TY - CONF A1 - Schmidt, Dirk T1 - Explosionen in Rohrleitungen N2 - Deflagrationssicherungen sind Sicherheitseinrichtungen, die den Durchfluss von brennbaren Gasen und Dämpfen brennbarer Flüssigkeiten ermöglichen, den Flammendurchschlag und weitere Explosionsausbreitung nach der Zündung von explosionsfähigen Gas-/Dampf-Luftgemischen jedoch verhindern sollen. Von besonderer Bedeutung für die Wirksamkeit der Deflagrationsrohrsicherung ist der Einbauort. Diesbezügliche Abweichungen von den normativen Anforderungen, die Grundlage der Prüfung und Zulassung von Deflagrationsrohrsicherungen sind, können zum Versagen der Sicherheitseinrichtung führen. Oft lassen sich allerdings aus betrieblichen bzw. verfahrenstechnischen Gründen der Norm entsprechende Einbaubedingungen nur schwer oder nicht realisieren. Deshalb besteht das Ziel der Untersuchungen eines F&E-Vorhabens mit der Braunschweiger Flammenfilter GmbH darin, einen Beitrag zur Schaffung einer belastbaren Datenbasis zu leisten, um den Einfluss von Rohrleitungsverzweigungen auf deflagrative Gasexplosionen systematisch zu bewerten. T2 - 606. Sitzung der AGS (Arbeitsgemeinschaft Schadenverhütung Berlin/Brandenburg) CY - Feuersozietät Berlin, Germany DA - 27.03.2019 KW - Explosionsschutz KW - Deflagration KW - Flammendurchschlagssicherung PY - 2019 AN - OPUS4-47925 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Dirk T1 - Entwicklung eines Prüfverfahrens für Detonationsrohrsicherungen N2 - Flammendurchschlagsicherungen sind Armaturen, die das Fortschreiten einer Explosion von einem Anlagenteil in den Anderen verhindern. Diese in Rohren verbauten Armaturen sind durchlässig für das jeweils zu transportierende Produkt, verhindern jedoch den Durchtritt von Flammen. Zum Einsatz kommen Flammendurchschlagsicherungen neben großchemischen Anlagen auch beim Transport von Treibstoffen oder an Tankstellen. Die derzeitige Norm zur Prüfung von Flammendurchschlagsicherungen (DIN EN ISO 16852) basiert nur auf Erkenntnissen aus atmosphärischen Tests. Zur Anwendung von Flammendurchschlagsicherungen bei erhöhten Ausgangsdrücken wird ein Verfahren benötigt, das die sichere und reproduzierbare Baumusterprüfung von Flammendurchschlagsicherungen auf ihre Wirksamkeit gegen Explosionen bei nicht-atmosphärischen Bedingungen erlaubt. Dies wiederum führt zu einer höheren Sicherheit und Verfügbarkeit beim Umgang mit brennbaren Stoffen in der Industrie. T2 - 14. Fachtagung "Anlagen-, Arbeits- und Umweltsicherheit" CY - Köthen, Germany DA - 07.11.2019 KW - Explosionsschutz KW - Detonation KW - Flammendurchschlagsicherung KW - Rohrleitungen PY - 2019 AN - OPUS4-49565 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Dirk A1 - Heidermann, Th. T1 - Untersuchungen zur Belastung von Deflagrationsrohrsicherungen in Rohrleitungsverzweigungen N2 - Im 2. Teil des Artikels zu den Untersuchungen zum Einfluss von Rohrleitungsverzweigungen auf die Wirksam­keit von Deflagrationsrohrsicherungen (s. a. [1]) werden die Ergebnisse der visuellen Beobachtungen des Re­aktionsverlaufes sowie die Belastungen der Flammendurchschlagsicherung (s. Bild 1) bei unterschiedlichen Einbaubedingungen in den Vordergrund gestellt. Gegenübergestellt wird die Belastungssituation der Flam­mensperre in einer geraden und einer verzweigten Rohrleitung. Ausdrücklich wurden Einbaubedingungen gewählt, die nicht Normgerecht [2] sind. Verwendet wurde dafür eine speziell gefertigte Deflagrationsrohrsi­cherung, die eine Beobachtung des Reaktionsverlaufs im Bereich der spiralförmig gewickelten Metallbänder erlaubt. Zusätzlich wurde im geschützten Bereich in der Rohrleitung eine Kamera installiert, die die Belas­tungssituation bei den einzelnen Versuchen dokumentierte. Die Ergebnisse bestätigen sehr eindrucksvoll, dass die Belastungssituation der Deflagrationsrohrsicherung sich in Abhängigkeit von der Konfiguration der Rohrleitung entscheidend ändert. KW - Deflagration KW - Flammendurchschlagsicherung KW - Rohrleitungen PY - 2019 SN - 2191-007 VL - 9 IS - 6 SP - 38 EP - 43 PB - VDI Fachmedien GmbH & Co. KG CY - Düsseldorf AN - OPUS4-48212 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Diaz Cubas, D. A1 - Colmenares, M. G. A1 - Schmidt, J. A1 - Bekheet, M. F. A1 - Pauw, Brian Richard A1 - Gurlo, A. A1 - Simon, U. T1 - High specific surface area ordered mesoporous silica COK-12 with tailored pore size N2 - Ordered mesoporous silica materials such as COK-12, analogous to the well-known SBA-15, are characterized by high surface areas and unique features such as defined pore sizes in the meso-size range and high pore ordering. The aim of this work was to prove the washing step and choice of calcination and aging temperature during the COK-12 synthesis as effective tools in tailoring, markedly improving the specific surface area, pore size, and pore volume. By controlling the aging temperature, the pore size was linearly adjusted between 5.7 and 8.1 nm, while preserving the hexagonal ordering of the pores. The synthesized COK-12 powders possess pore volumes and specific surface areas up to 1.23 cm3 g−1 and 860m2 g−1, respectively, which is markedly higher than what has previously been reported about COK-12. The presented results and the environmentally friendly character of the synthesis will make COK-12 more interesting for future adaption to the industrial processes, for example in catalysis, adsorption, or drug delivery. KW - Ordered mesoporous silica KW - Pore size tailoring KW - High specific surface area KW - SAXS KW - Small angle scattering PY - 2019 DO - https://doi.org/10.1016/j.micromeso.2019.01.050 SN - 1387-1811 VL - 280 SP - 133 EP - 143 PB - Elsevier AN - OPUS4-47378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zemke, F. A1 - Schölch, V. A1 - Bekheet, M.F. A1 - Schmidt, Franziska T1 - Surfactant-assisted sol–gel synthesis of mesoporous bioactive glass microspheres N2 - Spherical mesoporous bioactive glasses in the silicon dioxide (SiO2)-phosphorus pentoxide (P2O5)–calcium oxide (CaO) system with a high specific surface area of up to 300m2/g and a medium pore radius of 4 nm were synthesized by using a simple one-pot surfactant-assisted sol–gel synthesis method followed by calcination at 500–700°C. The authors were able to control the particle properties by varying synthesis parameters to achieve microscale powders with spherical morphology and a particle size of around 5–10 mm by employing one structure-directing agent. Due to a high Calcium oxide content of 33·6mol% and a phosphorus pentoxide content of 4·0mol%, the powder showed very good bioactivity up to 7 d of immersion in simulated Body fluid. The resulting microspheres are promising materials for a variety of life science applications, as further processing – for example, granulation – is unnecessary. Microspheres can be applied as materials for powder-based additive manufacturing or in stable suspensions for drug release, in bone cements or fillers. KW - bioactive KW - biomaterials KW - bone PY - 2019 DO - https://doi.org/10.1680/jnaen.18.00020 SN - 2045-9831 SN - 2045-984X VL - 8 IS - 2 SP - 126 EP - 134 PB - ICE Publishing CY - London AN - OPUS4-50148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, M. E. A1 - Vickery, W. M. A1 - Swift-Ramirez, W. A1 - Arnold, A. M. A1 - Orlando, J. D. A1 - Schmidt, S. J. A1 - Liu, Y. A1 - Er, Jasmin A1 - Schusterbauer, Robert A1 - Ahmed, R. A1 - Nickl, Philip A1 - Radnik, Jörg A1 - Donskyi, Ievgen A1 - Sydlik, S. A. T1 - The Mitsunobu reaction for the gentle covalent attachment of biomolecules to graphene oxide N2 - Graphene oxide (GO) has emerged as a promising biomaterial as it is easily and cheaply synthesized, strong, cytocompatible, osteoinductive, and has a well-characterized aqueous degradation pathway. It is also a great substrate for functionalization with biomolecules such as proteins, peptides, and small molecules that can enhance or add bioactivity. Covalent chemical linkages as opposed to typical noncovalent association methods are preferable so that the biomolecules do not quickly diffuse away or face replacement by other proteins, which is critical in long time scale applications like bone regeneration. However, covalent chemistry tends to carry a drawback of harsh reaction conditions that can damage the structure, conformation, and therefore function of a delicate biomolecule like a protein. Here, the Mitsunobu reaction is introduced as a novel method of covalently attaching proteins to graphene oxide. It features gentle reaction conditions and has the added benefit of utilizing the plentiful basal plane alcohol functionalities on graphene oxide, allowing for high yield protein functionalization. The amino acid Glycine (G), the protein bovine serum albumin (BSA), and the small molecule SVAK-12 are utilized to create the three Mitsunobu Graphene (MG) materials G-MG, BSA-MG, and SVAK-MG that demonstrate the wide applicability of this functionalization method. KW - Graphene oxide KW - Mitsunobu reaction KW - Covalent attachment KW - Bovine serum albumin KW - Macrophage polarization KW - Osteogenesis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630483 DO - https://doi.org/10.1016/j.carbon.2025.120221 VL - 238 SP - 1 EP - 15 PB - Elsevier Ltd. AN - OPUS4-63048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, R. T1 - SEM or TEM for the characterization of nanoparticles? N2 - Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM) ? This is a question, nowadays discussed in EM labs of research and industry involved in the characterization and metrology of nanoparticles. The Scanning principle is adapted to TEM, the Transmission mode is adapted to Ultra High Resolution SEM. Can modern SEM replace TEM, reach atomic resolution even without Cs corrector or nm lateral resolution for energydispersive X-ray spectroscopy (EDX)? Due to the development of a New Cold Field Emission (NCFE) electron source Hitachi SEMs SU9000 and SU8200 can deliver routinely sub-nm image resolution and EDX mappings at very high count rates and a lateral EDX resolution of a few nm. A TiO2 sample provided by BAM was analysed at 30kV using low kV STEM – simultaneously with the Through-the-lens (TTL) SE detector, the Bright Field transmitted and Dark Field transmitted signals. By this method a pixel precise information of the particles surface using SE, its chemical nature using DF-STEM and its crystalline structure using Bright Field signal is given in one 40sec scan. The advantage of this observation mode compared to Ultra Low Voltage imaging is outlined. T2 - Microscopy Conference 2017 CY - Lausanne, Switzerland DA - 21.08.2017 KW - SEM KW - TEM KW - Nanoparticles PY - 2017 UR - http://www.mc2017.ch/ AN - OPUS4-43890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hendriks, L. A1 - Ramkorun-Schmidt, Benita A1 - Grundlach-Graham, A. A1 - Koch, J. A1 - Grass, R. N. A1 - Jakubowski, Norbert A1 - Günther, D. T1 - Single-particle ICP-MS with online microdroplet calibration: toward matrix independent nanoparticle sizing N2 - Single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) has become an effective tool for the detection and quantification of inorganic nanoparticles (NPs). While sizing of NPs suspended in water is relatively straightforward by sp-ICP-MS, accurate mass quantification of NPs in complex media, such as consumer products and natural systems still remains a challenge. When NPs are suspended in a complex medium, the matrix may affect the analyte sensitivity and lead to inaccurate NP sizing. Here, we investigate the use of an online microdroplet calibration system to size NPs in a single step. In this setup, microdroplets—which are used as the calibrant to determine elemental sensitivities—and nebulized NP-containing solutions are introduced concurrently into the ICP via a dual-inlet sample introduction system. Because calibrant microdroplets and analyte NPs experience the same plasma conditions, both the microdroplets and the NPs are subjected to the same matrix-related signal enhancement or suppression. In this way, the microdroplet calibration standards are automatically matrix matched with the NP-containing solution. The online microdroplet calibration system is combined with an ICP-TOFMS instrument for simultaneous measurement of multiple elements in microdroplets and NPs. We investigate the ability of online microdroplet calibration to compensate for matrix effects through a series of experiments, in which Ag and Au NPs are measured with variable plasma-sampling positions, varying concentrations of HCl and HNO3, varying concentrations of single element solutions, and high concentrations of a salt matrix, i.e. phosphate buffered saline (PBS). Through these experiments, we demonstrate that the online microdroplet calibration strategy provides a matrix-independent mass quantification of analyte NPs in the presence of several established types of matrix effects, including acid effects, space-charge effects, and ionisation suppression. In results presented here, we focus on the size determination of the NPs. KW - Nanoparticle KW - ICP-MS KW - Calibration PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477589 DO - https://doi.org/10.1039/c8ja00397a SN - 0267-9477 VL - 34 IS - 4 SP - 716 EP - 728 PB - Royal Society of Chemistry CY - London AN - OPUS4-47758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Göbel, M. A1 - Kirsch, S. A1 - Schwarze, L: A1 - Schmidt, L. A1 - Scholz, H. A1 - Haußmann, J. A1 - Klages, M. A1 - Scholta, J. A1 - Markötter, Henning A1 - Alrwashdeh, S. A1 - Manke, I. A1 - Müller, Bernd R. T1 - Transient limiting current measurements for characterization of gas diffusion layers N2 - The water management in proton exchange membrane fuel cells (PEMFC) is strongly influenced by the design of the gas diffusion layers (GDL). Limiting current measurements in small-scale cells operating at high stoichiometries are useful to determine the oxygen transport resistance. The oxygen transport resistance increases, once water condenses inside the GDL. In this study a new electrochemical method for voltage loss estimation of GDL induced oxygen transport losses are presented. This new method, referred to as “transient limiting current” (TLC), is compared with the literature method. TLC allows a direct estimation of oxygen transport resistance at an arbitrarily conditioned state. This study also presents a case study of liquid water visualization of a PEM fuel cell with varying GDLs types. With the help of quasi in-situ synchrotron X-ray computed tomography and time resolved radiography measurements we investigate appearance and distribution of liquid water inside the GDLs under limiting current conditions. KW - In-situ characterization of GDLs KW - In-situ synchrotron X-ray computed tomography KW - In-situ synchrotron X-ray radiography KW - BAMline PY - 2018 DO - https://doi.org/10.1016/j.jpowsour.2018.09.003 SN - 0378-7753 SN - 1873-2755 VL - 402 SP - 237 EP - 245 PB - Elsevier B.V. AN - OPUS4-46552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Senoner, Mathias A1 - Maaßdorf, A. A1 - Rooch, Heidemarie A1 - Österle, Werner A1 - Malcher, M. A1 - Schmidt, M. A1 - Kollmer, F. A1 - Paul, D. A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Unger, Wolfgang T1 - Lateral resolution of nanoscaled images delivered by surface-analytical instruments: application of the BAM-L200 certified reference material and related ISO standards N2 - The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1–xAs and InxGa1–xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface-analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013. KW - AES KW - BAM-L200 KW - CRM KW - EDX KW - Imaging KW - Lateral resolution KW - Sharpness KW - Standardisation KW - STXM KW - ToF-SIMS KW - XPEEM KW - XPS KW - Certified reference material KW - Imaging surface analysis PY - 2015 DO - https://doi.org/10.1007/s00216-014-8135-7 SN - 1618-2642 SN - 1618-2650 VL - 407 IS - 11 SP - 3211 EP - 3217 PB - Springer CY - Berlin AN - OPUS4-33033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Salge, T. A1 - Mielke, Johannes A1 - Ortel, Erik A1 - Schmidt, R. T1 - Characterisation of nanoparticles by means of high-resolution SEM/EDS in transmission mode N2 - Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass – thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS. T2 - European Microbeam Analysis Society’s 14th European Workshop on Modern Developments and Applications in Microbeam Analysis (EMAS 2015) CY - Portorož, Slovenia DA - 03.05.2015 KW - High-resolution KW - SEM KW - T-SEM KW - EDX KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355628 UR - http://iopscience.iop.org/article/10.1088/1757-899X/109/1/012006 DO - https://doi.org/10.1088/1757-899X/109/1/012006 SN - 1757-899X VL - 109 SP - 012006-1 EP - 012006-12 PB - IOP Publishing Ltd CY - Bristol, UK AN - OPUS4-35562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald A1 - Schmidt, Alexandra A1 - Bachmann, V. A1 - Kämpf, K. A1 - Kuhlbusch, T. A1 - Schwirn, K. A1 - Völker, D. ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - OECD Test Guideline on particle size and size distribution of manufactured nanomaterials N2 - The properties of nanomaterials are influenced not only by their chemical composition but also by physical properties (such as size, geometry and crystal structure). For the reliable determination and assessment of behaviour and effects of nanomaterials as well as for the determination of the exposure of humans and environment a comprehensive physical-chemical characterization of nanomaterials is essential. This is an important prerequisite to identify them as nanomaterials and to interpret and compare test results and - in future – to forecast interaction and effects of nanomaterials. In 2006, the OECD launched a sponsorship program for the testing of nanomaterials in which 11 nanomaterials were thoroughly investigated using a variety of methods. The aim of the project was, among other things, to find out where problems occur and where there are gaps in the measurement and test procedures and where are changes required. An important outcome of the sponsorship program was the finding that the OECD Test Guidelines should in several cases be extended to the specific needs in testing of nanomaterials. The existing standardized test methods of the OECD for physical-chemical characterization have not been developed for nanomaterials in particular. A high demand for an extension of the test guidelines was identified. Germany complied with the OECD's request in 2017 and has agreed to extend the “Test Guideline on Particle Size Distribution / Fiber Length and Diameter Distributions Test Guideline” for Manufactured Nanomaterials (MN). UBA commissioned BAM and BAuA with the preparation of the Test Guideline. The aim of the project is the development of a harmonized test protocol for a valid and reproducible determination of particle size and size distribution which is one of the most relevant physical-chemical properties for MNs. Different measuring methods provide different results for the size distribution of the particles. This is caused by the different measuring principles of the methods. Each method measures a specific parameter that ultimately determines particle size. First, the measured quantity differs for each method (Scattered light intensity, 2D image / projection, electric mobility, etc.). Second, the calculated diameters of the MN may differ (Feret Diameter, Area Projection, Mobility Diameter, Aerodynamic Diameter, Hydrodynamic Diameter). Third, a measuring method provides a size distribution which is measured either mass-based, surface-based or number-based. A conversion between the results requires additional parameters and thus possibly increases the measurement error. In addition to the technical differences, the individual parameters are strongly influenced by the structure and material of the nanoparticles. For example, a surface functionalization can lead to very different results in the size distribution. The suitability of measurement methods differs with the material of the MN. As a result, two very different results can be measured for the particle size distribution using two different methods, which are nevertheless both correct. Several large projects in recent years therefore concluded that nanomaterials should be characterized by at least two complementary method. Imaging techniques are regarded as one of these methods for the characterization, the complementary methods are supposed to be statistical methods. The different results for the size distribution of nanomaterials become problematic for the registration of new MN. A comparable and reproducible size distribution is a prerequisite for a standardized registration. In the future, the particle size distribution in the EU will also decide on the classification of a substance as a nanomaterial or as a non-nanomaterial. Especially in borderline cases, a standardized and comparable measurement methodology is therefore essential. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - OECD KW - Guideline KW - Particle size distribution KW - Nano KW - Prüfrichtlinie PY - 2019 SN - 978-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - F-61 SP - 125 EP - 132 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kämpf, K. A1 - Bachmann, V. A1 - Bresch, Harald A1 - Schmidt, Alexandra A1 - Kuhlbusch, T. A1 - Schwirn, K. A1 - Völker, D. ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - OECD Test Guideline on particle size and particle size distribution of manufactured nanomaterials: simultaneous measurement of length and diameter of fibers N2 - The new OECD test guideline will address the following four main steps in the determination of the length and width distributions of fibers: sample preparation, image acquisition, data evaluation and uncertainty analysis. As the sample preparation has to be optimized for each material, general quality criteria will be given in the protocol. For full visibility of a fiber the appropriate resolution has to be chosen. In the data evaluation the length and diameter of each fiber will be determined concurrently to allow for application of different regulatory definitions. The quality of the results critically depends on the sample preparation as well as the data evaluation. In this step the classification rules have to be formulated and followed accurately in order to optimize reproducibility of the method. The SOP will be validated in an international round robin test, which is planned for 2018/2019. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - OECD KW - Nano KW - Guideline KW - Particle size distributuion KW - Prüfrichtlinie PY - 2019 SN - 978-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - F-61 SP - 302 EP - 302 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dayani, Shahabeddin A1 - Markötter, Henning A1 - Schmidt, Anita A1 - Widjaja, Martinus Putra A1 - Bruno, Giovanni T1 - Multi-level X-ray computed tomography (XCT) investigations of commercial lithium-ion batteries from cell to particle level N2 - Adopting X-ray computed tomography (XCT) for ex-situ characterization of battery materials has gained interest in the past decade. The main goal of this paper is to demonstrate the effectiveness of several X-ray computer tomography techniques to study commercial batteries. General guidelines are provided to select the most suitable imaging equipment and parameters for investigations of lithium-ion batteries, spanning the length scales from cell to electrode, down to particle level. Relevantly, such parameters would also be suitable for operando experiments. Safety mechanisms and manufacturing inconsistencies at cell level as well as defects and inhomogeneity in cathode and anode is illustrated and quantified. Furthermore, relation of beam energy and sample-detector-distance on contrast retrieved from attenuation and phase shift is inspected using Synchrotron XCT. KW - Non-destructive testing KW - X-ray computed tomography KW - Synchrotron X-ray computed tomography KW - Lithium-ion battery PY - 2023 DO - https://doi.org/10.1016/j.est.2023.107453 SN - 2352-152X VL - 66 SP - 107453 PB - Elsevier Ltd. AN - OPUS4-57512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Choi, Youngeun A1 - Schmidt, Carsten A1 - Tinnefeld, Philip A1 - Bald, Ilko A1 - Roedinger, Stefan T1 - A new reporter design based on DNA origami nanostructures for quantification of short oligonucleotides using microbeads N2 - The DNA origami technique has great potential for the development of brighter and more sensitive reporters for fluorescence based detection schemes such as a microbead-based assay in diagnostic applications. The nanostructures can be programmed to include multiple dye molecules to enhance the measured signal as well as multiple probe strands to increase the binding strength of the target oligonucleotide to these nanostructures. Here we present a proof-of-concept study to quantify short oligonucleotides by developing a novel DNA origami based reporter system, combined with planar microbead assays. Analysis of the assays using the VideoScan digital imaging platform showed DNA origami to be a more suitable reporter candidate for quantification of the target oligonucleotides at lower concentrations than a conventional reporter that consists of one dye molecule attached to a single stranded DNA. Efforts have been made to conduct multiplexed analysis of different targets as well as to enhance fluorescence signals obtained from the reporters. We therefore believe that the quantification of short oligonucleotides that exist in low copy numbers is achieved in a better way with the DNA origami nanostructures as reporters. KW - Origami KW - Nanostructures KW - Microbeads KW - DNA origami KW - Oligonucleotides PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476443 DO - https://doi.org/10.1038/s41598-019-41136-x SN - 2045-2322 VL - 9 SP - 4769, 1 EP - 8 PB - Nature AN - OPUS4-47644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Salge, T. A1 - Mielke, Johannes A1 - Ortel, Erik A1 - Schmidt, R. T1 - Characterisation of nanoparticles by means of high-resolution SEM/EDS N2 - Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass - thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS. T2 - EMAS 2015 - 14th European workshop on modern developments and applications in microbeam analysis CY - Portoroz, Slovenia DA - 03.05.2015 KW - SEM KW - T-SEM KW - EDX KW - Nanoparticles KW - High-resolution PY - 2015 SN - 978-90-8227-691-6 DO - https://doi.org/10.1088/1757-899X/109/1/012006 SP - NUR code:972 - Materials Science, 187-199 AN - OPUS4-33258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Alexandra A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. KW - Nano KW - Particle size distribution KW - Nanoparticle KW - Nanomaterial KW - OECD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891 DO - https://doi.org/10.3390/nano12132238 SN - 2079-4991 VL - 12 IS - 13 SP - 2238 PB - MDPI CY - Basel AN - OPUS4-55189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schwirn, K. A1 - Völker, D. A1 - Ahtianinen, J. A1 - Schmidt, Alexandra A1 - Bresch, Harald A1 - Kämpf, K. A1 - Bachmann, V. A1 - Kuhlbusch, T. ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - OECD Test Guidelines development for chemicals safety assessment of nanomaterials N2 - The OECD test guidelines (TGs) for testing chemicals have been widely used for regulatory purposes all over the world since the establishment of the Mutual Acceptance of Data (MAD) principle in 1984. This MAD principle ensures that, if a chemical is tested under the Good Laboratory Practice (GLP) conditions accordingly to an OECD TG, the data should be accepted in all OECD countries. The TGs have been developed, harmonized, internationally validated (round robin tests) and adopted by OECD countries to be used for the physical-chemical characterisation, fate estimation, and hazard identification for risk assessment of various chemicals. In addition to the TGs, OECD Guidance Documents (GDs) usually provide guidance on how to use TGs and how to interpret the results. These GDs do not have to be fully experimentally validated, and hence they are not under MAD, but they are based on relevant published scientific research. But are the existing TGs and the related GDs applicable and adequate for the regulatory testing of nanomaterials? In general, for nanomaterials it is accepted that most of the "endpoints" or more precisely measurement variables are applicable. However, for some endpoints new or amended TGs are needed. In addition, several GDs are needed to give more precise advice on the test performance in order to gain regulatory relevant data on nanomaterials. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - OECD KW - Nano KW - Guideline KW - Nanomaterials KW - Prüfrichtlinie PY - 2019 SN - 978-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - F-61 SP - 279 EP - 279 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pellegrino, Francesco A1 - Ortel, Erik A1 - Mielke, Johannes A1 - Schmidt, R. A1 - Maurino, V. A1 - Hodoroaba, Vasile-Dan T1 - Customizing New Titanium Dioxide Nanoparticles with Controlled Particle Size and Shape Distribution: A Feasibility Study Toward Reference Materials for Quality Assurance of Nonspherical Nanoparticle Characterization N2 - An overview is given on the synthesis of TiO2 nanoparticles with well-defined nonspherical shapes (platelet like, bipyramidal, and elongated), with the focus on controlled, reproducible synthesis, as a key requirement for the production of reference materials with homogeneous and stable properties. Particularly with regard to the nanoparticle shapes, there is a high need of certified materials, solely one material of this type being commercially available since a few months (elongated TiO2). Further, measurement approaches with electron microscopy as the golden method to tackle the nanoparticle shape are developed to determine accurately the size and shape distribution for such nonspherical particles. A prerequisite for accurate and easy (i.e., automated) image analysis is the sample preparation, which ideally must ensure a deposition of the nanoparticles from liquid suspension onto a substrate such that the particles do not overlap, are solvent-free, and have a high deposition density. Challenges in the Synthesis of perfectly monodispersed and solvent-free TiO2 nanoparticles of platelet and acicular shapes are highlighted as well as successful measurement approaches on how to extract from 2D projection electron micrographs the most accurate spatial information, that is, true 3D size, for example, of the bipyramidal nanoparticles with different geometrical orientations on a substrate. KW - Nanoparticles KW - Titanium dioxide KW - Reference materials KW - Standardisation KW - Particle size and shape distribution PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538849 DO - https://doi.org/10.1002/adem.202101347 VL - 24 IS - 6 SP - 1 EP - 10 PB - Wiley-VCH AN - OPUS4-53884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Alexandra T1 - OECD test guideline on particle size and size distribution: Comparability of measurement results N2 - OECD-Prüfrichtlinien werden weltweit für regulatorische Zwecke angewandt, da sie eine harmonisierte und über internationale Ringversuche validierte Vorschrift zur Analyse vorgeben. Die bestehende Prüfrichtlinie TG 110 zur Größencharakterisierung von Partikeln und Fasern ist für viele Methoden und Materialklassen nicht geeignet, weswegen es Bedarf an einer Neuentwicklung gibt. Im Fokus der neuen TG steht die reproduzierbare und vergleichbare Anwendung von Methoden zur Bestimmung von Partikelgröße sowie Größenverteilung annährend sphärischer und faserförmiger Nanomaterialien im Bereich 1-1000 nm. Berücksichtigt werden die häufig angewandten Methoden zur Größencharakterisierung mit ihren unterschiedlichen physikalisch-technischen Limitierungen und die Bestimmung unterschiedlicher Durchmesser (hydrodynamischer, Feret…). Weiterhin sind materialspezifische Einflüsse durch die Partikel sowie das Messmedium zu berücksichtigen. Jede der Methoden soll unter Berücksichtigung von ISO-Standards und den materialspezifischen Limitierungen in der neuen Prüfrichtlinie beschrieben und über einen Ringversuch validiert werden. T2 - BAM BfR Workshop CY - Berlin, Germany DA - 21.03.2019 KW - OECD KW - Nanoparticle KW - Particle Size KW - Nano KW - Characterization PY - 2019 AN - OPUS4-47633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Martin T1 - Brand- und Explosionsgefahren beim Umgang mit Metallstäuben N2 - Grundlagen des Brand- und Explosionsschutzes mit Schwerpunkt Metallstäube: - Gefahren - Prinzipien des Explosionschutzes - Ableiten von Schutzmaßnahmen - Bestimmung der Stoffeigenschaften - Umgang mit entsprechenden Datenbanken T2 - DGM Fortbildungsseminar "Metallpulver Erzeugen - Charakterisieren - Anwenden" CY - Universität Bremen, Germany DA - 14.03.2019 KW - Brandschutz KW - Explosionsschutz KW - Sicherheitstechnische Kenngrößen PY - 2019 AN - OPUS4-47948 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Martin A1 - Wu, D. A1 - Berghmans, J. T1 - Spontaneous ignition behaviour of coal dust accumulations: A comparison of extrapolation methods from lab-scale to industrial-scale N2 - Smouldering fires and explosions arising from self-ignition of coal dust deposits represent a serious hazard for human being, environment and industry. It is essential for plant operators to know the conditions (temperature, duration and quantity) at which storage will be safe. In this work, self-ignition behaviour of three bituminous coal dusts in large scales are theoretically studied, based on the experimental data via a standardized hot-basket apparatus. A comprehensive 2-D transient model is developed, using a 2nd-order reaction kinetics considering both coal and oxygen consumptions, to investigate self-ignition parameters of coal dust accumulations. The numerical model shows a less conservative prediction compared with the steady-state methods. The computational self-ignition temperature and ignition delay time show a satisfaction agreement with lab-scale experimental results. In addition, the influences of ambient temperature and moisture content are analysed. The result shows that the moisture content delays the ignition and a small variation of the ambient temperature nearby the critical condition will lead to a large difference of the ignition delay time. KW - Spontanious ignition KW - Self-ignition KW - Extrapolation methods PY - 2019 DO - https://doi.org/10.1016/j.proci.2018.05.140 SN - 1540-7489 VL - 37 IS - 3 SP - 4181 EP - 4191 PB - Elsevier AN - OPUS4-47291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Dirk A1 - T., Heidermann T1 - Ergebnisse der experimentellen Untersuchungen zur Visualisierung der Wirksamkeit von Deflagrationsrohrsicherungen in einer PVC-U Rohrleitung N2 - Deflagrationsrohrsicherungen sind Sicherheitseinrichtungen, die den Durchfluss von brennbaren Gasen und Dämpfen brennbarer Flüssigkeiten ermöglichen, den Flammendurchschlag und eine weitere Explosionsausbreitung nach der Zündung von explosionsfähigen Gas-/Dampf-Luftgemischen jedoch verhindern sollen. Die Einbaubedingungen sind dabei von besonderer Bedeutung für die Wirksamkeit der Deflagrationsrohrsicherungen. Oft lassen sich aus betrieblichen bzw. verfahrenstechnischen Gründen entsprechende Einbaubedingungen nur schwer oder nicht realisieren. So können beispielsweise Rohrleitungsverzweigungen zusätzliche Turbulenzen induzieren und dadurch zu erhöhten Flammenausbreitungsgeschwindigkeiten und Explosionsdrücken und ggf. zum Versagen der Deflagrationsrohrsicherung führen. Neben den „klassischen“ Untersuchungsmethoden dieser Belastungssituationen von Deflagrationsrohrsicherungen, wie die Erfassung des Explosionsdruckes und der Flammenausbreitungsgeschwindigkeiten, werden in diesem Beitrag die Ergebnisse der visuellen Beobachtungen des Reaktionsverlaufes sowie die Belastungen der Flammendurchschlagsicherung bei unterschiedlichen Einbaubedingungen in den Vordergrund gestellt. Gegenübergestellt wird die Belastungssituation der Flammensperre in einer geraden und einer verzweigten Rohrleitung. Verwendet wurde dafür eine speziell gefertigte Deflagrationsrohrsicherung, die eine Beobachtung des Reaktionsverlaufs im Bereich der spiralförmig gewickelten Metallbändern erlaubt. Zusätzlich wurde im geschützten Bereich in der Rohrleitung eine Kamera installiert, die die Belastungssituation bei den einzelnen Versuchen dokumentierte. Die Ergebnisse bestätigen sehr eindrucksvoll, dass die Belastungssituation der Deflagrationsrohrsicherung sich in Abhängigkeit von der Konfiguration der Rohrleitung entscheidend ändert T2 - 15. BAM/PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Brunswick, Germany DA - 21.05.2019 KW - Flammendurchschlagsicherungen KW - Rohrleitungen KW - Deflagrationen PY - 2019 DO - https://doi.org/10.7795/210.20190521A VL - 15. SP - 1 EP - 10 PB - PTB CY - Braunschweig AN - OPUS4-48084 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Dirk T1 - Ergebnisse der experimentellen Untersuchungen zur Visualisierung der Wirksamkeit von Deflagrationsrohrsicherungen in einer PVC-U Rohrleitung N2 - Deflagrationsrohrsicherungen sind Sicherheitseinrichtungen, die den Durchfluss von brennbaren Gasen und Dämpfen brennbarer Flüssigkeiten ermöglichen, den Flammendurchschlag und eine weitere Explosionsausbreitung nach der Zündung von explosionsfähigen Gas-/Dampf-Luftgemischen jedoch verhindern sollen. Die Einbaubedingungen sind dabei von besonderer Bedeutung für die Wirksamkeit der Deflagrationsrohrsicherungen. Oft lassen sich aus betrieblichen bzw. verfahrenstechnischen Gründen entsprechende Einbaubedingungen nur schwer oder nicht realisieren. So können beispielsweise Rohrleitungsverzweigungen zusätzliche Turbulenzen induzieren und dadurch zu erhöhten Flammenausbreitungsgeschwindigkeiten und Explosionsdrücken und ggf. zum Versagen der Deflagrationsrohrsicherung führen. Neben den „klassischen“ Untersuchungsmethoden dieser Belastungssituationen von Deflagrationsrohrsicherungen, wie die Erfassung des Explosionsdruckes und der Flammenausbreitungsgeschwindigkeiten, werden in diesem Beitrag die Ergebnisse der visuellen Beobachtungen des Reaktionsverlaufes sowie die Belastungen der Flammendurchschlagsicherung bei unterschiedlichen Einbaubedingungen in den Vordergrund gestellt. Gegenübergestellt wird die Belastungssituation der Flammensperre in einer geraden und einer verzweigten Rohrleitung. Verwendet wurde dafür eine speziell gefertigte Deflagrationsrohrsicherung, die eine Beobachtung des Reaktionsverlaufs im Bereich der spiralförmig gewickelten Metallbändern erlaubt. Zusätzlich wurde im geschützten Bereich in der Rohrleitung eine Kamera installiert, die die Belastungssituation bei den einzelnen Versuchen dokumentierte. Die Ergebnisse bestätigen sehr eindrucksvoll, dass die Belastungssituation der Deflagrationsrohrsicherung sich in Abhängigkeit von der Konfiguration der Rohrleitung entscheidend ändert. T2 - 15. BAM/PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Brunswick, Germany DA - 21.05.2019 KW - Flammendurchschlagsicherungen KW - Rohrleitungen KW - Deflagrationen PY - 2019 AN - OPUS4-48085 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Anita T1 - Alles über Lithiumbatterien (I) N2 - Der Auftakt der Artikelserie beschäftigt sich mit den neuen Verpackungsvorschriften für defekte Lithiumbatterien, die beim Transport gefährlich reagieren können. Die Antworten auf die wichtigsten Fragestellungen. KW - Gefahrgutverpackungen KW - Lithiumbatterien KW - Gefahrgut KW - ADR PY - 2019 SN - 0016-5808 VL - 2019 IS - 06 SP - 20 EP - 23 PB - Storck Verlag CY - Hamburg AN - OPUS4-50800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Aktuelle Forschung - Technik für sichere Gefahrguttransporte N2 - Lithiumbatterien, Tanks und Druckgasflaschen: Ihnen ist gemeinsam, dass Gefahrguttransporte mit Ihnen sicher erfolgen müssen. Um dies zu gewährleisten, führt die BAM verschiedene Untersuchungen und Forschungsvorhaben durch. T2 - 35. Internationale Gefahrgut-Tage Hamburg CY - Hamburg, Germany DA - 17.02.2019 KW - Lithiumbatterien KW - Druckgefäße KW - Gefahrguttransport KW - ADR KW - Sicherheit PY - 2019 AN - OPUS4-50802 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Aktuelles zur Sicherheit von Lithium-Ionen Akkus - Lagerung, Transporte, Brandschutzkonzepte N2 - Sicherheitskonzepte werden für die verschiedenen Szenarien für Lithiumakkus benötigt: Vor allem für den Bereich der Lagerung gibt es im Moment nur wenige Vorgaben. Im Vortrag werden verschiedene Brandschutzkonzepte vorgestellt. Für die Lagerung werden Empfehlungen ausgesprochen, die teilweise an die Vorgaben der Transportvorschriften anknüpfen. T2 - Forum 2019 zur Schadenverhütung der Arbeitsgemeinschaft Berlin Brandenburg (AGS) und AGBB Berlin e.V. CY - Berlin, Germany DA - 23.10.2019 KW - Lithiumbatterien KW - Brandschutzkonzepte KW - Lagerung KW - Gefahrguttransport PY - 2019 AN - OPUS4-50807 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Zulassungsregeln für Verpackungen von Lithiumbatterien N2 - Sicherer Transport defekter Batterien im Aufgabenbereich der BAM. T2 - 12. Fachkonferenz Lithiumbatterien CY - Frankfurt a.M., Germany DA - 21.01.2019 KW - Lithiumbatterien KW - ADR KW - Gefahrguttransport PY - 2019 AN - OPUS4-50803 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - New ADR regulations for critical lithium batteries N2 - End of life batteries may be damaged or defective and may cause the risk of dangerous reactions. New ADR regulations allow them nevertheless to be tansported with the specifications of the national competent authority. BAM's approach. T2 - End-of-Life Batteries from Electrified Vehicles CY - Fredrikstad Oslo, Norway DA - 13.06.2019 KW - Dangerous goods KW - Defective Lithium batteries KW - ADR KW - Transport PY - 2019 AN - OPUS4-50801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Martin A1 - Erdt, René A1 - Gödde, M. A1 - Salg, S. A1 - Ittemann, L. T1 - Selbstentzündungsverhalten von Feststoffen: Validierung der Extrapolation von Labortests mit Hilfe halbtechnischer Versuche bis 1 m³ N2 - Vorgestellt wird ein 2018 gestartetes Projekt zur Überprüfung der Extrapolation von im Labormaßstab ermittelten Selbstentzündungstemperaturen auf technisch relevante Volumina. Für die Ermittlung reaktionskinetischer Daten von Feststoffschüttungen stehen eine Reihe von Untersuchungsmethoden zur Verfügung. Dies sind thermische Analysen wie z.B. die differential scanning calorimetry DSC sowie Mikrokalorimetrie zur hochgenauen Messung von Wärmeströmen, bei denen sehr geringe Probenmengen zum Einsatz kommen. In der Regel wird das Selbstentzündungsverhalten jedoch mit Hilfe von isoperibolen oder adiabaten Warmlagerungsversuchen beurteilt, hier liegen die Probenvolumina üblicherweise im Bereich von ca. 100 cm³ bis zu einigen Litern. Die Extrapolation über mehrere Größenordnungen auf technische Volumina birgt Unsicherheiten, da mit Zunahme des Lagervolumens veränderte Start- und Randbedingungen vorliegen können. Zudem besteht die Möglichkeit, dass bei in technischen Lagern vorherrschenden niedrigen Temperaturen Reaktionen ablaufen, die in Standard- Laborversuchen nicht erfasst werden aber einen wesentlichen Einfluss auf das Selbstentzündungsverhalten aufweisen können. Hauptziel des Projektes ist es daher, die im Labormaßstab vorhandenen Prüfeinrichtungen durch einen Versuchsstand zur Untersuchung von Probengrößen von bis zu 1000 dm³ zu erweitern, die Eignung (oder Nichteignung) der etablierten Methoden nachzuweisen und im Labormaßstab nicht erfassbare Einflussgrößen zu ermitteln. Zudem sollen anhand der kleinskaligen Tests Entscheidungskriterien abgeleitet werden, ob eine Extrapolation nach den derzeit üblichen Methoden zulässig ist. T2 - 15. BAM-PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Brunswick, Germany DA - 21.05.2019 KW - Spontanious ignition KW - Self-ignition KW - Minimum ignition temperature KW - Dust layers KW - Große Volumina KW - Explosionsschutz KW - Selbstentzündung KW - DSC PY - 2019 DO - https://doi.org/10.7795/210.20190521B SP - 1 EP - 15 PB - Physikalisch-Technische Bundesanstalt (PTB) AN - OPUS4-48939 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, X. A1 - Schmidt, Franziska A1 - Gurlo, A. T1 - Fabrication of polymer-derived ceramics with hierarchical porosities by freeze casting assisted by thiol-ene click chemistry and HF etching N2 - The freeze casting technique assisted with cryo thiol-ene photopolymerization is successfully employed for the fabrication of macroporous polymer-derived silicon oxycarbide with highly aligned porosity. It is demonstrated that the free radical initiated thiol-ene click reaction effectively cross-linked the vinyl-containing liquid polysiloxanes into infusible thermosets even at low temperatures. Furthermore, mixed solution- and suspension-based freeze casting is employed by adding silica nanopowders. SiOC/SiO2 foams with almost perfect cylindrical shapes are obtained, demonstrating that the presence of nano-SiO2 does not restrict the complete photoinduced cross-linking. The post-pyrolysis HF acid treatments of produced SiOC monoliths yields hierarchical porosities, with SiOC/SiO2 nanocomposites after etching demonstrating the highest specific surface area of 494 m2/g and pore sizes across the macro-, meso- and micropores ranges. The newly developed approach gives a versatile solution for the fabrication of bulk polymer-derived ceramics with controlled porosity. KW - Freeze casting KW - Preceramic polymer KW - Hierarchical porosities KW - Thiol-ene click chemistry KW - Frozen state photopolymerization PY - 2019 DO - https://doi.org/10.1016/j.jeurceramsoc.2019.09.038 SN - 0955-2219 VL - 40 IS - 2 SP - 315 EP - 323 PB - Elsevier AN - OPUS4-49172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Melzer, Michael A1 - Makarov, D. A1 - Schmidt, O. G. T1 - A review on stretchable magnetic field sensorics N2 - The current establishment of stretchable electronics to form a seamless link between soft or even living materials and the digital world is at the forefront of multidisciplinary research efforts, bridging physics, engineering and materials science. Magnetic functionalities can provide a sense of displacement, orientation or proximity to this novel formulation of electronics. This work reviews the recent development of stretchable magnetic field sensorics relying on the combination of metallic thin films revealing a giant magnetoresistance effect with elastomeric materials. Stretchability of the magnetic nanomembranes is achieved by specific morphologic features (e.g. wrinkles or microcracks), which accommodate the applied tensile deformation while maintaining the electrical and magnetic integrity of the sensor device. The entire development, from the demonstration of the world’s first elastically stretchable magnetic sensor to the realization of a technology platform for robust, ready-to-use elastic magnetosensorics is described. Soft giant magnetoresistive elements exhibiting the same sensing performance as on conventional rigid supports, but with fully strain invariant properties up to 270% stretching have been demonstrated. With their unique mechanical properties, these sensor elements readily conform to ubiquitous objects of arbitrary shapes including the human skin. Stretchable magnetoelectronic sensors can equip soft and epidermal electronic systems with navigation, orientation, motion tracking and touchless control capabilities. A variety of novel technologies, like electronic skins, smart textiles, soft robotics and actuators, active medical implants and soft consumer electronics will benefit from these new magnetic functionalities. KW - Stretchable electronics KW - Giant magnetoresistance KW - Magnetic sensors KW - Magnetic thin films PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502049 DO - https://doi.org/10.1088/1361-6463/ab52cf SN - 0022-3727 (Druck) SN - 1361-6463 (Web) VL - 53 IS - 8 SP - Paper 083002, 34 PB - IOP Publishing AN - OPUS4-50204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gili, A. A1 - Bischoff, B. A1 - Simon, U. A1 - Schmidt, Franziska A1 - Kober, D. A1 - Görke, O. A1 - Bekheet, M. A1 - Gurlo, A. T1 - Ceria-based dual-phase membranes for high-temperature Carbon dioxide separation: Effect of iron doping and pore generation with MgO template N2 - Dual-phase membranes for high-temperature carbon dioxide Separation have emerged as promising technology to mitigate anthropogenic greenhouse gases emissions, especially as a pre- and post-combustion separation technique in coal burning power plants. To implement These membranes industrially, the carbon dioxide permeability must be improved. In this study, Ce_(0.8) Sm_(0.2) O_(2-d) (SDC) and Ce_(0.8)Sm_(0.19)Fe_(0.01)O_(2-d) (FSDC) ceramic powders were used to form the skeleton in dual-Phase membranes. The use of MgO as an environmentally friendly pore generator allows control over the membrane porosity and microstructure in order to compare the effect of the membrane’s ceramic phase. The ceramic powders and the resulting membranes were characterized using ICP-OES, HSM, gravimetric analysis, SEM/EDX, and XRD, and the carbon dioxide flux density was quantified using a high-temperature membrane permeation setup. The carbon dioxide permeability slightly increases with the addition of iron in the FSDC membranes compared to the SDC membranes mainly due to the reported scavenging effect of iron with the siliceous impurities, with an additional potential contribution of an increased crystallite size due to viscous flow sintering. The increased permeability of the FSDC system and the proper microstructure control by MgO can be further extended to optimize carbon dioxide permeability in this membrane system. KW - Samarium doped ceria KW - SDC KW - FSDC KW - CO2 separation membranes KW - Scavenging effect of iron KW - Permeability PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488612 DO - https://doi.org/10.3390/membranes9090108 SN - 2077-0375 VL - 9 IS - 9 SP - 108, 1 EP - 15 PB - MDPI AN - OPUS4-48861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lüth, Peter A1 - Frost, K. A1 - Kurth, Lutz A1 - Malow, Marcus A1 - Schmidt, Martin A1 - Michael-Schulz, Heike A1 - Uhlig, S. A1 - Zakel, S. T1 - CEQAT-DGHS Ringversuchsprogramm für die Chemikaliensicherheit - Schlussfolgerungen N2 - Die Ursachen für Chemikalienunfälle können vielfältig sein. Prävention beginnt bereits im Prüflabor, wenn Chemikalien auf ihre gefährlichen Eigenschaften getestet werden. Dazu sind Prüfmethoden entwickelt und veröffentlicht worden, die heute weltweit Anwendung finden. Auf die Validität der Prüfmethode und richtige Durchführung der Prüfung im Laboratorium müssen sich Sicherheitsfachkräfte, Transporteure oder Händler verlassen können. Anhand der in den letzten 10 Jahren im Rahmen des CEQAT-DGHS von BAM und PTB durchgeführten Ringversuche (RV) wird gezeigt, dass bei allen bisher untersuchten Prüfmethoden ein Verbesserungsbedarf besteht. Die RV müssen daher zunächst auf die Methodenverbesserung und -validierung abzielen und nicht auf Leistungstests. Das Labormanagement und die praktische Durchführung der Prüfung sind in vielen Laboratorien verbesserungsbedürftig. Der Begriff „Erfahrung der Prüfer“ ist kritisch zu sehen: Eine „lange Erfahrung mit vielen Prüfungen“ ist nicht unbedingt ein Garant für richtige Ergebnisse. T2 - 15. BAM-PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Braunschweig, Germany DA - 21.05.2019 KW - Gefahrgut KW - Gefahrstoff KW - Ringversuch KW - Prüfmethode KW - Validierung KW - Qualitätssicherung PY - 2019 UR - https://www.ptb.de/cms/index.php?id=18763 DO - https://doi.org/10.7795/210.20190521M SP - 1 EP - 8 PB - Physikalisch-Technische Bundesanstalt (PTB) CY - Braunschweig AN - OPUS4-49489 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lüth, Peter A1 - Frost, K. A1 - Kurth, Lutz A1 - Malow, Marcus A1 - Schmidt, Martin A1 - Michael-Schulz, Heike A1 - Uhlig, S. A1 - Zakel, S. T1 - CEQAT-DGHS Ringversuchsprogramm für die Chemikaliensicherheit – Entwicklung von Verfahren zur Verifizierung der Prüfapparatur am Beispiel der Prüfmethode UN Test N.5 N2 - Prävention beginnt im Prüflabor, wenn Chemikalien auf ihre gefährlichen Eigenschaften getestet werden. Dazu sind Prüfmethoden entwickelt und veröffentlicht worden, die heute weltweit Anwendung finden. Auf die Validität der Prüfmethode und richtige Durchführung der Prüfung im Laboratorium müssen sich Sicherheitsfachkräfte, Transporteure oder Händler verlassen können. Anhand der in den letzten 10 Jahren im Rahmen des CEQAT-DGHS von BAM und PTB durchgeführten Ringversuche (RV) wird gezeigt, dass bei allen bisher untersuchten Prüfmethoden ein Verbesserungsbedarf besteht. Die RV müssen daher zunächst auf die Methodenverbesserung und -validierung abzielen und nicht auf Leistungstests. Das Labormanagement und die praktische Durchführung der Prüfung sind in vielen Laboratorien verbesserungsbedürftig. Der Begriff „Erfahrung der Prüfer“ ist kritisch zu sehen: Eine „lange Erfahrung mit vielen Prüfungen“ ist nicht unbedingt ein Garant für richtige Ergebnisse. Bei der Prüfung der gefährlichen Eigenschaften von Chemikalien sind Referenzmaterialen auf Grund der Instabilität in der Regel nicht verfügbar. Für Prüflaboratorien sind RV daher eine Alternative bei der Qualitätssicherung. RV sind jedoch aufwendig und können nur in relativ großen Zeitabständen durchgeführt werden. Es sind deshalb Verfahren zur Verifizierung z. B. der in den Laboratorien verwendeten Prüfapparaturen zu entwickeln. Die Entwicklung von Verifizierungsverfahren wird am Bespiel der Prüfmethode UN Test N.5 demonstriert. T2 - 15. BAM-PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Braunschweig, Germany DA - 21.05.2019 KW - Gefahrgut KW - Gefahrstoff KW - Ringversuch KW - Prüfmethode KW - Validierung KW - Qualitätssicherung KW - Verifizierung PY - 2019 UR - https://www.ptb.de/cms/index.php?id=18763 DO - https://doi.org/10.7795/210.20190521E SP - 1 EP - 10 CY - Braunschweig AN - OPUS4-49495 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüth, Peter A1 - Frost, K. A1 - Kurth, Lutz A1 - Malow, Marcus A1 - Michael-Schulz, Heike A1 - Schmidt, Martin A1 - Schulte, Petra A1 - Uhlig, S. A1 - Zakel, S. T1 - CEQAT-DGHS Interlaboratory Test Programme for Chemical Safety - Need of Test Methods Validation N2 - Safety experts, manufacturers, suppliers, importers, employers or consumers must be able to rely on the validity of safety-related test methods and on correct test results and assessments in the laboratory. Via the eChemPortal lots of data from the REACH registration dossiers are available. However, the quality and correctness of the information remains in the responsibility of the data submitter. Unfortunately, we found more or less appropriate information on physicochemical properties and concluded that more quality or adequacy of any data submitted will be needed. Interlaboratory tests play a decisive role in assessing the reliability of test results. Interlaboratory tests on different test methods have been performed by Bundesanstalt für Materialforschung und –prüfung (BAM) and Physikalisch-Technische Bundesanstalt (PTB) in collaboration with the QuoData GmbH during the last 10 years. Significant differences between the results of the participating laboratories were observed in all interlaboratory tests. The deviations of the test results were not caused only by laboratory faults but also by deficiencies of the test method. In view of the interlaboratory test results the following conclusions can be drawn: • To avoid any discrepancy on classification and labelling of chemicals it should become state of the art to use validated test methods and the results accompanied by the measurement uncertainty. • A need for improvement is demonstrated for all examined test methods. Thus, interlaboratory tests shall initially aim at the development, improvement and validation of the test methods and not on proficiency tests. • The laboratory management and the practical execution of the tests need to be improved in many laboratories. • The term "experience of the examiner" must be seen critically: A "long experience with many tests" is not necessarily a guarantee for correct results. T2 - 16th International Symposium on Loss Prevention and Safety Promotion in the Process Industries and accompanying exhibition. Loss prevention 2019 CY - Delft, The Netherlands DA - 16.06.2019 KW - Dangerous goods KW - Hazardous substances KW - Round robin test KW - Interlaboratory comparison KW - Test method KW - Validation KW - Quality assurance PY - 2019 UR - https://www.aidic.it/cet/19/77/001.pdf SN - 978-88-95608-74-7 DO - https://doi.org/10.3303/CET1977001 SN - 2283-9216 VL - 77 SP - 1 EP - 6 PB - Italian Association of Chemical Engineering AN - OPUS4-49496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Martin T1 - CEQAT-DGHS Interlaboratory Test Programme for Chemical Safety - Need of Test Methods Validation - N2 - Safety experts, manufacturers, suppliers, importers, employers or consumers must be able to rely on the validity of safety-related test methods and on correct test results and assessments in the laboratory. Via the eChemPortal lots of data from the REACH registration dossiers are available. However, the quality and correctness of the information remains in the responsibility of the data submitter. Unfortunately, we found more or less appropriate information on physicochemical properties and concluded that more quality or adequacy of any data submitted will be needed. Interlaboratory tests play a decisive role in assessing the reliability of test results. Interlaboratory tests on different test methods have been performed by Bundesanstalt für Materialforschung und –prüfung (BAM) and Physikalisch-Technische Bundesanstalt (PTB) in collaboration with the QuoData GmbH during the last 10 years. Significant differences between the results of the participating laboratories were observed in all interlaboratory tests. The deviations of the test results were not caused only by laboratory faults but also by deficiencies of the test method. In view of the interlaboratory test results the following conclusions can be drawn: • To avoid any discrepancy on classification and labelling of chemicals it should become state of the art to use validated test methods and the results accompanied by the measurement uncertainty. • A need for improvement is demonstrated for all examined test methods. Thus, interlaboratory tests shall initially aim at the development, improvement and validation of the test methods and not on proficiency tests. • The laboratory management and the practical execution of the tests need to be improved in many laboratories. • The term "experience of the examiner" must be seen critically: A "long experience with many tests" is not necessarily a guarantee for correct results. T2 - 16th International Symposium on Loss Prevention and Safety Promotion in the Process Industrie CY - Delft, Netherlands DA - 16.06.2019 KW - Gefahrgut KW - Gefahrstoff KW - Ringversuch KW - Validierung KW - Qualitätssicherung KW - Prüfmethode PY - 2019 AN - OPUS4-49568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zakel, S. A1 - Schröder, Volkmar A1 - Askar, Enis A1 - Gabel, D. A1 - Hirsch, W. A1 - Kleinert, J. A1 - Krause, U. A1 - Krietsch, Arne A1 - Meistes, J. A1 - Sachtleben, A. A1 - Schmidt, Martin T1 - Sicherheitstechnische Kenngrößen des Explosionsschutzes von hybriden Stoffgemischen - Normungsfähige Bestimmungsverfahren N2 - In diesem Verbundvorhaben werden standardisierte Messverfahren für hybride Gemische erarbeitet, die der Bestimmung sicherheitstechnischer Kenngrößen des Explosionsschutzes dienen. Unter einem hybriden Gemisch wird dabei ein mehrphasiges System aus Brenngas oder brennbarem Dampf, sowie Luft und brennbarem Staub verstanden. Die Veröffentlichung der Ergebnisse erfolgt in einem Abschlussbericht und als DIN-Spezifikation (DIN SPEC). Diese DIN SPEC versetzt Prüfinstitute und Industrie in die Lage, Explosionsgefahren beim Betrieb technischer Anlagen mit hybriden Gemischen einzuschätzen und damit Prozesse sowohl sicherer als auch effizienter zu steuern. Dieses Projekt wird im Rahmen des WIPANOProgramms (Wissens- und Technologietransfer durch Patente und Normen) vom BMWi gefördert. T2 - 14. Fachtagung Anlagen-, Arbeits- und Umweltsicherheit CY - Köthen, Germany DA - 07.11.2019 KW - Explosionsschutz KW - Sicherheitstechnische Kenngrößen KW - Hybride Gemische KW - Normung PY - 2019 SN - 978-3-89746-220-5 SP - 73 CY - Frankfurt am Main AN - OPUS4-49954 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieder, Philipp A1 - Petrich, Lukas A1 - Serrano-Munoz, Itziar A1 - Fernández, Ricardo A1 - Bruno, Giovanni A1 - Schmidt, Volker T1 - Statistical Comparison of Substructures in Pure Aluminum Before and After Creep Deformation, Based on EBSD Image Data N2 - Electron backscatter diffraction (EBSD) images of extruded pure aluminum were statistically analyzed to investigate creep-induced subgrain structures after applying two different levels of creep stress, corresponding to the power law (PL) and power-law breakdown (PLB) regimes. Kernel average misorientation analysis of EBSD measurements revealed 2D morphologies, which were subdivided by a multi-step segmentation procedure into subgranular arrangements. Various descriptors were employed to characterize the “subgrains” quantitatively, including their size, shape, spatial arrangement, and crystallographic orientation. In particular, the analysis of the orientations of subgrains was conducted by neglecting rotations around the loading axis. This approach facilitated the individual investigation of the {001} and {111} subgrain families with respect to the loading axis for two investigated stress levels plus a reference specimen. For the PL regime, the statistical analysis of subgrain descriptors computed from segmented image data revealed a similar degree of strain accumulation for {111} and {001} subgrains. In contrast, for the PLB regime, the analyzed descriptors indicate that {111} subgrains tend to accumulate significantly more strain than {001} ones. These observations suggest that the mechanisms leading to PLB may be associated with strain localization dependent on intergranular stress, hindering the recovery process within {111} grains. KW - Crystallographic descriptor KW - Dislocation-climb-controlled creep KW - Electron backscatter diffraction (EBSD) KW - Geometric descriptor KW - Ernel average misorientation (KAM) KW - pure aluminum KW - Qquantification and segmentation KW - Statistical image analysis KW - subgrain PY - 2023 DO - https://doi.org/10.1093/micmic/ozad121 SN - 1431-9276 SP - 1 EP - 12 PB - Oxford University Press AN - OPUS4-58730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieder, Philipp A1 - Petrich, Lukas A1 - Serrano-Munoz, Itziar A1 - Mouiya, Mossaab A1 - Markötter, Henning A1 - Huger, Marc A1 - Bruno, Giovanni A1 - Schmidt, Volker T1 - Statistical analysis of grains and pores within polycrystalline Al2TiO5 ceramics, based on X-ray computed tomography N2 - Advanced statistical image analysis workflows were developed to segment and quantitatively evaluate 2D electron-backscatter diffraction (EBSD) maps and 3D synchrotron X-ray computed tomography (SXCT) volumes of a polycrystalline Al2TiO5 refractory composite that contains microcracks and pores. Several size, shape, and further geometric descriptors were determined for both the solid phase (Al2TiO5 grains) and the pore space. The resulting pore-size distribution is distinctly bimodal: coarse pores (tens to hundreds of micrometers), traced to incomplete powder compaction, coexist with fine pores generated during sintering. The two pore populations appear to be correlated with grain growth and crystallographic orientation in different ways. Finally, the descriptors obtained from the 2D EBSD and 3D SXCT data sets are internally consistent but complementary, highlighting the value of characterizations based on EBSD and SXCT in the microstructural study of refractory ceramics. KW - Synchrotron X-ray computed tomography KW - Electron-backscatter diffraction KW - Aluminum titanate KW - Morphological reconstruction KW - Image Segmentation KW - Statistical image analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643918 DO - https://doi.org/10.1016/j.matchar.2025.115602 SN - 1044-5803 VL - 229 SP - 1 EP - 13 PB - Elsevier Inc. AN - OPUS4-64391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfaff, Jonas A1 - Schopferer, Sebastian A1 - Markötter, Henning A1 - Rack, Alexander A1 - Bruno, Giovanni A1 - Schmidt, Anita A1 - Tichter, Tim A1 - Böttcher, Nils T1 - High-speed synchrotron radiography of nail penetration-induced thermal runaway: Understanding the explosive behavior of commercial sodium-ion batteries with NFM cathode N2 - The dynamics of mechanically initiated thermal runaway (TR) events in cylindrical 18650 cells with NFM (Na(Ni1/3Fe1/3Mn1/3)O2), LFP (LiFePO4), and NMC532 (LiNi1/2Mn1/3Co1/5O2) cathode chemistries were investigated using high-speed synchrotron X-ray imaging. Structural similarity index measures (SSIM) were employed to identify and track rapid structural changes. In this manner, thermal decompositions and internal propagation dynamics, influencing the safety mechanisms of the cells, were studied. This lead to two major findings: (I) Among NFM, LFP, and NMC532 cells, the TR-characteristics differ significantly in temperature and internal propagation speed. Internal safety mechanisms appear, however, visually similar. Among all samples, LFP cells exhibit higher safety performance concerning the initiation of TR by nail penetration and the progression of TR. (II) The NFM cells used in this study displayed an almost explosive TR. This finding appears counterintuitive on a first glance, since sodium-ion batteries are usually considered safe. High-speed imaging revealed that the explosive TR is not necessarily caused by the thermochemical decomposition reactions, but rather by a failure of the venting mechanism. This results in a significant pressure buildup within the cell upon TR initiation and eventually a severely violent TR. These results underline that battery safety depends on many factors and not solely on optimized cell chemistries or materials. KW - High-speed X-ray radiography KW - Synchrotron X-rays KW - 18650 KW - SIB KW - Na-NFM KW - Structure similarity index measure PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642649 DO - https://doi.org/10.1016/j.powera.2025.100188 SN - 2666-2485 VL - 36 SP - 1 EP - 7 PB - Elsevier Ltd. AN - OPUS4-64264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tötzke, C. A1 - Gaiselmann, G. A1 - Osenberg, M. A1 - Bohner, J. A1 - Arlt, Tobias A1 - Markötter, Henning A1 - Hilger, A. A1 - Wieder, F. A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. A1 - Banhart, J. A1 - Schmidt, V. A1 - Lehnert, W. A1 - Manke, I. T1 - Three-dimensional study of compressed gas diffusion layers using synchrotron X-ray imaging N2 - We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets. KW - Synchrotron X-ray tomography KW - Gas diffusion layer (GDL) KW - Microstructure KW - Water transport path KW - Pore size analysis KW - Geometrical tortuosity PY - 2014 DO - https://doi.org/10.1016/j.jpowsour.2013.12.062 SN - 0378-7753 VL - 253 SP - 123 EP - 131 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-29979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kim, K.J. A1 - Unger, Wolfgang A1 - Kim, J.W. A1 - Moon, D.W. A1 - Gross, Thomas A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Dieter A1 - Wirth, Thomas A1 - Jordaan, W. A1 - van Staden, M. A1 - Prins, S. A1 - Zhang, L. A1 - Fujimoto, T. A1 - Song, X.P. A1 - Wang, H. T1 - Inter-laboratory comparison: quantitative surface analysis of thin Fe-Ni alloy films N2 - An international interlaboratory comparison of the measurement capabilities of four National Metrology Institutes (NMIs) and one Designated Institute (DI) in the determination of the chemical composition of thin Fe-Ni alloy films was conducted via a key comparison (K-67) of the Surface Analysis Working Group of the Consultative Committee for Amount of Substance. This comparison was made using XPS (four laboratories) and AES (one laboratory) measurements. The uncertainty budget of the measured chemical composition of a thin alloy film was dominated by the uncertainty of the certified composition of a reference specimen which had been determined by inductively coupled plasma mass spectrometry using the isotope dilution method. Pilot study P-98 showed that the quantification using relative sensitivity factors (RSFs) of Fe and Ni derived from an alloy reference sample results in much more accurate result in comparison to an approach using RSFs derived from pure Fe and Ni films. The individual expanded uncertainties of the participants in the K-67 comparison were found to be between 2.88 and 3.40 atomic %. The uncertainty of the key comparison reference value (KCRV) calculated from individual standard deviations and a coverage factor (k) of 2 was 1.23 atomic %. KW - Quantification KW - Fe-Ni alloy KW - Uncertainty KW - Key comparison KW - Traceability PY - 2012 DO - https://doi.org/10.1002/sia.3795 SN - 0142-2421 SN - 1096-9918 VL - 44 IS - 2 SP - 192 EP - 199 PB - Wiley CY - Chichester AN - OPUS4-24505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tötzke, C. A1 - Gaiselmann, G. A1 - Osenberg, M. A1 - Arlt, Tobias A1 - Markötter, Henning A1 - Hilger, A. A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Schmidt, V. A1 - Lehnert, W. A1 - Manke, I. T1 - Influence of hydrophobic treatment on the structure of compressed gas diffusion layers N2 - Carbon fiber based felt materials are widely used as gas diffusion layer (GDL) in fuel cells. Their transport properties can be adjusted by adding hydrophobic agents such as polytetrafluoroethylene (PTFE). We present a synchrotron X-ray tomographic study on the felt material Freudenberg H2315 with different PTFE finishing. In this study, we analyze changes in microstructure and shape of GDLs at increasing degree of compression which are related to their specific PTFE load. A dedicated compression device mimicking the channel-land pattern of the flowfield is used to reproduce the inhomogeneous compression found in a fuel cell. Transport relevant geometrical parameters such as porosity, pore size distribution and geometric tortuosity are calculated and consequences for media transport discussed. PTFE finishing results in a marked change of shape of compressed GDLs: surface is smoothed and the invasion of GDL fibers into the flow field channel strongly mitigated. Furthermore, the PTFE impacts the microstructure of the compressed GDL. The number of available wide transport paths is significantly increased as compared to the untreated material. These changes improve the transport capacity liquid water through the GDL and promote the discharge of liquid water droplets from the cell. KW - Gas diffusion layer KW - Synchrotron Tomography KW - Compression KW - Hydrophobic treatment KW - Water transport PY - 2016 DO - https://doi.org/10.1016/j.jpowsour.2016.05.118 SN - 0378-7753 VL - 324 SP - 625 EP - 636 PB - Elsevier CY - Amsterdam AN - OPUS4-36918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jankuj, Vojtech A1 - Skrinsky, Jan A1 - Krietsch, Arne A1 - Schmidt, Martin A1 - Krause, Ulrich A1 - Kuracina, Richard A1 - Szabová, Zuzana A1 - Spitzer, Stefan T1 - Simplifying standards, opening restrictions Part I: The influence of the test vessel volume on the maximum explosion pressure of dusts N2 - Explosion characteristics are widely used in the process industries to determine the potential hazard of the used substances. In the American and European standards for determination of the maximum explosion pressure of dusts, the measured pressure is corrected if the tests are conducted in the 20L-sphere. This correction formula increases the measured values if they are above 5.5 bar g. It also causes, that the only two volumes for testing that are used are the standard 1m³ and the 20L-sphere because it is unclear whether corrections are necessary and, if so, what correction should be applied at other volumes. In this article explosion tests were performed with four different dusts, lycopodium, lignite, aluminum, and nitrocellulose, in four different vessel sizes: 20 L, 250 L, 365 L, and 1000 L to investigate the influence of the vessel size. KW - Explosion protection KW - Dusts KW - Pressure rise KW - Ignition PY - 2025 DO - https://doi.org/10.1016/j.jlp.2025.105556 VL - 94 SP - 1 EP - 7 PB - Elsevier Ltd. AN - OPUS4-62522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Eine sichere Zukunft für Lithium-Ionen Batterien N2 - Eine sichere Zukunft hat eine Technologie dann, wenn sie die Gesellschaft auch von ihrer Sicherheit überzeugen kann. Dies ist insbesondere für Lithiumbatterien von hoher Bedeutung. Die BAM trägt auf den verschiedene Ebenen auf vielfältige Art und Weise dazu bei, diese Sicherheit zu untersuchen und zu verbessern. T2 - 4. Batterieforum Berlin Brandenburg CY - Potsdam, Germany DA - 22.11.2024 KW - LIthiumbatterien KW - Sicherheit PY - 2024 AN - OPUS4-62328 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Spitzer, Stefan A1 - Pandal, Adrián A1 - Rodríguez, Manuel Velasco A1 - Schmidt, Martin A1 - Danzi, Enrico A1 - Dufaud, Olivier A1 - Janovsky, Bretislav T1 - Investigations on different distribution systems for dusts inside the 20L-sphere N2 - The determination of several safety characteristics for dusts requires the dispersion of it in air. This is normally conducted using two vessels, one with an overpressure holding the dust and dispersing it into the second one, where the explosion takes place, through a nozzle. This procedure has the disadvantage that some dusts cannot be conveyed through the nozzle properly. Another disadvantage is that the pressure balancing between the two vessels depends on the dust loading and especially for heavy dusts and high loadings the initial pressure inside the explosion vessel might be reduced. Flocky dusts or dusts that might be dangerous to convey through a thin nozzle with an overpressure (nano powders, zirconium) are also difficult to test according to the existing standards and may not be tested with the standard nozzles, that are so far used for the determination of safety characteristics. One very recent example, testing nitrocellulose, raised the question, whether some dusts even pose a risk being distributed and pressed through a nozzle for the testing device and, in worst case, for the operator. Previous researchers have developed alternative types of nozzles for specific types of dust, but provide limited evaluation of their performance relative to standard nozzles. Additionally, researchers have not provided sufficient geometry so that they can be reproduced by others. One alternative nozzle for the dispersion of flocky or coarse dusts is stated in the ISO standard but not described there either. This article investigates four types of nozzles: The two standard ones that are widely used already, an alternative type, that got introduced into the international standard in 2016 but is still seldomly used and one that was constructed to overcome some of the observed disadvantages. The injection curves are compared with and without dust loadings as well as the explosion characteristics. Eventually, a suggestion is given for different types of dusts. KW - Dust explosions KW - Safety characteristics PY - 2024 DO - https://doi.org/10.1016/j.jlp.2024.105492 SN - 0950-4230 VL - 92 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-61697 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Salge, T. A1 - Schmidt, R. A1 - Hodoroaba, Vasile-Dan T1 - Need for large-area EDS detectors for imaging nanoparticles in a SEM operating in transmission mode N2 - Accurate characterization of nanoparticles (NPs) with a high-resolution SEM with respect to morphology, shape and size distribution is carried out meanwhile routinely in more and more laboratories [1,2]. The valuable result of the metrological measurement of the NP size distribution -including traceability to the SI length unit - was also recently demonstrated by exploiting the transmission mode in a SEM, i.e. TSEM [1,3]. Especially for NPs prepared on thin foil supports like the typical TEM grids the transmission mode at low voltages (up to 30 kV) supplies a high imaging contrast so that sharp boarders of the NPs enable accurate lateral dimensional measurements of NPs size. There are just a few analytical methods which are able to characterize physico-chemical properties of individual NPs. In most cases a SEM has attached an EDS detector so that Information on the elemental composition of the sample to be analyzed becomes possible. The addressed sample volume typically in the micrometer ränge for bulk specimens is considerably reduced if thin, electron transparent Support films are used. Hence, one improves the spatial resolution however, at the cost of lower signal-to-noise ratios of the X-ray spectra, due to the tiny amount of substance excited [2,4,5]. One decisive technological development in the manufacturing of EDS detectors, namely the large-area SDD EDS, meanwhile available commercially in various designs, compensates this analytical drawback. If collection solid angles of 1-2 msr have been typically available for almost four decades, recent technological improvements in SDD EDS size and design have resulted in solid angles in the sr ränge. KW - EDS KW - EDX KW - Nanoparticles KW - High-resolution KW - SEM KW - T-SEM KW - Large-area EDS PY - 2014 DO - https://doi.org/10.1017/S1431927614005030 SN - 1431-9276 SN - 1435-8115 VL - 20 IS - Suppl. S 3 SP - 662 EP - 663 PB - Cambridge University Press CY - New York, NY AN - OPUS4-31389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Müller, J. T. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Schmidt, J. A1 - Bekheet, M. F. A1 - Gurlo, A. A1 - Simon, U. T1 - Hierarchically porous and mechanically stable monoliths from ordered mesoporous silica and their water filtration potential N2 - Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3 ), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling. KW - SAXS KW - Hierarchically porous KW - Silica KW - Water filtration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555928 DO - https://doi.org/10.1039/D2NA00368F SN - 2516-0230 SP - 1 EP - 17 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-55592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ganose, Alex M. A1 - Sahasrabuddhe, Hrushikesh A1 - Asta, Mark A1 - Beck, Kevin A1 - Biswas, Tathagata A1 - Bonkowski, Alexander A1 - Bustamante, Joana A1 - Chen, Xin A1 - Chiang, Yuan A1 - Chrzan, Daryl C. A1 - Clary, Jacob A1 - Cohen, Orion A. A1 - Ertural, Christina A1 - Gallant, Max C. A1 - George, Janine A1 - Gerits, Sophie A1 - Goodall, Rhys E. A. A1 - Guha, Rishabh D. A1 - Hautier, Geoffroy A1 - Horton, Matthew A1 - Inizan, T. J. A1 - Kaplan, Aaron D. A1 - Kingsbury, Ryan S. A1 - Kuner, Matthew C. A1 - Li, Bryant A1 - Linn, Xavier A1 - McDermott, Matthew J. A1 - Mohanakrishnan, Rohith Srinivaas A1 - Naik, Aakash A. A1 - Neaton, Jeffrey B. A1 - Parmar, Shehan M. A1 - Persson, Kristin A. A1 - Petretto, Guido A1 - Purcell, Thomas A. R. A1 - Ricci, Francesco A1 - Rich, Benjamin A1 - Riebesell, Janosh A1 - Rignanese, Gian-Marco A1 - Rosen, Andrew S. A1 - Scheffler, Matthias A1 - Schmidt, Jonathan A1 - Shen, Jimmy-Xuan A1 - Sobolev, Andrei A1 - Sundararaman, Ravishankar A1 - Tezak, Cooper A1 - Trinquet, Victor A1 - Varley, Joel B. A1 - Vigil-Fowler, Derek A1 - Wang, Duo A1 - Waroquiers, David A1 - Wen, Mingjian A1 - Yang, Han A1 - Zheng, Hui A1 - Zheng, Jiongzhi A1 - Zhu, Zhuoying A1 - Jain, Anubhav T1 - Atomate2: Modular workflows for materials science N2 - High-throughput density functional theory (DFT) calculations have become a vital element of computational materials science, enabling materials screening, property database generation, and training of “universal” machine learning models. While several software frameworks have emerged to support these computational efforts, new developments such as machine learned force fields have increased demands for more flexible and programmable workflow solutions. This manuscript introduces atomate2, a comprehensive evolution of our original atomate framework, designed to address existing limitations in computational materials research infrastructure. Key features include the support for multiple electronic structure packages and interoperability between them, along with generalizable workflows that can be written in an abstract form irrespective of the DFT package or machine learning force field used within them. Our hope is that atomate2's improved usability and extensibility can reduce technical barriers for high-throughput research workflows and facilitate the rapid adoption of emerging methods in computational material science. KW - Automation KW - Materials design KW - DFT workflows KW - Phonons KW - Thermal conductivity KW - Bonding analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635759 DO - https://doi.org/10.1039/d5dd00019j SN - 2635-098X SP - 1 EP - 30 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-63575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Neuartige Akku‘s/Batterien – Inhaltsstoffe und Reaktionsprodukte N2 - Die Inhaltsstoffe von Batterien sowie die Reaktionsprodukte beim Thermischen Durchgehen werden vorgestellt. T2 - 28. Sitzung der BfR-Kommission „Bewertung von Vergiftungen CY - Berlin, Germany DA - 04.04.2022 KW - Lithiumbatterien KW - Inhaltsstoffe PY - 2022 AN - OPUS4-56755 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -