TY - JOUR A1 - Fantin, Andrea A1 - Lepore, G. O. A1 - Widom, M. A1 - Kasatikov, S. A1 - Manzoni, Anna Maria T1 - How Atomic Bonding Plays the Hardness Behavior in the Al–Co–Cr–Cu–Fe–Ni High Entropy Family N2 - A systematic study on a face‐centered cubic‐based compositionally complex alloy system Al–Co–Cr–Cu–Fe–Ni in its single‐phase state is carried out, where a mother senary compound Al₈Co₁₇Cr₁₇Cu₈Fe₁₇Ni₃₃ and five of its suballoys, obtained by removing one element at a time, are investigated and exhaustively analyzed determining the contribution of each alloying element in the solid solution. The senary and the quinaries are compared using experimental techniques including X‐ray absorption spectroscopy, X‐ray diffraction, transmission electron microscopy, and first principles hybrid Monte Carlo/molecular dynamics simulations. Chemical short‐range order and bond length distances have been determined both at the experimental and computational level. Electronic structure and local atomic distortions up to 5.2 Å have been correlated to the microhardness values. A linear regression model connecting hardness with local lattice distortions is presented. KW - High entropy alloys KW - EXAFS KW - Short-range order KW - Microhardness KW - Alloy design KW - Transmission electron microscopy KW - Lattice distortion PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593333 DO - https://doi.org/https://doi.org/10.1002/smsc.202300225 SN - 2688-4046 SP - 1 EP - 12 PB - Wiley CY - Weinheim AN - OPUS4-59333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Richter, Silke A1 - Vogl, Jochen A1 - Kipphardt, Heinrich T1 - On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis N2 - During its 25 years of existence, the Inorganic Analysis Working Group of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM IAWG) has achieved much in establishing comparability of measurement results. Impressive work has been done on comparison exercises related to real-world problems in fields such as ecology, food, or health. In more recent attempts, measurements and comparisons were focused on calibration solutions which are the basis of most inorganic chemical measurements. This contribution deals with the question of how to achieve full and transparent SI traceability for the values carried by such solutions. Within this framework, the use of classical primary methods (CPMs) is compared to the use of a primary difference method (PDM). PDM is a method with a dual character, namely a metrological method with a primary character, based on the bundling of many measurement methods for individual impurities, which lead to materials with certified content of the main component. As in classical methods, where small corrections for interferences are accepted, in PDM, many small corrections are bundled. In contrast to classical methods, the PDM is universally applicable to all elements in principle. Both approaches can be used to certify the purity (expressed as mass fraction of the main element) of a high-purity material. This is where the metrological need of National Metrology Institutes (NMIs) for analytical methods meet the challenges of analytical methods. In terms of methods, glow discharge mass spectrometry (GMDS) with sufficient uncertainties for sufficiently small impurity contents is particularly noteworthy for the certification of primary transfer standards (PTS), and isotope dilution mass spectrometry (IDMS), which particularly benefits from PTS (back-spikes) with small uncertainties, is particularly noteworthy for the application. The corresponding relative uncertainty which can be achieved using the PDM is very low (< 10−4). Acting as PTS, they represent the link between the material aspect of the primary calibration solutions and the immaterial world of the International System of Units (SI). The underlying concepts are discussed, the current status of implementation is summarised, and a roadmap of the necessary future activities in inorganic analytical chemistry is sketched. It has to be noted that smaller measurement uncertainties of the purity of high-purity materials not only have a positive effect on chemical measurements, but also trigger new developments and findings in other disciplines such as thermometry or materials science. KW - Inorganic chemical analysis KW - Primary transfer standards (PTSs) KW - Traceability KW - Classical primary measurement method (CPM) KW - Primary difference measurement method (PDM) KW - Metrology in chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572743 DO - https://doi.org/10.1007/s00216-023-04660-4 SN - 1618-2642 SN - 1618-2650 VL - 415 SP - 3057 EP - 3071 PB - Springer CY - Berlin AN - OPUS4-57274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Piechotta, Christian A1 - Lisec, Jan A1 - Sommerfeld, Thomas A1 - Kluge, Stephanie A1 - Herzel, Hannes A1 - Huthwelker, T. A1 - Borca, C. A1 - Simon, Franz-Georg T1 - Levels of per- and polyfluoroalkyl substances (PFAS) in various wastewater-derived fertilizers - Analytical investigations from different perspectives N2 - Solid wastewater-based fertilizers were screened for per- and polyfluoroalkyl substances (PFAS) by the extractable organic fluorine (EOF) sum parameter method. The EOF values for ten sewage sludges from Germany and Switzerland range from 154 to 7209 mg kg−1. For thermal treated sewage sludge and struvite the EOF were lower with values up to 121 mg kg−1. Moreover, the application of PFAS targeted and suspect screening analysis of selected sewage sludge samples showed that only a small part of the EOF sum parameter values can be explained by the usually screened legacy PFAS. The hitherto unknown part of EOF sum parameter contains also fluorinated pesticides, pharmaceutical and aromatic compounds. Because these partly fluorinated compounds can degrade to (ultra-)short PFAS in wastewater treatment plants they should be considered as significant sources of organic fluorine in the environment. The combined results of sum parameter analysis and suspect screening reveal the need to update current regulations, such as the German fertilizer ordinance, to focus not solely on a few selected PFAS such as perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) but consider an additional sum parameter approach as a more holistic alternative. Moreover, diffusion gradient in thin-films (DGT) passive samplers were utilized as an alternative simplified extraction method for PFAS in solid wastewater-based fertilizers and subsequently quantified via combustion ion chromatography. However, the DGT method was less sensitive and only comparable to the EOF values of the fertilizers in samples with >150 mg kg−1, because of different diffusion properties for various PFAS, but also kinetic exchange limitations. KW - Combustion ion chromatography KW - Per- and polyfluoroalkyl substances (PFAS) KW - Sewage sludge KW - Fertilizer PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583429 DO - https://doi.org/10.1039/d3va00178d SN - 2754-7000 VL - 2 IS - 10 SP - 1436 EP - 1445 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-58342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kislenko, Evgeniia A1 - Incel, A. A1 - Gawlitza, Kornelia A1 - Sellergren, B. A1 - Rurack, Knut T1 - Towards molecularly imprinted polymers that respond to and capture phosphorylated tyrosine epitopes using fluorescent bis-urea and bis-imidazolium receptors N2 - Early detection of cancer is essential for successful treatment and improvement in patient prognosis. Deregulation of post-translational modifications (PTMs) of proteins, especially phosphorylation, is present in many types of cancer. Therefore, the development of materials for the rapid sensing of low abundant phosphorylated peptides in biological samples can be of great therapeutic value. In this work, we have synthesised fluorescent molecularly imprinted polymers (fMIPs) for the detection of the phosphorylated tyrosine epitope of ZAP70, a cancer biomarker. The polymers were grafted as nanometer-thin shells from functionalised submicron-sized silica particles using a reversible addition-fragmentation chain-transfer (RAFT) polymerisation. Employing the combination of fluorescent urea and intrinsically cationic bis-imidazolium receptor cross-linkers, we have developed fluorescent sensory particles, showing an imprinting factor (IF) of 5.0. The imprinted polymer can successfully distinguish between phosphorylated and non-phosphorylated tripeptides, reaching lower micromolar sensitivity in organic solvents and specifically capture unprotected peptide complements in a neutral buffer. Additionally, we have shown the importance of assessing the influence of counterions present in the MIP system on the imprinting process and final material performance. The potential drawbacks of using epitopes with protective groups, which can co-imprint with targeted functionality, are also discussed. KW - Functional monomers KW - Molecularly imprinted polymers KW - Phosphorylated peptides KW - Fluorescence KW - Core-shell particles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588089 DO - https://doi.org/10.1039/d3tb01474f SN - 2050-750X SP - 1 EP - 10 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-58808 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 - Abusafia, A. A1 - Scheid, C. A1 - Meurer, Maren A1 - Altmann, Korinna A1 - Dittmer, U. A1 - Steinmetz, H. T1 - Microplastic sampling strategies in urban drainage systems for quantification of urban emissions based on transport pathways N2 - Tracking waterborne microplastic (MP) in urban areas is a challenging task because of the various sources and transport pathways involved. Since MP occurs in low concentrations in most wastewater and stormwater streams, large sample volumes need to be captured, prepared, and carefully analyzed. The recent research in urban areas focused mainly on MP emissions at wastewater treatment plants (WWTPs), as obvious entry points into receiving waters. However, important transport pathways under wet-weather conditions are yet not been investigated thoroughly. In addition, the lack of comprehensive and comparable sampling strategies complicated the attempts for a deeper understanding of occurrence and sources. The goal of this paper is to (i) introduce and describe sampling strategies for MP at different locations in a municipal catchment area under dry and wet-weather conditions, (ii) quantify MP emissions from the entire catchment and two other smaller ones within the bigger catchment, and (iii) compare the emissions under dry and wet-weather conditions. WWTP has a high removal rate of MP (>96%), with an estimated emission rate of 189 kg/a or 0.94 g/[population equivalents (PEQ · a)], and polyethylene (PE) as the most abundant MP. The specific dry-weather emissions at a subcatchment were ≈30 g/(PEQ · a) higher than in the influent of WWTP with 23 g/(PEQ · a). Specific wet-weather emissions from large sub-catchment with higher traffic and population densities were 1952 g/(ha · a) higher than the emissions from smaller catchment (796 g/[ha · a]) with less population and traffic. The results suggest that wet-weather transport pathways are likely responsible for 2–4 times more MP emissions into receiving waters compared to dry-weather ones due to tire abrasion entered from streets through gullies. However, more investigations of wet-weather MP need to be carried out considering additional catchment attributes and storm event characteristics. KW - Combined sewer system KW - Large volume samplers KW - Microplastic pollution KW - Separate sewer system KW - Stormwater retention tank PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568271 DO - https://doi.org/10.1002/appl.202200056 SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brandt, S. A1 - Brozowski, F. A1 - Horn, Wolfgang A1 - Müller, B. T1 - Odour testing of building products: Examinations for an on-going development of the test standard ISO 16000-28 N2 - VOC-emissions and their odours from building products and furnishings present indoors should not have an impact on personal well-being or health. Odours can be measured by applying the standard ISO 16000-28. Indoor air determination of odour emissions from building products using test chambers. One of the described procedures is the assessment of perceived intensity using a comparative scale by a group of panellists. In this paper, the perceived intensity sampling procedure and its evaluation method are investigated and shown to need improvement. New technical developments in the methodology used to increase the reproducibility of measurement results are discussed. Since odour tests are used for labelling, they have a major influence on the assessment of construction products, similar to the procedure of the German Committee for Health Evaluation of Building Products (AgBB). In the original ISO standard, the evaluation is typically performed using a sampling container separated from the emission chamber. For a better sample presentation, an adapter was developed to connect the emission test chamber to the evaluation funnel and thus enable an odour assessment which is comparable to a direct measurement. The investigations show that losses of odourous substances can be greatly reduced, which is very desirable when seeking to obtain reliable results in odour measurement. Another experimental series was carried out to reduce the measurement effort in the evaluation of perceived intensity. Application of the developed greater than or less than/equal to. query could be helpful here. The results show that the query mostly leads to the same result as the evaluation of the perceived intensity using the method according to the standard but is much easier to perform. Overall, the results can contribute to improving the acceptance of the evaluation of perceived intensity using ISO 16000-28 and to determining odours from building materials increasingly more precisely. T2 - Healthy Buildings 2023 Europe CY - Aachen, Germany DA - 11.06.2023 KW - Building material KW - Odour KW - Perceived intensity KW - VOC KW - Emission test chamber PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580070 SP - 345 EP - 352 PB - ISIAQ (International Society of Indoor Air Quality and Climate) CY - Herndon, VA, USA AN - OPUS4-58007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Bednarz, Marius A1 - Braun, Ulrike A1 - Bannick, Claus Gerhard A1 - Ricking, Mathias A1 - Altmann, Korinna T1 - A promising approach to monitor microplastic masses in composts N2 - Inputs of plastic impurities into the environment via the application of fertilizers are regulated in Germany and the EU by means of ordinances. Robust and fast analytical methods are the basis of legal regulations. Currently, only macro- and large microplastic contents (>1 mm) are measured. Microplastics (1–1,000 µm), are not yet monitored. Thermal analytical methods are suitable for this purpose, which can determine the mass content and can also be operated fully automatically in routine mode. Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) allows the identification of polymers and the determination of mass contents in solid samples from natural environments. In accordance with the German or European Commission (EC) Fertiliser Ordinance, composting plants should be monitored for microplastic particles with this method in the future. In this context a compost plant was sampled. At the end of the rotting process, the compost was sieved and separated in a coarse (>1 mm) and a fine fraction (<1 mm). The fine fraction was processed using density separation comparing NaCl and NaI as possible salt alternative and screened for microplastic masses by TED-GC/MS with additional validation and quality assurance experiments. With TED-GC/MS total microplastics mass contents of 1.1–3.0 μg/mg in finished compost could be detected with polyethylene mainly. What differs much to the total mass of plastics in the coarse fraction with up to 60 μg/mg, which were visually searched, identified via ATR-FTIR and gravimetrically weighted. KW - Microplastics KW - TED-GC/MS KW - Compost KW - Monitoring KW - Soil PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586688 DO - https://doi.org/10.3389/fenvc.2023.1281558 SN - 2673-4486 VL - 4 SP - 1 EP - 12 PB - Frontiers Media CY - Lausanne AN - OPUS4-58668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Hoffmann, Thomas A1 - Range, David A1 - Altmann, Korinna T1 - Microplastics in sediments of the river Rhine—A workflow for preparation and analysis of sediment samples from aquatic river systems for monitoring purposes N2 - AbstractMicroplastics (MP) can be detected in all environmental systems. Marine and terrestrial aquatic systems, especially the transported suspended solids, have often been the focus of scientific investigations in the past. Sediments of aquatic river systems, on the other hand, were often ignored due to the time‐consuming sample preparation and analysis procedures. Spectroscopic measurement methods counting particle numbers are hardly suitable as detection methods, because there are plenty of natural particles next to a small number of MP particles. Integral methods, such as thermoanalytical methods are determining the particle mass independently of the inorganic components.In this study, a workflow for sample preparation via density separation and subsequent analysis by thermal extraction desorption‐gas chromatography/mass spectrometry is presented, which leads to representative and homogeneous samples and allows fast and robust MP mass content measurements suitable for routine analysis. Polymers were identified and quantified in all samples. Polyethylene and styrene‐butadiene rubber are the dominant polymers, besides polypropylene and polystyrene. Overall, total polymer masses between 1.18 and 337.0 µg/g could be determined. Highest MP concentrations in riverbed sediment are found in sites characterized by low flow velocities in harbors and reservoirs, while MP concentrations in sandy/gravelly bed sediments with higher flow velocities are small. KW - Microplastics KW - Density separation KW - TED-GC/MS KW - NaI PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597335 DO - https://doi.org/10.1002/appl.202200125 VL - 3 IS - 2 SP - 1 EP - 10 PB - Wiley VHC-Verlag AN - OPUS4-59733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Visileanu, Emilia A1 - Catalin Grosu, Marian A1 - Tiberiu Miclea, Paul A1 - Altmann, Korinna A1 - Brossell, Dirk T1 - Methods for the collection and characterization of airborne particles in the textile industry N2 - Airborne particulate matter is one of the main air pollutants. Their impact on mortality, and the occurrence of pulmonary and cardiovascular complications, have been the subject of numerous studies. Airborne particles are complex mixtures of organic and inorganic substances from different sources of particle emissions. Particulate Matter (PM) particles are classified according to their aerodynamic diameter expressed in µm and can vary from coarse (PM 10) to fine (less than PM 2.5). These diameter considerations are fundamental because they condition the penetration of particles into the bronchopulmonary system and the body. In recent years, there has been an interest in so-called “ultra-fine” particles, with a diameter of 0.1 µm (or 100 nm), or PM 0.1. They are nanoparticles and their impact on human health is not yet clear.With more than 1.5 million employees, textiles and clothing is a diverse sector that plays an important role in the European manufacturing industry, producing a turnover of €162 billion.An important component of the solid particles that generate air pollution in the textile industry is microplastics (MP) and nano plastics (NP), which also include microfibers (<5mm) and nanofibers (<100 nm), respectively. The particles released into the air during fiber and yarn processing range from 1 µg/m3 to 50 µg/m3.The paper presents the results of the determination of indoor and outdoor air concentration levels in textile companies, to identify the areas with the highest concentration level, by using an online recording system such as the Laser Aerosol Spectrometer MINI LAS model 11-E. The total concentration level TSP (µg/m3), the fractions PM 10(µg/m3), PM 2.5(µg/m3), PM1(µg/m3), as well as the total number of particles TC (1/l), were shown. It was noted that TSP is approximately at the same level both indoors and outdoors, but the fractions of PM10, PM2.5, and PM1 have much higher values indoors than outdoors with possible consequences on workers' health.The next step was the collection of fibers, namely micro and nano plastic particles from the vicinity of the workplaces of polyester, polyamide, and polypropylene fibers processing units in the textile industry in Romania, to obtain a sufficient quantity for laboratory analysis to determine the size and shape of the particles as well as their chemical composition. Two types of pumps were used, differentiated by their operating parameters: TECORA SKYPOST with airflow of 38 l/min and GILAIRPLUS with airflow 2l/min. Filters made of different materials with different diameters and pore sizes were used, namely: quartz filters (ø 47 mm, and ø 37 mm) on a TECORA SKYPOST type pump, polycarbonate nucleopore coated with a gold membrane (ø 25 mm) and silica filter (ø 9 mm) on GILAIRPLUS type pump.Using descriptive statistics, the calculation of correlation coefficients highlighted a strong correlation between the variables: "Collected mass/ Air concentration" and "Collected mass/ Air volume" for all diameters of the filters.The highest collected particle volume, determined by weighing the filters before and after collection, was obtained with the quartz filters (ø 47 mm) at an airflow of 38 l/min. The particles collected (polyester, polyamide, polypropylene) in the first stage were analyzed by SEM and thermogravimetric and it was found that the quartz filters absorbed the particles inside, with very few remaining on the surface. Thus no known methods can be used to perform analysis for particles collected on quartz filters. The number of particles on the filters was insufficient for analysis either because of the collection parameters used or because of the loss of particles during transport. As a result, in the next step, the use of 9 mm Si filters using the GILAIRPLUS pump at an airflow rate of 2l/min was chosen.To improve the transport conditions and avoid the loss of the particles and keep them on the surface of the filters, two methods were applied:- after weighing the filters were reintroduced into the collection pump holder;- a filtration system for airborne micro-nano plastics was designed and manufactured to selectively collect and transport PM10 and PM1 particles collected on SI filters.In both cases, SEM, Raman mapping, and GS-MS microscopy were used for analysis.Several times more PM10 than PM1 (74.5µg compared to 12.5 µg) was found. In all cases, both particles and fibers showed the same Raman fingerprint.The GS-MS analyses showed some contamination of the workspaces with particles other than the processed fibers. The presence of non-notifiable substances was also observed.The most viable filters are Si filters with a pore size of 10 microns to 1 micron and the use of the selected collection and transport filter system. In the following a filter system will be applied for collection on Au membrane-coated polycarbonate filters. T2 - 5th International Conference on Human Systems Engineering and Design: Future Trends and Applications (IHSED 2023) KW - Microplastics KW - Textiles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624442 DO - https://doi.org/10.54941/ahfe1004132 VL - 112 SP - 212 EP - 223 PB - AHFE International AN - OPUS4-62444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Tina A1 - Breese, Philipp Peter A1 - Metz, Christian A1 - Altenburg, Simon T1 - In-situ monitoring for PBF-LB/M processes: Does multispectral optical tomography add value in recognizing process deviations? N2 - Laser powder bed fusion of metallic components (PBF-LB/M) is gaining acceptance in industry. However, the high costs and lengthy qualification processes required for printed components create the need for more effective in-situ monitoring and testing methods. This article proposes multispectral Optical Tomography (OT) as a new approach for monitoring the PBF-LB/M process. Compared to other methods, OT is a low-cost process monitoring method that uses long-time exposure imaging to observe the build process. However, it lacks time resolution compared to expensive thermographic sensor systems. Monochromatic OT (1C-OT) is already commercially available and observes the building process layer-wise using a single wavelength window in the NIR range. Multispectral OT (nC-OT) utilizes a similar setup but can measure multiple wavelength ranges per location simultaneously. By comparing the classical 1C-OT and nC-OT approaches, this article examines the advantages of nC-OT (two channel OT and RGB-OT) in reducing the false positive rate for process deviations and approximating maximum temperatures for a better comparison between different build processes and materials. This could ultimately reduce costs and time for part qualification. The main goal of this contribution is to assess the advantages of nC-OT compared to 1C-OT for in-situ process monitoring of PBF-LB/M. T2 - Nolamp 2023 CY - Turku, Finland DA - 22.08.2023 KW - Thermography KW - Process Monitoring KW - Additive manufacturing KW - BPF-LB/M KW - In-situ PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-592498 DO - https://doi.org/10.1088/1757-899X/1296/1/012008 VL - 1296 SP - 1 EP - 11 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-59249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breese, Philipp Peter A1 - Becker, Tina A1 - Oster, Simon A1 - Metz, C. A1 - Altenburg, Simon T1 - In-situ defect detection via active laser thermographic testing for PBF-LB/M N2 - Great complexity characterizes Additive Manufacturing (AM) of metallic components via laser powder bed fusion (PBF-LB/M). Due to this, defects in the printed components (like cracks and pores) are still common. Monitoring methods are commercially used, but the relationship between process data and defect formation is not well understood yet. Furthermore, defects and deformations might develop with a temporal delay to the laser energy input. The component’s actual quality is consequently only determinable after the finished process. To overcome this drawback, thermographic in-situ testing is introduced. The defocused process laser is utilized for nondestructive testing performed layer by layer throughout the build process. The results of the defect detection via infrared cameras are shown for a research PBF-LB/M machine. This creates the basis for a shift from in-situ monitoring towards in-situ testing during the AM process. Defects are detected immediately inside the process chamber, and the actual component quality is determined. T2 - Lasers in Manufacturing (LiM) CY - Munich, Germany DA - 26.06.2023 KW - Additive manufacturing KW - Laser powder bed fusion KW - Nondestructive testing KW - Laser thermography KW - Defect detection PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-585060 SP - 1 EP - 10 PB - Wissenschaftliche Gesellschaft Lasertechnik und Photonik (WLT) CY - Hannover AN - OPUS4-58506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breese, Philipp Peter A1 - Becker, Tina A1 - Oster, Simon A1 - Metz, C. A1 - Altenburg, Simon T1 - In-situ defect detection for laser powder bed fusion with active laser thermography N2 - Defects are still common in metal components built with Additive Manufacturing (AM). Process monitoring methods for laser powder bed fusion (PBF-LB/M) are used in industry, but relationships between monitoring data and defect formation are not fully understood yet. Additionally, defects and deformations may develop with a time delay to the laser energy input. Thus, currently, the component quality is only determinable after the finished process. Here, active laser thermography, a nondestructive testing method, is adapted to PBF-LB/M, using the defocused process laser as heat source. The testing can be performed layer by layer throughout the manufacturing process. We study our proposed testing method along experiments carried out on a custom research PBF-LB/M machine using infrared (IR) cameras. Our work enables a shift from post-process testing of components towards in-situ testing during the AM process. The actual component quality is evaluated in the process chamber and defects can be detected between layers. T2 - 2023 International Solid Freeform Fabrication Symposium CY - Austin, TX, USA DA - 14.08.2023 KW - Additive Manufacturing KW - Laser Powder Bed Fusion KW - Nondestructive Testing KW - Thermography KW - Defect Detection PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606288 DO - https://doi.org/10.26153/tsw/51096 SP - 1978 EP - 1989 PB - University of Texas at Austin CY - Austin, TX, USA AN - OPUS4-60628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oster, Simon A1 - Breese, Philipp Peter A1 - Ulbricht, Alexander A1 - Mohr, Gunther A1 - Altenburg, Simon T1 - A deep learning framework for defect prediction based on thermographic in-situmonitoring in laser powder bed fusion N2 - The prediction of porosity is a crucial task for metal based additive manufacturing techniques such as laser powder bed fusion. Short wave infrared thermography as an in-situ monitoring tool enables the measurement of the surface radiosity during the laser exposure. Based on the thermogram data, the thermal history of the component can be reconstructed which is closely related to the resulting mechanical properties and to the formation of porosity in the part. In this study, we present a novel framework for the local prediction of porosity based on extracted features from thermogram data. The framework consists of a data pre-processing workflow and a supervised deep learning classifier architecture. The data pre-processing workflow generates samples from thermogram feature data by including feature information from multiple subsequent layers. Thereby, the prediction of the occurrence of complex process phenomena such as keyhole pores is enabled. A custom convolutional neural network model is used for classification. Themodel is trained and tested on a dataset from thermographic in-situ monitoring of the manufacturing of an AISI 316L stainless steel test component. The impact of the pre-processing parameters and the local void distribution on the classification performance is studied in detail. The presented model achieves an accuracy of 0.96 and an f1-Score of 0.86 for predicting keyhole porosity in small sub-volumes with a dimension of (700 × 700 × 50) μm3. Furthermore, we show that pre-processing parameters such as the porosity threshold for sample labeling and the number of included subsequent layers are influential for the model performance. Moreover, the model prediction is shown to be sensitive to local porosity changes although it is trained on binary labeled data that disregards the actual sample porosity. KW - Laser Powder Bed Fusion (PBF-LB/M, L-PBF) KW - Selective Laser Melting (SLM) KW - SWIR thermography KW - Online monitoring KW - Flaw detection KW - Machine learning KW - Convolutional neural networks (CNN) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575148 DO - https://doi.org/10.1007/s10845-023-02117-0 SN - 0956-5515 SP - 1 EP - 20 PB - Springer AN - OPUS4-57514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohr, Gunther A1 - Altenburg, Simon A1 - Hilgenberg, Kai T1 - On the limitations of small cubes as test coupons for process parameter optimization in laser powder bed fusion of metals N2 - The capability to produce complexly and individually shaped metallic parts is one of the main advantages of the laser powder bed fusion (PBF LB/M) process. Development of material and machine specific process parameters is commonly based on results acquired from small cubic test coupons of about 10 mm edge length. Such cubes are usually used to conduct an optimization of process parameters to produce dense material. The parameters are then taken as the basis for the manufacturing of real part geometries. However, complex geometries go along with complex thermal histories during the manufacturing process, which can significantly differ from thermal conditions prevalent during the production of simply shaped test coupons. This may lead to unexpected and unpredicted local inhomogeneities of the microstructure and defect distribution in the final part and it is a root cause of reservations against the use of additive manufacturing for the production of safety relevant parts. In this study, the influence of changing thermal conditions on the resulting melt pool depth of 316L stainless steel specimens is demonstrated. A variation of thermo-graphically measured intrinsic preheating temperatures was triggered by an alteration of inter layer times and a variation of cross section areas of specimens for three distinct sets of process parameters. Correlations between the preheating temperature, the melt pool depth, and occurring defects were analyzed. The limited expressiveness of the results of small density cubes is revealed throughout the systematic investigation. Finally, a clear recommendation to consider thermal conditions in future process parameter optimizations is given. T2 - Icaleo 2023 CY - Chicago, IL, USA DA - 16.10.2023 KW - Additive manufacturing KW - Heat accumulation KW - Thermal history KW - In situ monitoring KW - Representative specimens KW - Thermography PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586558 DO - https://doi.org/10.2351/7.0001080 SN - 1042-346X VL - 35 IS - 4 SP - 1 EP - 10 AN - OPUS4-58655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hurtado-Hurtado, G. A1 - Morales-Velazquez, L. A1 - Otremba, Frank A1 - Jáuregui-Correa, J. C. T1 - Railcar Dynamic Response during Braking Maneuvers Based on Frequency Analysis N2 - The dynamic response of a vehicle during braking is influenced by the tangential forces developed at the wheel-rail’s contact surface. The friction coefficient affects the load transfer from the wheel’s tread to the vehicle. In this work, the vibrations of a scale-down railway vehicle are monitored during braking and their relationship with the friction coefficient between wheel and rail is found out. The vehicle is instrumented with encoders, accelerometers, and is controlled via Bluetooth. The tests are carried out with clean and friction-modified rails. The tangential forces transmitted from the wheel to the railcar’s body are visualized in time and frequency using a proposed correlation algorithm based on the outputs of the ContinuousWavelet Transform (CWT). The results demonstrate that tangential forces have a significant impact on railway vehicles under conditions of high friction coefficients and large creep values. KW - Railway vibration measurements KW - Vibration signal analysis KW - Wheel-rail tangential forces KW - Railway braking forces KW - Wheel-rail friction coefficient PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572309 DO - https://doi.org/10.3390/app13074132 VL - 13 IS - 7 SP - 1 EP - 15 PB - MDPI AN - OPUS4-57230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprachmann, J. A1 - Grabicki, N. A1 - Möckel, Anna A1 - Maltitz, J. A1 - del Refugio Monroy Gómez, J. A1 - Smales, Glen Jacob A1 - Dumele, O. T1 - Substituted Benzophenone Imines for COF Synthesis via Formal Transimination N2 - Covalent organic frameworks (COFs) are a prominent class of organic materials constructed from versatile building blocks via reversible reactions. The quality of imine-linked COFs can be improved by using amine monomers protected with benzophenone forming benzophenone imines. Here, we present a study on substituted benzophenones in COF synthesis via formal transimination. 12 para-substituted N-aryl benzophenone imines, with a range of electron-rich to electron-poor substituents, were prepared and their hydrolysis kinetics were studied spectroscopically. All substituted benzophenone imines can be employed in COF synthesis and lead to COFs with high crystallinity and high porosity. The substituents act innocent to COF formation as the substituted benzophenones are cleaved off. Imines can be tailored to their synthetic demands and utilized in COF formation. This concept can make access to previously unattainable, synthetically complex COF monomers feasible. KW - Materials Chemistry KW - Metals and Alloys KW - Surfaces, Coatings and Films KW - General Chemistry KW - Ceramics and Composites KW - Electronic, Optical and Magnetic Materials KW - Catalysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586449 DO - https://doi.org/10.1039/D3CC03735E SN - 1359-7345 SP - 1 EP - 4 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dal Molin, E. S. A1 - Henning, L. M. A1 - Müller, J. T. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Bekheet, M. F. A1 - Gurlo, A. A1 - Simon, U. T1 - Robocasting of ordered mesoporous silica‐based monoliths: Rheological, textural, and mechanical characterization N2 - Hierarchically porous, high‐surface‐area silica materials are excellent candidates for multiple applications like catalysis and environmental remediation. Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on‐demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK‐12 slurries were robocasted into monoliths, containing different ratios of uncalcined COK‐12 and sodium bentonite (0–25 wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69 vs. 0.32) and higher yield stresses (96 vs. 259 Pa) compared to pure COK‐12 ones. Monoliths were printed in woodpile structures and calcined at 600°C. Micro‐CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20 ± 0.07 to 1.0 ± 0.3 MPa) with increasing binder/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK‐12 was retained. The structures exhibited open porosities of 52 ± 4% and showed higher specific mesopore volumes, and increased average mesopore size (6 vs. 8 nm) compared to COK‐12. Small‐angle x‐ray scattering analysis revealed an increased lattice parameter (10.3 vs. 11.0 nm) and reduced wall thickness (3.1 nm vs. 4.1 nm) of the COK‐12 in the monoliths. These properties indicate suitability for their application as porous supports and adsorbents. KW - Industrial and Manufacturing Engineering KW - Additive manufacturing KW - OMS KW - Porous materials KW - Robocasting KW - X-ray scattering KW - MOUSE PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582503 DO - https://doi.org/10.1002/nano.202300109 VL - 4 IS - 11-12 SP - 615 EP - 631 PB - Wiley-VCH GmbH AN - OPUS4-58250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hallier, Dorothea C. A1 - Smales, Glen Jacob A1 - Seitz, H. A1 - Hahn, Marc Benjamin T1 - Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine N2 - Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. KW - BioSAXS KW - Bio-SAXS KW - Cosolute KW - Ectoine KW - G5P KW - GVP KW - Radiation damage KW - Radical Scavenger KW - Single-stranded DNA-binding proteins KW - X-ray scattering KW - DNA KW - ssDNA KW - Protein KW - SAXS KW - Small-angle xray scattering KW - McSAS3 KW - Dosimetry KW - Microdosimetry KW - Geant4 KW - Geant4-DNA KW - Topas KW - Topas-MC KW - Monte-Carlo simulations KW - Particle scattering simulations KW - Topas-nBio KW - OH Radical KW - OH radical scavenger KW - LEE KW - Ionizing radiation damage KW - Protein unfolding KW - Ectoin PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568909 DO - https://doi.org/10.1039/d2cp05053f SN - 1463-9076 SN - 1463-9084 VL - 25 IS - 7 SP - 5372 EP - 5382 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-56890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hunter, R. D. A1 - Hayward, E. C. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Kulak, A. A1 - Guan, S. A1 - Schnepp, Z. T1 - The effect of nitrogen on the synthesis of porous carbons by iron-catalyzed graphitization N2 - This paper reports a systematic study into the effect of nitrogen on iron-catalyzed graphitization of biomass. Chitin, chitosan, N-acetylglucosamine, gelatin and glycine were selected to represent nitrogen-rich saccharides and amino-acid/polypeptide biomass precursors. The materials were pyrolyzed with an iron catalyst to produce carbons with a wide range of chemical and structural features such as mesoporosity and nitrogen-doping. Many authors have reported the synthesis of nitrogen-doped carbons by pyrolysis and these have diverse applications. However, this is the first systematic study of how nitrogen affects pyrolysis of biomass and importantly the catalytic graphitization step. Our data demonstrates that nitrogen inhibits graphitization but that some nitrogen survives the catalytic graphitization process to become incorporated into various chemical environments in the carbon product. KW - Graphitization KW - Nanoparticles KW - Nanocomposite KW - Porous carbon KW - Nitrogen KW - Scattering PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575351 DO - https://doi.org/10.1039/d3ma00039g VL - 4 SP - 2070 EP - 2077 PB - Royal Society of Chemistry AN - OPUS4-57535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Smales, Glen Jacob A1 - Colmenares, M. G. A1 - Bekheet, M. F. A1 - Simon, U. A1 - Gurlo, A. T1 - Synthesis and properties of COK-12 large-pore mesocellularsilica foam N2 - Large, ink-bottle-shaped pores in mesocellular foams (MCFs) are desired for various applications requiring enhanced mass transfer or the immobilization of larger compounds. Hence, the cylindrical pores of COK-12, an ordered mesoporous silica structurally comparable to SBA-15 but synthesized at room-temperature at quasi-neutral pH, are chemically swollen into ink-bottle pores. Therefore, p-xylene is used as a more sustainable swelling agent compared to popular alternatives. Its high boiling point allows for an additional thermal aging step to amplify the mesostructure enlargement without needing additional chemicals. For COK-12, the MCFs obtained at room temperature reach an unprecedented plateau for the modal mesopore cell and window diameter of 19.9 and 5.5 nm, respectively, with an underlying broad pore size distribution and distorted hexagonal lattice up to 14.5 nm, involving hexagonal and spherical structures. The combined chemical and thermal swelling resulted in the selective enlargement of the window diameter to more than 200% and a slightly increased cell diameter, pore size distribution, and hexagonal lattice distortion in comparison to the room temperature synthesis. Such materials are thought to be promising alternatives to SBA-15-based MCFs, often utilizing toxic catalysts during synthesis. The presented results pave the way for enhanced adsorptive, catalytic, and drug delivery performances for COK-12-based materials. KW - SAXS KW - MOUSE KW - Mesocellular foam KW - Mesoporous silica PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569590 DO - https://doi.org/10.1002/nano.202200223 SP - 1 EP - 11 AN - OPUS4-56959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzolin, R. H. A1 - Richter, Tim A1 - Pixner, F. A1 - Rhode, Michael A1 - Schröpfer, Dirk A1 - Enzinger, N. T1 - Microstructure characterisation of multi-principal element alloys welds produced by electron beam welding N2 - This work explores the feasibility of producing bead-on-plate welds of a CrCoNi medium entropy alloy and a CrMnFeCoNi high entropy alloy using electron beam welding. The alloys were welded in two states: one in an as-cold-rolled condition and the other in an annealed condition. In addition, the materials are welded with two different parameters. The FCC microstructure of the welds is investigated using scanning electron microscopy assisted by energy-dispersive X-ray spectroscopy and electron-backscattered diffraction. The impact of the weld on the microstructure is discussed. The heat-affected zone is negligible for the annealed condition of both medium and high entropy alloys since there is no driving force for recrystallisation and the exposure time to high temperature is insufficient for grain coarsening. The texture formed in the fusion zone is also discussed and compared to the texture in the base metal and the heat-affected zone. Although the grain growth along the (100) crystallographic direction is preferential in all cases, the crystallographic texture type differs from each weld. Higher hardness values are measured in the medium entropy alloy’s base metal and fusion zone than in the high entropy alloy. KW - Multi-principal element alloy KW - Electron backscattered diffraction KW - Electron beam welding KW - High-entropy alloy KW - Microstructure characterization PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568129 DO - https://doi.org/10.1016/j.matdes.2023.111609 SN - 1873-4197 VL - 225 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aliyah, K. A1 - Prehal, C. A1 - Diercks, J. S. A1 - Diklić, N. A1 - Xu, L. A1 - Ünsal, S. A1 - Appel, C. A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Guizar-Sicairos, M. A1 - Herranz, J. A1 - Gubler, L. A1 - Büchi, F. N. A1 - Eller, J. T1 - Quantification of PEFC Catalyst Layer Saturation via In Silico, Ex Situ, and In Situ Small-Angle X-ray Scattering N2 - The complex nature of liquid water saturation of polymer electrolyte fuel cell (PEFC) catalyst layers (CLs) greatly affects the device performance. To investigate this problem, we present a method to quantify the presence of liquid water in a PEFC CL using small-angle X-ray scattering (SAXS). This method leverages the differences in electron densities between the solid catalyst matrix and the liquid water filled pores of the CL under both dry and wet conditions. This approach is validated using ex situ wetting experiments, which aid the study of the transient saturation of a CL in a flow cell configuration in situ. The azimuthally integrated scattering data are fitted using 3D morphology models of the CL under dry conditions. Different wetting scenarios are realized in silico, and the corresponding SAXS data are numerically simulated by a direct 3D Fourier transformation. The simulated SAXS profiles of the different wetting scenarios are used to interpret the measured SAXS data which allows the derivation of the most probable wetting mechanism within a flow cell electrode. KW - Polymer electrolyte fuel cell KW - Water management KW - Catalyst layer KW - Representative morphology modeling KW - Small-angle X-ray scattering KW - MOUSE KW - SAXS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575973 DO - https://doi.org/10.1021/acsami.3c00420 SN - 1944-8244 VL - 15 IS - 22 SP - 26538 EP - 26553 PB - ACS Publications AN - OPUS4-57597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Diana A1 - Hahn, Oliver ED - Lois, C. T1 - Colours on East Asian Maps N2 - Maps and colours have a close connection. Drawn or printed in black on white, subsequently added colours enhance maps with additional information. Colours were not just there to improve maps aesthetically, but they regulated how they were read and thus reinforced their meanings, significances and ideas. Colour is an important key to a more precise understanding of the map’s purposes and uses; moreover, colours are also an important aspect of a map’s materiality. The material scientific analysis makes it possible to find out more about the making of colours and the process of colouring maps. By skillfully deploying colours, map colourists were able to create mimetic representations of nature or codify information in an abstract form. The use of colours involved many considerations as to the materials. ‘Reading’ colours in this way gives a glimpse into the social lives of mapmakers as well as map users and reveals the complexity of the historical and social context in which maps were produced and how the maps were actually made. Within the scope of the three-year joint research project Coloured Maps (2018–2021), we undertook an in-depth and systematic study of hand-drawn and hand-coloured maps from East Asia in the Museum am Rothenbaum (MARKK) in Hamburg and produced between the seventeenth and twentieth centuries. With a multi-perspective approach and transdisciplinary methods (humanities and the sciences), we were able to pool and compare the research results from different fields of research on Asian maps. The aim of this publication is to provide a first general overview of the subject of colours on maps in East Asia in the period from the seventeenth to the early twentieth century and to stimulate further research on the topic. KW - Maps and colours KW - Colouring KW - Colourants KW - Dyes and pigments KW - Map production and publishing KW - Non-invasive scientific methods PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569682 UR - https://brill.com/display/title/61839 SN - 978-90-04-54562-5 VL - 2023 SP - 1 EP - 79 PB - Brill CY - Leiden, Netherlands AN - OPUS4-56968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deubener, J. A1 - Behrens, H. A1 - Müller, Ralf T1 - An overview on the effect of dissolved water on the viscosity of soda lime silicate melts N2 - In this review article, the impact of dissolved water on the viscous properties of soda lime silicate melts is addressed against the background of the upcoming switch from natural gas to hydrogen combustion. This change will lead to an increase in the total water content of the glasses by up to 0.4 mol%. In order to better define possible influences of water speciation, water-rich glasses were synthesised under increasing pressure up to the kbar range. It is shown that a distinction must be made between the influence of dissolved OH-groups and H2Omolecules in order to accurately reflect the dependence of isokom temperatures on water content. In addition, an increase of one order of magnitude in the tolerance to higher deformation rates was observed for the range of expected increased water contents during isothermal deformation processes, which is based on the timetemperature superposition principle, i.e. congruent flow curves were determined under isokomal conditions. KW - Water in glass KW - Viscosity KW - Soda lime silicate glass KW - Shear thinning KW - Nydrogen melting PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587276 DO - https://doi.org/10.1016/j.nocx.2023.100195 VL - 19 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-58727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gomes Fernandes, Roger A1 - Al-Mukadam, Raschid A1 - Bornhöft, Hansjörg A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Selle, Susanne A1 - Deubener, Joachim T1 - Viscous Sintering of Acid Leached Glass Powders N2 - The process of viscous flow sintering is a phenomenon that is closely linked to the surface properties of the glass particles. In this work, we studied the extreme case of acid-leaching of soda-lime-silicate glass beads of two different particle size distributions and its effects on non-isothermal viscous sintering of powder compacts. Depth profiling of the chemical composition after leaching revealed a near-surface layer depleted in alkali and alkaline earth ions, associated with concurrent hydration as mass loss was detected by thermogravimetry. Heating microscopy showed that acid treatment of glasses shifted the sinter curves to higher temperatures with increasing leaching time. Modelling of the shrinkage with the cluster model predicted a higher viscosity of the altered surface layer, while analysis of the time scales of mass transport of mobile species (Na+, Ca2+ and H2O) during isochronous sintering revealed that diffusion of Na+ can compensate for concentration gradients before sintering begins. Also, exchanged water species can diffuse out of the altered layer, but the depletion of Ca2+ in the altered surface layer persists during the sinter interval, resulting in a glass with higher viscosity, which causes sintering to slow down. KW - Glass powder KW - Viscous sintering KW - Acid-leaching KW - Sinter retardation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589008 DO - https://doi.org/10.52825/glass-europe.v1i.681 VL - 1 SP - 37 EP - 53 AN - OPUS4-58900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Viscous healing of Vickers indentation–induced cracks in glass N2 - AbstractViscous healing of cracks induced by the Vickers indentation in a soda lime magnesium silicate, a soda borosilicate, and a soda aluminosilicate glass (NAS) was studied by laser scanning microscopy. Plots of the crack length, width, and depth normalized to the initial crack length versus time over viscosity merge into single master curves of each of these quantities for each glass. Despite glass properties do not differ strikingly from each other, however, these master curves strongly differ among the glasses. This finding was attributed to a different interplay of various crack healing phenomena. Lateral cracks were found to be responsible for the bulging of the sample surface around the Vickers imprint, which in turn promotes radial crack widening as the main cause of healing delay. The most rapid healing of lateral cracks was observed in NAS in which bulging and crack widening were least pronounced. KW - Crack healing KW - Glass KW - Vickers indentation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587295 DO - https://doi.org/10.1111/jace.19245 SN - 0002-7820 VL - 106 IS - 10 SP - 5795 EP - 5805 PB - Wiley AN - OPUS4-58729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinsch, Stefan A1 - Welter, T. A1 - Müller, Ralf A1 - Deubener, J. T1 - Hydrogen Permeability of Tectosilicate Glasses for Tank Barrier Liners N2 - The permeation of hydrogen gas was studied in meta-aluminous (tectosilicate) glass powders of Li2O×Al2O3×SiO2 (LAS), Na2O×Al2O3×SiO2 (NAS) and MgO×Al2O3×SiO2 (MAS) systems by pressure loading and vacuum extraction in the temperatures range 210–310 °C. With this method, both the solubility S and the diffusivity D were determined, while the permeability was given by the product SD. For all glasses, S was found to decrease with temperature, while D increased. Since the activation energy of diffusion of H2 molecules exceeded that of dissolution, permeation increased slightly with temperature. When extrapolated to standard conditions (25 °C), the permeability of tectosilicate glasses was found to be only 10-22–10-24 mol H2 (m s Pa)-1, which is 8–10 magnitudes lower than most polymers. Thin glass liners of these compositions are expected to be the most effective barrier for tanks of pressurised hydrogen. KW - Hydrogen permeation KW - Aluminosilicate glasses KW - Hydrogen storage tank KW - Glass liner PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587284 DO - https://doi.org/10.52825/glass-europe.v1i.425 VL - 1 SP - 1 EP - 11 AN - OPUS4-58728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheffler, Franziska A1 - Fleck, Mirjam A1 - Busch, Richard A1 - Casado, Santiago A1 - Gnecco, Enrico A1 - Tielemann, Christopher A1 - Brauer, Delia S. A1 - Müller, Ralf T1 - Surface Crystallization of Barium Fresnoite Glass: Annealing Atmosphere, Crystal Morphology and Orientation N2 - Controlled oriented crystallization of glass surfaces is desired for high precision applications, since the uppermost crystal layer significantly influences the properties of the material. In contrast to previous studies, the data presented here deal with separated crystals growing at defect-free surfaces in four atmospheres with different degrees of humidity (ambient/dry air, argon and vacuum). A glass with the composition 2 BaO–TiO2–2.75 SiO2 was heat-treated at 825 °C until fresnoite (Ba2TiSi2O8) grew to a significant size. The crystal growth rate is found to increase with increasing humidity. The morphology of the crystals changes from highly distorted dendrites in the driest atmosphere (vacuum) to circular/spear-head-shaped crystals in the wettest atmosphere (ambient air), which we attribute to a decrease in viscosity of the glass surface due to water uptake. The least distorted crystals appear in the form of depressions of up to 6 µm. This has an influence on the observed crystal orientation, as measured by electron backscatter diffraction (EBSD). The pulled-in crystals change the orientation during growth relative to the flat glass surface due to an enrichment in SiO2 at the crystal fronts. This confirms that the orientation of crystals is not fixed following nucleation. KW - Fresnoite KW - Surface crystallization KW - Crystal growth KW - Crystal morphology KW - Crystal orientation KW - EBSD PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587230 DO - https://doi.org/10.3390/cryst13030475 VL - 13 IS - 3 SP - 1 EP - 17 PB - MDPI AG CY - Basel AN - OPUS4-58723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seher, Julia A1 - Rübner, Katrin A1 - Müller, Constanze A1 - Pniok, N. A1 - Dreisow, B. T1 - Leichte Gesteinskörnungen hergestellt aus Bau- und Abbruchabfällen – Applikation in der Denkmalpflege N2 - Im Rahmen des BMBF-geförderten Forschungsprojekts ReMin – REALight werden in einem Projektteam aus Industriepartnern und Forschungseinrichtungen unter Koordination der Bauhaus-Universität Weimar leichte Gesteinskörnungen aus Bau- und Abbruchabfällen und industriellen Nebenprodukten auf thermischem Weg hergestellt. Die Aufgabe der Bundesanstalt für Materialforschung und -prüfung (BAM) ist es, diese im Drehrohrofen erzeugten Blähgranulate für gebundene Anwendungen in Beton und Mörtel umfassend zu charakterisieren. Gemeinsam mit der Opus Denkmalpflege GmbH wird die Applikation feiner, gebrochener Blähgranulate in leichten Steinergänzungsmörteln für die Restaurierung von Sandsteinobjekten untersucht. Hierzu wird ein zweischichtiges Mörtelsystem bestehend aus einem Füll- und einem Deckmörtel entwickelt. Erste Ergebnisse der Rezepturentwicklung verschiedener kalkhaltiger Leichtmörtel mit gebrochenen Blähgranulaten werden vorgestellt. Die neuen Leichtmörtel sind hinsichtlich der entwickelten Druckfestigkeit gleichwertig gegenüber herkömmlichen Restauriermörteln. T2 - 21. Internationale Baustofftagung (ibausil) CY - Weimar, Germany DA - 13.09.2023 KW - Baustoffrecycling KW - Mauerwerkbruch KW - Leichte Gesteinskörnungen KW - Denkmalpflege KW - Restauriermörtel KW - Steinergänzungsmassen PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590685 DO - https://doi.org/10.1002/cepa.2839 SN - 2509-7075 VL - 6 SP - 861 EP - 866 PB - Ernst & Sohn GmbH AN - OPUS4-59068 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Labrador-Paez, Lucia, L. A1 - Kankare, J. A1 - Hyppanen, I. A1 - Soukka, T. A1 - Andresen, Elina A1 - Resch-Genger, Ute A1 - Widengren, J A1 - Liu, H. T1 - Frequency-Domain Method for Characterization of Upconversion Luminescence Kinetics N2 - The frequency-domain (FD) method provides an alternative to the commonly used time-domain (TD) approach in characterizing the luminescence kinetics of luminophores, with its own strengths, e.g., the capability to decouple multiple lifetime components with higher reliability and accuracy. While extensively explored for characterizing luminophores with down-shifted emission, this method has not been investigated for studying nonlinear luminescent materials such as lanthanide-doped upconversion nanoparticles (UCNPs), featuring more complicated kinetics. In this work, employing a simplified rate-equation model representing a standard two-photon energy-transfer upconversion process, we thoroughly analyzed the response of the luminescence of UCNPs in the FD method. We found that the FD method can potentially obtain from a single experiment the effective decay rates of three critical energy states of the sensitizer/activator ions involved in the upconversion process. The validity of the FD method is demonstrated by experimental data, agreeing reasonably well with the results obtained by TD methods. KW - Quality assurance KW - Luminescence KW - Method KW - Quantitative spectroscopy KW - Nano KW - Particle KW - Lifetime KW - Method development PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597435 DO - https://doi.org/10.1021/acs.jpclett.3c00269 SP - 3436 EP - 3444 AN - OPUS4-59743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Koch, Matthias T1 - On-Site Detection of Volatile Organic Compounds (VOCs) N2 - Volatile organic compounds (VOCs) are of interest in many different fields. Among them are food and fragrance analysis, environmental and atmospheric research, industrial applications, security or medical and life science. In the past, the characterization of these compounds was mostly performed via sample collection and off-site analysis with gas chromatography coupled to mass spectrometry (GC-MS) as the gold standard. While powerful, this method also has several drawbacks such as being slow, expensive, and demanding on the user. For decades, intense research has been dedicated to find methods for fast VOC analysis on-site with time and spatial resolution. We present the working principles of the most important, utilized, and researched technologies for this purpose and highlight important publications from the last five years. In this overview, non-selective gas sensors, electronic noses, spectroscopic methods, miniaturized gas chromatography, ion mobility spectrometry and direct injection mass spectrometry are covered. The advantages and limitations of the different methods are compared. Finally, we give our outlook into the future progression of this field of research. KW - Volatile organic compounds KW - On-site detection KW - Mobile analytics KW - Sensors PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570885 DO - https://doi.org/10.3390/molecules28041598 VL - 28 IS - 4 SP - 1 EP - 19 PB - MDPI CY - Basel, Switzerland AN - OPUS4-57088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholtz, Lena A1 - Tavernaro, Isabella A1 - Eckert, J. G. A1 - Lutowski, Marc A1 - Geißler, Daniel A1 - Hertwig, Andreas A1 - Hidde, Gundula A1 - Bigall, N. C. A1 - Resch-Genger, Ute T1 - Influence of nanoparticle encapsulation and encoding on the surface chemistry of polymer carrier beads N2 - Surface-functionalized polymer beads encoded with molecular luminophores and nanocrystalline emitters such as semiconductor nanocrystals, often referred to as quantum dots (QDs), or magnetic nanoparticles are broadly used in the life sciences as reporters and carrier beads. Many of these applications require a profound knowledge of the chemical nature and total number of their surface functional groups (FGs), that control bead charge, colloidal stability, hydrophobicity, and the interaction with the environment and biological systems. For bioanalytical applications, also the number of groups accessible for the subsequent functionalization with, e.g., biomolecules or targeting ligands is relevant. In this study, we explore the influence of QD encoding on the amount of carboxylic acid (COOH) surface FGs of 2 μm polystyrene microparticles (PSMPs). This is done for frequently employed oleic acid and oleylamine stabilized, luminescent core/shell CdSe QDs and two commonly used encoding procedures. This included QD addition during bead formation by a thermally induced polymerization reaction and a post synthetic swelling procedure. The accessible number of COOH groups on the surface of QD-encoded and pristine beads was quantified by two colorimetric assays, utilizing differently sized reporters and electrostatic and covalent interactions. The results were compared to the total number of FGs obtained by a conductometric titration and Fourier transform infrared spectroscopy (FTIR). In addition, a comparison of the impact of QD and dye encoding on the bead surface chemistry was performed. Our results demonstrate the influence of QD encoding and the QD-encoding strategy on the number of surface FG that is ascribed to an interaction of the QDs with the carboxylic acid groups on the bead surface. These findings are of considerable relevance for applications of nanoparticle-encoded beads and safe-by-design concepts for nanomaterials. KW - Optical spectroscopy KW - Particle KW - Optical assay KW - IR spectroscopy KW - Fluorescence KW - Quantum yield KW - Quality assurance KW - Nano KW - Synthesis KW - Surface chemistry KW - Quantification KW - Method KW - Conductometry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581502 DO - https://doi.org/10.1038/s41598-023-38518-7 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 15 PB - Springer Nature CY - London AN - OPUS4-58150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohammad, W. A1 - Wegner, Karl David A1 - Comby-Zerbino, C. A1 - Trouillet, V. A1 - Ogayer, M. P. A1 - Coll, J.-L. A1 - Marin, R. A1 - Jaque Garcia, D. A1 - Resch-Genger, Ute A1 - Antoine, R. A1 - Le Guevel, X. T1 - Enhanced brightness of ultra-small gold nanoparticles in the second biological window through thiol ligand shell control N2 - Gold-based nanoparticles below 2 nm in size are promising as luminescent probes for in vivo bioimaging, owing to their brightness and rapid renal clearance. However, their use as contrast agents in the near-infrared II (NIR-II, 1000–1700 nm) range remains challenging due to their low photoluminescence (PL) quantum yield. To address this, PL enhancement can be achieved by either rigidifying the ligand-shell structure or increasing the size of the ligand shell. In this study, we synthesized ultra-small gold nanoparticles stabilized by co-ligands, namely monothiol and short dithiol molecules. By precisely controlling the amount of reducing agent used during particle preparation, we successfully modulated the physicochemical properties of the co-ligand shell, including its size, composition, and structure. Consequently, we achieved a remarkable 60-fold increase in the absorption cross-section at 990 nm while maintaining the small size of the 1.5-nm metal core. The analytical and optical characterization of our thiol-capped gold nanoparticles indicates that the ligand shell size is governed by the quantity of the reducing agent, which, in turn, impacts the balance between radiative and non-radiative processes, thereby influencing the PL quantum yield. KW - Gold nanocluster KW - NIR-II fluorescence KW - SWIR KW - Nanomaterial design KW - Calibrated fluorescence measurements PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588117 DO - https://doi.org/10.1039/D3TC03021K SN - 2050-7526 VL - 11 IS - 42 SP - 14714 EP - 14724 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Cui A1 - Ebel, Kenny A1 - Heinze, Katja A1 - Resch-Genger, Ute A1 - Bald, Ilko T1 - Quantum Yield of DNA Strand Breaks under Photoexcitation of a Molecular Ruby N2 - Photodynamic therapy (PDT) used for treating cancer relies on the generation of highly reactive oxygen species, for example, singlet oxygen 1O2, by light-induced excitation of a photosensitizer (PS) in the presence of molecular oxygen, inducing DNA damage in close proximity of the PS. Although many precious metal complexes have been explored as PS for PDT and received clinical approval, only recently, the potential of photoactive complexes of nonnoble metals as PS has been discovered. Using the DNA origami technology that can absolutely quantify DNA strand break cross sections, we assessed the potential of the luminescent transition metal complex [Cr(ddpd)2]3+ (ddpd=N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine) to damage DNA in an air-saturated aqueous environment upon UV/Vis illumination. The quantum yield for strand breakage, that is, the ratio of DNA strand breaks to the number of absorbed photons, was determined to 1–4%, indicating efficient transformation of photons into DNA strand breaks by [Cr(ddpd)2]3+. KW - Fluorescence KW - Synthesis KW - Production KW - Optical spectroscopy KW - Ligand KW - Photophysics KW - Cr(III) KW - Mechanism KW - NIR KW - PDT KW - Singlet oxygen KW - DNA KW - Origami KW - Quantum yield PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573631 DO - https://doi.org/10.1002/chem.202203719 SP - 1 EP - 7 AN - OPUS4-57363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuner, Maximilian A1 - Lisec, Jan A1 - Picher, Marie-Idrissa A1 - Rigo, Massimo A1 - Konetzki, Jörg A1 - Haase, Hajo A1 - Koch, Matthias T1 - Development and Application of Isotope Labelled Internal Standards in a Sum Parameter Method for Ergot Alkaloid Screening of Food N2 - Ergot alkaloids are a group of toxic compounds, formed by fungi on infested grasses. In 2022, the European Commission set into effect maximum levels for the sum of the twelve major ergot alkaloids in multiple foods. To facilitate the laborious and costly individual quantification of the twelve major ergot alkaloids by HPLC–MS/MS or -FLD, we recently reported a sum parameter method (SPM) for ergot alkaloid quantification. Here, derivatization to lysergic acid hydrazide—a derivative of the mutual ergoline backbone in all ergot alkaloids—allowed simplified determination of all ergot alkaloids in flour via HPLC-FLD. For the measurement of more complex matrices like processed foods, we now developed a MS/MS-based SPM. Two internal standards (IS), isotopically labelled at different positions of the molecule, were synthesized and employed in the MS/MS-measurements. Method performance using either the 13CD3-labelled or the 15N2-labelled IS was evaluated on naturally contaminated rye and wheat flour samples as well as on processed food matrices. Employing the 13CD3-labelled IS leads to lower variances and better consistency with the reference data (obtained by the FLD-based SPM) in flour samples compared to the 15N2-labelled IS. The novel method significantly improves the measurement of ergot alkaloids in complex food matrices, due to their increased selectivity and thus lower interferences. Furthermore, the application of isotope labelled IS obviates the need for time-consuming steps like the determination of recovery rate based, matrix specific correction factors as described in the MS/MS-based European standard method for ergot alkaloid quantification (EN 17425). KW - Mycotoxins KW - Sum Parameter Method KW - Isotope Labelling KW - HPLC-MS/MS KW - Analytical Chemistry KW - Lysergic acid hydrazide PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588582 DO - https://doi.org/10.1007/s12161-023-02553-x SN - 1936-976X VL - 17 IS - 1 SP - 119 EP - 128 PB - Springer CY - New York, NY AN - OPUS4-58858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Behnke, Thomas A1 - Gienger, J. A1 - Resch-Genger, Ute T1 - Efficiency scale for scatteringluminescent particles linkedto fundamental and measurablespectroscopic properties N2 - Comparing the performance of molecular and nanoscale luminophores and luminescent microand nanoparticles and estimating achievable signal amplitudes and limits of detection requires a standardizable intensity scale. This initiated the development of the relative MESF (number of molecules of equivalent soluble fluorochromes) and ERF (equivalent reference fluorophores) scales for flow cytometry and fluorescence microscopy. Both intensity scales rely on fluorescence intensity values assigned to fluorescent calibration beads by an intensity comparison to spectrally closely matching fluorophore solutions of known concentration using a spectrofluorometer. Alternatively, the luminophore or bead brightness (B) can be determined that equals the product of the absorption cross section (σa) at the excitation wavelength (σa(λex)) and the photoluminescence quantum yield (Φpl). Thereby, an absolute scale based on fundamental and measurable spectroscopic properties can be realized which is independent of particle size, material, and luminophore staining or labeling density and considers the sensitivity of the optical properties of luminophores to their environment. Aiming for establishing such a brightness scale for light-scattering dispersions of luminescent particles with sizes exceeding a few ten nanometers, we demonstrate how the brightness of quasi-monodisperse 25 nm, 100 nm, and 1 μm sized polystyrene particles (PSP), loaded with two different dyes in varying concentrations, can be obtained with a single custom-designed integrating sphere setup that enables the absolute determination of Φpl and transmittance and diffuse reflectance measurements. The resulting Φpl, σa(λex), imaginary parts of the refractive index, and calculated B values of these samples are given in dependence of the number of incorporated dye molecule per particle. Finally, a unitless luminescence efficiency (LE) is defined allowing for the direct comparison of luminescence efficiencies of particles with different sizes. KW - Brightness KW - Quantum yield KW - Cross section KW - Lluminescence PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573680 DO - https://doi.org/10.1038/s41598-023-32933-6 VL - 13 IS - 1 SP - 14 PB - Nature AN - OPUS4-57368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuner, Maximilian A1 - Lisec, Jan A1 - Mauch, Tatjana A1 - Konetzki, J. A1 - Haase, H. A1 - Koch, Matthias T1 - Quantification of Ergot Alkaloids via Lysergic Acid Hydrazide—Development and Comparison of a Sum Parameter Screening Method N2 - Ergot alkaloids are a group of mycotoxins occurring in products derived from various grasses (e.g., rye) and have been regulated in the EU recently. The new maximum levels refer to the sum of the six most common ergot alkaloids in their two stereoisomeric forms in different food matrices. Typically, these twelve compounds are individually quantified via HPLC-MS/MS or -FLD and subsequently summed up to evaluate food safety in a time-consuming process. Since all these structures share the same ergoline backbone, we developed a novel sum parameter method (SPM) targeting all ergot alkaloids simultaneously via lysergic acid hydrazide. After extraction and clean-up, in analogy to the current European standard method EN 17425 (ESM) for ergot alkaloid quantitation, the samples were derivatized by an optimized hydrazinolysis protocol, which allowed quantitative conversion after 20 min at 100 °C. The new SPM was evaluated against another established HPLC-FLD-based method (LFGB) and the HPLC-MS/MS-based ESM using six naturally contaminated rye and wheat matrix reference materials. While the SPM provided comparable values to the ESM, LFGB showed deviating results. Determined recovery rates, limits of detection and quantification of all three employed methods confirm that the new SPM is a promising alternative to the classical approaches for ergot alkaloid screening in food. KW - Ergot alkaloids KW - Sum Parameter KW - Mycotoxins KW - Derivatization KW - Hydrazinolysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573968 DO - https://doi.org/10.3390/molecules28093701 SN - 0015-2684 VL - 28 IS - 9 SP - 3701 PB - MDPI CY - Basel AN - OPUS4-57396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dopffel, N. A1 - An Stepec, Biwen Annie A1 - de Rezende, J. A1 - Machado de Sousa, D. A1 - Koerdt, Andrea T1 - Microbiology of Underground Hydrogen Storage N2 - Climate change is becoming one of the greatest challenges facing our society, particularly due to the continued use of fossil fuels. The steadily increasing demand for energy and the continuously growing world population will further intensify these challenges. The development of renewable energies is therefore of central importance. The 2020 EU Energy Roadmap aims to increase the share of renewable energies (gross energy consumption) to 55% by 2050. Hydrogen (H2) has the highest potential to become the primary renewable energy source. It is envisioned that by 2050 up to 24% of the total energy demand of Europe is to be ensured by H2. However, a decisive disadvantage of the climate friendly alternatives is the massive containment demand, which needs to be highly secure, cost efficient and easily extractable. Underground geological formations (UGF) represent a seemingly optimal alternative to meet the rapidly increasing storage demand. In this context, many studies are currently underway to determine the feasibility and risks of UGF. However, little or no consideration is being given to microbiology. Therefore, in this Research Topic we will focus on achieving a greater understanding of the impact microorganisms exert on UGF, with a particular emphasis on interdisciplinary studies. As many subsurface microbial communities can use H2 as an electron donor, production of seemingly undesirable metabolic byproducts, such as hydrogen sulfide, methane, and acids, are also to be expected. However, the rate of the H2 conversion by the microorganisms, how their metabolic activities impact the UGF on a short-term and long-term scale, the extent of damages microorganisms exert on the infrastructure, or potential use of microorganisms to enhance UGF are just a few questions that require urgent research to assess the role of microorganisms in this new anthropogenic use of the subsurface environment. These and many questions can be addressed in this article collection. In particular, understanding microbial community changes and activity rates will help assess operational and environmental risks, develop mitigation strategies and provide new insights on life under extreme conditions (i.e., pressure, salinity). In this Research Topic, the editorial team particularly welcomes Original Research, Hypothesis and Theory, Method, and Review manuscripts that deal with the latest advances in microbiology in formations that are planned or currently prepared for hydrogen storage, from both fundamental and practical points of view. The ultimate objective is to promote a deeper understanding into the sustainability of UGF and generate interdisciplinary research involving microbiologists, reservoir engineers, geologists, chemists, physicists. The topics of interest include, but are not limited to: • Microbial diversity in different underground hydrogen storage sites or formations currently being considered for hydrogen storage • Mechanism and impact of microbial growth under high H2 pressure • Potential role of microorganisms in the short-term and long-term storage of hydrogen • Potential influences of microorganisms on the hydrogen storage infrastructure systems, e.g., microbiologically influenced corrosion, biofilm growth • Hydrogen-solid-microorganism interactions, including the influence of microbial growth on UGF geological parameters • Mechanism and modelling of microbial impact on hydrogen storage UGF relevant for this Research Topic include porous media, salt caverns, deep aquifers, hard rock caverns and depleted oil/gas reservoirs. KW - Biodeterioration and biodegradation KW - Geology KW - Anaerobic pathways KW - Microbial simulation, KW - Hydrogen storage PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579042 DO - https://doi.org/10.3389/fenrg.2023.1242619 SN - 2296-598X VL - 11 SP - 1 EP - 3 PB - Frontiers CY - Frontiers in Energy Research AN - OPUS4-57904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müllner, S. A1 - Held, T. A1 - Tichter, Tim A1 - Rank, P. A1 - Leykam, D. A1 - Jiang, W. A1 - Lunkenbein, T. A1 - Gerdes, T. A1 - Roth, C. T1 - Impact of Functional Groups in Reduced Graphene Oxide Matrices for High Energy Anodes in Lithium-Ion Batteries N2 - Most high capacity anode materials for lithium-ion batteries (LiB) require a carbonaceous matrix. In this context one promising material is reduced graphene oxide (rGO). Herein, we present the influence of different reduction degrees of rGO on its physico-chemical properties, such as crystallinity, specific surface area, electrical conductivity and electrochemical lithiation/delithiation behavior. It is found that a heat treatment under inert and reducing atmospheres increases the long-range order of rGO up to a temperature of 700 °C. At temperatures around 1000 °C, the crystallinity decreases. With decreasing oxygen content, a linear decrease in irreversible capacity during cycle 1 can be observed, along with a significant increase in electrical conductivity. This decrease in irreversible capacity can be observed despite an increase in specific surface area indicating the more significant influence of the oxygen content on the capacity loss. Consequently, the reversible capacity increases continuously up to a carbon content of 84.4 at% due to the thermal reduction. Contrary to expectations, the capacity decreases with further reduction. This can be explained by the loss of functional groups that will be lithiated reversibly, and a simultaneous reduction of long-range order, as concluded from dq/dU analysis in combination with XRD analysis. KW - Batteries KW - Functional Materials KW - Graphene Oxide PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606852 DO - https://doi.org/10.1149/1945-7111/ace70a SN - 0013-4651 VL - 170 IS - 7 SP - 1 EP - 12 PB - The Electrochemical Society AN - OPUS4-60685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Solberg, S. B. B. A1 - Zimmermann, P. A1 - Wilhelmsen, Ø. A1 - Bock, Robert A1 - Burheim, O. S. T1 - Analytical treatment of ion-exchange permselectivity and transport number measurements for high accuracy N2 - We analyse electromotive force measurements of concentration cells using non-equilibrium thermodynamics, and determine the transference coefficients of ion-exchange membranes in aqueous KCl solutions. By taking advantage of the analytical expression for the permselectivity, we extract transport coefficients with high accuracy. The transport number of K+ and the transference coefficient of water in the Selemion CMVN cationexchange membrane are found to be 100𝑡K+ = 99.59 ± 0.56 and 𝑡𝑤 = 3.69 ± 0.40 respectively, while for the Selemion AMVN anion-exchange membrane they are 100𝑡Cl− = 100.21 ± 0.37 and 𝑡𝑤 = −3.75 ± 0.27. These results suggest that the membranes are perfectly selective to the target ion, and that each ion carries 3-4 water molecules through the membrane, which reduces the membrane permselectivity. In these concentration cells, the electrical potential contribution of the membrane alone was more easily isolated with bare Ag/AgCl electrodes without reference solutions and liquid junction plugs. Additionally, we find a large contribution to the measured concentration cell voltage from concentration gradients across the porous plug of the reference electrode, which cannot be explained by Henderson’s equation alone. For most of the concentration range, the transport number of the porous plug is determined to be 100𝑡K+ = 49.43 ± 0.78 with negligible water transport, similar to literature values for bulk electrolyte. In dilute electrolyte solutions with concentrations below 0.1 mol kg−1, the plug shows anomalous behaviour consistent with an increase in K+ selectivity and water co-transport. KW - Ion-exchange membranes KW - Electrodialysis KW - Non-equilibrium thermodynamics KW - Electroosmosis KW - Transport number PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580654 DO - https://doi.org/10.1016/j.memsci.2023.121904 SN - 1873-3123 VL - 2023 IS - 685 PB - Elsevier CY - New York, NY [u.a.] AN - OPUS4-58065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baensch, Franziska A1 - Baer, Wolfram A1 - Wossidlo, Peter A1 - Habib, Abdel Karim T1 - Damage evolution detection in a pipeline segment under bending by means of acoustic emission N2 - A steel pipeline segment of 2.5 m length was subjected to quasi-static four-point bending load in three steps for studying the initial cracking and damage accumulation based on the Acoustic Emission (AE) technique and by the direct current potential drop (DCPD) technique. For the latter, a new post-test analysis method was established. AE is found more sensitive to crack initiation than DCPD. Formation of mesoscopic and macroscopic cracks as well as their closure and the resulting friction generate weighted peak frequencies below 400 kHz, whereas microscopic cracking produces AE with broad band spectra identifiable by weighted peak frequencies above 400 kHz. Critical states alike the maximum load level and the leak opening were accompanied by peak amplitudes above 85 dBAE. This rather fundamental study provides a data base for possibly developing advanced strategies of detection and alarm systems based on acoustic monitoring of pipelines, or at least, steel structures. KW - Crack KW - Accoustic emission KW - Frequency domain KW - Potential drop technique KW - Fracture PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565171 DO - https://doi.org/10.1016/j.ijpvp.2022.104863 SN - 0308-0161 VL - 201 IS - 104863 SP - 1 EP - 9 PB - Elsevier Science CY - Amsterdam AN - OPUS4-56517 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 - JOUR A1 - Edzards, Joshua A1 - Saßnick, Holger-Dietrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Valencia, Ana M. A1 - Emmerling, Franziska A1 - Beyer, Sebastian A1 - Cocchi, Caterina T1 - Effects of Ligand Substituents on the Character of Zn-Coordination in Zeolitic Imidazolate Frameworks N2 - Due to their favorable properties and high porosity, zeolitic imidazolate frameworks (ZIFs) have recently received much limelight for key technologies such as energy storage, optoelectronics, sensorics, and catalysis. Despite widespread interest in these materials, fundamental questions regarding the zinc coordination environment remain poorly understood. By focusing on zinc(II)2-methylimidazolate (ZIF-8) and its tetrahedrally coordinated analogues with Br-, Cl-, and H-substitution in the 2-ring position, we aim to clarify how variations in the local environment of Zn impact the charge distribution and the electronic properties of these materials. Our results from densityfunctional theory confirm the presence of a Zn coordinative bond with a large polarization that is quantitatively affected by different substituents on the organic ligand. Moreover, our findings suggest that the variations in the Zn coordination induced by the functionalization have a negligible effect on the electronic structure of the considered compounds. On the other hand, halogen terminations of the ligands lead to distinct electronic contributions in the vicinity of the frontier region which ultimately reduce the band gap size by a few hundred millielectron volts. Experimental results obtained from X-ray absorption spectroscopy (Zn K-edge) confirm the trends predicted by theory and, together with them, contribute to a better understanding of the structure−property relationships that are needed to tailor ZIFs for target applications. KW - Surfaces KW - Physical and Theoretical Chemistry KW - General Energy KW - Electronic KW - Coatings and Films KW - Optical and Magnetic Materials PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589117 DO - https://doi.org/10.1021/acs.jpcc.3c06054 SN - 1932-7447 VL - 127 IS - 43 SP - 21456 EP - 21464 PB - American Chemical Society (ACS) AN - OPUS4-58911 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 - Peters, Stefan A1 - Kunkel, Benny A1 - Cakir, Cafer Tufan A1 - Kabelitz, Anke A1 - Witte, Steffen A1 - Bernstein, Thomas A1 - Bartling, Stephan A1 - Radtke, Martin A1 - Emmerling, Franziska A1 - Abdel-Mageed, Ali Mohamed A1 - Wohlrab, Sebastian A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy N2 - A novel setup for dispersive X-ray absorption spectroscopy (XAS) with simultaneous resolution of space, time and energy for in situ characterization of solid materials is demonstrated. KW - Dispersive XAS KW - Catalysis KW - In situ KW - Structure analysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584924 DO - https://doi.org/10.1039/d3cc03277a SN - 1359-7345 SP - 1 EP - 4 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58492 LA - eng 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 - 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 - Han, Ying A1 - Kruse, Julius A1 - Rosalie, Julian A1 - Radners, J. A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Influence of mean stress and overaging on fatigue life of aluminum alloy EN AW-2618A N2 - Fatigue tests were performed on the forged aluminum alloy EN AW-2618A in the T61 state. Different stress ratios (R = -1, R = 0.1) were selected to study the influence of mean stress on fatigue life. Two overaged states (10 h/230 ◦C, 1000 h/230 ◦C) were also tested to investigate the influence of overaging on fatigue life. Transmission electron microscopy (TEM) was used to characterize the precipitates (S-phase), which are mainly responsible for the strength of the alloy. A fractographic analysis was also performed to determine the failure mode. Overaging reduces the fatigue life compared to the T61 state. The longer the aging time, the lower the fatigue resistance. The reason is the decrease in (yield) strength, which correlates with the radius of the S-phase: the precipitate radius increases by a factor of approximately two for the overaged states compared to the initial state. The analysis of the fracture surfaces showed crack initiation occurs predominantly on the outer surface and is associated with the primary phases. KW - Aluminum alloys KW - Aging KW - Fatigue KW - Microstructure KW - Electron microscopy KW - S-Phase PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583708 DO - https://doi.org/10.1016/j.msea.2023.145660 SN - 0921-5093 VL - 886 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-58370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rehmer, Birgit A1 - Bayram, Faruk A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Skrotzki, Birgit T1 - Elastic modulus data for additively and conventionally manufactured variants of Ti-6Al-4V, IN718 and AISI 316 L N2 - This article reports temperature-dependent elastic properties (Young’s modulus, shear modulus) of three alloys measured by the dynamic resonance method. The alloys Ti-6Al-4V, Inconel IN718, and AISI 316 L were each investigated in a variant produced by an additive manufacturing processing route and by a conventional manufacturing processing route. The datasets include information on processing routes and parameters, heat treatments, grain size, specimen dimensions, and weight, as well as Young’s and shear modulus along with their measurement uncertainty. The process routes and methods are described in detail. The datasets were generated in an accredited testing lab, audited as BAM reference data, and are hosted in the open data repository Zenodo. Possible data usages include the verification of the correctness of the test setup via Young’s modulus comparison in low-cycle fatigue (LCF) or thermo-mechanical fatigue (TMF) testing campaigns, the design auf VHCF specimens and the use as input data for simulation purposes. KW - Elastic modulus KW - Young's modulus KW - Shear modulus KW - Additive manufacturing KW - AISI 316L KW - IN 718 KW - Ti-6Al-4V KW - Reference data KW - Temperature dependence PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579716 DO - https://doi.org/10.1038/s41597-023-02387-6 VL - 10 IS - 1 SP - 1 EP - 9 PB - Springer Nature AN - OPUS4-57971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Knigge, Xenia A1 - Ciornii, Dmitri A1 - Reed, B.P. A1 - Pollard, A.J. A1 - Clifford, C.A. A1 - Howe, T. A1 - Vyas, N. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Influence of the Morphology on the Functionalization of Graphene Nanoplatelets Analyzed by Comparative Photoelectron Spectroscopy with Soft and Hard X-Rays N2 - Since its isolation, graphene has received growing attention from academia and industry due to its unique properties. However, the “what is my material” barrier hinders further commercialization. X-ray photoelectron spectroscopy (XPS) is considered as a method of choice for the determination of the elemental and chemical composition. In this work the influence of the morphology of graphene particles on the XPS results is studied and investigated as a function of X-ray energy, using conventional XPS with Al K𝜶 radiation and hard X-ray photoemission spectroscopy (HAXPES) using Cr K𝜶 radiation. Thereby, the information depth is varied between 10 and 30 nm. For this purpose, two commercial powders containing graphene nanoplatelets with lateral dimensions of either ≈100 nm or in the micrometer range are compared. These larger ones exist as stack of graphene layers which is inspected with scanning electron microscopy. Both kinds of particles are then functionalized with either oxygen or fluorine. The size of the graphene particles is found to influence the degree of functionalization. Only the combination of XPS and HAXPES allows to detect the functionalization at the outermost surface of the particles or even of the stacks and to provide new insights into the functionalization process. KW - Functionalized graphene KW - Hard-energy X-ray photoelectron spectroscopy KW - X-ray photoelectron spectroscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578860 DO - https://doi.org/10.1002/admi.202300116 SN - 2196-7350 SP - 1 EP - 8 PB - Wiley VCH AN - OPUS4-57886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Terborg, R. A1 - Kim, K. J. A1 - Hodoroaba, Vasile-Dan T1 - Elemental composition and thickness determination of thin films by electron probe microanalysis N2 - Electron probe microanalysis (EPMA) applies to solid samples of homogenous (bulk) chemical composition and can usually not be applied to structures which are inhomogeneous in the micrometer range such as thin film systems down to a few nm. However, in combination with the established thin film software Stratagem, the thickness as well as the elemental composition of thin films on a substrate can be determined. This has been recently successfully demonstrated for Fe-Ni on Si and Si-Ge on Al2O3 thin film systems. For both systems five samples of different elemental composition and a reference were produced and characterised by inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM) as reference values. Last year, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we reevaluated the data acquired for the Fe-Ni and Si-Ge systems using the BadgerFilm software package and compared the obtained elemental compositions and thickness values with the results of the Stratagem software and the reference methods. The conclusion is that the BadgerFilm software shows good agreement with the elemental composition and thickness calculated by Stratagem (mostly <2% for both composition and thickness) and with the reference values for two representative thin film systems (<1%–2% for composition and <10%–20% for thickness). KW - Elemental composition KW - EPMA KW - Film thickness KW - Thin films PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576368 DO - https://doi.org/10.1002/sia.7183 SN - 0142-2421 VL - 55 SP - 496 EP - 500 PB - Wiley AN - OPUS4-57636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Jürgens, Maria A1 - Uhlemann, Patrick A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Experimental data from service-like creep-fatigue experiments on grade P92 steel N2 - This article refers to the research article entitled “Creep-Fatigue of P92 in Service-Like Tests with Combined Stress- and Strain-Controlled Dwell Times” [1]. It presents experimental mechanical data from complex service-like creep-fatigue experiments performed isothermally at 620 °C and a low strain amplitude of 0.2 % on tempered martensite-ferritic grade P92 steel. The data sets in text file format provide cyclic deformation (min. and max. stresses) and the total (hysteresis) data of all recorded fatigue cycles for three different creep-fatigue experiments: 1) a standard relaxation fatigue (RF) test with symmetrical dwell times of three minutes introduced at minimum and maximum strain, 2) a fully strain-controlled service-like relaxation (SLR) test combining these three-minute peak strain dwells with a 30-minute dwell in between at zero strain, and 3) a partly stress-controlled service-like creep (SLC) test combining the three-minute peak strain dwells with 30-minute dwells at constant stress. Such service-like (SL) tests with additional long-term stress- and strain-controlled dwell times are non-standard, rare, and expensive, making these data very valuable. They may be used to approximate cyclic softening in the technically relevant range, for the design of complex SL experiments, or for detailed analyses of stress-strain hystereses (e.g., for stress or strain partitioning methods, for the determination of hysteresis energies (work), inelastic strain components, etc.). In addition, the latter analyses may supply important input for advanced parametric lifetime modeling of components under creep-fatigue loading or model calibration parameters. KW - Tempered martensite-ferritic steel KW - Creep KW - Stress relaxation KW - Creep-fatigue KW - Dwell times PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578407 DO - https://doi.org/10.1016/j.dib.2023.109333 SN - 2352-3409 VL - 49 SP - 1 EP - 9 PB - Elsevier Inc. AN - OPUS4-57840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Bartczack, Dorota A1 - Taché, Olivier A1 - Hodoroaba, Vasile-Dan T1 - Report on the homogeneity assessment of bimodal gold materials (nPSize1 and nPSize2) and particle number concentration by frequency method N2 - The main objective was to assess homogeneity of two bimodal gold materials, namely nPsize1 and nPSize2, containing approximately 1:1 and 10:1 particle number-based ratio of ~30nm and ~60nm particles. Particle number-based concentration within the two size fractions was determined with spICP-MS using the particle frequency method of calibration. KW - Nanoparticles KW - Homogeneity KW - Particle number concentration KW - Gold KW - nPSize PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595451 DO - https://doi.org/10.5281/zenodo.10654245 SP - 1 EP - 5 PB - Zenodo CY - Geneva AN - OPUS4-59545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mehta, B. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Markötter, Henning A1 - Bruno, Giovanni A1 - Hryha, E. A1 - Nyborg, L. A1 - Virtanen, E. T1 - Microstructure, mechanical properties and fracture mechanisms in a 7017 aluminium alloy tailored for powder bed fusion – laser beam N2 - This study addressed a 7017 Al-alloy tailored for powder bed fusion – laser beam (PBF-LB) process. The alloy was prepared by mixing 3 wt% Zr and 0.5 wt% TiC powder to standard pre-alloyed 7017 grade aluminium powder. This made printing of the alloys possible avoiding solidification cracking in the bulk and achieving high relative density (99.8 %). Such advanced alloys have significantly higher Young’s modulus (>80 GPa) than conventional Al-alloys (70–75 GPa), thus making them attractive for applications requiring high stiffness. The resulting microstructure in as-printed condition was rich in particles originating from admixed powders and primary precipitates/inclusions originating from the PBF-LB process. After performing a T6-like heat treatment designed for the PBF-LB process, the microstructure changed: Zr-nanoparticles and Fe- or Mg/Zn- containing precipitates formed thus providing 75 % increase in yield strength (from 254 MPa to 444 MPa) at the cost of decreasing ductility (∼20 % to ∼9 %). In-situ tensile testing combined with SXCT, and ex-situ tensile testing combined with fracture analysis confirmed that the fracture initiation in both conditions is highly dependent on defects originated during printing. However, cracks are deflected from decohesion around Zr-containing inclusions/precipitates embedded in the Al-matrix. This deflection is seen to improve the ductility of the material. KW - Additive manufacturing KW - Powder bed fusion Laser beam KW - X-ray computed tomography KW - Strengthening mechanisms KW - Crack propagation KW - Zirconium PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568243 DO - https://doi.org/10.1016/j.matdes.2023.111602 SN - 0264-1275 VL - 226 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Bruno, Giovanni T1 - Noise and blur removal from corrupted X-ray computed tomography scans: A multilevel and multiscale deep convolutional framework approach with synthetic training data (BAM SynthCOND) N2 - Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc. KW - XCT Data Conditioning KW - Denoising Deblurring Sharpening KW - Deep Convolutional Neural Network (DCNN) KW - Synthetic Training Data KW - ACEnet KW - Metal Matrix Composite (MMC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579129 DO - https://doi.org/10.1016/j.tmater.2023.100011 VL - 2 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-57912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Ávila Calderón, Luis A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Evans, Alexander A1 - Skrotzki, Birgit A1 - Bruno, Giovanni T1 - Evolution of Creep Damage of 316L Produced by Laser Powder Bed Fusion N2 - The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed. KW - Creep KW - Computed Tomography KW - PBF-LB/M/316L KW - Laser Powder Bed Fusion KW - Microstructure KW - AISI 316L KW - Additive Manufacturing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574127 DO - https://doi.org/10.1002/adem.202201581 SP - 1 EP - 9 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-57412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jamro, R. A1 - Mente, Tobias A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Al-Falahat, Ala'A. M. A1 - Woracek, R. A1 - Manke, I. A1 - Griesche, Axel T1 - Temperature distribution during welding measured by neutron imaging N2 - This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data. KW - Neutron imaging KW - Debye-Waller-Faktor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586268 DO - https://doi.org/10.1088/1742-6596/2605/1/012026 VL - 2605 SP - 1 EP - 10 PB - IOP Publishing Ltd. AN - OPUS4-58626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Kai A1 - Mirabella, Francesca A1 - Knigge, Xenia A1 - Mezera, Marek A1 - Weise, Matthias A1 - Sahre, Mario A1 - Wasmuth, Karsten A1 - Voss, Heike A1 - Hertwig, Andreas A1 - Krüger, Jörg A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Bonse, Jörn T1 - Chemical and topographical changes upon sub-100-nm laser-induced periodic surface structure formation on titanium alloy: the influence of laser pulse repetition rate and number of over-scans N2 - Titanium and its alloys are known to allow the straightforward laser-based manufacturing of ordered surface nanostructures, so-called high spatial frequency laser-induced periodic surface structures (HSFL). These structures exhibit sub-100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi-method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near-surface chemical analyses hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (ToF-SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non-ablative laser-induced near-surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat-accumulation effects. T2 - 2023 E-MRS Spring Meeting, Symposium L "Making light matter: lasers in material sciences and photonics" CY - Strasbourg, France DA - 29.05.2023 KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses KW - Laser processing KW - Hard X-ray photoelectron spectroscopy (HAXPES) KW - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589902 UR - https://onlinelibrary.wiley.com/doi/full/10.1002/pssa.202300719 DO - https://doi.org/10.1002/pssa.202300719 SN - 1862-6319 VL - 221 IS - 15 SP - 1 EP - 12 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-58990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drobne, D. A1 - Ciornii, Dmitri A1 - Hodoroaba, Vasile-Dan A1 - Bohmer, N. A1 - Novak, S. A1 - Kranjc, E. A1 - Kononenko, V. A1 - Reuther, R. T1 - Knowledge, Information, and Data Readiness Levels (KaRLs) for Risk Assessment, Communication, and Governance of Nano-, New, and Other Advanced Materials N2 - The obvious benefits derived from the increasing use of engineered nano-, new, and advanced materials and associated products have to be weighed out by a governance process against their possible risks. Differences in risk perception (beliefs about potential harm) among stakeholders, in particular nonscientists, and low transparency of the underlying decision processes can lead to a lack of support and acceptance of nano-, new, and other advanced material enabled products. To integrate scientific outcomes with stakeholders needs, this work develops a new approach comprising a nine-level, stepwise categorization and guidance system entitled “Knowledge, Information, and Data Readiness Levels” (KaRLs), analogous to the NASA Technology Readiness Levels. The KaRL system assesses the type, extent, and usability of the available data, information, and knowledge and integrates the participation of relevant and interested stakeholders in a cocreation/codesign process to improve current risk assessment, communication, and governance. The novelty of the new system is to communicate and share all available and relevant elements on material related risks in a user/stakeholder-friendly, transparent, flexible, and holistic way and so stimulate reflection, awareness, communication, and a deeper understanding that ultimately enables the discursive process that is needed for the sustainable risk governance of new materials. KW - Risk asessment KW - Advanced materials KW - TRL KW - Governance KW - Data readiness level PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575344 DO - https://doi.org/10.1002/gch2.202200211 SP - 1 EP - 9 PB - Wiley-VCH AN - OPUS4-57534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Müller, P. A1 - Babick, F. A1 - Friedrich, C. M. A1 - Ghanem, A. A1 - Hodoroaba, Vasile-Dan A1 - Mech, A. A1 - Weigel, S. A1 - Wohlleben, W. A1 - Rauscher, H. T1 - NanoDefiner Framework and e-Tool Revisited According to the European Commission’s Nanomaterial Definition 2022/C 229/01 N2 - The new recommended definition of a nanomaterial, 2022/C 229/01, adopted by the European Commission in 2022, will have a considerable impact on European Union legislation addressing chemicals, and therefore tools to implement this new definition are urgently needed. The updated NanoDefiner framework and its e-tool implementation presented here are such instruments, which help stakeholders to find out in a straightforward way whether a material is a nanomaterial or not. They are two major outcomes of the NanoDefine project, which is explicitly referred to in the new definition. This work revisits the framework and e-tool, and elaborates necessary adjustments to make these outcomes applicable for the updated recommendation. A broad set of case studies on representative materials confirms the validity of these adjustments. To further foster the sustainability and applicability of the framework and e-tool, measures for the FAIRification of expert knowledge within the e-tool’s knowledge base are elaborated as well. The updated framework and e-tool are now ready to be used in line with the updated recommendation. The presented approach may serve as an example for reviewing existing guidance and tools developed for the previous definition 2011/696/EU, particularly those adopting NanoDefine project outcomes. KW - Nanomaterial definition KW - Nanomaterial categorisation KW - Nanomaterial regulation KW - Nanomaterial legislation KW - Decision support KW - FAIRification PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571618 DO - https://doi.org/10.3390/nano13060990 SN - 2079-4991 VL - 13 IS - 6 - Special Issue "Identification and Quantification of Nanomaterials" SP - 1 EP - 16 PB - MDPI CY - Basel, CH AN - OPUS4-57161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, Maha A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Understanding the recovery behaviour and the degradative processes of EPDM during ageing N2 - Recovery is an important measure for seal applications representing to which extent the elastomer regains its initial shape after deformation and release of an applied force. Compression set (CS) indicates the degree of recovery. Ethylene propylene diene rubber (EPDM) was aged at 75 ◦C, 100 ◦C, 125 ◦C and 150 ◦C for different ageing times up to five years and compression set measurements were performed at different times after disassembly and after additional tempering. Short- and long-term recovery up to one year after release for samples aged at 125 ◦C and 150 ◦C was also studied. To assess the curvature in the Arrhenius diagram that may occur due to non-sufficiently aged specimens, a degradation-rate based model was fitted to the CS data after tempering. For each ageing temperature, two decay fit functions were proposed, each with an activation energy and a corresponding degradative process. The influence of ageing on the leak-tightness after fast small partial release is investigated and estimated through the analysis of the shift factors from time temperature superposition (TTS) of CS measurements at different times after disassembly. Shift factors of CS measurement after 1 s and after additional tempering are in good agreement. KW - Compression set KW - Ageing KW - Recovery KW - Degradative processes KW - Leakage rate PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573699 DO - https://doi.org/10.1016/j.polymertesting.2023.107987 SN - 0142-9418 VL - 121 SP - 107987 PB - Elsevier Ltd. AN - OPUS4-57369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockenhäuser, Christian A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Brinell-Hardness data (HBW 2.5/62.5) of aluminum alloy EN AW-2618A after different aging times and temperatures N2 - The article covers data on the Brinell hardness of the forged precipitation-hardened aluminum alloy EN AW-2618A in the initial T61 condition (i. e. slightly underaged) and after isothermal aging for up to 25,0 0 0 h at aging temperatures between 160 °C and 350 °C. In addition, the hardness was determined on specimens after creep testing at 190 °C and various stresses. The hardness decreases with increasing ag- ing time due to the microstructural evolution of the harden- ing precipitates. The drop occurs faster the higher the aging temperature. Aging under creep load additionally accelerates the hardness decrease. KW - Aluminum alloy KW - EN AW-2618A KW - Brinell hardness KW - Aging KW - Creep KW - Ostwald ripening KW - Reheating PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567611 DO - https://doi.org/10.1016/j.dib.2022.108830 SN - 2352-3409 VL - 46 PB - Elsevier Inc. AN - OPUS4-56761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abel, Andreas A1 - Rosalie, Julian A1 - Reinsch, Stefan A1 - Zapala, Pawel A1 - Michels, Heiner A1 - Skrotzki, Birgit T1 - Influence of Mo and B additions in intermetallic near-Fe3Al alloys on microstructure and mechanical properties N2 - Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms. KW - Materials Chemistry KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials KW - General Chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-585284 DO - https://doi.org/10.1016/j.intermet.2023.108074 VL - 163 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-58528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Jürgens, Maria A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Creep-fatigue of P92 in service-like tests with combined stress- and strain-controlled dwell times N2 - Complex service-like relaxation- and creep-fatigue tests with strain- and stress-controlled dwells and fatigue cycle durations of approx. 2200 s were performed exemplarily on a grade P92 steel at 620 ◦C in this study. The results indicate deviations in the prevailing creep mechanisms of long-term relaxation and creep dwells, affecting subsequent dwells, load shifts, and the macroscopic softening behavior quite differently. In addition, fracture surfaces and longitudinal metallographic sections reveal intergranular crack growth for complex loading with stress-controlled dwells, whereas complex strain-controlled tests enhance oxidation and transgranular crack propagation. These findings substantiate the limited transferability of relaxation-fatigue to creep-fatigue conditions. KW - Tempered martensite-ferritic steel KW - P92 KW - Dwell periods KW - Creep-fatigue interaction KW - Stress relaxation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564239 DO - https://doi.org/10.1016/j.ijfatigue.2022.107381 SN - 0142-1123 VL - 168 SP - 1 EP - 12 PB - Elsevier Ltd. AN - OPUS4-56423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Hanke, T. A1 - Weber, M. A1 - Eisenbart, M. A1 - Bauer, F. A1 - Meissner, R. A1 - Dziwis, G. A1 - Tikana, L. A1 - Chen, Yue A1 - Skrotzki, Birgit T1 - Toward a digital materials mechanical testing lab N2 - To accelerate the growth of Industry 4.0 technologies, the digitalization of mechanical testing laboratories as one of the main data-driven units of materials processing industries is introduced in this paper. The digital lab infrastructure consists of highly detailed and standard-compliant materials testing knowledge graphs for a wide range of mechanical testing processes, as well as some tools that enable the efficient ontology development and conversion of heterogeneous materials’ mechanical testing data to the machine-readable data of uniform and standardized structures. As a basis for designing such a digital lab, the mechanical testing ontology (MTO) was developed based on the ISO 23718 and ISO/IEC 21838-2 standards for the semantic representation of the mechanical testing experiments, quantities, artifacts, and report data. The trial digitalization of materials mechanical testing lab was successfully performed by utilizing the developed tools and knowledge graph of processes for converting the various experimental test data of heterogeneous structures, languages, and formats to standardized Resource Description Framework (RDF) data formats. The concepts of data storage and data sharing in data spaces were also introduced and SPARQL queries were utilized to evaluate how the introduced approach can result in the data retrieval and response to the competency questions. The proposed digital materials mechanical testing lab approach allows the industries to access lots of trustworthy and traceable mechanical testing data of other academic and industrial organizations, and subsequently organize various data-driven research for their faster and cheaper product development leading to a higher performance of products in engineering and ecological aspects. KW - General Engineering KW - General Computer Science PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582698 DO - https://doi.org/10.1016/j.compind.2023.104016 SN - 0166-3615 VL - 153 SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-58269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yao, J. A1 - Zhu, G. A1 - Dong, K. A1 - Osenberg, M. A1 - Hilger, A. A1 - Markötter, Henning A1 - Ju, J. A1 - Sun, F. A1 - Manke, I. A1 - Cui, G. T1 - Progress and Perspective of Controlling Li Dendrites Growth in All-Solid-State Li Metal Batteries via External Physical Fields N2 - Li dendrites penetration through solid electrolytes (SEs) challenges the development of solid-state Li batteries (SSLBs). To date, significant efforts are devoted to understand the mechanistic dynamics of Li dendrites nucleation, growth, and propagation in SEs, and various strategies that aim to alleviate and even inhibit Li dendrite formation have been proposed. Nevertheless, most of these conventional strategies require either additional material processing steps or new materials/layers that eventually increase battery cost and complexity. In contrast, using external fields, such as mechanical force, temperature physical field, electric field, pulse current, and even magnetic field to regulate Li dendrites penetration through SEs, seems to be one of the most cost-effective strategies. This review focuses on the current research progress of utilizing external physical fields in regulating Li dendrites growth in SSLBs. For this purpose, the mechanical properties of Li and SEs, as well as the experimental results that visually track Li penetration dynamics, are reviewed. Finally, the review ends with remaining open questions in future studies of Li dendrites growth and penetration in SEs. It is hoped this review can shed some light on understanding the complex Li dendrite issues in SSLBs and potentially guide their rational design for further development. KW - Li dendrites KW - Li dendrites penetration mechanisms KW - Solid electrolytes KW - Solid-state batteries PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588331 DO - https://doi.org/10.1002/aesr.202300165 SN - 2699-9412 SP - 1 EP - 44 PB - Wiley-VCH CY - Weinheim AN - OPUS4-58833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Evsevleev, Sergei A1 - Arlt, T. A1 - Ulbricht, Alexander A1 - Dayani, Shahabeddin A1 - Bruno, Giovanni T1 - A Review of X-Ray Imaging at the BAMline (BESSY II) N2 - The hard X-ray beamline BAMline at BESSY II (Berlin, Germany) has now been in service for 20 years. Several improvements have been implemented in this time, and this review provides an overview of the imaging methods available at the BAMline. Besides classic full-field synchrotron X-ray computed tomography (SXCT), also absorption edge CT, synchrotron X-ray refraction radiography (SXRR), and synchrotron X-ray refraction tomography (SXRCT) are used for imaging. Moreover, virtually any of those techniques are currently coupled in situ or operando with ancillary equipment such as load rigs, furnaces, or potentiostats. Each of the available techniques is explained and both the current and the potential usage are described with corresponding examples. The potential use is manifold, the examples cover organic materials, composite materials, energy-related materials, biological samples, and materials related to additive manufacturing. The article includes published examples as well as some unpublished applications. KW - Material science KW - Radiography KW - Refraction KW - Tomography KW - X-ray imaging PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572417 DO - https://doi.org/10.1002/adem.202201034 SN - 1438-1656 SP - 1 EP - 22 PB - Wiley VHC-Verlag AN - OPUS4-57241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - De la Hoz Alford, L. A1 - Pecanha de Souza, C. G. A1 - Paciornik, S. A1 - d` Almeida, J. R. M. A1 - Santos Leite, B. A1 - Avila, H. C. A1 - Léonard, F. A1 - Bruno, Giovanni T1 - Three-Dimensional Characterization of Polyurethane Foams Based on Biopolyols N2 - Two biopolyol-based foams derived from banana leaves (BL) or stems (BS) were produced, and their compression mechanical behavior and 3D microstructure were characterized. Traditional compression and in situ tests were performed during 3D image acquisition using X-ray microtomography. A methodology of image acquisition, processing, and analysis was developed to discriminate the foam cells and measure their numbers, volumes, and shapes along with the compression steps. The two foams had similar compression behaviors, but the average cell volume was five times larger for the BS foam than the BL foam. It was also shown that the number of cells increased with increasing compression while the average cell volume decreased. Cell shapes were elongated and did not change with compression. A possible explanation for these characteristics was proposed based on the possibility of cell collapse. The developed methodology will facilitate a broader study of biopolyol-based foams intending to verify the possibility of using these foams as green alternatives to the typical petrol-based foams. KW - Compression mechanical KW - Biopolyol KW - Banana KW - 3D microstructure KW - X-ray microtomography PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571982 DO - https://doi.org/10.3390/ma16052118 SN - 1996-1944 VL - 16 IS - 5 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-57198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mouiya, M. A1 - Martynyuk, M. A1 - Kupsch, Andreas A1 - Laquai, R. A1 - Müller, Bernd R. A1 - Doyen, N.T. A1 - Tamraoui, Y. A1 - Serrano-Munoz, Itziar A1 - Huger, M. A1 - Kachanov, M. A1 - Bruno, Giovanni T1 - The stress–strain behavior of refractory microcracked aluminum titanate: The effect of zigzag microcracks and its modeling N2 - The stress–strain behavior of ceramics, such as aluminum titanate, has certain features that are unusual for brittle materials—in particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the sharp increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and are attributed to microcracking. Here we compare different degrees of stress–strain nonlinearity of aluminum titanate materials and quantitatively model them. We use advanced mechanical testing to observe the mechanical response at room and high temperature; electron microscopy, and X-ray refraction radiography to observe the microstructural changes. Experiments show that two types of microcracks can be distinguished: (i) microcracks induced by cooling from the sintering temperature (due to heterogeneity and anisotropy of thermal expansion), with typical sizes of the order of grain size, and (ii) much larger microcracks generated by the mechanical loading. The two microcrack types produce different effects on the stress–strain curves. Such microcracks and the features of the stress–strain behavior depend on the density of the cooling-induced microcracks and on the distribution of grain sizes. They are modeled analytically and numerically. KW - Hystersis KW - Nonlinear stress-strain curve KW - Refractory KW - Stiffness KW - X-ray refraction PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580517 DO - https://doi.org/10.1111/jace.19325 SN - 1551-2916 VL - 106 SP - 6995 EP - 7008 PB - Wiley-Blackwell CY - Oxford [u.a.] AN - OPUS4-58051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Serrano-Munoz, Itziar A1 - Laquai, René A1 - Bruno, Giovanni T1 - Anwendungen der Röntgenrefraktionstechnik zur zerstörungsfreien Charakterisierung von Keramiken und Verbundwerkstoffen N2 - Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede: a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1); Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für: a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung. Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie: a) Sintern von SiC-Grünkörpern b) Porositätsanalyse in Dieselpartikelfiltersilikaten c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen d) Mikrorissbildung in Glaskeramik. Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Verbundwerkstoffe KW - Keramik PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576171 UR - https://jahrestagung.dgzfp.de/Portals/jt2023/BB180/Inhalt/p9.pdf UR - https://jahrestagung.dgzfp.de/Portals/jt2023/BB180/Inhalt/default.htm SN - 978-3-947971-29-9 SP - 1 EP - 16 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-57617 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Piault, Pierre A1 - King, Andrew A1 - Henry, Laura A1 - Bruno, Giovanni T1 - Understanding the hot isostatic pressing efectiveness of laser powder bed fusion Ti‑6Al‑4V by in‑situ X‑ray imaging and difraction experiments N2 - In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate. KW - Additive manufacturing KW - Laser powder bed fusion KW - X-ray computed tomography KW - Hot isostatic pressing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587702 DO - https://doi.org/10.1038/s41598-023-45258-1 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 11 AN - OPUS4-58770 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -