TY - CONF A1 - Sobol, Oded T1 - Metallic materials for the transport and storage of hydrogen N2 - Um die Absorption von Wasserstoff und dessen Verhalten in den Werkstoffen beim Einsatz unter Druck-H2 sowie die H- abhängigen Materialeigenschaften zu definieren, entwickelt die BAM mit ihrer langjährigen Erfahrung adäquate Prüfkonzepte, die einsatzrelevante Bedingungen und reale Beanspruchungen (Temperatur, Wasserstoff und mech. Beanspruchung) hierarchisch berücksichtigen. Der Vortrag gibt eine Einführung in das Thema von wasserstoffunterstützen Materialschäden durch die Problematik der Einspeisung von Wasserstoff in bestehende Erdgasnetze. Ferner wird auf die Hochdruck-Infrastruktur (sowie H2-Tankstellen) und die Entwicklung von Prüfkonzepten für die Gasinfrastruktur unter Druckwasserstoffbeaufschlagung eingegangen. T2 - Die Deutsche Physikalische Gesellschaft (DPG): Veranstaltung der Arbeitsgruppe Senior Expert Netzwerk CY - Berlin, Germany DA - 20.10.2021 KW - Hydrogen Embrittlement KW - Hydrogen assisted cracking KW - Gaseous hydrogen KW - Time-of-Flight Mass Spectrometry KW - Tensile test PY - 2021 UR - https://www.dpg-physik.de/veranstaltungen/2021/mhb-agsen-2021-10-20 AN - OPUS4-53599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Challenges with metallic materials for the transport and storage of hydrogen N2 - The following presentation provides an overview on some of the challenges with metallic materials used as structural materials in the energy sector for the transport and storage of hydrogen. The presentation contains explanations about the methodologies utilized to characterize the susceptibility of these materials for hydrogen. T2 - Materials and Quality Assurance CY - Bergheim, Germany DA - 10.05.2023 KW - Hollow specimen KW - Slow strain tensile tests KW - Hydrogen assisted cracking PY - 2023 AN - OPUS4-57515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Lehmusto, Juho A1 - Falk, Florian A1 - Sobol, Oded A1 - Pint, Bruce T1 - Comprehensive insights into competitive oxidation/sulfidation reactions on binary ferritic alloys at high temperatures N2 - Interpreting high-temperature corrosion induced by mixed-gas atmospheres is challenging due to the different contributions of oxidizing gases. Here, a comprehensive study on the combined oxidation/sulfidation using label molecules is presented. Fe-Cr model alloys with 2 wt% and 9 wt% Cr were isothermally exposed using a volumetric mixture of 0.5%S16O2/27%H218O and 0.5%S16O2/7%H218O at 650 ◦C for 5 h and then characterized by secondary ion mass spectroscopy (SIMS). Additionally, the reactions were followed in-situ utilizing energy dispersive X-ray diffraction. The study showed that both S16O2 and H218O contribute to the oxidation of the alloys but to different extents depending on the Cr-content. KW - SEM KW - Steel KW - Iron KW - SIMS PY - 2022 DO - https://doi.org/10.1016/j.corsci.2022.110236 SN - 0010-938X VL - 203 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-58992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shikomba, Nikanor A1 - Böllinghaus, Thomas A1 - Konert, Florian A1 - Sobol, Oded A1 - Blasón Gonzalez, Sergio A1 - Krafft, Eike A1 - Staudt, Thorsten T1 - Testing the resistance of low-alloyed steel welds for pressurized gaseous hydrogen applications N2 - Green hydrogen has become an essential energy carrier to achieve a climate-neutral economy. The production, storage, transport and usage of green hydrogen (GH2) requires facilities and systems that are safe and sustainable. Systems for GH2 facilities, especially for storage and transport are mainly assembled of welded steel components. These components are exposed to the gaseous hydrogen environment throughout their service life. In contrast to hydrogen absorption from electrochemical environments entailing hydrogen-assisted corrosion cracking, the absorption and material degradation in gaseous environments have less been investigated. Nevertheless, the degradation of mechanical properties in materials and their welds due to absorbed hydrogen poses significant risks, including cracking and leakages. To ensure the safety and reliability of GH2 facilities throughout their service life, it is crucial to investigate and prevent such hydrogen-induced degradation, thereby avoiding potential incidental and accidental scenarios. Due to the worldwide technology push for new energy carriers like GH2 and its derivates, extensive research and testing of welded components is not an option to avoid delays in the GH2-readiness of respective facilities. The present contribution shows how to investigate the compatibility of low alloyed steels and their welds for GH2 storage and transport subjected to quasi-static mechanical loads in principle by utilizing the Slow Strain Rate Test (SSRT) with the Hollow Specimen Technique (HST). Exemplarily, low-alloyed steel welds of the P355NL1 type currently used for hydrogen storage tanks at intermediate pressures have been investigated and compared to welds of type X65, as a very common pipeline material. Test results show a higher value of the Hydrogen Embrittlement Index (HEI) in weld specimens than the base specimens in both investigated materials. HEI of 8.3% was recorded in base specimens and 15% in weld specimens of P355NL1, while X65 EI gives 30.2% in BM and 27.7 in WM. The fractography analysis reveals that hydrogen promotes the transition from tensile fracture to brittle fracture. Hydrogen did not show any effect on the yield strength and tensile strength of all tested specimens. However, it affects the plastic elongation of the tested materials. In conclusion, the obtained HEI values indicate a mild but significant degradation in the materials. The results confirm that hydrogen absorption from gaseous environments leads to a reduction in the mechanical properties of steels and their welds, with a more pronounced impact on ductility than on strength. T2 - IIW Annual Assembly July 2024, Commission XI CY - Rhodes, Greece DA - 07.07.2024 KW - Hydrogen-assisted cracking KW - Welded joint KW - Hollow specimens KW - SSRT KW - Structural steels PY - 2024 AN - OPUS4-61113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Challenges with metallic materials in H 2 technologies N2 - Increasing environmental problems with conventional energy technology are stimulating the demand for alternative energy solutions. With air quality reaching catastrophic levels in large cities worldwide, Fuel Cell Electric Vehicles offer the ideal combination of clean power with the amenities of electric drives. Hydrogen use on vehicles, nevertheless, also raises some issues about safe handling. As fuel cells and hydrogen applications, including vehicles, approach technological maturity, developing their business cases becomes crucial in introducing them to the consumer markets. The Joint European Summer School JESS 2021 addresses these issues by offering high quality graduate level courses on selected topics of vehicle technology, innovation & business development, safe handling of hydrogen, and modelling. This series of summer schools has been ongoing since 2004 and targets an audience of university students (MSc and PhD levels) and post-doctoral researchers. We also welcome more experienced researchers and engineers wishing to expand their general knowledge, for instance, to suit a newly acquired position or collect credits for Continuous Professional Development (CPD). The course content is tailored to the needs of a diverse audience: newcomers to the field, experienced students, and young professionals working at the forefront of fuel cell and hydrogen applications. T2 - Joint european summer school (JESS) CY - Online meeting DA - 06.09.2021 KW - Hydrogen Embrittlement KW - Hydrogen assisted cracking KW - Gaseous hydrogen PY - 2021 UR - https://www.jess-summerschool.eu/Week-2 SP - 1 EP - 41 AN - OPUS4-53402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Holzlechner, Gerald A1 - Holzweber, Markus A1 - Lohninger, H. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - First use of data fusion and multivariate analysis of ToF-SIMS and SEM image data for studying deuterium-assisted degradation processes in duplex steels N2 - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) and high-resolution scanning electron microscopy are well-acknowledged tools in materials characterization. The ability to map chemical species on the surface of an investigated sample with often low mass detection limits makes ToF-SIMS an essential tool in fields where many question marks concerning Degradation processes and damage mechanisms exist. The aim of this paper is to describe the power of data fusion of ToF-SIMS and high-resolution scanning electron microscopy results employing computational methods for multivariate data Analysis such as principal component analysis. As a case study the investigation of hydrogen distribution in an artificially charged Duplex stainless steel microstructure is presented aiming on a better understanding of hydrogen embrittlement. T2 - 16th European Conference on Applications of Surface and Interface Analysis CY - Granada, Spain DA - 28.09.2015 KW - ToF-SIMS KW - HR-SEM KW - Data fusion KW - Duplex stainless steel KW - Hydrogen embrittlement PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/sia.6015/full DO - https://doi.org/10.1002/sia.6015 VL - 48 IS - 7 SP - 474 EP - 478 PB - John Wiley & Sons, Ltd CY - Surface and Interface Analysis AN - OPUS4-36832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silverstein, R. A1 - Sobol, Oded A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang A1 - Eliezer, D. T1 - Hydrogen behavior in SAF 2205 duplex stainless steel N2 - This paper describes austenitic-ferritic duplex stainless steels, SAF 2205, in the presence of hydrogen. The duplex stainless steels (DSS) properties include excellent resistance to stress corrosion cracking, high strength and good weldability. Those steels are preferably used in industries combining hydrogen and loads. Hydrogen location in addition to hydrogen binding energy with the steel's defects are of great importance for the analysis of hydrogen embrittlement model in that steel. It is known from previously published works that the susceptibility to hydrogen embrittlement will depend on the competition between reversible and irreversible traps; meaning a direct relation to the hydrogen's state and position in the steel. In this work, we examine the local hydrogen concentration, trapping and distribution by two modern and advanced techniques: thermal desorption spectrometry (TDS) and we support it by time of flight-secondary ion mass spectrometer (ToF-SIMS). In this paper, we support and give for the first time new insights and better understanding to the hydrogen embrittlement mechanism in SAF 2205. The trapping energies levels were calculated using TDS and Lee and Lee's model. This model revealed reversible in addition to irreversible trapping sites. Also the trapping controlling mechanism was found to be a combination of detrapping controlled mechanism and diffusion controlled mechanism. The use of ToF-SIMS for local imaging the distribution of hydrogen species supports the discussion of the different hydrogen traps in this type of steel. The hydrogen embrittlemet phenomenon in SAF 2205 will be discussed in details in that paper. KW - Hydrogen trapping KW - Duplex stainless steel KW - Thermal desorption spectrometry (TDS) KW - ToF-SIMS PY - 2017 DO - https://doi.org/10.1016/j.jallcom.2016.11.184 SN - 0925-8388 SN - 1873-4669 VL - 695 SP - 2689 EP - 2695 PB - Elsevier B.V. AN - OPUS4-38856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Shikomba, Nikanor A1 - Böllinghaus, Thomas A1 - Konert, Florian A1 - Sobol, Oded A1 - Blasón Gonzalez, Sergio A1 - Ohijeagbon, Idehai Olayemi A1 - Krafft, Eike A1 - Staudt, Thorsten T1 - Correction: Resistance of welded low-alloyed pressure vessel and pipeline steels in gaseous hydrogen N2 - This is a corrigendum to the original article "Resistance of welded low-alloyed pressure vessel and pipeline steels in gaseous hydrogen" that was published in the journal "Welding in the world" (2025), doi: 10.1007/s40194-025-02074-7. PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634647 DO - https://doi.org/10.1007/s40194-025-02098-z SN - 0043-2288 SP - 1 PB - Springer CY - Berlin AN - OPUS4-63464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mente, Tobias A1 - Grimault de Freitas, Tomás A1 - Nietzke, Jonathan A1 - Konert, Florian A1 - Sobol, Oded A1 - Wackermann, Ken A1 - Ruchti, Peter A1 - Elsen-Humberg, Stefan A1 - Systermans, Thomas ED - Zimmermann, Martina T1 - Hohlzugprüfung als kostengünstige Methode zur Werkstoffcharakterisierung für die Wasserstoffwirtschaft N2 - Wasserstoff ist ein notwendiger Baustein zur Erreichung zukünftiger Klimaziele. Für eine schnell hochlaufende Wasserstoffwirtschaft ist es daher notwendig sowohl bestehende Infrastruktur als auch neue Werkstoffe für den sicheren und nachhaltigen Einsatz in Wasserstofftechnologien zu qualifizieren. Die akzeptierten und standardisierten Prüfverfahren zur Ermittlung des Einflusses gasförmigen Wasserstoffs auf die mechanischen Eigenschaften metallischer Werkstoffe sind meist sehr komplex, mit hohem technologischem und finanziellem Aufwand verbunden und stehen nur Wenigen Instituten weltweit zur Verfügung. Die Hohlzugprüftechnik bietet hier eine kostengünstige und einfach zu realisierende Alternative. Mit der im Jahr 2024 erstmals veröffentlichten ISO 7039 wurde diese Prüftechnik auch für die Wirtschaft anwendbar gemacht. Der Standard gilt allgemein für die Prüfung mit gasförmigen Medien, weist jedoch in Bezug auf die Prüfung mit gasförmigem Wasserstoff noch einige Wissenslücken auf. Im Teilvorhaben H2HohlZug des Leitprojekt TransHyDE werden die Lücken zum Einfluss der Geometrie, Oberflächenqualität sowie Gasreinheit in einzelnen Arbeitspaketen geschlossen und die Erkenntnisse in einen Standard überführt. T2 - 43. Vortrags- und Diskussionstagung Werkstoffprüfung 2025 - Werkstoffe und Bauteile auf dem Prüfstand CY - Dresden, Germany DA - 27.11.2025 KW - Hohlzugprüfung KW - Druckwasserstoff KW - ISO 7039 KW - H2HohlZug - TransHyDE PY - 2025 SN - 978-3-88355-454-9 SP - 11 EP - 17 PB - Deutsche Gesellschaft für Materialkunde e.V. (DGM) CY - Dresden AN - OPUS4-64937 LA - deu 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 - Sobol, Oded A1 - Böllinghaus, Thomas A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Eliezer, D. T1 - High resolution ToF-SIMS imaging of deuterium permeation and cracking in duplex stainless steels N2 - Fundamental understanding and elucidation of hydrogen assisted degradation and trapping mechanisms is dependent on sufficient imaging techniques for respective hydrogen interactions, in particular with multi-phase metallic microstructures. The present work shows the progress in elucidating the deuterium behavior in austenitic-ferritic duplex stainless steels under the consideration that deuterium behaves in many ways similarly to hydrogen. A novel combination of deuterium permeation and in-situ Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) imaging technique is compared with post charging ToF-SIMS imaging experiments. As a step beyond state-of-the-art, integration of chemo-metric and high resolution structural characterization techniques with computational multivariate data analysis (MVA) and data fusion is presented. T2 - 2016 International Hydrogen Conference CY - Grand Teton National Park, Jackson Lake Lodge, Wyoming, USA DA - 11.09.2016 KW - DSS KW - ToF-SIMS KW - Data-fusion KW - EBSD PY - 2017 SN - 978-0-7918-6138-7 SP - 407 EP - 415 PB - ASME Press CY - Two Park Ave. New-York, NY 10016, USA AN - OPUS4-42647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Nolze, Gert A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Use of time-of-flight secondary ion mass spectrometry for the investigation of hydrogen-induced effects in austenitic steel AISI 304L N2 - During the energy transformation from fossil fuels to renewable energy sources, the use of hydrogen as fuel and energy storage can play a key role. This presents new challenges to industry and the scientific community alike. The storage and transport of hydrogen, which is nowadays mainly realized by austenitic stainless steels, remains problematic, which is due to the degradation of mechanical properties and the possibility of phase transformation by hydrogen diffusion and accumulation. The development of materials and technologies requires a fundamental understanding of these degradation processes. Therefore, studying the behavior of hydrogen in austenitic steel contributes to an understanding of the damage processes, which is crucial for both life assessment and safe use of components in industry and transportation. As one of the few tools that is capable of depicting the distribution of hydrogen in steels, time-of-flight secondary ion mass spectrometry was conducted after electrochemical charging. To obtain further information about the structural composition and cracking behavior, electron-backscattered diffraction and scanning electron microscopy were performed. Gathered data of chemical composition and topography were treated employing data fusion, thus creating a comprehensive portrait of hydrogen-induced effects in the austenite grade AISI 304L. Specimens were electrochemically charged with deuterium instead of hydrogen. This arises from the difficulties to distinguish between artificially charged hydrogen and traces existing in the material or the rest gas in the analysis chamber. Similar diffusion and permeation behavior, as well as solubility, allow nonetheless to draw conclusions from the experiments. T2 - 21st International Conference on Secondary Ion Mass Spectrometry CY - Kraków, Poland DA - 10.09.2017 KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Austenitic stainless steel PY - 2018 DO - https://doi.org/10.1116/1.5013931 SN - 1071-1023 VL - 36 IS - 3 SP - Article 03F103, 1 EP - 6 PB - American Vacuum Society (AVS) AN - OPUS4-44840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leo, Reinhold A1 - Sobol, Oded A1 - Hango, Silas Ithete A1 - Saliwan Neumann, Romeo A1 - Askar, Enis A1 - Boellinghaus, Thomas T1 - Ex-situ investigation of the compatibility of Duplex Stainless Steel for high-pressure hydrogen applications N2 - The key to a successful transition into clean energy carriers such as hydrogen requires the construction of safe transportation pipelines made of alloys which are not susceptible to hydrogen assisted cracking. Duplex Stainless Steels (DSS) are considered as a proper class for components because of their many distinctive qualities. As this consideration depends strongly on the susceptibility level to Hydrogen Assisted Cracking (HAC), the DSS class has been broadly investigated under electrochemical charging conditions. In this work, the interplay between several factors controlling the level of HAC, was examined using light microscopy, high-pressure gaseous hydrogen pre-charging, Electron Backscatter Diffraction (EBSD), tensile testing, fractography and hydrogen concentration measurements using Carrier Gas Hot Extraction (CGHE). The effect of gaseous hydrogen on the mechanical properties with the role of hydrogen induced phase transformation have been investigated both in unused material and in high pressure pipeline section. In contrary to the common electrochemical charging described broadly in the literature, no significant martensitic phase transformation of the austenitic phase was observed. On the other hand, the influence of hydrogen on parameters such as elongation at fracture and reduction of area was noticeable. It is concluded based on the performance of DSS in gaseous hydrogen, that this material has a better potential for utilization in hydrogen applications. As for future experiments, the intention is to analyse the impact of high-pressure gaseous hydrogen on the welded components of this grade, and under mechanical load using the hollow specimen technique. T2 - 5th International Conference on Metals and Hydrogen CY - Ghent, Belgium DA - 14.10.2025 KW - High-Pressure Hydrogen KW - Pipelines KW - Duplex Stainless Steels KW - Hydrogen Assisted Cracking KW - Hollow Specimen Technique PY - 2025 SN - 978-9-08179-424-4 SP - 1 EP - 19 AN - OPUS4-64426 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 - CONF A1 - Sobol, Oded T1 - Investigations of Hydrogen Embrittlement (HE) by ToF-SIMS T2 - BAM Ph.D. Retreat 2015 CY - Wandlitz, Germany DA - 2015-06-05 PY - 2015 AN - OPUS4-33691 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Investigations of Hydrogen Embrittlement (HE) by Time-of-Flight Secondary Ion Mass Spectroscopy (ToF-SIMS) T2 - 18. Tagung Festkörperanalytik CY - Vienna, Austria DA - 2015-06-07 PY - 2015 AN - OPUS4-33692 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - The characterization of oxygen diffusion in (Na1/2Bi1/2)TiO3 piezo-ceramics by Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) N2 - The ferroelectric ceramic NBT and its solid solutions with barium titanate (BT) are examples for the most promising lead free materials to substitute the dominant Pb(Zr,Ti)O3 (PZT). Lead based material should generally be disregarded due to environmental and health reasons. However, there is no class of lead-free piezoelectric materials that can replace PZT entirely. Not only the often inferior ferroelectric properties but also the lack of understanding of the defect chemistry of NBT is still a challenge for the replacement of lead containing piezo-ceramics. Just recently it could be shown by Li et al.[1] that NBT obtains extraordinarily high oxygen ionic conductivity when doped with Mg as acceptor. It was actually expected that doping just leads to a hardening of the ferroelectric properties. However, it became clear that the known defect chemical behavior of PZT cannot be extrapolated to NBT materials. Hence, to gain information on general doping effects a better defect chemical investigation is needed. This is particularly important for the applications with high reliability demands to investigate possible degradation and fatigue mechanisms. In the present work Time-of-flight-secondary ion mass spectrometry (ToF-SIMS) was used in order to observe the influence of different acceptor dopants (Fe, Ni, Al) on the oxygen diffusion in NBT. ToF-SIMS holds the ability to gain a full elemental distribution in a sub-micron resolution and was therefore chosen to provide the essential information on the favorable diffusion paths of oxygen in NBT in dependence of the chosen doping element. 18O was used as a tracer for oxygen as its natural abundance is only 0.2%. The doped NBT samples have been annealed for 5 h at 500°C in a 0.2 bar 18O-tracer atmosphere to be able to detect oxygen ion diffusion. ToF-SIMS investigations were conducted on a ToF-SIMS IV (ION TOF GmbH, Münster, Germany) using a Bi+ primary ion beam (25KeV in collimated burst alignment mode with a beam diameter of ~150 nm) and a Cs+ sputter beam (3KeV). The results illustrate the different impact of dopants on the diffusion properties which is evidence for a highly non-linear dependence on dopant type and concentration. 1) Li, M., et al., Nature Materials, 2014. 13(1): p. 31-35. T2 - 21st International Conference on Secondary Ion Mass Spectrometry - SIMS21 CY - Krakow, Poland DA - 10.09.2017 KW - NBT-Piezoceramics KW - ToF-SIMS PY - 2017 UR - http://sims.confer.uj.edu.pl/boa_poster.php?id=93 AN - OPUS4-42863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Observations of the deuterium distribution and the structural changes in standard and lean duplex stainless steels by ToF-SIMS and EBSD N2 - The use of duplex stainless steels (DSS) in energy related applications is well known. Nowadays, DSSs become more favorable than austenitic steels due to the outstanding mechanical properties, the good corrosion resistance and the lower nickel content.However, the use of the duplex grade in acidic environments such as seawater can lead to a severe degradation in the structural integrity of the steel by hydrogen-induced/assisted cracking mechanisms, which can eventually result in premature failure. Hydrogen assisted degradation and cracking of steels remains unclear even though this topic is intensively studied for more than a century. The main gap lies in the validation of the proposed theoretical models at the sub-micron scale. Industrial and the research communities define a need for an accurate method by which it is possible to image the distribution of hydrogen in the microstructure. Among the very few available methods nowadays, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) provides precise mapping of hydrogen in the microstructure. Moreover, the powerful combination of ToF-SIMS with multivariate data analysis (MVA), electron backscattered diffraction (EBSD) for providing a the structural information and the use of data fusion techniques can contribute to a better understanding of the hydrogen induced degradation processes in the material. In the present work two types of duplex grades were chosen as a case study (standard and lean DSS). The duplex class, consist of equivalent amounts of ferrite and austenite, was investigated by ToF-SIMS and EBSD during and after electrochemical deuterium charging in order to simulate the service of a component in acidic environments. Deuterium is known to act on the steel similarly to hydrogen and therefore was used as a tracer for hydrogen. The results show that the ferrite was affected almost identical in both steels whereas in the austenitic phase significant differences were observed in the lean duplex in comparison to the standard duplex. The advantage of the combined techniques is reflected by the ability to correlate the hydrogen distribution in the microstructure to the resulted structural changes. T2 - 21st International Conference on Secondary Ion Mass Spectrometry - SIMS21 CY - Krakow, Poland DA - 10.09.2017 KW - ToF-SIMS KW - Duplex-steel KW - EBSD KW - Data-fusion PY - 2017 UR - http://sims.confer.uj.edu.pl/boa_oral.php?id=23 AN - OPUS4-42864 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 - CONF A1 - Sobol, Oded T1 - Influence of Hydrogen Uptake and Diffusion in Structural Components in the Field of Renewable Energy N2 - Great efforts are invested worldwide in the development of efficient electrolysis processes, fuel cells technologies and hydrogen transport and storage infrastructures. This includes the exploitation of existing gas-grid infrastructure for the injection of hydrogen. Considering transport and storage facilities, the utilization of gaseous hydrogen can be divided into two main groups which are differentiating in the pressure regime. Fueling stations are operating in high pressure (>800 bar) and high purity and therefore use austenitic stainless steels in their compression systems. On the other hand, existing gas infrastructure where the natural gas is transported across long distances is usually operating with up to 300 bar. In this case the pipe-systems consist of several steel classes, mainly low alloyed steels in which the surface quality and the gas mixture are strongly varying. Even though ingress of hydrogen can lead to catastrophic failures in all steels, its exact impact on the mechanical properties, as well as its interaction with the surface, microstructure and lattice and the underlying mechanisms remain unclear. Therefore, research on the impact of gaseous hydrogen in pressure vessels and pipes has clearly an integral part on the path to safe and sustainable use of the different components along the different chains. This becomes even more relevant considering the influence of impurities in the gas, e.g. sulfur and with the introduction of new production technologies, such as additive manufacturing, into the market. Determination of these interactions and impact that might lead to the degradation of the properties can allow a safe use of steels in present and future hydrogen-based energy applications. The following contribution gives an overview of the problem and introduction to the conventional and innovative tools used and developed nowadays to analyze it. For this purpose, materials were loaded with hydrogen by electrochemical means and under high pressure and elevated temperatures. The results presented provide an invaluable insight into the impact of hydrogen on the integrity of selected steels used in the two mentioned above applications. This work is part of an ongoing research in which mechanical, chemical, structural, and microstructural analyses tools are combined in-situ and ex-situ. T2 - MPA 46th Seminar: Additive Manufacturing, Hydrogen, Energy, Integrity CY - Leinfelden-Echterdingen, Germany DA - 12.10.2021 KW - Hydrogen Embrittlement KW - Hydrogen assisted cracking KW - Gaseous hydrogen PY - 2021 AN - OPUS4-53598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Observations of the deuterium distribution and the structural changes in standard and lean duplex stainless steels by ToF-SIMS and EBSD N2 - Duplex (DSS) and austenitic stainless steels (ASS) are frequently used in many energy related applications. The duplex grade is considered to have outstanding mechanical properties as well as good corrosion resistance. The austenitic phase combines high ductility, even at low temperatures, with sufficient strength, and therefore such materials are applied in storage and transport of high-pressure hydrogen. During service in acidic environments large amounts of hydrogen can ingress into the microstructure and induce many changes in the mechanical properties of the steel. Embrittlement of steels by hydrogen remains unclear even though this topic has been intensively studied for several decades. The reason for that lies in the inability to validate the proposed theoretical models in the sub-micron scale. Among the very few available methods nowadays, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) enables a highly accurate mapping of hydrogen in the microstructure in a spatial resolution below 100 nm. In the present work ToF-SIMS was used as a main tool in order to investigate the effect of deuterium on a duplex microstructure of lean and standard DSSs during and after the electrochemical charging process. Electrochemical charging simulates the service of a component in acidic environments under conditions of cathodic protection that are commonly applied to prevent corrosion reactions. ToF-SIMS after multivariate data analysis (MVA) was combined with high resolution topographic images and electron back-scattered diffraction (EBSD) data to characterize the structural changes. It was observed that the ferritic phase was affected almost identical in all steels whereas in the austenitic phase significant differences were obtained in the lean duplex in comparison to the standard DSS. The obtained results have been compared to similar investigations on a AISI 304L austenitic stainless steel. The advantage of the combined techniques is reflected by the ability to correlate the hydrogen distribution in the microstructure and the resulted phase transformation. T2 - Third International Conference on Metals & Hydrogen CY - Ghent, Belgien DA - 29.05.2018 KW - Data-fusion KW - ToF-SIMS KW - PCA KW - DSS KW - LDX KW - EBSD PY - 2018 AN - OPUS4-45094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Eliezer, D. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Novel approach to image hydrogen distribution and related phase transformation in duplex stainless steels at the sub-micron scale N2 - The effect of electrochemical charging of hydrogen on the structure of a lean duplex stainless steel LDX 2101® (EN 1.4162, UNS S32101) was examined by both Time-of-Flight secondary ion mass spectrometry and electron back-scatter diffraction. The goal is to correlate hydrogen concentration and induced structural changes. Chemical and structural characterizations were done for the same region at the sample's surface with sub-micron spatial resolution. Regions of interest were varying in size between 50 × 50 μm and 100 × 100 μm. The results show a phase transformation of austenite to mainly a defect-rich BCC and scarcely a HCP phase. The phase transformation occurred in deuterium rich regions in the austenite. KW - Time-of-flight secondary ion mass spectrometry KW - ToF-SIMS KW - Electron backscatter diffraction KW - EBSD KW - Hydrogen-assisted cracking KW - Data fusion KW - Lean duplex stainless steel PY - 2017 DO - https://doi.org/10.1016/j.ijhydene.2017.08.016 SN - 0360-3199 VL - 42 IS - 39 SP - 25114 EP - 25120 AN - OPUS4-42022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meinderink, D. A1 - Kielar, C. A1 - Sobol, Oded A1 - Ruhm, L. A1 - Rieker, F. A1 - Nolkemper, K. A1 - Orive, A. G. A1 - Özcan Sandikcioglu, Özlem A1 - Grundmeier, G. T1 - Effect of PAA-induced surface etching on the adhesion properties of ZnO nanostructured films N2 - Zinc oxide - polymer interfaces are known to exhibit interesting properties regarding molecular adhesion. This work is aimed at the investigation of the effect of the morphology and surface chemistry on the macroscopic adhesion of a model epoxy-based adhesive to nanorod (ZnO NR) and nanocrystalline (ZnO NC) ZnO-modified surfaces. Both ZnO films have been prepared using hydrothermal synthesis on hot-dip galvanized steel (HDG) surfaces by varying the precursor chemistry in order to control the film morphology. Poly (acrylic acid) (PAA) was used to improve the interfacial adhesion by modifying the morphology and surface chemistry of ZnO nanostructured films. The strong interaction of PAA from a dilute and neutral aqueous solution with the ZnO nanocrystallites was shown to significantly improve the interfacial adhesion by means of a nanoetching process. It was shown that the wet peel-forces correlate well with the considered morphology and surface chemistry. KW - Interfacial stability KW - Morphology control KW - Poly(acrylic acid) KW - Adhesion by mechanical interlocking KW - ZnO films KW - ZnO nanorods Nanocrystalline PY - 2021 DO - https://doi.org/10.1016/j.ijadhadh.2021.102812 SN - 0143-7496 VL - 106 SP - 102812 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-52600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Comprehensive study of deuterium-induced effects in in austenitic stainless steel AISI 304L N2 - The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed. To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place. By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules. KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Deuterium KW - Martensite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477540 DO - https://doi.org/10.1016/j.ijhydene.2019.03.058 SN - 0360-3199 SN - 1879-3487 VL - 44 IS - 23 SP - 12228 EP - 12238 PB - Elsevier Ltd. AN - OPUS4-47754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Celorrio, V. A1 - Stockmann, Jörg Manfred A1 - Sobol, Oded A1 - Sun, Z. A1 - Wang, W. A1 - Lawrence, M. J. A1 - Radnik, Jörg A1 - Russel, A. E. A1 - Hodoroaba, Vasile-Dan A1 - Huang, L. A1 - Rodriguez, P. T1 - Surface galvanic formation of Co-OH on Birnessite and its catalytic activity for the oxygen evolution reaction N2 - Low-cost, high-efficient catalysts for water splitting can be potentially fulfilled by developing earthabundant metal oxides. In this work, surface galvanic formation of Co-OH on K0.45MnO2 (KMO) was achieved via the redox reaction of hydrated Co2+ with crystalline Mn4+. The synthesis method takes place at ambient temperature without using any surfactant agent or organic solvent, providing a clean, green route for the design of highly efficient catalysts. The redox reaction resulted in the formation of ultrathin Co-OH nanoflakes with high electrochemical surface area. X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS) analysis confirmed the changes in the oxidation state of the bulk and surface species on the Co-OH nanoflakes supported on the KMO. The effect of the anions, such as chloride, nitrate and sulfate, on the preparation of the catalyst was evaluated by electrochemical and spectrochemical means. XPS and Time of flight secondary ion mass spectrometry (ToF-SIMS) analysis demonstrated that the layer of CoOxHy deposited on the KMO and its electronic structure strongly depend on the anion of the precursor used during the synthesis of the catalyst. In particular, it was found that Cl- favors the formation of Co-OH, changing the rate-determining step of the reaction, which enhances the catalytic activity towards the OER, producing the most active OER catalyst in alkaline media. KW - Nanoparticles KW - Oxygen evolution reaction (OER) KW - Catalysis KW - ToF-SIMS KW - XPS KW - K-rich Birnessite (K0.45MnO2) PY - 2021 DO - https://doi.org/10.1016/j.jcat.2021.02.025 VL - 396 SP - 304 EP - 314 PB - Elsevier Inc. AN - OPUS4-52328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - In-situ elucidation of Deuterium flux in 2205 duplex stainless steel by secondary ion mass spectrometry T2 - SIMS Europe 2014 CY - Münster, Germany DA - 2014-09-07 PY - 2014 AN - OPUS4-31398 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Sobol, Oded T1 - Hydrogen assisted cracking and transport studied by ToF-SIMS and data fusion with HR-SEM N2 - For almost 150 years it is known that hydrogen has a deleterious effect on the mechanical properties of metallic components. Nowadays, the problem of hydrogen assisted degradation is highly relevant in energy related fields due to the massive use of steel as a structural component in these applications and its sensitivity to hydrogen. Since the discovery of hydrogen assisted cracking (HAC), researchers studied intensively and suggested possible explanations and mechanisms in order to define how hydrogen is affecting the material. In general, it is considered that hydrogen changes the mechanical properties more in terms of ductility (deformation capacities) than in strength (load capacities). Hydrogen concentration is one of three crucial factors in the degradation process, together with the microstructure of the material and the internal/external mechanical load. The relatively high concentration of hydrogen resulting in this loss of ductility can originate during production or before service (e.g. welding processes) and during service (i.e. catholically protected systems to eliminate corrosion processes in sour environments). In parallel to the theoretical work, tremendous efforts were, and are still, invested in searching for a proper method to elucidate, map and quantify the hydrogen in the microstructure, which is the basis for this work. For steels, the focus is mainly on the observations of diffusion processes and the interaction of hydrogen with the microstructure in regions with high local stresses/strains (for example around evolving cracks). The challenge for reaching this goal arises from the fact that accurate indication of hydrogen by means of position, unlike heavier atoms, can be made only by mass spectrometry or by interaction with another element (e.g. silver decoration, special coating and resonant nuclear reaction by nitrogen). In addition to this, the difficulty recording the hydrogen behavior while it rapidly diffuses through the material, leaving only the unpredicted failure, should be taken into account. Although using powerful characterization methods, models and computational simulations, the key to defining the mechanisms behind HAC is still under debate and not fully understood. The relationship between material and hydrogen is determined by three factors, i.e., the material structure and microstructure – determining the physical properties, the mechanical load applied on the material and the hydrogen concentration. It is well known that in order to have a complete definition of HAC these three factors must be examined locally with the minimal scale and the maximal resolution reachable. The major gap is the lack in such a characterization method or a technique by which one has the ability to detect and observe the hydrogen in the metallic microstructure. The commonly used techniques nowadays are capable of characterization of the microstructure without the ability to observe the hydrogen distribution. Global hydrogen concentration and localized hydrogen observation are possible by some techniques which are incapable of indicating a change in the structure or microstructure therefore a comprehensive overview can be gained only by combining several methods. In the presented research, secondary ion mass spectrometry (SIMS) was adopted as the main tool to detect and locally map the hydrogen distribution in two types of duplex stainless steel grades: EN 1.4462 (standard 2205 duplex stainless steel) and EN 1.4162 (2101 lean duplex stainless steel). The term duplex stainless steel (DSS) refers to the austenitic-ferritic microstructure of the steel where the combination of physical and mechanical properties of the two phases is achieved. The DSS was selected as a case study for this work due to the wide use of this grade in many energy and the lack of knowledge on hydrogen behavior in two-phase containing microstructures. ToFSIMS was exploited in-situ and ex-situ in three experimental approaches during or following an electrochemical charging procedure. This type of hydrogen charging was selected as it simulated a procedure of cathodic protection of most sub-water oil and gas extraction and delivery systems. The experimental procedures were: 1. Ex-situ charging followed by ToF-SIMS imaging for basic understanding of hydrogen distribution. 2. Ex-situ charging followed by in-situ mechanical loading to obtain information on hydrogen behavior around a propagating crack. 3. In-situ permeation of hydrogen through a steel membrane inside the ToF-SIMS to obtain information on diffusion behavior of hydrogen in a two-phase microstructure. The comprehensive view of the effect of hydrogen on steel was gained by using supplementary methods, such as high resolution scanning electron microscopy (HR-SEM), focused ion beam (FIB) and electron back-scattered diffraction (EBSD). The state of the art in this work lies in applying both: in-situ experimental approaches and data treatment of the ToF-SIMS raw data. The data treatment includes the combination of data from several sources (data fusion). The results for the ex-situ charging followed by static sample imaging and data fusion showed that when the analyzed surface is directly exposed to the electrolyte the degradation is pronounced differently in the ferrite, austenite and interface. The degradation mechanisms in the ferrite and austenite were reflected by the formation of cracks on the surface of both, where a high concentration of hydrogen was obtained. This result supports the assumption that hydrogen is attracted to highly deformed regions. The advantage of using in-situ charging/permeation in comparison to ex-situ charging is that the effect of hydrogen on the ferrite and austenite phases when the hydrogen is evolving from within the microstructure is realized, in comparison to when the analyzed surface is initially exposed directly to the electrolyte. In both experiments the ferrite was observed as a fast diffusion path for the hydrogen. The faster diffusion of hydrogen through the ferrite is expected due to the higher diffusion coefficient, however, a direct proof for the diffusion sequence in this scale was never shown. Most significant results were achieved by the ‘core’ experiments of this research. These experiments included the design of a novel dynamic mechanical loading device to apply an external load during SIMS imaging of a hydrogen precharged-notched sample. For the first time it was shown that plastic deformation induced by applying a mechanical load is resulting in a redistribution of hydrogen locally around the notch. T3 - BAM Dissertationsreihe - 160 KW - Duplex stainless steels KW - Hydrogen assisted cracking KW - Time-of-Flight secondary ion mass spectrometry KW - Data fusion PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-447331 SN - 1613-4249 VL - 160 SP - I EP - 180 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-44733 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 - 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 - Nietzke, Jonathan A1 - Konert, Florian A1 - Poka, Konstantin A1 - Merz, Benjamin A1 - Sobol, Oded A1 - Böllinghaus, Thomas T1 - Comparison of hydrogen effects on additively manufactured and conventional austenitic steels N2 - Hydrogen and its derivatives are promising energy carriers for future renewable energy supplies. Austenitic stainless steels, such as AISI 316L, are commonly used in hydrogen transportation systems. While often thought to be resistant to hydrogen embrittlement, studies have shown that 316L is susceptible under certain conditions. As demand for hydrogen applications grows, additive manufacturing (AM) technologies offer design flexibility and customisation benefits. However, data on AM parts behaviour in hydrogen environments is lacking. This study investigates the influence of hydrogen on mechanical properties using slow strain rate testing (SSRT) on conventional AISI 304L, 316L and AM 316L specimens. The results indicate a greater effect of hydrogen on 304L compared to 316L, with AM 316L showing increased susceptibility. However, the ductility of AM 316L remains comparable to conventional 316L due to its initial ductility. The study provides insights into the performance of conventional and AM austenitic stainless steels in gaseous hydrogen environments. KW - Slow strain rate testing KW - Hollow specimen KW - Hydrogen embrittlement KW - Additive manufacturing KW - Austenitic steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615919 DO - https://doi.org/10.1016/j.engfailanal.2024.109042 SN - 1350-6307 VL - 167 SP - 1 PB - Elsevier B.V. AN - OPUS4-61591 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 - JOUR A1 - Konert, Florian A1 - Nietzke, Jonathan A1 - Grimault de Freitas, Tomás A1 - Rhode, Michael A1 - Sobol, Oded A1 - Böllinghaus, Thomas T1 - Investigation of resistance to gaseous hydrogen of a longitudinal weld seam in a X65 pipeline using the hollow specimen technique N2 - The constantly increasing demand for renewable energy sources leads to the necessity of transporting large amounts of hydrogen. Since pipelines enable a cost-effective way for the distribution of gaseous hydrogen, the interaction of hydrogen and the pipeline materials must be carefully investigated as hydrogen can cause a degradation of the mechanical properties under certain conditions. Especially welds, which are assumed to be more susceptible to the degradation enhanced by hydrogen, are of great interest. The aim of this study is to investigate the effect of gaseous hydrogen on the mechanical properties of an X65 pipeline, and the longitudinal submerged arc welding (SAW) welded joint. The tests are conducted using the hollow specimen technique on two types of specimens: one extracted from the base material (BM) and the other extracted as a cross-weld (CW) specimen consisting of BM and weld seam. The specimens are charged in situ under a pressure of 60 bar and tested using slow strain rate (SSR) tensile tests with a nominal strain rate of 10−5 s−1. The properties obtained of specimens tested in hydrogen atmosphere are compared to the properties of comparable specimen in inert argon atmosphere as a reference. The performed tests showed a decrease of the reduction of area (RA) from 72% in inert atmosphere to 52% in hydrogen atmosphere for the CW specimen and a decrease from 73% in inert atmosphere to 51% for the BM. Metallographic analyses showed the crack initiation between fine-grained heat-affected zone (FGHAZ) and BM for the specimens tested in hydrogen atmosphere as well as for the reference specimens. This leads to the conclusion that the location of the crack initiation does not change due to the presence of gaseous hydrogen. KW - Hydrogen KW - Hollow specimen technique KW - Pipeline KW - SSRT KW - Hydrogen embrittlement KW - Cross-weld specimen PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624658 DO - https://doi.org/10.1007/s40194-025-01953-3 SN - 0043-2288 SN - 1878-6669 VL - 69 IS - 3 SP - 861 EP - 870 PB - Springer CY - Berlin AN - OPUS4-62465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Straub, F. A1 - Wirth, Thomas A1 - Holzlechner, G. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Real Time Imaging of Deuterium in a Duplex Stainless Steel Microstructure by Time-of-Flight SIMS N2 - For more than one century, hydrogen assisted degradation of metallic microstructures has been identified as origin for severe technical component failures but the mechanisms behind have not yet been completely understood so far. Any in-situ observation of hydrogen transport phenomena in microstructures will provide more details for further elucidation of these degradation mechanisms. A novel experiment is presented which is designed to elucidate the permeation behaviour of deuterium in a microstructure of duplex stainless steel (DSS). A hydrogen permeation cell within a TOF-SIMS instrument enables electrochemical charging with deuterium through the inner surface of the cell made from DSS. The outer surface of the DSS permeation cell exposed to the vacuum has been imaged by TOF-SIMS vs. increasing time of charging with subsequent chemometric treatment of image data. This in-situ experiment showed evidently that deuterium is permeating much faster through the ferrite phase than through the austenite phase. Moreover, a direct proof for deuterium enrichment at the austenite-ferrite interface has been found. KW - Characterization and analytical techniques KW - Corrosion KW - Imaging technique KW - Mass spectrometry PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-353872 UR - http://www.nature.com/articles/srep19929 DO - https://doi.org/10.1038/srep19929 SN - 2045-2322 VL - 6 IS - 19929 SP - 1 EP - 7 PB - nature publishing group CY - London, United Kingdom AN - OPUS4-35387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Holzlechner, Gerald A1 - Nolze, Gert A1 - Wirth, Thomas A1 - Eliezer, D. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging of deuterium assisted cracking in a 2205 duplex stainless steel microstructure N2 - In the present work, the influence of deuterium on the microstructure of a duplex stainless steel type EN 1.4462 has been characterized by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) supported by scanning electron microscopy (SEM), focused ion beam (FIB), electron back scattered diffraction(EBSD) and energy dispersive x-ray (EDX) investigations. Characterization has been carried out before and after electrochemical charging with deuterium which has been used as a tracer, due to its similar behavior to hydrogen in the steel microstructure. In a first approach, the distribution of the deuterium occurring at temperatures above 58 °C has been visualized. Further it turned out that sub-surface micro blisters are formed in the ferrite-austenite interface, followed by the formation of needle shaped plates and subsequent cracking at the ferrite surface. In the austenite phase, parallel cracking alongside twins and hexagonal close packed (martensitic) regions has been observed. In both phases and even in the apparent interface, cracking has been associated with high deuterium concentrations, as compared to the surrounding undamaged microstructure. Sub-surface blistering in the ferrite has to be attributed to the accumulation and recombination of deuterium at the ferrite-austenite interface underneath the respective ferrite grains and after fast diffusing through this phase. Generally, the present application of chemometric imaging and structural analyses allows characterization of hydrogen assisted degradation at a sub-micron lateral resolution. KW - ToF-SIMS KW - Hydrogen assisted cracking KW - Hydrogen embrittlement KW - SEM KW - FIB KW - EBSD PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S0921509316310334 DO - https://doi.org/10.1016/j.msea.2016.08.107 SN - 0921-5093 VL - 676 SP - 271 EP - 277 PB - Elsevier B.V. AN - OPUS4-37298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shikomba, Nikanor A1 - Böllinghaus, Thomas A1 - Konert, Florian A1 - Sobol, Oded A1 - Blasón Gonzalez, Sergio A1 - Ohijeagbon, Idehai Olayemi A1 - Krafft, Eike A1 - Staudt, Thorsten T1 - Resistance of welded low-alloyed pressure vessel and pipeline steels in gaseous hydrogen N2 - Green hydrogen has become an essential energy carrier to achieve a climate-neutral economy. The production, storage, transport and usage of green hydrogen require safe and sustainable facilities and systems. The present contribution provides a procedure guideline to investigate the compatibility of steel welds for pressurised gaseous hydrogen applications under quasi-static mechanical loads, utilising the slow strain rate test and hollow specimen technique. Exemplarily, a weld of the low-alloyed steel P355NL1 was investigated and compared to an X65 weld. The results indicate that the base metal exhibits a higher ductility than the weld metal for both steels. Generally, hydrogen-exposed specimens exhibited a reduced strain, as compared to reference specimens. The hydrogen degradation, evaluated by the hydrogen embrittlement index, was more pronounced in the weld metal compared to the base P355NL1 material, whereas the X65 exhibited a larger hydrogen degradation of the base material than in the weld metal. Fractographic analysis of the test specimens revealed that hydrogen causes a transition from ductile to brittle features. Generally, the results of this study indicate a mild but significant degradation of the mechanical properties in terms of the ductility of the welds in the respective pressurised hydrogen atmosphere. KW - Hydrogen-assisted cracking KW - Welded joint KW - Slow strain rate test KW - Hollow Specimen KW - Structural steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634138 DO - https://doi.org/10.1007/s40194-025-02074-7 SN - 0043-2288 SP - 1 EP - 15 PB - Springer CY - Berlin AN - OPUS4-63413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - BAM’s role in materials science and hydrogen in metals: TOF-SIMS imaging N2 - Due to its low mass and high diffusivity in presence of compositional, thermal and mechanical gradients, hydrogen within a metallic microstructure can result in severe loss in ductility even at low concentrations and might lead eventually to a catastrophic and unpredictable failure of structural components during service. In this context, hydrogen mapping at the microscale is still considered among the most important challenges on the pathway towards a better understanding of the hydrogen transport and assisted cracking phenomena in metals, specifically in structural components, e.g. steels. Among the very few available techniques to localize hydrogen at the microscale, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. Based on the assumption that deuterium influence the microstructure similarly to hydrogen, in the following contribution ToF-SIMS was applied as the main technique to detect and locally map the deuterium distribution in several alloys: lean 2101 and standard 2205 duplex stainless steel (DSS), AISI 304L austenitic stainless steel and titanium 6Al-4V alloy. These alloys were selected as case studies in this work due to the wide use of them in many applications and environments which frequently provide critical conditions for hydrogen absorption and assisted degradation. The innovative design of in-situ and ex-situ experiments enabled us to elucidate the permeation, transport and trapping of deuterium in the microstructure in sub-micron resolution for the first time. In addition to the novel experimental setups, further progress was gained by applying computational multivariate data analysis (MVA) on the raw data and data fusion with high resolution structural characterization methods (scanning electron microscopy and electron back-scattered diffraction – SEM/EBSD). This combination allowed us to correlate the deuterium distribution and the influence on the microstructure. T2 - 4th Symposium on Innovative Measurement and Analysis for Structural Materials CY - Tokyo, Japan DA - 13.11.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - Austenitic stainless steel KW - Principal Component Analysis KW - Data-fusion PY - 2018 UR - https://unit.aist.go.jp/tia-co/project/SIP-IMASM/sympo/2018/index.html AN - OPUS4-46867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - 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 - Röhsler, Andreas A1 - Sobol, Oded A1 - Hänninen, H. A1 - Böllinghaus, Thomas T1 - In-situ ToF-SIMS analyses of deuterium re-distribution in austenitic steel AISI 304L under mechanical load N2 - Hydrocarbons fuel our economy. Furthermore, intermediate goods and consumer products are often hydrocarbon-based. Beside all the progress they made possible, hydrogen-containing substances can have severe detrimental effects on materials exposed to them. Hydrogen-assisted failure of iron alloys has been recognised more than a century ago. The present study aims to providing further insight into the degradation of the austenitic stainless steel AISI 304L (EN 1.4307) exposed to hydrogen. To this end, samples were electrochemically charged with the hydrogen isotope deuterium (2H, D) and analysed by scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). It was found that deuterium caused a phase transformation from the original γ austenite into ε- and α’-martensite. Despite their low solubility for hydrogen, viz. deuterium, the newly formed phases showed high deuterium concentration which was attributed to the increased density of traps. Information about the behaviour of deuterium in the material subjected to external mechanical load was gathered. A four-point-bending device was developed for this purpose. This allowed to analyse in-situ pre-charged samples in the ToF-SIMS during the application of external mechanical load. The results indicate a movement of deuterium towards the regions of highest stress. KW - ToF-SIMS KW - Hydrogen KW - Deuterium KW - AISI 304L KW - EBSD PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505142 DO - https://doi.org/10.1038/s41598-020-60370-2 VL - 10 IS - 1 SP - 3611 PB - Nature AN - OPUS4-50514 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 - TY - JOUR A1 - Konert, Florian A1 - Wieder, Frank A1 - Nietzke, Jonathan A1 - Meinel, Dietmar A1 - Böllinghaus, Thomas A1 - Sobol, Oded T1 - Evaluation of the impact of gaseous hydrogen on pipeline steels utilizing hollow specimen technique and μCT N2 - The high potential of hydrogen as a key factor on the pathway towards a climate neutral economy, leads to rising demand in technical applications, where gaseous hydrogen is used. For several metals, hydrogen-metal interactions could cause a degradation of the material properties. This is especially valid for low carbon and highstrength structural steels, as they are commonly used in natural gas pipelines and analyzed in this work. This work provides an insight to the impact of hydrogen on the mechanical properties of an API 5L X65 pipeline steel tested in 60 bar gaseous hydrogen atmosphere. The analyses were performed using the hollow specimen technique with slow strain rate testing (SSRT). The nature of the crack was visualized thereafter utilizing μCT imaging of the sample pressurized with gaseous hydrogen in comparison to one tested in an inert atmosphere. The combination of the results from non-conventional mechanical testing procedures and nondestructive imaging techniques has shown unambiguously how the exposure to hydrogen under realistic service pressure influences the mechanical properties of the material and the appearance of failure. KW - Energy Engineering and Power Technology KW - Condensed Matter Physics KW - Fuel Technology KW - Renewable Energy, Sustainability and the Environment KW - µCT KW - Hollow Specimen Technique KW - Hydrogen Embrittlement PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595077 DO - https://doi.org/10.1016/j.ijhydene.2024.02.005 SN - 0360-3199 VL - 59 SP - 874 EP - 879 PB - Elsevier B.V. AN - OPUS4-59507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steiner, S. A1 - Heldt, J. A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Frömeling, T. T1 - Influence of oxygen vacancies on core-shell formation in solid solutions of (Na,Bi)TiO3 and SrTiO3 N2 - Solid solutions of (Na,Bi)TiO3 (NBT) and SrTiO3 (ST) are materials of interest for high-strain or high-energy density capacitor applications. Often, they exhibit chemical heterogeneity and develop core-shell structures during regular solid-state synthesis with an NBT-rich core. In this case, the NBT forms first so that the strontium needs to diffuse into the material to reach chemical homogeneity. Depending on the presence of core-shell structures, the electrical properties can vary drastically. In this work, we rationalize the effect of variations in oxygen vacancy concentration by Fe-acceptor and Nb-donor doping. It can be shown that a diffusion couple of strontium and oxygen is responsible for chemical homogenization and that the oxygen vacancy content can control the formation of a core-shell structure. KW - Lead-free ceramics KW - Bismuth titanates KW - Core-shell structures KW - Diffusion/diffusivity KW - Ferroelectricity/ferroelectric materials PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525988 DO - https://doi.org/10.1111/jace.17845 SP - 1 EP - 10 PB - Wiley Periodicals LLC, John Wiley & Sons, Inc. AN - OPUS4-52598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - The characterization of oxygen diffusion in (Na1/2Bi1/2)TiO3 piezo-ceramics by Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) N2 - The ferroelectric ceramic NBT and its solid solutions with barium titanate (BT) are examples for the most promising lead free materials to substitute the dominant Pb(Zr,Ti)O3 (PZT). Lead based material should generally be disregarded due to environmental and health reasons. However, there is no class of lead-free piezoelectric materials that can replace PZT entirely. Not only the often inferior ferroelectric properties but also the lack of understanding of the defect chemistry of NBT is still a challenge for the replacement of lead containing piezo-ceramics. Just recently it could be shown by Li et al. that NBT obtains extraordinarily high oxygen ionic conductivity when doped with Mg as acceptor. It was actually expected that doping just leads to a hardening of the ferroelectric properties. However, it became clear that the known defect chemical behavior of PZT cannot be extrapolated to NBT materials. Hence, to gain information on general doping effects a better defect chemical investigation is needed. This is particularly important for the applications with high reliability demands to investigate possible degradation and fatigue mechanisms. In the present work Time-of-flight-secondary ion mass spectrometry (ToF-SIMS) was used in order to observe the influence of different acceptor dopants (Fe, Ni, Al) on the oxygen diffusion in NBT. ToF-SIMS holds the ability to gain a full elemental distribution in a sub-micron resolution and was therefore chosen to provide the essential information on the favorable diffusion paths of oxygen in NBT in dependence of the chosen doping element. 18O was used as a tracer for oxygen as its natural abundance is only 0.2%. The doped NBT samples have been annealed for 5 h at 500°C in a 0.2 bar 18O-tracer atmosphere to be able to detect oxygen ion diffusion. ToF-SIMS investigations were conducted on a ToF-SIMS IV (ION TOF GmbH, Münster, Germany) using a Bi+ primary ion beam (25KeV in collimated burst alignment mode with a beam diameter of ~150 nm) and a Cs+ sputter beam (3KeV). The results illustrate the different impact of dopants on the diffusion properties which is evidence for a highly non-linear dependence on dopant type and concentration. T2 - 21st International Conference on Secondary Ion Mass Spectrometry - SIMS21 CY - Krakow, Poland DA - 10.09.2017 KW - ToF-SIMS KW - NBT KW - Piezoceramics PY - 2017 UR - http://sims.confer.uj.edu.pl/boa_poster.php?id=93 AN - OPUS4-42911 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 - 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 - Sobol, Oded T1 - Sputtering derived artefacts in austenitic steel during Time-of-Flight Secondary Ion Mass Spectrometry analyses N2 - Among the very few techniques to localize hydrogen (H) at the microscale in steels, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. The necessity to detect hydrogen stems from its deleterious effects in metals, that are often used as structural components and to obtain better understanding of the underlying metallurgical mechanisms of hydrogen embrittlement (HE) which are still unclear. Austenitic stainless steels are nowadays commonly used in a wide variety of application, from hydrogen transport and storage facilities to petrochemical and offshore applications where they are exposed to aggressive environments and therefore prone to HE. One of the greater risks in the austenitic class is the embrittlement of the material due to the instability of the γ austenite and its transformation into a brittle α martensitic phase. This transformation takes place due to the local stresses that are induced by the uptake of hydrogen during service. Nonetheless, it was shown that this transformation can occur as an artefact during SIMS analysis itself where Cs-sputtering is necessary not only to remove surface contaminations but mainly to enhance H/D secondary ion yield. In the following contribution we show the influence of different sputtering conditions on AISI 304L austenitic stainless steel in order to distinguish the artefact from the hydrogen induced transformation. The material was charged electrochemically in a deuterium based electrolyte. Deuterium (D) must be in these experiments as a replacement for hydrogen which cannot be used because adsorbed hydrogen superimposes hydrogen originating from charging the sample in the SIMS images. ToF-SIMS analyses were conducted by ToF SIMS IV (IONTOF GmbH, Münster, Germany). The experiments were carried out on deuterium charged and non-charged samples. The structural characterization was carried out by SEM and EBSD examinations before and after charging, both with a Leo Gemeni 1530VP field-emission scanning electron microscope and a Zeiss Supra 40 instrument (Carl Zeiss Microscopy GmbH, Oberkochen, Germany). The results showed that the use of 1keV Cs+ beam induces stacking faults while higher sputter beam energies results in γ→α transformation. T2 - SIMS Europe 2018 CY - Münster, Germany DA - 16.09.2018 KW - Austenitic steel KW - Hydrogen KW - ToF-SIMS KW - Artefact PY - 2018 AN - OPUS4-46701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Challenges with metallic materials in hydrogen technologies N2 - The contribution was presented in the Joint European Summer School in Athens as part of several contributions from BAM in the field of hydrogen safety. These presentations are given in order to provide an overview about the activities of BAM as part of the competence center H2Safety@BAM T2 - JOINT EUROPEAN SUMMER SCHOOL (JESS) CY - Athens, Greece DA - 12.09.2022 KW - Gaseous hydrogen KW - Hydrogen Embrittlement KW - Hydrogen assisted cracking PY - 2022 AN - OPUS4-55822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wurzler, Nina A1 - Sobol, Oded A1 - Altmann, Korinna A1 - Radnik, Jörg A1 - Özcan Sandikcioglu, Özlem T1 - Preconditioning of AISI 304 stainless steel surfaces in the presence of flavins—Part I: Effect on surface chemistry and corrosion behavior N2 - Stainless steel AISI 304 surfaces were studied after a mild anodic polarization for oxide growth in the presence and absence of two derivatives of vitamin B2 (riboflavin and flavin mononucleotide) that can be secreted by metal‐reducing bacteria and act as a chelating agent for iron species. The alterations in oxide chemistry were studied by means of surface‐sensitive techniques such as X‐ray photoelectron spectroscopy and time‐of‐flight secondary ion mass spectrometry analysis. The complementary electrochemical characterization revealed a preferential growth of an oxide/hydroxide iron‐rich film that is responsible for an altered pit initiation and nucleation behavior. These findings suggest that as the corrosion behavior is determined by the interplay of the chemical and electronic properties, only a mild anodic polarization in the presence of redox‐active molecules is able to alter the chemical and electronic structure of the passive film formed on stainless steel AISI 304. This helps to achieve a profound understanding of the mechanisms of microbially influenced corrosion (MIC) and especially the possible effects of the redox‐active biomolecules, as they may play an important role in the corrosion susceptibility of stainless steel surfaces. KW - Corrosion KW - Stainless steel KW - Surface analysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528117 DO - https://doi.org/10.1002/maco.202012191 VL - 72 IS - 6 SP - 974 EP - 982 PB - Wiley AN - OPUS4-52811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ekici, Nilsah A1 - Sobol, Oded T1 - SHIMMER Database for Hydrogen Integration in European Gas Grids N2 - The integration of hydrogen into existing natural gas infrastructure is an important pathway for achieving the European Union’s climate neutrality goals. However, hydrogen blending in gas networks raises technical challenges related to material compatibility, operational safety, and the lack of harmonized assessment methodologies across Europe. These challenges are addressed within the Safe Hydrogen Injection Modelling and Management for European Gas Network Resilience (SHIMMER) project, funded by the Clean Hydrogen Partnership under the Horizon Europe programme. A key outcome of the project is the development of an openly accessible database designed to support the assessment of hydrogen readiness in European gas networks and to facilitate knowledge sharing. The database compiles infrastructure data provided by project partners, including several European transmission and distribution system operators. It contains detailed information on gas network components such as pipelines, valves, fittings, gaskets, and compressors. In addition, a new category has been introduced focusing on the hydrogen compatibility of gas grid components and materials. This section provides structured information linking infrastructure components with material types and their hydrogen compatibility, enabling more systematic evaluation of hydrogen injection scenarios. By organizing heterogeneous datasets into a harmonized and user-friendly structure, the SHIMMER database supports research, best-practice development, and the safe integration of hydrogen into existing European gas infrastructure. T2 - EHEC 2026 CY - Seville, Spain DA - 11.03.2026 KW - Database KW - Gas Grid KW - Hydrogen KW - Low-carbon KW - Pipeline Steel PY - 2026 AN - OPUS4-65683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -