtration and drying of the filtered-off solids, a direct determination of the MP mass content from the crucible sample can be done by thermal extraction desorption gas chromatography mass spectroscopy (TED-GC/MS). The new filter crucible allows a filtration of MP down to particle sizes of 5 µm. We determined MP contents below 0.01 µg/L up to 2 µg/L, depending on beverages bottle type. This may be directly related to the bottle type, especially the quality of the plastic material of the screw cap. Dependent on the plastic material, particle formation increases due to opening and closing operations during the use phase. However, we have also found that some individual determinations of samples were subjected to high errors due to random events. A conclusive quantitative evaluation of the products is therefore not possible at present. KW - Microplastic KW - TED-GC/MS KW - Plastic bottles KW - Bbeverages KW - Filter crucible PY - 2021 DO - https://doi.org/10.1080/19440049.2021.1889042 SN - 1944-0057 VL - 38 IS - 4 SP - 691 EP - 700 PB - Taylor & Francis AN - OPUS4-52323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Braun, Ulrike A1 - Bannick, C.-G. A1 - Bednarz, M. A1 - Herper, D. A1 - Knefel, M. T1 - TED-GC/MS: Schnelle Bestimmung von Mikroplastik-Massegehalten in verschiedenen Proben N2 - Zur Ermittlung von Mikroplastik-Gehalten in verschiedenen Umweltmatrices ist ein schnelles Detektionsverfahren für die Routineanalytik notwendig. Ein solches Verfahren wird hier in Form der ThermoExtraktion/Desorption-GasChromatographie/ MassenSpektroskopie (TED-GC/MS) vorgestellt. Neben grundlegenden verfahrensspezifischen Erläuterungen zur Identifizierung und Quantifizierung von Mikroplastik werden auch exemplarische Beispiele aus unterschiedlichen Umweltkompartimenten und Produkten dargestellt. Neu vorgestellt wird ein neues Verfahren zur Analytik von Flaschenwasser. Dazu wurde ein Messfiltertiegel entwickelt, der besonders für Proben mit geringen Gehalten an abfiltrierbaren Stoffen geeignet ist KW - Mikroplasik KW - Mikroplastik-Analyse KW - TED-GC/MS KW - Thermoanalytische Verfahren KW - Mikroplastik-Massengehalte PY - 2020 VL - 2020 IS - 02 SP - 55 EP - 57 PB - Gesellschaft Deutscher Chemiker (GDCh) CY - Frankfurt am Main AN - OPUS4-50835 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Goedecke, Caroline A1 - Bannick, C.-G. A1 - Abusafia, A. A1 - Scheid, C. A1 - Steinmetz, H. A1 - Paul, Andrea A1 - Beleites, C. A1 - Braun, U. T1 - Identification of microplastic pathways within a typical European urban wastewater system N2 - In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other. KW - Microplastics KW - Microplastic analysis KW - TED-GC/MS KW - Microplastic pathways KW - Mass contents PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568289 DO - https://doi.org/doi.org/10.1002/appl.202200078 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Heymann, S. A1 - Braun, U. A1 - Bannick, C.-G. A1 - Heller, C. A1 - Fuchs, M. A1 - Scheid, C. A1 - Abusafia, A. A1 - Steinmetz, H. A1 - Ricking, M. A1 - Kerndorff, A. T1 - Untersuchungsverfahren von Mikroplastikgehalten im Wasser für Praxis und Wissenschaft N2 - Zielsetzung des vom Bundesministerium für Bildung und Forschung geförderten Projektes RUSEKU war es, repräsentative Untersuchungsstrategien für die Detektion von Mikroplastik mittels TED GC/MS in wässerigen Medien zu ermitteln. Dabei wurden verschiedene Probenahmekonzepte und – verfahren für unterschiedliche Fallgestaltungen und Fragestellungen untersucht, sowie neue Filtersysteme entwickelt. Bei der Detektion der Partikel lag der Fokus auf der Anwendung und Weiterentwicklung der ThermoExtraktion/Desorption-Gaschromatographie-Massenspektrometrie (TED-GC/MS) zur Bestimmung von Mikroplastikgehalten. Anwendung fanden die Methoden bei der Beprobung von Flaschenwasser, Waschmaschinenabläufen, dem urbanen Abwassersystem der Stadt Kaiserslautern, sowie in Oberflächengewässer. KW - Mikroplastik KW - TED-GC/MS KW - Mikroplastik-Analytik KW - Probennahme PY - 2021 VL - 14. Jahrgang IS - 3 SP - 147 EP - 152 PB - Deutschen Vereinigung für Wasserwirtschaft, Abwasser und Abfall CY - Hennef AN - OPUS4-52260 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Portela, Raquel A1 - Barbero, Francesco A1 - Breuninger, Esther A1 - Camassa, Laura Maria Azzurra A1 - Velickovic, Tanja Cirkovic A1 - Charitidis, Costas A1 - Costa, Anna A1 - Fadda, Marta A1 - Fengler, Petra A1 - Fenoglio, Ivana A1 - Giovannozzi, Andrea M. A1 - Haugen, Øyvind Pernell A1 - Kainourgios, Panagiotis A1 - von der Kammer, Frank A1 - Kirchner, Markus J. A1 - Lomax-Vogt, Madeleine A1 - Lujic, Tamara A1 - Milczewski, Frank A1 - Moussawi, Mhamad Aly A1 - Ortelli, Simona A1 - Parac-Vogt, Tatjana N. A1 - Potthoff, Annegret A1 - Reinosa, Julian J. A1 - Röschter, Sophie A1 - Sacco, Alessio A1 - Wimmer, Lukas A1 - Zanoni, Ilaria A1 - Dailey, Lea Ann T1 - Characterizing nanoplastic suspensions of increasing complexity: Inter-laboratory comparison of size measurements using dynamic light scattering N2 - Understanding the potential human health risks associated with micro- and nanoplastic exposure is currently a priority research area. Nanoplastic toxicity studies are complicated by the lack of available, well-characterized test and reference materials. Further, many nanoplastic test materials are inherently more polydisperse and heterogenous in shape compared to polystyrene beads, making accurate and representative size distribution measurements particularly challenging. The aim of this study was to conduct an inter-laboratory comparison of dynamic light scattering measurements, the most commonly used particle sizing method for nanomaterials. Using a published standard operating procedure, size measurements in water and a standardized cell culture medium (CCM) were generated for spherical, carboxy-functionalized polystyrene nanoparticles (PS-COOH; 50 nm; benchmark material), and for increasingly complex in-house produced spherical poly(ethylene terephthalate) (nanoPET) and irregular shaped polypropylene (nanoPP) test materials. The weighted mean of hydrodynamic diameters of PS-COOH dispersed in water (55 ± 5 nm) showed moderate variation between labs (coefficient of variation, CV = 8.2%) and were similar to literature reports. Measurements of nanoPET (82 ± 6 nm) and nanoPP (182 ± 12 nm) in water exhibited similar CV values (nanoPET: 7.3% and nanoPP; 6.8%). Dispersion of PS-COOH and nanoPET in CCM increased the CV to 15.1 and 14.2%, respectively, which is lower than literature reports (CV = 30%). We conclude with a series of practical recommendations for robust size measurements of nanoplastics in both water and complex media highlighting that strict adherence to a standard operating procedure is required to prevent particle agglomeration in CCM KW - Nanoplastics KW - Reference materials KW - Polypropylene PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644571 DO - https://doi.org/10.1039/d5en00645g SN - 2051-8153 SP - 1 EP - 15 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-64457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Wimmer, Lukas A1 - Alcolea-Rodriguez, Victor A1 - Waniek, Tassilo A1 - Wachtendorf, Volker A1 - Matzdorf, Kay A1 - Ciornii, Dmitri A1 - Fengler, Petra A1 - Milczewski, Frank A1 - Otazo-Aseguinolaza, Itziar A1 - Ferrer, Manuel A1 - Bañares, Miguel A. A1 - Portela, Raquel A1 - Dailey, Lea Ann T1 - Quality-by-design and current good practices for the production of test and reference materials for micro- and nano-plastic research N2 - Understanding the environmental and human health impacts of micro- and nanoplastic pollutants is currently a high priority, stimulating intensive methodological research work in the areas of sampling, sample preparation and detection as well as intensive monitoring and testing. It is challenging to identify and quantify microplastics in complex organic matrices and concepts for nanoplastic detection are still in their infancy. All analytical techniques employed in studying micro- and nanoplastics require suitable reference materials for validation measurements, with requirements as diverse as the analytical tools used, ranging from different polymer types, size distributions and shapes of the material to the concentrations employed in different experimental set ups (ng to g amounts). The aim of this manuscript is to outline current good practices for small-scale laboratory production and characterization of suitable test and reference materials. The focus is placed on top-downfragmentation methods as well as bottom-up precipitation methods. Examples using polyethylene, polypropylene, polystyrene and polyethylene terephthalate with size distribution classes of mainly 10–1000, 1–10 and <1 μm particles will be provided. Experiences and suggestions on how to produce well-characterized micro- and nano-plastics for internal research needs will ensure that studies using the materials have robust and informative outcomes. KW - Mmicroplastics KW - Nanoplastics KW - Reference materials KW - Standard validation method PY - 2025 DO - https://doi.org/10.1016/j.jhazmat.2025.139595 SN - 0304-3894 VL - 497 SP - 1 EP - 20 PB - Elsevier B.V. AN - OPUS4-63958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Amariamir, Sasan A1 - George, Janine A1 - Benner, Philipp T1 - SynCoTrain: a dual classifier PU-learning framework for synthesizability prediction N2 - Material discovery is a cornerstone of modern science, driving advancements in diverse disciplines from biomedical technology to climate solutions. Predicting synthesizability, a critical factor in realizing novel materials, remains a complex challenge due to the limitations of traditional heuristics and thermodynamic proxies. While stability metrics such as formation energy offer partial insights, they fail to account for kinetic factors and technological constraints that influence synthesis outcomes. These challenges are further compounded by the scarcity of negative data, as failed synthesis attempts are often unpublished or context-specific. We present SynCoTrain, a semi-supervised machine learning model designed to predict the synthesizability of materials. SynCoTrain employs a co-training framework leveraging two complementary graph convolutional neural networks: SchNet and ALIGNN. By iteratively exchanging predictions between classifiers, SynCoTrain mitigates model bias and enhances generalizability. Our approach uses Positive and Unlabeled (PU) learning to address the absence of explicit negative data, iteratively refining predictions through collaborative learning. The model demonstrates robust performance, achieving high recall on internal and leave-out test sets. By focusing on oxide crystals, a well-characterized material family with extensive experimental data, we establish SynCoTrain as a reliable tool for predicting synthesizability while balancing dataset variability and computational efficiency. This work highlights the potential of co-training to advance high-throughput materials discovery and generative research, offering a scalable solution to the challenge of synthesizability prediction. KW - Synthesizability KW - Accelerated Materials Design KW - Materials Acceleration Platforms KW - Materials Design KW - Materials Discovery KW - Co-training PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637907 DO - https://doi.org/10.1039/D4DD00394B SN - 2635-098X VL - 4 IS - 6 SP - 1437 EP - 1448 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Amiri, Hesam A1 - Nikookhesal, Aidin A1 - Murugan, Divagar A1 - Scholz, Stefan A1 - Frentzen, Michael A1 - Cao, Yuan A1 - Nickl, Philip A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Vu, Xuan-Thang A1 - Narayanan, Madaboosi S. A1 - Knoch, Joachim A1 - Ingebrandt, Sven A1 - Adeli, Mohsen A1 - Pachauri, Vivek T1 - High precision correlative analysis of dielectric behavior evolution and anisotropy in graphene oxide thin film as a function of thermal annealing parameters N2 - Graphene oxide (GO) and reduced graphene oxide (rGO) attract keen interest from different science and technology sectors owing to their tunable material characteristics dependent on C/O ratio. Thermal annealing in different gaseous environments serves as an effective approach to manipulate the C/O ratio in graphitic lattice, making it suitable for various electronic, optical and composites applications. Despite regular use of thermal annealing, systematic studies on dielectric properties evolution in GO against different annealing parameters remain elusive. This work reports on a reliable approach that adopts a joint Raman Spectroscopy, Mueller Matrix Spectroscopic Ellipsometry (MMSE) and high-precision electrical impedance spectroscopy (HP-EIS) framework for studying the evolution of dielectric behavior and anisotropies in GO. The experimental platform involved lithography-defined GO patterns connected to metal microelectrodes and glass passivation for protection from gaseous environments during annealing and measurements using Raman, MMSE and HP-EIS. The presented study delineates the effects of annealing parameters such as temperature, heating rate, and gaseous environment on GO permittivity. Novel findings include the discovery of a direct relationship between heating rate and dielectric properties, as well as determination of vertical limitation of MMSE for permittivity distribution characterization in GO, for the first time, to be around 8 nm. KW - Thermal annealing KW - Reduced graphene oxide KW - Thin films KW - 2D materials KW - Spectroscopic ellipsometry PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652428 DO - https://doi.org/10.1016/j.nwnano.2025.100130 SN - 2666-9781 VL - 11 SP - 1 EP - 10 PB - Elsevier Ltd. AN - OPUS4-65242 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - An, Biwen Annie A1 - Kleinbub, Sherin A1 - Özcan Sandikcioglu, Özlem A1 - Koerdt, Andrea T1 - Iron to Gas: Versatile Multiport Flow-Column Revealed Extremely High Corrosion Potential by Methanogen-Induced Microbiologically Influenced Corrosion (Mi-MIC) N2 - Currently, sulfate-reducing bacteria (SRB) is regarded as the main culprit of microbiologically influenced corrosion (MIC), mainly due to the low reported corrosion rates of other microorganisms. For example, the highest reported corrosion rate for methanogens is 0.065 mm/yr. However, by investigating methanogen-induced microbiologically influenced corrosion (Mi-MIC) using an in-house developed versatile multiport flow test column, extremely high corrosion rates were observed. We analyzed a large set of carbon steel beads, which were sectionally embedded into the test columns as substrates for iron-utilizing methanogen Methanobacterium IM1. After 14 days of operation using glass beads as fillers for section separation, the highest average corrosion rate of Methanobacterium IM1 was 0.2 mm/yr, which doubled that of Desulfovibrio ferrophilus IS5 and Desulfovibrio alaskensis 16109 investigated at the same conditions. At the most corroded region, nearly 80% of the beads lost 1% of their initial weight (fast-corrosion), resulting in an average corrosion rate of 0.2 mm/yr for Methanobacterium IM1-treated columns. When sand was used as filler material to mimic sediment conditions, average corrosion rates for Methanobacterium IM1 increased to 0.3 mm/yr (maximum 0.52 mm/yr) with over 83% of the beads having corrosion rates above 0.3 mm/yr. Scanning electron images of metal coupons extracted from the column showed methanogenic cells were clustered close to the metal surface. Methanobacterium IM1 is a hydrogenotrophic methanogen with higher affinity to metal than H2. Unlike SRB, Methanobacterium IM1 is not restricted to the availability of sulfate concentration in the environment. Thus, the use of the multiport flow column provided a new insight on the corrosion potential of methanogens, particularly in dynamic conditions, that offers new opportunities for monitoring and development of mitigation strategies. Overall, this study shows under certain conditions methanogenic archaea can cause higher corrosion than SRB, specific quantifications, i.e., maximum, average, and minimum corrosion rates can be determined, and that spatial statistical evaluations of MIC can be carried out. KW - Microbiologically influenced corrosion KW - Methanogen KW - Methane KW - Biocorrosion KW - Flow system KW - Modeling KW - Multiport PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506084 DO - https://doi.org/10.3389/fmicb.2020.00527 VL - 11 SP - Article 527 PB - Frontiers in microbiology AN - OPUS4-50608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anker, Andy S. A1 - Aspuru-Guzik, Alán A1 - Bechtel, Tim A1 - Bigi, Filippo A1 - Briling, Ksenia R. A1 - Das, Basita A1 - David, Nicholas A1 - Day, Graeme M. A1 - Deringer, Volker L. A1 - Dyer, Matthew A1 - Eardley-Brunt, Annabel A1 - Evans, Matthew L. A1 - Evans, Rob A1 - Franklin, Barnabas A. A1 - Ganose, Alex M. A1 - George, Janine A1 - Goulding, Mark A1 - Hickey, Niamh A1 - James, Gillian A1 - Kalikadien, Adarsh V. A1 - Kapil, Venkat A1 - Kulik, Heather J. A1 - Kumar, Vishank A1 - Kuttner, Christian A1 - Lam, Erwin A1 - Lederbauer, Magdalena A1 - Lou, Yuchen A1 - Martin, Jennie A1 - Marulanda Bran, Andres A1 - Mathea, Miriam A1 - Pickard, Chris J. A1 - Ruscic, Branko A1 - Ryder, Matthew R. A1 - Sabanza Gil, Victor A1 - Schwaller, Philippe A1 - Segler, Marwin H. S. A1 - Sun, Wenhao A1 - Tanovic, Sara A1 - Treyde, Wojtek A1 - Walsh, Aron A1 - Wu, Ruiqi T1 - Discovering synthesis targets: General discussion N2 - This article is a discussion of the paper "Analysis of uncertainty of neural fingerprint-based models" by Christian W. Feldmann, Jochen Sieg and Miriam Mathea (Faraday discussions, 2025, DOI: 10.1039/D4FD00095A). KW - Automation KW - Materials acceleration platforms KW - Machine learning KW - Materials design KW - Materials discovery KW - Density functional theory KW - Ab initio PY - 2025 DO - https://doi.org/10.1039/D4FD90064B SN - 1359-6640 SN - 1364-5498 VL - 256 IS - Themed collection: Data-driven discovery in the chemical sciences SP - 639 EP - 663 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-62317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anker, Andy S. A1 - Aspuru-Guzik, Alán A1 - Ben Mahmoud, Chiheb A1 - Bennett, Sophie A1 - Briling, Ksenia R. A1 - Changiarath, Arya A1 - Chong, Sanggyu A1 - Collins, Christopher M. A1 - Cooper, Andrew I. A1 - Crusius, Daniel A1 - Darmawan, Kevion K. A1 - Das, Basita A1 - David, Nicholas A1 - Day, Graeme M. A1 - Deringer, Volker L. A1 - Duarte, Fernanda A1 - Eardley-Brunt, Annabel A1 - Evans, Matthew L. A1 - Evans, Rob A1 - Fairlamb, Ian A1 - Franklin, Barnabas A. A1 - Frey, Jeremy A1 - Ganose, Alex M. A1 - Goulding, Mark A1 - Hafizi, Roohollah A1 - Hakkennes, Matthijs A1 - Hickey, Niamh A1 - James, Gillian A1 - Jelfs, Kim E. A1 - Kalikadien, Adarsh V. A1 - Kapil, Venkat A1 - Koczor-Benda, Zsuzsanna A1 - Krammer, Ferdinand A1 - Kulik, Heather J. A1 - Kumar, Vishank A1 - Kuttner, Christian A1 - Lam, Erwin A1 - Lou, Yuchen A1 - Mante, Eltjo A1 - Martin, Jennie A1 - Mroz, Austin M. A1 - Nematiaram, Tahereh A1 - Pare, Charles W. P. A1 - Patra, Sarbani A1 - Proudfoot, James A1 - Ruscic, Branko A1 - Ryder, Matthew R. A1 - Sakaushi, Ken A1 - Saßmannshausen, Jörg A1 - Savoie, Brett M. A1 - Schneider, Nadine A1 - Schwaller, Philippe A1 - Skjelstad, Bastian Bjerkem A1 - Sun, Wenhao A1 - Szczypiński, Filip T. A1 - Torrisi, Steven A1 - Ueltzen, Katharina A1 - Vishnoi, Shubham A1 - Walsh, Aron A1 - Wang, Xinwei A1 - Wilson, Chloe A1 - Wu, Ruiqi A1 - Zeitler, Jakob T1 - Discovering structure–property correlations: General discussion N2 - This article is a discussion of the paper "Web-BO: Towards increased accessibility of Bayesian optimisation (BO) for chemistry" by Austin M. Mroz, Piotr N. Toka, Ehecatl Antonio del Río Chanona and Kim E. Jelfs (Faraday discussions, 2025, 256, 221-234). KW - Materials design KW - Machine learning KW - Automation KW - Materials discovery PY - 2025 DO - https://doi.org/10.1039/d4fd90062f SN - 1359-6640 SN - 1364-5498 VL - 256 IS - Themed collection: Data-driven discovery in the chemical sciences SP - 373 EP - 412 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-62208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ankli, P. P. A1 - Abdelwahab, A. A. A1 - Logachov, A. A1 - Bugiel, R. A1 - Drobne, D. A1 - Novak, S. A1 - Kranjc, E. A1 - Saje, S. A1 - Pellegrino, F. A1 - Alladio, E. A1 - Sordello, F. A1 - Corrao, E. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg A1 - Mrkwitschka, Paul A1 - Madbouly, Loay Akmaal A1 - Akdemir, Yücel A1 - Gulumian, M. A1 - Wepener, V. A1 - Andraos, C. A1 - Boodhia, K. A1 - Jones, E. A1 - Doolin, A. A1 - Leuchtenberg, K. A1 - Valsami Jones, E. A1 - Rocca, C. A1 - Ibrahim, B. A1 - Singh, D. A1 - Chakraborty, S. A1 - Jurkschat, K. A1 - Johnston, C. A1 - Van Der Zande, M. A1 - Fernandez, D. A1 - Queipo, P. A1 - Clifford, C. A1 - Hardy, B. T1 - Knowledge Infrastructure supporting image-based characterisation of 2D graphene materials N2 - As part of the European Horizon ACCORDs project, advanced methods are being developed for the image-based characterisation of 2D nanomaterials. Given the complexity of this task, robust nd wellorganised data management is critical to ensuring high-quality outcomes. To support this, we have established a knowledge infrastructure that serves as the central repository for protocols, images and experimental data which are stored in a standardised, harmonised manner and in accordance with the FAIR principles – Findable, Accessible, Interoperable and Reusable and open science. This machine-readable framework enables the systematic and computationally automated correlation of image features with experimental descriptors, facilitating accurate material characterisation and transparent reporting which is all integrated in the ACCORDs KI. KW - Graphene-related 2D materials (GR2M) KW - 2D materials KW - Knowledge infrastructure KW - Characterisation PY - 2025 DO - https://doi.org/10.1016/j.toxlet.2025.07.660 SN - 0378-4274 VL - 411 SP - S281 EP - S282 PB - Elsevier B.V. AN - OPUS4-65061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ankli, P.P. A1 - Ali, A. A1 - Hodzic, S. A1 - Logachov, A. A1 - Maciejczuk, K. A1 - Milochiv, A. A1 - Hardy, S. A1 - Hardy, B. A1 - Novak, S. A1 - Kranjc, E. A1 - Kononenko, V. A1 - Saje, S. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg A1 - Akmal, Loay A1 - Mrkwitschka, Paul A1 - Pellegrino, F. A1 - Rossi, A. A1 - Alladio, E. A1 - Sordello, F. A1 - Gulumian, M. A1 - Valsami-Jones, E. A1 - Andraos, C. A1 - Wepener, V. A1 - Jurkschat, K. A1 - Jones, E. A1 - Singh, D. A1 - Ibrahim, B. A1 - van der Zande, M. A1 - Fernandez-Poulussen, D. A1 - Queipo, P. A1 - Drobne, D. T1 - Data management for image-based characterisation of 2D nano-materials N2 - The ACCORDs project, funded through Horizon Europe, is pioneering a novel approach to investigate Graphene Family Materials (GFMs) through image analysis. Our aim is to unveil how these materials might influence health and the environment. To achieve this, we are developing a platform designed for the easy retrieval, access, sharing, and utilisation of GFM data and the coordination between biological and physico-chemical data formats. Integral to this platform is an OMERO-based library for image storage, alongside data collection forms and image analysis tools. Efforts are underway to streamline the process for researchers to upload and disseminate their findings, manage information within a database and navigate the data with ease. Adhering to REMBI guidelines, which set the standard for annotating biological images with metadata, we ensure our data collection is comprehensive and adheres to established best practices. Initially, we are employing thresholding and basic machine learning techniques for image segmentation, laying the groundwork for advanced analysis through deep learning to gain more profound insights. Upon completion, the project will deliver a comprehensive platform facilitating efficient data and image management concerning GFMs. This platform will enable the straightforward discovery and use of protocols and results, all organised in accordance with the FAIR principles – Findable, Accessible, Interoperable, and Reusable. This initiative is poised to significantly impact materials science, enhancing our comprehension of the safety and environmental implications of 2D materials. KW - Graphene KW - Image analysis KW - Data management PY - 2024 DO - https://doi.org/10.1016/j.toxlet.2024.07.655 VL - 399 SP - S271 PB - Elsevier B.V. AN - OPUS4-61011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Appel, Paul Alexander A1 - Prinz, Carsten A1 - Low, Jian Liang A1 - Asres, Nahom Enkubahri A1 - Wu, Shu-Han A1 - Freytag, Annica A1 - Krug von Nidda, Jonas A1 - de Sousa Amadeu, Nader A1 - Fellinger, Tim-Patrick T1 - Kern–Schale: Versiegelung nanoporöser Partikel mit semipermeablen Kohlenstoffschichten befreit Hartkohlenstoffanoden von ihrem Dilemma N2 - In der vorliegenden Arbeit wird eine Kern-Schale-Strategie vorgestellt, die das grundlegende Problem gängiger nichtgraphitischer Hartkohlenstoff-Anoden adressiert: Hohe reversible Kapazitäten gehen bislang typischerweise mit erheblichen irreversiblen Verlusten in den ersten Zyklen einher. Analog zu Graphit, das sowohl Lithiumspeicherung als auch die Abtrennung von Elektrolytlösungsmitteln in einer homogenen Struktur vereint, zeigen wir, dass sich diese beiden Funktionen auch in nichtgraphitischen Kohlenstoffen gezielt in einer heterogenen Architektur kombinieren lassen. Hochporöse Aktivkohlen werden durch kinetisch kontrollierte Gasphasenabscheidung mit einer dünnen Schicht nichtgraphitischen Kohlenstoffs überzogen, sodass eine funktionale Kern-Schale-Struktur entsteht. Gasadsorptionsmessungen an Kern-, Schalen-, Kern-Schale- und mechanisch beschädigte Kern-Schale-Partikeln, bestätigen, dass die Porosität des Kerns erhalten bleibt und die Schale semipermeabel ist. Die Sorption von Diethylcarbonat wird als geeignetere Methode im Vergleich zu N2- oder CO2-Sorptionsmessungen eingeführt, um die irreversiblen Verluste des ersten Zyklus mit der tatsächlichen Flüssig-Fest-Grenzfläche von Kohlenstoffanoden zu verknüpfen. Die funktionalen Kern-Schale-Partikel zeigen eine stark reduzierte Aufnahme von Diethylcarbonat, was hohe reversible Kapazitäten bei deutlich geringeren Erstzyklusverlusten ermöglicht. Bei einer reversiblen Kapazität von 400 ± 24 mAh g−1 und einer initialen Coulombeffizienz von 82 ± 2% zeigt sich, dass die dreistufige Natriumspeicherung in der gezielt entwickelten Kern-Schale-Architektur den größeren Ionenradius von Natrium gegenüber Lithium (372 mAh g−1 in Graphit) kompensieren kann. Die entwickelten Kern-Schale-Anoden erreichen damit ein Leistungsniveau, das für eine kommerzielle Anwendung vielversprechend ist. KW - Kern-Schale-Struktur KW - Natriumionenbatterie KW - Hartkohlenstoffanode KW - Diethylcarbonatdampfsorption KW - Aktivkohle PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655354 DO - https://doi.org/10.1002/ange.202519457 SN - 1521-3757 N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-65535 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Appel, Paul Alexander A1 - Prinz, Carsten A1 - Low, Jian Liang A1 - Asres, Nahom Enkubahri A1 - Wu, Shu-Han A1 - Freytag, Annica A1 - Krug von Nidda, Jonas A1 - de Sousa Amadeu, Nader A1 - Fellinger, Tim-Patrick T1 - Core‐Shell: Resolving the Dilemma of Hard Carbon Anodes by Sealing Nanoporous Particles With Semi‐Permeable Coatings N2 - A core-shell strategy is introduced to overcome the dilemma of common non-graphitic hard carbon anodes, linking high reversible storage capacity to practically unacceptable irreversible losses in the first cycle(s). Just as Graphite homogeneously combines effective lithium storage with an electrolyte solvent-sieving function, we show that both of these functions could be strategically integrated into non-graphitic carbons in a heterogeneous structure. Highly porous activated carbons are sealed by kinetically tuned gas-phase deposition of non-graphitic carbon to form a functional core-shell structure. Gas sorption porosimetry on core, shell, core–shell, and cracked core-shell particles confirms preserved core porosity and a semi-permeable shell. Diethyl carbonate sorption analysis is introduced as a more suitable probe than N2 or CO2 sorption, linking first-cycle losses to the liquid–solid interface of carbon anodes. The functional core-shell particles with much reduced diethyl carbonate uptake allow for high storage capacity and reduced first cycle losses. Delivering 400 ± 24 mAh g−1 with 82 ± 2% first-cycle reversibility, it is shown that three-stage Na storage in designed core-shell anodes can compensate for the larger size of sodium compared to lithium stored in graphite anodes (372 mAh g−1). The designed core-shell anodes show state-of-the-art performance with commercial promise. KW - Sodium-ion battery KW - Activated carbon KW - Core-shell KW - Hard carbon anode KW - Diethyl carbonate vapor sorption PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655346 DO - https://doi.org/10.1002/anie.202519457 SN - 1433-7851 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-65534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aratsu, K. A1 - Takeya, R. A1 - Pauw, Brian Richard A1 - Hollamby, M.J. A1 - Kitamoto, Y. A1 - Shimizu, N. A1 - Takagi, H. A1 - Haruki, R. A1 - Adachi, S. A1 - Yagai, S. T1 - Supramolecular copolymerization driven by integrative self-sorting of hydrogen-bonded rosettes N2 - Molecular recognition to preorganize noncovalently polymerizable supramolecular complexes is a characteristic process of natural supramolecular polymers, and such recognition processes allow for dynamic self-alteration, yielding complex polymer systems with extraordinarily high efficiency in their targeted function. We herein show an example of such molecular recognition-controlled kinetic assembly/disassembly processes within artificial supramolecular polymer systems using six-membered hydrogen-bonded supramolecular complexes (rosettes). Electron-rich and poor monomers are prepared that kinetically coassemble through a temperature-controlled protocol into amorphous coaggregates comprising a diverse mixture of rosettes. Over days, the electrostatic interaction between two monomers induces an integrative self-sorting of rosettes. While the electron-rich monomer inherently forms toroidal homopolymers, the additional electrostatic interaction that can also guide rosette association allows helicoidal growth of supramolecular copolymers that are comprised of an alternating array of two monomers. Upon heating, the helicoidal copolymers undergo a catastrophic transition into amorphous coaggregates via entropy-driven randomization of the monomers in the rosette. KW - Self-assembly KW - Coaggregation KW - Scattering KW - Simulation KW - AFM PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506555 DO - https://doi.org/10.1038/s41467-020-15422-6 VL - 11 IS - 1 SP - Article number: 1623 PB - Springer Nature AN - OPUS4-50655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aree, T. A1 - McMonagle, C. J. A1 - Michalchuk, Adam A1 - Chernyshov, D. T1 - Low-frequency lattice vibrations from atomic displacement parameters of a-FOX-7, a high energy density material N2 - Highly anharmonic thermal vibrations may serve as a source of structural instabilities resulting in phase transitions, chemical reactions and even the mechanical disintegration of a material. Ab initio calculations model thermal motion within a harmonic or sometimes quasi-harmonic approximation and must be complimented by experimental data on temperature-dependent vibrational frequencies. Here multi-temperature atomic displacement parameters (ADPs), derived from a single-crystal synchrotron diffraction experiment, are used to characterize low-frequency lattice vibrations in the alpha-FOX-7 layered structure. It is shown that despite the limited quality of the data, the extracted frequencies are reasonably close to those derived from inelastic scattering, Raman measurements and density functional theory (DFT) calculations. Vibrational anharmonicity is parameterized by the Grüneisen parameters, which are found to be very different for in-layer and out-of-layer vibrations. KW - Energetic Materials KW - DFT KW - Structural dynamics KW - X-ray diffraction PY - 2022 DO - https://doi.org/10.1107/S2052520622002700 SN - 2052-5206 VL - 78 SP - 376 EP - 384 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-54832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arinchtein, A. A1 - Schnack, R. A1 - Kraffert, K. A1 - Radnik, Jörg A1 - Dietrich, P. A1 - Sachse, René A1 - Krähnert, R. T1 - Role of Water in Phase Transformations and Crystallization of Ferrihydrite and Hematite N2 - The oxides, hydroxides, and oxo-hydroxides of iron belong to the most abundant materials on earth. They also feature a wide range of practical applications. In many environments, they can undergo facile phase transformations and crystallization processes. Water appears to play a critical role in many of these processes. Despite numerous attempts, the role of water has not been fully revealed yet. We present a new approach to study the influence of water in the crystallization and phase transformations of iron oxides. The approach employs model-type iron oxide films that comprise a defined homogeneous nanostructure. The films are exposed to air containing different amounts of water reaching up to pressures of 10 bar. Ex situ analysis via scanning electron microscopy, Transmission electron microscopy, selected area electron diffraction, and X-ray diffraction is combined with operando near-ambient pressure X-ray photoelectron spectroscopy to follow water-induced changes in hematite nd ferrihydrite. Water proves to be critical for the nucleation of ematite domains in ferrihydrite, the resulting crystallite orientation, and the underlying crystallization mechanism. KW - Iron oxide KW - Ferrihydrite KW - Hematite KW - Water KW - NAP-XPS KW - High pressure PY - 2020 DO - https://doi.org/10.1021/acsami.0c05253 VL - 12 SP - 38714 EP - 38722 PB - ACS Publication AN - OPUS4-51201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arinchtein, A. A1 - Ye, M.-Y. A1 - Yang, Q. A1 - Kreyenschulte, C. A1 - Wagner, Andreas A1 - Frisch, M. A1 - Brückner, A. A1 - Kondratenko, E. A1 - Kraehnert, R. T1 - Dynamics of Reaction-Induced Changes of Model-Type Iron Oxide Phases in the CO2-Fischer-Tropsch-Synthesis N2 - Iron-based catalysts are employed in CO2-FTS due to their ability to convert CO2 into CO in a first step and their selectivity towards higher hydrocarbons in a second CO hydrogenation step. According to the literature, iron carbides represent the active phase for hydrocarbon formation and are claimed to emerge in the presence of CO. We propose nanostructured FeOx films as model systems to assess information about the complex phase transformations during CO2-FTS. Mesoporous hematite, ferrihydrite, maghemite, maghemite/magnetite films were exposed to CO2-FTS atmospheres at 20 bar and 300°C. Up to three distinct phases were observed depending on the timeon-stream (TOS): a sintered maghemite/magnetite phase, a carbidic core-shell structure, and a low-crystalline, needle-type oxide phase. Our findings indicate that the formation of an intermediary maghemite/magnetite phase, predominant after short TOS (30 h), precedes the evolution of the carbide phase. Yet, even after prolonged TOS (185 h), no full conversion into a bulk carbide is observed. KW - Nanostructured FeOx films KW - CO2 KW - Scanning Auger Spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549709 DO - https://doi.org/10.1002/cctc.202200240 SN - 1867-3880 VL - 14 IS - 14 SP - 1 EP - 11 PB - Wiley-VCH AN - OPUS4-54970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arnold, M. A1 - Katzmann, J. A1 - Naik, Aakash A1 - Görne, A. L. A1 - Härtling, Thomas A1 - George, Janine A1 - Schuster, C. T1 - Investigations on electron beam irradiated rare-earth doped SrF2 for application as low fading dosimeter material: Evidence for and DFT simulation of a radiation-induced phase N2 - A recent approach to measure electron radiation doses in the kGy range is the use of phosphors with an irradiation dose-dependent luminescence decay time. However, the applicability of the previously investigated material NaYF4:Yb3+,Er3+ is limited as it shows pronounced fading. Therefore, in this work, a modified SrF2 synthesis is presented that results in SrF2 nanoparticles codoped with Yb and either Er, Hm, or Tm. To assess their suitability as dosimeter material, dose response, as well as its degree of fading over 50 up to 140 days after irradiation were measured. Fading rates as small as 5% in SrF2:Er,Yb and 4% in SrF2:Ho,Yb were derived, which are comparable to established dosimeter materials. A combination of spectroscopy, diffraction and DFT calculations was used to elucidate the effect of irradiation, pointing towards the formation of a secondary phase of Yb2+ that we predict could be Yb2OF2. This irreversible formation of a secondary phase is considered to be the explanation for the low fading behavior in SrF2-based phosphors compared to NaYF4:Yb, Er, a highly attractive feature for electron beam dosimetry. KW - DFT KW - Structure prediction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554115 DO - https://doi.org/10.1039/D2TC01773C SN - 2050-7526 VL - 10 IS - 32 SP - 11579 EP - 11587 PB - RSC CY - London AN - OPUS4-55411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asanova, T.I. A1 - Asanov, Igor A1 - Yusenko, Kirill A1 - Le Fontane, Camille A1 - Gerasimov, E.Y. A1 - Zadesenetz, A.V. A1 - Korenev, S.V. T1 - Time-resolved study of Pd-Os and Pt-Os nanoalloys formation through thermal decomposition of Pd(NH3)(4) OsCl6 and Pt(NH3)(4) OsCl6 complex salts N2 - The formation mechanisms of Pd-Os and Pt-Os alloys in the course of thermal decomposition of iso-formular and isostructural complex salts [Pd(NH3)4][OsCl6] and [Pt(NH3)4][OsCl6] in an inert atmosphere have been studied by in-situ QXAFS, XPS and PXRD. The mechanisms of thermal decomposition of the precursors are found to differ from each other, but the detected intermediate products show no significant effect on the local atomic structure around Os, Pt/Pd in their final products. A crystalline beta-trans-[Pd(NH3)2Cl2] intermediate of the first step of thermal decomposition of [Pd(NH3)4][OsCl6] makes the anion [OsCl6]2− transform differently than that of [Pt(NH3)4][OsCl6]. It transforms into a short-lived [Os(NH3)xCl6-x] (2≤x≤4), and then to a distorted octahedron [OsCl6]2−, similar to the high-temperature modification of OsCl4. In case of [Pt(NH3)4][OsCl6], the intermediate [Os(NH3)2Cl4] modifies into four chlorine coordinated Os,{OsCl4}0/1−. Consecutive reduction of Pd(II)/Pt(II) and Os(IV) to the metals defines the homophilic atomic order with the fcc-Pd covered by a random Pd-Os alloy layer and Os on the surface, that is supported by High-Resolution Transmission Electron Mictroscopy (HRTEM) and Scanning TEM (STEM) energy dispersive X-ray (EDX) data, and the diffusion direction going from the surface (hcp-Os) to bulk (fcc-Pd/Pt). As a result, the heterogeneous alloys are formed with a very similar electronic and local atomic structure of Os and Pd/Pt. Upon alloying, the Os 5d5/2,3/2 and Pt 5d5/2,3/2 levels are depleted in the Pt-Os alloys compared to dispersed hcp-Os, fcc-Pt, and Pt foil. This is an unusual behaviour for Os and Pt, calling into question the versatility of d-band theory in bimetallic Os-alloys. The spin-orbit effect at the Os site has been found for both the Pd-Os and Pt-Os alloys, but it is about 4 times less compared to the complex salts. The obtained values for the complex compounds are comparable with those for the iridates, proposed as materials with spin-orbit-induced properties. KW - Thermal decomposition KW - Quick-EXAFS PY - 2021 DO - https://doi.org/10.1016/j.materresbull.2021.111511 VL - 144 SP - 111511 PB - Elsevier Ltd. AN - OPUS4-54010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Atila, Achraf A1 - Bakhouch, Yasser A1 - Xie, Zhuocheng T1 - Revealing the void-size distribution of silica glass using persistent homology N2 - Oxide glasses have proven to be useful across a wide range of technological applications. Nevertheless, their medium-range structure has remained elusive. Previous studies focused on ring statistics as a metric of the medium-range structure, but this metric provides an incomplete picture of the glassy structure. Here, we use atomistic simulations and state-of-the-art topological analysis tools, namely persistent homology (PH), to analyze the medium-range structure of the archetypal oxide glass (Silica) at ambient temperatures and with varying pressures. PH presents an unbiased definition of loops and voids, providing an advantage over other methods for studying the structure and topology of complex materials, such as glasses, across multiple length scales. We captured subtle topological transitions in medium-range order and cavity distributions, providing new insights into glass structure. Our work provides a robust way for extracting the void distribution of oxide glasses based on PH. KW - Medium-range KW - Voids KW - Topology KW - Silica glass KW - Atomistic simulations KW - Persistent homology PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655690 DO - https://doi.org/10.1016/j.mtla.2025.102613 VL - 44 SP - 1 EP - 11 PB - Elsevier Inc. AN - OPUS4-65569 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ayerdi, J. J. A1 - Aginagalde, A. A1 - Llavori, I. A1 - Bonse, Jörn A1 - Spaltmann, Dirk A1 - Zabala, A. T1 - Ball-on-flat linear reciprocating tests: Critical assessment of wear volume determination methods and suggested improvements for ASTM N2 - In the present work it was shown the importance of the correct selection, implementation, and reporting of wear volume computation method and quanitifies the potential errors. KW - Wear KW - Sliding KW - Surface KW - Analysis KW - ASTM KW - D7755-11 PY - 2021 DO - https://doi.org/10.1016/j.wear.2021.203620 VL - 470-471 SP - 3620 AN - OPUS4-52080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Babutzka, Martin A1 - Grabowski, Sven A1 - Sahrhage, H. A1 - Lampke, T. T1 - Electrochemical corrosion investigations on binary and ternary zinc alloy coatings using gel electrolytes N2 - Novel agar-based test electrolytes are used to perform electrochemical corrosion investigations on ZnFe and ZnNi binary as well as ZnFeMo ternary zinc coatings. The objectives of the electrochemical investigations include the characterization of the corrosion behavior, the description of the protective effect of the coatings as well as the investigation of the layer formation and degradation under artificial aging. ZnFe and ZnFeMo coatings are applied with varying iron content as well as an additional passivation layer, respectively, to study the effect on corrosion resistance. The results show that the protective effect of the coatings is not negatively influenced by different iron contents or the addition of molybdenum. Additional passivation of the ZnFe-containing coatings by means of a passivating agent leads to a significant improvement in the protective effect. Artificial aging leads to slight degradation of the additional passivation layer whereas coatings without post-treatment enhance their protective effect by the formation of corrosion product layers. KW - Binary zinc alloys KW - Ternary zinc alloys KW - Corrosion testing KW - Gel electrolytes KW - Corrosion PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543013 DO - https://doi.org/10.1002/adem.202101336 SN - 1438-1656 SP - 1 EP - 14 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baláž, M. A1 - Tešinský, M. A1 - Marquardt, Julien A1 - Škrobian, M. A1 - Daneu, N. A1 - Rajňák, M. A1 - Baláž, P. T1 - Synthesis of copper nanoparticles from refractory sulfides using a semi-industrial mechanochemical approach N2 - The large-scale mechanochemical reduction of binary sulfides chalcocite (Cu2S) and covellite (CuS) by elemental iron was investigated in this work. The reduction of Cu2S was almost complete after 360 min of milling, whereas in the case of CuS, a significant amount of non-reacted elemental iron could still be identified after 480 min. Upon application of more effective laboratory-scale planetary ball milling, it was possible to reach almost complete reduction of CuS. Longer milling leads to the formation of ternary sulfides and oxidation product, namely cuprospinel CuFe2O4. The rate constant calculated from the magnetometry measurements using a diffusion model for Cu2S and CuS reduction by iron in a large-scale mill is 0.056 min−0.5 and 0.037 min−0.5, respectively, whereas for the CuS reduction in a laboratory-scale mill, it is 0.1477 min−1. The nanocrystalline character of the samples was confirmed by TEM and XRD, as the produced Cu exhibited sizes up to 16 nm in all cases. The process can be easily scaled up and thus copper can be obtained much easier from refractory minerals than in traditional metallurgical approaches. KW - Mechanochemistry KW - Copper sulfides KW - Copper nanoparticles KW - Magnetometry KW - Oxidation PY - 2020 DO - https://doi.org/10.1016/j.apt.2019.11.032 VL - 31 IS - 2 SP - 782 EP - 791 PB - Elsevier B.V. AN - OPUS4-50665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baláž, Matej A1 - Birinci, Mustafa A1 - Şentürk, Kader A1 - Achimovičová, Marcela A1 - Baláž, Peter A1 - Tampubolon, Imelda Octa A1 - Stolar, Tomislav A1 - Bienert, Ralf A1 - Emmerling, Franziska A1 - Erdemoğlu, Sema A1 - Sis, Hikmet A1 - Erdemoğlu, Murat T1 - Utilizing Taguchi method and in situ X-ray powder diffraction monitoring to determine the influence of mechanical activation conditions on the physico-chemical properties and Al leachability of K-feldspar N2 - K-feldspar represents an important natural resource of potassium and aluminum. Within the framework of this study, the K-feldspar was mechanically activated in a planetary ball mill under different conditions planned according to 43 Taguchi orthogonal array experimental design. As outputs, specific surface area (SBET), median particle size (d50), amorphization degree of mineral phases , and Al recovery were used. It was found that the initial d50 value of 293 μm could be reduced to 6.7 μm and the SBET value of 4.7 m2/g could be increased up to 32.5 m2/g upon milling. Both microcline KAl3SiO8, and albite NaAl3SiO8 could be almost completely amorphized, whereas quartz SiO2 still maintained some crystallinity even under the most intensive conditions. Increasing SBET and decreasing the d50 values did not lead to a significant improvement in Al leach recovery, whereas a clear relationship between the amorphization of microcline and the recovered aluminum was found. Analysis of Variance (ANOVA) showed that increasing ball-to-powder ratio is the most beneficial for the improvement in Al recovery. In situ powder X-ray diffraction monitoring performed in an oscillation ball mill under synchrotron irradiation has shown very rapid amorphization of microcline phase at the beginning. However, amorphization of microcline was only partial after two hours of the treatment in this mill, apart from almost complete process in the planetary ball mill. In the end, regressions for the calculation of Al recovery by knowing the values of input parameters were calculated. In general, by just using mechanical activation without the subsequent roasting process that is commonly used to boost metal recoveries, it was possible to quantitatively recover aluminum from K-feldspar. KW - Mechanochemistry KW - Mechanical activation KW - Design of experiments PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611059 DO - https://doi.org/10.1016/j.jmrt.2024.08.156 SN - 2238-7854 VL - 32 SP - 3886 EP - 3895 PB - Elsevier B.V. AN - OPUS4-61105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartczak, Dorota A1 - Sikora, Aneta A1 - Goenaga-Infante, Heidi A1 - Altmann, Korinna A1 - Drexel, Roland A1 - Meier, Florian A1 - Alasonati, Enrica A1 - Lelong, Marc A1 - Cado, Florence A1 - Chivas-Joly, Carine A1 - Fadda, Marta A1 - Sacco, Alessio A1 - Rossi, Andrea Mario A1 - Pröfrock, Daniel A1 - Wippermann, Dominik A1 - Barbero, Francesco A1 - Fenoglio, Ivana A1 - Booth, Andy M. A1 - Sørensen, Lisbet A1 - Igartua, Amaia A1 - Wouters, Charlotte A1 - Mast, Jan A1 - Barbaresi, Marta A1 - Rossi, Francesca A1 - Piergiovanni, Maurizio A1 - Mattarozzi, Monica A1 - Careri, Maria A1 - Caebergs, Thierry A1 - Piette, Anne-Sophie A1 - Parot, Jeremie A1 - Giovannozzi, Andrea Mario T1 - Multiparameter characterisation of a nano-polypropylene representative test material with fractionation, light scattering, high-resolution microscopy, spectroscopy, and spectrometry methods N2 - Reference and quality control materials with comparable physicochemical properties to nanoplastic contaminants present in environmental and food nanoplastics are currently lacking. Here we report a nanoplastic polypropylene material prepared using a top-down approach involving mechanical fragmentation of larger plastics. The material was found to be homogeneous and stable in suspension and has been characterised for average particle size, size distribution range, particle number concentration, polypropylene mass fraction and inorganic impurity Content using a wide range of analytical methods, including AF4, cFFF, PTA, (MA)DLS, MALS, SEM, AFM, TEM, STEM, EDS,Raman, ICP-MS and pyGC-MS. The material was found to have a broad size distribution, ranging from 50 nm to over 200 nm, with the average particle size value dependent on the technique used to determine it. Particle number concentration ranged from 1.7–2.4 × 1010 g−1 , according to PTA. Spectroscopy techniques confirmed that the material was polypropylene, with evidence of aging due to an increased level of oxidation. The measured mass fraction was found to depend on the marker used and ranged between 3 and 5 μg g−1 . Inorganic impurities such as Si, Al, Mg, K, Na, S, Fe, Cl and Ca were also identified at ng g−1 levels. Comparability and complementarity across the measurement methods and techniques is also discussed. KW - Polypropylene KW - Nanoplastics KW - Analytics KW - Reference material KW - Scattering methods PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654680 DO - https://doi.org/10.1039/D5EN00917K SN - 2051-8153 SP - 1 EP - 15 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batatia, Ilyes A1 - Benner, Philipp A1 - Chiang, Yuan A1 - Elena, Alin M. A1 - Kovács, Dávid P. A1 - Riebesell, Janosh A1 - Advincula, Xavier R. A1 - Asta, Mark A1 - Avaylon, Matthew A1 - Baldwin, William J. A1 - Berger, Fabian A1 - Bernstein, Noam A1 - Bhowmik, Arghya A1 - Bigi, Filippo A1 - Blau, Samuel M. A1 - Cărare, Vlad A1 - Ceriotti, Michele A1 - Chong, Sanggyu A1 - Darby, James P. A1 - De, Sandip A1 - Della Pia, Flaviano A1 - Deringer, Volker L. A1 - Elijošius, Rokas A1 - El-Machachi, Zakariya A1 - Fako, Edvin A1 - Falcioni, Fabio A1 - Ferrari, Andrea C. A1 - Gardner, John L. A. A1 - Gawkowski, Mikołaj J. A1 - Genreith-Schriever, Annalena A1 - George, Janine A1 - Goodall, Rhys E. A. A1 - Grandel, Jonas A1 - Grey, Clare P. A1 - Grigorev, Petr A1 - Han, Shuang A1 - Handley, Will A1 - Heenen, Hendrik H. A1 - Hermansson, Kersti A1 - Ho, Cheuk Hin A1 - Hofmann, Stephan A1 - Holm, Christian A1 - Jaafar, Jad A1 - Jakob, Konstantin S. A1 - Jung, Hyunwook A1 - Kapil, Venkat A1 - Kaplan, Aaron D. A1 - Karimitari, Nima A1 - Naik, Aakash A. A1 - Csányi, Gábor T1 - A foundation model for atomistic materials chemistry N2 - Atomistic simulations of matter, especially those that leverage first-principles (ab initio) electronic structure theory, provide a microscopic view of the world, underpinning much of our understanding of chemistry and materials science. Over the last decade or so, machine-learned force fields have transformed atomistic modeling by enabling simulations of ab initio quality over unprecedented time and length scales. However, early machine-learning (ML) force fields have largely been limited by (i) the substantial computational and human effort required to develop and validate potentials for each particular system of interest and (ii) a general lack of transferability from one chemical system to the next. Here, we show that it is possible to create a general-purpose atomistic ML model, trained on a public dataset of moderate size, that is capable of running stable molecular dynamics for a wide range of molecules and materials. We demonstrate the power of the MACE-MP-0 model—and its qualitative and at times quantitative accuracy—on a diverse set of problems in the physical sciences, including properties of solids, liquids, gases, chemical reactions, interfaces, and even the dynamics of a small protein. The model can be applied out of the box as a starting or “foundation” model for any atomistic system of interest and, when desired, can be fine-tuned on just a handful of application-specific data points to reach ab initio accuracy. Establishing that a stable force-field model can cover almost all materials changes atomistic modeling in a fundamental way: experienced users obtain reliable results much faster, and beginners face a lower barrier to entry. Foundation models thus represent a step toward democratizing the revolution in atomic-scale modeling that has been brought about by ML force fields. KW - Materials Design KW - Thermal Conducitivity KW - Nanoparticles KW - Batteries PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647829 DO - https://doi.org/10.1063/5.0297006 SN - 0021-9606 VL - 163 IS - 18 SP - 1 EP - 89 PB - AIP Publishing AN - OPUS4-64782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batteas, James A1 - Blank, Kerstin G. A1 - Colacino, Evelina A1 - Emmerling, Franziska A1 - Friščić, Tomislav A1 - Mack, James A1 - Moore, Jeffrey A1 - Rivas, Maria Elena A1 - Tysoe, Wilfred T1 - Moving mechanochemistry forward N2 - Arguably mechanochemistry is one of the oldest, and at the same time one of the newest, areas of chemistry. One of the oldest, because it has been theorized that early hominids were able to develop rapidly due to their ability to heat and mechanically process their food to make it easier to digest. Old, because the ancient Greeks knew that mechanically activating stones (consisting of cinnabar) with vinegar in a copper pestle and mortar caused them to convert into mercury. We might be forgiven for thinking that this could have led our alchemical forbears to wonder if there were other stones that might also be persuaded to convert into gold. Early chemical luminaries such as Michael Faraday and Wilhelm Röntgen dabbled in mechanochemistry. However, in the late 19th and early 20th centuries, the field developed separately in many areas. Perhaps most significantly, synthetic chemists realized that reactions could be carried out with surprisingly high yields and selectivities by shaking them in a ball mill, and that they could even make novel compounds that their colleagues just using heat were not able to. Physicists were mechanically rearranging atoms into new configurations (i.e., doing chemistry) using exotic means such as atomic force microscope tips and optical tweezers. Scientists and engineers studying the formation of lubricious and anti-wear films realized that they were mechanochemically formed. Biochemists found molecular motor proteins, such as myosin and kinesin, that were able to convert chemical energy into motion or, vice versa, mechanical energy into the biochemical energy storage molecule adenosine triphosphate. In 2023, this confluence of advances convinced the Royal Society of Chemistry that the time was ripe to establish a new journal dedicated to the field of mechanochemistry. It is rare that a journal has the privilege of helping to create a new sub-branch of chemistry but, having done so, it has the obligation of helping to define the field and, optimistically, suggesting how the field might develop. This editorial has two major goals. The first is to bring to the attention of the scientific community the challenges faced by the field to set people thinking about how they might contribute and, second, to form the basis for more thorough discussions in the future. The sub-topics below outline current thoughts brought forward from members of our editorial board. We lay out areas and topics here with the intent of establishing a new editorial series, which we invite the community to contribute to, and outline topics and hopefully lay out challenges, which will enable us as a community to come together to move mechanochemistry forward. KW - Mechanochemistry PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646086 DO - https://doi.org/10.1039/d4mr90021a SN - 2976-8683 VL - 2 IS - 1 SP - 10 EP - 19 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Battig, Alexander A1 - Müller, Patrick A1 - Bertin, Annabelle A1 - Schartel, Bernhard T1 - Hyperbranched Rigid Aromatic Phosphorus-Containing Flame Retardants for Epoxy Resins N2 - A rigid aromatic phosphorus-containing hyperbranched flame retardant structure is synthesized from 10-(2,5 dihydroxyphenyl)-10H-9-oxa- 10-phosphaphenanthrene-10-oxide (DOPO-HQ), tris(4-hydroxyphenyl)phosphine oxide (THPPO), and 1,4-terephthaloyl chloride (TPC). The resulting poly-(DOPO-HQ/THPPO-terephthalate) (PDTT) is implemented as a flame retardant into an epoxy resin (EP) at a 10 wt% loading. The effects on EP are compared with those of the monomer DOPO-HQ and triphenylphosphine oxide (OPPh3) as low molar mass flame retardants. The glass transition temperature, thermal decomposition, flammability (reaction to small flame), and burning behavior of the thermosets are investigated using differential scanning calorimetry, thermogravimetric analysis, pyrolysis combustion flow calorimetry, UL 94-burning chamber testing, and cone calorimeter measurements. Although P-contents are low at only 0.6 wt%, the study aims not at attaining V-0, but at presenting a proof of principle: Epoxy resinswith PDTT show promising fire performance, exhibiting a 25% reduction in total heat evolved (THE), a 30% reduction in peak heat release rate (PHRR) due to flame inhibition (21% reduction in effective heat of combustion (EHC)), and an increase in Tg at the same time. This study indicates that rigid aromatic hyperbranched polymeric structures offer a promising route toward multifunctional flame retardancy. KW - Hyperbranched KW - Aromatic KW - Phosphorus KW - Phosphine oxide KW - DOPO KW - Flame retardant KW - Xpoxy resin KW - Rigid PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525910 DO - https://doi.org/10.1002/mame.202000731 SN - 1439-2054 VL - 306 IS - 4 SP - 731 PB - Wiley AN - OPUS4-52591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baumann, Maria A1 - Falkenhagen, Jana A1 - Weidner, Steffen A1 - Wold, C. A1 - Uliyanchenko, E. T1 - Characterization of copolymers of polycarbonate and polydimethylsiloxane by 2D chromatographic separation, MALDI-TOF mass spectrometry, and FTIR spectroscopy N2 - The structure and composition of polycarbonate polydimethylsiloxane copolymer (PC-co-PDMS) was investigated by applying various analytical approaches including chromatographic separation methods, spectrometric, and spectroscopic detection techniques. In particular, size exclusion chromatography (SEC) and liquid adsorption chromatography operating at different conditions (e.g. using gradient solvent systems) were used to achieve separations according to molar mass and functionality distribution. The coupling of both techniques resulted in fingerprint two-dimensional plots, which could be used to easily compare different copolymer batches. Matrix-assisted laser desorption/ionization-time-of-flight (MALDI-TOF) mass spectrometry was applied for structural investigations. The different ionization behavior of both comonomers, however, strongly limited the applicability of this technique. In contrast to that, Fourier-transform Infrared (FTIR) spectroscopy could be used to quantify the amount of PDMS in the copolymer at different points in the chromatogram. The resulting methodology was capable of distinguishing PC-co-PDMS copolymer from PC homopolymer chains present in the material. KW - FTIR KW - Liquid chromatography KW - Mass spectrometry KW - Gradient elution KW - Polycarbonate-co-dimethylsiloxane copolymer PY - 2020 DO - https://doi.org/10.1080/1023666X.2020.1820170 VL - 25 IS - 7 SP - 1 EP - 12 PB - Taylor & Francis AN - OPUS4-51369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bawadkji, O. A1 - Cherri, M. A1 - Schäfer, A. A1 - Herziger, S. A1 - Nickl, Philip A1 - Achazi, K. A1 - Donskyi, Ievgen A1 - Adeli, M. A1 - Haag, R. T1 - One-pot covalent functionalization of 2D black phosphorus by anionic ring opening polymerization N2 - In this work, a one-pot approach for the covalent functionalization of few-layer black phosphorus (BP) by anionic ring opening polymerization of glycidol to obtain multifunctional BP-polyglycerol (BP-PG) with high amphiphilicity for near-infrared-responsive drug delivery and biocompatibility is reported. Straightforward synthesis in combination with exceptional biological and physicochemical properties designates functionalized BP-PG as a promising candidate for a broad range of biomedical applications. KW - 2D nanomaterial KW - Amphiphilicity KW - Black phosphorus KW - Hyperbranched KW - Polyglycerol KW - Water dispersibility PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568833 DO - https://doi.org/10.1002/admi.202201245 SN - 2196-7350 VL - 9 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Waitelonis, Jörg A1 - Birkholz, Henk A1 - Jung, Matthias A1 - Schilling, Markus A1 - v. Hartrott, Philipp A1 - Bruns, Marian A1 - Schaarschmidt, Jörg A1 - Beilke, Kristian A1 - Mutz, Marcel A1 - Nebel, Vincent A1 - Königer, Veit A1 - Beran, Lisa A1 - Kraus, Tobias A1 - Vyas, Akhilesh A1 - Vogt, Lars A1 - Blum, Moritz A1 - Ell, Basil A1 - Chen, Ya‐Fan A1 - Waurischk, Tina A1 - Thomas, Akhil A1 - Durmaz, Ali Riza A1 - Ben Hassine, Sahar A1 - Fresemann, Carina A1 - Dziwis, Gordian A1 - Beygi Nasrabadi, Hossein A1 - Hanke, Thomas A1 - Telong, Melissa A1 - Pirskawetz, Stephan A1 - Kamal, Mohamed A1 - Bjarsch, Thomas A1 - Pähler, Ursula A1 - Hofmann, Peter A1 - Leemhuis, Mena A1 - Özçep, Özgür L. A1 - Meyer, Lars‐Peter A1 - Skrotzki, Birgit A1 - Neugebauer, Jörg A1 - Wenzel, Wolfgang A1 - Sack, Harald A1 - Eberl, Chris A1 - Portella, Pedro Dolabella A1 - Hickel, Tilmann A1 - Mädler, Lutz A1 - Gumbsch, Peter T1 - Concepts for a Semantically Accessible Materials Data Space: Overview over Specific Implementations in Materials Science N2 - This article describes advancements in the ongoing digital transformation in materials science and engineering. It is driven by domain‐specific successes and the development of specialized digital data spaces. There is an evident and increasing need for standardization across various subdomains to support science data exchange across entities. The MaterialDigital Initiative, funded by the German Federal Ministry of Education and Research, takes on a key role in this context, fostering collaborative efforts to establish a unified materials data space. The implementation of digital workflows and Semantic Web technologies, such as ontologies and knowledge graphs, facilitates the semantic integration of heterogeneous data and tools at multiple scales. Central to this effort is the prototyping of a knowledge graph that employs application ontologies tailored to specific data domains, thereby enhancing semantic interoperability. The collaborative approach of the Initiative's community provides significant support infrastructure for understanding and implementing standardized data structures, enhancing the efficiency of data‐driven processes in materials development and discovery. Insights and methodologies developed via the MaterialDigital Initiative emphasize the transformative potential of ontology‐based approaches in materials science, paving the way toward simplified integration into a unified, consolidated data space of high value. KW - Semantic Interoperability KW - Data Spaces KW - Integration Workflows KW - MaterialDigital PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622952 DO - https://doi.org/10.1002/adem.202401092 SN - 1527-2648 SP - 1 EP - 25 PB - Wiley-VCH CY - Weinheim AN - OPUS4-62295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Altmann, Korinna A1 - Sommerfeld, Thomas A1 - Braun, Ulrike T1 - Quantification of microplastics in a freshwater suspended organic matter using different thermoanalytical methods – outcome of an interlaboratory comparison N2 - A sedimented freshwater suspended organic matter fortified with particles of polyethylene (PE), polypropylene (PP), polystyrene (PS), and polyethylene terephthalate (PET) was employed in an interlaboratory comparison of thermoanalytical methods for microplastics identification and quantification. Three laboratories performed pyrolysis gas chromatography-mass spectrometry (Py-GC-MS), three others provided results using thermal extraction desorption followed by gas chromatography coupled to mass spectrometry (TED-GC-MS). One participant performed thermogravimetry-infrared spectroscopy (TGA-FTIR) and two participants used thermogravimetry coupled to mass spectrometry (TGA-MS). Further participants used differential scanning microscopy (DSC), a procedure based on micro combustion calorimetry (MCC) and a procedure based on elemental analysis. Each participant employed a different combination of sample treatment, calibration and instrumental Settings for polymer identification and quantification. Though there is obviously room for improvements regarding the between-laboratory reproducibility and the harmonization of procedures it was seen that the participants Performing Py-GC-MS, TED-GC-MS, and TGA-FTIR were able to correctly identify all polymers and to report reasonable quantification results in the investigated concentration range (PE: 20.0 μg/mg, PP: 5.70 μg/mg; PS: 2.20 μg/mg, PET: 18.0 μg/mg). Although for the other methods limitations exists regarding the detection of specific polymers, they showed potential as alternative approaches for polymer quantification in solid environmental matrices. KW - Interlaboratory comparison KW - Microplastics KW - Suspended organic matter KW - Pyrolysis PY - 2020 DO - https://doi.org/10.1016/j.jaap.2020.104829 VL - 148 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-50977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Scholz, Philipp A1 - Jung, Christian A1 - Weidner, Steffen T1 - Thermo-Desorption Gas Chromatography-Mass Spectrometry for investigating the thermal degradation of polyurethanes N2 - Thermo-Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to investigate the thermal degradation of two different polyurethanes (PU). PU samples were heated at different heating rates and the desorbed products were collected in a cold injection system and thereafter submitted to GC-MS. Prospects and limitations of the detection and quantification of semi-volatile degradation products were investigated. A temperature dependent PU depolymerization was found at temperatures above 200 °C proved by an increasing release of 1,4-butanediol and methylene diphenyl diisocyanate (MDI) representing the main building blocks of both polymers. Their release was monitored quantitatively based on external calibration with authentic compounds. Size Exclusion Chromatography (SEC) of the residues obtained after thermodesorption confirmed the initial competitive degradation mechanism indicating an equilibrium of crosslinking and depolymerization as previously suggested. Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry of SEC fractions of thermally degraded PUs provided additional hints on degradation mechanism. KW - Thermo-desorption KW - Mass spectrometry KW - Polyurethanes KW - Thermal degradation PY - 2023 DO - https://doi.org/10.1039/D3AY00173C SN - 1759-9660 SP - 1 EP - 6 PB - Royal Society for Chemistry AN - OPUS4-57307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bekemeier, Simon A1 - Caldeira Rêgo, C. R. A1 - Mai, H. L. A1 - Sikia, Ujjal A1 - Waseda, O. A1 - Apel, M. A1 - Arendt, F. A1 - Aschemann, A. A1 - Bayerlein, Bernd A1 - Courant, R. A1 - Dziwis, G. A1 - Fuchs, F. A1 - Giese, U. A1 - Junghanns, K. A1 - Kamal, M. A1 - Koschmieder, L. A1 - Leineweber, S. A1 - Luger, M. A1 - Lukas, M. A1 - Maas, J. A1 - Mertens, J. A1 - Mieller, Björn A1 - Overmeyer, L. A1 - Pirch, N. A1 - Reimann, J. A1 - Schröck, S. A1 - Schulze, P. A1 - Schuster, J. A1 - Seidel, A. A1 - Shchyglo, O. A1 - Sierka, M. A1 - Silze, F. A1 - Stier, S. A1 - Tegeler, M. A1 - Unger, Jörg F. A1 - Weber, M. A1 - Hickel, Tilmann A1 - Schaarschmidt, J. T1 - Advancing Digital Transformation in Material Science: The Role of Workflows Within the MaterialDigital Initiative N2 - The MaterialDigital initiative represents a major driver toward the digitalization of material science. Next to providing a prototypical infrastructure required for building a shared data space and working on semantic interoperability of data, a core focus area of the Platform MaterialDigital (PMD) is the utilization of workflows to encapsulate data processing and simulation steps in accordance with findable, accessible, interoperable, and reusable principles. In collaboration with the funded projects of the initiative, the workflow working group strives to establish shared standards, enhancing the interoperability and reusability of scientific data processing steps. Central to this effort is the Workflow Store, a pivotal tool for disseminating workflows with the community, facilitating the exchange and replication of scientific methodologies. This article discusses the inherent challenges of adapting workflow concepts, providing the perspective on developing and using workflows in the respective domain of the various funded projects. Additionally, it introduces the Workflow Store’s role within the initiative and outlines a future roadmap for the PMD workflow group, aiming to further refine and expand the role of scientific workflows as a means to advance digital transformation and foster collaborative research within material science. KW - Digitalisation KW - FAIR principles KW - MaterialDigital KW - Scientific workflows KW - Semantic interoperability PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624088 DO - https://doi.org/10.1002/adem.202402149 SN - 1527-2648 IS - 2402149 SP - 1 EP - 25 PB - Wiley-VCH GmbH AN - OPUS4-62408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belenguer, A A1 - Michalchuk, Adam A1 - Lampronti, G A1 - Sanders, J T1 - Using solid catalysts in disulfide-based dynamic combinatorial solution- and mechano-chemistry N2 - We here show for the first time that solid amines can act as catalysts for disulfide-based dynamic combinatorial chemistry by ball mill grinding. The mechanochemical Equilibrium for the two disulfide reactions studied is reached within one to three hours using ten different amine catalysts. This contrasts with the weeks to months to achieve solution equilibrium for most solid amine catalysts at 2%M at 2mM concentration in a suitable solvent. The final mechanochemical equilibrium is independent of the catalyst used, but varies with other ball mill grinding factors such as the presence of traces of solvent. The different efficiencies of the amines tested are discussed. KW - Mechanochemistry KW - Green chemistry KW - Catalysis PY - 2022 DO - https://doi.org/10.1002/cssc.202102416 SN - 1864-5631 VL - 15 IS - 3 SP - 1 EP - 10 PB - Wiley AN - OPUS4-53930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belenguer, A. A1 - Lampronti, G. A1 - Michalchuk, Adam A1 - Emmerling, Franziska A1 - Sanders, J. T1 - Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding N2 - We demonstrate here using a disulfide system the first example of reversible, selective, and quantitative transformation between three crystalline polymorphs by ball mill grinding. This includes the discovery of a previously unknown polymorph. Each polymorph is reproducibly obtained under well-defined neat or liquid-assisted grinding conditions, revealing subtle control over the apparent thermodynamic stability. We discovered that the presence of a contaminant as low as 1.5% mol mol−1 acting as a template is required to enable all these three polymorph transformations. The relative stabilities of the polymorphs are determined by the sizes of the nanocrystals produced under different conditions and by surface interactions with small amounts of added solvent. For the first time, we show evidence that each of the three polymorphs is obtained with a unique and reproducible crystalline size. This mechanochemical approach gives access to bulk quantities of metastable polymorphs that are inaccessible through recrystallisation. KW - Mechanochemistry KW - Polymorph KW - XRD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549934 DO - https://doi.org/10.1039/D2CE00393G SP - 1 EP - 7 PB - Royal Society of Chemistry AN - OPUS4-54993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Burr, L. A1 - Schmid, D. A1 - Hodoroaba, Vasile-Dan T1 - Towards a method for quantitative evaluation of nanoparticle from suspensions via microarray printing and SEM analysis N2 - As part of the development of a library of accurate and efficient methods for measurement of nanoparticle properties, we develop and optimize a method for the efficient analysis of nanoparticle size distribution from suspensions via microprinting and digital analysis of electron microscopy (SEM and TEM) images, with the ultimate aim of automated quantitative concentration analysis (calculated from drop volume). A series of different nanoparticle suspensions (gold, latex, and SiO2 in varying sizes and concentrations) were printed onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 nanoparticles/mL and imaged with SEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee-ring effect. KW - Nanoparticles KW - Particle size distribution KW - Electron microscopy KW - Microarray printing KW - Sample preparation KW - Nanoparticle concentration PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528455 DO - https://doi.org/10.1088/1742-6596/1953/1/012002 VL - 1953 SP - 012002 PB - IOP Publishing AN - OPUS4-52845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Müller, Anja A1 - Radnik, Jörg A1 - Hachenberger, Y. A1 - Jungnickel, H. A1 - Laue, P. A1 - Luch, A. A1 - Tentschert, J. T1 - Preparation of Nanoparticles for ToF-SIMS and XPS Analysis N2 - Nanoparticles have gained increasing attention in recent years due to their potential and application in different fields including medicine, cosmetics, chemistry, and their potential to enable advanced materials. To effectively understand and regulate the physico-chemical properties and potential adverse effects of nanoparticles, validated measurement procedures for the various properties of nanoparticles need to be developed. While procedures for measuring nanoparticle size and size Distribution are already established, standardized methods for analysis of their surface chemistry are not yet in place, although the influence of the surface chemistry on nanoparticle properties is undisputed. In particular, storage and preparation of nanoparticles for surface analysis strongly influences the analytical results from various methods, and in order to obtain consistent results, sample preparation must be both optimized and standardized. In this contribution, we present, in detail, some standard procedures for preparing nanoparticles for surface analytics. In principle, nanoparticles can be deposited on a suitable substrate from suspension or as a powder. Silicon (Si) Wafers are commonly used as substrate, however, their cleaning is critical to the process. For sample preparation from suspension, we will discuss drop-casting and spin-coating, where not only the cleanliness of the substrate and purity of the suspension but also its concentration play important roles for the success of the preparation methodology. For nanoparticles with sensitive ligand shells or coatings, deposition as powders is more suitable, although this method requires particular care in fixing the sample. KW - Titania nanoparticles KW - X-ray photoelectron spectroscopy KW - Secondary ion mass spectrometry KW - Surface chemisttry PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520103 UR - https://www.jove.com/video/61758 DO - https://doi.org/10.3791/61758 VL - 163 SP - e61758 AN - OPUS4-52010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Opitz, R. A1 - Ghoreishi, N. A1 - Plate, K. A1 - Barnes, J.-P. A1 - Bellew, A. A1 - Bellu, A. A1 - Ceccone, G. A1 - de Vito, E. A1 - Delcorte, A. A1 - Franquet, A. A1 - Fumageli, F. A1 - Gilliland, D. A1 - Jungnickel, H. A1 - Lee, T.G. A1 - Poleunis, C. A1 - Rading, D. A1 - Shon, H.K. A1 - Spampinato, V. A1 - Son, J.G. A1 - Wang, F. A1 - Wang, Y.-C. A. A1 - Zhao, Y. A1 - Roloff, A. A1 - Tentschert, J. A1 - Radnik, Jörg T1 - VAMAS TWA2 interlaboratory comparison: Surface analysis of TiO2 nanoparticles using ToF-SIMS N2 - Due to the extremely high specific surface area of nanoparticles and corresponding potential for adsorption, the results of surface analysis can be highly dependent on the history of the particles, particularly regarding sample preparation and storage. The sample preparation method has, therefore, the potential to have a significant influence on the results. This report describes an interlaboratory comparison (ILC) with the aim of assessing which sample preparation methods for ToF-SIMS analysis of nanoparticles provided the most intra- and interlaboratory consistency and the least amount of sample contamination. The BAM reference material BAM-P110 (TiO2 nanoparticles with a mean Feret diameter of 19 nm) was used as a sample representing typical nanoparticles. A total of 11 participants returned ToF-SIMS data,in positive and (optionally) negative polarity, using sample preparation methods of “stick-and-go” as well as optionally “drop-dry” and “spin-coat.” The results showed that the largest sources of variation within the entire data set were caused by adventitious hydrocarbon contamination or insufficient sample coverage, with the spin-coating protocol applied in this ILC showing a tendency toward insufficient sample coverage; the sample preparation method or the participant had a lesser influence on results. KW - Secondary Ion Mass Spectrometry KW - VMAAS KW - Titania KW - Interlaboratory comparison KW - Reproducibility PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582290 DO - https://doi.org/10.1116/6.0002814 SN - 0734-2101 VL - 41 IS - 5 SP - 053210-1 EP - 053210-13 PB - AIP (American Institute of Physics) AN - OPUS4-58229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernardes, C. E. S. A1 - Feliciano, I.O. A1 - Naese, Christoph A1 - Emmerling, Franziska A1 - Minas da Piedade, M. T1 - Energetics of dehydroepiandrosterone polymorphs I and II from solution and drop-sublimation Calvet microcalorimetry measurements N2 - The lattice enthalpies and monotropic relationship of two dehydroepiandrosterone (DEHA) polymorphs (forms I and II) were evaluated through a combination of differential scanning calorimetry (DSC), isothermal solution microcalorimetry, and drop-sublimation Calvet microcalorimetry experiments. The standard molar enthalpy of transition between both forms was determined as ΔtrsHom (II→I, 298.15 K) = - 0.90 ± 0.07 kJ mol-1 and ΔtrsHom (II→I, 417.8 K) = - 1.7 ± 1.0 kJ mol- 1, from measurements of standard molar enthalpies of solution in dimethyl sulfoxide and enthalpies of fusion, respectively. Drop-sublimation Calvet microcalorimetry experiments on form I led to ΔsubHom (cr I, 298.15 K) = 132.0±3.3 kJ mol - 1. This result, when combined with the more precise ΔtrsHom (II→I) value obtained by solution calorimetry, afforded ΔsubHom (cr II, 298.15 K) = 131.1±3.3 kJ mol - 1. The overall data indicate that on enthalpic grounds form I is more stable than form II from 298.15 K up to fusion. This conclusion, and the fact that DSC experiments indicated that form I has also a considerably higher temperature fusion, namely, Tfus(cr I)= 422.5±0.2 K and Tfus(cr II) = 413.1±0.2 K, suggest that the two polymorphs are monotropically related. KW - Calorimetry KW - Polymorphism KW - Enthalpy of solution KW - Enthalpy of sublimation KW - Thermochemistry KW - Lattice enthalpy PY - 2023 DO - https://doi.org/10.1016/j.jct.2023.107137 SN - 0021-9614 SN - 1096-3626 VL - 186 SP - 1 EP - 7 PB - Elsevier AN - OPUS4-58418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernges, T. A1 - Hanus, R. A1 - Wankmiller, B. A1 - Imasato, K. A1 - Lin, S. A1 - Ghidiu, M. A1 - Gerlitz, M. A1 - Peterlechner, M. A1 - Graham, S. A1 - Hautier, G. A1 - Pei, Y. A1 - Hansen, M. R. A1 - Wilde, G. A1 - Snyder, G. J. A1 - George, Janine A1 - Agne, M T. A1 - Zeier, W. G. T1 - Considering the Role of Ion Transport in Diffuson-Dominated Thermal Conductivity N2 - Next-generation thermal management requires the development of low lattice thermal conductivity materials, as observed in ionic conductors. For example, thermoelectric efficiency is increased when thermal conductivity is decreased. Detrimentally, high ionic conductivity leads to thermoelectric device degradation. Battery safety and design also require an understanding of thermal transport in ionic conductors. Ion mobility, structural complexity, and anharmonicity have been used to explain the thermal transport properties of ionic conductors. However, thermal and ionic transport are rarely discussed in direct comparison. Herein, the ionic conductivity of Ag+ argyrodites is found to change by orders of magnitude without altering the thermal conductivity. Thermal conductivity measurements and two-channel lattice dynamics modeling reveal that the majority of Ag+ vibrations have a non-propagating diffuson-like character, similar to amorphous materials. It is found that high ionic mobility is not a requirement for diffuson-mediated transport. Instead, the same bonding and structural traits that can lead to fast ionic conduction also lead to diffuson-mediated transport. Bridging the fields of solid-state ionics and thermal transport, it is proposed that a vibrational perspective can lead to new design strategies for functional ionic conducting materials. As a first step, the authors relate the so-called Meyer-Neldel behavior in ionic conductors to phonon occupations. KW - Diffusons KW - DFT KW - Phonons KW - Thermoelectrics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547140 DO - https://doi.org/10.1002/aenm.202200717 SN - 1614-6832 VL - 12 IS - 22 SP - 1 EP - 13 PB - Wiley VHC-Verlag AN - OPUS4-54714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Berry, Charlotte A. A1 - Reinart, Katre A1 - Smales, Glen J. A1 - Wilkinson, Holly N. A1 - Hardman, Matthew J. A1 - Marchesini, Sofia A1 - Lee, William A1 - Nery, Eveliny Tomás A1 - Moghaddam, Zarrin A1 - Hoxha, Agron A1 - Felipe-Sotelo, Mónica A1 - Gutierrez-Merino, Jorge A1 - Carta, Daniela T1 - Hierarchically porous copper and gallium loaded sol–gel phosphate glasses for enhancement of wound closure N2 - In this work, we have developed hierarchically porous phosphate-based glasses (PPGs) as novel materials capable of promoting wound closure and simultaneously delivering antibacterial effects at the glass-biological tissue interface. PPGs are characterised by extended porosity, which enhances the controlled release of therapeutic ions, whilst facilitating cell infiltration and tissue growth. Two series of PPGs in the systems P2O5–CaO–Na2O–CuO and P2O5–CaO–Na2O–Ga2O3 with (CuO and Ga2O3 0, 1, 5 and 10 mol%) were manufactured using a supramolecular sol–gel synthesis strategy. Significant wound healing promotion (up to 97%) was demonstrated using a human ex vivo wound model. A statistically significant reduction of the bacterial strains Staphylococcus aureus and Escherichia coli was observed in both series of PPGs, particularly those containing copper. All PPGs exhibited good cytocompatibility on keratinocytes (HaCaTs), and analysis of PPG dissolution products over a 7-day period demonstrated controlled release of phosphate anions and Ca, Na, Cu, and Ga cations. These findings indicate that Cu- and Ga-loaded PPGs are promising materials for applications in soft tissue regeneration given their antibacterial capabilities, in vitro biocompatibility with keratinocytes and ex vivo wound healing properties at the biomaterial-human tissue interface. KW - Porous glass KW - Phosphates KW - Wound healing materials KW - Antibacterial KW - X-ray scattering KW - MOUSE PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650867 DO - https://doi.org/10.1039/d5tb01945a SN - 2050-750X VL - 13 IS - 48 SP - 15662 EP - 15677 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Besselink, R. A1 - Stawski, Tomasz A1 - Freeman, H. M. A1 - Hovelmann, J. A1 - Tobler, D. J. A1 - Benning, L. G. T1 - Mechanism of Saponite Crystallization from a Rapidly Formed Amorphous Intermediate N2 - Clays are crucial mineral phases in Earth’s weathering engine, but we do not know how they form in surface environments under (near-)ambient pressures and temperatures. Most synthesis routes, attempting to give insights into the plausible mechanisms, rely on hydrothermal conditions, yet many geological studies showed that clays may actually form at moderate temperatures (<100 °C) in most terrestrial settings. Here, we combined high-energy X-ray diffraction, infrared spectroscopy, and transmission electron microscopy to derive the mechanistic pathways of the low-temperature (25–95 °C) crystallization of a synthetic Mg-clay, saponite. Our results reveal that saponite crystallizes via a two stage process: (1) a rapid (several minutes) coprecipitation where ∼20% of the available magnesium becomes incorporated into an aluminosilicate network, followed by (2) a much slower crystallization mechanism (several hours to days) where the remaining magnesium becomes gradually incorporated into the growing saponite sheet structure. KW - Saponite KW - FTIR KW - PDF KW - Diffraction PY - 2020 DO - https://doi.org/10.1021/acs.cgd.0c00151 VL - 20 IS - 5 SP - 3365 EP - 3373 PB - American Chemical Society AN - OPUS4-50917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyranvand, S. A1 - Pourghobadi, Z. A1 - Sattari, S. A1 - Soleymani, K. A1 - Donskyi, Ievgen A1 - Gharabaghi, M. A1 - Unger, Wolfgang A1 - Farjanikish, G. A1 - Nayebzadeh, H. A1 - Adeli, M. T1 - Boronic acid functionalized graphene platforms for diabetic wound N2 - While noncovalent interactions between graphene derivatives and biosystems are extensively studied, less knowledge about their covalent multivalent interactions at biointerfaces is available. Due to the affinity of boronic acids towards cis-diol bearing biosystems, graphene sheets with this functionality were synthesized and their covalent interactions with the bacteria and nematode were investigated. As expected, graphene platforms with boronic acid functionality were able to wrap bacteria and destroy it in a short time. Surprisingly, body of nematodes was ruptured and their viability decreased to 30% after 24 h incubation with the functionalized graphene sheets. Because of their antibacterial and antiparasitic activities as well as their ability for wound dressing, graphene platforms with the boronic acid functionality were further investigated for diabetic wound healing. In vivo experiments showed that graphene platforms are more efficient than the commercially available drug, phenytoin, and restore both infected and non-infected diabetic wounds in ten days. Taking advantage of their straightforward synthesis, strong interactions with different biosystems as well as their ability to heal diabetic wounds, the boronic Acid functionalized graphene sheets are promising candidates for a broad range of future biomedical applications. KW - Graphene KW - Boronic acid KW - Functionalized graphene KW - XPS PY - 2020 UR - https://www.sciencedirect.com/science/article/abs/pii/S0008622319310954 DO - https://doi.org/doi.org/10.1016/j.carbon.2019.10.077 VL - 158 SP - 327 EP - 336 PB - Elsevier Ltd. AN - OPUS4-50559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhatia, S. A1 - Donskyi, Ievgen A1 - Block, S. A1 - Nie, C. A1 - Burdinski, A. A1 - Lauster, D. A1 - Radnik, Jörg A1 - Herrmann, A. A1 - Haag, R. A1 - Ludwig, K. A1 - Adeli, M. T1 - Wrapping and Blocking of Influenza A Viruses by Sialylated 2D Nanoplatforms N2 - Inhibition of respiratory viruses is one of the most urgent topics as underlined by different pandemics in the last two decades. This impels the development of new materials for binding and incapacitation of the viruses. In this work, we have demonstrated that an optimal deployment of influenza A virus (IAV) targeting ligand sialic acid (SA) on a flexible 2D platform enables its binding and wrapping around IAV particles. A series of 2D sialylated platforms consisting graphene and polyglycerol are prepared with different degrees of SA functionalization around 10%, 30%, and 90% named as G-PG-SAL, G-PG-SAM, and G-PG-SAH, respectively. The cryo-electron tomography (Cryo-ET) analysis has proved wrapping of IAV particles by G-PG-SAM. A confocal-based colocalization assay established for these materials has offered the comparison of binding potential of sialylated and non-sialylated nanoplatforms for IAV. With this method, we have estimated the binding potential of the G-PG-SAM and G-PG-SAH sheets for IAV particles around 50 and 20 times higher than the control sheets, respectively, whereas the low functionalized G-PG-SAL have not shown any significant colocalization value. Moreover, optimized G-PG-SAM exhibits high potency to block IAV from binding with the MDCK cells. KW - 2D Materials KW - Graphhene KW - Influenza A virus KW - Sialic acid KW - wrapping PY - 2021 DO - https://doi.org/10.1002/admi.202100285 VL - 8 IS - 12 SP - 285 PB - Wiley VCH AN - OPUS4-52715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhattacharya, Biswajit A1 - Das, S. A1 - Lal, G. A1 - Soni, S. R. A1 - Ghosh, A. A1 - Reddy, C. M. A1 - Ghosh, S. T1 - Screening, crystal structures and solubility studies of a series of multidrug salt hydrates and cocrystals of fenamic acids with trimethoprim and sulfamethazine N2 - Multidrug solids have a potential use to efficiently treat and control a superfluity of medical conditions. To address the current drawbacks of drug development in R&D, it was targeted to achieve new pharmaceutical solid forms of fenamic acids having improved solubility and thermal stability. Subsequently, five new multicomponent solids consisting of three salt hydrates of trimethoprim (TMP) with mefenamic acid (TMP-MFA-H2O), tolfenamic acid (TMP-TFA-H2O) and flufenamic acid (TMP-FFA-H2O), and two cocrystals of sulfamethazine (SFZ) with flufenamic acid (SFZ-FFA) and niflumic acid (SFZ-NFA) were prepared by liquid assisted grinding. Looking at the structures of active pharmaceutical ingredient (API) molecules, it was quite expected that a wide range of supramolecular synthons would lead to cocrystallization. New forms were characterized thoroughly by various solid-state techniques, including single crystal X-ray diffraction (SCXRD), which provided details of hydrogen bonding, molecular packing and interactions between drug and coformer. Kinetic solubility at pH 7.4 buffer study has been carried out and a comparison is made with respect to the parent drugs. A significant enhancement of NSAIDs solubility was observed in all salt hydrate systems of TMP. Thus with increasing physicochemical properties such as improved solubility further leads to the enhancement of bioavailability, which has implications to overcoming the formulation related problems of active pharmaceutical ingredients (APIs). KW - Cocrystals KW - Crystal engineering KW - Solubility PY - 2020 DO - https://doi.org/10.1016/j.molstruc.2019.127028 SN - 0022-2860 VL - 1199 SP - 127028 PB - Elsevier B.V. AN - OPUS4-49873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam A1 - Silbernagl, Dorothee A1 - Rautenberg, Max A1 - Schmid, Thomas A1 - Feiler, Torvid A1 - Reimann, K. A1 - Ghalgaoui, A. A1 - Sturm, Heinz A1 - Paulus, B. A1 - Emmerling, Franziska T1 - A Mechanistic Perspective on Plastically Flexible Coordination Polymers N2 - Mechanical flexibility in single crystals of covalently bound materials is a fascinating and poorly understood phenomenon. We present here the first example of a plastically flexible one-dimensional (1D) coordination polymer. The compound [Zn(m-Cl)2(3,5-dichloropyridine)2]n is flexible over two crystallographic faces. Remarkably, the single crystal remains intact when bent to 1808. A combination of microscopy, diffraction, and spectroscopic studies have been used to probe the structural response of the crystal lattice to mechanical bending. Deformation of the covalent polymer chains does not appear to be responsible for the observed macroscopic bending. Instead, our results suggest that mechanical bending occurs by displacement of the coordination polymer chains. Based on experimental and theoretical evidence, we propose a new model for mechanical flexibility in 1D coordination polymers. Moreover, our calculations propose a cause of the different mechanical properties of this compound and a structurally similar elastic material KW - Coordination polymer KW - Flexible crystals KW - Mechanical properties KW - Plastic deformation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504755 DO - https://doi.org/10.1002/anie.201914798 VL - 59 IS - 14 SP - 5557 EP - 5561 PB - Wiley-VCH AN - OPUS4-50475 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam A1 - Silbernagl, Dorothee A1 - Yasuda, N. A1 - Feiler, Torvid A1 - Sturm, Heinz A1 - Emmerling, Franziska T1 - An atomistic mechanism for elasto-plastic bending in molecular crystals N2 - Mechanically flexible single crystals of molecular materials offer potential for a multitude of new directions in advanced materials design. Before the full potential of such materials can be exploited, insight into their mechanisms of action must be better understood. Such insight can be only obtained through synergistic use of advanced experimentation and simulation. We herein report the first detailed mechanistic study of elasto-plastic flexibility in a molecular solid. An atomistic origin for this mechanical behaviour is proposed through a combination of atomic force microscopy, μ-focus synchrotron X-ray diffraction, Raman spectroscopy, ab initio simulation, and computed elastic tensors. Our findings suggest that elastic and plastic bending are intimately linked and result from extensions of the same molecular deformations. The proposed mechanism bridges the gap between contested mechanisms, suggesting its applicability as a general mechanism for elastic and plastic bending in organic molecular crystals. KW - Mechanical property KW - Mechanical flexibility KW - Organic crystal PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-577722 DO - https://doi.org/10.1039/D2SC06470G SN - 2041-6520 VL - 14 IS - 13 SP - 3441 EP - 3450 PB - Royal Society of Chemisty (RSC) CY - London/Cambridge AN - OPUS4-57772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn T1 - Quo vadis LIPSS? - Recent and future trends on laser-induced periodic surface structures N2 - Nanotechnology and lasers are among the most successful and active fields of research and technology that have boomed during the past two decades. Many improvements are based on the controlled manufacturing of nanostructures that enable tailored material functionalization for a wide range of industrial applications, electronics, medicine, etc., and have already found entry into our daily life. One appealing approach for manufacturing such nanostructures in a flexible, robust, rapid, and contactless one-step process is based on the generation of laser-induced periodic surface structures (LIPSS). This Perspectives article analyzes the footprint of the research area of LIPSS on the basis of a detailed literature search, provides a brief overview on its current trends, describes the European funding strategies within the Horizon 2020 programme, and outlines promising future directions. KW - Laser-induced periodic surface structures (LIPSS) KW - Direct laser interference patterning (DLIP) KW - Surface functionalization KW - Literature survey KW - European funding strategies PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513530 DO - https://doi.org/10.3390/nano10101950 SN - 2079-4991 VL - 10 IS - 10 SP - 1950-1 EP - 1950-19 PB - MDPI CY - Basel AN - OPUS4-51353 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Gräf, S. T1 - Maxwell Meets Marangoni — A Review of Theories on Laser‐Induced Periodic Surface Structures N2 - Surface nanostructuring enables the manipulation of many essential surface properties. With the recent rapid advancements in laser technology, a contactless large‐area processing at rates of up to m2 s−1 becomes feasible that allows new industrial applications in medicine, optics, tribology, biology, etc. On the other hand, the last two decades enable extremely successful and intense research in the field of so‐called laser‐induced periodic surface structures (LIPSS, ripples). Different types of these structures featuring periods of hundreds of nanometers only—far beyond the optical diffraction limit—up to several micrometers are easily manufactured in a single‐step process and can be widely controlled by a proper choice of the laser processing conditions. From a theoretical point of view, however, a vivid and very controversial debate emerges, whether LIPSS originate from electromagnetic effects or are caused by matter reorganization. This article aims to close a gap in the available literature on LIPSS by reviewing the currently existent theories of LIPSS along with their numerical implementations and by providing a comparison and critical assessment of these approaches. KW - Laser-induced periodic surface structures (LIPSS) KW - Electromagnetic theories KW - Matter reorganization theories KW - Surface plasmon polaritons KW - Self-organization PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514089 DO - https://doi.org/10.1002/lpor.202000215 SN - 1863-8899 VL - 14 IS - 10 SP - 2000215-1 EP - 2000215-25 PB - Wiley CY - Berlin AN - OPUS4-51408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Gräf, S. T1 - Ten Open Questions about Laser-Induced Periodic Surface Structures N2 - Laser-induced periodic surface structures (LIPSS) are a simple and robust route for the nanostructuring of solids that can create various surface functionalities featuring applications in optics, medicine, tribology, energy technologies, etc. While the current laser technologies already allow surface processing rates at the level of m2/min, industrial applications of LIPSS are sometimes hampered by the complex interplay between the nanoscale surface topography and the specific surface chemistry, as well as by limitations in controlling the processing of LIPSS and in the long-term stability of the created surface functions. This Perspective article aims to identify some open questions about LIPSS, discusses the pending technological limitations, and sketches the current state of theoretical modelling. Hereby, we intend to stimulate further research and developments in the field of LIPSS for overcoming these limitations and for supporting the transfer of the LIPSS technology into industry. KW - Laser-induced periodic surface structures (LIPSS) KW - Industrial application KW - Functional properties KW - Surface functionalization KW - Modelling PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539503 DO - https://doi.org/10.3390/nano11123326 SN - 2079-4991 VL - 11 IS - 12 SP - 1 EP - 21 PB - MDPI CY - Basel, Switzerland AN - OPUS4-53950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Structuring of thin films by ultrashort laser pulses N2 - Modern life and global communication would not be possible without technologically tailored thin films; they are omnipresent in daily life applications. In most cases, the films are deposited entirely at the carrying substrates in a specific processing step of the device or sample. In some cases, however, removal or modification must be performed locally, i.e., site-controlled and material selective through an additional laser processing step. For that ultrashort laser pulses with durations in the femtosecond and picosecond range can provide unique advantages and capabilities in industrially scalable schemes. This article reviews the current state of the research and corresponding industrial transfer related to the structuring of thin films by ultrashort pulsed lasers. It focuses on the pertinent historic developments, reveals the relevant physical and chemical effects, explores the ultimate limits, and discusses selected industrial and scientific applications. KW - Thin films KW - Laser processing KW - Ultrashort lasers KW - Laser damage KW - Femtosecond laser ablation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565732 DO - https://doi.org/10.1007/s00339-022-06229-x SN - 0947-8396 SN - 1432-0630 VL - 129 IS - 1 SP - 1 EP - 38 PB - Springer CY - Berlin AN - OPUS4-56573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Lasagni, A. F. T1 - Editorial: Laser micro- and nano-material processing – Part 1 N2 - This special issue of Advanced Optical Technologies (AOT) is dedicated to the field of laser-based micro- and nanostructuring methods. KW - Laser processing KW - Microstructures KW - Nanostructures KW - Applications PY - 2020 DO - https://doi.org/10.1515/aot-2020-0009 SN - 2193-8576 SN - 2193-8584 VL - 9 IS - 1-2 SP - 7 EP - 9 PB - De Gruyter CY - Berlin AN - OPUS4-50797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Paun, I. A. A1 - Heitz, J. A1 - Stoian, R. T1 - Guest editorial: Making light matter N2 - This article represents the Guest Editorial of the Special Issue associated with the Symposium L "Making light matter: lasers in material sciences and photonics" held during the 2023 E-MRS Spring Meeting in Strasbourg, France, June 25th - July 2nd, 2023. T2 - 2023 E-MRS Spring Meeting, Symposium L "Making light matter: lasers in material sciences and photonics" CY - Strasbourg, France DA - 29.05.2023 KW - Guest Editorial KW - Laser KW - Material Science KW - Photonics PY - 2024 DO - https://doi.org/10.1002/pssa.202400528 SN - 1862-6319 VL - 221 IS - 15 SP - 1 EP - 5 PB - Wiley-VCH CY - Weinheim AN - OPUS4-60948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Sokolowski‐Tinten, Klaus T1 - Probing Laser‐Driven Structure Formation at Extreme Scales in Space and Time N2 - Irradiation of solid surfaces with high intensity, ultrashort laser pulses triggers a variety of secondary processes that can lead to the formation of transient and permanent structures over a large range of length scales from mm down to the nano‐range. One of the most prominent examples are LIPSS – Laser‐Induced Periodic Surface Structures. While LIPSS have been a scientific evergreen for of almost 60 years, experimental methods that combine ultrafast temporal with the required nm spatial resolution have become available only recently with the advent of short pulse, short wavelength free electron lasers. Here, the current status and future perspectives in this field are discussed by exploiting the unique possibilities of these 4th‐generation light sources to address by time‐domain experimental techniques the fundamental LIPSS‐question, namely why and how laser irradiation can initiate the transition of a “chaotic” (rough) surface from an aperiodic into a periodic structure. KW - Laser-induced periodic surface structures (LIPSS) KW - Free electron laser KW - Pump-probe experiments KW - Time-resolved scattering KW - Capillary waves PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595048 DO - https://doi.org/10.1002/lpor.202300912 SN - 1863-8899 VL - 18 SP - 1 EP - 11 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-59504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Spaltmann, Dirk T1 - Editorial: Special issue "Laser-induced periodic surface nano- and microstructures for tribological applications" N2 - Laser material processing is an emerging technology that generates surface functionalities on the basis of optical, mechanical, or chemical properties. In the form of laser surface texturing (LST), it has attracted a remarkable amount of research to tailor surface properties towards various tribological applications. The main advantages of this single-step, laser-based technology are the contactless machining, featuring a high flexibility, efficiency, and speed, along with the excellent quality of the processed products. LST can be applied precisely localized to sub-micrometric areas, but, via laser beam scanning, it is also feasible for structuring large surface areas at the square meter size. This Special Issue focuses on the latest developments concerning the tribological performance of laser-generated periodic surface nano- and microstructures and their applications. This includes the laser-based processing of different surface patterns, such as “self-organized” laser-induced periodic surface structures (LIPSS, ripples), grooves, micro-spikes, hierarchical hybrid nano-/micro-structures, microfeatures generated by direct laser interference patterning (DLIP), or even dimples or other topographic geometries shaped by direct laser modification or ablation. The applications of these periodically nano- and micro-patterned surfaces may improve the lubricated or non-lubricated tribological performance of surfaces in conformal and even non-conformal contact through a reduction of wear, a variation of the coefficient of friction, altered load carrying capacity, etc., resulting in energy saving, improved reliability, increased lifetimes as well as durability, leading in turn to extended maintenance intervals/reduced down-time. This can be beneficial in terms of bearings, gears, engines, seals, cutting tools, or other tribological components. Fundamental aspects addressed may involve the investigation of the relevant physical and chemical effects accompanying the laser-generated nano- and microscale topographies, such as alterations of the material structures, the hardness, superficial oxidation, the role of additives contained in lubricants, surface wettability, micro-hydrodynamic effects, etc. For this Special Issue we aim to attract both academic and industrial researchers and would like to provide a bridge between research in the fields of tribology and laser material processing in order to foster the current knowledge and present new ideas for future applications and new technologies. KW - Laser-induced periodic surface structures (LIPSS) KW - Tribology KW - Applications KW - Wear KW - Friction PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505948 DO - https://doi.org/10.3390/lubricants8030034 SN - 2075-4442 VL - 8 IS - 3 SP - 34, 1 EP - 34, 3 PB - MDPI CY - Basel AN - OPUS4-50594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bornemann-Pfeiffer, Martin A1 - Wolf, Jakob A1 - Meyer, Klas A1 - Kern, S. A1 - Angelone, D. A1 - Leonov, A. A1 - Cronin, L. A1 - Emmerling, Franziska T1 - Standardization and control of Grignard reactions in a universal chemical synthesis machine using online NMR T1 - Standardisierung und Kontrolle von Grignard-Reaktionen mittels Online-NMR in einer universellen chemischen Syntheseplattform N2 - A big problem with the chemistry literature is that it is not standardized with respect to precise operational parameters, and real time corrections are hard to make without expert knowledge. This lack of context means difficult reproducibility because many steps are ambiguous, and hence depend on tacit knowledge. Here we present the integration of online NMR into an automated chemical synthesis machine (CSM aka. “Chemputer” which is capable of small-molecule synthesis using a universal programming language) to allow automated analysis and adjustment of reactions on the fly. The system was validated and benchmarked by using Grignard reactions which were chosen due to their importance in synthesis. The system was monitored in real time using online-NMR, and spectra were measured continuously during the reactions. This shows that the synthesis being done in the Chemputer can be dynamically controlled in response to feedback optimizing the reaction conditions according to the user requirements. N2 - Ein Problem der chemischen Literatur ist die fehlende Standardisierung bezüglich genauer Bedingungen, auch Echtzeit-Korrekturen sind ohne Expertenwissen nur schwer möglich. Dieser Mangel an Details erschwert experimentelle Reproduzierbarkeit, da Schritte oft mehrdeutig sind und daher von implizitem Wissen abhängen. Hier präsentieren wir die Integration von Online-NMR Spektroskopie in eine automatisierte chemische Syntheseplattform (CSM aka. “Chemputer”, unter Verwendung einer universellen Programmiersprache zur Synthese kleiner Moleküle fähig), um eine automatisierte Analyse und Anpassung von Reaktionen im laufenden Betrieb zu ermöglichen. Das System wurde anhand von Grignard-Reaktionen, die aufgrund ihrer Bedeutung für die Synthese ausgewählt wurden, validiert und einem Härtetest unterzogen. Synthesen wurden in Echtzeit mit Online-NMR überwacht, und die Spektren wurden während der Reaktionen kontinuierlich aufgenommen und analysiert. Dies zeigt, dass der Chemputer dynamisch mittels einer Regelung kontrolliert werden kann, um die Reaktionsbedingungen entsprechend den Anforderungen des Benutzers zu optimieren. KW - Grignard reaction KW - NMR spectroscopy KW - Process analytical technology KW - Process control KW - Grignard-Reaktion KW - NMR-Spektroskopie KW - Prozessanalytik KW - Prozesskontrolle PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531260 DO - https://doi.org/10.1002/anie.202106323 SN - 1521-3773 SN - 1433-7851 N1 - Bibliografische Angaben für die deutsche Version: Angewandte Chemie 2021, Jg. 133, S. 1–7, ISSN 0044-8249, ISSN 1521-3757, https://doi.org/10.1002/ange.202106323 - Bibliographic information for the German version: Angewandte Chemie 2021, vol. 133, p. 1–7, ISSN 0044-8249, ISSN 1521-3757, https://doi.org/10.1002/ange.202106323 VL - 60 IS - 43 SP - 1 EP - 6 PB - Wiley-VCH CY - Weinheim AN - OPUS4-53126 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Božičević, Lucija A1 - Altmann, Korinna A1 - Hildebrandt, Jana A1 - Knigge, Xenia A1 - Vrček, Valerije A1 - Peranić, Nikolina A1 - Kalcec, Nikolina A1 - Vinkovic Vrcek, Ivana T1 - Estrogenic activity of plastic nanoparticles mixture under in vitro settings N2 - The plastic value chain, central part of modern living, caused environmental pollution and bioaccumulation of plastic nanoparticles (PNPs). Their ubiquitous presence in different environmental and biological compartments has become a serious threat to human health and ecosystems. Frequently used plastic materials such as polypropylene (PP), polystyrene (PS) and polyethylene (PE) have been detected in the form of PNPs in the food chain, soil, water and air, as well as in human feces and blood. In this study, we aimed to provide novel insights in endocrine disrupting properties of PNPs using in vitro estrogen receptor (ER) transactivation assay. The effects of PP-NPs, PE-NPs and PS-NPs and their mixture on T47D-KBluc cell line stably transfected with luciferase as reporter enzyme was evaluated by means of cytotoxicity, cellular uptake and ER activation. Tested dose range for PNPs was 0.001 – 10 mg/L. Both cellular uptake and cytotoxicity for all PNPs was found to be dose-dependent. Only the highest dose of PP-NPs and PE-NPs induced apoptosis and cell death, while PS-NPs were not cytotoxic in tested dose range. For tested concentrations, PP-NPs and PE-NPs showed significant agonistic activity on ER, while PS-NPs cannot be considered ER active. When, applied as mixture, PNP demonstrated additive toxicity effects compared to the effect of each individual PNPs. Additivity was also observed for ER agonistic effect of PNPs mixture according to the benchmark dose-addition modelling approach. This study provides missing science-based evidence on endocrine disrupting effects of PE-NPs, PP-NPs, PS-NPs and their mixtures and highlights the importance of considering unintentional, aggregate and combined exposure to different PNPs in risk management. KW - Risk assessment KW - Nanoplastics KW - Estrogenic activity of plastic nanoparticles PY - 2024 DO - https://doi.org/10.1039/D3EN00883E SN - 2051-8153 VL - 11 IS - 5 SP - 2112 EP - 2126 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Breitenbach, Romy A1 - Gerrits, Ruben A1 - Dementyeva, Polina A1 - Knabe, Nicole A1 - Schumacher, Julia A1 - Feldmann, Ines A1 - Radnik, Jörg A1 - Ryo, M. A1 - Gorbushina, Anna T1 - The role of extracellular polymeric substances of fungal biofilms in mineral attachment and weathering N2 - The roles extracellular polymeric substances (EPS) play in mineral attachment and weathering were studied using genetically modified biofilms of the rock-inhabiting fungus Knufia petricola strain A95. Mutants deficient in melanin and/or carotenoid synthesis were grown as air-exposed biofilms. Extracted EPS were quantified and characterised using a combination of analytical techniques. The absence of melanin affected the quantity and composition of the produced EPS: mutants no longer able to form melanin synthesised more EPS containing fewer pullulan-related glycosidic linkages. Moreover, the melanin-producing strains attached more strongly to the mineral olivine and dissolved it at a higher rate. We hypothesise that the pullulan-related linkages, with their known adhesion functionality, enable fungal attachment and weathering. The released phenolic intermediates of melanin synthesis in the Δsdh1 mutant might play a role similar to Fe-chelating siderophores, driving olivine dissolution even further. These data demonstrate the need for careful compositional and quantitative analyses of biofilm-created microenvironments. KW - Biofilms PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549025 DO - https://doi.org/10.1038/s41529-022-00253-1 SN - 2397-2106 VL - 6 SP - 1 EP - 11 PB - Springer Nature CY - London AN - OPUS4-54902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Alexandra A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. KW - Nano KW - Particle size distribution KW - Nanoparticle KW - Nanomaterial KW - OECD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891 DO - https://doi.org/10.3390/nano12132238 SN - 2079-4991 VL - 12 IS - 13 SP - 2238 PB - MDPI CY - Basel AN - OPUS4-55189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brirmi, M A1 - Chabbah, T. A1 - Chatti, S. A1 - Schiets, F. A1 - Casabianca, H. A1 - Marestin, C. A1 - Mercier, R. A1 - Weidner, Steffen A1 - Errachid, A. A1 - Jaffrezic-Renault, N. A1 - Ben Romdhane, H. T1 - Effect of the pendent groups on biobased polymers, obtained from click chemistry suitable, for the adsorption of organic pollutants from water N2 - In this work, four triazole-based poly(ether-pyridine)s polymers were synthesized and used as an adsorbent for the removal of phenolic compounds from aqueous solutions. For this purpose, new fluoromonomers containing 1,2,3-triazole units were prepared by the Cu(I)-catalyzed 1,3-dipolar cycloaddition reaction and then used for the elaboration of novel poly(ether-pyridine-triazole)s (PEPTs) by direct polyconden-sation with isosorbide and bisphenol A. Chemical structure of fluorinated pyridinicmonomers as well as resulting polymers was confirmed by 1H and 19F NMR spectroscopic methods. The thermal behavior of the obtained PEPTs was characterized using differential scanning calorimetry and thermogravimetric analysis. Results of sorption showed that polymers can be effectively used as a sorbent for the removal of polarorganic pollutants. The isosorbide-based poly(ether-pyridine-triazole) which contains hydrophilic hydroxyl groups as pendants chains (P4) exhibited the highest sorption efficiencies (78%–100% after 1 h). In order to explain the results an adsorption mech-anism mainly based on π–π interactions and hydrogen bonding with the pendent groups is proposed. KW - Adsorption KW - Biobased polymers KW - Cycloaddition KW - Pentafluoropyridine KW - Phenolic compounds PY - 2022 DO - https://doi.org/10.1002/pat.5809 SN - 1042-7147 SP - 1 EP - 21 PB - Wiley online library AN - OPUS4-55389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brockmann, N. A1 - Sicken, A. A1 - Krüger, Jörg T1 - Effects of laser cleaning on the condition of different silk model samples using varying wavelengths and pulse durations N2 - The cleaning of aged silk fibers poses a common challenge in the conservation of textiles, since traditional cleaning techniques often yield unsatisfactory results or even harm objects. In this regard, cleaning objects with laser radiation is a promising addition to the range of available methods. Due to it being contactless, even brittle and touch-sensitive objects with disfiguring or harmful soiling could potentially be cleaned and therefore made accessible for research and presentation. Examples of treatment have sometimes shown spectacular results. Still there is some skepticism concerning the safety of this treatment for textile materials, which has been strengthened through previous 532 nm wavelength nanosecond laser cleaning studies on silk fibers. Taking these published results into account, the range of examined laser parameters has been extended in this study, from 532 nm nanosecond laser to 1064 nm nanosecond and even 800 nm femtosecond laser, reevaluating the effect of this treatment on the fibers. The physicochemical processes taking place on the silk fibers when cleaning with lasers are complex and still not fully understood. The aim of this project was therefore to bring more clarification about potential effects of those processes on the condition of silk samples treated with a set of different parameters for wavelength, pulse duration, energy density and number of pulses per spot. It also looks at the influence of the presence of soiling on the results. The analysis of potential effects was then carried out using statistical methods and advanced analytics. Scanning electron microscopy, Fourier-transform infrared spectroscopy and colorimetry technology provided the required insights to better assess the effects. Results show that laser cleaning of silk fibers, like most other conventional cleaning techniques, is not completely without risk, but knowing what the possible effects are helps making decisions on whether the benefits of the technique used justify these risks. KW - Laser cleaning KW - Cultural heritage KW - Conservation KW - Silk PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594601 DO - https://doi.org/10.1186/s40494-024-01152-1 SN - 2050-7445 VL - 12 IS - 1 SP - 1 EP - 15 PB - Springer AN - OPUS4-59460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Broicher, Cornelia A1 - Zeng, F. A1 - Pfänder, N. A1 - Frisch, M. A1 - Bisswanger, T. A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Palkovits, S. A1 - Beine, A. K. A1 - Palkovits, R. T1 - Iron and Manganese Containing Multi-Walled Carbon Nanotubes as Electrocatalysts for the Oxygen Evolution Reaction - Unravelling Influences on Activity and Stability N2 - Hydrogen economy is a central aspect of future energy supply, as hydrogen can be used as energy storage and fuel. In order tomake water electrolysis efficient, the limiting oxygen evolution reaction (OER) needs to be optimized. Therefore, C-based composite materials containing earth-abundant Fe and Mn were synthesized, characterized and tested in the OER. For pyrolysis temperatures above 700°C N-rich multi-walled carbon nanotubes (MWCNT) are obtained. Inside the tubes Fe3C particles are formed, Fe and Mn oxides are incorporated in the carbon matrix and metal spinel nanoparticles cover the outer surface. The best catalyst prepared at 800°C achieves a low overpotential of 389 mV (at 10 mA/cm2) and high stability (22.6 h). From electrochemical measurements and characterization it can be concluded that the high activity is mainly provided by MWCNT, Fe3C and the metal oxides in the conductive carbon matrix. The metal spinel nanoparticles in contrast protect the MWCNT from oxidation and thereby contribute to the high stability. KW - Oxygen Evolution Reaction KW - Carbon Nanotubes KW - Stability PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513955 DO - https://doi.org/10.1002/cctc.202000944 VL - 12 IS - 21 SP - 1 EP - 8 PB - Wiley Online Libary AN - OPUS4-51395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Broichert, C. A1 - Klingenhof, M. A1 - Frisch, M. A1 - Dresp, S. A1 - Kubo, N.M. A1 - Artz, J. A1 - Radnik, Jörg A1 - Palkovits, S. A1 - Beine, A.K. A1 - Strasser, P. A1 - Palkovits, R. T1 - Particle size-controlled synthesis of highperformance MnCo-based materials for alkaline OER at fluctuating potentials N2 - For the large-scale generation of hydrogen via water electrolysis the design of long term stable and active catalysts for the oxygen evolution reaction (OER) remains a key challenge. Most catalysts suffer from severe structural corrosion that becomes even more pronounced at fluctuating potentials. Herein, MnCo based cubic particles were prepared via a hydrothermal approach, in which the edge length of the micron-sized particles can be controlled by changing the pH value of the precursor solution. The cubes are composed of varying amounts of MnCo2O4, CoCO3 and a mixed (Mn/Co)CO3 phase. Structure–activity relationships were deduced revealing a volcano-type behavior for the intrinsic OER activity and fraction of spinel oxide phase. A low overpotential of 0.37 V at 10 mA cm−2 and a stability of more than 25 h was achieved in 1.0 M KOH using a rotating disc electrode (RDE) setup. The best performing catalyst material was successfully tested under dynamic process conditions for 9.5 h and shows a superior catalytic activity as anode for the Overall water splitting in an electrolyser setup in 1.0 M KOH at 333 K compared to a reference NiCo-spinel catalyst. KW - Water electrolysis KW - Oxygen evolution reaction KW - Structure activity relationships PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536050 DO - https://doi.org/10.1039/d1cy00905b SN - 2044-4753 VL - 11 IS - 12 SP - 7278 EP - 7286 PB - Royal Society of Chemistry AN - OPUS4-53605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruna, F. G. A1 - Prokop, M. A1 - Bystron, T. A1 - Loukrakpam, R. A1 - Melke, J. A1 - Lobo, C. M. S. A1 - Fink, M. A1 - Zhu, M. A1 - Voloshina, E. A1 - Kutter, M. A1 - Hoffmann, H. A1 - Yusenko, Kirill A1 - de Oliveira Guilherme Buzanich, Ana A1 - Röder, B. A1 - Bouzek, K. A1 - Paulus, B. A1 - Roth, C. T1 - Following adsorbed intermediates on a platinum gas diffusion electrode in H3PO3‑containing electrolytes using in situ X‑ray absorption spectroscopy N2 - One of the challenges of high-temperature polymer electrolyte membrane fuel cells is the poisoning of the Pt catalyst with H3PO4. H3PO4 is imbibed into the routinely used polybenzimidazole-based membranes, which facilitate proton conductivity in the temperature range of 120−200 °C. However, when leached out of the membrane by water produced during operation, H3PO4 adsorbs on the Pt catalyst surface, blocking the active sites and hindering the oxygen reduction reaction (ORR). The reduction of H3PO4 to H3PO3, which occurs at the anode due to a combination of a low potential and the presence of gaseous H2, has been investigated as an additional important contributing factor to the observed poisoning effect. H3PO3 has an affinity toward adsorption on Pt surfaces even greater than that of H2PO4 −. In this work, we investigated the poisoning effect of both H3PO3 and H3PO4 using a half-cell setup with a gas diffusion electrode under ambient conditions. By means of in situ X-ray absorption spectroscopy, it was possible to follow the signature of different species adsorbed on the Pt nanoparticle catalyst (H, O, H2PO4 −, and H3PO3) at different potentials under ORR conditions in various electrolytes (HClO4, H3PO4, and H3PO3). It was found that H3PO3 adsorbs in a pyramidal configuration P(OH)3 through a Pt−P bond. The competition between H3PO4 and H3PO3 adsorption was studied, which should allow for a better understanding of the catalyst poisoning mechanism and thus assist in the development of strategies to mitigate this phenomenon in the future by minimizing H3PO3 generation by, for example, improved catalyst design or adapted operation conditions or changes in the electrolyte composition. KW - H3PO4 life cycle KW - XAS KW - In situ coupling KW - High-temperature fuel cells KW - Δμ XANES KW - H3PO3 PY - 2022 DO - https://doi.org/10.1021/acscatal.2c02630 SN - 2155-5435 VL - 12 IS - 18 SP - 11472 EP - 11484 PB - ACS CY - Washington, DC AN - OPUS4-55815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Müller, P. A1 - Babick, F. A1 - Friedrich, C. M. A1 - Ghanem, A. A1 - Hodoroaba, Vasile-Dan A1 - Mech, A. A1 - Weigel, S. A1 - Wohlleben, W. A1 - Rauscher, H. T1 - NanoDefiner Framework and e-Tool Revisited According to the European Commission’s Nanomaterial Definition 2022/C 229/01 N2 - The new recommended definition of a nanomaterial, 2022/C 229/01, adopted by the European Commission in 2022, will have a considerable impact on European Union legislation addressing chemicals, and therefore tools to implement this new definition are urgently needed. The updated NanoDefiner framework and its e-tool implementation presented here are such instruments, which help stakeholders to find out in a straightforward way whether a material is a nanomaterial or not. They are two major outcomes of the NanoDefine project, which is explicitly referred to in the new definition. This work revisits the framework and e-tool, and elaborates necessary adjustments to make these outcomes applicable for the updated recommendation. A broad set of case studies on representative materials confirms the validity of these adjustments. To further foster the sustainability and applicability of the framework and e-tool, measures for the FAIRification of expert knowledge within the e-tool’s knowledge base are elaborated as well. The updated framework and e-tool are now ready to be used in line with the updated recommendation. The presented approach may serve as an example for reviewing existing guidance and tools developed for the previous definition 2011/696/EU, particularly those adopting NanoDefine project outcomes. KW - Nanomaterial definition KW - Nanomaterial categorisation KW - Nanomaterial regulation KW - Nanomaterial legislation KW - Decision support KW - FAIRification PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571618 DO - https://doi.org/10.3390/nano13060990 SN - 2079-4991 VL - 13 IS - 6 - Special Issue "Identification and Quantification of Nanomaterials" SP - 1 EP - 16 PB - MDPI CY - Basel, CH AN - OPUS4-57161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bugel, S. A1 - Hahnel, M. A1 - Kunde, T. A1 - de Sousa Amadeu, Nader A1 - Sun, Y. A1 - Spieß, A. A1 - Beglau, T. H. Y. A1 - Janiak, C. A1 - Schmidt, B. M. T1 - Synthesis and Characterization of a Crystalline Imine-Based Covalent Organic Framework with Triazine Node and Biphenyl Linker and Its Fluorinated Derivate for CO2/CH4 Separation N2 - A catalyst-free Schiff base reaction was applied to synthesize two imine-linked covalent organic frameworks (COFs). The condensation reaction of 1,3,5-tris-(4-aminophenyl)triazine (TAPT) with 4,4′-biphenyldicarboxaldehyde led to the structure of HHU-COF-1 (HHU = Heinrich-Heine University). The fluorinated analog HHU-COF-2 was obtained with 2,2′,3,3′,5,5′,6,6′-octafluoro-4,4′-biphenyldicarboxaldehyde. Solid-state NMR, infrared spectroscopy, X-ray photoelectron spectroscopy, and elemental analysis confirmed the successful formation of the two network structures. The crystalline materials are characterized by high Brunauer–Emmett–Teller surface areas of 2352 m2/g for HHU-COF-1 and 1356 m2/g for HHU-COF-2. The products of a larger-scale synthesis were applied to prepare mixed-matrix membranes (MMMs) with the polymer Matrimid. CO2/CH4 permeation tests revealed a moderate increase in CO2 permeability at constant selectivity for HHU-COF-1 as a dispersed phase, whereas application of the fluorinated COF led to a CO2/CH4 selectivity increase from 42 for the pure Matrimid membrane to 51 for 8 wt% of HHU-COF-2 and a permeability increase from 6.8 to 13.0 Barrer for the 24 wt% MMM. KW - MOF KW - Filter PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547632 DO - https://doi.org/10.3390/ma15082807 SN - 1996-1944 VL - 15 IS - 8 SP - 1 EP - 18 PB - MDPI AN - OPUS4-54763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bui, M. A1 - Hoffmann, K. F. A1 - Braun, T. A1 - Riedel, S. A1 - Heinekamp, Christian A1 - Scheurell, K. A1 - Scholz, G. A1 - Stawski, Tomasz A1 - Emmerling, Franziska T1 - An Amorphous Teflate Doped Aluminium Chlorofluoride: A Solid Lewis-Superacid for the Dehydrofluorination of Fluoroalkanes N2 - Ananion-dopedaluminiumchlorofluoride AlCl0.1F2.8(OTeF5)0.1(ACF-teflate) was synthesized.The material contains pentafluor-oorthotellurate(teflate)groups, which mimic fluoride ions electronically, but are sterically more demanding. They are embedded into the amorphous structure. The latter was studied by PDF analysis, EXAFS data and MAS NMR spectroscopy. The mesoporous powder is a Lewis superacid, and ATR-IR spectra of adsorbed CD3CN reveal a blue-shift of the adsorption band by73 cm-1, which is larger than the shift for SbF5. Remarkably,ACF-teflate catalyzes dehydrofluorination reactions of mono-fluoroalkanes to yield olefins in C6D6. In these cases,no Friedel-Crafts products were formed. KW - Aluminium fluorides KW - Aluminium teflates KW - C-F bond activation KW - Lewis superacids KW - Silanes PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572290 DO - https://doi.org/10.1002/cctc.202300350 SN - 1867-3880 SP - 1 EP - 7 PB - Wiley VHC-Verlag AN - OPUS4-57229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bui, Minh A1 - Heinekamp, Christian A1 - Fuhry, Emil A1 - Weidner, Steffen A1 - Radnik, Jörg A1 - Ahrens, Mike A1 - Scheurell, Kerstin A1 - Balasubramanian, Kannan A1 - Emmerling, Franziska A1 - Braun, Thomas T1 - Lewis-acid induced mechanochemical degradation of polyvinylidene fluoride: transformation into valuable products N2 - Polyvinylidene fluoride (–[CH2CF2]n–, PVDF) waste poses significant environmental challenges due to its recalcitrant nature and widespread use. This study addresses the end-of-life management of PVDF by introducing a novel, sustainable mechanochemical approach for its valorisation. We investigated the degradation of PVDF into value-added materials using ball milling with anhydrous AlCl3 to achieve a quantitative mineralisation producing AlF3 and halide-functionalised graphite, along with gaseous products (HCl and CH4). Mechanistic key steps involve Lewis-acid catalysed C–F bond activation, dehydrofluorination and aromatisation. This approach provides an effective solution for PVDF waste management while offering a promising route for the production of high-value materials from polymer waste streams. Our findings contribute to sustainable practices in polymer recycling and resource recovery, respond to pressing environmental concerns associated with fluoropolymer disposal, and demonstrate the potential to convert polymer wastes into useful products. KW - Mechanochemistry KW - Polyvinylidenfluoride KW - Degradation KW - Ball mill PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649015 DO - https://doi.org/10.1039/d5sc05783c SN - 2041-6520 VL - 16 IS - 40 SP - 18903 EP - 18910 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bustos, Jenna A1 - Shohel, Mohammad A1 - Guilherme Buzanich, Ana A1 - Zakharov, Lev A1 - Buils, Jordi A1 - Segado‐Centellas, Mireia A1 - Bo, Carles A1 - Nyman, May T1 - Technetium and Rhenium Auto‐reduction, Polymerization and Lability towards Group VII Polyoxometalate Chemistry N2 - AbstractGroup VII Tc and Re have long been studied to develop both radiopharmaceuticals and technologies for nuclear materials management. Fundamental research has targeted understanding this periodic table crossroads where polyoxometalates meets metal‐metal bonded complexes. Here we have isolated green hygroscopic and metastable crystals of (ReVI,oct)2(ReVII,tet)2(OH)2(O)12⋅H2O (ReVI,VII‐green, tet=tetrahedral, oct=octahedral), determined by single‐crystal x‐ray diffraction. In addition to color, Re‐L1 X‐ray absorption near‐edge spectroscopy confirms the reduced oxidation state. ReVI,VII‐green provides the first demonstration of Re autoreduction, long‐observed for Mn and Tc. We also isolated and structurally characterized [Tc4O4(H2O)2(ReO4)14]2− (Tc4Re14) polyanion crystals that contain Tc(V) and Re(VII), consistent with greater stability of reduced Tc compared to reduced Re. Small angle X‐ray scattering of both compounds and prior‐reported polyanion [Tc4O4(H2O)2(TcO4)14]4− (Tc20) dissolved in acetonitrile indicated a qualitative lability order of oxo‐linkages of Re‐O−Re Re‐O−Tc Tc‐O−Tc, and lability of Tc20 was also probed by 99Tc nuclear magnetic resonance spectroscopy. Computation provided insight into 99Tc chemical shifts as well as lability. Based on both reducibility and solution phase dynamics of polynuclear compounds investigated here, Re is an imperfect surrogate for Tc, and further expansion of group VII polyoxometalate chemistry seems promising. KW - XANES KW - Polyoxometalate KW - Technetium PY - 2025 DO - https://doi.org/10.1002/chem.202404144 SN - 0947-6539 VL - 31 IS - 21 SP - 1 EP - 7 PB - Wiley-VCH Verl. AN - OPUS4-65491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bäßler, Ralph A1 - Amela Keserović, Amela A1 - Sobetzki, Joana A1 - Sarmiento Klapper, Helmuth A1 - Dimper, Matthias T1 - Geeignete Werkstoffe für Geothermieanwendungen (2) N2 - Durch Auslagerungs- und elektrochemische Tests im Labor kann das Korrosionsverhalten verschiedener metallener Werkstoffe beurteilt werden. Aus den Versuchsergebnissen, die in verschiedenen synthetischen Geothermalwässern im Labor erzielt wurden, lassen sich die folgenden Schlussfolgerungen ziehen: • Die Anfälligkeit für Spaltkorrosion wurde als wichtigster Aspekt für die Werkstoffqualifizierung ermittelt. • Der niedriglegierte Stahl 25CrMo4 zeigte bei niedrigem Salzgehalt in MB-Geothermalwasser eine gleichmäßige Korrosion unterhalb der akzeptierten Schwelle von 0,3 mm/Jahr. Daher kann er als geeignet für geothermische Bedingungen mit niedrigem Salzgehalt angesehen werden, wie sie für MB getestet wurden. Es besteht keine Notwendigkeit, auf höherlegierte (teurere) Werkstoffe auszuweichen. Ein niedrigerer pH-Wert (wie bei LHD) führt zu Korrosionsraten oberhalb der akzeptablen Grenzwerte, so dass die niedriglegierten Werkstoffe nicht für Flüssigkeiten mit niedrigem pH-Wert geeignet sind. • Stark salzhaltige Geothermalwässer erfordern höherlegierte Werkstoffe, da die Korrosionsrate von niedriglegiertem Stahl zu hoch ist. • Der Duplexstahl X2CrNiMo22-5-3 und der Superduplexstahl X2CrNiMoCuWN25-7-4 wurden aufgrund ihrer kritischen Anfälligkeit für örtliche Korrosion in Form von Loch- und Spaltkorrosion unter Betriebsbedingungen nicht als geeignet für geothermische Anwendungen in Geothermalwässern mit einer mit NDB und ORG vergleichbaren Zusammensetzung angesehen. • Der superaustenitische Stahl X1CrNiMoCu32-28-7 eignet sich für ORG und salzarme Wässer. In NDB-Geothermalwasser wurde er bei 100 °C als geeignet angesehen. Jedoch schränkt seine Anfälligkeit für Spaltkorrosion seine Anwendbarkeit ein. Neben seiner guten Korrosionsbeständigkeit ist sein Repassivierungsverhalten für seine begrenzte Anwendbarkeit in Geothermalwässern mit niedrigem pH-Wert verantwortlich. • Die Nickelbasislegierung NiCr23Mo16Al wurde als geeignet erachtet und stellt eine sichere Option für den Einsatz in geothermischen Anlagen dar, selbst wenn mit stark salzhaltigem Geothermalwasser gearbeitet wird. KW - Geothermie KW - Korrosion KW - Legierungen KW - Anlagensicherheit PY - 2024 SN - 0016-4232 VL - 2024 IS - 3 SP - 370 EP - 374 PB - Eugen G. Leuze Verlag CY - Bad Saulgau AN - OPUS4-59997 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bäßler, Ralph A1 - Amela Keserović, Amela A1 - Sobetzki, Joana A1 - Sarmiento Klapper, Helmuth A1 - Dimper, Matthias T1 - Geeignete Werkstoffe für Geothermieanwendungen (1) N2 - Durch Auslagerungs- und elektrochemische Tests im Labor kann das Korrosionsverhalten verschiedener metallener Werkstoffe beurteilt werden. Aus den Versuchsergebnissen, die in verschiedenen synthetischen Geothermalwässern im Labor erzielt wurden, lassen sich die folgenden Schlussfolgerungen ziehen: • Die Anfälligkeit für Spaltkorrosion wurde als wichtigster Aspekt für die Werkstoffqualifizierung ermittelt. • Der niedriglegierte Stahl 25CrMo4 zeigte bei niedrigem Salzgehalt in MB-Geothermalwasser eine gleichmäßige Korrosion unterhalb der akzeptierten Schwelle von 0,3 mm/Jahr. Daher kann er als geeignet für geothermische Bedingungen mit niedrigem Salzgehalt angesehen werden, wie sie für MB getestet wurden. Es besteht keine Notwendigkeit, auf höherlegierte (teurere) Werkstoffe auszuweichen. Ein niedrigerer pH-Wert (wie bei LHD) führt zu Korrosionsraten oberhalb der akzeptablen Grenzwerte, so dass die niedriglegierten Werkstoffe nicht für Flüssigkeiten mit niedrigem pH-Wert geeignet sind. • Stark salzhaltige Geothermalwässer erfordern höherlegierte Werkstoffe, da die Korrosionsrate von niedriglegiertem Stahl zu hoch ist. • Der Duplexstahl X2CrNiMo22-5-3 und der Superduplexstahl X2CrNiMoCuWN25-7-4 wurden aufgrund ihrer kritischen Anfälligkeit für örtliche Korrosion in Form von Loch- und Spaltkorrosion unter Betriebsbedingungen nicht als geeignet für geothermische Anwendungen in Geothermalwässern mit einer mit NDB und ORG vergleichbaren Zusammensetzung angesehen. • Der superaustenitische Stahl X1CrNiMoCu32-28-7 eignet sich für ORG und salzarme Wässer. In NDB-Geothermalwasser wurde er bei 100 °C als geeignet angesehen. Jedoch schränkt seine Anfälligkeit für Spaltkorrosion seine Anwendbarkeit ein. Neben seiner guten Korrosionsbeständigkeit ist sein Repassivierungsverhalten für seine begrenzte Anwendbarkeit in Geothermalwässern mit niedrigem pH-Wert verantwortlich. • Die Nickelbasislegierung NiCr23Mo16Al wurde als geeignet erachtet und stellt eine sichere Option für den Einsatz in geothermischen Anlagen dar, selbst wenn mit stark salzhaltigem Geothermalwasser gearbeitet wird. KW - Geothermie KW - Korrosion KW - Legierungen KW - Anlagensicherheit PY - 2024 SN - 0016-4232 VL - 2024 IS - 2 SP - 240 EP - 243 PB - Eugen G. Leuze Verlag CY - Bad Saulgau AN - OPUS4-59996 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Béalu, Zoé A1 - Walther, Johanna A1 - Abusafia, Attaallah A1 - Altmann, Korinna A1 - Meurer, Maren A1 - Gretzschel, Oliver A1 - Schäfer, Michael A1 - Steinmetz, Heidrun T1 - Removal of Organic Micropollutants and Microplastics via Ozonation Followed by Granular Activated Carbon Filtration N2 - Discharge from Wastewater Treatment Plants (WWTPs) can result in the emission of organic micropollutants (OMPs) and microplastics (MPs) into the aquatic environment. To prevent this harmful release, a pilot plant consisting of an ozonation followed by a granular activated carbon (GAC) filter was operated at a WWTP in Germany, and its side-effects on the concentrations of nitrogen (N) and phosphorous (P) compounds were measured. Over 80% of OMPs and transformation products were removed during the operating time (around 6000 bed volumes) no matter the ozone dose (from around 0.1 to 0.5 mgO3/mgDOC), except for Diatrizoic acid, whose breakthrough appeared at 3500 BV. Formation of the oxidation by-product, NDMA, increased with higher ozone doses, but the concentration remained below 100 ng/L. Bromate was formed at a higher ozone dose (0.4 mgO3/mgDOC) but at a low concentration—below 10 µg/L. The MP particles detected in the inflow (PE, SBR, PP, and PS) were effectively eliminated to a high degree, with a removal rate of at least 92%. Carbon parameters (COD, DOC, and SAC254) were removed further by the pilot plant, but to different extents. As expected, nitrate was formed during ozonation, while nitrite’s concentration decreased. Further, nitrite decreased and nitrate increased within the GAC filter, while ammonium was eliminated by at least 90%. Total P concentration decreased after the pilot, but the concentration of PO4-P increased. KW - Microplastics KW - TED-GC/MS KW - Granular Activated Carbon Filtration KW - Removal of Organic Micropollutants KW - Wastewater treatment plant PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615209 DO - https://doi.org/10.3390/environments11110241 VL - 11 IS - 11 SP - 1 EP - 38 PB - MDPI AG AN - OPUS4-61520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böttcher, Katrin A1 - Kraft, Sebastian A1 - Weise, Matthias A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - X-ray emission during ultrafast laser grooving N2 - Ultrashort pulse lasers offer the possibility to process materials with minimal heat input and high precision. However, the X-ray emission at high laser peak intensities represents an undesirable side effect. A laser system (1030 nm wavelength, 40 W maximum average laser power, 925 fs pulse duration, 100 μJ maximum pulse energy, 400 kHz pulse repetition frequency) was used to analyze the X-ray skin dose rates for applied peak intensities between 9.2 × 10^12 W/cm^2 and 1.3 × 10^14 W/cm^2 for mild steel, stainless steel and tungsten during groove processing. The lowest laser peak intensity at which X-ray emission could be measured was 9.2 × 10^12 W/cm^2 for processing of stainless steel. The X-ray emission showed a characteristic evolution in dependence on the number of overscans at the same line positions. For low peak intensities, a measurable X-ray emission only begins after a few passes. The number of scans to reach the maximum dose rate increases with lower laser peak intensity. Analysis of the evolving surface topography by white light interference microscopy in connection with ray-tracing simulations led to the interpretation that the increase in X-ray emission is due to the local intensity redistribution by multiple reflection within the laser-generated grooves which is promoted by a particular choice of the linear laser polarization. KW - Ultrashort pulsed laser KW - Laser-induced X-rays KW - X-ray hazard KW - X-ray emission PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639483 DO - https://doi.org/10.1007/s00339-025-08728-z SN - 1432-0630 VL - 131 IS - 8 SP - 1 EP - 12 PB - Springer CY - Berlin AN - OPUS4-63948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böttcher, Katrin A1 - Schmitt Rahner, M. A1 - Stolzenberg, U. A1 - Kraft, Sebastian A1 - Bonse, Jörn A1 - Feist, C. A1 - Albrecht, D. A1 - Pullner, B. A1 - Krüger, Jörg T1 - Worst-case X-ray photon energies in ultrashort pulse laser processing N2 - Ultrashort pulse laser processing can result in the secondary generation of unwanted X-rays if a critical laser irradiance of about 10^13 W/cm^2 is exceeded. Spectral X-ray emissions were investigated during the processing of tungsten and steel using three complementary spectrometers (based on CdTe and silicon drift detectors) simultaneously for the identification of a worst-case spectral scenario. Therefore, maximum X-ray photon energies were determined, and corresponding dose equivalent rates were calculated. An ultrashort pulse laser workstation with a pulse duration of 274 fs, a center wavelength of 1030 nm, pulse repetition rates between 50 kHz and 200 kHz, and a Gaussian laser beam focused to a spot diameter of 33 µm was employed in a single pulse and burst laser operation mode. Different combinations of laser pulse energy and repetition rate were utilized, keeping the average laser power constant close to the maximum power of 20 W. Peak irradiances ranging from 7.3 × 10^13 W/cm^2 up to 3.0 × 10^14 W/cm^2 were used. The X-ray dose equivalent rate increases for lower repetition rates and higher pulse energy if a constant average power is used. Laser processing with burst mode significantly increases the dose rates and the X-ray photon energies. A maximum X-ray photon energy of about 40 keV was observed for burst mode processing of tungsten with a repetition rate of 50 kHz and a peak irradiance of 3 × 10^14 W/cm^2. KW - Ultrashort pulsed laser KW - X-ray emission KW - X-ray spectrum KW - X-ray energies KW - Radiation protection PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-566176 DO - https://doi.org/10.3390/ma15248996 VL - 15 IS - 24 SP - 1 EP - 17 PB - MDPI AN - OPUS4-56617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bügel, Stefanie A1 - Hähnel, Malte A1 - Kunde, Tom A1 - de Sousa Amadeu, Nader A1 - Sun, Yangyang A1 - Spieß, Alex A1 - Beglau, Thi Hai Yen A1 - Schmidt, Bernd M. A1 - Janiak, Christoph T1 - Synthesis and Characterization of a Crystalline Imine-Based Covalent Organic Framework with Triazine Node and Biphenyl Linker and Its Fluorinated Derivate for CO2/CH4 Separation N2 - : A catalyst-free Schiff base reaction was applied to synthesize two imine-linked covalent organic frameworks (COFs). The condensation reaction of 1,3,5-tris-(4-aminophenyl)triazine (TAPT) with 4,40-biphenyldicarboxaldehyde led to the structure of HHU-COF-1 (HHU = Heinrich-Heine University). The fluorinated analog HHU-COF-2 was obtained with 2,20,3,30,5,50,6,60-octafluoro 4,40 -biphenyldicarboxaldehyde. Solid-state NMR, infrared spectroscopy, X-ray photoelectron spectroscopy, and elemental analysis confirmed the successful formation of the two network structures. The crystalline materials are characterized by high Brunauer–Emmett–Teller surface areas of 2352 m2/g for HHU-COF-1 and 1356 m2/g for HHU-COF-2. The products of a larger-scale synthesis were applied to prepare mixed-matrix membranes (MMMs) with the polymer Matrimid. CO2/CH4 permeation tests revealed a moderate increase in CO2 permeability at constant selectivity for HHU-COF-1 as a dispersed phase, whereas application of the fluorinated COF led to a CO2/CH4 selectivity increase from 42 for the pure Matrimid membrane to 51 for 8 wt% of HHU-COF-2 and a permeability increase from 6.8 to 13.0 Barrer for the 24 wt% MMM KW - Separation KW - COF KW - MMM KW - CO2 PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618625 DO - https://doi.org/10.3390/ma15082807 VL - 15 IS - 8 SP - 2807 PB - MDPI AN - OPUS4-61862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - C. Pardo Pérez, L. A1 - Arndt, A. A1 - Stojkovikj, S. A1 - Y. Ahmet, I. A1 - T. Arens,, J. A1 - Dattila, F. A1 - Wendt, R. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Davies, V. A1 - Höflich, K. A1 - Köhnen, E. A1 - Tockhorn, P. A1 - Golnak, R. A1 - Xiao, J. A1 - Schuck, G. A1 - Wollgarten, M. A1 - López, N. A1 - T. Mayer, M. T1 - Determining Structure-Activity Relationships in Oxide Derived CuSn Catalysts During CO2 Electroreduction Using X-Ray Spectroscopy N2 - The development of earth-abundant catalysts for selective electrochemical CO2 conversion is a central challenge. Cu-Sn bimetallic catalysts can yield selective CO2 reduction toward either CO or formate. This study presents oxide-derived Cu-Sn catalysts tunable for either product and seeks to understand the synergetic effects between Cu and Sn causing these selectivity trends. The materials undergo significant transformations under CO2 reduction conditions, and their dynamic bulk and surface structures are revealed by correlating observations from multiple methods—X-ray absorption spectroscopy for in situ study, and quasi in situ X-ray photoelectron spectroscopy for surface sensitivity. For both types of catalysts, Cu transforms to metallic Cu0 under reaction conditions. However, the Sn speciation and content differ significantly between the catalyst types: the CO-selective catalysts exhibit a surface Sn content of 13 at. % predominantly present as oxidized Sn, while the formate-selective catalysts display an Sn content of ≈70 at. % consisting of both metallic Sn0 and Sn oxide species. Density functional theory simulations suggest that Snδ+ sites weaken CO adsorption, thereby enhancing CO selectivity, while Sn0 sites hinder H adsorption and promote formate production. This study reveals the complex dependence of catalyst structure, composition, and speciation with electrochemical bias in bimetallic Cu catalysts. KW - Electrochemical CO2 conversion KW - Cu catalysts KW - X-ray absorption spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547116 DO - https://doi.org/10.1002/aenm.202103328 SN - 1614-6832 VL - 12 IS - 5 SP - 2103328 PB - Wiley-VCH GmbH AN - OPUS4-54711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cakir, Cafer Tufan A1 - Bogoclu, Can A1 - Emmerling, Franziska A1 - Streli, Christina A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin T1 - Machine learning for efficient grazing-exit x-ray absorption near edge structure spectroscopy analysis: Bayesian optimization approach N2 - In materials science, traditional techniques for analyzing layered structures are essential for obtaining information about local structure, electronic properties and chemical states. While valuable, these methods often require high vacuum environments and have limited depth profiling capabilities. The grazing exit x-ray absorption near-edge structure (GE-XANES) technique addresses these limitations by providing depth-resolved insight at ambient conditions, facilitating in situ material analysis without special sample preparation. However, GE-XANES is limited by long data acquisition times, which hinders its practicality for various applications. To overcome this, we have incorporated Bayesian optimization (BO) into the GE-XANES data acquisition process. This innovative approach potentially reduces measurement time by a factor of 50. We have used a standard GE-XANES experiment, which serve as reference, to validate the effectiveness and accuracy of the BO-informed experimental setup. Our results show that this optimized approach maintains data quality while significantly improving efficiency, making GE-XANES more accessible to a wider range of materials science applications. KW - Machine Learning KW - GE-XANES KW - Bayesian Optimization PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603955 DO - https://doi.org/10.1088/2632-2153/ad4253 VL - 5 IS - 2 SP - 1 EP - 12 PB - IOP Publishing AN - OPUS4-60395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cakir, Cafer Tufan A1 - Piotrowiak, T. A1 - Reinholz, Uwe A1 - Ludwig, A. A1 - Emmerling, Franziska A1 - Streli, C. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin T1 - Exploring the Depths of Corrosion: A Novel GE-XANES Technique for Investigating Compositionally Complex Alloys N2 - In this study, we propose the use of nondestructive, depth-resolved, element-specific characterization using grazing exit X-ray absorption near-edge structure spectroscopy (GE-XANES) to investigate the corrosion process in compositionally complex alloys (CCAs). By combining grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry and a pnCCD detector, we provide a scanning-free, nondestructive, depth-resolved analysis in a sub-micrometer depth range, which is especially relevant for layered materials, such as corroded CCAs. Our setup allows for spatial and energy-resolved measurements and directly extracts the desired fluorescence line, free from scattering events and other overlapping lines. We demonstrate the potential of our approach on a compositionally complex CrCoNi alloy and a layered reference sample with known composition and specific layer thickness. Our findings indicate that this new GE-XANES approach has exciting opportunities for studying surface catalysis and corrosion processes in real-world materials. KW - Degradation mechanisms KW - Grazin exit XANES KW - Depth resolved XANES KW - Compositional complex alloys KW - Corrosion PY - 2023 DO - https://doi.org/10.1021/acs.analchem.3c00404 VL - 95 SP - 4810 EP - 4818 PB - ACS Publications AN - OPUS4-57823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Campbell, C. G. A1 - Jordon Astorga, D. A1 - Dümichen, Erik A1 - Celina, M. T1 - Thermoset materials characterization by thermal desorption or pyrolysis based gas chromatography-mass spectrometry methods N2 - Thermoset materials characterization is often limited to solid state analytical techniques such as IR, NMR, DSC, TGA and mechanical testing. Alternatively, their off-gassing behavior can also be evaluated using GC based techniques such as TD-GC-MS, allowing this method to be applied to thermoset materials analyses such as identification, aging characterization, and formulation optimization. As an overview, common thermoset materials were evaluated by analyzing their gaseous degradation products via TGA-based pyrolysis and subsequent TD-GC-MS for the identification of representative volatile signatures. It is thereby possible to distinguish different classes of phenolic materials or cured epoxy resins, as well as their amine or anhydride curatives. Additionally, this method enabled quantification of a volatile fragment (bisphenol A, BPA) which is associated with oxidation of epoxy/amine thermoset materials. The amount of evolved BPA increased linearly with aging time and this trend exhibits linear Arrhenius behavior over the temperature range (80–125 °C) studied, in agreement with oxidation sensitivies based on oxygen consumption data. Further, TD-GC-MS was used to explore how off-gassing of residual anhydride curative from an epoxy/anhydride material depends on formulation stoichiometry. Even in formulations that theoretically contained enough epoxy to consume all anhydride (1:1 stoichiometry), an imperfect final cure state resulted in residual anhydride which could evolve from the material. For such materials, a slightly epoxy-rich formulation is required to ensure that the material contains no residual unreacted anhydride. Analysis of volatiles generated by thermal exposure is an attractive characterization approach enabling compositional analysis as well as complementary diagnostics for materials degradation. KW - Polymer analysis/characterization KW - Thermal desorption mass spectrometry KW - Thermoset composition KW - Volatiles from thermosets KW - Degradation signatures PY - 2020 DO - https://doi.org/10.1016/j.polymdegradstab.2019.109032 VL - 174 SP - 109032 PB - Elsevier Ltd. AN - OPUS4-50435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cancella, Erick Paiva A1 - de Paula Guarnieri, Guilherme A1 - de Sousa Amadeu, Nader A1 - Radtke, Martin A1 - Garcia, Rodrigo Henrique A1 - de Azevedo, Eduardo Ribeiro A1 - Cosentino, Ivana Conte A1 - Mascarenhas, Yvonne Primerano A1 - Nery, José Geraldo T1 - Synthesis and physicochemical characterization of a novel bismuth silicate templated by tetrapropylammonium bromide and polydiallyldimethylammonium chloride N2 - A bismuth silicate (BiSi-1) was hydrothermally synthesized using tetrapropylammonium bromide (TPA·Br) as the organic structure-directing agent and shown by multi-scale characterization to be distinct from known Bi–silicates. Powder X-ray diffraction is indexable with an orthorhombic metric (a = 23.234 Å, b = 17.109 Å, c = 3.897 Å), consistent with a highly anisotropic, possibly layered framework. High-resolution TEM/SAED reveals nanocrystalline, plate-like domains assembled into sub-micrometric aggregates with locally oriented lamellae; lattice fringes (0.27–0.32 nm) match the strongest XRD spacings. Solid-state NMR establishes a silica-rich network with a dominant Q4 population (77%) and minor Q3 (11%) and Q2 (12%) sites; the contact-time dependence of 1H to 29Si cross-polarization is consistent with increasing proximal-proton density from Q4 to Q2. Aging to 24 h sharpens the 29Si lineshape, while calcination progressively removes the OSDA and vicinal hydroxyls; at 750 °C, 29Si spectra indicate framework densification/rearrangement. XANES/EXAFS places bismuth predominantly as Bi3+ in an oxide-like environment with a pronounced Bi–O first shell and no detectable Bi⁰ or Bi–Br contributions. ICP–OES yields a reproducible Bi/Si atomic ratio of 1:3. Thermogravimetry shows stepwise desorption, dehydroxylation, and template removal, with thermal stability maintained to 750 °C. Nitrogen sorption confirms mesoporosity in the as-made and Soxhlet-extracted solids (the latter exhibiting the highest surface area), whereas high-temperature calcination reduces porosity. Collectively, BiSi-1 emerges as a nanocrystalline, anisotropic Bi–silicate whose connectivity, local Bi–O environment, and accessible texture are tunable by aging and post-treatments, positioning it as a promising platform for heterogeneous catalysis and environmental remediation. KW - 29Si NMR KW - Bismuth KW - Silicate PY - 2025 DO - https://doi.org/10.1007/s10853-025-11732-6 SN - 0022-2461 VL - 60 IS - 45 SP - 22615 EP - 22635 PB - Springer Science and Business Media LLC AN - OPUS4-64755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cano Murillo, Natalia A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Emamverdi, Farnaz A1 - Cacua, K. A1 - Hodoroaba, Vasile-Dan A1 - Sturm, Heinz T1 - Carrier Fibers for the Safe Dosage of Nanoparticles in Nanocomposites: Nanomechanical and Thermomechanical Study on Polycarbonate/Boehmite Electrospun Fibers Embedded in Epoxy Resin N2 - The reinforcing effect of boehmite nanoparticles (BNP) in epoxy resins for fiber composite lightweight construction is related to the formation of a soft but bound interphase between filler and polymer. The interphase is able to dissipate crack propagation energy and consequently increases the fracture toughness of the epoxy resin. Usually, the nanoparticles are dispersed in the resin and then mixed with the hardener to form an applicable mixture to impregnate the fibers. If one wishes to locally increase the fracture toughness at particularly stressed positions of the fiber-reinforced polymer composites (FRPC), this could be done by spraying nanoparticles from a suspension. However, this would entail high costs for removing the nanoparticles from the ambient air. We propose that a fiber fleece containing bound nanoparticles be inserted at exposed locations. For the present proof-of-concept study, an electrospun polycarbonate nonwoven and taurine modified BNP are proposed. After fabrication of suitable PC/EP/BNP composites, the thermomechanical properties were tested by dynamic mechanical analysis (DMA). Comparatively, the local nanomechanical properties such as stiffness and elastic modulus were determined by atomic force microscopy (AFM). An additional investigation of the distribution of the nanoparticles in the epoxy matrix, which is a prerequisite for an effective nanocomposite, is carried out by scanning electron microscopy in transmission mode (TSEM). From the results it can be concluded that the concept of carrier fibers for nanoparticles is viable. KW - Advanced materials KW - Electrospun nanocomposite fiber KW - Nanomechanical charecteisation KW - Nanosafety KW - Epoxy nanocomposites PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528265 DO - https://doi.org/10.3390/nano11061591 VL - 11 IS - 6 SP - 1591 PB - MDPI CY - CH - 4020 Basel, Switzerland AN - OPUS4-52826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -