TY - JOUR A1 - Tichter, Tim A1 - Tichter, Alex A1 - Andrae, Dirk A1 - Roth, Christina T1 - Simulating cyclic voltammetry at rough electrodes by the digital-simulation–deconvolution–convolution algorithm N2 - The influence of electrode roughness on diffusional cyclic voltammetry (CV) is investigated from a theoretical perspective. For this purpose, the digital-simulation–deconvolution–convolution (DSDC) algorithm, initially developed for the simulation of CV at porous electrodes, is subjected to three substantial modifications. First, by employing adaptive numerical resolution and sample volumina, the computational demand of the digital simulation (DS) step is reduced significantly. Second, by modifying the Douglas–Gunn algorithm of the DS-step to operate on an arbitrarily incremented spatial grid perpendicular to the macroscopically planar electrode surface, the bulk of the fluid can be treated with an exponentially increasing spatial discretization which uses computational power even more efficiently. The third modification is an optimization of the computationally demanding deconvolution step which is used to extract the mass-transfer function from the data computed in the DS-step. This, initially recursive procedure, is replaced by a three-step sequence consisting of (I) a numerical Laplace transformation (NLT) on an exponentially expanding time-grid, (II) a Laplace-domain integration (LDI) and finally (III) a numerical inversion of Laplace transformation (NILT) using the Gaver–Stehfest (GS) inversion formula. Based on this novel strategy for CV simulation, the effects of electrode roughness are thoroughly investigated. It is demonstrated that for an ideally reversible reaction the effects of electrode roughness on the CV response are insignificant at common experimental timescales. In contrast, for scenarios with electrochemically quasi-reversible (or irreversible) kinetics, the apparent rate constants are allegedly upscaled by the area ratio 𝜓 = 𝐴rough∕𝐴planar . This manifests in a lower peak-to-peak separation without a distortion of the shape of the voltammetric profile. This behavior is finally explained in a quantitative manner in terms of convolution-sums and mass-transfer functions which ultimately puts the parameter electrode roughness into the semianalytical framework of convolutive modeling. KW - Rough electrodes KW - Electrode kinetics and Peak-to-Peak separation KW - Vanadium redox-flow batteries KW - Convolutive modeling KW - Digital-simulation KW - Numerical inversion of Laplace transformation KW - Gaver–Stehfest inversion formula PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614620 DO - https://doi.org/10.1016/j.electacta.2024.145175 VL - 508 SP - 1 EP - 17 PB - Elsevier B.V. AN - OPUS4-61462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Lithiumbatterien im Seeschiffsverkehr: lassen sich zukünftig Brände verhindern? N2 - Ausgehend von der Vielzahl an Bränden im Seeverkehr, die Lithiumbatteriebränden zugeschrieben werden, wird betrachtet, wie ein sichererer Transport von Lithiumbatterien im Seeverkehr erfolgen kann und inwiefern die BAM durch Ihre Mitarbeit in der Regelwerksentwicklung und Forschung dazu beiträgt. T2 - KLIB Mitgliederforum CY - Frankfurt am Main, Germany DA - 19.03.2024 KW - Lithiumbatterien KW - Gefahrguttransport KW - Seeverkehr KW - Sicherheit PY - 2024 AN - OPUS4-62324 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eberwein, Robert T1 - NICOLHy - 1st Stakeholder Advisory Board meeting N2 - The NICOLHy project aims to develop a novel insulation concept based on Vacuum Insulation Panels (VIP) that enables the safe, cost- and energy efficient storage of large quantities of LH2. Such large scale LH2 storage technology is necessary for establishing a hydrogen economy with dimensions between 40.000 m³ and more than 200.000 m³ of LH2. However, new design concepts are needed because the currently available technologies used in small and medium storages today are not suitable for up-scaling. The main problems prohibiting the up-scaling are the long production time due to the process chain, the low failure tolerance and the spherical shape, which reduces the payload in technical applications by up to 50% compared to other shapes. The novel concept will change these conditions by a system which is modular, open-form, time-and cost efficient while production, operation and service, multi-failure tolerant and applicable for onshore and offshore applications. The presentations shows details to the concept and presents several safety concerns the project has to deal with. This document contains all presentations from NICOLHys first Stakeholder Meeting. T2 - NICOLHy 1st Stakeholder Meeting CY - Trondheim, Norway DA - 24.06.2024 KW - Liquefied hydrogen KW - Insulation KW - Tanks PY - 2024 AN - OPUS4-61393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cano Murillo, Natalia A1 - Balasooriya, Winoj A1 - Theiler, Geraldine T1 - Effect of hydrogen environment on the physical and mechanical properties of elastomers N2 - The development of a robust hydrogen infrastructure poses challenges to materials exposed to high pressurized hydrogen environments. Polymeric materials, which are expected to perform as seals, gaskets, O-rings, hoses among other applications face high risk of damage due to rapid gas decompression (RGD) which might cause operational safety issues. In this study, we intend to assess the effects of a high pressurized hydrogen environment on carbon black filled (CB) elastomers. The materials were exposed to 100 MPa hydrogen atmosphere at room temperature and at 85°C. Ex-situ characterization was performed during the first 30 minutes after decompression and repeated two days after the exposure when total gas desorption has taken place. The physical and mechanical characteristics of the materials were determined by means of density and volume change, hardness and tensile tests, and dynamic mechanical analysis. T2 - EHEC, the European Hydrogen Energy Conference 2024 CY - Bilbao, Spain DA - 06.03.2024 KW - High pressurized Hydrogen KW - Sealing Materials KW - Carbon Black Filled Elastomers PY - 2024 AN - OPUS4-60706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Theiler, Geraldine A1 - Cano Murillo, Natalia A1 - Halder, Karabi A1 - Balasooriya, Winoj A1 - Hausberger, Andreas A1 - Kaiser, Andreas T1 - Effect of high-pressure hydrogen environment on the physical and mechanical properties of elastomers N2 - This study presents the influence of high-pressure hydrogen environment on the physical and mechanical properties of two types of cross-linked hydrogenated acrylonitrile butadiene rubbers. Based on the CSA/ANSI standard, static exposures in hydrogen experiments were performed up to 100 MPa at 120 °C. Characterization before and after exposure was conducted by means of density and hardness measurements, dynamic mechanical analysis (DMA), tensile tests, compression set, FT-IR and AFM analyses to assess effects after decompression. While the effect of high-pressure exposure is significant immediately after exposure, most of the physical and mechanical properties recover after 48 hours. FT-IR, AFM, SEM and compression set results indicate, however, permanent effects. KW - Hydrogen KW - Mechanical properties KW - Elastomers KW - High-pressure hydrogen environment PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597102 DO - https://doi.org/10.1016/j.ijhydene.2024.01.148 SN - 0360-3199 VL - 58 SP - 389 EP - 399 PB - Elsevier Ltd. AN - OPUS4-59710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Theiler, Geraldine A1 - Cano Murillo, Natalia A1 - Hausberger, Andreas T1 - Effect of hydrogen pressure on the fretting behavior of rubber materials N2 - Safety and reliability are the major challenges to face for the development and acceptance of hydrogen technology. It is therefore crucial to deeply study material compatibility, in particular for tribological components that are directly in contact with hydrogen. Some of the most critical parts are sealing materials that need increased safety requirements. In this study, the fretting behavior of several elastomer materials were evaluated against 316L stainless steel in an air and hydrogen environment up to 10 MPa. Several grades of cross-linked hydrogenated acrylonitrile butadiene (HNBR), acrylonitrile butadiene (NBR) and ethylene propylene diene monomer rubbers (EPDM) were investigated. Furthermore, aging experiments were conducted for 7 days under static contions in 100 MPa of hydrogen followed by rapid gas decompression. Fretting tests revealed that the wear of these compounds is significantly affected by the hydrogen environment compared to air, especially with NBR grades. After the aging experiment, the friction response of the HBNR grades is characterized by increased adhesion due to elastic deformation, leading to partial slip. KW - Fretting wear KW - Rubbers KW - Hydrogen KW - High-pressure PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608462 DO - https://doi.org/10.3390/lubricants12070233 VL - 12 IS - 7 SP - 1 EP - 17 PB - MDPI AN - OPUS4-60846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tichter, Tim T1 - Simulating diffusional cyclic voltammetry at rough electrodes by means of the DSDC algorithm N2 - Electrode roughness is an exceptionally important, yet oftentimes overlooked factor in electrokinetic analysis and catalyst research. Essentially any electroanalytical experiment involving an electrode with a surface which is not perfectly smooth will be subjected to more or less severe effects of roughness. This includes any circumstance where electrodes are decorated with micro- or nanoparticles and is therefore relevant for a plethora of experimental scenarios. Since the roughness-related gain in surface area scales the reaction rate – and thus the current – it is an inherently non-straightforward task to assess intrinsic electrode kinetics from experimental data of rough structures. In other words, a significant overestimation of kinetic constants may arise when rough electrodes are employed and kinetics are analyzed under the assumption of perfectly planar surfaces. For this reason, it is fundamentally interesting to approach electrode roughness from a purely theoretical point of view, since surface roughness and kinetics can be tuned in a deliberate manner for separating their individual contributions. In this study, we propose a strategy for the simulation of the most common electroanalytical technique – cyclic voltammetry – at mesoscopically rough surfaces. For this purpose, our previously introduced digital simulation - deconvolution - convolution (DSDC) algorithm [1] is employed. By modifying, the Douglas--Gunn algorithm, which is used in the digital simulation step to operate on an arbitrarily incremented spatial grid, a high numerical resolution near the electrode/electrolyte boundary and a larger spatial discretization in the bulk of the electrolyte can be used. This provides a fine resolution of artifacts of surface roughness and efficiently utilizes computational power. As a consequence, simulations can be performed on real-space data of rough electrodes which is obtained from atomic force microscopy (AFM). It is demonstrated that for an ideally reversible reaction the effects of electrode roughness on the CV response are insignificant. In contrast, for practically relevant scenarios with electrochemically irreversible or quasi-reversible kinetics, the apparent rate constants are allegedly upscaled by the area-ratio Arough/Aplanar up to a certain threshold. Qualitatively, this manifests in a lower peak-to-peak separation without a distortion of the shape of the voltammetric profile. As soon as the surface profile becomes much deeper than wide, a distortion of the CV response occurs which is associated with an increasingly finite diffusion domain. This behavior is finally explained in terms of convolution-sums and mass-transfer functions and provides a quantitative interpretation of roughness effects. T2 - Electrochemistry 2024 CY - Braunschweig, Germany DA - 16.09.2024 KW - Rough electrodes KW - Convolutive Modeling KW - Digital Simulation KW - Cyclic voltammetry KW - Redox-Flow Batteries PY - 2024 AN - OPUS4-62308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Clute, C. A1 - Balasooriya, Winoj A1 - Cano Murillo, Natalia A1 - Theiler, Geraldine A1 - Kaiser, A. A1 - Fasching, M. A1 - Schwarz, Th. A1 - Hausberger, A. A1 - Pinter, G. A1 - Schloegl, S. T1 - Morphological investigations on silica and carbon-black filled acrylonitrile butadiene rubber for sealings used in high-pressure H2 applications N2 - Effects of NBR formulations on properties for high-pressure gas systems were tested. Functionalized silica enhances typical properties to a comparable range like CB. The balance of additives results in suitable RGD performance. Silica filled NBR shows lower H2 uptake compared to non-plasticized CB filled NBR. Morphology of CB filled NBR is less affected by H2 than silica filled grades. KW - High-pressure hydrogen gas KW - Sealing KW - Acrylonitrile butadiene rubber KW - Filler-rubber-interaction KW - Rapid gas decompression (RGD) PY - 2024 DO - https://doi.org/10.1016/j.ijhydene.2024.04.133 SN - 0360-3199 VL - 67 SP - 540 EP - 552 PB - Elsevier Ltd. AN - OPUS4-60559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Theiler, Geraldine T1 - On the way to sustainable and hydrogen compatible sealing materials N2 - In this contribution, the sliding performance of newly formulated polymer materials with improved sustainability are investigated and compared with conventional materials. Tribological tests were performed in hydrogen at ambient temperature as well as cryogenic medium. The samples were arranged in a pin-on-disk configuration with a flat pin sliding against a rotating austenitic steel disk. The friction and wear mechanisms are described and discussed by means of surface analyses. T2 - PolyTrib 2024 CY - Portoroz, Slowenia DA - 03.10.2024 KW - High-performance polymers KW - Sliding wear KW - Hydrogen KW - Cryogenic PY - 2024 AN - OPUS4-61419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tichter, Tim T1 - Frühwarnsystem für EV-Batterien: Prädiktion des Thermischen Durchgehens von Lithium-Ionen-Speichern N2 - Kritisch defekte Lithium-Ionen Batterien bergen ein signifikantes Gefährdungspotenzial, da die Möglichkeit eines so genannten thermischen Durchgehens (TD) besteht. Dabei handelt es sich um eine autoamplifizierende Reaktion, welche zu einer unkontrollierten Erwärmung mit Rauch- und Flammenerscheinung oder gar einer Explosion führt. Insbesondere bei großen Batterien mit einer Kapazität von über 100 kWh, stellt ein TD ein sehr großes Schadensereignis dar. Folglich gilt es, dieses Ereignis strikt zu vermeiden. Im Rahmen der Präsentation werden aktuelle Arbeiten der BAM im Bereich der TD-Früherkennung vorgestellt. T2 - Gefahrguttag 2024 CY - Hannover, Germany DA - 19.09.2024 KW - Thermisches Durchgehen KW - Lithium-Ionen Batterien KW - Automotive Anwendungen PY - 2024 AN - OPUS4-62309 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Theiler, Geraldine A1 - Cano Murillo, Natalia A1 - Hashimoto, H. A1 - Aoyagi, A. A1 - Dobbelaar, E. T1 - On the way to sustainable and hydrogen compatible sealing materials N2 - In this contribution, the sliding performance of newly formulated polymer materials with improved sustainability are investigated and compared with conventional materials. Tribological tests were performed in hydrogen at ambient temperature as well as cryogenic medium. The samples were arranged in a pin-on-disk configuration with a flat pin sliding against a rotating austenitic steel disk. The friction and wear mechanisms are described and discussed by means of surface analyses. T2 - PolyTrib 2024 CY - Portoroz, Slowenia DA - 03.10.2024 KW - High-performance polymers KW - Sliding wear KW - Hydrogen KW - Cryogenic PY - 2024 SP - 1 EP - 2 AN - OPUS4-61421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Natrium-Ionen Batterien N2 - Der Bedarf an Forschung der Bundesoberbehörden zu Natrium-Batterien als neues Thema wurde identifiziert. Hier kann die BAM jedoch bereits zahlreiche Untersuchungen im Rahmen des BAM-internen Projekts "SIB-Links" vorweisen. T2 - BoB Bundes-Oberbehörden CY - Online meeting DA - 10.06.2024 KW - Natrium-Ionen Batterien PY - 2024 AN - OPUS4-62325 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Lithiumbatterien - Transport und Sicherheit N2 - Fachwissen zum Transport und sicherem Umgang mit Lithiumbatterien ist eine essentielle für die Arbeit der Gefahrgutbeauftragten der Polizei. Dabei geht e nicht nur um selbstgenutzte Geräte sondern häufig auch um sichergestellte und möglicherweise beschädigte Geräte / Akkus. Diese müssen bestmöglich vor Datenverlust bewahrt werden, gleichzeitig ist die Sicherheit für die zuständigen Mitarbeiter unabdingbar. Der Vortrag dient dazu, die Zuhörer in die Lage zu versetzen, fallbezogene Entscheidungen für Maßnahmen für den sicheren Umgang und den Transport zu treffen. T2 - Polizeiakademie Niedersachsen Gefahrgutbeauftragte CY - Dannenberg, Germany DA - 10.12.2024 KW - Lithiumbatterien KW - Gefahrguttransport KW - Lagerung PY - 2024 AN - OPUS4-62331 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita A1 - Moench, Lars A1 - Rausch, Talea T1 - Vorstellung des Berichtes Batteriezellenherstellung des Arbeitskreises Elektrische Energiespeichersysteme der Kommission für Anlagensicherheit N2 - In der Kommission Anlagensicherheit (KAS) Arbeitsgruppe Elektrische Energiespeicher wurde ein Bericht erstellt, der den Stand der Technik für die Batteriezellproduktion in Deutschland widerspiegelt und die Einstufung nach Störfallverordnung mittels einer Liste aller enthaltenen Stoffe ermöglicht. Dieser wird vorgestellt und die Anwendung der maßgeblich durch die BAM erstellte Liste erläutert. T2 - UBA Fachbereichgespräch CY - Online meeting DA - 24.10.2024 KW - Störfallverordnung KW - Batterie-Zellproduktion KW - LIthiumbatterien KW - Anlagensicherheit PY - 2024 AN - OPUS4-62327 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holtappels, Kai T1 - Vertrauen in Wasserstofftechnologien - Sicherheitsaspekte in der Wasserstoff-Wertschöpfungskette N2 - Wo stehen wir bei Wasserstoff in Sachen Sicherheit? Welche Lücken gibt es aktuell, und wie sind sie zu schließen? Der Weg zur Wasserstoffwirtschaft verlangt die Einführung zahlreicher „neuer“ Technologien in vielen Bereichen. Dies kann aber nur gelingen, wenn Entscheidungsträger und Öffentlichkeit gleichermaßen davon überzeugt sind, dass diese Technologien ausreichend erprobt und sicher sind. Die Sicherheit der Wasserstofftechnologien muss dabei mindestens mit der technologischen Entwicklung Schritt halten - besser noch sie vorwegnehmen - um allzu konservative und kostspielige Sicherheitslösungen zu vermeiden und die praktische Nutzbarkeit und Sicherheit von Wasserstoff zu demonstrieren. Gelingt dies nicht, können schon einzelne sicherheitsrelevante Vorfälle schnell zu Unsicherheiten und erheblichem Vertrauensverlust führen. Im Rahmen einer Webinarreihe des VDMA stellte die BAM vor, wie es aktuell um die Sicherheit in Sachen Wasserstoff bestellt ist, welche konkreten Herausforderungen noch zu bewältigen sind und wie erkannte Lücken geschlossen werden können. T2 - VDMA Power-to-X Webseminar CY - Online meeting DA - 29.10.2024 KW - Wasserstoff KW - Sicherheit KW - Vertrauen KW - Akzeptanz KW - Wertschöpfungskette PY - 2024 AN - OPUS4-61481 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holtappels, Kai T1 - Kompetenzzentrum H2Safety – Aktuelle Themen zur Wasserstoffsicherheit N2 - In einer Keynote bei der VDI-Fachkonferenz Wasserstoff 2024: Technische Sicherheit hat die BAM das Kompetenzzentrum H2Safety@BAM sowie verschiedene Arbeiten zum Thema Wasserstoffsicherheit sowie Wissens- und Technologietransfer halten dürfen. Wichtige Kernbotschaften waren allgemein Sicherheitsfragen entlang der Wasserstoff-Wertschöpfungskette, Sicherheit muss von Beginn an bei der Entwicklung einer Technologie berücksichtigt werden und Sicherheitskonzepte müssen mit dem Technologiereifegrad mitwachsen. T2 - VDI-Fachtagung Wasserstoff 2024: Technische Sicherheit CY - Cologne, Germany DA - 24.09.2024 KW - Wasserstoff KW - Sicherheit KW - Wertschöpfungskette KW - Sicherheitskonzepte PY - 2024 AN - OPUS4-61482 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holtappels, Kai T1 - Sicherheit von Wasserstofftechnologien - Quo Vadis N2 - Die Sicherheit stellt eine wichtige Säule dar, um Vertrauen in neue Technologien zu gewinnen. Je größer die Zahl an Wasserstoffanwendungen im industriellen Bereich sowie in weiteren Bereichen des öffentlichen Lebens wird, umso mehr steigt die Wahrscheinlichkeit für Zwischenfälle. Die Sicherheit muss mit den Trends der technologischen Entwicklung Schritt halten oder sie besser noch vorwegnehmen. Gleichzeitig gilt es sowohl die Öffentlichkeit als auch insbesondere die Rettungskräfte über die Besonderheiten von Wasserstoff zu informieren, ohne dabei Verunsicherung zu erzeugen. Der Vortrag gibt einen Überblick über aktuelle Entwicklungen und offene Sicherheitsfragen. T2 - 25. Münchner Feuerwehrsymposium CY - Munich, Germany DA - 16.11.2024 KW - Wasserstoffsicherheit KW - Feuerwehr KW - Unfälle PY - 2024 AN - OPUS4-61856 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Jordan, T. A1 - Askar, Enis A1 - Holtappels, Kai A1 - Jopen, M. A1 - Stoll, U. A1 - Reinecke, E.-A. A1 - Krause, U. A1 - Beyer, M. A1 - Markus, D. T1 - Fuels – Introduction | Hydrogen safety N2 - The introduction of hydrogen as a safe energy carrier needs a robust knowledge base, tools for the design and safety assessment of hydrogen technologies built on it, and an internationally harmonized set of standards and regulations. Many of the innovative technologies imply hydrogen at high pressures and/or cryogenic temperatures, with which private users come into contact for the first time in distributed applications. In order to avoid over-conservative, expensive safety solutions, while at the same time demonstrating the usability and safety of hydrogen applications and maintaining acceptance for the technology, safety research must also keep pace with, or better yet anticipate, trends in technological development. Thus, this overview article describes not only the current state of knowledge and technology regarding hydrogen safety, but also its further development. KW - Explosion protection KW - Accidental scenarios KW - Hazard and risk assessment KW - Regulations codes and standards (RCS) KW - Ignition KW - Hydrogen storage KW - Energy carrier PY - 2024 SN - 978-0-1240-9547-2 DO - https://doi.org/10.1016/B978-0-323-96022-9.00195-X VL - 2nd Edition SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-59940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Namwoonde, Andreas Sheuyange T1 - Polymer Composites Under Continuous and Reciprocating Sliding Conditions In Hydrogen N2 - The implementation of hydrogen as an alternative energy source to fossil fuels necessitates the use of compatible materials for safety purposes, and thermoplastics are widely utilized in this context. The application of polymers in gaseous and liquid hydrogen environments requires careful consideration of their tribological performance, as the operating environment is dramatically different from ambient conditions. Friction, wear, and lubrication are crucial factors to consider in this regard. Researchers have investigated various strategies to enhance the tribological performance of polymers in hydrogen environments, including modifying the composition and structure of polymers by incorporating fillers to improve their friction and wear resistance. The tribological properties of polymer composites based on matrices of PEEK, PPS, and PI have been mostly investigated using the continuous sliding test method, and the results indicate that these materials are suitable candidates for tribological applications in both gaseous and liquid hydrogen. This project explores the tribological properties of related polymer composites in hydrogen using continuous and reciprocating motion with a pin-on-disc testing method. T2 - Polytrib2024 CY - Portorož, Slovenia DA - 03.10.2024 KW - Polymers KW - Friction KW - Wear KW - Tribological behaviour KW - Hydrogen PY - 2024 AN - OPUS4-61378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimault de Freitas, Tomás T1 - Hollow Specimen Method for Tests in High-Pressure Hydrogen Gas: The Role of Geometry, Surface Quality and Gas Purity N2 - The hollow specimen technique is a simple and cost-effective method that has the potential to make materials qualification with pressurised gaseous hydrogen widely accessible to academia and industry. The feasibility of this method for slow strain tensile tests has been demonstrated in several studies, leading to the establishment of the ISO/TC 164/SC 1/WG 9 ISO committee for its standardisation. Questions have emerged during this process, that currently prevent the method from being standardised for hydrogen testing. These questions relate to specimen geometry, specimen manufacturing and gas quality and are being systematically addressed in the TransHyDE-H2HohlZug project. The first results are presented in this poster. T2 - TransHyDE Vollversammlung 2024 CY - Leipzig, Germany DA - 27.11.2024 KW - Hydrogen KW - Hydrogen Embrittlement KW - Hollow Specimen Technique KW - High-Pressure Gaseous Hydrogen KW - Austenitic Stainless Steel KW - TransHyDE KW - H2HohlZug PY - 2024 AN - OPUS4-61847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konert, Florian T1 - Investigation of the resistance of X65 pipeline steel and weld to gaseous hydrogen using the hollow specimen technique N2 - The constantly increasing demand for renewable energy sources lead to the necessity of transporting large amounts of hydrogen. Since pipelines enable a cost-effective way for the distribution of gaseous hydrogen, the interaction of hydrogen and the pipeline materials must be carefully investigated as hydrogen can cause a degradation of the mechanical properties under certain conditions. Especially welds, which are assumed to be more susceptible to the degradation enhanced by hydrogen, are of great interest. The aim of this study is to investigate the effect of gaseous hydrogen on the mechanical properties of an X65 pipeline, and the longitudinal submerged arc welding (SAW) welded joint. The tests are conducted using the hollow specimen technique on two types of specimens: one extracted from the base material (BM) and the other extracted as a cross-weld (CW) specimen consisting of base material and weld seam. The specimens are charged in-situ under a pressure of 60 bar and tested using slow strain rate (SSR) tensile tests with a nominal strain rate of 10-5 s-1. The performed tests showed a decrease of the reduction of area (RA) from 72% in inert atmosphere to 52% in hydrogen atmosphere for the CW-specimen and a decrease from 73% in inert atmosphere to 51% for the BM. Metallographic analyses showed the crack initiation between fine grain heat affected zone (FGHAZ) and BM for the specimens tested in hydrogen atmosphere as well as for the reference specimens. This leads to the conclusion that the location of the crack initiation does not change due to the presence of gaseous hydrogen. T2 - 77th IIW Annual Assembly and International Conference 2024 CY - Rhodes, Greece DA - 07.07.2024 KW - Hydrogen KW - Hollow-specimen KW - Pipeline steel KW - SSRT KW - Hydrogen embrittlement PY - 2024 AN - OPUS4-60617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konert, Florian T1 - The applicability of the hollow specimen technique for testing various metals under high pressure hydrogen atmosphere N2 - The transition to a decarbonised economy will require large amounts of hydrogen over a broad variety of applications. The use of hydrogen poses high safety requirements as hydrogen can be absorbed by metallic materials and result in hydrogen embrittlement under certain condi-tions. For this reason, interactions of gaseous hydrogen and metallic materials are of high sci-entific and industrial interest. Slow strain rate tensile (SSRT) tests are commonly used to evaluate the hydrogen-induced ductility loss of alloys. However, the current standardised test method describes a complex and expensive procedure with limited availability worldwide. The hollow specimen technique promises huge potential for scaling suitable in-situ testing infra-structure and is currently under intensive development in several institutes around the world. As this method has only gained significant attention in the last decade, there are varying interpretations, particularly when testing materials with vastly different mechanical properties. Most available literature focuses on common steels used in hydrogen and natural gas piping systems. The present work provides an overview of the widespread applicability of hollow specimens in evaluating the effect of high-pressure hydrogen on the tensile properties of vari-ous metallic materials. The research presented includes Near-Net shape produced additively manufactured (AM) AISI 316 L, ferritic X65 steel, its weld seam, and solution annealed and hardened 100Cr6 steel. T2 - European Conference on Fracture 2024 CY - Zagreb, Croatia DA - 26.08.2024 KW - Hydrogen KW - Hollow specimen technique KW - SSRT PY - 2024 AN - OPUS4-60912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Askar, Enis T1 - Safety Issues in connection with electrolyzer systems N2 - In this presentation current and future challenges for the safety of hydrogen technologies are discussed. Furrthermore, the specific hazards for the operation of electrolyzers are shown and finally the trhreshold values (storage and power) for the approval of electrolyzers are presented. T2 - Online Workshop: Regulation on hydrogen thresholds and permitting processes for electrolyzers CY - Online meeting DA - 17.09.2024 KW - Hydrogen technologies KW - Process & plant safety KW - Hydrogen production PY - 2024 AN - OPUS4-61086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Askar, Enis T1 - BAM - Short Presentation N2 - The activities of the competence center H2Safety@BAM are presented. In more detail the testing facilities at Technical Test Site TTS are shown as well as recent testing activities in the field of hydrogen safety. T2 - 5th In-Person IEA Task 43 Meeting - Safety and RCS of Large Scale Hydrogen Energy Applications CY - Minneapolis, MN, USA DA - 26.09.2024 KW - Explosion protection KW - Consequence analysis KW - H2safety@BAM KW - Living Lab PY - 2024 AN - OPUS4-61746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Askar, Enis T1 - Safety of Electrolyzers N2 - After a short introduction on the BAM activities, the development of the electrolyzer technology is shown briefly. Then future challenges for the safety of hydrogen technologies are discussed and the general safety issues in the electrolysis system are presented. Finally, accidents in context with electrolyzers are discussed and the legal framework is summarized. T2 - Hydrogen Europe - Workshop on safety standards for electrolysers CY - Online meeting DA - 01.10.2024 KW - Explosion protection KW - Process & plant safety KW - Hydrogen production PY - 2024 AN - OPUS4-61745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mente, Tobias T1 - MatCom - Materialeigenschaften und Kompatibilität für Wasserstofftechnologien - MatCom 1 - Metallische Werkstoffe N2 - Aufbauend auf dem historischen Schadensfall von A. Martens im Jahr 1894 zur Explosion von H2-Gasflaschen auf dem Tempelhofer Feld und den dabei durchgeführten Untersuchungen wird im Hauptteil des Vortrages auf die Standardisierung der Hohlzugprüftechnik eingegangen. Dabei wird zunächst auf die Vor- und Nachteile unterschiedlicher Prüfmöglichkeiten zur Wasserstoffkompatibilität metallischer Werkstoffe und deren Schweißverbindungen eingegangen und im Weiteren die Umsetzung der Prüftechnik an der BAM beschrieben. Für die Standardisierung der Hohlzugprüftechnik wurden verschiedene Randbedingungen mit Einfluss auf die Ergebnisqualität überprüft. Dabei wurde der Pipelinestahl X65 als auch der additiv gefertigte Werkstoff 316L genutzt. Abschließend wird auf die Verwaltungspartnerschaft mit Namibia eingegangen und die umzusetzenden Projekte mit Bezug zur Schweißtechnik dargestellt. T2 - BAM-PTB Workshop CY - Magdeburg, Germany DA - 04.09.2024 KW - MatCom1 KW - H2Safety@BAM KW - Hohlzugprobe PY - 2024 AN - OPUS4-61036 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ekici, Nilsah T1 - SHIMMER project: safe hydrogen injection modelling and management for european gas network resilience N2 - To accelerate the transition to a low-carbon economy while exploiting existing infrastructure, hydrogen can be injected to the natural gas network. However, many technical and regulatory gaps should be closed, and adaptations and investments made to ensure that multi-gas networks across Europe will be able to operate in a reliable and safe way while providing a highly controllable gas quality and required energy demand. The SHIMMER project aims to enable a higher integration and safer hydrogen injection management in multi-gas networks by contributing to the knowledge and better understanding of hydrogen projects, their risks, and opportunities. T2 - EGATEC 2024 CY - Hamburg, Germany DA - 18.06.2024 KW - Hydrogen KW - Gas grid KW - Database KW - Low-carbon PY - 2024 AN - OPUS4-60519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaanika, Sam T1 - Compatibility of welded austenitic stainless steel (316L) tube for green hydrogen applications N2 - The increase in the energy demand and the need to comply to net zero carbon regulations, as per the Paris 2015 climate agreement by 2050, has necessitated the urgency to consider hydrogen as alternative energy carrier. Moreover, hydrogen interaction with metals tend to cause degradation of the mechanical properties in terms of the ductility of the materials. More concern is on the weldment and repair of tubes or pipelines of hydrogen transportation and storage systems. In this study, the heat inducted weld tubes of the cold drawn and annealed austenitic stainless steel (316L) were investigated by slow strain rate test. To achieve the most realistic component-related testing, hollow tube specimens have been fabricated from 1/2-inch Swagelok pipes filled with internal gaseous hydrogen or inert air for reference. The hydrogen concentration measurement is undertaken before and after the autoclave high-pressure pre-charging of the specimens using carrier gas hot extraction. SEM analysis was used to carry out fractographic analysis to determine the crack initiation sites, crack size and was compared for the base material and heat affected zone influence in the gaseous hydrogen. The effect of hydrogen on the material compatibility of the welded austenitic stainless steel is assessed and compared to none-welded tubes tested in defined testing parameters that contribute to Hydrogen Assisted Cracking. A better understanding on the impact of weldment on the structural integrity for stainless steel is elucidated for green hydrogen application. T2 - IIW 77th Annual Assembly 2024 CY - Rhodes, Greece DA - 07.07.2024 KW - Austenitic stainless steel KW - Slow strain rate KW - Burst pressure KW - Orbital welding KW - Heat Induction PY - 2024 AN - OPUS4-60698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - El Harrab, Hayat T1 - Evaluation of the Impact of Lubricating Oil on Pre-Ignition of Hydrogen for Engine Relevant Conditions N2 - A successful transition to clean energy depends on ensuring that the world's growing energy needs are met while reducing greenhouse gas emissions. Achieving this goal requires the use of carbon-free energy sources. Many utilities have already begun the shift from conventional carbon-based fuels to cleaner alternatives, such as hydrogen. However, numerous challenges persist regarding the use of hydrogen in internal combustion engines. The use of hydrogen in engines, which have extremely lower ignition energy, has raised concerns about the risk of pre-ignition due to the undesirable presence of lubricating oil during combustion. Due to its low auto-ignition temperature, lubricating oil is widely regarded as the main cause of abnormal combustion. To verify and understand the potential influence of lubricating oil on hydrogen reactivity, the auto-ignition temperature was measured using a constant volume reactor. Auto-ignition was identified by a sudden increase in pressure combined with a rapid rise in temperature. The experimental results verified that the addition of 0.2 ml lubricating oil to stoichiometric hydrogen-air mixtures at 20 bar reduced the auto-ignition temperature from 460°C to 270°C, reducing the ignition temperature by 190K. Moreover, the auto-ignition temperature of oil showed a decreasing trend as the initial amount of oil increased, indicating that the ignition process mainly occurs by vaporization. T2 - CI’s 40th International Symposium - Emphasizing Energy Transition CY - Milan, Italy DA - 24.07.2024 KW - Hydrogen KW - Lubricating oil KW - Auto-ignition temperature KW - Internal combustion engines and pre-ignition PY - 2024 AN - OPUS4-61373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leo, Reinhold T1 - Duplex stainless steels - Compatibility for high-pressure hydrogen applications N2 - The key for a transition into clean energy sources is based on the construction of safe energy infrastructure, such as transportation pipelines for Hydrogen. Duplex Stainless Steels (DSS) are an essential component used nowadays in the construction of transportation pipelines because of their many distinctive qualities. The choice of DSS for a particular hydrogen application mainly depends on its susceptibility level to Hydrogen Embrittlement (HE) or Hydrogen Assisted Cracking (HAC). Since the 20th century, the literature indicates three factors that must be considered: the microstructure of the alloy steel, the hydrogen concentration, and the mechanical load. Several mechanisms have been also proposed to describe the occurring microscale processes behind HE or HAC, and these include metastable phase transformation, Hydrogen Enhanced Localized Plasticity (HELP), and Hydrogen Enhanced Decohesion (HEDE). The following contribution describes the path to ascertain if DSS is suitable for high-pressure gaseous hydrogen applications. The interplay between several critical factors that result in HAC was examined using high-pressure gaseous hydrogen charging, Electron Backscatter Diffraction (EBSD), and hydrogen concentration measurements using Carrier Gas Hot Extraction (CGHE). It was determined whether the strain-induced martensitic transformation of the austenite was present in a DSS 1.4462 (DSS2205) in-service pipe and in samples of freshly charged DSS 1.4462. In comparison to the common electrochemical charging described broadly in the literature, no major direct martensitic phase transformation of the austenite phase under a high-pressure hydrogen environment was observed. As for future experiments, the intention is to analyse the impact of high-pressure gaseous hydrogen on the welded components of this grade, and under mechanical load via the hollow specimen technique. T2 - Oxford - EPRI Workshop on Hydrogen Embrittlement 2024 CY - Oxford, United Kingdom DA - 23.06.2024 KW - High-Pressure Hydrogen KW - Pipelines KW - Duplex Stainless Steels KW - Haydrogen Assisted Cracking KW - Hollow Specimen Technique PY - 2024 AN - OPUS4-60525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimault de Freitas, Tomás T1 - Comprehensive standardization of the hollow specimen method for tests in high pressure hydrogen gas N2 - As the world moves towards a decarbonised economy, the demand for sustainable and low-carbon alternatives is rapidly increasing. Hydrogen plays an important role in this transition, but in order to make the most of hydrogen as an energy carrier, a comprehensive understanding of its impact on the integrity of structural materials is necessary. Metallic materials, mostly steels, are the most regularly used structural materials in various components throughout the hydrogen supply chain. Ensuring their sustainable and safe use in hydrogen technologies is a crucial factor in the development of the hydrogen economy. This is particularly important since hydrogen can promote crack formation and ultimately lead to premature failure in these materials when combined with mechanical load. This process is commonly known as Hydrogen Embrittlement and can occur in almost all the steels used for the hydrogen technologies. Extensive materials qualification is needed for the rapid implementation of hydrogen technologies, however, most accepted, and standardised test methods for determining the effect of gaseous hydrogen on metallic materials describe complex and costly procedures that are only available to a very limited extent worldwide. The hollow specimen technique is a simple and economical method that has the potential to overcome the limitations of the current methods and complement them for qualifying metallic materials under high-pressure hydrogen gas. In this method, an axial hole is drilled in a tensile specimen, which is then filled with hydrogen gas, sealed, and placed in a standard testing machine. This method requires significantly lower amounts of hydrogen, resulting in fewer safety measures and no need for complex equipment or a specialised laboratory, unlike the conventional autoclave technique. The technique's low investment and testing costs, simple operation, and shorter testing time make it optimal for widespread use around the world, thereby increasing the output of results. Initial studies have demonstrated the feasibility of assessing hydrogen effects in metallic materials using the hollow specimen technique. This led to the establishment of the committee ISO/TC 164/SC 1/WG 9 “Tensile testing, method in high-pressure hydrogen environment“ to standardise the method, however, there are open questions that currently prevent the technique from being standardised for hydrogen testing. These open questions relate to specimen geometry, inner hole surface and gas quality and are being addressed in the H2HohlZug project. Here, the aim is to systematically address and close the gaps towards the standardisation of this technique for tests with hydrogen. This contribution presents the structure and milestones of the project, followed by initial results regarding the optimisation of the specimen geometry, as well as the influence of different manufacturing and finishing processes on the inner hole surface of the hollow specimen and its response to hydrogen effects. T2 - TestXpo | 32nd International Expo for Materials Testing CY - Ulm, Germany DA - 21.10.2024 KW - Hydrogen KW - Hydrogen Embrittlement KW - High-Pressure Gaseous Gas KW - Hollow Specimen Technique KW - H2HohlZug KW - TransHyDE KW - Standardisation KW - Tensile Test PY - 2024 AN - OPUS4-61453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hickel, Tilmann T1 - Data driven research on hydrogen in metals N2 - The talk gives an overview on data-driven research on hydrogen in metals performed at BAM. The focus is on a ab-initio based high-throughput study on the hydrogen solubility in metals and metallic alloys. Furthermore, the redistribution of hydrogen in transforming microstructures is addressed. The talk ends with an explanation of participant projects in NFDI-MatWerk, motivating the formation of a new project connected to hydrogen technology. T2 - DGM Fachausschuss “Wasserstoffeffekte in Werkstoffen" CY - Saarbrücken, Germany DA - 05.05.2024 KW - Hydrogen KW - Solubility KW - High-throughput study KW - Ab initio simulation KW - NFDI-MatWerk PY - 2024 AN - OPUS4-62721 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hickel, Tilmann T1 - Hydrogen redistribution during electrochemical charging and mechanical testing: insights from a combined ab initio and finite element method N2 - In advanced high strength steels the mechanisms of hydrogen embrittlement are expected to be strongly connected to the amount of retained austenite (RA) contained in the microstructure and its transformation upon deformation. We have developed a multi-scale model for the hydrogen redistribution during hydrogen charging and tensile loading within martensitic/austenitic microstructure. Ab initio simulations have been used to resolve the complex energy profile of hydrogen in the martensite/austenite interface. Representative microstructures with different amounts of RA have been converted form experimental SEM-EBSD measurements. Simulations with the finite element method (FEM) have been used to analyse H concentration profiles within the microstructure. The simulations confirm an accumulation of H within the austenitic phase during charging, which undergoes a phase transformation under applied mechanical load during tensile testing and releases accumulated H into the martensite matrix. As a result, there is a pronounced H segregation to the microstructure regions subjected to high hydrostatic tensile stresses and plastic strains, which has a strong impact on the embrittlement behaviour. T2 - DPG Frühjahrstagung Sektion SKM CY - Berlin, Germany DA - 17.03.2024 KW - Hydrogen KW - Steel KW - Structural transformation KW - Ab initio simulation KW - Multiscale simulation PY - 2024 AN - OPUS4-62726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hickel, Tilmann T1 - Effect of Hydrogen on the Phase Stability of Steels N2 - In this work, we studied the role of extreme hydrogen concentrations on the relative stability of the fcc/bcc/hcp phases using the ab initio thermodynamics. The results indicate that at low hydrogen chemical potentials the stability of the fcc phase, which can be representative of retained austenite (RA) in steels, is slightly enhanced by the presence of H atoms. In contrast, at high hydrogen chemical potentials the bcc phase is stabilized by H. Moreover, since the excess volume of the hydrogen-rich bcc phase is significantly larger than that of the fcc phase, the presence of a stress field can change the relative stability of these phases in the coexistence regions of the phase diagram. This feature is particularly important for cyclic loading conditions: during loading cycles forward and reverse phase transformations occur and the H released by these transformations can damage the material. T2 - TMS Annual Meeting 2024 CY - Orlando, FL, USA DA - 03.03.2024 KW - Hydrogen KW - Ab initio thermodynamics KW - Multiscale simulation KW - Hydride formation KW - Workflow PY - 2024 AN - OPUS4-62730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hickel, Tilmann T1 - Fundamental insights into the mechanism of hydrogen embrittlement N2 - The talks starts with a study on H trapping and embrittlement in high-strength Al alloys. Then the phase stability and transformation between different Fe-H phases is discussed, together with implications on crack nucleation. In the last part MD-MC simulation of hydride formation at crack tips in Al alloys are shown. T2 - Integrated Computational Materials, Process and Product Engineering Conference, IC-MPPE CY - Leoben, Austria DA - 06.06.2024 KW - Hydrogen KW - Ab initio thermodynamics KW - Multiscale simulation KW - Hydride formation KW - Cracks PY - 2024 AN - OPUS4-62727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chakraborty, P. A1 - Mouton, I. A1 - Gault, B. A1 - Tehranchi, Ali A1 - Neugebauer, J. A1 - Hickel, Tilmann T1 - Effect of Sn on stacking fault energies in zirconium and its hydrides N2 - Hydrogen embrittlement in Zr-alloy fuel cladding is a primary safety concern for water-based nuclear reactors. Here we investigated the stabilization of planar defects within the forming hydrides by Sn, the primary alloying element of Zircaloy-4 used in the cladding. In order to explain the formation of hydrides and planar defects observed in our experiments, we performed atomic-scale ab initio calculations focusing on the solute interactions with generalized stacking faults in hcp 𝛼-Zr and fcc zirconium hydrides. Our calculations showed that an increase in Sn concentration leads to a stabilization of stacking faults in both the 𝛼-Zr and hydride phases. However, the solution enthalpy of Sn is lower in the 𝛼-Zr as compared to the other hydride phases, indicative of two competing processes of Sn depletion/enrichment at the Zr hydride/matrix interface. This is corroborated by experimental findings, where Sn is less soluble in hydrides and is mostly found trapped at interfaces and planar defects, indicative of stacking faults inside the hydride phases. Our systematic investigation enables us to understand the presence and distribution of solutes in the hydride phases, which provides a deeper insight into the microstructural evolution of such alloy's properties during its service lifetime. KW - Defects KW - First-principles calculations KW - Interface and surface thermodynamics KW - Microstructure KW - Hydrides KW - Structural properties PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618044 DO - https://doi.org/10.1103/PhysRevMaterials.8.033605 SN - 2475-9953 VL - 8 IS - 3 SP - 1 EP - 9 PB - APS AN - OPUS4-61804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böttcher, Nils A1 - Dayani, Shahabeddin A1 - Markötter, Henning A1 - Bau, Alexander A1 - Setzchen, Max A1 - Schmidt, Anita A1 - Kowal, Julia A1 - Krug von Nidda, Jonas T1 - High Precision Nail‐Penetration Setup for the Controlled Thermal Runaway Initiation of Lithium‐Ion Cells at Very Low Temperatures N2 - A high precision nail‐penetration (NP) tool for characterizing the mechanically induced thermal‐runaway (TR) of lithium‐ion battery (LIB) cells in a defined range of temperatures down to −140 °C was developed. To understand the cell specific behavior at low temperatures aiming at the determination of safe handling conditions, different scenarios are analyzed. First, accuracy tests of the NP‐tool regarding motion and penetration depth are conducted with cylindrical cells at different temperatures. Thus, postmortem computer tomographic (CT) images are compared to the data measured with the newly integrated 3‐axis force sensor which is further combined with a high‐resolution position sensor. The herein developed setup allows evaluation of the NP‐metrics at an accuracy of ±1 pierced electrode layer without CT‐scans. Further NP examinations at 20 °C of fully charged cylindrical lithium nickel manganese cobalt oxide cells reveal a reproducible minimum damage as a reliable TR‐trigger. Moreover, NP‐tests at low temperature disclose a relation of the short circuit conductivity and TR‐reactions during subsequent rethermalization to room temperature. Finally, the implementation of a novel fixture for a controlled very fast cooling of LIB‐cells during critical damage opens the way to investigate the individual steps during a TR and, thus, to gain important information of the specific TR‐mechanism of different LIB‐cells. KW - Battery Safety KW - High-precision nail penetration KW - Lithium-ion batteries KW - Abuse testing KW - Thermal runaway PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598127 DO - https://doi.org/10.1002/ente.202301379 SN - 2194-4288 SP - 1 EP - 13 PB - Wiley VHC-Verlag AN - OPUS4-59812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leonhardt, Robert A1 - Böttcher, Nils A1 - Dayani, Shahabeddin A1 - Rieck, Arielle A1 - Markötter, Henning A1 - Schmidt, Anita A1 - Kowal, Julia A1 - Tichter, Tim A1 - Krug von Nidda, Jonas T1 - Exploring the electrochemical and physical stability of lithium-ion cells exposed to liquid nitrogen N2 - The transport and storage of lithium-ion (Li-ion) batteries — damaged or in an undefined state — is a major safety concern for regulatory institutions, transportation companies, and manufacturers. Since (electro)chemical reactivity is exponentially temperature-dependent, cooling such batteries is an obvious measure for increasing their safety. The present study explores the effect of cryogenic freezing on the electrochemical and physical stability of Li-ion cells. For this purpose, three different types of cells were repeatedly exposed to liquid nitrogen (LN2). Before and after each cooling cycle, electrical and electrochemical measurements were conducted to assess the impact of the individual freezing steps. While the electrochemical behavior of the cells did not change significantly upon exposure to LN2 , it became apparent that a non-negligible number of cells suffered from physical changes (swelling) and functional failures. The latter defect was found to be caused by the current interrupt device of the cylindrical cells. This safety mechanism is triggered by the overpressure of expanding nitrogen which enters the cells at cryogenic temperatures. This study underlines that the widely accepted reversibility of LN2 -cooling on a material scale does not allow for a direct extrapolation toward the physical integrity of full cells. Since nitrogen enters the cell at cryogenic temperatures and expands upon rethermalization, it can cause an internal overpressure. This can, in turn, lead to mechanical damage to the cell. Consequently, a more appropriate temperature condition — less extreme than direct LN2 exposure — needs to be found KW - Lithium-ion battery KW - LN2 cooling KW - Battery characterization PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599248 DO - https://doi.org/10.1016/j.est.2024.111650 VL - 89 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-59924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böttcher, Nils A1 - Dayani, Shahabeddin A1 - Markötter, Henning A1 - Schmidt, Anita A1 - Kowal, J. A1 - Lu, Y. A1 - Krug von Nidda, Jonas A1 - Bruno, Giovanni T1 - Visualization of stepwise electrode decomposition in a nail penetrated commercial lithium-ion cell using low-temperature synchrotron X-ray computed tomography N2 - The transition towards zero carbon emissions in power generation hinges on the integration of efficient electrical energy storage systems, with lithium-ion batteries (LIBs) positioned as a pivotal technology. While generally safe, deviations in their operational guidelines due to manufacturing defects or misuse can lead to critical safety concerns, notably thermal runaway (TR) events. Internal short circuits (ISCs) are primary initiators of TR within LIBs. For abuse testing, ISCs are often triggered by nail penetration. This study explores the morphological changes and mechanisms underlying ISC-induced TR in LIBs using operando synchrotron X-ray computed tomography (SXCT) at subzero temperatures. A novel cryogenic setup was developed to control a stepwise temperature increase in the damaged sample while monitoring electrochemical characteristics and simultaneously enabling acquisition of high-resolution SXCT images. The findings reveal that conducting nail penetration at minus 80°C prevents immediate TR, enabling detailed analysis of subsequent structural and electrochemical behavior during controlled thawing. Thus, the initiation of TR processes at localized ISC sites has been observed, evidenced by voltage fluctuations and morphological changes, such as cathode material cracking and decomposition. These results underscore the importance of temperature control in mitigating TR risks and provide critical insights into the internal dynamics of LIBs under abusive conditions. The developed cryogenic SXCT methodology offers a powerful tool for non-destructive, high-resolution investigation of battery failure mechanisms, contributing to the enhancement of LIB safety. KW - Tomography KW - X-ray imaging KW - Lithium-ion battery PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611327 DO - https://doi.org/10.1016/j.jpowsour.2024.235472 VL - 623 SP - 1 EP - 10 PB - Elsevier CY - New York, NY AN - OPUS4-61132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Appel, Paul Alexander T1 - Developing Tailor-Made Core-Shell Carbon Anode Materials for Sodium Ion Batteries N2 - Hard carbons (HCs) are currently one of the most promising anode materials for sodium-ion batteries (SIBs). However, the Na storage mechanism remains controversial, leaving the theoretical limits of carbon anodes unclear. To deconvolute the specific capacity from irreversible capacity losses, resulting from the formation of solid electrolyte interphase (SEI), core-shell carbon materials were synthesized. Based on these core-shell materials, extensive operando characterization was developed and undertaken to investigate the storage mechanism of sodium. T2 - Sodium Ion Battery Symposium CY - Berlin, Germany DA - 23.09.2024 KW - Energy Materials PY - 2024 AN - OPUS4-62005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sander, Luise T1 - Commercially Available Sodium-Ion Cells: Multi-Scale Analysis and Material Characterisation N2 - As the first commercial sodium-ion-batteries (SIBs) are available for purchase, it is possible to investigate material composition. Gaining an insight into the material composition of these SIBs is of interest not only for the classification of possible safety risks and hazards, but also in regards to recycling. Herein we report the preliminary investigations of the chemical and structural composition of first commercial SIB-cells. Two different SIB-cells with different specification were compared regarding electrode size, thickness and further parameters. Furthermore, the composition of the active materials and electrolyte was investigated and compared. T2 - Adlershofer Forschungsforum 2024 CY - Berlin, Germany DA - 11.11.2024 KW - Sodium-Ion KW - Multi-Scale Analysis PY - 2024 AN - OPUS4-61757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bäßler, Ralph A1 - Amela Keserović, Amela A1 - Sobetzki, Joana A1 - Sarmiento Klapper, Helmuth A1 - Dimper, Matthias T1 - Geeignete Werkstoffe für Geothermieanwendungen (1) N2 - Durch Auslagerungs- und elektrochemische Tests im Labor kann das Korrosionsverhalten verschiedener metallener Werkstoffe beurteilt werden. Aus den Versuchsergebnissen, die in verschiedenen synthetischen Geothermalwässern im Labor erzielt wurden, lassen sich die folgenden Schlussfolgerungen ziehen: • Die Anfälligkeit für Spaltkorrosion wurde als wichtigster Aspekt für die Werkstoffqualifizierung ermittelt. • Der niedriglegierte Stahl 25CrMo4 zeigte bei niedrigem Salzgehalt in MB-Geothermalwasser eine gleichmäßige Korrosion unterhalb der akzeptierten Schwelle von 0,3 mm/Jahr. Daher kann er als geeignet für geothermische Bedingungen mit niedrigem Salzgehalt angesehen werden, wie sie für MB getestet wurden. Es besteht keine Notwendigkeit, auf höherlegierte (teurere) Werkstoffe auszuweichen. Ein niedrigerer pH-Wert (wie bei LHD) führt zu Korrosionsraten oberhalb der akzeptablen Grenzwerte, so dass die niedriglegierten Werkstoffe nicht für Flüssigkeiten mit niedrigem pH-Wert geeignet sind. • Stark salzhaltige Geothermalwässer erfordern höherlegierte Werkstoffe, da die Korrosionsrate von niedriglegiertem Stahl zu hoch ist. • Der Duplexstahl X2CrNiMo22-5-3 und der Superduplexstahl X2CrNiMoCuWN25-7-4 wurden aufgrund ihrer kritischen Anfälligkeit für örtliche Korrosion in Form von Loch- und Spaltkorrosion unter Betriebsbedingungen nicht als geeignet für geothermische Anwendungen in Geothermalwässern mit einer mit NDB und ORG vergleichbaren Zusammensetzung angesehen. • Der superaustenitische Stahl X1CrNiMoCu32-28-7 eignet sich für ORG und salzarme Wässer. In NDB-Geothermalwasser wurde er bei 100 °C als geeignet angesehen. Jedoch schränkt seine Anfälligkeit für Spaltkorrosion seine Anwendbarkeit ein. Neben seiner guten Korrosionsbeständigkeit ist sein Repassivierungsverhalten für seine begrenzte Anwendbarkeit in Geothermalwässern mit niedrigem pH-Wert verantwortlich. • Die Nickelbasislegierung NiCr23Mo16Al wurde als geeignet erachtet und stellt eine sichere Option für den Einsatz in geothermischen Anlagen dar, selbst wenn mit stark salzhaltigem Geothermalwasser gearbeitet wird. KW - Geothermie KW - Korrosion KW - Legierungen KW - Anlagensicherheit PY - 2024 SN - 0016-4232 VL - 2024 IS - 2 SP - 240 EP - 243 PB - Eugen G. Leuze Verlag CY - Bad Saulgau AN - OPUS4-59996 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sander, Luise T1 - Multi-Scale Analysis of Commercially Available Sodium-Ion Cells N2 - As the first commercial sodium-ion-batteries (SIBs) are available for purchase, it is possible to investigate material composition. Gaining an insight into the material composition of these SIBs is of interest not only for the classification of possible safety risks and hazards, but also in regards to recycling. Herein we report the preliminary investigations of the chemical and structural composition of first commercial SIB-cells. Two different SIB-cells with different specification were compared regarding electrode size, thickness and further parameters. Furthermore, the composition of the active materials and electrolyte was investigated and compared. T2 - Solid State Ionics (SSI) CY - London, United Kingdom DA - 15.07.2024 KW - Sodium Ion-Cells KW - Multi-Scale PY - 2024 AN - OPUS4-60764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Negative Electrode Ionophoric Core-Shell Carbon for Sodium-Ion Batteries N2 - The current strong interest in electromotive mobility and the need to transition to an energy grid with sustainable storage devices has led to a renewed interest in sodium ion batteries (SIBs). Amorphous disordered carbons such as hard carbons (HCs) are promising candidates for high-capacity negative electrode materials in SIBs. Their high capacities, however, are often accompanied with high irreversible capacity losses during the initial cycles,[1] while low initial losses are accompanied with moderate capacities.[2] In our research we are aiming morphologically and chemically functional carbons. Morphologically, our target is a local separation of reversible sodium storage and irreversible losses in novel synthetic carbon anodes, using a core-shell concept. On chemical side, we aim at ion-binding functional groups. We investigated different methods to obtain core-shell structures to restrict SEI formation to the external particle surface, while leveraging the Na storage potential of porous carbon core materials. Moreover, we apply active-site imprinting to realise disting ion-binding features into the core carbons. The electrochemical performance of those materials can be rather easily altered upon removing/exchanging the ions bound to the functional group. Herein, we will focus on the synthesis of zeolitic imidazolate framework (ZIF) based NDCs. Different analytical methods, e.g., physisorption (N2, Ar, CO2), XPS, XAS, and NMR, will be used to understand the alteration of morphological and chemical features upon ion exchange. T2 - Mat-Sus Spring Meeting 2024 CY - Barcelona, Spain DA - 04.03.2024 KW - Ionophoric carbon PY - 2024 AN - OPUS4-61938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Menga, Davide A1 - Li, Yan‐Sheng A1 - Damjanović, Ana Marija A1 - Proux, Olivier A1 - Wagner, Friedrich E. A1 - Fellinger, Tim-Patrick A1 - Gasteiger, Hubert A. A1 - Piana, Michele T1 - On the Stability of an Atomically‐Dispersed Fe−N−C ORR Catalyst: An In Situ XAS Study in a PEMFC N2 - The stability of Fe−N−C oxygen reduction reaction (ORR) electrocatalysts has been considered a primary challenge for their practical application in proton exchange membrane fuel cells (PEMFCs). While several studies have attempted to reveal the possible degradation mechanism of Fe−N−C ORR catalysts, there are few research results reporting on their stability as well as the possible Fe species formed under different voltages in real PEMFC operation. In this work, we employ in‐situ X‐ray absorption near‐edge structure (XANES) to monitor the active‐site degradation byproducts of an atomically dispersed Fe−N−C ORR catalyst under a H2/O2‐operating PEMFC at 90 % relative humidity and 80 °C. For this, stability tests were carried out at two constant cell voltages, namely 0.4 and at 0.8 V. Even though the ORR activity of the Fe−N−C catalyst decreased significantly and was almost identical at the end of the tests for the two voltages employed, the analysis of the XANES recorded under H2/N2 configuration at 0.6 and 0.9 V within the stability test suggests that two different degradation mechanisms occur. They are demetalation of iron cations followed by their precipitation into Fe oxides upon operation at 0.8 V, versus a chemical carbon oxidation close to the active sites, likely triggered by reactive oxygen species (ROS) originated from the H2O2 formation, during the operation at 0.4 V. KW - PGM-free catalysts PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638981 DO - https://doi.org/10.1002/celc.202400228 SN - 2196-0216 VL - 11 IS - 18 SP - 1 EP - 16 PB - Wiley VHC-Verlag AN - OPUS4-63898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Menga, D. A1 - Low, Jian Liang A1 - de Oliveira Guilherme Buzanich, Ana A1 - Paulus, B. A1 - Fellinger, Tim-Patrick T1 - The Tetrapyrollic Motif in Nitrogen Doped Carbons and M-N-C Electrocatalysts as Active Site in the Outer-Sphere Mechanism of the Alkaline Oxygen Reduction Reaction N2 - Development and fundamental understanding of precious-group-metal-free electrocatalysts is hampered by limitations in the quantification of the intrinsic activity of different catalytic sites and understanding the different reaction mechanisms. Comparing isomorphic nitrogen-doped carbons, Zn-N-Cs and Fe-N-Cs with the common tetrapyrrolic motif, a catalyst-independent outer-sphere rate-determining step in the alkaline oxygen reduction reaction is observed. Density functional theory (DFT) simulations on tetrapyrrolic model structures indicate the highest occupied molecular orbital (HOMO) level as a good descriptor for the catalytic activity. Contour plots suggest that the electron transfer occurs directly from the tetrapyrrolic coordination site, rather than from the metal center. Metal-free tetrapyrrolic N4 sites are discovered to be highly active oxygen reduction reaction (ORR) active sites in alkaline that reach turnover frequencies (TOF) of 0.33 and 1.84 s−1 at 0.80 and 0.75 VRHE in the order of magnitude of tetrapyrrolic Fe–N4 sites in the acidic ORR. While Zn-coordination lowers the HOMO level and therefore the catalytic activity, Fe-coordination lifts the HOMO level resulting in TOF values of 0.4 and 4 s−1 for tetrapyrrolic Fe–N4 sites at 0.90 and 0.85 VRHE, respectively. At higher mass activities, the peroxide reduction becomes rate-limiting, where highest peroxide production rates are observed for the nitrogen-doped carbon. KW - Tetrapyrollic KW - Motif KW - Nitrogen KW - Carbons KW - Alkaline Oxygen PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606239 DO - https://doi.org/https://doi.org/10.1002/aenm.202400482 SN - 1614-6832 VL - 2024 SP - 1 EP - 8 PB - Wiley-VCH AN - OPUS4-60623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwarz, I. A1 - Rieck, Arielle A1 - Mehmood, Asad A1 - Bublitz, R. A1 - Bongers, L. A1 - Weuster-Botz, D. A1 - Fellinger, Tim-Patrick T1 - PEM Electrolysis in a Stirred-Tank Bioreactor Enables Autotrophic Growth of Clostridium ragsdalei with CO2 and Electrons N2 - Acetogenic bacteria produce CO2-based chemicals in aqueous media by hydrogenotrophic conversion of CO2, but CO is the preferred carbon and electron source. Consequently, coupling CO2 electrolysis with bacterial fermentation within an integrated bio-electrocatalytical system (BES) is promising, if CO2 reduction catalysts are available for the generation of CO in the complex biotic electrolyte. A standard stirred-tank bioreactor was coupled to a zero-gap PEM electrolysis cell for CO2 conversion, allowing voltage control and separation of the anode in one single cell. The cathodic CO2 reduction and the competing hydrogen evolution enabled in-situ feeding of C. ragsdalei with CO and H2. Proof-of-concept was demonstrated in first batch processes with continuous CO2 gassing, as autotrophic growth and acetate formation was observed in the stirred BES in a voltage range of 􀀀 2.4 to 􀀀 3.0 V. The setup is suitable also for other bioelectrocatalytic reactions. Increased currents and lower overvoltages are however requ KW - PEM KW - Stirred-Tank Bioreactor KW - Clostridium ragsdalei PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615239 UR - http://www.chemelectrochem.org/ DO - https://doi.org/10.1002/celc.202300344 VL - 11 IS - 6 SP - 1 EP - 9 PB - Chemistry Europe and Wiley-VCH GmbH AN - OPUS4-61523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krug von Nidda, Jonas T1 - Core-Shell Materials as Advanced Anodes for Sodium Ion Batteries N2 - The current imperative to shift towards an energy grid equipped with sustainable energy storage solutions has caused a renewed interest in sodium-ion batteries (SIBs). Hard carbons (HCs) are a promising option high-capacity anode materials in SIBs. Nevertheless, their elevated capacities frequently come at the cost of experiencing substantial non-reversible initial capacity losses. Commonly, significant losses are associated with irreversible reactions, such as the creation of the solid electrolyte interphase (SEI), that occur during the initial sodium insertion in HC-materials. Intriguingly, high values of irreversible capacity are often found for samples with experimentally determined low specific surface area.[1] A more comprehensive understanding of the structure-property relations is essential for quantifying and grasping the potential of hard carbon materials in sodium-ion batteries (SIBs). Thus, the objective is to employ analytical methods to establish a link between the structure and the electrochemical attributes of HC materials. This has been a challenge, partly due to the non-stoichiometric nature of the sodium storage mechanism and the disordered structure of HCs. To address the challenges mentioned above, our approach is to explore whether a core-shell structure can separate sodium storage and SEI-formation. This way, we can investigate and fine-tune storage capacity and irreversible losses, independently. The strategy involves the synthesis of various porous carbon structures to serve as the core material and their combination with sodium-conductive structures to core-shell materials. Herein, we will present different synthesis routes towards tailor-made carbon core materials. Moreover, different coatings concepts will be introduced, and the electrochemical performance of the core and core-shell materials compared. To elucidate the storage mechanism, the results of advanced analytical methods such as operando NMR and SAXS will be presented. Generally, these core-shell anodes promise to enable high capacities accompanied with low irreversible losses due to optimized SEI-formation. T2 - GDCh Electrochemistry 2024 CY - Braunschweig, Germany DA - 16.09.2024 KW - Sodium Ion Batteries KW - Negative Electrodes KW - Core Shell Materials KW - Energy Storage PY - 2024 AN - OPUS4-61145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Valorization of carbon dioxide by the electrocatalytic reduction coupled to acetogens via multiple electron carriers N2 - A summary of the DFG project "Ecat-Acetogens" within the SPP priority programm Ebiotech (2240) was given. The successful developmante of a bioelectrocataltic reactor system based on standard 2l stirred tank bioreactors and common 5cm2 singel cell electrolysis reactors was presnted and first results discussed based on the catlytic properties of a specifically designed cathode catalyst for CO2 reduction. T2 - DFG SPP Statusmeeting Ebiotech 2024 CY - Jena, Germany DA - 22.04.2024 KW - CO2 conversion KW - Bioelectrocatalytic reactor PY - 2024 AN - OPUS4-61939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schwarz, I. A1 - Rieck, Arielle A1 - Fellinger, Tim-Patrick A1 - Weuster-Botz, Dirk T1 - Bio-electrochemical CO2 conversion into organic products using precious-metal free electrocatalysts N2 - For the realization of a sustainable economy, it is of great importance to make use of CO2 for the production of multi-carbon organic chemicals used as feedstock in the chemical industry as well as carbon-neutral fuels (Varela et al. 2019). A promising approach is the electrochemical CO2 reduction followed by microbial conversion of the reduced products. KW - Bio-electrochemical KW - Organic products KW - Electrocatalysts PY - 2024 SP - 1 EP - 2 AN - OPUS4-59572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane T1 - Fluorinated Additives used in LiBs - Forever Chemicals of Tomorrow? N2 - Lithium-ion batteries (LiBs) are increasingly crucial in modern society, serving as advanced portable energy storage systems and playing a vital role in the energy revolution. Despite their importance, challenges such as safety risks, capacity decline, and the need for higher energy density persist. Researchers are exploring the use of fluorinated organic compounds (FOCs) in LiBs electrolytes as a potential solution [1-3]. These compounds, similar to per- and polyfluorinated alkyl substances (PFAS), offer improved oxidative and chemical resistance due to their strong fluorine-carbon bond. However, concerns over their environmental impact remain, as FOCs could persist in the environment or create harmful degradation products, which accumulate and contribute to global health problems. To investigate the environmental fate of two structurally similar and prominent FOCs found in electrolytes, various methods are used to simulate transformation products (TPs). These methods include the TOP (total oxidizable precursor) assay, the Fenton reaction, electrochemistry, photoinduced degradation, and hydrolysis. TPs are identified using gas chromatography and liquid chromatography coupled with high resolution mass spectrometry (GC- and LC-HRMS). First results of this TP screening will be presented. T2 - ISC 2024 CY - Liverpool, GB DA - 06.10.2024 KW - Transformation products KW - Lithium-ion batteries KW - Fluorinated Compounds KW - Gas chromatography/ QTOF-MS KW - Liquid chromatography/ QTOF-MS KW - PFAS PY - 2024 AN - OPUS4-61341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Processing and application properties of multiple principal element alloys (MPEA) N2 - The presentation gives an overview of BAM's activities on processing influences and application properties of MPEAs in the form of joined and machined high and medium entropy alloys (CoCrFeMnNi and CoCrNi). In the case of welding, the focus is on defect-free welded joints with sufficient mechanical properties. In the case of machining, the focus is on the possible influence on the surface quality of the materials through adequate milling parameters. In addition, the hydrogen absorption and diffusion properties as well as the electrochemical corrosion behavior are fundamentally examined. T2 - FAU-Department Werkstoffwissenschaften, Seminar: Aktuelle Probleme der Werkstoffwissenschaften CY - Erlangen, Germany DA - 25.04.2024 KW - Welding KW - Application properties KW - Machining KW - High-entropy alloy KW - Hydrogen PY - 2024 AN - OPUS4-59975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böttcher, Nils T1 - Low Temperature Tomographic In-Situ and Operando Studies in Energy Research N2 - Using low temperatures empowers in-depth investigations of abuse processes in Li-ion cells. A thermal runaway (TR) can be suppressed also on material level at low temperatures.The rethermalization of a critical damaged cell not always leads to a TR. Using the snyergies at BAM enables now In-depth investigation of low temperature inertisation mechanisms in commercial Lithium-Ion-Batteries. In future the synergies will be used for in-depth investigation of other abuse processes in commercial cells e.g., plating or aeging. T2 - HZB Usermeeting CY - Berlin, Germany DA - 11.12.2024 KW - Lithiumbatteries KW - Thermal Runaway KW - Sychrotron computer tomopgrahy KW - Low temperature PY - 2024 AN - OPUS4-62300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tichter, Tim A1 - Böttcher, Nils A1 - Schmidt, Anita A1 - Krug von Nidda, Jonas T1 - Exploring the Low-Temperature Threshold for Reactions in Commercial Lithium-Ion Cells N2 - Low-temperature passivation of lithium-ion batteries (LIBs) can reduce the probability of thermal runaway events [1]. In this context, we explore the thermal threshold at which reactions in commercial Li-cells become feasible. It is found that electrochemical reactions take place even below the first phase transition of the electrolyte. Finally, it is concluded that the passivation temperature for all samples in our study does not require cryogenic conditions which is of great relevance for defining the conditions for a safe transportation. T2 - Advanced Battery Power Konferenz CY - Münster, Germany DA - 10.04.2024 KW - Batteries KW - Thermal passivation KW - Arrhenius-law KW - Cyclic voltammetry KW - Chronoamperometry PY - 2024 AN - OPUS4-62307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Comparative chemical analysis of Ni-Fe oxide nanoparticles N2 - Ni-Fe oxide nanoparticles have gained a lot of interest because of their high activity in the oxygen evolution reaction (OER) which is crucial for water splitting. [1] Although there have been great efforts in the last years, the understanding of the synergistic effect between Fe and Ni is still under discussion. Therefore, we prepared different Ni-Fe oxide nanoparticles with different compositions from pure iron oxide to pure nickel oxide adapting a known procedure. [2,3] Size and morphology of the nanoparticles depend on the composition which was shown with Transmission Electron Microscopy (TEM). The compositions of the nanoparticles were measured with a comparative approach using X-ray Photoelectron Spectroscopy (XPS), Hard X-ray Photoelectron Spectroscopy (HAXPES), and Energy Dispersive X-Ray Spectroscopy (EDS) coupled with the TEM providing detailed chemical information of the nanoparticles in different sample regions. EDS reveals that the different sample regions are dominated by one of the components, Fe or Ni, but a slight mixing between the components can be found (see Figure 1), which was confirmed with X-ray Diffraction (XRD). XPS indicates the enrichment of Fe at the sample surface, while HAXPES and EDS data agree on the stoichiometry of the bulk. High-resolution XPS and HAXPES exhibit some differences in the valence states of Fe and Ni, whereas Ni seems to be easier to reduce than Fe. Further investigations combining these different techniques and additionally Secondary Ion Mass Spectrometry (ToF-SIMS) are ongoing by using in situ approaches and coupling cyclic voltammetry to the analytical techniques. T2 - ECASIA 2024 CY - Gothenburg, Sweden DA - 09.06.2024 KW - Oxygen evolution reaction KW - Transmission Electron Microscopy KW - (Hard) X-ray Photoelectron Spectroscopy KW - Synergistic effects PY - 2024 AN - OPUS4-60534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - In situ tomographic imaging with hard x rays at Bamline (BESSY II) N2 - The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science [1]. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography (SXCT) with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented. In series-connected lithium-ion cells are susceptible to an electrical safety hazard called over-discharge. Here the behavior of copper dissolution and deposition during over-discharge is presented, which leads to irreversible loss of capacity and internal short circuits. The concentration of dissolved and deposited copper is quantified. Also, a non-uniform distribution pattern of copper deposition on the cathode is shown. The second example deals with an Al alloy 7017 customized for a 3d-printing process by means of laser-based powder bed fusion (PBF-LB) technique. These advanced alloys have a significantly higher modulus of elasticity than conventional Al alloys, making them attractive for applications requiring high stiffness. SXCT during In-situ tensile tests confirmed that fracture initiation strongly depends on defects created during printing. However, the cracks are deflected from decohesion around inclusions/precipitates embedded in the Al matrix, increasing ductility. Low temperature cofired ceramic (LTCC) multilayer housings offer 3D-circuits for a wide range of applications in telecommunications, microsystems and sensor technology. Such housings are produced by combining structured and metallized ceramic layers using tape-casting and multilayer technology. The characterization of the integrity, deformation, defects, and positioning of the internal metal features was carried out using in-situ SXCT at up to 950°C. A high-precision nail penetration tool was developed to characterize the mechanically induced thermal runaway (TR) of lithium-ion battery (LIB) cells in a dynamic temperature range down to -190 °C. To investigate safety-specific low-temperature transport conditions, the damaged cells were tomographically imaged during thawing. T2 - ICTMS - International Conference on Materials and Structures 2024 CY - Cape Town, South Africa DA - 01.07.2024 KW - Synchrotron radiation KW - X-ray tomography KW - Li-ion battery PY - 2024 AN - OPUS4-60658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scharpmann, Philippa T1 - Segregating the Degradation Mechanisms in Lithium-Ion Cells during Strongly Accelerated Ageing with Critically Extended Voltage Ranges N2 - Repurposing end-of-life (EOL) lithium-ion batteries from mobile applications, such as electric vehicles, is of utmost importance for a sustainable handling of scarce resources. For an economically and ecologically desirable reuse of aged batteries in second-life applications, a guarantee for safe and reliable operation is urgently required. However, the assessment of the state of safety (SOS) is not straightforward, as multiple abuse cases, variables and interactions need to be considered [1]. Therefore, defining safety parameters and test procedures, as well as determining the SOS requires a plethora of aged cells to be tested. In this study, a novel method of greatly accelerating the ageing process of lithium-ion batteries is proposed. Overcharging and overdischarging are embedded in cyclic ageing, continuously employing a depth of discharge larger than 100 %. Different electrical abuse conditions (overcharge, overdischarge, high current rates) are applied on lithium-ion NMC and LFP pouch cells in a preliminary test series. In this manner, the cells are stressed until a cell failure or a thermal runaway is induced. Thus, the critical state in proximity to a cell failure is spotted for individual and combined stress parameters. Based on this knowledge, a test protocol for strongly accelerated ageing with cell-specific, abusive electrical parameters is developed. The aging dynamics under these critical conditions are monitored by systematic capacity, open circuit voltage and electrochemical impedance spectroscopy (EIS) measurements. This enables an assessment of the degradation mechanisms induced by overdischarge and overcharge cycling. A special focus is set on the comparative assessment of the electrical behaviour, following conventional vs. greatly accelerated ageing. This novel method is suitable for providing cells with a defined SOH at a reasonable timescale. Furthermore, the results are of high relevance for the evaluation to which degree cyclic ageing can be accelerated without changing the characteristic degradation mechanisms of lithium-ion batteries. T2 - Advanced Battery Power Conference 2024 CY - Münster, Germany DA - 10.04.2024 KW - Lithium-Ion Battery KW - Safety KW - Ageing PY - 2024 AN - OPUS4-61492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Overview of Battery Research Activities at BAM N2 - An overview on battery research activities of BAM was given using a seletion of activities of all work packages within the field of activity EES and selected activities of divsion 3.6. T2 - Boot Camp of the BAccara Graduate School on Batteries CY - Bad Sassendorf, Germany DA - 24.04.2024 KW - State of Safety KW - Compositional traceability KW - Sustainable energy materials KW - Sodium Ion Batteries PY - 2024 AN - OPUS4-61940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Chemie der Energiewende N2 - Es wurde ein Überblick über die BAM-Aktivitäten im Bereich Chemie der Energiewende gegeben. Dabei wurde ein Fokus auf Aktivitäten in Aktivitätsfeld EES und im Fachbereich 3.6 gelegt. T2 - 30 Jahre Naturwissenschaftliches Studium in Zittau CY - Zittau, Germany DA - 13.04.2024 KW - Chemie KW - Energiewende PY - 2024 AN - OPUS4-61941 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Sodium-Ion Battery Research and Testing at BAM N2 - An overview of activities at BAM on the topic of sodium ion batteries was given. Examples of the internal SIB-links project were given and a focus on novel synthetic anodes. T2 - Sodium Battery Sympoium-5 (2024) CY - Berlin, Germany DA - 23.09.2024 KW - Sodium ion batteries KW - Synthetic carbon anodes PY - 2024 AN - OPUS4-61944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick A1 - Krug von Nidda, Jonas T1 - Porous „Ionophoric“ Carbon Materials: Synthesis Routes and Electrochemical Applications N2 - Porous carbon materials play an important role for energy storage and conversion, e.g., as fuel cell catalysts, supercapacitor or battery electrodes. Tuning porosity features such as pore connectivity, specific surface area, maximum pore size and pore volume is one of the key strategies to improve the performance of those materials.[1] Moreover, the alteration of the chemistry allows further enhancement in performance, even leading to the applicability in new fields. In this context, nitrogen doped carbons (NDCs) are a very promising material class. Highly porous NDCs for example show interesting Na-storage features.[2] Moreover, the integration of iron ions in an NDC, forming FeN4-sites, can results in materials with very promising properties as fuel cell cathode catalysts.[3] However, to relate certain sites to specific performance indicators is still challenging as the variation of the present N-sites is very large in typically obtained NDCs. In the past, we were able to develop an ionothermal synthesis strategy which results in highly porous materials with specific, i.e., tetrapyrrolic, N4-sites.[4] Such N4 sites and there metal complexes are reminiscent of biomolecules like the heme molecule, which originally inspired the research on such materials.[5] The N4-sites are mainly occupied by Zn2+ as the synthesis is performed in a ZnCl2-containing salt melt. Moreover, the electrochemical performance of those materials can be rather easily altered upon removing/exchanging the Zn2+. Moreover, again looking at biomolecules, those kind of materials can be regarded as ionophoric carbons as they possess distinct, metal-binding N4-sites embedded in a carbon matrix. Herein, we will focus on the synthesis of zeolitic imidazolate framework (ZIF) based NDCs with high porosity. We will discuss different strategies to remove and/or exchange Zn2+ in the obtained ZnN4-containing materials. Different analytical methods, e.g., physisorption (N2, Ar, CO2), XPS, XAS, and NMR, will be used to understand the alteration of morphological and chemical features upon ion exchange (see Figure 1). Figure 1: A) Schematic illustration of the partial Zn-removal in a ZnN4-containing, ionophoric carbon. B) High resolution N 1s XPS-results of a ZIF-derived ionophoric carbon before and after metal leaching. Due to the ion exchange/removal, the chemistry of the NDCs is altered, however, typically preserving the porosity features as well as the general structure of the N-motifs. Thus, the influence of the occupancy of the N4-sites on the electrochemical performance can be studied in detail. Finally, structure-property-relations of the different ZIF-derived ionophoric NDCs regarding the performance as anodes in sodium ion batteries will be discussed. T2 - Deutsche Zeolith-Tagung 2024 CY - Jena, Germany DA - 28.02.2024 KW - Ionophoric carbon KW - Sodium ion battery KW - PGM-free catalysts PY - 2024 AN - OPUS4-61955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - DialySorb und Eigenschaften kommerzieller Zellen N2 - In dem Vortrag wurden zunächst die Eigenschaften erster kommerzieller Natrium-Ionen-Batterien vorgestellt, die an der BAM elektrotechnisch untersucht wurden und auf ihre Bestandteile hin analysiert wurden. Weiterhin wurden die aktuellen Projektergebnisse des BMBF-geförderten Verbundprojekts Dialysorb vorgestellt. T2 - KLiB-Gesprächsrunde zu Natrium-Ionen-Batterien und Festkörperbatterien CY - Frankfurt am Main, Germany DA - 09.07.2024 KW - Natrium-Ionen-Batterien PY - 2024 AN - OPUS4-61942 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Leveraging the Potential of Na-Ion-Batteries with Tailormade Anodes N2 - The concept of sodium-ion-batteries and their expected impact for the energy change is introduced, by explaining differences to lithium-ion-batteries. The challenge as well as the potential may be illustrated on the example of novel carbon anodes.While the general suitability is proven since the recent commercialization, limitations and detailed structure-performance relations remain topic to research. The progress in activities of BAM division 3.6 are illustrated further supporting the future impact of the technology. T2 - TechConnect Adlershof 2024: Sustainable Energy Future CY - Berlin, Germany DA - 09.11.2024 KW - Synthetic Carbon Anodes PY - 2024 AN - OPUS4-61947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Research on Synthetic Anodes for Na-Ion-Batteries N2 - Carbons with an amorphous structure are currently revisited as candidates for Li- and Na-ion batteries. High irreversible capacities (due to SEI formation) were considered an intrinsic problem of such hard carbons, rendering them irrelevant for practical use. Amorphous carbon anodes would present safety-related advantages such as lower heat dissipation throughout lithiation per mol of lithium, mechanical stability throughout cycling and a larger set of optional electrolytes. T2 - Advanced Automotive Battery Conference Europe 2024 CY - Strasbourg, France DA - 13.05.2024 KW - Synthetic Carbon Anodes PY - 2024 AN - OPUS4-61956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geisler, J. T1 - The Influence of Interface Modification on Gassing of Sodium Ion Battery Anodes N2 - This flash talk will briefly introduce the DEMS method[3,4] and highlight a recent piece of our research from the DIALYSORB project. Fitting to the main topic of the conference, interfaces, we will present and the measurement technique to understand the side reactions occurring at this interface and recent data on anode materials with designed interface and interphase. T2 - Humboldt Universität zu Berlin CY - Berlin, Germany DA - 17.09.2024 KW - Gasing of Sodium KW - Ion Battery KW - Anodes PY - 2024 AN - OPUS4-60811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krug von Nidda, Jonas T1 - Separating Initial Loss from Storage Capacity: Core-Shell Materials as Advanced Anode Materials for Sodium Ion Batteries N2 - The current imperative to shift towards an energy grid equipped with sustainable energy storage solutions has caused a renewed interest in sodium-ion batteries (SIBs). Hard carbons (HCs) are a promising option high-capacity anode materials in SIBs. Nevertheless, their elevated capacities frequently come at the cost of experiencing substantial non-reversible initial capacity losses Commonly, significant losses are associated with irreversible reactions, such as the creation of the solid electrolyte interphase (SEI), that occur during the initial sodium insertion in HC-materials. Intriguingly, high values of irreversible capacity are often found for samples with experimentally determined low specific surface area.[1] A more comprehensive understanding of the structure-property relations is essential for quantifying and grasping the potential of hard carbon materials in sodium-ion batteries (SIBs). Thus, the objective is to employ analytical methods to establish a link between the structure and the electrochemical attributes of HC materials. This has been a challenge, partly due to the non-stoichiometric nature of the sodium storage mechanism and the disordered structure of HCs. To address the challenges mentioned above, our approach is to explore whether a core-shell structure can separate sodium storage and SEI-formation. This way, we can investigate and fine-tune storage capacity and irreversible losses, independently. The strategy involves the synthesis of various porous carbon structures to serve as the core material and their combination with sodium-conductive structures to core-shell materials. Herein, we will present different synthesis routes towards tailor-made carbon core materials. Moreover, different coatings concepts will be introduced, and the electrochemical performance of the core and core-shell materials compared. To elucidate the storage mechanism, the results of advanced analytical methods such as operando NMR and -SAXS will be presented. Generally, these core-shell anodes promise to enable high capacities accompanied with low irreversible losses due to optimized SEI-formation. T2 - Advanced Battery Power Conference 2024 CY - Münster, Germany DA - 10.04.2024 KW - Battery KW - Anode KW - Hard Carbon PY - 2024 AN - OPUS4-61968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Shu-Han T1 - Synthetic Carbon Anodes for SIBs N2 - Hard carbon (HC) is currently one of the most promising anode materials for sodium-ion batteries (SIBs). However, the Na storage mechanism remains controversial, leaving the theoretical limits carbon anodes unclear. To deconvolute the specific capacity from irreversible capacity losses resulting from the formation of solid electrolyte interphase (SEI), core-shell carbon materials with tailored pore structure and defined surface functionalities are synthesized. Meanwhile, these synthetic designer carbons could achieve more competitive capacities for use as better anodes for SIBs. T2 - Adlershofer Forschungsforum (AFF) CY - Berlin, Germany DA - 11.11.2024 KW - Na-ion Battery PY - 2024 AN - OPUS4-61998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Shu-Han T1 - Mole sieving, artificial cathode electrolyte interphase enables stable cycling of room temperature sodium sulfur cells N2 - Porous carbon particles derived from zeolitic imidazolate framework (ZIF-8) were used as a matrix to improve the electrode conductivity and buffer the volume change of sulfur (S). In addition, the porous carbon particles were coated with an additional ion-sieving tailor-made covalent organic framework (COF) shell, which can be regarded as an artificial cathode electrolyte interphase (CEI). The introduced shell can avoid polysulfides from dissolving in the ether-based electrolyte, thus, preventing the shuttling of polysulfides. The as-synthesized sulfur-infiltrated core-shell cathode delivers a reversible capacity of 975 mAh gS–1 (@C/33) and a reasonable rate capability. T2 - 5th International Sodium Battery Symposium, SBS-5 CY - Berlin, Germany DA - 23.09.2024 KW - NaS Battery PY - 2024 AN - OPUS4-61992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon T1 - X-Ray Absorption Spectroscopy to Reveal the „Molecular“ Structure of Metal and Nitrogen doped Carbon Electrocatalysts N2 - High-performance electrocatalysts and sodium-ion (Na+) storage materials for Na-ion batteries anodes are required for energy conversion and storage systems. Metal and nitrogen enriched carbons (M-N-Cs) are promising candidates as they are conductive and can be tuned to the desired properties by appropriate modification. Structural characterization is essential to understand and optimize the active sites at the pseudo-molecular level and the storage of Na+ in the anode T2 - Bessy User Meeting CY - Berlin, Germany DA - 11.12.2024 KW - Single-atom-catalyst KW - Electrochemistry KW - Porous carbons PY - 2024 AN - OPUS4-62074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Falahat, A. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Kupsch, Andreas A1 - Woracek, R. A1 - Alrwashdeh, S. A1 - Manke, I. T1 - Investigation of detector backlighting and other effects in neutron darkfield images N2 - Neutron imaging can provide unique contrast mechanisms. In order to yield reliable and reproducible attenuation coefficients for quantification, one needs to fully understand and characterize the experimental set-up. One effect that has been largely overlooked in scintillator-camera based neutron imaging systems is the backlight scattering or back illumination in the detection system which can significantly affect the quantification of attenuation coefficients and lead to severe errors and image artifacts. Herein, backlighting is investigated by varying the illuminated detector area and the magnitude of the attenuation. The attenuation coefficient of multiple metal plates was determined by polychromatic neutrons bu the CONRAD V7 instrument. The strength of the back illumination strongly depends upon the sample absorption. While it is relatively moderate (a few percent) for weak absorbing samples, it can be severe when the sample is a strong absorber or thick. KW - Attenuation coefficient KW - Neutron imaging KW - Neutron scattering KW - Polycromatic neutrons KW - Scintillator PY - 2024 SN - 1073-9149 DO - https://doi.org/10.1080/10739149.2024.2380772 SP - 1 EP - 11 PB - Taylor & Francis AN - OPUS4-60752 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - An update on metal seal tests performed at BAM and implications for interim storage N2 - The investigation of the long-term performance of sealing systems employed in containers for radioactive waste and spent nuclear fuel is one research focus area for division 3.4 “Safety of Storage Containers” at the Bundesanstalt für Materialforschung und -prüfung. Metallic seals are in use in interim storage casks for used fuel and high active waste. Their change in performance over time is of high importance for maintaining safe enclosure. Therefore, investigations on these systems were started at BAM to get a general understanding of the relevant processes. Our investigations comprise investigations on different parameters which influence the seal performance and the main part is focussed on the time and temperature dependent behaviour. In this contribution an update on the performed tests and their respective results will be given in respect to the overview presented in 2020. The understanding of the long-term behaviour of the sealing systems and the performance evaluation during interim storage and subsequent transportation are our goals. T2 - SEDS-Workshop: Sicherheit der längerfristigen trockenen Zwischenlagerung CY - Garching, Germany DA - 15.05.2024 KW - Metal seals KW - Ageing KW - Leakage rate KW - Creep PY - 2024 AN - OPUS4-60640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Correlative analysis with electron microscopy applied in different operating modes (SEM, STEM-in-SEM and TEM) for the accurate morphological characterisation of non-spherical fine nanoparticles N2 - Electron microscopy applied in different operating modes, e.g., SEM, TEM or STEM-in-SEM, is the gold standard method to investigate the exact size and shape of individual nanoparticles. However, when fine nanoparticles with a non-monodisperse size distribution and non-spherical shapes are analysed, achieving an accurate result is challenging. Deviations in size measurements of more than 10% may occur. Understanding of the contrasts and sensitivities characteristic to the individual operating modes of an electron microscope is key in interpreting and evaluating quantitatively the measurement uncertainties needed for an eventual certification of specific nanoparticles via traceable results. Further, beyond the pure measurement, the other components in the analysis workflow with significant impact on the overall measurement uncertainties are the sample preparation and the image segmentation. In the present study the same areas of selected iron oxide fine nanoparticles (<25 nm) as reference nanomaterial (candidate) prepared on substrate for electron microscopy imaging are analysed correlatively with SEM, STEM-in-SEM and TEM with respect to their size and shape distribution. Individual significant measurement uncertainties are discussed, e.g., the sensitivity of secondary electron detectors of InLens-type to the surface morphology, particularly to the presence of an ultrathin organic coating or signal saturation effects on the particle edges, to electron beam exposure, to surface contamination, or the selection of the threshold for image segmentation. Another goal of this study is to establish a basis of analysis conditions which shall guarantee accurate results when both manual and particularly (semi-)automated segmentation approaches are applied. Advantages as well as limitations of the use of different electron microscopy operating modes, applied individually and correlatively, are highlighted. T2 - E-MRS 2024 Spring Meeting CY - Strasbourg, France DA - 27.05.2024 KW - Nanoparticles KW - Electron Microscopy KW - Metrology KW - Imaging KW - Reference materials PY - 2024 AN - OPUS4-60436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rossi, Andrea A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Publisher correction: Development of a one-pot synthesis of rGO in water by optimizing Tour’s method parameters N2 - This is a publisher's correction to the original article "Development of a one-pot synthesis of rGO in water by optimizing Tour’s method parameters" that was published online on 27th September 2024 in "Scientific reports" (DOI: 10.1038/s41598-024-73606-2). PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-617590 DO - https://doi.org/10.1038/s41598-024-77468-6 SN - 2045-2322 VL - 14 IS - 1 SP - 1 PB - Springer Nature CY - London AN - OPUS4-61759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Tests of metallic seals at Bam 3.4 performed over more than 15 years N2 - The investigation of the long-term performance of sealing systems employed in containers for radioactive waste and spent nuclear fuel is one research focus area for division 3.4 “Safety of Storage Containers” at the Bundesanstalt für Materialforschung und -prüfung (BAM) in Germany. The time dependant behaviour of metallic seals, which are employed in interim storage casks for used fuel and high active waste, is of high importance for ensuring safe enclosure. Therefore, investigations on these systems were started at BAM to get a general understanding of the relevant processes. Our investigations comprise investigations on different parameters which influence the seal performance and the main part is focussed on the time and temperature dependent behaviour. In this contribution an overview of the performed tests and their respective results will be given. T2 - 5th sealing workshop by Maestral CY - Avignon, France DA - 05.11.2024 KW - Metal seal KW - Aging KW - Interim storage PY - 2024 AN - OPUS4-62048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Role of Sample Preparation for Accurate and Automated Morphological Analysis of Nanoparticles proven in Interlaboratory Comparison Exercises N2 - Traceable morphological and chemical characterization of nanomaterials with respect to the various possible sizes, size distributions, shapes, and concentrations of real-world nanoparticles (NPs) is a challenging task. Particularly for the nonspherical, non-monodisperse nanoparticles – as typically for most of the commercial particles, including their strong tendency to agglomerate, there is a lack of standard operation procedures providing accurate nanoparticle characterisation. In the framework of the pre-standardisation framework of VAMAS (Versailles Project on Advanced Materials and Standards, www.vamas.org) two interlaboratory comparison (ILC) studies are being carried out under the Technical Working Area (TWA) 34 “Nanoparticle Populations”:i) Project #15 addresses the analysis of the size and shape distribution of TiO2 bipyramidal NPs by traceable imaging methods such as TEM, SEM, STEM-in-SEM, AFM as well as with SAXS as an ensemble method. This ILC is thought as the next level development of the case studies exemplified in the published ISO standards ISO 21363 and ISO 19749. It was agreed to complete the first ILC with the NPs already prepared according to the same procedure on a TEM grid, and, at a later stage, to carry out second ILCs with the same NPs distributed to the participants as liquid suspensions together with protocols for the uniform NP deposition on suited substrates - as developed and optimized within the European project nPSize. Once having good deposition protocols available, the door for automated image analysis gets opened. Corresponding image analysis protocols and reporting templates have been distributed to the ILC participants, too. ii) Project #16: two spherical SiO2 NP samples with bi-modal size distributions in two nominal relative number concentrations were prepared and distributed also as liquid suspensions accompanied by sample preparation, measurement, and image analysis protocols and reporting templates. Here, the NP concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations (relative populations of the two modes). The results of all the participating laboratories, in both ILCs, compiled in comparative representations will be shown and discussed for the first time. The reduction of the measurement uncertainties associated to the size, shape and number-concentration results induced by the significant improvement of the sample preparation on substrates (as single particles with a high-density coverage), combined with welldefined image analysis procedures will be highlighted. T2 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Nanoparticles KW - VAMAS KW - Interlaboratory comparison KW - Sample preparation KW - Nanoparticle concentration PY - 2024 AN - OPUS4-60453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, M. A1 - Kömmling, Anja A1 - Böhning, Martin A1 - Jaunich, Matthias T1 - Ageing of elastomers in air and in hydrogen environment - A comparative study N2 - EPDM, HNBR and FKM materials were exposed at 150 ◦C to air under atmospheric pressure and to hydrogen at 50 bar for different ageing times. All measurements after hydrogen exposure were conducted on samples in degassed condition to assess irreversible effects resulting from that exposure and to compare them to those after ageing in air. Density, hardness, tensile properties, compression set, and hydrogen permeability of all samples were analysed. In both ageing environments, HNBR exhibited the most significant changes of material properties. However, for both EPDM and HNBR, considerably less severe ageing effects were observed under hydrogen in comparison to ageing in air. On the other hand, FKM showed about the same low level of deterioration in both ageing environments but exhibited poor resistance against damage due to rapid gas decompression in hydrogen environment that can lead to seal failure. The obtained results may serve as a guidance toward a better understanding for design and utilisation of elastomeric materials in future hydrogen infrastructure components. KW - Rapid gas decompression KW - Condensed matter physics KW - Hydrogen KW - Sustainability and the environment KW - Rubber sealing KW - Renewable energy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597417 DO - https://doi.org/10.1016/j.ijhydene.2024.03.053 SN - 0360-3199 SN - 1879-3487 VL - 63 SP - 207 EP - 216 PB - Elsevier CY - Oxford AN - OPUS4-59741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Zaghdoudi, M. A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar ED - Altenbach, H. ED - Hitzler, L. ED - Johlitz, M. ED - Merkel, M. ED - Öchsner, A. T1 - Analysis of Heterogeneous Ageing of HNBR O-Rings N2 - Abstract Hydrogenated nitrile butadiene rubber (HNBR) elastomer was thermo-oxidatively aged at different temperatures up to 150 °C. Fourier transform infrared spectroscopy (FTIR), compression stress relaxation (CSR) and international rubber hardness degree (IRHD) microhardness were used to characterise the chemo-mechanical changes of HNBR O-rings during thermo-oxidative ageing. FTIR shows the development of carbonyl, methyl and ester groups but the nitrile content was not affected by ageing. The effect of sample geometry during CSR was investigated. CSR data were converted through integrated kinetic laws. The conversion has proven its sensibility to detect heterogeneous ageing. This was confirmed by the IRHD measure-ments across the section of O-rings. The influence of compression during ageing was assessed through IRHD measurements across the section of compressed and uncom-pressed aged O-rings. The DLO effect was more pronounced in compressed O-rings. By applying the model of Wise et al., theoretical IRHD and oxidation profiles were determined on the basis of IRHD experimental data of compressed O-rings. Good agreements between the experimental and the theoretical IRHD profiles in the core region were obtained. However, near the edge, the theoretical IRHD values were overestimated. KW - Ageing KW - Rubber seals KW - Stress relaxation KW - Modelling PY - 2024 SN - 978-3-031-49042-2 DO - https://doi.org/10.1007/978-3-031-49043-9 SN - 1869-8433 SP - 331 EP - 348 PB - Springer Nature CY - Cham, Switzerland AN - OPUS4-59769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paulus, Daniel A1 - Bresch, Sophie A1 - Moos, Ralf A1 - Schönauer-Kamin, Daniela T1 - Powder aerosol deposited calcium cobaltite as textured P-type thermoelectric material with power factors approaching single crystal values N2 - In this work, the thermoelectric material calcium cobaltite Ca3Co4O9 (CCO), a promising p-type conducting thermoelectric oxide with anisotropic properties, was processed by the powder aerosol deposition method (PAD) to form a dense ceramic CCO film with a thickness in the µm range. The prepared films were characterized regarding their microstructure and thermoelectric properties between room temperature and 900 °C. After heat treatment at 900 °C, the CCO PAD film in-plane shows excellent properties in terms of electrical conductivity (280 S/cm at 900 °C) and Seebeck coefficient (220 µV/K at 900 °C). The calculated power factor in-plane (ab) reaches with 1125 µW/(m K2) 40 % of the single crystal value, surpassing the known-properties of CCO bulk ceramics. Examination of the microstructure shows a strong fiber texture of the film as well as a strong coarsening of the grains during the first heat treatment up to 900 °C. KW - thermoelectrics KW - calcium cobaltite KW - thermoelectric oxide KW - aerosol deposition method (ADM) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606246 DO - https://doi.org/10.1016/j.jeurceramsoc.2024.116717 SN - 0955-2219 VL - 44 IS - 15 SP - 1 EP - 8 PB - Elsevier BV AN - OPUS4-60624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel T1 - In situ bragg edge imaging with neutrons for crystallographic phase and temperature field mapping during tig welding N2 - In Neutron-Bragg-Edge Imaging (NBEI) experiments, we studied the phase transition during butt-welding of martensitic Low Temperature Transformation (LTT) Steel [1]. Tungsten inert gas (TIG) welding was used with a moveable torch allowing for automated weldments. The austenitization in the heat affected zone (HAZ) underneath the welding head could be clearly visualized at λ = 0.39 nm, a wavelength smaller than the Bragg edge wavelengths of both austenite and martensite. Also, the re-transformation upon cooling from austenite into martensitic phase was detected. However, we observed an unexpected additional change in transmission at λ = 0.44 nm that is a wavelength larger than the wavelength of the Bragg edges of both the martensitic and austenitic phases. We attribute this change to the Deybe-Waller-Factor that describes the temperature dependence of coherent scattering at a crystal lattice [2]. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS [3]. Here, the absolute temperature values could be achieved by calibrating the modelled attenuation with help of a thermocouple placed at the steel sample plate. This allows in return for a direct two-dimensional temperature reading based on the Debye-Waller-relation between neutron attenuation and sample temperature. T2 - MSE 2024 CY - Darmstadt, Germany DA - 24.09.2024 KW - In situ neutron Bragg edge imaging KW - Temperature field mapping KW - Crystallographic phase mapping KW - TIG welding PY - 2024 AN - OPUS4-61268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eddah, Mustapha A1 - Markötter, Henning A1 - Mieller, Björn A1 - Sintschuk, Michael A1 - Beckmann, Jörg A1 - Bruno, Giovanni T1 - Mitigation of DMM-induced stripe patterns in synchrotron X-ray radiography through dynamic tilting N2 - In synchrotron X-ray radiography, achieving high image resolution and an optimal signal-to-noise ratio (SNR) is crucial for the subsequent accurate image analysis. Traditional methods often struggle to balance these two parameters, especially in situ applications where rapid data acquisition is essential to capture specific dynamic processes. For quantitative image data analysis, using monochromatic X-rays is essential. A double multilayer monochromator (DMM) is successfully used for this aim at the BAMline, BESSY II (Helmholtz Zentrum Berlin, Germany). However, such DMMs are prone to producing an unstable horizontal stripe pattern. Such an unstable pattern renders proper signal normalization difficult and thereby causes a reduction of the SNR. We introduce a novel approach to enhance SNR while preserving resolution: dynamic tilting of the DMM. By adjusting the orientation of the DMM during the acquisition of radiographic projections, we optimize the X-ray imaging quality, thereby enhancing the SNR. The corresponding shift of the projection during this movement is corrected in post-processing. The latter correction allows a good resolution to be preserved. This dynamic tilting technique enables the homogenization of the beam profile and thereby effectively reduces noise while maintaining high resolution. We demonstrate that data captured using this proposed technique can be seamlessly integrated into the existing radiographic data workflow, as it does not need hardware modifications to classical X-ray imaging beamline setups. This facilitates further image analysis and processing using established methods. KW - Double multilayer monochromators KW - Synchrotron X-ray imaging KW - Signal normalization KW - BAMline KW - Dynamic tilting PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615049 DO - https://doi.org/10.1107/S1600577524008646 SN - 1600-5775 VL - 31 SP - 1551 EP - 1560 PB - International Union of Crystallography (IUCr) AN - OPUS4-61504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ulbricht, Alexander T1 - Skalenübergreifende Materialcharakterisierung basierend auf Computertomographiedaten N2 - Die BAM präsentiert anhand ausgewählter Beispiele wie mithilfe von Computertomographiedaten dringende technische Fragestellungen zum Verständnis von Schädigungsmechanismen in verschiedensten Materialien und Komponenten, zum Beispiel in additiv gefertigten Metallen oder Batterien, beantwortet werden können. T2 - VisiConsult Röntgen-Technologietag 2024 -- Transformation in der ZfP CY - Stockelsdorf, Germany DA - 10.10.2024 KW - Computertomographie KW - Batterie KW - Additive Fertigung KW - Synchrotron KW - BAMline PY - 2024 AN - OPUS4-61431 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, M. A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Oxidative ageing of elastomers: experiment and modelling N2 - During an extensive test programme at the Bundesanstalt für Materialforschung und prüfung, material property changes of EPDM O-rings were investigated at different ageing times and two ageing temperatures of 125 ◦ C and 150 ◦ C. To exclude possible diffusion-limited oxidation (DLO) effects that can distort the data, IRHD microhardness measurements were taken over the cross section of compressed O-rings. Continuous stress relaxation measurements were taken on samples free of DLO effects. The additional effect of physical processes to irreversible chemical ones during a long-term thermal exposure is quantified by the analysis of compression set measurements under various test conditions. By combining the different experimental methods, characteristic times relative to the degradation processes were determined. On the basis of experimental data, a microphysically motivated model that takes into account reversible and irreversible processes was developed. The parameter identification strategy of the material model is based on our experimental investigations on homogeneously aged elastomer O-rings. The simulated results are in good agreement with the experiments. KW - Compression Set KW - Compression stress relaxation KW - Modelling KW - Ageing KW - Microhardness PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609332 DO - https://doi.org/10.1007/s00161-022-01093-9 VL - 36 SP - 289 EP - 297 PB - Springer Nature AN - OPUS4-60933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trogadas, P. A1 - Cho, J. I. S. A1 - Rasha, L. A1 - Lu, X. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Manke, I. A1 - Shearing, P. R. A1 - Brett, D. J. L. A1 - Coppens, M. O. T1 - A nature-inspired solution for water management in flow fields for electrochemical devices N2 - A systematic, nature-inspired chemical engineering approach is employed to solve the issue of flooding in electrochemical devices. The mechanism of passive water transport utilized by lizards living in arid environments is leveraged to design flow-fields with a microchannel structure on their surface, through which capillary pressure rapidly removes the water generated in the electrochemical device. This water management strategy is implemented in proton exchange membrane fuel cells (PEMFCs) with a lunginspired flow-field, which ensures uniform distribution of reactants across the catalyst layer. Jointly, this nature-inspired approach results in flood-free, stable operation at 100% RH and a B60% increase in current (B1.9 A cm-2) and peak power density (B650 mW cm−2) compared to current PEMFCs with a flood-prone, serpentine flow-field (B0.8 A cm-2 and 280 mW cm-2, respectively). This significant advance allows for PEMFC operation at fully humidified conditions. KW - Neutron imaging KW - X-ray tomography KW - Fuel cell PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596662 DO - https://doi.org/10.1039/d3ee03666a VL - 17 SP - 2007 EP - 2017 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59666 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tang, F. A1 - Li, D. A1 - Liu, X. A1 - Huang, H. A1 - Wu, C. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Manke, I. A1 - Sun, F. A1 - Chen, L. T1 - Exploring optimal Li composite electrode anodes for lithium metal batteries through in situ X-ray computed tomography N2 - The uncontrolled Li dissolution/deposition dynamics and rapid Li pulverizations hinder the widespread deployment of Li metal batteries (LMB). Designing a Li composite electrode possessing a mechanically robust and lithiophilic three-dimensional (3D) framework represents a promising strategy to address these challenges. This study involves the preparation of three uniquely tailored Li-B-Mg composites using a combined metallurgical process of melting, casting, and rolling, along with the synergistic application of in situ X-ray computed tomography (CT) and post-mortem failure analysis to explore the most promising composite electrode candidate for LMBs. During the in-depth investigation, the optimal 70Li-B-Mg composite electrode stands out due to its robust skeleton fiber structure, uniform Li dissolution/deposition characteristics and high capacity of free-Li. Its promising prospects for enabling high-performance LMBs are showcased by the superior performance of the built Li||O2, Li||LiFePO4, Li||NCM622 and Li||NCM811 battery systems. This work offers a novel approach for exploring universally applicable and robust Li composite electrodes to realize high-performance LMBs using in situ CT analysis. KW - Li metal batteries KW - Li composite electrode KW - X-ray computed tomography KW - Li-B-Mg PY - 2024 DO - https://doi.org/10.1016/j.ensm.2024.103746 VL - 72 SP - 12 PB - Elsevier B.V. AN - OPUS4-61039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lucaßen, J. T1 - Bottom-up grown CISe micro absorber arrays: microstructure analysis and solar cell integration N2 - A reduction of critical raw materials like indium and gallium in chalcopyrite thin-film solar cells is aimed for the micro-concentrator concept. Bottom-up grown micro absorbers for operation under light concentration on the micrometer scale allow improved heat dissipation. T2 - 41st European Photovoltaic Solar Energy Conference and Exhibition (EU PVSEC 2024) CY - Vienna, Austria DA - 23.09.2024 KW - Laser-assisted MO-CVD KW - CISe micro-absorber KW - Micro solar cell arrays KW - Solar cell efficiency PY - 2024 AN - OPUS4-62075 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 - Sachse, René A1 - Kotil, Leyla A1 - Matjacic, Lidija A1 - McMahon, Greg A1 - Bernicke, Michael A1 - Bernsmeier, Denis A1 - Kraehnert, Ralph A1 - Hertwig, Andreas A1 - Hodoroaba, Vasile-Dan T1 - Morphological and Chemical Nanoscale Analysis of Mesoporous Mixed IrOx-TiOy Thin Films as Electrode Materials N2 - orous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach (1). Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too. In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted. KW - Mesoporous thin films KW - Imaging KW - TiO2 KW - Ir oxid KW - Auger electron spectroscopy KW - ToF-SIMS KW - SEM/EDX PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.252 VL - 30 IS - Supplement 1 SP - 541 EP - 542 PB - Oxford University Press (OUP) AN - OPUS4-61185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Aging investigations of metal seals used in containers for interim storage of spent fuel N2 - In Germany dual purpose containers with double lid systems are used for the transport and storage of spent fuel and high level radioactive waste. The bolted lids are equipped with metal seals (e.g. Helicoflex®) to ensure the safe enclosure of the inventory for the required time period. The used metal seals have a layered structure consisting of three components. In the center a helical spring is positioned that is surrounded by two C-shaped jackets. The helical spring is mainly responsible for generation of the required restoring force. The inner jacket is made of stainless steel and homogenizes the restoring force generated by the helical spring. The outer jacket is made of silver or aluminum. Both metals are soft in comparison to the contact partners (lid and container body). During bolting of the lid the seal is compressed between lid and container body. The generated restoring force of the helical spring causes a plastic deformation of the outer jacket which adapts to the surfaces of the lid and the container body. Hence, leakage paths are closed and the sealing function is caused. Typical durations for existing interim storage licenses in Germany are 40 years, but due to the challenges in selection and construction of a final repository it can be expected that they have to be extended to longer periods. An extension of license periods requires knowledge of the long-term behavior of the seals. To meet this challenge long-term investigations have been started at Bundesanstalt für Materialforschung und –prüfung (BAM) in 2009. These tests focus on seals assembled in test flanges which are stored at temperatures ranging from room temperature to 150 °C for accelerated aging. The aged seals are tested repeatedly after certain aging steps and the performance is evaluated in respect to the leakage rate, the remaining seal force, and the useable resilience upon decompression. In this contribution an update on the running investigations in respect to earlier publications (Grelle et al. 2019, Goral et al. 2023) will be given and the implications of the results for resilient long-term safety will be presented. New activities will be addressed and their expected outcome be discussed. T2 - PVP2024, Pressure Vessels & Piping Conference CY - Bellevue, WA, USA DA - 29.07.2024 KW - Metal seal KW - Aging KW - Interim storage PY - 2024 AN - OPUS4-61355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rossi, Andrea A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Development of a one-pot synthesis of rGO in water by optimizing Tour’s method parameters N2 - Since its first synthesis in 2004, graphene has been widely studied and several different synthesis methods has been developed. Solvent exfoliation of graphite and the reduction of graphene oxide previously obtained through graphite oxidation are the most employed. In this work, we exploited synthesis conditions of a method usually employed for obtaining graphene oxide (the Tour’s method) for directly obtaining a very poorly oxidised material with characteristics like reduced graphene oxide. For the first time, a one-pot synthesis of reduced graphene oxide (rGO) is reported avoiding the use of a post-synthesis chemical or thermal reduction of the graphene oxide that requires further reagents, heat and time. KW - Graphene KW - 2D-materials KW - Tour's method KW - rGO KW - One-pot synthesis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611827 DO - https://doi.org/10.1038/s41598-024-73606-2 SN - 2045-2322 VL - 14 SP - 1 EP - 10 PB - Springer Nature CY - London AN - OPUS4-61182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matthews, Lauren T1 - Rapid Desease Monitoring with Resistive-Pulse Sensing in Nanopipettes N2 - Following parts of the research project as proceeded at University of Birminngham are presented: Translocation, Experiments, Synthesis of DNA Structures, Antibody, Biomarker, Binding. Following works have been carried out at BAM: High Resolution Electron Microscopy, Dedicated Sample Preparation, Surface Analysis Methods. T2 - UoB-BAM Chemistry Theme Meeting CY - Online meeting DA - 15.05.2024 KW - Nanopipettes KW - Sensing KW - Diagnosis KW - Surface analysis PY - 2024 AN - OPUS4-60451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of Lateral Dimensions of Particles & Flakes (2D) by Imaging Methods N2 - An overview with the basics of size and shape measurement of particles and 2D structures according to established methodologies (and popular imaging processing software packages) with imaging techniques is given. Main descriptors are explained based on practical cases are determined interactively at the flipchart. T2 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Nanoparticles KW - 2D materials KW - Lateral dimensions KW - ISO KW - Imaging PY - 2024 AN - OPUS4-60454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Handling and Transport of defective lithiumbatteries N2 - Safe handling and transport of Lithiumbatteries is fundamental for their global trade and use. BAM is the German competent authority responsible for the transport of defective lithium batteries and as such approves transport conditions and packaging for the transport. Also BAM is providing the test protocol for fire testing of packagings. Results and topics around safe transport are described and discussed. T2 - Sino-German Workshop on Dangerous Goods Packaging CY - Online meeting DA - 27.11.2024 KW - Lithium batteries PY - 2024 AN - OPUS4-62330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Morcillo, Dalia T1 - Study of Age-Induced Isotope Fractionation in Lithium-ion Batteries using Microwave-Induced Cold Nitrogen Plasma Mass Spectrometry N2 - This study investigates the use of a microwave-induced cold nitrogen plasma ionization source, coupled with a single quadrupole mass analyzer, as a cost-effective alternative to multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for analyzing lithium isotopic composition in lithium-ion batteries. The performance of both instruments was compared in measuring δ7Li values vs an isotopic standard in new and aged commercial lithium cobalt oxide (LCO) batteries. Results indicate that the microwave-induced ionization source, operating under cold plasma conditions at 800 W with an 8 mm torch depth position, achieves precision comparable to MC-ICP-MS, with δ7Li values ranging from 0.7 ‰ to 3.4 ‰. This method benefits from a dielectric resonator for uniform plasma, better ion velocity control, and higher energy efficiency [1-3]. Optimal settings were established as dwell times of 10 ms for 6Li and 1 ms for 7Li. The study found that 6Li migrates to the anode during multiple charge/discharge cycles, leading to the accumulation of 7Li at the cathode. This fractionation effect becomes more visible with repeated cycling. The microwave-induced ionization source offers a cost-effective and accurate alternative to MC-ICP-MS, with increased portability, facilitating further research into isotopic fractionation and aging of lithium-ion batteries. T2 - Adlershofer Forschungsforum 2024 CY - Berlin, Germany DA - 11.11.2024 KW - Cold nitrogen plasma KW - Lithium isotope KW - Battery PY - 2024 AN - OPUS4-62024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böttcher, Nils T1 - Sicherheit von Lithium-und Natrium-Batterien - Brandprüfungen und Sicherheitsmaßnahmen N2 - Die Präsentation gibt einen ganzheitlichen Überblick im sicheren Umgang mit elektrochemischen Energiespeichertechnologien. Ferner enthält diese Präsentation einen Überblick über die aktuell an der BAM durchgeführten Forschungsprojekte und hoheitlichen Aufgaben mit Bezug diesen Energiespeichern T2 - Lehrgang "Moderne elektrochemische Energiespeicher" (905350) CY - Mannheim, Germany DA - 16.09.2024 KW - Lithiumbatterien KW - Thermal Runaway KW - Sicherheit KW - Natriumbatterien PY - 2024 AN - OPUS4-62302 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tichter, Tim T1 - Electroanalytical experiments at macroporous electrodes for redox-flow batteries N2 - Macroporous carbon felts (CFs) are the prevalently used electrode material for redox-flow batteris. Owing to their large internal surface area, these structures can efficiently drive the Faradaic reactions in a RFB. However, the electrochemical characterization of novel CFs, or modified CF-materials is a cumbersome task. This is essentially related to the complex mass-transport phenomena which are convoluted with the electrode kinetics. This talk will focus on ex-situ cyclic voltammetry and operando electrochemical impedance spectroscopy as electroanalytical techniques for porous RFB electrodes. Common pitfalls in the voltammetric analysis of CFs are elucidated and recent strategies for modeling and evaluating CV experiments on porous structures are introduced. Finally, a method based on electrochemical impedance spectroscopy is introduced which allows for an operando fingerprinting of electrochemical reactions in a vanadium-based RFB. T2 - Flow4U-Event CY - Eindhoven, Netherlands DA - 08.04.2024 KW - Porous Electrodes KW - Redox-Flow Batteries KW - Digital Simulation KW - Convolutive modeling KW - Impedance Spectroscopy KW - Distribution of Relaxation Times PY - 2024 AN - OPUS4-62304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tichter, Tim T1 - The DSDC Algorithm - A Universal Strategy for Simulating Voltammetry of Rough and Porous Electrodes N2 - Porous electrodes or electrodes with rough surfaces offer a multitude of tailored applications. The theoretical treatment of such structures is, however, challenging since their voltammetric profile is a convolution of the time-dependent current with an inherently random mass-transfer function. Since the latter quantity has no analytical solution, the classical convolutive techniques cannot be applied. Therefore, simulations have been based on severe simplifications of the diffusion space [1,2] or were performed by means of digital simulation. Unfortunately, the latter approach becomes computationally prohibitive when a large and/or highly resolved, three-dimensional diffusion space needs to be considered. To mitigate these problems, we introduce the digital simulation, deconvolution, convolution (DSDC) algorithm, consisting of four successive steps [3]. Firstly, the three-dimensional image of the electrode under investigation is extracted via micro X-ray computed tomography (µ-CT) or atomic-force microscopy (AFM). Subsequently, the purely mass-transfer controlled current of this spatial template is generated by means of digital simulation. In the third and fourth steps, the mass-transfer function is extracted for a set of discrete points in time by numerical deconvolution and finally used for classical convolutive simulations. In this manner, any simplification of the diffusion domain becomes obsolete and the advantages of digital simulation and convolutive modelling are most favourably combined. Finally, this DSDC-algorithm provides an interdisciplinary connection of ex-situ imaging and in-situ electrochemistry which results in excellent agreement of simulated and experimentally acquired data. T2 - Bunsentagung 2024 CY - Aachen, Germany DA - 25.03.2024 KW - Porous Electrodes KW - Convolutive Modeling KW - Digital Simulation KW - Diffusion KW - Redox-Flow Batteries PY - 2024 AN - OPUS4-62303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kunkel, Benny A1 - Seeburg, Dominik A1 - Kabelitz, Anke A1 - Witte, Steffen A1 - Gutmann, Torsten A1 - Breitzke, Hergen A1 - Buntkowsky, Gerd A1 - de Oliveira Guilherme Buzanich, Ana A1 - Wohlrab, Sebastian T1 - Highly productive V/Zn-SiO2 catalysts for the selective oxidation of methane N2 - The production of formaldehyde on industrial scale requires huge amounts of energy due to the involvement of reforming processes in combination with the demand in the megaton scale. Hence, a direct route for the transformation of (bio)methane to formaldehyde would decrease costs and puts less pressure on the environment. Herein, we report on the use of zinc modified silicas as possible support materials for vanadium catalysts and the resulting consequences for the performance in the selective oxidation of methane to formaldehyde. After optimization of the Zn content and reaction conditions, a remarkably high space-time yield of 12.4 kgCH2O⋅kgcat − 1 ⋅h− 1 was achieved. As a result of the extensive characterization by means of UV–vis, Raman, XANES and NMR spectroscopy it was found that vanadium is in the vicinity of highly dispersed zinc atoms which promote the formation of active vanadium species as supposed by theoretical calculations. This work presents a further step of catalyst development towards direct industrial methane conversion which may help to overcome current limitations in the future. KW - Catalysis KW - XANES KW - Selective oxidation PY - 2024 DO - https://doi.org/10.1016/j.cattod.2024.114643 SN - 0920-5861 VL - 432 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-60137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Theiler, Geraldine T1 - Polymer tribology in cryogenic hydrogen N2 - In this presentation, an overview of polymer tribology in cryogenic hydrogen is given along comparison with other environments. T2 - Hydrogenius Symposium 2024 CY - Kyushu University Ito Campus, Japan DA - 12.09.2024 KW - Hydrogen KW - Friction KW - Wear KW - Polymer materials KW - Cryogenic PY - 2024 AN - OPUS4-61426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Campari, Alessandro A1 - Konert, Florian A1 - Sobol, Oded A1 - Alvaro, Antonio T1 - A comparison of vintage and modern X65 pipeline steel using hollow specimen technique for in-situ hydrogen testing N2 - The transition toward a hydrogen-based economy requires a widespread transport and distribution network, and repurposed natural gas pipelines are a viable option. An assessment of the hydrogen-induced degradation of pipeline steels is needed to inject H2 gas into the existing infrastructure safely. The conservative and standardized method consists of in-situ tensile tests in an autoclave filled with high-pressure hydrogen gas. A proposed alternative method involves using a hollow specimen as containment volume and applying the gas pressure in the inner cavity. This technique has lower costs and shorter test preparation time but is not standardized yet. This study aims to evaluate and compare the tensile properties of API 5L X65 pipeline steel in two states: vintage and modern. The influence of the surface roughness is investigated through parallel tests with drilled and reamed specimens. Hydrogen tests are compared with reference tests in an inert environment. A significant hydrogen-induced decrease in tensile properties is observed, and no significant difference between vintage and modern X65 can be drawn. The reduction in tensile properties is more significant in specimens with higher inner surface roughness. The evaluation of surface conditions appears crucial when assessing the HE susceptibility of hydrogen transport and storage equipment. KW - Hydrogen embrittlement KW - Hollow specimen technique KW - Pipeline steel KW - SSRT PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603013 DO - https://doi.org/10.1016/j.engfailanal.2024.108530 VL - 163 SP - 1 EP - 15 PB - Elsevier Ltd. AN - OPUS4-60301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -