TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, Rita A1 - Faglioni, Francesco A1 - Bruno, Giovanni T1 - A Complete Strategy to Achieve High Precision Automatic Segmentation of Challenging Experimental X‐Ray Computed Tomography Data Using Low‐Resemblance Synthetic Training Data N2 - It is shown that preconditioning of experimental X‐ray computed tomography (XCT) data is critical to achieve high‐precision segmentation scores. The challenging experimental XCT datasets and deep convolutional neural networks (DCNNs) are used that are trained with low‐resemblance synthetic XCT data. The material used is a 6‐phase Al–Si metal matrix composite‐reinforced with ceramic fibers and particles. To achieve generalization, in our past studies, specific data augmentation techniques were proposed for the synthetic XCT training data. In addition, two toolsets are devised: (1) special 3D DCNN architecture (3D Triple_UNet), slicing the experimental XCT data from multiple views (MultiView Forwarding), the i.S.Sy.Da.T.A. iterative segmentation algorithm, and (2) nonlocal means (NLM) conditioning (filtering) for the experimental XCT data. This results in good segmentation Dice scores across all phases compared to more standard approaches (i.e., standard UNet architecture, single view slicing, standard single training, and NLM conditioning). Herein, the NLM filter is replaced with the deep conditioning framework BAM SynthCOND introduced in a previous publication, which can be trained with synthetic XCT data. This leads to a significant segmentation precision increase for all phases. The proposed methods are potentially applicable to other materials and imaging techniques. KW - Automatic Segmentation KW - XCT KW - Artificial Intelligence KW - Synthetic Training Data KW - i.S.Sy.Da.T.A. KW - BAM SynthMAT KW - BAM SynthCOND KW - Triple UNet KW - Convolutional Neural Network (DCNN) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590912 DO - https://doi.org/10.1002/adem.202301030 SN - 1438-1656 VL - 26 IS - 2 SP - 1 EP - 9 PB - Wiley online library AN - OPUS4-59091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Spitzer, Stefan A1 - Riesner, G. A1 - Zakel, S. A1 - Schierding, C. T1 - A New Ignition Source for the Determination of Safety Characteristics of Gases N2 - Safety characteristics are used to keep processes, including flammable gases, vapors, and combustible dusts, safe. In the standards for the determination of safety characteristics of gases and vapors, the induction spark is commonly used. However, classic transformers are hard to obtain, and replacement with new electronic transformers is not explicitly allowed in the standards. This article presents the investigation of five gases that are normally used to calibrate devices for the determination of safety characteristics, the maximum experimental safe gap (MESG), with an electronic transformer, and the values are compared to the ones that are obtained with the standard transformer. Additionally, calorimetric measurements on the net energy of both ignition sources were performed as well as open-circuit voltage measurements. It is concluded that the classic type of transformer can be replaced by the new type obtaining the same results for the MESG and introducing the same amount of energy into the system. KW - Safety characteristics KW - Ignition sources KW - MESG PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578528 DO - https://doi.org/10.3390/gases3030007 VL - 3 IS - 3 SP - 106 EP - 111 PB - MDPI CY - Basel AN - OPUS4-57852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sano, Silvia Di A1 - Costa, Giancarlo A1 - Giordano, Pier Francesco A1 - Pregnolato, Maria A1 - Limongelli, Maria Pina T1 - Multi‐risk assessment for bridges: The application of the Italian Guidelines N2 - Bridges are essential elements in the built environment since they underpin the functioning of transportation systems. Nevertheless, they are vulnerable due to aggressive environment, demand beyond the design level, and other contingencies such as extreme events. The management of bridges represents a significant challenge for improving transport performance and ensure the safety of users. In Italy, bridge management is addressed by the recent “Guidelines for risk classification and management, safety evaluation and monitoring of existing bridges” which were issued by the Italian Ministry for Public Work in 2020. The guidelines propose an operational approach with distinctive characteristics: (i) risk‐based, i.e., based on the typical parameters of hazard, vulnerability, and exposure; (ii) multi‐level, i.e., they include six assessment levels (0‐5) of increasing complexity; and (iii) multi‐risk, i.e., they assess structural/foundation, seismic, hydrological and landslide risk. This paper presents a general overview of the 2020 Italian Guidelines and their application to a selected case study. Lessons from the application to the case study are drafted and possible criticalities highlighted. KW - Bridge management KW - Infrastructures KW - Italian guidelines KW - Structural safety KW - Risk assessment KW - Risk classification PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653392 DO - https://doi.org/10.1002/cepa.2046 SN - 2509-7075 VL - 6 IS - 5 SP - 772 EP - 779 PB - Wiley CY - Berlin AN - OPUS4-65339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Kannengießer, Thomas T1 - Rapid solidification during welding of duplex stainless steels – in situ measurement of the chemical concentration by Laser-Induced Breakdown Spectroscopy (LIBS) N2 - Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process. T2 - ICASP-6 CY - Le Bischenberg, France DA - 20.06.2022 KW - LIBS KW - In situ measurement KW - Duplex stainless steel KW - TIG welding KW - Evaporation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571308 DO - https://doi.org/10.1088/1757-899X/1274/1/012018 VL - 1274 SP - 1 EP - 8 PB - IOP Publishing CY - Bristol AN - OPUS4-57130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baglo, K. A1 - Sauermoser, M. A1 - Lid, M. A1 - Paschke, T. A1 - Bin Afif, A. A1 - Lunzer, M. A1 - Bock, Robert A1 - Steinert, M. A1 - Flaten, A. A1 - Torgersen, J. T1 - Overcoming the transport limitations of photopolymer-derived architected carbon N2 - Photopolymer derived carbon grows in popularity, yet the range in available feature sizes is limited. Here we focus on expanding the field to low surface to volume ratio (SVR) structures. We describe a high temperature acrylic photopolymerizable precursor with FTIR and DSC and develop a thermal inert-gas treatment for producing architected carbon in the mm scale with SVR of 1.38 x10-3 μm-1. Based on TGA and MS, we distinguish two thermal regimes with activation energies of ~79 and 169 kJ mol-1, which we reason with mechanisms during the polymer’s morphologic conversion between 300 - 500 °C. The temperature range of the major dimensional shrinkage (300-440 °C, 50%) does not match the range of the largest alteration in elemental composition (440-600 °C, O/C 0.25-0.087%). The insights lead to an optimized thermal treatment with an initial ramp (2 °C min-1 to 350 °C), isothermal hold (14h), post hold ramp (0.5 °C min-1 to 440 °C) and final ramp (10 °C min-1 to 1000 °C). The resulting carbon structures are dimensionally stable, non-porous at the μm scale, and comprise an unprecedented variation in feature sizes (from mm to μm scale). The findings shall advance architected carbon to industrially relevant scales. KW - Carbon KW - Photopolymer KW - Transport limitations KW - Porous materials KW - Additive manufacturing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575038 DO - https://doi.org/10.1002/admt.202300092 SN - 2365-709X SP - 2300092 PB - Wiley-VCH GmbH AN - OPUS4-57503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gawek, Marcel A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Schönhals, Andreas T1 - Growth kinetics of the adsorbed layer of poly(2-vinylpyridine) - An indirect observation of desorption of polymers from substrates N2 - The growth kinetics of the adsorbed layer of poly(2-vinylpiridine) on silicon oxide is studied using a leaching technique which is based on the Guiselin brushes approach. The adsorbed layer is grown from a 200 nm thick P2VP film for several annealing time periods at different annealing temperatures. Then the film is solvent-leached, and the height of the remaining adsorbed layer is measured by atomic force microscopy. At the lowest annealing temperature only a linear growth regime is observed, followed by a plateau. Here, the molecular mobility of segments is too low to allow for a logarithmic growth. At higher annealing temperatures, both linear and logarithmic growth regimes are observed, followed by a plateau. At even higher annealing temperatures, the growth kinetics of the adsorbed layer changes. A linear growth followed by logarithmic growth kinetics is observed for short annealing time periods. For longer annealing time periods, an upturn of the growth kinetics is observed. At the highest annealing temperature, only a logarithmic growth regime is found. The change in the growth kinetics is discussed by an alteration in the structure of the adsorbed layer. Moreover, the interaction between the polymer segments and the substrate becomes weaker due to both enthalpic and entropic effects. Therefore, at high annealing temperatures the polymer segments might more easily desorb from the substrate. KW - Ultra thin polymer films PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575423 DO - https://doi.org/10.1039/d3sm00129f SN - 1744-683X SN - 1744-6848 VL - 19 IS - 21 SP - 3975 EP - 3982 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-57542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Srivastava, Priyanka A1 - Tavernaro, Isabella A1 - Scholtz, Lena A1 - Genger, C. A1 - Welker, P. A1 - Schreiber, Frank A1 - Meyer, Klas A1 - Resch-Genger, Ute T1 - Dual color pH probes made from silica and polystyrene nanoparticles and their performance in cell studies N2 - Ratiometric green–red fluorescent nanosensors for fluorometrically monitoring pH in the acidic range were designed from 80 nm-sized polystyrene (PS) and silica (SiO2) nanoparticles (NPs), red emissive reference dyes, and a green emissive naphthalimide pH probe, analytically and spectroscopically characterized, and compared regarding their sensing performance in aqueous dispersion and in cellular uptake studies. Preparation of these optical probes, which are excitable by 405 nm laser or LED light sources, involved the encapsulation of the pH-inert red-fuorescent dye Nile Red (NR) in the core of self-made carboxylated PSNPs by a simple swelling procedure and the fabrication of rhodamine B (RhB)-stained SiO2-NPs from a silane derivative of pH-insensitive RhB. Subsequently, the custom-made naphthalimide pH probe, that utilizes a protonation-controlled photoinduced electron transfer process, was covalently attached to the carboxylic acid groups at the surface of both types of NPs. Fluorescence microscopy studies with the molecular and nanoscale optical probes and A549 lung cancer cells confirmed the cellular uptake of all probes and their penetration into acidic cell compartments, i.e., the lysosomes, indicated by the switching ON of the green naphthalimide fluorescence. This underlines their suitability for intracellular pH sensing, with the SiO2-based nanosensor revealing the best performance regarding uptake speed and stability. KW - Sensors KW - Silica and polystyrene nanoparticles KW - pH probe KW - Fluorescence spectroscopy KW - Cell studies KW - Dye KW - Particle synthesis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569198 DO - https://doi.org/10.1038/s41598-023-28203-0 SN - 2045-2322 VL - 13 IS - 1 SP - 1321 EP - 1336 PB - Nature CY - London AN - OPUS4-56919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valentin, Jules D. P. A1 - Altenried, Stefanie A1 - Varadarajan, Adithi R. A1 - Ahrens, Christian H. A1 - Schreiber, Frank A1 - Webb, Jeremy S. A1 - van der Mei, Henny C. A1 - Ren, Qun T1 - Identification of Potential Antimicrobial Targets of Pseudomonas aeruginosa Biofilms through a Novel Screening Approach N2 - Pseudomonas aeruginosa is an opportunistic pathogen of considerable medical importance, owing to its pronounced antibiotic tolerance and association with cystic fibrosis and other life-threatening diseases. The aim of this study was to highlight the genes responsible for P. aeruginosa biofilm tolerance to antibiotics and thereby identify potential new targets for the development of drugs against biofilm-related infections. By developing a novel screening approach and utilizing a public P. aeruginosa transposon insertion library, several biofilm-relevant genes were identified. The Pf phage gene (PA0720) and flagellin gene (fliC) conferred biofilm-specific tolerance to gentamicin. Compared with the reference biofilms, the biofilms formed by PA0720 and fliC mutants were completely eliminated with a 4-fold-lower gentamicin concentration. Furthermore, the mreC, pprB, coxC, and PA3785 genes were demonstrated to play major roles in enhancing biofilm tolerance to gentamicin. The analysis of biofilm-relevant genes performed in this study provides important novel insights into the understanding of P. aeruginosa antibiotic tolerance, which will facilitate the detection of antibiotic resistance and the development of antibiofilm strategies against P. aeruginosa. KW - Antimicrobial resistance KW - Bacteria KW - Biofilms KW - Pseudomonas aeruginosa PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570205 DO - https://doi.org/10.1128/spectrum.03099-22 SP - 1 EP - 5 PB - ASM Journals AN - OPUS4-57020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chacón, Luz A1 - Kuropka, B. A1 - González-Tortuero, E. A1 - Schreiber, Frank A1 - Rojas-Jiménez, K. A1 - Rodríguez-Rojas, A. T1 - Mechanisms of low susceptibility to the disinfectant benzalkonium chloride in a multidrug-resistant environmental isolate of Aeromonas hydrophila N2 - Excessive discharge of quaternary ammoniumdisinfectants such as benzalkonium chloride (BAC) into aquatic systems can trigger several physiological responses in environmental microorganisms. In this study, we isolated a less-susceptible strain of Aeromonas hydrophila to BAC, designated as INISA09, froma wastewater treatment plant in Costa Rica. We characterized its phenotypic response upon exposure to three di􀀀erent concentrations of BAC and characterizedmechanisms related to its resistance using genomic and proteomic approaches. The genome of the strain, mapped against 52 di􀀀erent sequenced A. hydrophila strains, consists of approximately 4.6Mb with 4,273 genes. We found a massive genome rearrangement and thousands of missense mutations compared to the reference strain A. hydrophila ATCC 7966. We identified 15,762 missense mutations mainly associated with transport, antimicrobial resistance, and outer membrane proteins. In addition, a quantitative proteomic analysis revealed a significant upregulation of several efflux pumps and the downregulation of porins when the strain was exposed to three BAC concentrations.Other genes related tomembrane fatty acid metabolism and redox metabolic reactions also showed an altered expression. Our findings indicate that the response of A. hydrophila INISA09 to BAC primarily occurs at the envelop level, which is the primary target of BAC. Our study elucidates the mechanisms of antimicrobial susceptibility in aquatic environments against a widely used disinfectant and will help better understand howbacteria can adapt to biocide pollution. To our knowledge, this is the first study addressing the resistance to BAC in an environmental A. hydrophila isolate. We propose that this bacterial species could also serve as a new model to study antimicrobial pollution in aquatic environments. KW - Antimicrobial resistance KW - Bacteria KW - Disinfection KW - Biocides PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578555 DO - https://doi.org/10.3389/fmicb.2023.1180128 SN - 1664-302X VL - 14 SP - 1 EP - 18 PB - Frontiers SA CY - Lausanne AN - OPUS4-57855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drexler, A.-K. A1 - Konert, Florian A1 - Nietzke, Jonathan A1 - Hodžić, E. A1 - Pastore, S. A1 - Domitner, J. A1 - Rhode, Michael A1 - Sommitsch, C. A1 - Böllinghaus, Thomas T1 - Effect of Tensile Loading and Temperature on the Hydrogen Solubility of Steels at High Gas Pressure N2 - The hydrogen solubility in ferritic and martensitic steels is affected by hydrostatic stress, pressure, and temperature. In general, compressive stresses decrease but tensile stresses increase the hydrogen solubility. This important aspect must be considered when qualifying materials for high‐pressure hydrogen applications (e.g., for pipelines or tanks) by using autoclave systems. In this work, a pressure equivalent for compensating the effect of compressive stresses on the hydrogen solubility inside of closed autoclaves is proposed to achieve solubilities that are equivalent to those in pipelines and tanks subjected to tensile stresses. Moreover, it is shown that the temperature effect becomes critical at low temperatures (e.g., under cryogenic conditions for storing liquid hydrogen). Trapping of hydrogen in the microstructure can increase the hydrogen solubility with decreasing temperature, having a solubility minimum at about room temperature. To demonstrate this effect, the generalized law of the hydrogen solubility is parameterized for different steels using measured contents of gaseous hydrogen. The constant parameter sets are verified and critically discussed with respect to the high‐pressure hydrogen experiments. KW - Hydrogen KW - Solubility KW - Temperature KW - Tensile loading KW - Analytical calculation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586701 DO - https://doi.org/10.1002/srin.202300493 SN - 1611-3683 SP - 1 EP - 9 PB - Wiley AN - OPUS4-58670 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manes, M. A1 - El Houssami, M. A1 - Campbell, R. A1 - Sauca, A. A1 - Rush, D. A1 - Hofmann-Böllinghaus, Anja A1 - Andersson, P. A1 - Wagner, P. A1 - Veeneklaas, J. A1 - van Hees, P. A1 - Guillaume, E. T1 - Closing Data Gaps and Paving the Way for Pan-European Fire Safety Efforts: Part I—Overview of Current Practices for Fire Statistics N2 - The analysis of the current state of fire statistics and data collection in Europe and other countries is needed to increase awareness of how fire incidents affect buildings and to support pan-European fire prevention and fire mitigation measures. The terminology and data collected regarding fire incidents in buildings in the EU Member States were mapped to obtain meaningful datasets to determine common terminology, collection methodology, and data interpretation system. An extensive literature review showed that fire data collection systems have been instrumental in informing firefighting strategies, evidence-based planning, prevention, and educational programmes. Differences and similarities between fire data collection systems were also investigated. The amount and quality of the information in fire statistical recording systems appear to be influenced by the complexity and structure with which the data are collected. The analysis also examined the existing fire statistics in the EU Member States and a few other countries. Finally, a detailed investigation of the number of fires, fire deaths, and injuries from 2009 to 2018 in several countries was examined based on data from a report by CTIF. The trends showed differences attributable to the existing fire statistical practices in terms of terminology and data collection, and interpretation. Part II proposes a common terminology for selected fire statistical variables. The results provide relevant information regarding fire safety at the European level and should be used to guide the development of more uniform fire statistics across Europe. KW - Fire statistics KW - European project PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575711 DO - https://doi.org/10.1007/s10694-023-01415-6 SN - 1572-8099 SP - 1 EP - 44 PB - Springer CY - Heidelberg AN - OPUS4-57571 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El Houssami, M. A1 - Försth, M. A1 - Fredriksson, H. A1 - Drean, V. A1 - Guillaume, E. A1 - Hofmann-Böllinghaus, Anja A1 - Sandinge, A. T1 - Fire safety of interior materials of buses N2 - This study provides an analysis on the fire safety of passengers and the fire protection of coaches and buses. A brief review of major bus fire incidents, an overview of current regulations in Europe, and their limitations are presented. The study finds that the current small-scale fire test methods described in UN ECE Reg No. 118 need to be replaced by test methods that can assess the reaction to fire of materials when exposed to ignition sources of varying sizes. To address these shortcomings, the study proposed an expert recommendation to update the material fire safety requirements and testing for buses. Additional measures are proposed, derived from objectives and strategies applied in other transport sectors, and can be tested through existing European and international standards, which are widely used by several industries. These measures aim to extend the time with tenable conditions for a safe evacuation in case of fire, reduce the degree of damage to buses, reduce the risk for fast and excessive thermal exposure on modern energy carriers needed for a more sustainable transport sector. KW - Fire KW - Bus interior materials KW - Rregulations PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575700 DO - https://doi.org/10.1002/fam.3134 SN - 1099-1018 SP - 1 EP - 15 PB - Wiley CY - London AN - OPUS4-57570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmadian, A. A1 - Scheiber, D. A1 - Zhou, X. A1 - Gault, B. A1 - Darvishi Kamachali, Reza A1 - Romaner, L. A1 - Ecker, W. A1 - Dehm, G. A1 - Liebscher, C. H. T1 - Interstitial segregation has the potential to mitigate liquid metal embrittlement in iron N2 - The embrittlement of metallic alloys by liquid metals leads to catastrophic material failure and severely impacts their structural integrity. The weakening of grain boundaries by the ingress of liquid metal and preceding segregation in the solid are thought to promote early fracture. However, the potential of balancing between the segregation of cohesion-enhancing interstitial solutes and embrittling elements inducing grain boundary decohesion is not understood. Here, we unveil the mechanisms of how boron segregation mitigates the detrimental effects of the prime embrittler, zinc, in a Σ5 [0 0 1] tilt grain boundary in α −Fe (4 at.% Al). Zinc forms nanoscale segregation patterns inducing structurally and compositionally complex grain boundary states. Ab-initio simulations reveal that boron hinders zinc segregation and compensates for the zinc induced loss in grain boundary cohesion. Our work sheds new light on how interstitial solutes intimately modify grain boundaries, thereby opening pathways to use them as dopants for preventing disastrous material failure. KW - Materials Modelling KW - Liquid Metal Embrittlement KW - Alloy Safety KW - CALPHAD KW - Microstructure Design PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573576 DO - https://doi.org/10.1002/adma.202211796 SN - 0935-9648 IS - e2211796 PB - Wiley online library AN - OPUS4-57357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocano, Patricia A1 - Agudo Jácome, Leonardo A1 - Lopez-Galilea, I. A1 - Darvishi Kamachali, Reza A1 - Fries, S. G. T1 - Data regarding the experimental findings compared with CALPHAD calculations of the AlMo0.5NbTa0.5TiZr refractory high entropy superalloy N2 - This contribution contains the raw data used to compare experimental results with thermodynamic calculations using the CALPHAD method, which is related to the research article “The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: experimental findings and comparison with calculations using the CALPHAD method” [1] , and therefore this article can be used as a basis for interpreting the data contained therein. The AlMo0.5NbTa0.5TiZr refractory superalloy was characterized in the cast and annealed condition (1400 °C for 24 h) in order to measure grain size and to identify and measure the size and area fraction of the phases present. The raw data of this article include X-ray diffraction (XRD) measurements, microstructural characterization by scanning and transmission electron microscopy (SEM and TEM), and elemental analysis by energy dispersive X-ray spectroscopy (EDX). XRD includes the determination of phases and the lattice parameters (A2, B2, and hexagonal structure). Microstructural analysis by scanning and transmission electron microscopy includes (1) identification of composition, size, and volume fraction of the present phases and (2) determination of grain size. Based on these experimental data, it is possible to identify similarities and discrepancies with the data calculated using the CALPHAD method for the alloy under study in Ref. [1] , which provides the basis for better and more efficient development of reliable databases. KW - Transmission electron microscopy KW - Scanning electron microscopy KW - Microstructural characterization KW - Refractory high entropy alloys PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568009 DO - https://doi.org/10.1016/j.dib.2022.108858 SN - 2352-3409 VL - 46 SP - 1 EP - 19 PB - Elsevier CY - Amsterdam AN - OPUS4-56800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jordan, T. A1 - Askar, Enis A1 - Holtappels, Kai A1 - Deeg, S. A1 - Jopen, M. A1 - Stoll, U. A1 - Reinecke, E.-A. A1 - Krause, U. A1 - Beyer, M. A1 - Markus, D. T1 - Stand der Kenntnisse und Technik bezüglich Wasserstoffsicherheit N2 - Die Einführung von Wasserstoff als sicherer Energieträger braucht eine robuste Wissensbasis, darauf aufgebaute Werkzeuge zur Auslegung und Sicherheitsbewertung von Wasserstofftechnologien und ein international harmonisiertes Regelwerk. Viele der innovativen Technologien implizieren Wasserstoff bei hohen Drücken und/oder kryogenen Temperaturen, mit denen in verteilten Anwendungen erstmalig private Nutzer in Kontakt kommen. Um überkonservative, teure Sicherheitslösungen zu vermeiden, gleichzeitig aber die Einsetzbarkeit und Sicherheit von Wasserstoffanwendungen zu demonstrieren und die Akzeptanz für die Technologie aufrecht zu halten, muss auch die Sicherheitsforschung mit den Trends der technologischen Entwicklung Schritt halten, oder sie besser noch antizipieren. So beschreibt dieser Überblicksartikel nicht nur den gegenwärtigen Stand der Kenntnisse und Technik bezüglich Wasserstoffsicherheit, sondern auch ihre Weiterentwicklung. KW - Alternative Energieträger KW - Explosionsschutz KW - Flüssigwasserstoff KW - Unfallszenarien KW - Wasserstoffspeicherung KW - Sicherheitsbewertung KW - Regelsetzung KW - Gefährdungs- und Risikobeurteilung PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593629 DO - https://doi.org/10.1002/cite.202300141 SN - 0009-286X VL - 96 IS - 1-2 SP - 1 EP - 20 PB - Wiley-VCH AN - OPUS4-59362 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klippel, A. A1 - Hofmann-Böllinghaus, Anja A1 - Gnutzmann, Tanja A1 - Piechnik, K. T1 - Reaction-to-fire testing of bus interior materials: Assessing burning behaviour and smoke gas toxicity N2 - Although fire safety regulations for buses have been adapted in recent years regarding, for example, fire detection and engine fire suppression systems, the changes in regulations for bus interior materials are minimal. A comparison of fire safety regulations for interior materials in other transport sectors for trains, ships or aircraft reveals a much lower level of requirements for bus materials. Although repeated bus accidents as well as fire statistics show the danger a bus fire can pose to passengers. In particular, the combination of a fire incident and passengers with reduced mobility led to severe disasters in Germany and other European countries. To enhance the fire safety for passengers, the interior bus materials are crucial as the fire development in the bus cabin determines whether escape and rescue is possible. Against this background, bus interior materials were tested in different fire test scenarios. Measurement of a wide variety of parameters, for example, the mass loss, ignition time, smoke gas composition, heat release rate among others were carried out. Tested materials complied to the newest set of requirements. For this purpose, interior materials and their components had to be identified according to their chemical structure. Parts of the tests were funded by BASt (Federal Highway Research Institute) in the project 82.0723/2018. Experimental results show reaction-to-fire behaviour which lead to very limited times for escape and rescue in case of fire in a bus cabin. Based on the studies on fire behaviour and toxicity assessment, recommendations for improved fire safety regulations for interior materials could be made. KW - Burning behaviour KW - Bus interior materials KW - Cone calorimeter KW - DIN tube furnace KW - FTIR spectroscopy KW - Reference values KW - Smoke toxicity PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576085 DO - https://doi.org/10.1002/fam.3108 SN - 1099-1018 VL - 47 IS - 5 SP - 665 EP - 680 PB - Wiley CY - New York, NY AN - OPUS4-57608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manes, M. A1 - Sauca, A. A1 - El Houssami, M. A1 - Andersson, P. A1 - McIntyre, C. A1 - Campbell, R. A1 - Rush, D. A1 - Hofmann-Böllinghaus, Anja A1 - Wagner, P. A1 - Leene, M. A1 - Oberhagemann, D. A1 - Jomaas, G. A1 - Grone, F. A1 - Guillaume, E. T1 - Closing Data Gaps and Paving the Way for Pan-European Fire Safety Efforts: Part II—Terminology of Fire Statistical Variables N2 - A well-defined terminology of fire-related variables is important for correct analyses and supporting knowledge-based decisions regarding the evaluation of building fires at the European level. After developing an overview of current practices for fire statistics in Part I, the terminology used and the data collected by the EU Member States and eight other countries regarding fire incidents, property damage and human losses were mapped to increase awareness of their practice and support a comprehensive assessment of several fire statistical datasets. A questionnaire was distributed to relevant authorities responsible for the collection, elaboration/analysis, and fire statistical data publications to define and select the essential variables for an appropriate fire assessment and fire incident description. Based on the results of the questionnaire able to identify the essential fire statistical variables and a detailed analysis of current definitions adopted in the fire statistics of the EU Member States and other countries, a common terminology is proposed to collect the necessary data in the EU Member States and obtain meaningful datasets based on standardised terms and definitions. The results will generate essential outputs to move towards harmonised fire statistics at the EU level and contribute to an appropriate analysis able to improve fire prevention and fire mitigation in building fires. KW - Fire statistics PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575725 DO - https://doi.org/10.1007/s10694-023-01408-5 SN - 1572-8099 SP - 1 EP - 32 PB - Springer CY - Heidelberg AN - OPUS4-57572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jacobson, D. A1 - Darvishi Kamachali, Reza A1 - Thompson, G. B. T1 - Extending Density Phase-Field Simulations to Dynamic Regimes N2 - Density-based phase-field (DPF) methods have emerged as a technique for simulating grain boundary thermodynamics and kinetics. Compared to the classical phase-field, DPF gives a more physical description of the grain boundary structure and chemistry, bridging CALPHAD databases and atomistic simulations, with broad applications to grain boundary and segregation engineering. Notwithstanding their notable progress, further advancements are still warranted in DPF methods. Chief among these are the requirements to resolve its performance constraints associated with solving fourth-order partial differential equations (PDEs) and to enable the DPF methods for simulating moving grain boundaries. Presented in this work is a means by which the aforementioned problems are addressed by expressing the density field of a DPF simulation in terms of a traditional order parameter field. A generic DPF free energy functional is derived and used to carry out a series of equilibrium and dynamic simulations of grain boundaries in order to generate trends such as grain boundary width vs. gradient energy coefficient, grain boundary velocity vs. applied driving force, and spherical grain radius vs. time. These trends are compared with analytical solutions and the behavior of physical grain boundaries in order to ascertain the validity of the coupled DPF model. All tested quantities were found to agree with established theories of grain boundary behavior. In addition, the resulting simulations allow for DPF simulations to be carried out by existing phase-field solvers. KW - CALPHAD KW - Phase-field modelling KW - Phase-Field Simulations PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581365 DO - https://doi.org/10.3390/met13081497 VL - 13 SP - 1 EP - 16 AN - OPUS4-58136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mezhov, Alexander A1 - Kulisch, D. A1 - Goncharov, A. A1 - Zhutovsky, S. T1 - A Comparative Study of Factors Influencing Hydration Stoppage of Hardened Cement Paste N2 - There is no consensus on which hydration stoppage method is optimal to preserve the microstructure and mineral composition of samples, especially considering the specific aspects of different testing methods, such as TGA, MIP, or XRD. This paper presents a quantitative comparison between the most popular hydration stoppage strategies and parameters such as the sample piece size, the soaking time in a solvent, and the type, as examined on cement paste hydrated for 7 days. It was found that the carbonation appears either for samples smaller than 2.36 mm and bigger than 4.75 mm or samples soaked in a solvent for longer than 1 h. Fast solvent replacement leads to ettringite diminution and total pore volume increase. Among others, solvent replacement with subsequent gentle heating under a vacuum was found to be the most efficient, whereas it was experimentally demonstrated that isopropyl alcohol stops hydration faster than ethanol and acetone. KW - Hydration stoppage KW - Solvent replacement KW - Soaking time KW - Sample piece size PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582430 DO - https://doi.org/10.3390/su15021080 VL - 15 IS - 2 SP - 1 EP - 21 PB - MDPI CY - Basel, Switzerland. AN - OPUS4-58243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madia, Mauro A1 - Baer, Wolfram A1 - Wagener, Rainer A1 - Kiyak, Yusuf T1 - Betriebsfestigkeit und Bruchverhalten von bainitischen Schmiedestählen N2 - Die neue Generation von bainitischen Schmiedestählen bietet auf der einen Seite ein erhebliches Festigkeitspotenzial, das es im Sinne des Leichtbaus auch für zyklisch belastete Sicherheitsbauteile zu heben gilt. Auf der anderen Seite geht mit dieser Festigkeitssteigerung im Vergleich zu Vergütungsstählen ein Verlust an Duktilität und Zähigkeit einher. Am Beispiel des Demonstratorbauteils Achsschenkel ging das Forschungsvorhaben der Frage nach, wie ein Freigabeprozess zu gestalten ist, damit das Festigkeitspotenzial der neuen Stähle zuverlässig ausgenutzt werden kann. Als Ergebnis wird eine Vorgehensweise dargestellt, die den Eigenschaften der neuen Generation von Schmiedestählen Rechnung trägt, um den sicheren Betrieb der Komponenten zu gewährleisten. KW - Bainitischer Schmiedestahl KW - Bruchmechanik KW - Sicherheit KW - Betriebsfestigkeit KW - Bauteilauslegung PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594296 SN - 2366-5106 SP - 50 EP - 54 PB - Industrieverband Massivumformung e. V CY - Hagen AN - OPUS4-59429 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kapoor, M. A1 - Overgaard Christensen, Ch. A1 - Wittrup Schmidt, J. A1 - Dalsgaard Sørensen, J. A1 - Thöns, Sebastian T1 - Decision analytic approach for the reclassification of concrete bridges by using elastic limit information from proof loading N2 - Reclassification of bridges, i.e., a change in load rating, using reliability-based methods and a direct update with proof load information has been presented by many authors. However, bridge reclassification has hardly been studied from a decision analytic perspective, i.e., with quantification of the risks and benefits of different classification choices, and the expected benefit gain from proof loading. We derive, explain and exemplify a decision analytic approach for bridge reclassification along with models for (1) elastic and ultimate capacity and their adaptation with proof load information, (2) proof load information with classification outcomes accounting for target reliabilities and, (3) utilities including socio-economic benefits from reclassification. The approach and models are exemplified with a case study based on reclassification of bridges with a low existing classification. Decision rules, for practical use by a highway authority to find the optimal classification, are identified and documented based on: (1) the measurement of the capacity at elastic limit by proof loading, (2) the bridge reclassification benefits, and, (3) the required annual reliability level. From a Value of Information analysis, it is concluded that the proof load information is highly valuable for reclassification in cases of high socio-economic benefits and high reliability requirements. KW - Proof loading KW - Structural reliability KW - Value of information KW - Decision analysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596845 DO - https://doi.org/10.1016/j.ress.2022.109049 SN - 0951-8320/ VL - 232 SP - 1 EP - 16 PB - Elsevier Ltd. AN - OPUS4-59684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Anker, A. S. A1 - Annadurai, V. A1 - Balazs, D. M. A1 - Bienert, Ralf A1 - Bouwman, W. G. A1 - Breßler, Ingo A1 - Breternitz, J. A1 - Brok, E. S. A1 - Bryant, G. A1 - Clulow, A. J. A1 - Crater, E. R. A1 - De Geuser, F. A1 - Del Giudice, A. A1 - Deumer, J. A1 - Disch, S. A1 - Dutt, S. A1 - Frank, K. A1 - Fratini, E. A1 - Garcia, P. R. A. F. A1 - Gilbert, E. P. A1 - Hahn, Marc Benjamin A1 - Hallett, J. A1 - Hohenschutz, M. A1 - Hollamby, M. A1 - Huband, S. A1 - Ilavsky, J. A1 - Jochum, J. K. A1 - Juelsholt, M. A1 - Mansel, B. W. A1 - Penttilä, P. A1 - Pittkowski, R. K. A1 - Portale, G. A1 - Pozzo, L. D. A1 - Rochels, L. A1 - Rosalie, Julian A1 - Saloga, Patrick E. J. A1 - Seibt, S. A1 - Smith, A. J. A1 - Smith, G. N. A1 - Spiering, G. A. A1 - Stawski, Tomasz M. A1 - Taché, O. A1 - Thünemann, Andreas A1 - Toth, K. A1 - Whitten, A. E. A1 - Wuttke, J. T1 - The human factor - Results of a small-angle scattering data analysis round robin N2 - A round-robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%. Due to the added complexity of the structure factor, far fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 and 86%, respectively. This round-robin experiment highlights several causes for the discrepancies, for which solutions are proposed. KW - Round Robin KW - Data analysis KW - Small-angle scattering KW - Nanomaterials KW - Interlaboratory comparability KW - Nanostructure quantification KW - Methodology KW - MOUSE PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587091 DO - https://doi.org/10.1107/S1600576723008324 SN - 1600-5767 VL - 56 IS - 6 SP - 1618 EP - 1629 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-58709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kinne, Marko A1 - Thöns, Sebastian T1 - Fatigue Reliability Based on Predicted Posterior Stress Ranges Determined from Strain Measurements of Wind Turbine Support Structures N2 - In the present paper, an approach for updating the continuous stress range distribution of a welded connection of a wind turbine support structure with predicted information from strain measurements is presented. Environmental conditions, such as wind or, in offshore fields, waves and currents, in combination with rotor excitations generate cyclic stresses affecting the reliability of welded joints of the support structure over the service life. Using strain measurements, these conditions can be monitored, and the resulting stress ranges, under consideration of measurement, mechanical and material uncertainties, can be reconstructed. These stress ranges can be used as an input for updating the prior probability density function (PDF) of the stress ranges predicted by the overall dynamics and a detailed design analysis. Applying Bayesian probability theory and decision theoretical implications, the predicted posterior probability density of the stress ranges is calculated based on the design information and uncertainties. This approach is exemplified, and it is shown how the predicted stress ranges and the design stress ranges are distributed. The prior and the predicted posterior stress ranges are used for a reliability calculation for potentially entering a pre-posterior decision analysis KW - Strain measurements of wind turbine support structures KW - Bayesian updating of stress ranges KW - Posterior fatigue reliability PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572663 DO - https://doi.org/10.3390/en16052225 VL - 16 IS - 5 SP - 1 EP - 26 PB - MDPI AN - OPUS4-57266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hildebrandt, Jana A1 - Taubert, Andreas A1 - Thünemann, Andreas T1 - Synthesis and Characterization of Ultra‐Small Gold Nanoparticles in the Ionic Liquid 1‐Ethyl‐3‐methylimidazolium Dicyanamide, [Emim][DCA] N2 - AbstractWe report on gold clusters with around 62 gold atoms and a diameter of 1.15±0.10 nm. Dispersions of the clusters are long‐term stable for two years at ambient conditions. The synthesis was performed by mixing tetrachloroauric acid (HAuCl4 ⋅ 3 H2O) with the ionic liquid 1‐ethyl‐3‐methylimidazolium dicyanamide ([Emim][DCA]) at temperatures of 20 to 80 °C. Characterization was performed with small‐angle X‐ray scattering (SAXS), UV‐Vis spectroscopy, and MALDI‐TOF mass spectrometry. A three‐stage model is proposed for the formation of the clusters, in which cluster growth from gold nuclei takes place according to the Lifshitz‐Slyozov‐Wagner (LSW) model followed by oriented attachment to form colloidal stable clusters. KW - Reference materials KW - SAXS KW - Gold KW - Nanoparticle KW - Small-angle X-ray scattering KW - Ionic liquid PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588203 DO - https://doi.org/10.1002/open.202300106 SN - 2191-1363 VL - 44 SP - 1 EP - 19 PB - Wiley AN - OPUS4-58820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hildebrandt, Jana A1 - Thünemann, Andreas T1 - Aqueous Dispersions of Polypropylene: Toward Reference Materials for Characterizing Nanoplastics N2 - Microplastics and nanoplastics pollute the natural environment all over the world, but the full extent of the hazards posed by this waste is unclear. While research on microplastics is well advanced, little work has been done on nanoplastics. This discrepancy is mainly due to the lacking ability to detect nanoplastics in biologically and environmentally relevant matrices. Nanoplastics reference materials can help the development of suitable methods for identifying and quantifying nanoplastics in nature. The aim is to synthesize nanoplastics made from one of the most commonly used plastics, namely polypropylene. An easy way to produce long-term stable aqueous dispersions of polypropylene nanoparticles (nano polypropylene) is reported. The nanoplastic particles, prepared by mechanical breakdown, show a mean hydrodynamic diameter of D h = 180.5 ± 5.8 nm and a polydispersity index of PDI = 0.084 ± 0.02. No surfactant is needed to obtain dispersion which is stable for more than 6 months. The colloidal stability of the surfactant-free nano polypropylene dispersions is explained by their low zeta potential of 𝜻 = −43 ± 2 mV. KW - Nanoparticles KW - Reference Material KW - Nanoplastics PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571799 DO - https://doi.org/10.1002/marc.202200874 SN - 1022-1336 VL - 44 IS - 6 SP - 1 EP - 15 PB - Wiley-VCH CY - Weinheim AN - OPUS4-57179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sauermoser-Yri, M. A1 - Veldurthi, N. A1 - Wölfle, C. H. A1 - Svartvatn, P. J. A1 - Flo Hoem, S. O. A1 - Lid, M. J. A1 - Bock, Robert A1 - Palko, J. A1 - Torgersen, J. T1 - On the porosity-dependent permeability and conductivity of triply periodic minimal surface based porous media N2 - With the fast development in the field of additive manufacturing, triply periodic minimal surface (TPMS) based porous media have recently found many uses in mechanical property tuning. However, there is still a lack of understanding in their porosity-dependent permeability and electrical as well as thermal conductivity. Here, we perform finite volume simulations on the solid and void domains of the Schoen gyroid (SG), Schwarz primitive (SP) and Schwarz primitive beam (SPB) TPMS with porosities between 63% and 88% in Ansys Fluent. A simple cubic lattice (CL) of equivalent porosity served as reference. The SPB and CL showed up to one order of magnitude higher permeabilities than the SG and SP. However, SG and SP have about 1.3 and 2.6 times the electrical and thermal conductivity of SPB and CL, respectively. Furthermore, the properties of SPB and CL are largely affected by the surface area density, whereas tortuosity variation does not impact permeability and conductivity to a major extent. Finally, empirical relations are adapted to describe the presented data and thus, they may enable future designers of TPMS based porous structures to fine-tune the geometries according to the requirements on permeability and electrical as well as thermal conductivity. KW - Metals and Alloys KW - Surfaces, Coatings and Films KW - Biomaterials KW - Ceramics and Composites PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-585250 DO - https://doi.org/10.1016/j.jmrt.2023.09.242 SN - 2238-7854 VL - 27 SP - 585 EP - 599 PB - Elsevier B.V. AN - OPUS4-58525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Theiler, Geraldine A1 - Gradt, Thomas T1 - Comparison of the sliding behavior of several polymers in gaseous and liquid hydrogen N2 - The development of hydrogen technologies entails high safety requirements in distribution and dispensing infrastructure. Therefore, it is necessary to pursue research on material compatibility in hydrogen, especially for critical parts with tribological issues. The focus of this study is to evaluate the influence of hydrogen on a wider range of commercially available polymer materials. Thereby, the friction and wear behavior of different grades of TPE, POM, PA66, PA12, PPA, PEEK, PPS, PTFE, PAI, PI and PBI were investigated against a rotating steel disk (AISI 304). Filled and unfilled polymers from different suppliers were evaluated at room temperature in air, vacuum and hydrogen gas (H2) as well as in liquid hydrogen at - 253°C (LH2). The sliding behavior of the polymer materials is discussed by means of surface analyses, whereby special attention is paid to the formation of a transfer film. According to the results at ambient temperature, the effect of hydrogen environment on the tribological behavior of neat polymers may be related to lack of moisture, but also to saturated hydrocarbons in gaseous hydrogen. In liquid hydrogen, the best tribological performances were achieved with neat PA polymers as well as PPS and PI composites. KW - Polymers KW - Composites KW - Sliding wear KW - Hydrogen KW - Cryogenic temperature PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597123 DO - https://doi.org/10.2474/trol.18.217 SN - 1881-2198 VL - 18 IS - 5 SP - 217 EP - 231 PB - Japanese Society of Tribologists AN - OPUS4-59712 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Guerra, M.F. A1 - Martinón-Torres, M. A1 - Lemasson, Q. A1 - Moignard, B. A1 - Pacheco, C. A1 - Pichon, L. A1 - Macdonald, L. A1 - Hess, M. A1 - Tissot, I. ED - Guerra, M. F. ED - Martinón-Torres, M. ED - Quirke, S. T1 - Analytical approaches to Egyptian goldwork N2 - The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail. KW - Gold KW - Synchrotron KW - D2XRF KW - Egypt PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586039 DO - https://doi.org/10.17863/CAM.99681 SP - 131 EP - 191 AN - OPUS4-58603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Licht, M. A1 - Nikoonasab, Ali A1 - Gluth, Gregor A1 - Raupach, M. ED - Claßen, M. ED - Hegger, J. ED - Matschei, T. ED - Raupach, M. T1 - Alkali-aktivierte Hüttensandbetone – CO2-reduzierte Bindemittel mit hohem Korrosionsschutzpotential N2 - Durch den Ersatz von Portlandzement können alkali-aktivierte Bindemittel einen bedeutenden Beitrag zur Verringerung der durch die Zementklinkerherstellung verursachten CO2-Emissionen leisten. Für die Verwendung von alkali-aktivierten Bindemitteln in Stahlbetonkonstruktionen, die Chloriden oder Carbonatisierung ausgesetzt sind, ist die Fähigkeit des Stahls, den passiven Zustand zu erreichen und aufrechtzuerhalten, von großer Bedeutung. Die Prozesse der Deckschichtbildung von Stahl in alkali-aktivierten Materialien unterscheiden sich jedoch zum Teil grundlegend von denen in Portlandzementen. Alkali-aktivierte Hüttensandbetone weisen gute technische Eigenschaften auf, bisher fehlen jedoch grundlegende Kenntnisse bzgl. ihrer schützenden Wirkung bei korrosiven Angriffen. Dies ist vor allem auf ihre sulfidhaltige Porenlösung zurückzuführen, welche die elektrochemischen Eigenschaften der Stahloberfläche beeinflusst und die Verwendung herkömmlicher Bewertungsmaßstäbe erschwert. Es werden erste Ergebnisse eines DFG-Forschungsprojektes vorgestellt, in dem das Passivierungsverhalten von Stahl in alkali-aktivierten Hüttensandmörteln unterschiedlicher Zusammensetzungen sowie in Mörteln auf Basis hüttensandhaltiger Normzemente untersucht wird. Über einen Zeitraum von mindestens 28 Tagen werden an Zylinderprüfkörpern im 3-Elektroden-Aufbau das Ruhepotential sowie die Polarisationswiderstände der Stahlelektroden ermittelt. T2 - 10. DAfStb-Jahrestagung mit 62. Forschungskolloquium CY - Aachen, Germany DA - 26.09.2023 KW - Bewehrung KW - Stahlkorrosion KW - Hüttensandmehl KW - Sulfid PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593775 DO - https://doi.org/10.18154/RWTH-2023-06676 SP - 233 EP - 238 PB - RWTH Aachen CY - Aachen AN - OPUS4-59377 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudić, O. A1 - Mittermayr, F. A1 - Gluth, Gregor A1 - Simon, Sebastian A1 - Ukrainczyk, N. A1 - Seyrek, Y. A1 - Freytag, B. A1 - Juhart, J. A1 - Grengg, C. T1 - On the benefits of vegetable oil addition for the pore structure and acid resistance of alkali-activated systems N2 - The impact of high additions of vegetable oil (12 vol%) on the mechanical and microstructural properties of metakaolin-slag-based alkali-activated materials (AAMs) was studied. The addition of oil resulted in a slight decrease in initial polymerization kinetics but did not affect the final degree of reaction. AAM-oil-composite-mortars exhibited approximately ∼30% lower compressive strength primarily due to the entrainment of air voids. Newly formed soap phases significantly reduced the volume of small capillary and gel pores (pore radii <15 nm), leading to a decrease in specific inner surface area by a factor of up to 15. The porosity modification induced by the oil addition greatly enhanced the resistance of AAMs against sulfuric acid attack, shifting the dominant processes from diffusion and cracks to framework-dissolution controlled by the inherent phase stabilities. Following the immersion in sulfuric acid (pHstat = 2) for 8 weeks, the depth of corroded layer decreased by 70% and no cracks due to expansive phases were observed. These promising findings suggest that the incorporation of vegetable oil in AAMs has the potential to address durability concerns associated with diffusion-based corrosion processes, thereby expanding the range of future applications. KW - Alkali-activated materials KW - Acid resistance KW - Pore structure PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581719 DO - https://doi.org/10.1016/j.ceramint.2023.08.036 VL - 49 IS - 20 SP - 33275 EP - 33290 PB - Elsevier Ltd. AN - OPUS4-58171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mundra, S. A1 - Samson, G. A1 - Masi, G. A1 - Achenbach, R. A1 - Bastidas, D. M. A1 - Bernal, S. A. A1 - Bignozzi, M. C. A1 - Criado, M. A1 - Cyr, M. A1 - Gartner, N. A1 - von Greve-Dierfeld, S. A1 - Legat, A. A1 - Nikoonasab, Ali A1 - Provis, J. L. A1 - Raupach, M. A1 - Gluth, Gregor T1 - Application of electrochemical methods for studying steel corrosion in alkali-activated materials N2 - Alkali-activated materials (AAMs) are binders that can complement and partially substitute the current use of conventional cement. However, the present knowledge about how AAMs protect steel reinforcement in concrete elements is incomplete, and uncertainties exist regarding the application of electrochemical methods to investigate this issue. The present review by EFC WP11-Task Force ‘Corrosion of steel in alkali-activated materials’ demonstrates that important differences exist between AAMs and Portland cement, and between different classes of AAMs, which are mainly caused by differing pore solution compositions, and which affect the outcomes of electrochemical measurements. The high sulfide concentrations in blast furnace slag-based AAMs lead to distinct anodic polarisation curves, unusually low open circuit potentials, and low polarisation resistances, which might be incorrectly interpreted as indicating active corrosion of steel reinforcement. No systematic study of the influence of the steel–concrete interface on the susceptibility of steel to corrosion in AAMs is available. Less common electrochemical methods present an opportunity for future progress in the field. KW - Alkali-activated materials KW - Reinforcement corrosion KW - Steel corrrosion KW - Electrochemical methods KW - Concrete PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572241 DO - https://doi.org/10.1002/maco.202313743 SN - 1521-4176 VL - 74 IS - 7 SP - 988 EP - 1008 PB - Wiley-VCH CY - Weinheim AN - OPUS4-57224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Page, T.M. A1 - Nie, C. A1 - Neander, L. A1 - Povolotsky, T.L. A1 - Sahoo, A.K. A1 - Nickl, Philip A1 - Adler, J.M. A1 - Bawadkji, O. A1 - Radnik, Jörg A1 - Achazi, K. A1 - Ludwig, K. A1 - Lauster, D. A1 - Netz, R.R. A1 - Trimpert, J. A1 - Kaufer, B. A1 - Haag, R. A1 - Donskyi, Ievgen T1 - Functionalized Fullerene for Inhibition of SARS-CoV-2 Variants N2 - As virus outbreaks continue to pose a challenge, a nonspecific viral inhibitor can provide significant benefits, especially against respiratory viruses. Polyglycerol sulfates recently emerge as promising agents that mediate interactions between cells and viruses through electrostatics, leading to virus inhibition. Similarly, hydrophobic C60 fullerene can prevent virus infection via interactions with hydrophobic cavities of surface proteins. Here, two strategies are combined to inhibit infection of SARS-CoV-2 variants in vitro. Effective inhibitory concentrations in the millimolar range highlight the significance of bare fullerene’s hydrophobic moiety and electrostatic interactions of polysulfates with surface proteins of SARS-CoV-2. Furthermore, microscale thermophoresis measurements support that fullerene linear polyglycerol sulfates interact with the SARS-CoV-2 virus via its spike protein, and highlight importance of electrostatic interactions within it. All-atom molecular dynamics simulations reveal that the fullerene binding site is situated close to the receptor binding domain, within 4 nm of polyglycerol sulfate binding sites, feasibly allowing both portions of the material to interact simultaneously. KW - Covalent functionalization KW - Fullerene KW - SARS-CoV 2 KW - Sulfated materials KW - Virus inhibition PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568672 DO - https://doi.org/10.1002/smll.202206154 SN - 1613-6810 SP - 1 EP - 8 PB - Wiley VCH AN - OPUS4-56867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knigge, Xenia A1 - Radnik, Jörg T1 - 1,3-Dimethyl-imidazolium dimethyl phosphate ([MMIM]+[DMP]−) analyzed by XPS and HAXPES N2 - The ionic liquid 1,3-dimethyl-imidazolium-dimethylphosphate ([MMIM]+[DMP]−) was analyzed using (hard) x-ray photoelectron spectroscopy. Here, XPS and HAXPES spectra are shown in comparison. For the acquisition of the XPS spectra, monochromatic Al Kα radiation at 1486.6 eV was used, while for the acquisition of the HAXPES spectra, monochromatic Cr Kα radiation at 5414.8 eV was applied. Here, survey scans and high-resolution spectra of P 2p, P 2s, C 1s, O 1s, and N 1s for both methods and P 1s, P KL2,3L2,3, and P KL1L2,3 for HAXPES are shown. KW - C7H15N2O4P KW - [MMIM]+[DMP]− KW - Lonic liquid KW - Hard x-ray photoelectron spectroscopy KW - HAXPES KW - XPS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571604 DO - https://doi.org/10.1116/6.0002297 VL - 30 IS - 1 SP - 1 EP - 20 PB - AIP Publishing AN - OPUS4-57160 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 - Getenet, M. A1 - Otálora, F. A1 - Emmerling, Franziska A1 - Al-Sabbagh, Dominik A1 - García-Ruiz, J. M. T1 - Mineral precipitation and hydrochemical evolution through evaporitic processes in soda brines (East African Rift Valley) N2 - Soda lakes of the East African Rift Valley are hyperalkaline, hypersaline lakes extremely enriched in Na+, K+, Cl−, CO32−, HCO3−, and SiO2. In this paper, we investigate the chemical evolution in these lakes and the production of chemical sediments by salt precipitation via evaporation. Water samples from tributary springs and three lakes (Magadi, Nasikie Engida and Natron) have been experimentally studied by in-situ X-ray diffraction during evaporation experiments to characterize the sequence of mineral precipitation. These data are complemented by ex-situ diffraction studies, chemical analyses and thermodynamic hydrochemical calculations producing detailed information on the activity of all solution species and the saturation state of all minerals potentially generated by the given composition. Major minerals precipitating from these samples are sodium carbonates/bicarbonates as well as halite. The CO3/HCO3 ratio, controlled by pH, is the main factor defining the Na‑carbonates precipitation sequence: in lake brines where CO3/HCO3 > 1, trona precipitates first whereas in hot springs, where CO3/HCO3 ≪ 1, nahcolite precipitates instead of trona, which forms later via partial dissolution of nahcolite. Precipitation of nahcolite is possible only at lower pH values (pCO2 higher than −2.7) explaining the distribution of trona and nahcolite in current lakes and the stratigraphic sequences. Later, during evaporation, thermonatrite precipitates, normally at the same time as halite, at a very high pH (>11.2) after significant depletion of HCO3− due to trona precipitation. The precipitation of these soluble minerals increases the pH of the brine and is the main factor contributing to the hyperalkaline and hypersaline character of the lakes. Villiaumite, sylvite, alkaline earth carbonates, fluorapatite and silica are also predicted to precipitate, but most of them have not been observed in evaporation experiments, either because of the small amount of precipitates produced, kinetic effects delaying the nucleation of some phases, or by biologically induced effects in the lake chemistry that are not considered in our calculations. Even in these cases, the chemical composition in the corresponding ions allows for discussion on their accumulation and the eventual precipitation of these phases. The coupling of in-situ and ex-situ experiments and geochemical modelling is key to understanding the hydrogeochemical and hydroclimatic conditions of soda lakes, evaporite settings, and potentially soda oceans of early Earth and other extraterrestrial bodies. KW - Crystallization sequence KW - Hydrochemical evolution KW - Alkaline brines KW - Sodium carbonate minerals KW - Soda lakes KW - Evaporite deposits PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568431 DO - https://doi.org/10.1016/j.chemgeo.2022.121222 SN - 0009-2541 VL - 616 SP - 1 EP - 13 PB - Elsevier CY - New York, NY AN - OPUS4-56843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karafiludis, Stephanos A1 - de Oliveira Guilherme Buzanich, Ana A1 - Heinekamp, Christian A1 - Smales, Glen Jacob A1 - Hodoroaba, Vasile-Dan A1 - ten Elshof, J. E. A1 - Emmerling, Franziska A1 - Stawski, Tomasz T1 - Template-free synthesis of mesoporous, amorphous transition metal phosphate materials N2 - We present how mesoporosity can be engineered in transition metal phosphate (TMPs) materials in a template-free manner. The method involves a transformation of a precursor metal phosphate phase, called M-struvite (NH4MPO4·6H2O, M = Mg2+, Ni2+, Co2+, NixCo1-x2+). It relies on the thermal decomposition of crystalline M-struvite precursors to an amorphous and simultaneously mesoporous phase, which forms while degassing of NH3 and H2O. The temporal evolution of mesoporous frameworks and the response of the metal coordination environment were followed with in-situ and ex-situ scattering and diffraction, as well as X -ray spectroscopy. Despite sharing the same precursor struvite structure, different amorphous and mesoporous structures were obtained depending on the involved transition metal. We highlight the systematic differences in absolute surface area, pore shape, pore size, and phase transitions depending on a metal cation present in the analogous M-struvites. The amorphous structures of thermally decomposed Mg-, Ni- and NixCo1-x-struvites exhibit high surface areas and pore volumes (240 m²g-1 and 0.32 cm-3 g-1 for Mg and 90 m²g-1 and 0.13 cm-3 g-1 for Ni). We propose that the low-cost, environmentally friendly M-struvites could be obtained as recycling products from industrial and agricultural wastewaters. These waste products could be then upcycled into mesoporous TMPs through a simple thermal treatment for further applications, for instance, in (electro)catalysis. KW - Struvite KW - Pphosphates KW - Transition metal KW - In-situ SAXS/WAXS KW - Mesoporosity PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569503 DO - https://doi.org/10.1039/D2NR05630E SN - 2040-3364 SP - 1 EP - 15 PB - Royal Society of Chemistry (RSC) AN - OPUS4-56950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karafiludis, Stephanos A1 - Bhattacharya, Biswajit A1 - de Oliveira Guilherme Buzanich, Ana A1 - Fink, Friedrich A1 - Feldmann, Ines A1 - ten Elshof, J. E. A1 - Emmerling, Franziska A1 - Stawski, Tomasz T1 - Thermally processed Ni-and Co-struvites as functional materials for proton conductivity N2 - We present how mesoporosity can be engineered in transition metal phosphate (TMPs) materials in a template-free manner. The method involves the transformation of a precursor metal phosphate phase, called M-struvite (NH4MPO4·6H2O, M = Mg2+, Ni2+, Co2+, NixCo1−x2+). It relies on the thermal decomposition of crystalline M-struvite precursors to an amorphous and simultaneously mesoporous phase, which forms during degassing of NH3 and H2O. The temporal evolution of mesoporous frameworks and the response of the metal coordination environment were followed by in situ and ex situ scattering and diffraction, as well as X-ray spectroscopy. Despite sharing the same precursor struvite structure, different amorphous and mesoporous structures were obtained depending on the involved transition metal. We highlight the systematic differences in absolute surface area, pore shape, pore size, and phase transitions depending on the metal cation present in the analogous M-struvites. The amorphous structures of thermally decomposed Mg-, Ni- and NixCo1−x-struvites exhibit high surface areas and pore volumes (240 m2 g−1 and 0.32 cm−3 g−1 for Mg and 90 m2 g−1 and 0.13 cm−3 g−1 for Ni). We propose that the low-cost, environmentally friendly M-struvites could be obtained as recycling products from industrial and agricultural wastewaters. These waste products could be then upcycled into mesoporous TMPs through a simple thermal treatment for further application, for instance in (electro)catalysis. KW - Struvite KW - Phosphates KW - Transition metals KW - Proton conductivity PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575862 DO - https://doi.org/10.1039/D3DT00839H SN - 1477-9226 SP - 1 EP - 13 PB - Royal Society of Chemisty (RSC) CY - London/Cambridge AN - OPUS4-57586 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karafiludis, Stephanos A1 - Ryll, T. W. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Stawski, Tomasz Maciej T1 - Phase stability studies on transition metal phosphates aided by an automated synthesis N2 - Transition metal phosphates (TMPs) have attracted interest as materials for (electro-) catalysis, and electrochemistry due to their low-cost, stability, and tunability. In this work, an automated synthesis platform was used for the preparation of transition metal phosphate crystals to efficiently explore the multidimensional parameter space, determining the phase selection, crystal sizes, shapes. By using X-ray diffraction and spectroscopy-based methods and electron microscopy imaging, a complete characterization of the phase stability fields, phase transitions, and crystal morphology/sizes was achieved. In an automated three-reactant synthesis, the individual effect of each reactant species NH4+, M2+, and PO43- on the formation of transition metal phosphate phases: M-struvite NH4MPO4·6H2O, M-phosphate octahydrate M3(PO4)2·8H2O with M = Ni, Co and an amorphous phase, was investigated. The NH4+ concentration dictates the phase composition, morphology, and particle size in the Ni-system (crystalline Ni-struvite versus amorphous Ni-PO4 phase), whereas in the Co-system all reactant species - NH4+, Co2+, and PO43- - influence the reaction outcome equivalently (Co-struvite vs. Co-phosphate octahydrate). The coordination environment for all crystalline compounds and of the amorphous Ni-PO4 phase was resolved by X-ray absorption spectroscopy, revealing matching characteristics to its crystalline analogue, Ni3(PO4)2·8H2O. The automated synthesis turned out to be significantly advantageous for the exploration of phase diagrams due to its simple modularity, facile traceability, and enhanced reproducibility compared to a typical manual synthesis. KW - Automated synthesis KW - Phase diagrams KW - Transition metals KW - Phosphates KW - Local structure KW - Struvite PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579151 DO - https://doi.org/10.1039/D3CE00386H VL - 25 IS - 30 SP - 4333 EP - 4344 PB - CrystEngComm CY - London AN - OPUS4-57915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Akhmetova, Irina A1 - Das, Chayanika A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska T1 - Synthesis and In Situ Monitoring of Mechanochemical Preparation of Highly Proton Conductive Hydrogen-Bonded Metal Phosphonates N2 - Crystalline porous materials are recognized as promising proton conductors for the proton exchange membrane (PEM) in fuel cell technology owing to their tunable framework structure. However, it is still a challenging bulk synthesis for real-world applications of these materials. Herein, we report the mechanochemical gram-scale synthesis of two isostructural metal hydrogen-bonded organic frameworks (MHOFs) of Co(II) and Ni(II) based on 1-hydroxyethylidenediphosphonic acid (HEDPH4) with 2,2′-bipyridine (2,2′-bipy): Co(HEDPH3)2(2,2′-bipy)·H2O (1) and Ni(HEDPH3)2(2,2′-bipy)·H2O (2). In situ monitoring of the mechanochemical synthesis using different synchrotron-based techniques revealed a one-step mechanism – the starting materials are directly converted to the product. With the existence of extensive hydrogen bonds with amphiprotic uncoordinated phosphonate hydroxyl and oxygen atoms, both frameworks exhibited proton conduction in the range of 10–4 S cm–1 at room temperature under humid conditions. This study demonstrates the potential of green mechanosynthesis for bulk material preparation of framework-based solid-state proton conductors. KW - Mechanochemistry KW - Proton conductivity KW - Metal Organic Frameworks PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-577777 DO - https://doi.org/10.1021/acssuschemeng.2c07509 VL - 8 IS - 19 SP - 16687 EP - 16693 PB - ACS Publications AN - OPUS4-57777 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 - 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 - Heinekamp, Christian A1 - de Oliveira Guilherme Buzanich, Ana A1 - Ahrens, M. A1 - Braun, T. A1 - Emmerling, Franziska T1 - An amorphous Lewis-acidic zirconium chlorofluoride as HF shuttle: C–F bond activation and formation N2 - An exceptional HF transfer reaction by C–F bond activation of fluoropentane and a subsequent hydrofluorination of alkynes at room temperature is reported. An amorphous Lewis-acidic Zr chlorofluoride serves as heterogeneous catalyst, which is characterised by an eightfold coordination environment at Zr including chlorine atoms. The studies are seminal in establishing sustainable fluorine chemistry. KW - ZCF KW - Heterogeneous catalysis KW - C-F bond activation KW - HF-shuttle PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582249 DO - https://doi.org/10.1039/D3CC03164K SN - 1359-7345 VL - 59 IS - 75 SP - 11224 EP - 11227 PB - RSC CY - Cambridge AN - OPUS4-58224 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 - Feiler, Torvid A1 - Yasuda, N. A1 - Michalchuk, Adam A1 - Emmerling, Franziska A1 - Bhattacharya, Biswajit T1 - Mechanistic Investigation of an Elastically Flexible Organic Crystal N2 - Mechanical flexibility in molecular crystals is a fascinating behavior with potential for developing advanced technologies. However, the phenomenon of mechanical bending is poorly understood. We explore for the first time the atomistic origin of elastic bending in a single component organic crystal using a combination of μ-focus synchrotron X-ray diffraction and ab initio simulation. KW - Flexible crystals KW - DFT calculation KW - Bending mechanism PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581949 DO - https://doi.org/10.1021/acs.cgd.3c00473 SN - 1528-7483 VL - 23 IS - 9 SP - 6244 EP - 6249 PB - ACS Publications AN - OPUS4-58194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Kaufmann, Jan Ole A1 - Mangarova, D. B. A1 - Moeckel, J. A1 - Adams, L. C. A1 - Brangsch, J. A1 - Heyl, J. L. A1 - Zhao, J. A1 - Verlemann, C. A1 - Karst, U. A1 - Collettini, F. A1 - Auer, T. A. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Collagen-specific molecular magnetic resonance imaging of prostate cancer N2 - Constant interactions between tumor cells and the extracellular matrix (ECM) influence the progression of prostate cancer (PCa). One of the key components of the ECM are collagen fibers, since they are responsible for the tissue stiffness, growth, adhesion, proliferation, migration, invasion/metastasis, cell signaling, and immune recruitment of tumor cells. To explore this molecular marker in the content of PCa, we investigated two different tumor volumes (500 mm3 and 1000 mm3) of a xenograft mouse model of PCa with molecular magnetic resonance imaging (MRI) using a collagen-specific probe. For in vivo MRI evaluation, T1-weighted sequences before and after probe administration were analyzed. No significant signal difference between the two tumor volumes could be found. However, we detected a significant difference between the signal intensity of the peripheral tumor area and the central area of the tumor, at both 500 mm3 (p < 0.01, n = 16) and at 1000 mm3 (p < 0.01, n = 16). The results of our histologic analyses confirmed the in vivo studies: There was no significant difference in the amount of collagen between the two tumor volumes (p > 0.05), but within the tumor, higher collagen expression was observed in the peripheral area compared with the central area of the tumor. Laser ablation with inductively coupled plasma mass spectrometry further confirmed these results. The 1000 mm3 tumors contained 2.8 +- 1.0% collagen and the 500 mm3 tumors contained 3.2 +- 1.2% (n = 16). There was a strong correlation between the in vivo MRI data and the ex vivo histological data (y = 0.068x + 1.1; R2 = 0.74) (n = 16). The results of elemental analysis by inductively coupled plasma mass spectrometry supported the MRI data (y = 3.82x + 0.56; R2 = 0.79; n = 7). MRI with the collagen-specific probe in PCa enables differentiation between different tumor areas. This may help to differentiate tumor from healthy tissue, potentially identifying tumor areas with a specific tumor biology. KW - Molecular imaging KW - Magnetic resonance imaging KW - MRI KW - Prostate cancer KW - Collagen KW - Laser ablation-inductively coupled plasma-mass spectroscopy KW - EP-3533 KW - Peptide probe KW - Gd-DOTA KW - Contrast agent KW - Tumor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568449 DO - https://doi.org/10.3390/ijms24010711 SN - 1422-0067 SN - 1661-6596 VL - 24 IS - 1 SP - 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-56844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tannenberg, Robert A1 - Paul, Martin A1 - Röder, Bettina A1 - Gande, S. L. A1 - Sreeramulu, S. A1 - Saxena, K. A1 - Richter, C. A1 - Schwalbe, H. A1 - Swart, C. A1 - Weller, Michael G. T1 - Chemiluminescence biosensor for the determination of cardiac troponin I (cTnI) N2 - Cardiac troponin I (cTnI) is a crucial biomarker for diagnosing cardiac vascular diseases, including acute myocardial infarction (AMI). This study presents a proof-of-concept chemiluminescence-based immunosensor for rapid and accurate measurement of cTnI, with the potential for online monitoring. The immunosensor incorporates a flow cell design and a sensitive complementary metal-oxide-semiconductor (CMOS) camera for optical readout. A microfluidic setup was established to enable selective and quasi-online determination of cTnI within ten minutes. The sensor was tested with recombinant cTnI in phosphate buffer, demonstrating measurements in the concentration range of 2–25 µg/L, with a limit of detection (LoD) of 0.6 µg/L (23 pmol/L) achieved using the optimized system. The immunosensor exhibited high selectivity, as no cross-reactivity was observed with other recombinant proteins such as cTnT and cTnC at a concentration of 16 µg/L. Measurements with diluted blood plasma and serum yielded an LoD of 60 µg/L (2.4 nmol/L) and 70 µg/L (2.9 nmol/L), respectively. This biosensor offers a promising approach for the rapid and sensitive detection of cTnI, contributing to the diagnosis and management of acute myocardial infarction and other cardiac vascular diseases. N2 - Das kardiale Troponin I (cTnI) ist ein wichtiger Biomarker für die Diagnose von Herz-Kreislauf-Erkrankungen, einschließlich des akuten Myokardinfarkts (AMI). In dieser Studie wird ein auf Chemilumineszenz basierender Immunsensor für die schnelle und genaue Messung von cTnI vorgestellt, der das Potenzial für eine Online-Überwachung hat. Der Immunsensor besteht aus einer Durchflusszelle und einer empfindlichen CMOS-Kamera (Complementary Metal-Oxide-Semiconductor) zur optischen Detektion. Es wurde ein mikrofluidischer Aufbau entwickelt, der eine selektive und quasi Online-Bestimmung von cTnI innerhalb von zehn Minuten ermöglicht. Der Sensor wurde mit rekombinantem cTnI in Phosphatpuffer getestet und zeigte einen Messbereich von 2-25 µg/L, wobei mit dem optimierten System eine Nachweisgrenze (LoD) von 0,6 µg/L (23 pmol/L) erreicht wurde. Der Immunsensor zeigte eine hohe Selektivität, da keine Kreuzreaktivität mit anderen rekombinanten Proteinen wie cTnT und cTnC bei einer Konzentration von 16 µg/L beobachtet wurde. Messungen mit verdünntem Blutplasma und Serum ergaben einen LoD von 60 µg/L (2,4 nmol/L) bzw. 70 µg/L (2,9 nmol/L). Dieser Biosensor bietet einen vielversprechenden Ansatz für den schnellen und empfindlichen Nachweis von cTnI, der zur Diagnose und Behandlung des akuten Myokardinfarkts und anderer kardialer Gefäßerkrankungen beitragen kann. KW - Acute myocardial infarction KW - Heart attack KW - Emergency KW - Diagnosis KW - Cardiac troponin KW - Biomarker KW - Immunosensor KW - Biosensor KW - Chemiluminescence KW - Luminol KW - Peroxidase KW - Monoclonal antibodies KW - Flow injection immunoassay KW - Immunometric assay KW - Immunometric biosensor KW - Microfluidic system KW - Monolithic column KW - Online biosensor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575471 DO - https://doi.org/10.3390/bios13040455 SN - 2079-6374 VL - 13 IS - 4 SP - 1 EP - 20 PB - MDPI CY - Basel AN - OPUS4-57547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völzke, Jule L. A1 - Smatty, Sarah A1 - Döring, Sarah A1 - Ewald, Shireen A1 - Oelze, Marcus A1 - Fratzke, Franziska A1 - Flemig, Sabine A1 - Konthur, Zoltán A1 - Weller, Michael G. T1 - Efficient Purification of Polyhistidine-Tagged Recombinant Proteins Using Functionalized Corundum Particles N2 - Immobilized metal affinity chromatography (IMAC) is a widely used technique for purifying polyhistidine-tagged recombinant proteins. However, it often has practical limitations that require complex optimizations and additional steps for purification. In this study, we introduce functionalized corundum particles as a novel, efficient, and economical method for purifying recombinant proteins in a column-free format. The corundum surface is modified with amino silane APTES, followed by EDTA dianhydride, and then loaded with nickel ions. We used the Kaiser test to monitor the modification process and ICP-MS to quantify the metal-binding capacity. To evaluate the system, we used His-tagged protein A/G (PAG) mixed with bovine serum albumin (BSA). The corundum particles exhibited a binding capacity of approximately 3 mg of protein per gram of corundum or 2.4 mg per 1 mL of corundum suspension. We also examined cytoplasm obtained from different E. coli strains as an example of a complex matrix. Varying the imidazole concentration in the loading and washing buffers showed that higher concentrations during loading improved purity. Even with sample volumes as large as one liter, we successfully isolated recombinant proteins down to a concentration of 1 µg/mL. We found higher purity levels with corundum when comparing the corundum material to standard Ni–NTA agarose beads. We successfully purified His6-MBP-mSA2, a fusion protein comprising monomeric streptavidin and maltose-binding protein, from E. coli cytoplasm, demonstrating the method's applicability. We also purified SARS-CoV-2-S-RBD-His8 expressed in human Expi293F cells, confirming its suitability for mammalian cell culture supernatants. The material cost of the nickel-loaded corundum material (without regeneration) is estimated to be less than 30 cents per gram of functionalized support or 10 cents per milligram of isolated protein. Another advantage of this system is the exceptional physical and chemical stability of corundum particles. Overall, we have demonstrated that this novel material offers an efficient, robust, and cost-effective purification platform for His-tagged proteins, even in challenging, complex matrices and large sample volumes with low product concentrations. This method has potential applications in both small laboratories and large-scale industrial settings. N2 - Die immobilisierte Metallaffinitätschromatographie (IMAC) ist eine weit verbreitete Technik zur Reinigung von rekombinanten Proteinen mit Polyhistidin-Markierung. Sie hat jedoch oft praktische Einschränkungen, die komplexe Optimierungen und zusätzliche Schritte für die Aufreinigung erfordern. In dieser Studie stellen wir funktionalisierte Korundpartikel als neuartige, effiziente und wirtschaftliche Methode zur Reinigung rekombinanter Proteine in einem säulenfreien Format vor. Die Korundoberfläche wird mit dem Aminosilan APTES und anschließend mit EDTA-Dianhydrid modifiziert und dann mit Nickelionen beladen. Wir haben den Kaiser-Test zur Überwachung des Modifizierungsprozesses und ICP-MS zur Quantifizierung der Metallbindungskapazität verwendet. Zur Charakterisierung des Systems verwendeten wir His-markiertes Protein A/G (PAG) in Kombination mit Rinderserumalbumin (BSA). Die Korundpartikel wiesen eine Bindungskapazität von etwa 3 mg Protein pro Gramm Korund oder 2,4 mg pro 1 ml Korundsuspension auf. Als Beispiel für eine komplexe Matrix untersuchten wir auch Zytoplasma, das aus verschiedenen E. coli-Stämmen gewonnen wurde. Die Variation der Imidazolkonzentration in den Lade- und Waschpuffern zeigte, dass höhere Konzentrationen beim Laden die Reinheit verbesserten. Selbst bei einem Probenvolumen von bis zu einem Liter konnten wir rekombinante Proteine von 1 µg/mL isolieren. Beim Vergleich des Korundmaterials mit Standard-Ni-NTA-Agarose-Beads stellten wir einen höheren Reinheitsgrad mit Korund fest. Wir reinigten erfolgreich His6-MBP-mSA2 aus E. coli-Zytoplasma, ein Fusionsprotein, das aus monomerem Streptavidin und Maltose-bindendem Protein besteht. Wir reinigten auch SARS-CoV-2-S-RBD-His8, das in humanen Expi293F-Zellen exprimiert wurde, und bestätigten damit die Eignung des Materials für Zellkulturüberstände von Säugetieren. Die Materialkosten für nickelbeladenen Korund (ohne Regenerierung) werden auf weniger als 30 Cent pro Gramm funktionalisierten Trägers oder 10 Cent pro Milligramm isolierten Proteins geschätzt. Ein weiterer Vorteil dieses Systems ist die außergewöhnliche physikalische und chemische Stabilität der Korundpartikel. Insgesamt haben wir gezeigt, dass dieses neuartige Material eine effiziente, robuste und kostengünstige Reinigungsplattform für His-markierte Proteine bietet, selbst bei schwierigen, komplexen Matrices und großen Probenmengen mit niedrigen Produktkonzentrationen. Diese Methode könnte sowohl in kleinen Labors als auch in der Großindustrie eingesetzt werden. KW - Aluminum oxide KW - Sapphire KW - Ethylenediaminetetraacetic acid KW - Nickel chelate KW - EDTAD KW - HexaHis-Tag KW - His6 KW - 6xHis KW - His8 KW - Bioseparation KW - IMAC purification KW - Immunocapture KW - Affinity chromatography KW - Carrier KW - Nickel KW - Recombinant protein KW - Escherichia coli KW - Bacterial lysates KW - Cytoplasm KW - Polishing KW - Downstream processing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575672 DO - https://doi.org/10.3390/biotech12020031 VL - 12 IS - 2 SP - 1 EP - 18 PB - MDPI CY - Basel, Schweiz AN - OPUS4-57567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Filimonova, S. M. A1 - Melnikov, E. S. A1 - Kaufmann, Jan Ole A1 - Shchepochkina, O. Y. A1 - Eremin, S. A. A1 - Gravel, I. V. A1 - Raysyan, Anna T1 - Exploring the anti‐α‐amylase activity of flavonoid aglycones in fabaceae plant extracts: a combined MALDI‐TOF‐MS and LC–MS/MS approach N2 - A combination of TLC-bioautography, MALDI-TOF-MS and LC–MS/MS methods was used to identify flavonoids with anti-α-amylase activity in extracts of Lathyrus pratensis L. (herb), L. polyphillus L. (fruits), Thermopsis lanceolata R. Br. (herb) and S. japonica L. (buds). After the TLC-autobiography assay, substances with anti-amylase activity were identified by MALDI-TOF-MS followed by confirmation of the result by LC–MS/MS. Results of the study revealed that the flavonoids apigenin, luteolin, formononetin, genistein and kaempferol display marked anti-α-amylase activity. Formononetin showed the largest activity. Compared with LC–MS/MS, MALDI-TOF-MS is a quick and convenient method; results can be obtained within minutes; and only minor sample amounts are required which allows us to analyse mixtures of substances without preliminary separation. However, the inability to distinguish between isomers is the main limitation of the method. KW - Enzyme KW - MALDI-TOF-MS KW - LC-MS/MS KW - Massenspektrometrie PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-577128 DO - https://doi.org/https://doi.org/10.1111/ijfs.16491 SN - 0950-5423 VL - 58 IS - 7 SP - 3902 EP - 3911 PB - Wiley & Sons CY - Hoboken, NJ, USA AN - OPUS4-57712 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghiringhelli, Luca M. A1 - Baldauf, Carsten A1 - Bereau, Tristan A1 - Brockhauser, Sandor A1 - Carbogno, Christian A1 - Chamanara, Javad A1 - Cozzini, Stefano A1 - Curtarolo, Stefano A1 - Draxl, Claudia A1 - Dwaraknath, Shyam A1 - Fekete, Ádám A1 - Kermode, James A1 - Koch, Christoph T. A1 - Kühbach, Markus A1 - Ladines, Alvin Noe A1 - Lambrix, Patrick A1 - Himmer, Maja-Olivia A1 - Levchenko, Sergey V. A1 - Oliveira, Micael A1 - Michalchuk, Adam A1 - Miller, Ronald E. A1 - Onat, Berk A1 - Pavone, Pasquale A1 - Pizzi, Giovanni A1 - Regler, Benjamin A1 - Rignanese, Gian-Marco A1 - Schaarschmidt, Jörg A1 - Scheidgen, Markus A1 - Schneidewind, Astrid A1 - Sheveleva, Tatyana A1 - Su, Chuanxun A1 - Usvyat, Denis A1 - Valsson, Omar A1 - Wöll, Christof A1 - Scheffler, Matthias T1 - Shared metadata for data-centric materials science N2 - The expansive production of data in materials science, their widespread sharing and repurposing requires educated support and stewardship. In order to ensure that this need helps rather than hinders scientific work, the implementation of the FAIR-data principles (Findable, Accessible, Interoperable, and Reusable) must not be too narrow. Besides, the wider materials-science community ought to agree on the strategies to tackle the challenges that are specific to its data, both from computations and experiments. In this paper, we present the result of the discussions held at the workshop on “Shared Metadata and Data Formats for Big-Data Driven Materials Science”. We start from an operative definition of metadata, and the features that a FAIR-compliant metadata schema should have. We will mainly focus on computational materials-science data and propose a constructive approach for the FAIRification of the (meta)data related to ground-state and excited-states calculations, potential-energy sampling, and generalized workflows. Finally, challenges with the FAIRification of experimental (meta)data and materials-science ontologies are presented together with an outlook of how to meet them. KW - Library and Information Sciences KW - Statistics, Probability and Uncertainty KW - Computer Science Applications KW - Education KW - Information Systems KW - Statistics and Probability PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584846 DO - https://doi.org/10.1038/s41597-023-02501-8 VL - 10 IS - 1 SP - 1 EP - 18 PB - Springer Science and Business Media LLC AN - OPUS4-58484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Driscoll, Laura L. A1 - Driscoll, Elizabeth H. A1 - Dong, Bo A1 - Sayed, Farheen N. A1 - Wilson, Jacob N. A1 - O’Keefe, Christopher A. A1 - Gardner, Dominic J. A1 - Grey, Clare P. A1 - Allan, Phoebe K. A1 - Michalchuk, Adam A1 - Slater, Peter R. T1 - Under pressure: offering fundamental insight into structural changes on ball milling battery materials N2 - Synthesis of Li ion battery materials via ball milling has been a huge area of growth, leading to new high-capacity electrode materials, such as a number of promising disordered rocksalt (DRS) phases. In prior work, it was generally assumed that the synthesis was facilitated simply by local heating effects during the milling process. In this work, we show that ball milling Li2MoO4 leads to a phase transformation to the high pressure spinel polymorph and we report electrochemical data for this phase. This observation of the formation of a high pressure polymorph shows that local heating effects alone cannot explain the phase transformation observed (phenakite to spinel) and so indicates the importance of other effects. In particular, we propose that when the milling balls collide with the material, the resulting shockwaves exert a localised pressure effect, in addition to local heating. To provide further support for this, we additionally report ball milling results for a number of case studies (Li2MnO3, Li2SnO3, Nb2O5) which reinforces the conclusion that local heating alone cannot explain the phase transformations observed. The work presented thus provides greater fundamental understanding of milling as a synthetic pathway and suggests potential strategies to prepare such samples without milling (e.g., doping to create internal chemical pressure). In addition, we suggest that further research is needed into the effect of the use of milling as a route to smaller particles, since we believe that such milling may also be affecting the surface structure of the particles through the influence of the shockwaves generated. KW - Pollution KW - Nuclear Energy and Engineering KW - Sustainability and the Environment KW - Environmental Chemistry KW - Renewable Energy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590086 DO - https://doi.org/10.1039/d3ee00249g VL - 16 IS - 11 SP - 5196 EP - 5209 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -