TY - CONF A1 - Mayer, Uwe T1 - Untersuchung des Master Curve-Konzeptes für ferritisches Gusseisen mit Kugelgraphit N2 - In dem Vortrag werden der Forschungsansatz, die Ziele, das Untersuchungsprogramm und die erwarteten Ergebnisse des BMUVForschungsvorhabens 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 - Master Curve KW - Gusseisen mit Kugelgraphit KW - Sprödbruch PY - 2023 AN - OPUS4-59061 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzwarth, M. T1 - First results for the modification of the master curve concept for ferritic ductile cast iron N2 - Within the scope of fracture mechanics safety, ferritic ductile cast iron (DCI) does currently not have an established and validated method to determine and assess dynamic fracture toughness values in the ductile-to-brittle transition regime. For this reason, the applicability of the fracture mechanics Master Curve concept according to ASTM E1921 to DCI is being investigated in a joint research project between MPA Stuttgart and BAM Berlin. To investigate the applicability of the Master Curve concept for DCI, a DCI material of grade GJS-400 has been procured via a detailed manufacturing specification. From this material test specimens of various geometries and sizes (Tensile, Charpy-V, Pellini, SE(B)10, SE(B)25, SE(B)140, DC(T)9, C(T)25 and C(T)50) were produced. In total, about 500 test specimens will be tested to investigate and validate the Master Curve Concept as well as other assumptions (e.g. size effects, Weakest-Link, Weibull distribution) for DCI. While the whole project has not yet concluded, several work packages have yet been completed. Selected test results using C(T)25 specimens are presented. T2 - European Conference on Fracture 2024 CY - Zagreb, Croatia DA - 26.08.2024 KW - Dynamic fracture toughness KW - Ductile cast iron KW - Master curve PY - 2024 AN - OPUS4-61451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baer, Wolfram A1 - Ohm, Katrin A1 - Holzwarth, Marcel A1 - Mayer, Uwe T1 - Master Curve-Auswertungen und fraktographische Analysen zum Bruchmechanismus – neue Ergebnisse zur Untersuchung des Master Curve Konzepts für ferritisches Gusseisen mit Kugelgraphit bei dynamischer Beanspruchung (Projekt MCGUSS) N2 - In diesem Beitrag werden erste Master Curve (MC)-Auswertungen und fraktographische Analysen zum Bruchmechanismus aus dem laufenden Kooperationsprojekt MCGUSS zwischen der BAM Berlin und der MPA Stuttgart diskutiert. Für zwei SE(B)140-Großprobenversuchsserien mit je 6-8 Versuchen bei -40 °C bzw. -60 °C und Belastungsraten von 5-8x10^4 MPa√m/s wurden Referenztemperaturen T0 bestimmt. Ergänzt wird dies für erste Versuchsreihen an SE(B)25-Kleinproben, die bei -60 °C und Belastungsraten von ca. 2x10^5 MPa√m/s geprüft wurden. An ausgewählten Bruchflächen dieser Versuche wurden detaillierte fraktographische REM-Analysen vorgenommen. Im Vordergrund stand die Charakterisierung des Bruchmechanismus in Abhängigkeit von den Einflussfaktoren Temperatur und Probengröße. In Richtung der Zähigkeitstieflage werden die Analysen komplettiert durch die Ergebnisse von zwei SE(B)140-Großprobenversuchen bei -100 °C bzw. -140 °C und Belastungsraten von ca. 5-8x10^4 MPa√m/s. T2 - 57. Tagung des DVM-Arbeitskreises Bruchmechanik und Bauteilsicherheit CY - Köln, Germany DA - 18.02.2025 KW - Dynamische Beanspruchung KW - Bruchmechanik KW - Master Curve-Konzept KW - Gusseisen mit Kugelgraphit PY - 2025 DO - https://doi.org/10.48447/BR-2025-467 SP - 113 EP - 122 PB - DVM-Verlag CY - Berlin AN - OPUS4-62554 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzwarth, Marcel A1 - Baer, Wolfram A1 - Mayer, Uwe A1 - Weihe, Stephan T1 - Investigation of the Master Curve Concept for Ferritic Ductile Cast iron N2 - Within fracture mechanics safety assessment for steels in nuclear technology, the probabilistic master curve (MC) concept according to ASTM E1921 is currently used for quasi-static loading conditions as a supplement to the established deterministic ASME reference curve concept. However, for ductile cast iron (DCI), a systematic review of potential modifications to the assumptions and the procedure according to ASTM E1921 and an associated validation are still lacking. For this reason, the application of the fracture mechanics MC concept to ferritic ductile cast iron is being investigated in a recently started joint research project between MPA Stuttgart and BAM Berlin. According to the IAEA guidelines SSG 26, the safety assessment of DCI containers for transport as well as storage of radioactive materials is based on the fracture mechanics criterion of general crack initiation exclusion. Within this context, the focus of the current research project is on the further development of brittle fracture safety assessment methods. Therefore, a methodology shall be established to determine and assess dynamic fracture toughness values of DCI in the ductile-to-brittle transition regime, using samples extracted from a component. For the experimental program, a DCI material will be produced as it is generally used for transport and storage containers. A basic mechanical-technological material characterization consisting of tensile, Charpy and Pellini tests is planned and a comprehensive fracture mechanics test program was compiled covering dynamic testing of DC(T)9, C(T)25, C(T)50, SE(B)10, SE(B)25, and SE(B)140 specimens. Numerical analyses of different specimen geometries and test setups are planned to investigate the influences of stress triaxiality and loading rate. Throughout the experimental program, the microstructure-property relationship will be investigated based on quantitative metallographic and fractographic analyses. Finally, different MC assessment strategies will be considered and modifications will be made if necessary. T2 - 21st International Symposium ASTM/ESIS Symposium on Fatigue and Fracture Mechanics CY - Washington, D.C., USA DA - 08.11.2023 KW - Dynamic Fracture Toughness KW - Cleavage fracture KW - Master Curve Concept KW - Ductile Cast Iron PY - 2023 AN - OPUS4-59063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzwarth, Marcel T1 - Investigation of the Master Curve Concept for Ferritic Ductile Cast Iron N2 - Within fracture mechanics safety assessment for steels in nuclear technology, the probabilistic master curve (MC) concept according to ASTM E1921 is currently used for quasi-static loading conditions as a supplement to the established deterministic ASME reference curve concept. However, for ferritic ductile cast iron (DCI), a systematic review of potential modifications to the assumptions and the procedure according to ASTM E1921 and an associated validation are still lacking. For this reason, the application of the fracture mechanics MC concept to ferritic ductile cast iron is being investigated in a joint research project between MPA Stuttgart and BAM Berlin. According to IAEA SSG-26, the safety assessment of DCI containers for transport as well as storage of radioactive materials is based on the fracture mechanics criterion of general crack initiation exclusion. Within this context, the focus of the research project is on brittle fracture. The goal is the establishment of a methodology to determine and assess dynamic fracture toughness values of DCI in the ductile-to-brittle transition regime, using samples extracted from a component. The experimental program uses a DCI material of grade GJS-400, which is generally used for transport and storage containers of radioactive materials. Firstly, a basic mechanical-technological material characterization will be performed consisting of tensile, Charpy and Pellini tests. Following the material characterization, the loading rate relevant for brittle fracture will be determined using instrumented C(T)25-fracture tests at a temperature of -40°C. To be able to transfer the relevant loading rate to other specimen geometries or sizes, the time-dependent course of the Weibull stress is assessed via numerical analyses. With this information an extensive experimental program consisting of DC(T)9, C(T)25, C(T)50, SE(B)10, SE(B)25 and SE(B)140 specimens is performed. These experimental results will be further supported by numerical and fractographic analyses. The empirical experimental database developed for DCI materials will be used to assess the applicability of the MC concept for DCI materials under dynamic loading. At the current time manufacturing and precracking of test specimens is ongoing. The authors provide first results concerning the mechanical-technological material characterization, the relevant loading rate for brittle fracture determined via C(T)25 tests, and some early results of other specimen types. These experimental results are also supported by preliminary numerical and statistical analyses. T2 - Conference SMiRT27 CY - Yokohama, Japan DA - 04.03.2024 KW - Dynamic fracture toughness KW - Ductile cast iron KW - ASTM E1921 KW - Master curve KW - Brittle fracture PY - 2024 AN - OPUS4-59859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzwarth, Marcel A1 - Mayer, Uwe A1 - Baer, Wolfram A1 - Weihe, Stefan T1 - Investigation of the Master Curve Concept for Ferritic Ductile Cast Iron N2 - Within fracture mechanics safety assessment for steels in nuclear technology, the probabilistic master curve (MC) concept according to ASTM E1921 is currently used for quasi-static loading conditions as a supplement to the established deterministic ASME reference curve concept. However, for ductile cast iron (DCI), a systematic review of potential modifications to the assumptions and the procedure according to ASTM E1921 and an associated validation are still lacking. For this reason, the application of the fracture mechanics MC concept to ferritic ductile cast iron is being investigated in a joint research project between MPA Stuttgart and BAM Berlin. According to Hojo et al. (2008) the MC concept is already in use for the brittle fracture safety assessment of ferritic forged steel containers, which would suggest an extension to ductile cast iron containers. In compliance with IAEA SSG-26, the safety assessment of DCI containers for transport as well as storage of radioactive materials is based on the fracture mechanics criterion of general exclusion of crack initiation. Within this context, the focus of the current research project is on the further development of brittle fracture safety assessment methods. Therefore, a methodology shall be established to determine and assess dynamic fracture toughness values of DCI in the ductile-to-brittle transition regime, using only a low number of small fracture mechanics test specimens extracted from a component. For the experimental program, a DCI material of grade GJS-400 (GGG-40) has been produced as it is generally used for transport and storage containers for nuclear material. A basic mechanical-technological material characterization consisting of tensile, Charpy, and Pellini tests has been planned and a comprehensive fracture mechanics test program was compiled covering dynamic testing of DC(T)9, C(T)25, C(T)50, SE(B)10, SE(B)25, and SE(B)140 specimens at various loading rates and temperatures. The specimen testing is divided between the project partners based on specimen geometry. MPA Stuttgart has been tasked with the testing of the C(T), DC(T) and Pellini specimens, while BAM Berlin was assigned the SE(B), Charpy and tensile tests. These tests allow for the determination of the loading rate relevant for brittle fracture via C(T)25 specimens and an assessment of size effects by transferring the relevant loading rate to other specimen geometries and sizes. Numerical analyses of different specimen geometries and test setups are planned to investigate the influence of stress triaxiality and loading rate. Furthermore, the time-dependent course of the Weibull stress is assessed via these numerical analyses. Throughout the experimental program, the microstructure-property relationship will also be investigated based on quantitative metallographic and fractographic analyses like scanning electron microscope images and metallographic sections. With the acquired experimental database fundamental assumptions of the MC concept, like the weakest link model and the Weibull distribution, will be assessed for the application to DCI. In the end, the applicability of the MC concept will be evaluated and if necessary, modifications to the MC concept for DCI will be proposed. This paper will present the preliminary results of the GJS400 material characterization and the related selection of test specimen extraction points. First results of the C(T)25 and SE(B)140 specimen testing will also be discussed supported by first metallographic analyses. T2 - SMiRT27 Conference CY - Yokohama, Japan DA - 03.03.2024 KW - Ductile Cast iron KW - Dynamic Fracture Toughness KW - Safety Assessment KW - Master Curve Concept PY - 2024 SP - 1 EP - 10 AN - OPUS4-59302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzwarth, Marcel A1 - Baer, Wolfram A1 - Mayer, Uwe A1 - Weihe, Stefan T1 - On the Applicability of the Master Curve Concept for Ductile Cast Iron based on experimental and microstructural results N2 - Based on the state-of-the-art research and regulations, the application of the fracture mechanics master curve (MC) concept to ferritic ductile cast iron (DCI) is being investigated in a joint research project (MCGUSS) between BAM Berlin and MPA Stuttgart. The experimental program included a basic mechanical-technological material characterization consisting of tensile, Charpy and Pellini tests. To determine the relevant loading rate for brittle fracture, instrumented C(T)25 fracture tests were performed at different loading rates at a temperature of -40°C. The relevant loading rates are 5x10^3 MPa√ms-1 and 5x10^4 MPa√ms-1. A series of dynamic fracture tests consisting of DC(T)9, C(T)25 and C(T)50 specimens were performed at MPA. BAM performed corresponding test series with SE(B)10 (pre-cracked Charpy), SE(B)25 and SE(B)140 specimens to cover the influence of specimen geometry. In total about 400 tests were performed during this project. The experimental program is complemented by extensive fractographic and metallographic studies using scanning electron microscopy and cross sectioning, as well as characterizations of the chemical composition of the material and of the morphology and distribution of the graphite particles. KJcd values were evaluated for all C(T)25 specimens and some C(T)50 and DC(T)9 specimens. First Master Curve analyses suggest that modifications on the Master Curve setup will be neccessary for instance changing the coefficient from 0.019 to 0.045. This modification requires further validation and is only one of many possible modifications. The SE(B) specimen results clearly show an inverse size effect. This does not correlate with the weakest link effect attributed to steels which dictates lower fracture toughness values for larger specimens. Due to the presence of graphite particles in the DCI material, it is currently assumed that these particles play a significant role in the failure behavior of DCI materials and the following fracture mechanism is proposed: “Specimen size-dependent arrest of local brittle fracures before global brittle failure by weakest link”. T2 - 9th SEDS Workshop: Safety of Extended Dry Storage, 20.-22. Mai 2025 CY - Garching, Germany DA - 20.05.2025 KW - Statistics KW - Dynamic fracture toughness KW - Ductile cast iron KW - Master curve KW - Safety assessment PY - 2025 SP - 1 EP - 3 AN - OPUS4-63566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Castells-Gil, Javier A1 - Zhu, Jinjie A1 - Itskou, Ioanna A1 - Wolpert, Emma H. A1 - Hunter, Robert D. A1 - Tidey, Jeremiah P. A1 - Pedersen, Angus A1 - Solvay, Elisa A1 - Tyrrell, Helen A1 - Petit, Camille A1 - Barrio, Jesús T1 - Impact of N-heterocyclic amine modulators on the structure and thermal conversion of a zeolitic imidazole framework N2 - The zeolitic imidazole framework-8 (ZIF-8) is a crystalline porous material that has been widely employed as template to fabricate porous nitrogen-doped carbons with high microporosity via thermal treatment at high temperatures. The properties of the carbon scaffold are influenced by the pore structure and chemical composition of the parent ZIF. However, the narrow pore size distribution and microporous nature from ZIF-8 often results in low mesopore volume, which is crucial for applications such as energy storage and conversion. Here we show that insertion of N-heterocyclic amines can disrupt the structure of ZIF-8 and dramatically impact the chemical composition and pore structure of the nitrogen-doped carbon frameworks obtained after high-temperature pyrolysis. Melamine and 2,4,6-triaminopyrimidine were chosen to modify the ZIF-8 structure owing to their capability to both coordinate metal ions and establish supramolecular interactions. Employing a wide variety of physical characterization techniques we observed that melamine results in the formation of a mixed-phase material comprising ZIF-8, Zn(Ac)6(Mel)2 and crystallized melamine, while 2,4,6-triaminopyrimidine induces the formation of defects, altering the pore structure. Furthermore, the absence of heterocyclic amine in the ZIF-8 synthesis leads to a new crystalline phase, unreported to date. The thermal conversion of the modified ZIFs at 1000 °C leads to nitrogen-doped carbons bearing Zn moieties with increased surface area, mesopore volume and varying degree of defects compared to ZIF-8 derived carbon. This work therefore highlights both the versatility of heterocyclic amines to modify the structure of framework materials as well as their role in tuning pore structure in nitrogen-doped carbons, paving the way to targeted design of high-performance electrodes for energy storage and conversion. KW - Zeolitic imidazole framework KW - Heterocyclic amine KW - Triaminopyrimidine PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639177 DO - https://doi.org/10.1039/D5TA04831A SN - 2050-7488 SP - 1 EP - 13 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braga, Daniel S. A1 - Pedersen, Angus A1 - Riyaz, Mohd A1 - Barrio, Jesús A1 - Bagger, Alexander A1 - Neckel, Itamar T. A1 - Mariano, Thiago M. A1 - Winkler, Manuel E. G. A1 - Stephens, Ifan E. L. A1 - Titirici, Maria‐Magdalena A1 - Nagao, Raphael T1 - In situ structural evolution and activity descriptor of atomically dispersed catalysts during nitrate electroreduction N2 - Single‐Atom Catalysts (SAC) have emerged as a promising class of materials for various catalytic applications, including the electrochemical nitrate reduction reaction (eNO3RR) and consequently ammonia production. While the efficiency and selectivity of these materials have been extensively highlighted for the eNO3RR, the in situ evolution to their structure and composition during electrocatalysis is largely unexplored and lacks catalyst design principles. To solve this, we investigated a series of high utilization metal‐nitrogen‐carbon (MNC) SACs (M = Cr, Fe, Co, Ni, and Cu) for eNO3RR. Except for CuNC, which selectively produced nitrite, all catalysts exhibited Faradaic efficiencies (FE) for ammonia exceeding 50%. NiNC demonstrated the highest performance (FE of 78.0 ± 2.9% at −0.4 V versus reversible hydrogen electrode (RHE) at pH 13 and maximum ammonia production rate of 615.7 ± 176.5 µmol·h−1·, corresponding to an energy efficiency of 15.1 ± 1.4% at −0.6 VRHE), followed by CoNC. In situ Synchrotron X‐ray fluorescence (SXRF) mapping at various cathodic potentials (from open circuit potential to 0.0 VRHE and then −0.6 VRHE at 100 mV steps) revealed significant mobility of Ni within the carbon matrix, leading to the formation of metallic clusters from 0.0 VRHE. Similar in situ metal clustering is observed for CoNC. Structure‐activity plots are generated from both MNC literature and results obtained here, finding a clear trend between OH binding energy and turnover frequency, with the high activity of NiNC and CoNC in this work explained by their stronger OH binding in the metallic structure compared to their SAC coordination. This work therefore, reveals the structure‐activity‐stability of MNCs for eNO3RR and provides a simple descriptor for identifying highly active eNO3RR catalysts and their in situ structural evolution. KW - Single atom KW - Nitrate reduction KW - Structure-activity-selectivity KW - In situ PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640353 DO - https://doi.org/10.1002/advs.202510282 SN - 2198-3844 VL - 12 IS - 39 SP - 1 EP - 14 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64035 LA - eng 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 - JOUR A1 - Morcillo, Dalia A1 - Winckelmann, Alexander A1 - Oelze, Marcus A1 - Leonhardt, Robert A1 - Schmidt, Anita A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - Exploring Age-Induced Lithium Isotope Fractionation in Lithium-Ion Batteries using Microwave-Induced Cold Nitrogen Plasma Mass Spectrometry N2 - This study explores Microwave-Inductively Coupled Atmospheric-pressure Plasma Mass Spectrometry (MICAP-MS) 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 (LIBs). We investigate the performance of MICAP-MS in measuring Li isotope ratios in new and aged commercial lithium cobalt oxide (LCO) batteries. Our results show that MICAP-MS, operating under cold plasma conditions at 800 W with an 8 mm torch position, achieves results metrologically compatible with MC-ICP-MS, with a precision ranging from 0.6‰ to 3.4‰ for δ7Li values. MICAP-MS benefits from a dielectric resonator for uniform plasma, better ion velocity control, and higher energy efficiency. Optimal settings were identified with dwell times of 10 ms for 6Li and 1 ms for 7Li. The study of LIBs revealed that 6Li migrates towards the anode over multiple charge–discharge cycles, causing 7Li to accumulate in the cathode, a fractionation effect that becomes more pronounced with prolonged cycling. MICAP-MS provides a cost-effective, precise alternative to MC-ICP-MS, with lower operational costs and enhanced portability, advancing the study of isotopic fractionation and aging in lithium-ion batteries. KW - MICAP-MS KW - Lithium KW - Battery aging KW - Lithium isotopes KW - Nitrogen plasma KW - Isotope fractionation KW - lithium cobalt oxide KW - LCO PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643777 DO - https://doi.org/10.1039/d4ja00324a SN - 0267-9477 SP - 1 EP - 11 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Data-Driven Spectrochemical Sensing for Elemental and Isotopic Analysis—from Energy Systems to Biomedicine N2 - High-resolution optical spectrometers generate spectra containing tens of thousands of data points per sample. Picometre-scale isotope shifts, matrix-induced line broadening, and strong inter-feature correlations render classical peak fitting unreliable. Current analytical challenges, therefore, require rigorous algorithms able to expose latent structure, quantify uncertainty, and remain chemically interpretable. The research program presented in this lecture integrates state-of-the-art spectrochemical instrumentation with mathematically disciplined data models. Principal Component Analysis and Partial Least Squares provide chemically meaningful latent variables, while gradient-boosted decision trees or deep neural networks (ANNDL) capture residual non-linearity without sacrificing traceability. All models are trained on isotope-enriched or synthetically generated spectra and distributed with full validation workflows. Two research areas illustrate this strategy: (1) Isotopic analytics for materials, environment, and medicine. (2) Data-fusion diagnostics for battery ageing and failure. T2 - Temple University: Mechanical Engineering Transformative Science and Technology Engineering Lecture Series CY - Philadelphia, PA, USA DA - 02.10.2025 KW - Isotope KW - Data analysis KW - Machine learning KW - Elemental analysis KW - Battery PY - 2025 AN - OPUS4-64877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Tracking Lithium-Ion Battery Ageing via Lithium Isotope Fractionation N2 - Lithium-ion batteries power portable devices, electric vehicles, and stationary power grids, yet hidden aging reactions still shorten their service life and raise concerns about cost and safety. An analytical proxy is needed to report these reactions and accelerate product development, quality control, and recycling. Here, we demonstrate that subtle shifts in the natural 7Li/6Li ratio accurately record the two decisive stages of cell aging, solid-electrolyte interphase (SEI) formation and field-driven aging, which can be detected using multi-collector ICP-MS. Because Li is easily stripped from digested electrodes or electrolyte in a one-step cation-exchange column, high-purity solutions reach the spectrometer in minutes. A streamlined MC-ICP-MS run yields a δ7LiLSVEC precision of 0.4 ‰, enabling dozens of battery fractions to be analyzed per day. Applying the workflow to LiCoO2 coin cells as models, sampled from pristine to 700 cycles, reveals a clear isotopic narrative. During the first ≈45 cycles, 7Li leaves the LiCoO2 lattice, dissolves into the electrolyte, and is locked in the SEI on graphite, driving cathode δ7Li from +8 to –10 ‰ and raising the anode to +13 ‰ while capacity drops by 10 %. After the interphase matures, the electric field takes over: the lighter 6Li migrates faster to the anode, 7Li accumulates in the contracting Li1-xCoO2 lattice, and the bulk separation factor rises to α≈1.045 by 700 cycles. The δ7Li curve flattens roughly 70 cycles before capacity falls to 80%, providing an early warning of end-of-life. Isotopic gradients scale linearly with impedance growth, SEI thickness, and crack density confirmed by LA-ICP-MS mapping, FIB-SEM, XANES, and EXAFS. Although each data point requires one cell, lithium-isotope fractionation provides direct, element-specific, and structural fatigue insight unavailable from non-destructive tests. The straightforward chemistry and fast MC-ICP-MS routine make the approach practical for targeted aging studies, additive screening, and forensic autopsies, complementing high-throughput electrochemical methods and supporting the design of longer-lived batteries. T2 - SciX 2025 CY - Covington, KY, USA DA - 05.10.2025 KW - Isotope KW - Lithium KW - MC-ICP-MS KW - MICAP-MS KW - Isotope fractionation KW - Battery PY - 2025 AN - OPUS4-64879 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 - Askar, Enis T1 - Challenges for hydrogen technologies - Activities of H2Safety@BAM N2 - In this presentation the drivers for the rise of hydrogen technologies are outlined and main challenges for the market ramp-up are shown. Finally, the activities and capabilities of the competence center H2Safety@BAM are characterized and some of the current projects at BAM adressing the main challenges for hydrogen technologies are presented focussing on the hydrogen transport and infrastructure. T2 - Wasserstoff-Dialog - Stakeholder-Konferenz des Wasserstoff-Kompass CY - Berlin, Germany DA - 10.10.2022 KW - Hydrogen strategy KW - ModuH2Pipe KW - Hydrogen transport KW - Hydrogen infrastructure KW - Liquid hydrogen (LH2) PY - 2022 AN - OPUS4-57065 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 - Sobol, Oded T1 - Hydrogen assisted cracking phenomena in duplex stainless steels elucidated by in- and ex-situ ToF-SIMS experiments N2 - In the presented research, the high potential and abilities of secondary ion mass spectrometry (ToF-SIMS) to detect and locally map the hydrogen distribution in two types of duplex stainless steels are shown. The research validates certain proposed mechanisms by combining ToF-SIMS with high-resolution scanning electron microscopy and electron-backscattered diffraction. The combination of data from several techniques on the same region was conducted in this field for the first time by applying data treatment of the ToF-SIMS raw data and data fusion approach. This powerful combination of methods allows reviewing of the occurring processes related to hydrogen assisted cracking. The step beyond the state of the art in this field was gained here by developing permeation and mechanical loading experiments within the ToF-SIMS during chemometric imaging of the hydrogen distribution in the microstructure. The research presents the necessary correlation between the hydrogen distribution and the resulted structural changes, the diffusion behavior in a duplex microstructure and stress induced diffusion of hydrogen by applying external load at the microscale. T2 - 6th WMRIF Early Career Scientist Summit CY - NPL Teddington UK DA - 18.06.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - LDX KW - EBSD KW - Data-fusion PY - 2018 AN - OPUS4-46865 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 - Nietzke, Jonathan T1 - Evolution of tensile testing methodologies for hydrogen embrittlement in austenitic steels: a comparative study N2 - The energy transition towards hydrogen utilisation has increased the demand for reliable testing methods to evaluate the susceptibility of metallic materials to hydrogen degradation. However, traditional electrochemical pre-charging techniques have limitations in represent-ing realistic gaseous hydrogen exposure conditions. This study presents three comparative analyses of tensile testing methodologies, focusing on the differences between electrochem-ical pre-charging, gaseous pre-charging, and in-situ testing using hollow specimens for aus-tenitic steels AISI 304L and 316L type austenitic steels. Based on the results obtained, the first comparison reveals that electrochemically pre-charged and gaseously pre-charged specimens exhibit different behaviours regarding the impact on the mechanical properties. This effect can be retraced to the varying distribution of hydrogen throughout the specimens. Although comparable embrittlement was observed for similar hydrogen concentrations, the relationship appears to be non-systematic. The second comparison evaluates the performance of pre-charged hollow specimens (300°C, 100 bar, 21 days) in comparison to hollow specimens tested in-situ under 200 bar hydrogen during slow strain rate tensile tests (SSRT). While pre-charged specimens show a slight de-crease in elongation at fracture and a noticeable decrease in reduction of area (RA), in-situ tested specimens exhibit significantly more pronounced embrittlement. This is in accord-ance with the results of Michler et. al. In the third comparison, geometry effects between pre-charged conventional and pre-charged hollow specimens are explored. In this case, the hydrogen effect appears to be of the same order of magnitude for both specimen types, although some differences are ob-served. The study's findings underscore the importance of considering differences between test methods when assessing materials’ compatibility with hydrogen. It specifically emphasises the need for in-situ testing with gaseous hydrogen to better represent real conditions in ap-plications within the hydrogen sector. Furthermore, the study provides an initial compari-son between conventional and hollow specimens, demonstrating their capability to reveal hydrogen effects. However, additional research is essential to enhance the comparability of results yielded by these testing methods. T2 - European Conference on Fracture 2024 CY - Zagreb, Croatia DA - 26.08.2024 KW - Hollow Specimen Technique KW - Hydrogen KW - Austenitic Stainless Steel KW - Hydrogen Testing KW - AISI 316L PY - 2024 AN - OPUS4-60929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nietzke, Jonathan T1 - The relationship between surface condition and the influence of hydrogen on the mechanical properties of additively manufactured 316L N2 - The following contribution presents the analyses of additively manufactured (AM) 316L using hollow specimens at 200 bar hydrogen and a strain rate of 1E-5 s-1. The work includes a comparison of three types of hollow specimens: mechanically extracted from fully additively manufactured cylinders, near-net-shape additively manufactured specimens, i.e. as printed, and specimens made of conventional 316L. AM specimens were manufactured via powder bed fusion with laser beam of metals (PBF-LB/M). For the near-net-shape specimens the inner hole remained without any mechanical processing. The inner holes of the cylindric specimens were manufactured by drilling with subsequent honing. The susceptibility to hydrogen embrittlement was found to be strongly dependent on the surface being in contact with hydrogen. While specimens with a clean surface had a relative reduction of area (RRA) of around 78 %, those with an as-printed surface showed a significantly larger RRA of around 90 %. One possible reason for this are oxide layers formed due to small amounts of oxygen during the AM-process. Further research is required to determine if the lower effect on the mechanical properties is permanently for as printed parts or e.g. time dependent. Additionally, further work with variation in the nominal strain rate is required. T2 - IIW 77th Annual Assembly 2024 CY - Rhodes, Greece DA - 07.07.2024 KW - Austenitic steel 316L KW - Additive manufacturing KW - PBF-LB/M KW - Hydrogen degradation KW - Hydrogen embrittlement KW - Hollow specimen technique PY - 2024 AN - OPUS4-60618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -