TY - CONF A1 - Böttcher, Nils T1 - Visualizing the progression of the thermal runaway in lithium-ion-cells by controlled abuse tests at low temperatures N2 - Due to their increasing energy density, lithium-ion-batteries (LIBs) play a key role in the traffic energy transition. Regarding their safety behavior, the main challenge of LIB-cells remains the thermal runaway (TR) process. In situ/operando investigations of the TR on commercial cells is possible with radiographic and computer tomographic measurements. Nonetheless, high resolution visualization of the TR persists as a challenge due to the high progression speed of the TR-process itself. Generally, performing abuse tests at cryogenic temperatures allows to slow down or even prevent the TR. Nevertheless, not all abuse methods are suitable for TR investigations at low temperatures. Nail penetration is an appropriate option, however, contains numerous unknown parameters and therefore suffers regarding reproducibility. Herein, a self-developed high precision nail-penetration-setup is introduced, approaching the necessary mechanically reproducibility with controlled temperatures down to -190°C. The setup allows the preparation of critically abused, however, at cryogenic temperatures stable LIB-cells. These cells were controlled rethermalized to room temperature during synchrotron x-ray computer tomography (SXCT) with a pixel size up to 0.7 μm. During this measurement, the temperature and voltage of the cell is monitored allowing the visualization of the initial internal cell reactions. This study reveals the relation between internal reactions and cell voltage. Finally, the developed set-up enables in-depth analysis of thermal runaway behavior down to material level for various commercial battery cells in the future. T2 - International Battery Safety Workshop CY - Ulm, Germany DA - 28.09.2023 KW - Thermal Runaway KW - Lithium Ion Batteries KW - Computer Tomography PY - 2023 AN - OPUS4-59270 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 - Porous Carbon Supported Ni or Co Single Atom Catalysts for Electrochemical Reduction of CO2 N2 - Isomorphous, but chemically unequal Ni-, Co- and Zn-N-C electrocatalysts are investigated for their electrocatalytic properties towards the electrochemical CO2 conversion. It turns out that Ni-N-Cs are clearly most favourable, because of the isomorphism to other catalysts, also clearly due to the NiN4 sites properties. T2 - Deutsche Zeolith-Tagung 2024 CY - Frankfurt am Main, Germany DA - 23.03.2024 KW - M-N-C catalysts KW - CO2 reduction PY - 2022 AN - OPUS4-61953 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 - Wutthiprom, Juthaporn T1 - Sol-Gel Carbonization towards Tailor-Made Boron- and Nitrogen-doped Carbon N2 - The activation of carbon is normally proceeded in top-down or bottom-up strategies. Therein pore formation (porogenesis) occurs by reaction with steam, CO2 , KOH, or the use of acidic agents, in which chemical leaching of carbon atoms occurs. The sol-gel type synthesis of N-doped carbon in excess amounts of molten acids was presented recently, questioning the general validity of a leaching activation mechanism.[1] The protocol using inorganic salt melts (MgCl2 or ZnCl2 ) and organic precursors additionally generated N functionalities. Interestingly, it can be noticed that the imprinting cations play a crucial role towards the chemical structure of N-doped carbon framework. The coordinated geometry is wellknown from phthalocyanine, a macrocyclic Ncomplexes (MN4 -sites, where M is metal cation) which are desirable surface complexes, e.g. in electrocatalysis. The analogous phenomenon may be observed when using H3BO3 agent via sol-gel chemistry. T2 - International Sol-Gel Conference 2022 CY - Lyon, France DA - 24.06.2022 KW - Boron-Nitrogen-Doped-Carbon KW - Sol-Gel-Carbonization PY - 2022 AN - OPUS4-61959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mehmood, Asad A1 - Fellinger, Tim-Patrick T1 - Porous Carbon Supported Ni and Co Single Atom Catalysts for Electrochemical Reduction of Carbon Dioxide N2 - Non-precious metal single atom catalysts (generally labelled as M/NCs where M= Co, Fe, Ni etc.) consist of active metal centres dispersed on nitrogen doped porous carbon (NC) matrix at atomic level and exhibit promising activities e. g. for electrochemical reduction of CO2, selectively forming CO. We herein use identical Mg/NCs as platform for ion-exchange reactions towards morphologically equivalent Ni/NCs and Co/NCs. The Ni/NC catalyst shows almost double the specific activity and a Faraday efficiency of >80% at a very low overpotential of U= -0.43 V (even 95% at U= -0.5 to -0.8 V) with high stability. T2 - GDCh Electrochemistry 2022 CY - Berlin, Germany DA - 27.09.2022 KW - Electrochemical CO2 conversion KW - Single atom catalysts KW - Porous Carbons PY - 2022 AN - OPUS4-61980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Appel, Paul Alexander T1 - Development of tailormade core-shell hard carbon materials as anode materials in sodium ion batteries N2 - The current strong interest in electromotive mobility and the need to transition to an energy grid with sustainable energy storage has led to a renewed interest in sodium ion batteries (SIBs). Hard carbons 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] The goal of this project is to synthesize carbon materials using different zeolite templates to obtain electrode materials that feature a defined and adjustable pore structure. A better understanding of the structure-property relationship by investigating porosity-tailored anode materials, should enable quantification and understanding of the potential of hard carbon materials for SIBs. Furthermore, a goal is to explore whether a core-shell structure can separate sodium storage and solid electrolyte interphase formation allowing the independent investigation of storage capacity and irreversible losses. T T2 - 34. Deutsche Zeolith-Tagung CY - Vienna, Austria DA - 21.02.2023 KW - Energy Materials PY - 2023 AN - OPUS4-62002 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 - CONF A1 - Appel, Paul Alexander T1 - Developing Tailor-Made Core-Shell Carbon Negative Electrode 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, an investigation of the storage mechanism of sodium is possible. T2 - Batterieforum 2025 CY - Berlin, Germany DA - 21.01.2025 KW - Electrochemical Energy Materials KW - Negative Electrodes KW - Sodium Ion Batteries PY - 2025 AN - OPUS4-65110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghafafian, Carineh T1 - Restoring structural integrity - localized repairs for wind turbine rotor blades N2 - The effect of localized repairs on the mechanical properties and thus the lifespan of wind turbine rotor blade shells is examined. T2 - SAMPE Symposium 2019 CY - Dresden, Germany DA - 06.02.2019 KW - Fatigue KW - Glass fiber reinforced polymers KW - Lightweight materials KW - Sandwich KW - Wind turbine blades PY - 2019 AN - OPUS4-47443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - Proposed Project SealWasteSafe: Materials Technology, Quality Assurance and Monitoring Techniques for Safe Sealing Systems in Underground Repositories N2 - The proposed BAM project SealWasteSafe will advance the state of the art for the construction and monitoring of safe sealing systems for underground repositories of radioactive or toxic waste. During this project, a novel salt concrete exhibiting neither significant cracking nor shrinkage will be optimized for use in the sealing systems. The composition of this material will be based on alkali-activated materials, which are characterized by particularly small thermal deformations during the hardening reaction. Quality assurance and continuous monitoring systems developed during this project will be demonstrated not only for high reliability, but also for resistance to highly alkaline environments and to water intrusion along cables or at sensor locations. A variety of sensors will be used in combination with wireless Radio Frequency Identification (RFID) technology to record moisture, temperature, and, if necessary, corrosion activity within the sealing system. Distributed Fibre Optic Sensor (FOS) technology will also be used for strain, temperature, and moisture content measurement. Ultrasound-based measuring methods will be utilized for the detection of cracks and delaminations. Additionally, digital image correlation and acoustic emission analysis will be used for deformation measurements and crack detection. A novel borehole probe and advanced ultrasound imaging techniques will be further developed to track cracks and delaminations within the host rock in 3D. The surface-based Large Aperture Ultrasound System (LAUS) will also be utilized to detect cracks and delaminations deep below the exterior surface of the sealing system. Although the focus of this project will be on the host rock salt, the resulting technologies will be intentionally developed in a way that facilitates their adaptation to other host rocks. T2 - 2nd International Conference on Monitoring in Geological Disposal of Radioactive Waste CY - Paris, France DA - 09.04.2019 KW - SealWasteSafe KW - Radioactive Waste Disposal KW - Underground Repositories KW - Alkali-Activated Material KW - Monitoring PY - 2019 AN - OPUS4-47776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blaeß, Carsten T1 - Effects of microstructure on crack healing in glass matrix composites N2 - Crack healing in glass ceramic solid oxide fuel cell (SOFC) sealants is of utmost importance as cracks caused by thermal cycling remain a bottleneck in developing durable SOFC. Whereas no or low crystal volume fraction seems most favorable for viscous crack healing, it does not for load bearing and undesired diffusion. On the other hand, crystals or filler particles can make the sealant less prone to these disadvantages but it could increase the effective composite viscosity and retard crack healing. Against this background, the influence of crystal volume fraction, phi, on viscous crack healing in glass matrix composites prepared from soda lime silicate glass and zirconia filler particles was studied. Vickers indention induced radial cracks were healed isothermally during interrupted annealing steps and monitored with optical microscopy. Due to the slow crystallization of the glass under study, phi could be kept constant during crack healing. For bulk glass samples (phi = =), the decrease in radial crack length was retarded by an initial increase in crack width due to crack rounding. Up to phi = 0.15 the increase in effective viscosity retarded this crack broadening thereby yielding faster crack healing. For phi > 0.15, crack broadening was progressively suppressed but the same was true for crack healing, which was fully prevented above phi = 0.3. Results indicate that optimum micro structures can prevent crack broadening limited by the global effective composite viscosity and this way promote crack healing limited by local glass viscosity. T2 - 93. Glastechnische Tagung CY - Nürnberg, Germany DA - 12.05.2019 KW - Crack healing KW - Glass matrix composite KW - Vickers indentation PY - 2019 AN - OPUS4-48543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zencker, Uwe T1 - Brittle failure of spent fuel claddings under long-term dry interim storage conditions – Preliminary analysis N2 - The evaluation of cladding integrity is a major issue to be demonstrated in Germany for extended interim storage periods up to 100 years and subsequent transportation considering operational and accidental conditions with respect to reactor operation, cask drying and dry interim storage. The chemical reaction between the zirconium fuel cladding and the cooling water in water-cooled reactors produces hydrogen and zirconium oxide. Hydrogen diffuses into the cladding and precipitates as zirconium hydrides when the solubility limit is reached, preferably oriented in hoop direction. At high temperatures during vacuum drying procedures, the hydrides can dissolve. Over a succeeding period of slow cooling with existing hoop stress the hydrides precipitate again, but partly reoriented along the radial direction of the cladding. This change of microstructure in combination with a decreasing temperature (0.5...2 K/year) during (extended) interim storage and additional mechanical load by handling procedures or under accident conditions could lead to a potential cladding embrittlement and consequently increased failure probability. The current research project BRUZL (Fracture mechanical analysis of spent fuel claddings under long-term dry interim storage conditions) has been launched by BAM to investigate potential sudden brittle failure of spent fuel claddings at small deformation under long-term dry interim storage conditions and is presented. T2 - IAEA International Conference on the Management of Spent Fuel from Nuclear Power Reactors CY - Vienna, Austria DA - 24.06.2019 KW - Ageing Management KW - Cladding Embrittlement KW - Extended Storage KW - Ring Compression Test KW - Spent Nuclear Fuel PY - 2019 AN - OPUS4-48868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heuser, Lina T1 - Sintering of silver-glass composites N2 - High conductive silver metallization pastes are key components in advanced electronics and photovoltaics. Increasing demands on efficiency, miniaturization and ever shorter time-to-market require tailored glass-silver-pastes. In these pastes, low-melting glasses act as a sintering aid achieving better sintering, adhesion and contact formation for solar cells. Yet, the related liquid phase sintering of silver-glass-composites and the underlying mechanism of silver dissolution, transport and reprecipitation are rarely investigated. In this study, systematically varied low melting alkaline zinc borate, alkaline earth borate, and Pb- and Bi-glasses are investigated. Glass transition and crystallization are studied with dilatometry, DTA and XRD. Sintering of the pure glasses, pure silver and silver-glass-composites is analyzed with Hot Stage Microscopy, optical and electron microscopy. Since oxygen dissolved in silver powders can affect the silver dissolution as silver oxide in the matrix oxide glasses, the O2-content of silver powders is determined by Vacuum Hot Extraction. The glass transition temperature of the glasses under study varies between 370 °C and 590 °C whereas the sinter onset largely ranges between 400 °C and 600 °C. On the other hand, it scattered between 200 °C and 450 °C for selected commercial Ag-powders of different particle size and morphology. T2 - 93rd Annual Meeting of DGG in Conjunction with the Annual Meeting of  USTV CY - Nuremberg, Germany DA - 13.05.2019 KW - Silver glass paste KW - Sintering KW - Microstructure PY - 2019 AN - OPUS4-48906 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Deborah T1 - Post-impact evaluation at RC plates with planar tomography and FEM N2 - The aim of the work is to develop experimental investigation strategies to determine damage quantities and the liquid Intrusion behaviour of containment structures in case of aircraft collision. T2 - 36th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republik DA - 24.09.2019 KW - Impact KW - Damage characterization KW - Planar tomography KW - Numeric simulation KW - Reinforced concrete structure PY - 2019 AN - OPUS4-49542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Karsten T1 - Fire tests of RAM packages and containers under high thermal load N2 - Fire testing is an essential part of the hypothetical, cumulative mechanical and thermal test conditions that shall guarantee package safety in severe accidents. Within regulatory approval of transport or storage packages for radioactive material, specific thermal load tests are required in accordance to licensing conditions and international standards, respectively. The specifications of these thermal tests are based on test conditions with equivalent heat input to that of a hydrocarbon fuel fire. In the past, light heating oil, diesel or kerosene was mostly used as the fuel to generate the pool fire. In accordance with IAEA regulations for a fire in an accident, the temperature of 800 °C over a period of 30 minutes must be fulfilled. Furthermore, the delivery acceptance criteria for containers in nuclear waste repositories could reach for example average temperatures of 800 °C during a period of one hour in combination with defined requirements on activity release. BAM as a scientific and technical German federal government institute operates an open air Technical Safety Test Site for experimental investigations of dangerous good and its containment. In this areal a large fire test facility is under operation. Liquid Propane is utilized as fuel which is pumped via pipelines from a central storage tank to the fire exposed test facility areas. In the ring burner system, the gas is released from nozzles, and ignited by ignition burners. The paper includes examples of fire test performance with prototypes of a transport package and a storage container, respectively. In preparation of the thermal load, calorimeter tests have been performed using test specimens of appropriate size and behavior. For the fire test scenario is demonstrated that the IAEA thermal test requirements are fulfilled. T2 - 19th International Symposium on the Packaging and Transportation of Radioactive Materials PATRAM 2019 CY - New Orleans, LA, USA DA - 04.08.2019 KW - IAEA Thermal Test KW - Thermal package testing KW - Transport package KW - Container for radioactive waste PY - 2019 AN - OPUS4-49092 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Auster, Jürgen T1 - Dynamic impact tests on materials & components of RAM packages - Advanced experimental and measurement methods N2 - In accident scenarios of transport packages or hypothetical crashes of containers in a storage facility or repository, the materials resistance against dynamic failure of the involved components is a deciding factor for package and container integrity during the handling, transport and storage for each type of radioactive material. For example, different dynamic impact tests on containers and components like lid sealing systems and specimens made of ductile cast iron and shock-absorbing materials are carried out by BAM. In order to perform dynamic impact tests with packages and its parts BAM operates two free-fall drop test facilities with maximum capacities of 200 t and 55 t, and a test bench for guided drop tests. This latter drop test machine enables a clearly specified component loading by a precisely positioned test object or drop weight and has been used recently for numerous investigations. The paper gives an overview of the wide range of experimental testing methods carried out within guided Impact and bending tests. Examples of methodological challenges are presented, especially such experimental analysis of dynamic impact conditions. In addition to known applied methods of dynamic, non-contact displacement measurements like high-speed 3-D surface deformation a recently patented 2-D tracking method is presented. By means of in-situ determination of fracture parameters with relevance to the materials stress intensity factor, the method has been successfully applied for a typical specimen geometry. Also shown are the possibility of detecting in-situ He-leakage rates on laterally impact loaded lid sealing systems as well as a method of acceleration sensor-temperature control under test conditions in the low temperature range. T2 - 18th International Symposium on the Packaging and Transportation of Radioactive Materials PATRAM 2019 CY - New Orleans, USA DA - 04.08.2019 KW - Dynamic impact tests KW - Materials KW - RAM packages KW - Advanced experimental KW - Measurement methods PY - 2019 AN - OPUS4-49062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jansson, P. T1 - EURAD: SFC WP Spent fuel characterisation and evolution until disposal N2 - The European Joint Programme on Radioactive Waste Management (EURAD) has been launched to coordinate activities on agreed priorities of common interest between European partners. The main actions include scientific and technical activities on radioactive waste characterization and processing, interim storage of radioactive waste as well as predisposal and disposal solutions. As part of the programme, the work package on Spent Fuel Characterization and Evolution until Disposal (SFC) was proposed and accepted by the European Commission. The objectives of this work package include the development of beyond-state-of-the-art characterization techniques for spent nuclear fuel during its evolution from reactor unloading until disposal, the understanding of the spent fuel performance during prolonged storage, transport and emplacement in a deep geological repository, the understanding of the behaviour of fuel, cladding, pellet-cladding interaction and ageing effect under normal and postulated accident scenarios until disposal, and contributions to operational safety concepts for fuel handling at spent nuclear fuel packaging facilities. T2 - EURADWASTE '19 CY - Pitesti, Romania DA - 04.06.2019 KW - Radioactive waste KW - Interim storage KW - Transport KW - Disposal KW - Spent fuel characterisation PY - 2019 AN - OPUS4-48211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Vibrational density of states and molecular mobility in a polymer with intrinsic microporosity PIM-1 as revealed by inelastic neutron scattering N2 - Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, by means of inelastic neutron scattering, the vibrational density of states (VDOS) and the molecular mobility were investigated for PIM-1, the prototypical polymer with intrinsic microporosity. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to the VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. Elastic fixed window scans were measured on a neutron backscattering spectrometer to have an overview about the molecular dynamics at a time scale of ca. 1 ns. The temperature dependence of the estimated mean squared displacement shows a step-like increase in the temperature range from 100 K to 250 K indicating the onset of some molecular mobility. The nature of this motional process was analyzed in detail by quasielastic neutron scattering combining Time-of-Flight and backscattering where the data are discussed with regard to both the q- and the temperature dependence. T2 - 7. European Conference on Neutron Scattering 2019 CY - Saint Petersburg, Russia DA - 30.06.2019 KW - Neutron Scattering KW - Polymer of intrinsic microporosity PY - 2019 AN - OPUS4-48421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kömmling, Anja T1 - Discoloration effects of high-dose γ-irradiation and long-term thermal ageing of (U)HMW-PE N2 - Two polyethylene types with ultra high (UHMWPE) and high molecular weight (HMWPE), which are used as neutron radiation shielding materials in storage casks for radioactive waste, were subjected to gamma irradiation doses up to 600 kGy and subsequent thermal ageing at 125 °C for up to one year. One material was a medical grade UHMWPE and the other a HMWPE containing an antioxidant. Degradation effects in the materials were characterized using colorimetry, UV-Vis spectroscopy, MIR and FTIR measurements, DSC and, in the case of HMWPE, insoluble content determination. Both materials exhibited a yellowing upon irradiation. The discoloration of UHMWPE disappeared again after thermal ageing, which is why it was attributed to annealable color centers in the form of free radicals entrapped in the crystalline regions of the polymer that recombine during thermal ageing. Furthermore, oxidation species were observed with MIR and FTIR spectroscopy. For HMWPE, the yellowing occurred during both irradiation and thermal ageing and was correlated to antioxidant decomposition. Additionally, black spots were observed after thermal ageing of HMWPE that were attributed to reaction products of antioxidant derivatives and catalyst residues. While only little evidence of oxidation species was found in the light material parts, oxidation is expected to concentrate in the black spots as the catalyst residue promotes hydroperoxide decomposition and thus radical formation that initiate polymer oxidation T2 - Ionizing Radiation and Polymers Conference CY - Giens, France DA - 25.09.2016 KW - Polyethylene KW - Gamma-irradiation KW - Yellowing KW - Degradation PY - 2016 AN - OPUS4-38001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kömmling, Anja T1 - Analysis of O-ring seal failure in the context of radioactive waste containers N2 - At BAM, which is a federal institute for materials research and testing in Germany, it is one of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes assessment of elastomeric seals applied in the casks. Besides examining the low-temperature behaviour and irradiation effects of elastomeric seals, it is our goal to estimate the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. Therefore, we started an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) which are aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) up to five years. In order to assess sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates as well as in flanges that allow leakage rate measurements. For comparison, uncompressed O-rings were aged as well. Further methods characterising seal performance are compression stress relaxation (CSR) reflecting the loss of sealing force of a compressed seal over time, and compression set (CS) which represents the recovery behaviour of a seal after release from compression. Additionally, material properties such as hardness, elastic modulus, glass transition temperature and viscoelastic loss factor as well as relaxation and recovery behaviour are examined in order to understand the underlying ageing mechanisms in each material. For obtaining results closely related to practical conditions, O-rings with a full-scale cord diameter of 10 mm were aged. However, this set-up can lead to heterogeneous aging caused by diffusion-limited oxidation (DLO) effects, resulting in distorted bulk properties such as compression stress relaxation and compression set. However, if DLO-affected data is excluded, extrapolations of CS data are possible using time-temperature shifts and Arrhenius graphs. For selecting an appropriate end-of-lifetime criterion, leakage rate measurements were performed, since leakage rate is the only characteristic directly correlated to the performance of the sealing system. A significant increase in leakage rate was considered as the end of the lifetime. However, the O-rings remained leak tight under static conditions and even exhibited an improved, i.e. decreased leakage rate while other properties already indicated strong deterioration. These tests were extended by seal tests with fast partial decompression. Overall an update will be given on the current investigations and results and the planned activities. T2 - Kautschuk Herbst Kolloquium 2022 CY - Online meeting DA - 08.11.2022 KW - Seal KW - Ageing KW - Compression set PY - 2022 AN - OPUS4-56397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voss, Heike T1 - Picosecond laser processing of hierarchical micro-nanostructures on Ti-alloy upon pre- and post-anodization N2 - Recent publications indicate that the order of electrochemical anodization (before or after the laser-processing step) plays an important role for the response of boneforming osteoblasts – an effect that can be utilized for improving permanent dental- or removable bone-implants. For exploring these different surface functionalities, multi-method chemical and structural characterizations were performed for two different characteristic micro-spikes covered by nanometric laserinduced periodic surface structures (LIPSS) on Ti-6Al-4V upon irradiation with nearinfrared ps-laser pulses (1030 nm wavelength, ~1 ps pulse duration, 66 & 80 kHz pulse repetition rate) at two distinct sets of laser fluence and beam scanning parameters. This involves morphological and topographical investigations by scanning electron microscopy (SEM) and white light interference microscopy (WLIM), near-surface chemical analysis by X-ray photoelectron spectroscopy (XPS) and hard X-ray photoelectron spectroscopy (HAXPES), as well as structural material examination via X-ray diffraction (XRD) measurements. The results allow to qualify the laser ablation depth, assess the spike geometry and surface roughness parameters, and provide detailed insights into the near-surface oxidation that may cause the different cell growth behavior for pre- or post-anodized medical implants. T2 - E-MRS Spring Meeting 2023 CY - Strasbourg, France DA - 29.05.2023 KW - Hard X-ray photoelectron spectroscopy (HAXPES) KW - Laser-induced periodic surface structures (LIPSS) KW - Ti6Al4V alloy KW - Hierarchical micro-nanostructures KW - Ultrashort laser processing PY - 2023 AN - OPUS4-60344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Morpho-Chemical Characterisation of Me-TiO2 Nanoparticles for Enhanced Photocatalytical Activity N2 - The conversion of solar energy into electricity and solar fuels is of crucial importance for a green and sustainable future. Water splitting using semiconductor photo-catalysts is considered a sustainable method to produce clean hydrogen (H2) fuel. Nevertheless, H2 photo-production efficiency remains still low, although extensive research works to understand better the mechanisms of the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER) are being carried out. In this respect, TiO2 is a key photoactive material, usually employed with a co-catalyst deposited onto the surface to enhance charge carriers’ separation and catalyze surface charge transfer reactions. The deposition of a co-catalyst on the TiO2 nanoparticle surface represents one successful way to enhance the activity of the photocatalyst through a modification of its surface and redox properties. In this context, high-resolution scanning electron microscopy coupled with elemental analysis by energy-dispersive X-ray spectroscopy (EDS) is fundamental for studying and understanding the effect of the nanoparticle morphology on the functional properties of shape-controlled TiO2 crystals (bipyramides, platelets, and elongated particles). Different types of metal-semiconductor combinations, TiO2 shapes and dopant metals (Ag, Pt, etc) and metal concentrations will be discussed. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Titania nanoparticles KW - Photocatalysis KW - Scanning electron microscopy KW - Energy dispersive X-ray spectroscopy PY - 2022 AN - OPUS4-54977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jürgens, Maria A1 - Olbricht, Jürgen A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - FLEXIKON - Teil 2: Ermüdungsverhalten, Schädigungsentwicklung und Lebensdauer von 9-12% Cr-Stählen im zyklischen Kraftwerksbetrieb N2 - Schnelle Lastwechsel führen v.a. in dickwandigen Kraftwerksbauteilen zu starken thermischen und mechanischen Beanspruchungen, da sich hohe Temperaturgradienten über der Wand des Bauteils einstellen. Es ergeben sich komplexe Lastkollektive aus zeitlich veränderlichen Spannungen/Dehnungen und Temperaturen, die formal einer Kombination aus Kriechbeanspruchung, Kriechermüdung und thermomechanischer Ermüdung (TMF) entsprechen. T2 - 47. Kraftwerkstechnisches Kolloquium CY - Dresden DA - 13.10.2015 KW - TMF KW - LCF KW - P91 KW - P92 PY - 2015 AN - OPUS4-35613 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Measurement of Porous TiO2 Layers with spectroscopic ellipsometry – a multi-method study N2 - By means of an effective medium (EMA) based approach, it is possible to use spectroscopic ellipsometry to determine the mixing ratios between air and material in porous dielectrics and calculate a quantitative value of the porosity for these materials. As this method is model-based, it is very difficult to provide a quantitative measure for the accuracy of porosity values determined by this method. Valuable additional information can often be obtained by combining ellipsometry with other complementary methods. In the present study, the ellipsometry results were validated by Electron Probe Microanalysis (EPMA) with the option of layer analysis (by the socalled “STRATAGem” approach), gravimetry, and electron microscopy. We analysed porous TiO2 thin layers synthesised by means of a template synthesis approach (evaporation induced self assembly). Ellipsometry measurements on porous samples are difficult to analyse due to the complexity of the models necessary. Often it is difficult to decide if the measured data contains enough information to successfully determine the target quantities (mixing ratio, dielectric function of the matrix material). One method to decrease the complexity of the fit and therefore use the measurement data most efficiently is a multi-sample analysis. In the present case, multi-sample analysis was used for determining the porosity factors of the individual layers while using one common set of dielectric function values for the matrix in all cases. While the results of the fit analysis in this case can be used to show the feasibility and also the limitations of the multi-method approach, the porosity values themselves show a promising agreement between the independent methods. It can therefore be concluded that determining porosity values with ellipsometry is in accordance to other methods to the level of accuracy provided by the complementary methodologies. T2 - International conference on spectroscopic ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic Ellipsometry KW - Electron Microscopy KW - Multi-method Metrology KW - Porous Materials KW - Thin Films KW - Titanium Dioxide PY - 2016 AN - OPUS4-37202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, Mike T1 - Reproducing and discussion of mechanisms in the contact area between metallic seals and flange during aging by finite element analysis (FEA) N2 - When the first site-specific interim storage licenses for DPCs (dual purpose casks), loaded with spent nuclear fuel or vitrified high-level waste from reprocessing were issued, a duration of 40 years was considered for interim storage license application and the long-term safety assessment of casks. In the meantime, the availability of a final repository is further delayed by several decades and thus interim storage for more than a century becomes a necessity. To assess the long-term performance of the typically used metal seals (e.g. Helicoflex), consisting of a helical spring (Nimonic), an inner stainless steel liner and an outer liner made from silver or aluminum, several experimental programs were conducted and are still ongoing. The investigated metal seals are typically mounted in mock-up flange systems and stored at increased temperatures to accelerate the aging process. In certain intervals the remaining seal force, the useable resilience and the corresponding leakage rate are determined. BAM has accompanied such programs for many years and started independent investigations in 2009. Although the remaining seal force is often used as “…one of the key parameters regarding sealing performances over time…” the presented results so far have shown that the courses of the leakage rate and the remaining seal force do not always correlate as expected. In 2016 BAM firstly published results of seals with aluminum liners where the measured leakage rate started to rise after a quite short time period (< 1 year) at 150 °C, although the seal force decreased only slightly compared to the previous measurement. After exceeding the required leakage rate of 10-8 Pa*m3/s it decreased again to acceptable values in the further course of aging. With reference to already published works, BAM has developed a new detailed ABAQUS finite-element (FE) model to represent the behavior of the seal mounted in the mock-up flange during aging, mainly characterized by the creeping of the outer liner. The main goal of the numerical simulation is to reproduce and understand the changing distribution of contact stresses (outer liner/flange) during aging and to discuss if and how it could be causative for the observed early breach of the leak tightness criteria and its later recovery. T2 - PATRAM 2025, 21st International Symposium on the Packaging and Transportation of Radioactive Materials CY - San Antonio, Texas, USA DA - 27.07.2025 KW - Finite element analysis KW - Metallic seals KW - Aging KW - Contact area PY - 2025 AN - OPUS4-63883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - Photolytically and Thermally Initiated Destruction N2 - Casks for storage and transportation of used fuel rods of radioactive material are equipped with polyethylene (PE) for improved neutron flux shielding. The embedded PE structures are additionally exposed to gamma radiation and heat flow due to the specific high activity of the fission products. 60Co γ-radiation and heat load experiments at 125°C has been performed to evaluate PE degradation during the ageing process. FAR-FTIR-experiments were subsequently performed at differently aged PE test samples to characterize the oxidation process and morphological changes in the samples during the ageing at 125°C. T2 - 11'th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 04.12.2019 KW - FTIR KW - High Molecular Polyethylene KW - Ageing PY - 2019 AN - OPUS4-49988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Comparison of ageing behaviour of O-ring seals under hydrogen and air N2 - Elastomeric seals are essential components in the infrastructure which prevent leakage of gas and proper function of technical devices and are therefore highly safety relevant. For proper function a remaining resilience and tolerance to pressure changes is required. The ageing of elastomers is an undesirable but inevitable process leading to a limited lifetime of rubber products such as seals. Independent of the application, as e.g. automotive, piping or container applications, a long lifetime or at least a timely exchange of a seal before occurrence of critical failure is desired. Hydrogen is a key element for the energy turnaround and therefore the compatibility of seals with hydrogen is essential. In addition to the effect of hydrogen uptake and release, which might also cause destructive effects such as rapid gas decompression, ageing at high temperature under hydrogen atmosphere is of interest too. Most of the existing work is addressing the performance of new materials and comprises only very limited investigations concerning long-term use and the behaviour of aged materials in contact with hydrogen. As ageing can lead to substantial changes of material properties, it must be evaluated whether these changes are beneficial or deteriorating for the component function. In this work we present and compare results of the characterisation of three sealing materials (EPDM, HNBR, FKM) after ageing at high temperature under hydrogen and air. Despite the common assumption that ageing under hydrogen atmosphere should be less severe for the material in comparison to air ageing, this is not the case for every material. T2 - RubberCon 2023 CY - Edinburgh, Scotland DA - 09.05.2023 KW - Hydrogen KW - Ageing KW - Seal PY - 2023 AN - OPUS4-58178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - Photolytically and Thermally Initiated Destruction on the Stability of (Ultra)High Molecular Polyethylene N2 - THz and mid IR spectroscopy of high-molecular PE (HMW) and ultra high-molecular PE (UHMW) reveals modifications of the molecular structure. Characteristic absorption bands are changed if the two materials are exposed by γ-Co60 radiation up to 600 kGy and subsequently stored at an annealing temperature of 398 K until for 729 days. UHMW-PE and HMW-PE behave differently during the ageing process because of their molecular weight and inherent structure distinctions. The spectroscopic data offer characteristic absorption bands, which have been used to describe the complete ageing process in more detail. For instance, the integral absorption in the B1u THz-region can be used to describe quantitatively the reduction of crystallinity. The formation of trans vinylene unsaturation and the decay of vinyl during ageing can be observed in detail in the mid IR range. T2 - 9th International Workshop on Terahertz Technology and Applications CY - Kaiserslautern, Germany DA - 03.03.2020 KW - Degradation KW - MID IR Spectroscopy PY - 2020 AN - OPUS4-50555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gröke, Carsten T1 - Requirements for Package Design Testing and Quality Assurance Measures for Packages not Requiring Competent Authority Design Approval N2 - Übersicht über die gefahrgutrechtlichen Anforderungen zur Bauartprüfung und dem Qualitätsmanagement für Verpackungen für nicht zulassungspflichtige Versandstücke. T2 - KONTEC 2019 CY - Dresden, Germany DA - 27.03.2019 KW - Bauartprüfung KW - Qualitätsmanagement KW - Nicht zulassungspflichtig PY - 2019 AN - OPUS4-56352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gräf, S. T1 - Large-area fabrication of low- and high-spatial-frequency laser-induced periodic surface structures on carbon fibers N2 - The properties of fiber-reinforced polymers (CFRP) or concretes (ECC) strongly depend on the interface between the fiber and the surrounding matrix. Different methods such as plasma oxidation, chemical or electrolytic etching and chemical vapor deposition have been investigated to increase, for example, the bonding strength. The present study deals with the functionalization of the fiber surface based on laser-induced periodic surface structures (LIPSS). They can be characterized as a modulation of the surface topography on the nano- and microscale that results from the irradiation of the surface with linearly polarized laser radiation close to the ablation threshold. According to their spatial period, LIPSS are classified into low-spatial frequency LIPSS (LSFL) and high-spatial frequency LIPSS (HSFL). The great potential of both types of LIPSS structures regarding functional surface properties was demonstrated in numerous investigations. The objective of the present study was the homogenous manufacturing of both types of LIPSS on large areas of carbon fiber arrangements without damage. The results are discussed based on a detailed analysis of the topographic and chemical surface properties. T2 - 15th International Conference on Laser Ablation (COLA 2019) CY - Hawaii, USA DA - 08.09.2019 KW - Laser-induced periodic surface structures (LIPSS) KW - Carbon fibers KW - Femtosecond laser ablation KW - Surface functionalization PY - 2019 AN - OPUS4-49676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Quercetti, Thomas T1 - Drop Testing of a New Package Design for the Transport of SNF from German Research Reactors N2 - A new dual purpose cask design was developed for the safe transport and interim storage of spent fuel elements of German research reactors. In the framework of the safety assessment within the package approval procedure the Bundesanstalt für Materialforschung und –prüfung (BAM) as competent authority performed a series of drop tests according with the IAEA Transport Regulations. The package consists of a cylindrical thick-walled ductile cast iron cask body closed by a bolted lid system with metallic seals. A lid and bottom sided impact limiter consisting of a wood/steel construction limit the mechanical impact loading. The full-scale test specimen was equipped with a basket and assembled with dummy-fuel elements. The package and test specimen, respectively have a total mass of approximately 24 metric tons. The mechanical drop test program included three 9m free drop tests, in horizontal, vertical and oblique cask orientation onto the lid system. Additionally, a 1m-puncture bar drop test followed the horizontal drop test to consider an IAEA-drop test sequence. The horizontal and vertical drop tests were performed at a temperature of minus 40°C. During the oblique drop test the upper impact limiter was heated up to +80°C. The tests were conducted onto an unyielding target, fulfilling the IAEA requirements. The test specimen was considerably instrumented with strain gauges and accelerometers. Transient strains at selected locations of the inner and outer container walls, of the primary and secondary lid, as well as of the corresponding lid bolts were measured during the drop tests. Furthermore, decelerations in different locations at the cask body and the lids were measured. The complex geometrical deformation of the impact limiters due to the impact were determined by optical 3D- measurements. Before and after the drop tests the leakage rate of the lid system was determined by helium leakage testing. The experimental results contribute to the evaluation of the package response to mechanical tests, demonstrating safety under normal and accident conditions of transport and especially to the verification of the dynamic finite-element model of the package used in the package design safety report. T2 - PATRAM 2019 CY - New Orleans, LA, USA DA - 04.08.2019 KW - SNF KW - Drop testing KW - New package design PY - 2019 AN - OPUS4-50623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning A1 - Dayani, Shahabeddin T1 - Tomographic Imaging of Battery Materials at BAMline (Bessy II) N2 - Different scientific questions in battery research can be addressed by synchrotron X-Ray imaging. The BAMline at the 3rd generation synchrotron X-ray source BESSY II has been supporting researchers in a wide range of research areas for over 20 years. Being a non-destructive characterization method, synchrotron X-ray imaging, in particular tomography (SXCT), plays a particularly important role in structural characterization. This poster gives few examples from battery research conducted at BAMline. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The upgraded dual multilayer monochromator offers flexibility by providing different energy spectra to optimize flux and energy resolution as desired. The upgraded detector (in white beam configuration, equipped with an sCMOS camera) allows the higher flux to be exploited with reduced readout times. Shorter tomographic acquisition times in the range of seconds are now possible. Hence, in-situ and operando examinations are routinely available. An integrated slip ring allows continuous rotation of the sample stage for ease of wiring. The pink beam option allows tomographic observation of processes occurring in the time domain of a few seconds with a resolution down to ~ 1 µm. The in-situ capabilities include electrochemical cycling, mechanical load (tension and compression) and heating up to 1100°C. Ergebnisse The method, equipment, data handling pipeline as well as various examples from battery research conducted at BAMline are presented and discussed. In particular, the 3D morphology and distribution of deposited Li within the widely used Celgard® 2325 polyolefin separator are visualized in situ, thus promoting the understanding of the short-circuiting process of Li metal batteries. In addition, we also visualized and quantified the spatial distribution of Li depositions inside a porous carbon host to unravel the deposition behavior that can hardly be probed by surface imaging techniques. The Li electrodeposition behavior found here could help to promote the understanding and development of surface modifications related to Li anodes, separators as well as novel 3D geometry electrode designs for accommodation of Li depositions and alleviation of volumetric changes. T2 - Batterieforum Deutschland CY - Berlin, Germany DA - 18.01.2023 KW - BAMline KW - X-ray tomography KW - Li-ion battery PY - 2023 AN - OPUS4-56909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stargardt, Patrick T1 - Comparison of design concepts for ceramic oxide thermoelectric multilayer generators N2 - Multilayer thermoelectric generators are a promising perspective to the conventional π-type generators. Ceramic multilayer technology is well established for production of microelectronics and piezo-stacks. Key features of ceramic multilayer technology are full-automation, cost-effectiveness, and the co-firing of all materials in one single step. This requires similar sintering temperatures of all used materials. The development of multilayer thermoelectric generators is a subject of current research due to the advantages of this technology. One of the challenges is the compatibility of the different materials with respect to the specific design. The presented study compares three different designs of multilayer generators based on a given set of material properties. Dualleg, unileg and transverse multilayer generators are compared to conventional π-type generators., the designs are evaluated regarding the expected maximum output power and power density using analytical calculations and FEM simulations. Additionally, the complexity of the production process and material requirements are assessed and design optimizations to simplify production are discussed. Besides the theoretical aspects, unileg multilayer generator prototypes were produced by tape-casting and pressure-assisted sintering. These prototypes are compared to other multilayer generators from literature regarding the power factors of the used material system and the power density. Improvements of the power output by design optimizations are discussed T2 - 18th European Conference on Thermoelectrics CY - Barcelona, Spain DA - 13.09.2022 KW - Thermoelectric oxides KW - Thermoelectric generator design PY - 2022 AN - OPUS4-55820 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 - Dayani, Shahabeddin T1 - Quantification of Deep Discharge Mechanism in a Li-Ion Battery by operando X-ray Computed Tomography N2 - Lithium-ion batteries connected in series are prone to an electrical abuse called over discharge. We present a comprehensive investigation of the over discharge abuse mechanism in lithium-ion batteries using operando non-destructive imaging. The study focuses on understanding the behavior of copper dissolution and deposition during over discharge, which can lead to irreversible capacity loss and internal short circuits. By utilizing synchrotron X-ray computed tomography (SXCT), the concentration of dissolved and deposited copper per surface area is quantified as a function of depth of discharge (DoD). T2 - HZB user meeting CY - Berlin, Germany DA - 22.06.2023 KW - Non-destructive testing PY - 2023 AN - OPUS4-57793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Synchrotron X-Ray Tomography Techniques at BAMline N2 - A recent upgrade of key equipment of the BAMline widens its imaging capabilities: shorter scan acquisition times are now possible, in situ and operando studies can now be routinely performed, and different energy spectra can easily be set up. In fact, the upgraded double-multilayer monochromator brings full flexibility by yielding different energy spectra to optimize flux and energy resolution as desired. T2 - HZB User Meeting CY - Online meeting DA - 08.12.2022 KW - BAMline KW - X-ray imaging KW - Tomography PY - 2022 AN - OPUS4-56568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Optimization of Solid-State-Reactions of Calcium Cobaltite Ca3Co4O9 N2 - Calcium cobaltite is a promising p-type oxide thermoelectric material for high temperature applications due to its high figure of merit between 600 °C and 900 °C in air. The solid-state-reaction is well known for large scale powder synthesis of functional materials. As a high temperature process, the powder synthesis consumes a lot of energy. In different studies, different synthesis conditions were used for the preparation of calcium cobaltite powder. This study showed that a higher energy input (elevated temperatures, longer dwell times, or repeated calcinations) during powder synthesis does not increase but decrease the Seebeck coefficient and the electrical conductivity. The same correlation was determined for the densification. As a higher energy input leads to a larger grain size and therefore to a reduced sinter activity, it can be concluded that the thermoelectric properties are correlated with the sinter activity of the powder. These results can be used to minimize the energy demand for the powder synthesis of Ca₃Co₄ O₉. T2 - 14th European Conference on Thermoelectrics CY - Lisbon, Portugal DA - 20.09.2016 KW - Thermoelectrics KW - Solid-State-Reaction KW - Calcium cobaltite PY - 2016 AN - OPUS4-37543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sagradov, Ilja T1 - Long-term tests and numerical simulations on metal seals based on continuous force measurement in compressed state N2 - In Germany, the search for a disposal site for heat-generating radioactive waste will take decades longer than originally assumed. Transport and storage casks must therefore ensure safe containment for extended interim storage periods, possibly over 100 years. In order to maintain the required leak tightness, spring core metal seals with aluminum or silver cladding are used. As sealing force decreases over time, BAM has been conducting tests for over 15 years to prove their long-term reliability. This work - a joint project of BASE and BAM - aims to obtain additional material data using a new device for continuous measurement of compression force over time and temperature for lifetime prediction models and is supported by FEM simulations. Initial tests on aluminum and silver seals have been completed, and first results are presented. T2 - safeND 2025 CY - Berlin, Germany DA - 17.09.2025 KW - Interim storage KW - Metal seal KW - Restoring force PY - 2025 AN - OPUS4-64991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grelle, Tobias T1 - Creep Investigations on Aluminum Seals for Application in Radioactive Waste Containers N2 - In Germany spent nuclear fuel (SNF) and high level radioactive waste (HLW) are stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. Being licensed for up to 40 years of interim storage the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads. T2 - International Conference on Aluminum Alloys CY - Montreal, Canada DA - 17.06.2018 KW - Metal seal KW - Creep KW - Long-term behavior PY - 2018 AN - OPUS4-45843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sagradov, Ilja T1 - Long-term tests on metal seals using continuous force measurement in compressed state N2 - In Germany, spent fuel and heat generating radioactive waste is stored in casks for transport and storage (DPCs). The storage licenses were granted for up to 40 years. Due to the delay in identifying a final repository site for such radioactive waste, the storage periods are to be extended significantly. The objective of our research work is to collect additional material data for metal seals in order to be able to better assess the long-term safety of the sealing system of the casks for a period of up to 100 years. A principal safety consideration for the DPCs is the long-term performance of bolted lid sealing systems utilizing metal seals to ensure the safe enclosure of the radioactive inventory during interim storage. To assess the sealing behavior, it is necessary to examine the aging-dependent residual restoring force for the metal seals and the usable resilience. By investigating the change in these values as a function of time and temperature, further insight can be gained into the assessment of long-term safety for extended interim storage. In the present study, the restoring force of metal seals with an outer aluminum jacket and a torus diameter of 9.9 mm was measured continuously. For this purpose, a specially designed device equipped with a load cell was used under isothermal conditions. As part of the investigation, the level and rate of decrease of the restoring seal force were recorded over test periods of one and two months. The seal temperature was set to 35 °C, 75 °C, 100 °C, 125 °C, and 150 °C, respectively. A direct correlation was observed between the temperature of the seal, the level of the restoring force after compressing and heating the seal, and the drop-off characteristics of the restoring force. It was found that in our test device the force level immediately after reaching the respective temperature is lower for higher seal temperatures, while the drop rate of the restoring force is higher. This paper describes the experimental setting and discusses first results in comparison with our long-term discontinuous measurements. T2 - 21st International Symposium on the Packaging and Transportation of Radioactive Materials - PATRAM 2025 CY - San Antonio, TX, USA DA - 27.07.2025 KW - Temperature-Dependent Performance KW - Extended Interim Storage KW - Long-Term Safety Assessment KW - Metal Seal Aging KW - Restoring Force Degradation PY - 2025 AN - OPUS4-63891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eberwein, Robert T1 - Systems With Cryogenic Liquefied Gases In Fire-Incidents N2 - The volumetric energy density of a gas can be increased by liquefaction, which occurs when the gas is cooled below the saturation point. Liquefied gases of great importance to the energy transition are Liquefied Hydrogen (LH2) and Liquefied Natural Gas (LNG), which can be liquefied at temperatures below 160°C. Systems for storing these gases typically must be overpressure resistant and require thermal super insulations (TSI) to hold cryogenic conditions and minimize boil-off losses from evaporation. TSI with vacuum and MLI or perlites are suitable for many applications involving LNG and LH2. Such systems are typically double-walled structures where the inner wall is in contact with the cryogenic liquefied gas. MLI or perlites are located in the gap between the inner and the outer wall, that is kept under vacuum conditions. This combination of insulations strongly reduces the heat transfer between the environment and the cryogenic liquefied gas. From an economic point of view the systems are well sophisticated. However, knowledge of the behavior of this kind of systems in a typical event such as a fire is limited, but necessary to evaluate the safety of the increasing number of applications. The objective of the research is to determine how TSI behaves at different fire temperatures during fire exposure and afterwards. Special attention is paid to changes in the heat flux, the material properties and vacuum state over time. For this purpose, thermogravimetric analysis (TGA) studies have been carried out. In addition, a test rig was developed that allows testing of TSI at temperatures up to 1000°C under realistic integration conditions and subsequent analysis of the TSI samples. In the test rig the double-wall with vacuum and MLI or perlites inside is simulated. The fire conditions are simulated on one side of the double-wall by adjustable electrical heating elements. This process allows the implementation of repeatable heat flows of up to 100 kW/m². On the other side of the double-wall, cold or cryogenic conditions are simulated with a heat exchanger through which water or the vapor of liquid nitrogen (approx. -196°C) flows. The heat exchanger is also used to determine the heat flux through the double-wall. Thus, the test rig allows thermal loading and performance analysis of TSI samples at the same time. Compared to tests with real cryogenic systems, tests with this experimental setup have the advantage that, first, the instrumentation is easier to realize, and a higher repeatability is ensured. Second, the local heat flow can be determined over time, and the sample of a TSI can be taken non-destructively and thus analyzed. Third, the tests are less risky as well as time+ and material intensive, so that more tests and variants can be investigated with the same budget. Preliminary results obtained considering several types of MLI under vacuum show that all observed typs of MLI can be damaged under strong thermal loading. The damages observed were outgassing, melting, shrinkage, cracking, lump formation, and concomitant local loss of the MLI's function as a radiation shield. However, the study also shows that a damage does not always have an extreme effect on the insulating performance. T2 - IMECE2022 CY - Columbus, Ohio, USA DA - 30.10.2022 KW - LH2 KW - LNG KW - Safety KW - Insulation KW - Tank PY - 2022 AN - OPUS4-56445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayat, Mehmet A1 - Kipphardt, Heinrich A1 - Tiebe, Carlo A1 - Engelhard, Carsten T1 - Effect of Trace Humidity on Trace Ammonia Quantification N2 - Hydrogen is receiving growing attention as a promising medium for energy storage and transportation. Proton exchange membrane (PEM) fuel cells are a key technology for energy conversion from hydrogen. However, high purity hydrogen is required for this technology, as described in standards such as ISO 14687:2019. A critical impurity that impairs PEM efficiency is ammonia, for which a limit value of 100 nmol/mol applies. In addition, the maximum amount of humidity is specified with 5 µmol/mol. The presence of humidity in hydrogen at levels up to 50 times higher than ammonia raises the critical question of whether ammonia can still be quantified accurately in the lower nmol/mol range without interference from water. In addition, the general question arises as to whether the critical analyte, ammonia, can still be detected at all, given the expected surface effects at such amounts of trace humidity. In this work, we describe the influence of trace humidity on the surface behavior of adsorbed ammonia on stainless steel. Samples with ammonia at approximately 100 nmol/mol in hydrogen, with trace humidity levels ranging from 3 µmol/mol to 10 µmol/mol, were carefully prepared using dynamic mixing. Humidification was conducted using an advanced saturation method. These samples were investigated under atmospheric conditions using low pressure sampling Optical Feedback Cavity Enhanced Absorption Spectroscopy (OFCEAS). From the observed time-dependent signals, kinetics were determined and analyzed, yielding insights on the strength of the adsorption behavior of the analytes. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - OF-CEAS KW - Hydrogen KW - Ammonia KW - Water KW - Humidity KW - Kinetics KW - Adsorption PY - 2025 UR - https://veranstaltungen.gdch.de/microsite/index.cfm?l=11713&sp_id=2&selSiteID=vplanner AN - OPUS4-64046 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 - Winckelmann, Alexander T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by glow-discharge optical emission spectroscopy N2 - Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - Lithium Ion Batteries KW - GD-OES KW - FIB KW - SEM KW - EDX PY - 2022 AN - OPUS4-56246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by glow-discharge optical emission spectroscopy N2 - Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs.[1] Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs. T2 - European Winter Conference on Plasma Spectrochemistry (EWCPS 2023) CY - Ljubljana, Slovenia DA - 29.01.2023 KW - Lithium-ion batteries KW - Aging mechanisms KW - Depth-profiling PY - 2023 AN - OPUS4-56992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Hydrogen in Welded Microstructures of T24 Steel: Effect on Mechanical Properties and Corresponding Hydrogen Diffusion N2 - Low-alloyed CrMoV steels, such as T24, are widely used for welded components in fossil power stations due to their excellent creep-strength. Spectacular failure cases in the recent years exhibited severe cracking in T24 welds. The results showed that hydrogen-assisted cracking (HAC) occurring up to 200 degree Celsius cannot be excluded. Hence, a basic understanding is necessary on how hydrogen affects the material properties of welded microstructures. In this regard, each weld microstructure (HAZ and weld metal) has influence on the HAC susceptibility and respective hydrogen diffusion. Thus, the present contribution summarizes different results obtained from experiments with grades T24 (CrMoV alloy) and T22 (CrMo) and thermally simulated HAZ. Tensile tests were conducted with hydrogen charged specimens and compared to hydrogen-assisted stress corrosion cracking results obtained from slow strain rate tests (SSRT) up to 200 degree Celsius. Electrochemical permeation and degassing experiments were performed to identify a particular weld microstructure influence on hydrogen diffusion and trapping (especially in the HAZ). The results showed that T24 base material has improved resistance to hydrogen-assisted degradation/cracking. In contrast, the as-welded HAZ had remarkably increased susceptibility (tesnile tests at hydrogen concentration of 1 to 2 ppm). SSRT experiments confirmed this at elevated temperatures for both the T24 and the T22. Hence, the evaluation of a particular degradation of the mechanical properties should be performed independently for each weld microstructure. In addition, the HAZ showed decreased diffusion coefficients (at room temperature) of approximately one magnitude compared to the base materials. Trapped hydrogen was determined in the T24 at temperatures up to 120 degree Celsius compared to 75 degree Celsius in the T22. This has to be considered in case of changing operational temperatures, e.g. in the case of start-up and shutdown processes of boiler components. T2 - 10th Conference on Trends in Welding Research CY - Tokyo, Japan DA - 11.10.2016 KW - Degradation of Mechanical Properties KW - Hydrogen KW - Creep-resistant Steel KW - Weld Joint KW - Diffusion PY - 2016 AN - OPUS4-37827 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 TransHyDE - H2HohlZug Project N2 - As the world moves towards a decarbonised economy, the demand for sustainable and low-carbon alternatives is growing rapidly. Hydrogen has an important role to play 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, mainly steels, are the most commonly 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 required 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. Unlike the conventional autoclave technique, this method requires significantly lower amounts of hydrogen, resulting in fewer safety measures and no need for complex equipment or a specialised laboratory. The technique's low investment and testing costs, simple operation, and shorter testing time make it an 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 an ISO committee 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, of which the overall aim is to systematically close the gaps towards a standard. This contribution presents the structure and milestones of the project, followed by initial results. T2 - TransHyDE Vollversammlung 2025 CY - Leipzig, Germany DA - 26.11.2025 KW - Hydrogen KW - Hydrogen Embrittlement KW - Hollow Specimen Technique KW - High-Pressure Gaseous Hydrogen KW - TransHyDE KW - H2HohlZug KW - Standardisation PY - 2025 AN - OPUS4-64938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - El Harrab, Hayat A1 - Askar, Enis A1 - Franken, T. A1 - Mauss, F. T1 - Experimental and Kinetic Study of Lubrication Oil Composition on Hydrogen Auto-Ignition N2 - Hydrogen internal combustion engines (H₂ ICEs) present a promising alternative to conventional fuels, but they face challenges such as pre-ignition, where lubricating oils play a critical role. This study investigates the auto-ignition behavior of two base oils — Group II (mineral) and Group V (Ester) — and three formulated oils (Oils A, B, and C) at 20 bar using a heated constant-volume autoclave. Oil A and Oil B share a Group II (mineral) base, with Oil A containing lower levels of calcium-based detergents and higher levels of phosphorus-based antioxidants compared to Oil B. In contrast, Oil C is formulated with a Group V (ester) base oil, incorporating magnesium-calcium detergents. The auto-ignition temperature was measured in both air and stoichiometric hydrogen-air mixtures to assess the influence of oil composition, additives, and hydrogen addition on ignition characteristics. Results show that hydrogen’s AIT at 20 bar is 460°C but drops to 270°C with the addition of 0.2 ml of base oil. Base oils exhibited similar AITs in air (260°C) and hydrogen-air mixtures (270°C), with reactivity differences linked to molecular composition — ester (Group V) displayed lower reactivity compared to mineral oil (Group II). Formulated oils demonstrated slightly higher AITs (up to 290°C), where phosphorus-based additives reduced reactivity, while lower calcium content further slowed ignition. Among the tested oils, the ester-based oil with a mixture of calcium and magnesium detergents exhibited the lowest reactivity, making it a promising candidate for hydrogen engines. Additionally, reduced oxygen availability increased AIT by 10°C and prolonged ignition delay. A chemical analysis was also performed to evaluate the ignition properties of Group II (mineral) and Group V (ester) oils under varying temperatures. These findings highlight the impact of lubricant composition on pre-ignition behavior in H₂ ICEs, offering valuable insights for optimizing lubricant formulations. T2 - 12th European Combustion Meeting CY - Edinburgh, United Kingdom DA - 07.04.2025 KW - Hydrogen KW - Pre-Ignition KW - Group V Ester Oil KW - Auto-Ignition Temperature KW - Additive Effects KW - Ignition Delay Time KW - Group II Mineral Oil KW - Lubricating Oil PY - 2025 AN - OPUS4-64761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konert, Florian T1 - Evaluation of hydrogen effect on hardened and annealed 100Cr6 steel N2 - The use of hydrogen demands high safety requirements, since hydrogen can be absorbed by metallic materials and may cause hydrogen embrittlement (HE) under certain conditions. Slow strain rate (SSR) tensile testing is a widespread method to quantify the hydrogen-induced ductility loss of alloys. Here, the hollow specimen technique was used to evaluate the effect of 150 bar hydrogen on the tensile properties of solution annealed and hardened 100Cr6 steel, which is a common material for bearing systems. This technique reduces the required amount of hydrogen and minimizes the duration and costs of the tests performed compared to in-situ tensile tests in autoclaves. T2 - EPRI Workshop on Hydrogen Embrittlement 2024 CY - Oxford, UK DA - 23.06.2024 KW - Hydrogen KW - Hydrogen Embrittlement KW - Hollow Specimen Technique KW - 100Cr6 PY - 2024 AN - OPUS4-60476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nietzke, Jonathan T1 - Influence of strain rate on the effect of hydrogen in pre-charged 316L stainless steel: A comparison of conventional and hollow specimen testing N2 - The growing demand for hydrogen requires an expansion of testing capabilities to assess the performance of metallic materials under hydrogen exposure. Considering only gaseous atmospheres, there is a variety of in-situ and ex-situ methods used to investigate the material behavior while or after exposed to hydrogen, respectively. Among these methods, a more conservative one is the in-situ testing at slow strain rates (SSRT) using conventional tensile specimens. While results obtained by a conservative procedure may be more applicable in many cases than those of ex-situ experiments, the tests are quite demanding, leading to limited testing capacities and high costs, especially for very slow strain rates. A possible solution that can enable in-situ testing at relatively low cost is the hollow specimen technique which gained increasing interest in the last decade. The main reasons are the minimal volume of hydrogen required and the elimination of a high-pressure hydrogen autoclave leading to significantly lower costs and enabling more laboratories worldwide to perform these tests. However, interpreting results from hollow specimens, especially when compared to conventional ones, remains a significant challenge. To address this, an experimental study was conducted using conventional and hollow specimens, both uncharged and pre-charged. Pre-charging was achieved using pure hydrogen (5.0, i.e. 99.999 %) at 100 bar and 300 °C for around 21 days. In order to obtain suitable reference specimens, other specimens were stored in argon at 100 bar and 300 °C for the same period of time. The tests were performed at various strain rates, down to 1E-6 1/s. While these ex-situ experiments are not directly comparable to in-situ tests with both types of specimens, they do provide some insights into the differences between the results of hollow and conventional specimens. Therefore, the elongation at fracture and reduction of area (RA) were compared, among other aspects. In addition, fractographical analyses were carried out using SEM images. Elongation at fracture was not significantly affected by hydrogen in conventional specimens, but it was slightly reduced in hollow specimens. RA, on the other hand, was lower for tests with hydrogen in both types of specimens across all strain rates. Moreover, the strain rate did not appear to influence hydrogen embrittlement in conventional specimens whereas in hollow specimens, tests conducted at higher strain rates (1E-4 1/s) showed a greater impact of hydrogen on elongation at fracture than those at lower strain rates (1E-6 1/s), which is contrary to the typical expectation. These findings suggest that the influence of hydrogen differs between conventional and hollow specimens, possibly due to factors such as surface roughness and differing stress states. However, further experiments are needed to fully understand these differences, including in-situ experiments to understand potential differences in hydrogen absorption between the two specimen types. T2 - EPRI Workshop on Hydrogen Embrittlement CY - Oxford, England, United Kingdom DA - 23.06.2024 KW - Stainless steel KW - Hollow specimen KW - Pre-charging KW - Hydrogen PY - 2024 AN - OPUS4-60494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mosquera Feijoo, Maria T1 - Thermal-mechanical fatigue of oxide scales in cyclic water vapor oxidation of 9-12 % Cr steels N2 - Ferritic-martensitic steels with 9-12 % Cr-content are widely used as high temperature construction materials in power plant due to their high temperature properties such as creep resistance, strength, and favorable oxidation resistances. However, typical operating conditions include cyclic thermal/mechanical loading, and as a result the oxide scale might fail; cracks are formed and the oxide scale is spalled off. The oxide spalls can cause steam tube blocking and local thermal stresses, which might provoke shorter component service life. This work investigates the scale spallation behavior of ferritic-martensitic steels under cyclic load condition between 320°C and 620°C for up to 210 cycles in pure steam. All samples were isothermally pre-oxidized at 620°C for 500 h in water steam with 30 bar pressure to create an initial magnetite layer with low porosity. Different sample shapes, rectangular coupons, full rings and U-shape segments, are investigated to evaluate the impact of the geometry on these conditions. After oxidation experiments the oxidation kinetics in terms of mass change, metal loss and thickness scale is determined. In addition, the integrity of the oxide layer as well as its adherence to the matrix are characterized by modified hardness tests and scratch tests. Breakage of the layers at lower applied forces indicates a substantial loss of adhesion strength at intermediate cycle numbers. T2 - EUROCORR 2017 CY - Prague, Czech-Republic DA - 03.09.2017 KW - Geometry influence KW - Therma-mechanical fatigue KW - Oxide layer KW - Cyclic test KW - Scale adherence PY - 2017 AN - OPUS4-42635 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 - Duplex Stainless Steels (DSS) are an essential component used 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 Assisted Cracking (HAC). Several mechanisms have been proposed to describe the occurring microscale processes behind HAC, and these include metastable phase transformation, Hydrogen Enhanced Localized Plasticity (HELP), and Hydrogen Enhanced Decohesion (HEDE). This 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), tensile testing and hydrogen concentration measurements using Carrier Gas Hot Extraction (CGHE). T2 - Third German-African Green Hydrogen Forum 2025 CY - Bernburg (Saale), Germany DA - 23.09.2025 KW - Hydrogen Assisted Cracking KW - High Pressure Hydrogen KW - Duplex Stainless Steels KW - Hollow Specimen Technique PY - 2025 AN - OPUS4-64302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mayer, Uwe T1 - Untersuchung des Master Curve-Konzeptes für ferritisches Gusseisen mit Kugelgraphit N2 - In dem Poster werden der Forschungsansatz, die Ziele, das Untersuchungsprogramm und die erwarteten Ergebnisse des BMUV-Forschungsvorhabens MCGUSS "Untersuchung des Master Curve-Konzeptes für ferritisches Gusseisen mit Kugelgraphit" vorgestellt. Mit Blick auf bruchmechanische Sicherheitsbewertungen in der Kerntechnik werden Stähle momentan mit dem deterministischen ASME-Referenzkurvenkonzept, ergänzt durch das probabilistische Master Curve-Konzept nach ASTM E1921, bewertet. Das Master Curve-Konzept wird bereits für die Bewertung von ferritischen Schmiedestahlbehältern verwendet. Bewertungsmethoden für ferritisches Gusseisen mit Kugelgraphit sind im Moment unvollständig. Normen wie die nationale BDG-Richtlinie P300 oder der internationale ASME-Code, Sect. III, Div. 3, WC-2330 decken Sprödbruch nicht ausreichend ab. Die Verwendung des Master Curve-Konzepts für ferritisches Gusseisen mit Kugelgraphit würde eine bruchmechanische Bewertung via einer KJc,d Verteilung erlauben und gleichzeitig Größeneffekte und einen Temperaturbereich von 100 K berücksichtigen. T2 - GRS-Projektstatusgespräch 2023 CY - Karlsruhe, Germany DA - 06.11.2023 KW - Dynamische Bruchzähigkeit KW - Sprödbruch KW - Gusseisen mit Kugelgraphit KW - Master Curve PY - 2023 AN - OPUS4-59060 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Butz, Adam T1 - Experimental and analytical investigation of notched components of a Nickel based superalloy under high temperature cyclic loading N2 - While the increase in use of renewable energy sources is a necessity in times of climate change the use of gas turbines as back-up requires them to be run in a much more flexible manner in order to compensate for side effects like sudden fluctuations of energy generation. The significant changes of stress and temperature levels in turbine blades due to start-up and shut down can cause crack initiation and growth in the blades‘ alloy. The aim of this research project is to identify a model for lifetime prediction for gas turbine components made of a Nickel base superalloy under high temperature with a Focus on stress concentration points such as cooling holes. T2 - HIDA-7 Conference on Life/Crack Assessment & Failures in Industrial Structures, UK CY - Portsmouth, UK DA - 15.05.2017 KW - LCF KW - Gas turbine KW - Service life model PY - 2017 AN - OPUS4-42274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mesquita Silva da Veiga, Marcia T1 - Ultrasonic-assisted leaching of Li and Co from black mass using deep eutectic solvent N2 - The recovery of critical metals from spent lithium-ion batteries is a key strategy for sustainable resource management and the circular economy. Conventional hydrometallurgical processes typically rely on strong mineral acids and elevated temperatures, which, although effective, generate hazardous waste and demand high energy inputs. As a greener alternative, deep eutectic solvents (DES) combine low toxicity, non-volatility, simple synthesis, and tunable physicochemical properties, making them promising media for selective metal recovery1-2. Here, we report for the first time the use of ultrasound (US) to assist the leaching of Li and Co from LiCoO₂ black mass employing a deep eutectic solvent based on choline chloride and formic acid (ChCl:HCOOH, 1:2 molar ratio). The DES was synthesized at 90 °C for 3 h under stirring (300 rpm) and was characterized in terms of its molecular structure and formation by 1H-NMR and FT-IR, as well as by its viscosity and density. For each experiment, ~0.100 g of LiCoO2 was treated with 5 g of DES-FA in an ultrasonic bath (35 kHz, 60 °C) for different irradiation times (30–120 min), followed by three sequential extractions. All measurements were performed by ICP OES. Lithium solubilization reached ~80% at 90 min, while cobalt extraction was stabilizing at ~79% after 120 min. The enhanced performance under US is attributed to sonochemical effects that promote cavitation and microjets, leading to the disruption of particle agglomerates, the thinning of diffusion layers, and the generation of highly reactive local environments. These processes accelerate deintercalation and mass transfer within the solid–liquid interface. Combined with the mild acidity of DES-FA, which enables simultaneous leaching of both metals while favoring faster kinetics for Li, ultrasound provided a synergistic effect that enhanced the overall process and preserved the distinct extraction profiles of Li and Co. The extraction behavior of the two metals can be explained by their different speciation in the DES-FA medium. Cobalt is likely reduced from Co(III) to Co(II) by formic acid and stabilized through the formation of chloro-complexes such as [CoCl4]2- with chloride anions from ChCl, favoring its solubilization. In contrast, lithium does not form stable complexes with chloride under these conditions. It is primarily extracted as a solvated cation, stabilized by the extensive hydrogen-bond network of the DES. This difference accounts for the faster leaching kinetics observed for Li compared to Co. Selective recovery was achieved by pHcontrolled precipitation, with cobalt oxalate at pH 4-5 and lithium carbonate at pH 10. The Eco-Scale score of 85 confirmed the greenness of the method. This pioneering approach highlights the potential of coupling DES chemistry with ultrasound. Together, they represent a sustainable and efficient route for recovering critical metals from battery waste. T2 - 17th Rio Symposium on Atomic Spectrometry (17th RSAS) CY - São Pedro City, Brazil DA - 09.11.2025 KW - Black mass KW - deep eutectic solvent KW - Lithium KW - Cobalt KW - Lithium-ion battery recycling KW - Ultrasound-assisted extraction KW - Lithium and cobalt recovery KW - Green hydrometallurgy PY - 2025 AN - OPUS4-64956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimault de Freitas, Tomás T1 - Comprehensive Standardisation of the Hollow Specimen Technique for Tests in High-Pressure Hydrogen Gas N2 - The hollow specimen technique is a simple and economical method that has the potential to overcome the limitations and complement the current techniques for qualifying metallic materials under highpressure hydrogen gas. In this technique, an axial hole is manufactured 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 does not require complex equipment or a specialised laboratory, unlike the conventional autoclave technique. 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 to standardise the method, however, there are still open questions that currently prevent the technique from being standardised for hydrogen testing. These open questions are being addressed in the H2HohlZug project, which is presented in this contribution. T2 - Oxford - EPRI Hydrogen Embrittlement Workshop CY - Oxford, United Kingdom DA - 23.06.2024 KW - Hollow Specimen Technique KW - High-pressure Gaseous Hydrogen KW - Hydrogen Embrittlement KW - Tensile Testing PY - 2024 AN - OPUS4-60501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Junias, Josua Kondja T1 - Prediction of Explosion Characteristics of Hydrogen Mixtures Using Machine Learning Models N2 - An understanding of Hydrogen-Oxygen/Air-Diluents gas mixtures combustion characteristics and their accurate prediction is crucial for ensuring the safety of hydrogen-related applications, reducing accidents risk, and protecting lives and property. Hydrogen detonation propagations are characterized by the detonation cell size, used to quantitatively predict for a mixture to detonate including, among others, the initiation energy, critical and minimum tube diameters. For the prediction of explosion limits, detonation run-up-distances and cell sizes, various empirical, semi-empirical and numerical models can be found in literature. These models are usually limited to a narrow range of explosion process or geometrical experimental parameters. Moreover, based on the limited availability of the detonation cell widths measurements, current estimation models are seemingly inaccurate. Machine learning models can be utilized to make justifiable prediction on the detonation cell sizes of hydrogen-air mixtures and other gaseous explosive mixtures cell sizes, explosion limits or run-up distance to detonation based on the mixture type, temperature, pressure, equivalence ratios as well as on geometrical parameters with consideration of highly diverse experimental data measurements uncertainties. Therefore, an up-to date database for explosion characteristics will be established and machine learning models will be developed, trained, tested, and validated using experimental data to predict explosion characteristics of hydrogen mixtures. The models predicted results will be validated against existing models. It will be tested whether machine learning models are able to predict the explosion characteristics of hydrogen mixtures with better accuracy and more comprehensively than conventional empirical and numerical models to be found in literature. T2 - Combustion Institute 40th International Symposium CY - Milano, Italy DA - 21.07. 2024 KW - Prediction, detonation KW - Machine Learning KW - Flammability limits PY - 2024 AN - OPUS4-60769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nattuveettil, Keerthana A1 - Brunner, Nanine A1 - Tiebe, Carlo A1 - Melzer, Michael A1 - Johann, Sergej A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Einsatz von Sensortechnologien an einer Wasserstofftankstelle als Beitrag zur digitalen Qualitätsinfrastruktur T1 - Use of sensor technologies at hydrogen test platform as a part of QI Digital N2 - Die Optimierung und Validierung des digitalen Wasserstofftankstellenmanagements mit Sensortechnologien ist das übergeordnete Ziel des Teilprojekts Digitale Qualitätsinfrastruktur mit Sensortechnologien (QIST) am Use Case H2, im Rahmen der digitalen Qualitätsinfrastruktur (QI digital[1]). Hierfür sollen u.a. Sensornetzwerke mit digital-gestützten Auswertungsstrategien intelligent gestaltet werden (Stichwort KI bzw. digitaler Zwilling). Verschiedene, sich ergänzende Sensoren, Systemkomponenten und KI-Methoden stehen als Bausteine intelligenter Sensorsysteme zur Verfügung, mit dem Zweck, die physikalischen und chemischen Parameter an und in Anlagen umfassend und effizient zu überwachen sowie Fehlfunktionen zuverlässig zu detektieren und zu interpretieren, Abbildung 1. Konkrete Arbeitsschritte sind, nach dem Aufbau der Versuchsplattform „Wasserstofftankstelle“, die Instrumentierung von Sensorik und deren digitale Integration in das Tankstellenmanagementsystem sowie die Validierung im Realbetrieb. Die somit erzielten Messergebisse sowie die Messunsicherheiten, Historien und Verfahren werden in digitaler Form aufbereitet, gespeichert und fortlaufend in die KI-basierte Datenauswertung einbezogen, inkl. der Anbindung an die metrologische Rückführungskette. Ziele sind: • Einführung eines neuen messtechnischen Ansatzes und eines digitalen Zwillings für den Anwendungsfall "Wasserstofftankstelle" auf Basis der H2-Sensorik sowie der Zustandsgrößen Druck und Temperatur • Qualitätssicherung durch Applikationen zuverlässiger Gassensorik, Manometer und Thermometer sowie KI-Methoden zur Prozesskontrolle und Detektion von Fehlfunktionen • Nutzung von digitalen Kalibrierscheinen (DCCs) insbesondere für die Messgröße Temperatur zur Realisierung der metrologischen Rückführung in einer digitalen Qualitätsinfrastruktur T2 - Sensorik für die Digitalisierung chemischer Produktionsanlagen CY - Frankfurt a. M., Germany DA - 13.06.2022 KW - QI Digital KW - H2Safety@BAM KW - Wasserstoff KW - Hydrogen KW - Sensorik KW - Digitalisierung KW - Digitalisation PY - 2022 AN - OPUS4-55399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Theiler, Geraldine T1 - Effect of temperature on the friction behaviour of rubber materials in hydrogen N2 - Safety and reliability are the major challenges to face for the development and acceptance of hydrogen technology. It is therefore crucial to study deeply material compatibility, in particular for tribological components that are directly in contact with hydrogen. Some of the most critical parts are sealing components that face high risk of damage due variation of pressure, temperature and mechanical stress. In this study, the friction and wear behaviour of several rubber materials was evaluated in hydrogen environment at ambient and low temperature. Tests were performed against 316L disks in a reciprocation motion. Results reveal that the hydrogen affects the friction and wear behaviour of most materials. The friction mechanism is dominated by deformation for most rubber materials at ambient temperature while sliding occurs at low temperature due to the increased hardness of the rubbers. T2 - Polytrib 2024 CY - Portorož, Slovenia DA - 03.10.2024 KW - Reciprocating sliding KW - Rubber materials KW - Hydrogen KW - Low temperature PY - 2024 AN - OPUS4-62019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eberwein, Robert T1 - LH2 Tanks In Fire Incidents - The Cryogenic High Temperature Thermal Vacuum Chamber Enables In-Depth Insights N2 - Liquefied Hydrogen (LH2) and Liquefied Natural Gas (LNG) establish themselves as important energy carriers in the transport sector. Their storage requires tanks with thermal super-insulations to keep them at cryogenic conditions for a long time. These insulation systems have proven itself in various applications over a long time. However, these insulations are still new in land transportation, where accidents involving collisions, fires, and their combination are to be expected. This study summarizes the results of the ongoing research program in which insulations commonly used in industry were analysed through experimental and numerical studies under fire-like conditions. It was found that there are strong differences among the various insulation systems. Several safety concerns and research gaps exists for layered insulations, which are typically used in land transport. To further analyse these insulation systems, a new test concept called Cryogenic High Temperature Thermal Vacuum Chamber (CHTTVC) was developed and manufactured. This concept enables the testing of large insulation samples under industrial conditions and the consideration of cryogenic conditions relevant for the investigation of various phenomena. The results are important for the evaluation of accident scenarios, the improvement of thermal super-insulations, and the development of emergency measures. T2 - IMECE 2024 CY - Portland, OR, USA DA - 17.11.2024 KW - LH2 KW - LNG KW - Fire KW - Insulation KW - Safety PY - 2024 AN - OPUS4-61752 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzwarth, Marcel A1 - Baer, Wolfram T1 - Investigation of the Master Curve Concept for Ferritic Ductile Cast Iron N2 - The current framework for safety assessment of ferritic ductile cast iron (DCI) containers for transport and storage of radioactive materials applies fracture mechanics principles. As established by the IAEA safety standard SSG 26, prevention of crack initiation is the governing criterion and no reliance in design should be placed on any predicted ductile tearing resistance. Similarly, the ASME-Code, Sect. III, Div. 3 explicitly deals with DCI and requires a safety proof for dynamic loading conditions. However, information given in the guidelines does not seem to be sufficient to appropriately perform such dynamic fracture mechanics safety assessments. The ongoing German research project MCGUSS is tailored to tackle this status. In MCGUSS, the application potential of the probabilistic fracture mechanics master curve (MC) concept according to ASTM E1921 is being systematically investigated and potential modifications specific for dynamic brittle fracture of DCI will be identified. While MCGUSS covers testing of a high number of SE(B)- and C(T)-type specimens, this poster focuses on preliminary C(T) results. The obtained data was statistically analyzed, and current results of MC analyses are discussed. Special emphasis of MCGUSS is on using optical and scanning electron microscopy to link microstructural damage and failure processes to the fracture toughness data gained. A fracture mechanism called "specimen size-dependent arrest of local brittle fractures before global brittle failure by weakest link" is proposed to describe the established dynamic toughness data. Concerning the MC concept, it was shown that the ASTM E1921 procedure cannot simply be adopted to dynamic DCI toughness data on a one-to-one basis. Material specific modifications are being investigated and the DCI dynamic fracture toughness data base is to be expanded. T2 - MPA Conference 2025 CY - Stuttgart, Germany DA - 06.10.2025 KW - Dynamic fracture toughness KW - Ductile cast iron KW - Safety assessment KW - Master curve KW - Statistics PY - 2025 AN - OPUS4-64367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sander, Luise T1 - Linking material and electrode properties to the cell performance 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 regard to recycling. Herein we report the preliminary investigations of the chemical and structural composition of first commercial SIB-cells.[1,2] Two different SIB-cell types were compared in terms of electrode size, thickness, loading etc. Furthermore, the composition of the active materials and electrolyte was investigated and compared. Finally, the gained results were linked to the different data sheet performance of the two cell types. T2 - Batterieforum Deutschland 2026 CY - Berlin, Germany DA - 20.01.2026 KW - Electrochemical Energy Storage KW - Battery KW - Sodium-ion-battery KW - EES KW - Energy Storage PY - 2026 AN - OPUS4-65588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bhattacharya, Biswajit A1 - Akhmetova, Irina A1 - Rautenberg, Max A1 - Emmerling, Franziska T1 - Mechanochemical synthesis of phosphonate-based proton conducting metal organic frameworks and hydrogen-bonded metal phosphonates N2 - Proton exchange membrane fuel cells (PEMFCs) are one of the most promising alternative green energy technologies that deliver high energy density without CO2 emissions. The proton conductivity of proton exchange membranes (PEM) contributes to the overall efficiency of a PEMFC. Materials being used as PEMs must exhibit high proton conductivity at the working conditions of the targeted PEMFC. To date, Nafion and Nafion-like polymers with acidic functionality are widely used as membrane materials due to their high proton conductivity in the range of 10-1 to 10-2 Scm-1 at higher relative humidity. However, these materials suffer from high costs, hazardous production process, and poor performance at high temperatures, limiting their versatility. In this context, crystalline porous materials are recognized as promising proton conductors for the proton exchange membrane (PEM) in fuel cell technology, owing to their tunable framework structure. However, it is still challenging bulk synthesis for real-world applications of these materials. Herein, we present mechanochemical gram-scale synthesis of series of mixed ligand metal organic frameworks (MOFs) and metal hydrogen‐bonded organic frameworks (MHOFs) using phenylene diphosphonic acid and 1-hydroxyethylidene-1,1-diphosphonic acid with different bipyridyl type of ligands, respectively. In all cases, the existence of extensive hydrogen bonds with amphiprotic uncoordinated phosphonate hydroxyl and oxygen atoms, the frameworks exhibited high proton conductivity. The study demonstrates the potential of green mechanosynthesis for preparations of framework-based proton conducting materials in bulk scale for green energy generation. T2 - 4th International Conference on Phosphonate Chemistry, Science and Technology, ICOPHOS-4 CY - Crete, Greece DA - 02.10.2023 KW - Proton exchange membrane fuel cells KW - Metal organic frameworks KW - Proton conducting materials PY - 2023 AN - OPUS4-58837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon T1 - Between Homogenous and Heterogenous Catalysis: Single-Atom-Catalysts N2 - Catalysis is a very important process in chemistry as it lowers the energy barrier for chemical reactions. This saves energy and/or some reactions are only possible with a catalyst under the desired conditions (temperature and pressure). Catalysts can be roughly categorized depending on the phase they interact with the substrates in homogenous and heterogenous catalysis. T2 - 5. Deutsche Tagung für Forschung mit Synchrotronstrahlung, Neutronen und Ionenstrahlen an Großgeräten (SNI2022) CY - Berlin, Germany DA - 05.09.2022 KW - Single-atom-catalyst KW - Electrochemistry KW - Porous carbons PY - 2022 AN - OPUS4-61989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon T1 - Between Homogenous and Heterogenous Catalysis: Single-Atom-Catalysts N2 - Catalysis is a very important process in chemistry as it lowers the energy barrier for chemical reactions. This saves energy and/or some reactions are only possible with a catalyst under the desired conditions (temperature and pressure). Catalysts can be roughly categorized depending on the phase they interact with the substrates in heterougenous and heterogenous catalyst T2 - RÅC international summer school CY - Varberg, Sweden DA - 14.08.2022 KW - Single-atom-catalyst KW - Electrochemistry KW - Porous carbons PY - 2022 AN - OPUS4-61983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon T1 - XAS for structural characterization of atomically dispersed materials N2 - metal and nitrogen enriched carbons (M-N-C) are promising electrocatalysts for small molecule activation. It is proposed that the nitrogen is forming a stabilizing N4-site for the catalytically active metal. This can be proven by XAS measurements to confirm the coordination sphere around the metal. T2 - Bessy User Meeting CY - Online meeting DA - 08.12.2024 KW - Single-atom-catalyst KW - Structural characterization KW - Porous carbons PY - 2022 AN - OPUS4-61994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Shu-Han T1 - MOF-derived Synthetic Carbon Anode Materials for Sodium-Ion Batteries N2 - Metal-organic frameworks (MOFs), particularly the zeolitic imidazolate framework (ZIF) family, are attractive precursors for advanced energy-storage materials. Upon pyrolysis, ZIFs can be transformed into electrically conductive carbon materials while preserving their original particle morphology, which is crucial for achieving high-performance sodium-ion battery anodes. Despite these advantages, large-scale implementation remains challenging due to the need for synthesis routes that balance performance, cost, and sustainability. The present study addresses these challenges by developing environmentally benign and economically feasible strategies for the scalable production of ZIF-8-derived carbon anodes suitable for industrial applications. T2 - Batterieforum Deutschland 2026 CY - Berlin, Germany DA - 20.01.2026 KW - Sodium-ion battery KW - Negative electrode KW - Metalorganic frameworks PY - 2026 AN - OPUS4-65644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roy, Arkendu T1 - Hydroxide Based High Entropy MOF for Oxygen Evolution Reaction N2 - The energy crisis becomes more prominent in higher altitude countries like Germany, with higher annual energy demand. Thus, the generation of higher energy density fuel like hydrogen from renewable resources become the only way to solve the zero-emission energy system while avoiding the expensive batteries as an energy storage option. Therefore, water electrolysis cells to produce hydrogen and oxygen by storing of solar/wind energy in chemical bonds is a fruitful alternative for renewable and long-term energy generation. Thus, designing inexpensive water-splitting electrocatalyst material becomes a field of research of utmost importance. High entropy metal hydroxide organic frameworks (HE-MHOFs) are composed of high entropy hydroxide layer inside MOFs, resulting in a high degree of structural complexity and diversity than conventional MOFs. The concept of ‘high entropy’ refers to multiple types of metal ions (Metal = TM) in a near equimolar ratio in the same framework, creating a high degree of disorder and many possible structural configurations. Here, the HE-MHOF successfully synthesized by a conventional solvothermal process, crystallizes in the single phase with significant lattice distortion. A special-quasi-random (SQS) structure was simulated with equimolar compositions (~20% TM = Mn, Co, Ni, Cu and Zn) and a comparison was made with the ICP-AES (inductively coupled plasma atomic emission spectroscopy), XANES (X-ray absorption near edge structure) and XAFS (X-ray absorption fine structure) observations. Further, the elemental mapping (Energy dispersive Spectroscopy) of HE-MHOF shows the presence of all five different metals in the same crystallite to substantiate the ‘high entropy’ state of the MOF. The HE-MHOF offers improved thermal stability than mono-metallic MHOF and exhibit unique properties compared to traditional monometallic (Ni2+) MOF variants. Firstly, to elucidate the effect of the multimetallic system on the catalytic performance, we have performed density functional theory (DFT) calculations to investigate pre-redox cycles involved in the catalytic activation of HE (and Ni)-MOFs. HE-MHOF is further investigated as an electrocatalyst for oxygen evolution reaction (OER) due to its special high entropy hydroxide layered structure and electronic properties. Our DFT results have examined the traditional proton-coupled electron transfer (PCET) steps involving the single transition-metal site. The scrutiny of d-band centers and their behaviour in catalytic upgradation is investigated with density of states (DOS) analysis. It exhibits outstanding performance towards oxygen evolution reaction (OER) comparable to the experimental findings, which is also comparable to state-of-the-art OER catalysts based on precious metals such as iridium oxide and platinum carbon. We have considered different electrolyte solutions to elucidate the fast kinetics oxygen evolution reaction in the presence of various external nucleophilic anions. In hydroxyl-based MOFs, electrolytes' influence can substantially enhance catalytic activities. Here, with the help of DFT simulations, we have investigated the effect of the nucleophilicity of anion on each elementary reaction involved in the PCET mechanism of OER. T2 - EuroMOF 2023 CY - Granada, Spain DA - 24.09.2023 KW - Metal-organic Framework KW - High Entropy Materials KW - Electrocatalysis PY - 2023 AN - OPUS4-58971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon A1 - Mehmood, Asad A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Fellinger, Tim-Patrick A1 - Thomas, A. T1 - Characterization of Solid-State Complexes by XAS N2 - Atomically dispersed metal-nitrogen doped carbons (M-N-C) are promising catalysts for the activation of small molecules such as O2 and CO2. These single atom catalysts (SAC) operate at the interface between homogenous and heterogenous catalysts. Currently, many examples of M-N-C are known with good oxygen reduction reaction activity but lacking a controlled synthesis of the specific active sites of the precatalyst. Recently, our group facilitated the synthesis of pure pyrrolic M-N4 sites using Zn ions as imprinters.[1] These amorphous materials obtained by active site imprinting method are characterized at the BAMline (Bessy II) by X-ray absorption spectroscopy (XAS). In-situ/operando measurements will be crucial in future work for a better understanding of the dynamic changes of the active site. T2 - InSynX Workshop 2023 CY - Sao Paulo, Brazil DA - 06.03.2023 KW - Solid-State Complexes PY - 2023 AN - OPUS4-58933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gugin, Nikita T1 - Large-Scale Synthesis of ZIF-8 for Hydrogen Storage: Batch and Continuous Modes N2 - We report the scale-up of a batch solid synthesis of zeolitic imidazolate framework-8 (ZIF-8) for reactive extrusion. The crystalline product forms in the extruder directly under the mixture of solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic amount of liquid. Highly crystalline ZIF-8 with a Brunauer−Emmett−Teller (BET) surface area of 1816 m2 g−1 was quantitatively prepared at mild temperature using a catalytic amount of ethanol and a small excess of the linker. Extruded ZIF-8 is an affordable alternative to commercial Basolite Z1200 as a reference material for H2 cryoadsorption. T2 - Metrology for Advanced Hydrogen Storage Solutions (MefHySto) Closing Conference CY - Berlin, Germany DA - 03.07.2023 KW - In situ Raman KW - Large-scale processing KW - Mechanochemistry KW - Twin-screw extrusion (TSE) PY - 2023 AN - OPUS4-58926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moss, Caitlin T1 - Framework Materials for the Electrocatalytic Reduction of Nitrate to Ammonia N2 - The electrocatalytic reduction of nitrate to ammonia offers a sustainable alternative to the energy-intensive Haber-Bosch process while simultaneously addressing the pressing issue of nitrate pollution in water sources. Developing efficient catalysts for this reaction is therefore vital for both environmental remediation and green ammonia production. Framework materials such as metal-organic frameworks (MOFs), covalent organic frameworks (COFs), and coordination polymers present an emerging class of electrocatalytic materials due to their high surface area, tunable porosity, and structural modularity. Their ability to incorporate diverse metal centers and functional groups makes them promising candidates for selective and efficient nitrate reduction. In order to change and improve catalytic properties, different synthesis strategies can be pursued, such as metal alloying or calcination under different conditions. To fully understand and optimize these materials, advanced characterization techniques are essential to correlate structural features with catalytic performance, alongside in-situ methods for real-time mechanistic insights. T2 - Tag der Chemie 2025 CY - Berlin, Germany DA - 03.07.2025 KW - Electrocatalysis KW - Electrochemisty KW - Framework Materials KW - Ammonia Synthesis KW - Nitrate Reduction PY - 2025 AN - OPUS4-63815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmalz, Alina T1 - Framework Materials for the Electrocatalytic Reduction of Nitrate to Ammonia N2 - The electrocatalytic reduction of nitrate to ammonia offers a sustainable alternative to the energy-intensive Haber-Bosch process while simultaneously addressing the pressing issue of nitrate pollution in water sources. Developing efficient catalysts for this reaction is therefore vital for both environmental remediation and green ammonia production. Framework materials such as metal-organic frameworks (MOFs) or metalated covalent organic frameworks (COFs) present an emerging class of electrocatalytic materials due to their high surface area, tunable porosity, and structural modularity. Their ability to incorporate diverse metal centers and functional groups makes them promising candidates for selective and efficient nitrate reduction. In order to change and improve catalytic properties, different synthesis strategies can be pursued, such as metal alloying, doping or calcination. To fully understand and optimize these materials, advanced characterization techniques are essential to correlate structural features with catalytic performance, alongside in-situ methods for real-time mechanistic insights. T2 - 10th European Crystallography School CY - Ohrid, North Macedonia DA - 23.06.2025 KW - Electrocatalysis KW - Electrochemistry KW - Framework Materials KW - Ammonia Synthesis KW - Nitrate Reduction PY - 2025 AN - OPUS4-63846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hartwig, Peter T1 - Sichere Wasserstoffnetze ModuH2Pipe N2 - Modulare Testplattform für den sicheren Transport von Wasserstoff in neuen und vorhandenen Gasverteilnetzen Die BAM schafft mit der modularen Testplattform ModuH2Pipe erstmals in Europa eine Testinfrastruktur, welche die Betrachtung sicherheitstechnischer Fragestellungen im Realmaßstab und zugleich unter kritischen Bedingungen erlaubt, die sich im Zusammenhang mit Wasserstoff-und Wasserstoff-Erdgas-Pipelines stellen. Ziel ist, Gasnetzbetreibern u. a. ein Dienstleistungsangebot zur Verfügung zu stellen, welches die umfassende Beantwortung dieser und weiterer sicherheitstechnischer Fragestellungen ermöglicht. Die Testplattform ModuH2Pipe wird auf dem BAM Testgelände Technische Sicherheit (BAM TTS) stehen und integriert zwei Module, die für die experimentelle Untersuchung von Pipelinesegmenten, -komponenten (Dichtungen, Ventile etc.) und Polymerkomponenten im Originalmaßstab ausgelegt sind. Aber auch digitale Aspekte für Wasserstoffnetze können betrachtet werden. T2 - 1. Fachtagung für Anlagen- und Prozesstechnik CY - Berlin, Germany DA - 24.03.2026 KW - Wasserstoff KW - ModuH2Pipe KW - Testplattform KW - Realmaßstab KW - Wasserstoffkernnetz PY - 2026 AN - OPUS4-65765 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -