TY - JOUR A1 - An, Biwen Annie A1 - Deland, Eric A1 - Sobol, Oded A1 - Yao, Jizheng A1 - Skovhus, T. L. A1 - Koerdt, Andrea T1 - The differences in the corrosion product compositions of Methanogen-induced microbiologically influenced corrosion (Mi-MIC) between static and dynamic growth conditions N2 - Currently, corrosion rates (CR) and/or corrosion products (CP) obtained for methanogen-induced microbiologically influenced corrosion (Mi-MIC) on carbon steel are mainly analyzed from static-incubations. By using a multiport-flow-column, much higher CRs (0.72 mm/yr) were observed, indicating static-incubations are not suitable for determining the corrosive potential of Mi-MIC. With the combination of various analytical methods (ToF-SIMS/SEM-EDS/SEM-FIB) and contrary to previously published data, we observed that CPs contained phosphorus, oxygen, magnesium, calcium and iron but lacked carbon-related species (e.g. siderite). Overall, siderite nucleation is disrupted by methanogens, as they convert aqueous bicarbonate into carbon dioxide for methanogenesis resulting in increased localized corrosion. KW - Carbon steel KW - Modelling studies KW - SIMS KW - SEM KW - Reactor conditions KW - Microbiologically influenced corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517632 DO - https://doi.org/10.1016/j.corsci.2020.109179 SN - 0010-938X VL - 180 SP - 9179 PB - Elsevier AN - OPUS4-51763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Campari, Alessandro A1 - Konert, Florian A1 - Razavi, Nima A1 - Sobol, Oded A1 - Alvaro, Antonio T1 - Hydrogen-assisted cracking: A deep learning approach for fractographic analysis N2 - Hydrogen handling equipment suffers from interaction with their operating environment, which degrades the mechanical properties and compromises component integrity. Hydrogen-assisted cracking is responsible for several industrial failures with potentially severe consequences. A thorough failure analysis can determine the failure mechanism, locate its origin, and identify possible root causes to avoid similar events in the future. Postmortem fractographic analysis can classify the fracture mode and determine whether the hydrogen-metal interaction contributed to the component’s breakdown. Experts in fracture classification identify characteristic marks and textural features by visual inspection to determine the failure mechanism. Although widely adopted, this process is time-consuming and influenced by subjective judgment and individual expertise. This study aims to automate fractographic analysis through advanced computer vision techniques. Different materials were tested in hydrogen atmospheres and inert environments, and their fracture surfaces were analyzed by scanning electron microscopy to create an extensive image dataset. A pre-trained Convolutional Neural Network was finetuned to accurately classify brittle and ductile fractures. In addition, Grad-CAM interpretability method was adopted to identify the image regions most influential in the model’s prediction and compare the saliency maps with expert annotations. This approach offered a reliable data-driven alternative to conventional fractographic analysis. KW - Failure analysis KW - Fractographic analysis KW - Hydrogen embrittlement KW - Material compatibility PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646610 DO - https://doi.org/10.1016/j.commatsci.2025.114366 SN - 0927-0256 VL - 262 SP - 1 EP - 16 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-64661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Campari, Alessandro A1 - Konert, Florian A1 - Sobol, Oded A1 - Alvaro, Antonio T1 - A comparison of vintage and modern X65 pipeline steel using hollow specimen technique for in-situ hydrogen testing N2 - The transition toward a hydrogen-based economy requires a widespread transport and distribution network, and repurposed natural gas pipelines are a viable option. An assessment of the hydrogen-induced degradation of pipeline steels is needed to inject H2 gas into the existing infrastructure safely. The conservative and standardized method consists of in-situ tensile tests in an autoclave filled with high-pressure hydrogen gas. A proposed alternative method involves using a hollow specimen as containment volume and applying the gas pressure in the inner cavity. This technique has lower costs and shorter test preparation time but is not standardized yet. This study aims to evaluate and compare the tensile properties of API 5L X65 pipeline steel in two states: vintage and modern. The influence of the surface roughness is investigated through parallel tests with drilled and reamed specimens. Hydrogen tests are compared with reference tests in an inert environment. A significant hydrogen-induced decrease in tensile properties is observed, and no significant difference between vintage and modern X65 can be drawn. The reduction in tensile properties is more significant in specimens with higher inner surface roughness. The evaluation of surface conditions appears crucial when assessing the HE susceptibility of hydrogen transport and storage equipment. KW - Hydrogen embrittlement KW - Hollow specimen technique KW - Pipeline steel KW - SSRT PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603013 DO - https://doi.org/10.1016/j.engfailanal.2024.108530 VL - 163 SP - 1 EP - 15 PB - Elsevier Ltd. AN - OPUS4-60301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drexler, A A1 - Konert, Florian A1 - Sobol, Oded A1 - Rhode, Michael A1 - Domitner, J A1 - Sommitsch, C A1 - Böllinghaus, Thomas T1 - Enhanced gaseous hydrogen solubility in ferritic and martensitic steels at low temperatures N2 - Metals that are exposed to high pressure hydrogen gas may undergo detrimental failure by embrittlement. Understanding the mechanisms and driving forces of hydrogen absorption on the surface of metals is crucial for avoiding hydrogen embrittlement. In this study, the effect of stress-enhanced gaseous hydrogen uptake in bulk metals is investigated in detail. For that purpose, a generalized form of Sievert's law is derived from thermodynamic potentials considering the effect of microstructural trapping sites and multiaxial stresses. This new equation is parametrized and verified using experimental data for carbon steels, which were charged under gaseous hydrogen atmosphere at pressures up to 1000 bar. The role of microstructural trapping sites on the parameter identification is critically discussed. KW - Hydrogen KW - Thermodynamic modelling KW - Pressure-dependent solubility KW - Steel KW - Trapping PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559307 DO - https://doi.org/10.1016/j.ijhydene.2022.09.109 SN - 0360-3199 VL - 47 IS - 93 SP - 39639 EP - 39653 PB - Elsevier Ltd. AN - OPUS4-55930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falk, Florian A1 - Sobol, Oded A1 - Stephan-Scherb, Christiane T1 - The impact of the microstructure of Fe-16Cr-0.2C on high-temperature oxidation – sulphidation in SO2 N2 - This study elucidates the impact of the microstructure of Fe-16Cr-0.2C on oxide layer formation at 650 ◦C in Ar-0.5 % SO2. A cold-rolled and two heat-treated states of the alloy were exposed for up to 1000 h. The samples were characterised in detail from microstructural and chemical perspectives using scanning electron microscopy (SEM), X-ray diffraction (XRD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The microstructural modification of the alloy by heat-treatment was advantageous. It was found that Cr-carbides support chromia formation and reduce sulphidation when their area fraction is low and diameter is small. KW - Steel KW - Iron KW - SIMS KW - SEM KW - High temperature corrosion KW - Oxidation KW - Sulphidation PY - 2021 DO - https://doi.org/10.1016/j.corsci.2021.109618 VL - 190 SP - 109618 PB - Elsevier Ltd. AN - OPUS4-53001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grimault de Freitas, Tomás A1 - de Araujo Abilio, André A1 - Konert, Florian A1 - Nietzke, Jonathan A1 - Krzysch, Zephanja A1 - Böllinghaus, Thomas A1 - Sobol, Oded T1 - Challenges with metallic materials for the transport and storage of hydrogen N2 - The hydrogen economy is one of the most important solutions to achieve climate neutrality in Europe. It involves the production, storage, transport and use of large quantities of hydrogen in existing and new infrastructures. Components along this supply chain, such as pipelines and storage tanks, are made of various metallic materials, with steel being the most common construction material. The rapid introduction of hydrogen therefore brings with it major challenges, in particular the need for comprehensive qualification of components and materials to ensure the sustainable and safe use of hydrogen technologies. This article provides an overview of the state of the art in the testing of materials and components as well as corresponding future trends and developments for a successful transition to a hydrogen economy. T2 - VGBE - Materials and Quality Assurance 2023 CY - Bergheim, Germany DA - 10.05.2023 KW - Hydrogen Embrittlement KW - Materials Testing KW - Component Testing KW - High-Pressure Gaseous Hydrogen KW - Hollow Specimen Technique PY - 2024 VL - 4 SP - 60 EP - 64 PB - VGBE Energy AN - OPUS4-60686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grimault de Freitas, Tomás A1 - Konert, Florian A1 - Nietzke, Jonathan A1 - Krzysch, Zephanja A1 - Böllinghaus, Thomas A1 - Michler, Thorsten A1 - Wackermann, Ken A1 - Oesterlin, Heiner A1 - Tlili, Mohamed A1 - Ruchti, Peter A1 - Beitelschmidt, Denise A1 - Elsen-Humberg, Stephan A1 - Koenigs, Timo A1 - Systermans, Thomas A1 - Sobol, Oded T1 - Tensile testing in high-pressure gaseous hydrogen using the hollow specimen method N2 - Metallic materials, predominantly steels, are the most common structural materials in the various components along the hydrogen supply chain. Ensuring their sustainable and safe use in hydrogen technologies is a key factor in the ramp-up of the hydrogen economy. This requires extensive materials qualification, however, most of the accepted; and standardized test methods for determining the influence 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, rapid, and economical method designed to overcome the limitations of the current methods for the qualification of metallic materials under high-pressure hydrogen gas. However, this technique is not yet standardized. The TransHyDE-H2Hohlzug project is presented in this article, along with the main steps required to optimize the hollow specimen technique. This includes closing knowledge gaps related to the specimen geometry, surface quality, and gas purity in dedicated working packages, thus contributing to a comprehensive standardization of the technique for tests in high-pressure hydrogen gas. KW - High-pressure Gaseous Hydrogen KW - Hydrogen Embrittlement KW - Tensile Testing KW - Hollow Specimen Technique PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610557 DO - https://doi.org/10.1557/s43577-024-00776-9 VL - 49 SP - 1 EP - 9 PB - Springer Nature AN - OPUS4-61055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Holzlechner, Gerald A1 - Sobol, Oded A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang ED - Udomkichdecha, W. ED - Mononukul, A. ED - Böllinghaus, Thomas ED - Lexow, Jürgen T1 - Imaging ToF-SIMS as a chemical metrology tool to support material and analytical science N2 - As a chemical metrology tool time-of-flight secondary ion mass spectrometry (ToF-SIMS) has become a very popular technique to monitor the elemental, isotopic and molecular distribution in two or three dimensions. Its reduced sampling depth, high sensitivity, great structural specificity and the direct detection of hydrogen thereby increase the emergence of ToF-SIMS for material and analytical surface science, particularly due to recent instrumental developments improving mass, depth and lateral resolution. For basic surface science, adsorption processes and surface reactivity thus can be investigated in high detail on organic as well as inorganic samples. The use of multivariate data analysis in addition can effectively assist to identify trends in the complex SIMS raw data set and define key co-variances between certain samples or mass spectra. In this contribution the essence of ToF-SIMS is illustrated by discussing two highly relevant energy applications. First, for piezoelectric electroceramics oxygen exchange active zones have been visualized to determine the impact of external field-load to the oxygen vacancy distribution between anode and cathode. As a second case study the interaction of hydrogen species with the microstructure of a duplex stainless steel was investigated. It was concluded that ToF-SIMS has a valuable essence for detailing hydrogen related degradation mechanisms. T2 - 4th WMRIF Young scientists workshop CY - Boulder, CO, USA DA - 08.09.2014 PY - 2016 SN - 978-981-287-723-9 SN - 978-981-287-724-6 DO - https://doi.org/10.1007/978-981-287-724-6_7 SP - 63 EP - 72 PB - Springer AN - OPUS4-34881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzweber, Markus A1 - Sobol, Oded A1 - Wirth, Thomas A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Deuterium permeation and cracking in duplex steels as viewed by ToF-SIMS and HR-SEM with data fusion N2 - Better understanding of hydrogen assisted degradation and trapping mecha-nisms requires sufficient imaging techniques for respective hydrogen-microstructure interaction studies, in particular with multi-phase metallic micro-structures [1]. The present work is focusing on the elucidation of deuterium be-havior in two austenitic-ferritic duplex stainless steels (DSS) under the assumption that deuterium behaves in many ways similarly to hydrogen [2]. For case studies standard 2205 and lean 2101 DSSs were chosen due to the extensive use of these steels in industry [3]. The analyses were conducted by using a novel in-situ permeation and Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging technique or by ex-situ ToF-SIMS imaging following electrochemical charging experiments. Another pioneering procedure was data fusion (including chemometry) of results of powerful laterally resolved chemical analysis and high resolution structural characterization techniques . Results for the ex-situ observations showed a different influence of deuterium loading on the two steel grades as well as different damage mechanisms in each phase. Formation of sub-surface blisters between the ferrite and austenite were obtained in both the standard and the lean DSS. In both steels, an increased deuterium concentration was observed around deformed regions such as cracks, confirming that they originate from the presence of deuterium [4]. The formation of parallel cracks was obtained only in the austenite within the standard duplex whereas in the lean duplex the highest intensity of deuterium was obtained in the austenite along the ferrite-austenite interphase. In comparison, application of the novel in-situ permeation technique enabled to register and record the deuterium permeation through the material and the respective saturation sequence of the two phases as well as the interfaces. Faster diffusion of the deuterium was observed in the ferrite and a direct proof for deuterium enrichment at the austenite-ferrite interface has been given [1]. The integration of the specified techniques gives a better insight into the processes leading to hydrogen induced failure. These two experimental techniques provide very valuable tools for elucidation of respective metallurgical failure mechanisms that can be used for the validation of respective numerical models for hydrogen assisted cracking (HAC). T2 - 19. Arbeitstagung Angewandte Oberflächenanalytik CY - Soest, Germany DA - 05.09.2016 KW - ToF-SIMS KW - Hydrogen assisted cracking KW - Data fusion KW - SEM PY - 2016 AN - OPUS4-37484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konert, Florian A1 - Campari, Alessandro A1 - Nietzke, Jonathan A1 - Sobol, Oded A1 - Paltrinieri, Nicola A1 - Alvaro, Antonio T1 - Evaluation of the tensile properties of X65 pipeline steel in compressed gaseous hydrogen using hollow specimens N2 - Hydrogen has great potential on the path towards decarbonization of the energy and transport sectors and can mitigate the urgent issue of global warming. It can be sustainably produced through water electrolysis with potentially zero emissions, and efficiently used (e.g., in fuel cell systems). Despite its environmental advantages, hydrogen-metal interactions could result in the degradation of the mechanical properties of several structural materials. In order to determine the magnitude of the material degradation in relation to hydrogen exposure, extensive material testing is required. The standardized procedure for in-situ testing for the quantification of the impact of compressed gaseous hydrogen (CGH2) relies on the utilization of an autoclave around the tested specimen. Such test set-up is complex, expensive, time-consuming and requires special equipment, trained personnel, and strict safety procedures. A relatively recent method to circumvent these issues and provide affordable results consists of using hollow specimens, thus applying the hydrogen pressure inside rather than outside the specimen. It allows to reduce the volume of hydrogen by several orders of magnitude and to perform the tests more efficiently and in a safer manner. This study focuses on evaluating the tensile properties of X65 vintage pipeline steel tested in a high-pressure hydrogen environment using hollow specimens. Tests are performed in 6 MPa H2 and Ar at the nominal strain rate of 10−6 s−1 to evaluate the reduced area at fracture and the elongation loss. The effect of surface finishing on crack initiation and propagation is investigated by comparing two different manufacturing techniques. In this way, this study provides insights into the applicability of a novel, reliable, and safe testing method which can be used to assess the hydrogen-assisted ductility loss in metallic materials. KW - Mechanical Engineering KW - Hydrogen Embrittlement KW - SSRT KW - Hollow specimen KW - Pipeline steel KW - In-situ tensile test PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595887 DO - https://doi.org/10.1016/j.prostr.2024.01.074 SN - 2452-3216 VL - 54 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-59588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -