TY - JOUR A1 - Markwart, J. C. A1 - Battig, Alexander A1 - Urbaniak, T. A1 - Haag, K. A1 - Koschek, K. A1 - Schartel, Bernhard A1 - Wurm, F. R. T1 - Intrinsic flame retardant phosphonate-based vitrimers as a recyclable alternative for commodity polymers in composite materials N2 - Recycling of crosslinked fiber-reinforced polymers is difficult. Moreover, as they are often based on flammable resins, additional additives are needed. So-called “vitrimers” open the possibility of Recycling and reprocessing and repairing with dynamically crosslinked chemistries. To date, vitrimer-based composites still need flame retardant additives, such as organophosphates. An additive-free vitrimer composite has not been reported. Herein, we synthesized an intrinsic flame-retardant vitrimer, relying on vinylogous polyurethanes containing covalently installed phosphonates as flame-retardant units and prepared glassfiber-reinforced composites. We studied recycling and flame retardant properties and compared the data to phosphorus-free vitrimers and conventional epoxy resins (with and without additive flame retardant). Our phosphonate-based vitrimer proved in first tests, a flame retardant effect comparable to commercial flame retardant resins. The bending strength and bending modulus for the phosphorus-vitrimer glass fiber composites were comparable to glass fiber composites with permanently cross-linked epoxies. In summary, we were able to prove that the covalent installation of phosphonates into vitrimers allows the preparation of recyclable and intrinsic flame retardant composites that do not need flame retardant additives. We believe this concept can be expanded to other polymer networks and additives to generate recyclable and sustainable high-performance materials. KW - Vitrimer KW - Flame retardant KW - Recyclable KW - Organophosphonate KW - Polyurethane PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510889 DO - https://doi.org/10.1039/d0py00275e VL - 11 IS - 30 SP - 4933 EP - 4941 AN - OPUS4-51088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Marschall, Niklas A1 - Niebergall, Ute A1 - Wachtendorf, Volker A1 - Böhning, Martin T1 - Characteristics of environmental stress cracking of PE-HD induced by biodiesel and diesel fuels N2 - In the context of the increasing effect of carbon dioxide emissions on the global climate biodiesel produced from renewable sources has emerged as a promising contender replacing fossil fuels, especially in long-range transport vehicles, using existing engines and infrastructure. High-density polyethylene is one of the prevailing materials for pipe and container applications for storage and transport of such fuels, both, from fossil and renewable resources. The contact with the respective fuels raises questions concerning material compatibility as biodiesel exhibits significant differences compared to conventional diesel fuel affecting its sorption and plasticization behavior in polyethylene. In this study, its behavior with respect to environmental stress cracking, considered one of the most frequent damage mechanisms leading to failure of polymer parts and packaging, was evaluated using the well-established Full Notch Creep Test. This approach allows for a detailed fracture surface analysis using imaging techniques, such as optical and laser scanning microscopy, as well as infrared spectroscopy. Comparing the environmental stress cracking behavior in standard surfactant solutions with that in biodiesel and diesel, respective crack propagation rates, showing different levels of acceleration, were determined and details of the underlying mechanisms could be revealed. Furthermore, the specific infrared absorption of the biodiesel’s ester functionality allows its semi-quantitative determination on the fracture surface of the tested specimens after failure. Thus, a preferred uptake of sorptive fluids in the fracture zone due to local morphological changes of the polyethylene could be directly evidenced by infrared spectroscopy. KW - Environmental stress cracking (ESC) KW - Full notch creep test (FNCT) KW - Confocal laser scanning microscopy (LSM) KW - Biodiesel KW - Diesel PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608591 DO - https://doi.org/10.1016/j.polymertesting.2024.108547 SN - 0142-9418 VL - 138 SP - 1 EP - 16 PB - Elsevier Ltd. AN - OPUS4-60859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, Xiangmeng A1 - Bachmann, Marcel A1 - Yang, Fan A1 - Rethmeier, Michael T1 - Toward prediction and insight of porosity formation in laser welding: A physics-informed deep learning framework N2 - The laser welding process is an important manufacturing technology for metallic materials. However, its application is often hindered by the occurrence of porosity defects. By far, an accurate prediction of the porosity defects and an insight into its formation mechanism are still challenging due to the highly nonlinear physics involved. In this paper, we propose a physics-informed deep learning (PIDL) framework by utilizing mechanistic modeling and experimental data to predict the porosity level during laser beam welding of aluminum alloys. With a proper selection of the physical variables (features) concerning the solidification, liquid metal flow, keyhole stability, and weld pool geometry, the PIDL model shows great superiority in predicting the porosity ratio, with a reduction of mean square error by 41 %, in comparison with the conventional DL model trained with welding parameters. Furthermore, the selected variables are fused into dimensionless features with explicit physical meanings to improve the interpretability and extendibility of the PIDL model. Based on a well-trained PIDL model, the hierarchical importance of the physical variables/procedures on the porosity formation is for the first time revealed with the help of the Shapley Additive Explanations analysis. The keyhole ratio is identified as the most influential factor in the porosity formation, followed by the downward flow-driven drag force, which offers a valuable guideline for process optimization and porosity minimization. KW - Laser beam welding KW - Physics-informed deep learning KW - Porosity prediction KW - Feature fusion KW - Hierarchical importance PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624708 DO - https://doi.org/10.1016/j.actamat.2025.120740 VL - 286 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-62470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilhelm, Eugen A1 - Mente, Tobias A1 - Rhode, Michael T1 - Waiting time before NDT of welded offshore steel grades under consideration of delayed hydrogen-assisted cracking N2 - Offshore wind turbines (OWT) are a major goal of the energy strategy of Germany encompassing the increase of the installed wind power. OWT components are manufactured from welded steel plates with thicknesses up to 200 mm. The underlying standards and technical recommendations for construction of OWTs encompass specifications of so-called minimum waiting time (MWT) before non-destructive testing of the weld joints is allowed. Reason is the increased risk of time-delayed hydrogen assisted cold cracking as hydrogen diffusion is very slow due to the very thick plates. The strict consideration of those long MWT up to 48 h during the construction of OWTs leads to significant financial burden (like disproportionately high costs for installer ships as well as storage problems (onshore)). In this study, weld joints made of S355 ML were examined in comparison with the offshore steel grade S460 G2+M. The aim was to optimize, i.e., reduce, the MWT before NDT considering varied heat input, hydrogen concentration and using self-restraint weld tests. This would significantly reduce the manufacturing time and costs of OWT construction. To quantify the necessary delay time until hydrogen-assisted cold cracks appear, acoustic emission analysis was applied directly after welding for at least 48 h. KW - Hydrogen KW - Welding KW - Cracking KW - Offshore KW - Steel PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524959 DO - https://doi.org/10.1007/s40194-020-01060-5 SN - 0043-2288 VL - 65 SP - 947 EP - 959 PB - Springer Nature AN - OPUS4-52495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Czeskleba, Denis A1 - Nietzke, Jonathan A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Investigation of stress relief crack susceptibility of CrMoV steels coarse grain HAZ via simulation of uniaxial stress conditions during PWHT N2 - Creep-resistant steels such as the 13CrMoV9-10, used in the construction of thick-walled pressure vessels, are most commonly submerged arc welded (SAW). These steels can develop stress relief cracks (SRC) if the mandatory post weld heat treatment (PWHT) is performed improperly. Current PWHT parameters, such as heating rate and holding time at a specific holding temperature, are based on both empirical experience and conventional free shrinking welding experiments to characterize the SRC-susceptibility of the weld. These cannot adequately depict the higher residual stresses caused by the structurally induced stiffness of the surrounding construction. This study discusses the development of a repeatable, precise, and time-efficient methodology to study the effects of different stress levels and heating rates on the SRC susceptibility of the coarse grain heat-affected zone (CGHAZ). For that purpose, samples were thermically treated to simulate a coarse grain heat-affected zone (CGHAZ) and subsequently exposed to representative levels of stress during the heating phase of a PWHT. The recorded stress and heating rate–dependent strains were mathematically analyzed via curve tracing/calculus to identify interdependent effects. This procedure facilitates the measurement of material characteristics such as carbide growth on grain boundaries at the µm-scale via an integrated value over the entire sample volume. The first and second derivatives show a slight, precipitate-dependent, increase in hardness of the sample, depending on the heating rate and applied stress. This new methodology generates an improved assessment of the SRC susceptibility of SAW microstructures of creep-resistant CrMoV steels. KW - Submerged arc welding KW - Creep-resistant steel KW - Stress relief cracking KW - Component-like test KW - Post weld heat treatment PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576007 DO - https://doi.org/10.1007/s40194-023-01539-x SN - 0043-2288 SP - 1 EP - 9 PB - Springer Nature CY - Basel (CH) AN - OPUS4-57600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Kromm, Arne A1 - Mente, Tobias A1 - Brackrock, Daniel A1 - Czeskleba, Denis A1 - Kannengießer, Thomas T1 - Component test for the assessment of delayed hydrogen-assisted cracking in thick-walled SAW joints for offshore applications N2 - Offshore wind turbines continuously increase in size and weight and demand adequate offshore foundations concepts like monopiles, tripods, or jackets. These components are typically constructed using submerged arc welding (SAW) with high-strength thick steel plates like the S420ML. During welding, the occurrence of delayed hydrogen-assisted cracking (HAC) must be anticipated. HAC is a critical combination of the local hydrogen concentration within a susceptible microstructure under certain mechanical load, i.e., the occurring (welding) residual stresses. The welding sequence of the thick-walled plates complicates the residual stress distribution due to the necessary repeated thermal cycling, i.e., welding seam/layer deposition to fill the joint. For that purpose, SAW with two-wire-technique was used to weld a specially designed and prototype-like mock-up of a real component with a thickness of 50 mm, filled with over 20 passes and a seam length of 1000 mm. Additional welded stiffeners simulated the effect of a high restraint, to achieve critical HAC conditions. The necessity of a minimum waiting time (MWT) before the NDT can be conducted (to exclude HAC) was critically verified by the application of ultrasonic testing of the welded joint at different time-steps of the NDT of up to 48 h after the completion welding. The residual stresses were determined by a robot XRD goniometer. Tensile residual stresses up to the yield limit are found both in the weld metal and in the heat-affected zone. Numerical modeling allowed the qualitative estimation of the hydrogen diffusion in the weld. No noticeable HAC occurrence was identified and confirms the high cracking resistance of the investigated material. Finally, the applicability of the MWT concept should be critically discussed. KW - Hydrogen KW - Cold cracking KW - Minimum Waiting Time KW - Offshore steel grade KW - Component test PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591981 DO - https://doi.org/10.1007/s40194-023-01658-5 SP - 1 EP - 15 PB - Springer Science and Business Media LLC AN - OPUS4-59198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröpfer, Dirk A1 - Witte, Julien A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Stresses in repair welding of high-strength steels—part 1: restraint and cold cracking risk N2 - AbstractThe sustainable and resource-efficient production of wind energy plants requires the use of modern high-strength fine-grain structural steels. This applies to both foundation and erection structures, like mobile or ship cranes. During the assembly of steel structures, unacceptable defects can occasionally be found in the weld area. In most cases, the economical solution would be local thermal gouging of the affected areas and re-welding. Due to the high shrinkage restraint of the joint groove in the overall structure, the superposition of global and local welding-induced stresses may lead to crack formation and component failure, particularly in interaction with the degradation of the microstructure and mechanical properties of high-strength steels during the repair process. However, manufacturers hardly have any information about these issues and there is a lack of recommendations and guidelines to take these safety-relevant aspects into account in adequate repair concepts. The aim of this research is to derive recommendations for repair concepts appropriate to the stresses and materials involved providing a basis for standards and guidelines to avoid cold cracking, damage and expensive reworking especially for high-strength steels. Part 1 of this study involves systematic investigations of influences of shrinkage restraint during repair welding of two high-strength steels S500MLO for offshore application and S960QL for mobile crane structures. The quantification of the shrinkage restraint of repair weld joints was achieved by means of experimental and numerical restraint intensity analysis. In welding experiments with self-restrained slot specimens, restraint intensity and introduction of hydrogen via the welding arc using anti spatter spray were varied systematically to analyse the effect on welding result, residual stresses and cold cracking. It could be shown that increasing restraint intensities result in significantly higher transverse residual stress levels. In the case of hydrogen introduction S500MLO showed no cold cracking independent of the restraint conditions. However, S960QL was found to be considerably cold cracking sensitive if hydrogen is introduced. With increasing restraint intensity length and number of cold cracks increases significantly. Part 2 [1] of this study is focussed on microstructure and residual stresses due to gouging and stress optimization via adequate heat control parameters in repair welding. KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595212 DO - https://doi.org/10.1007/s40194-024-01691-y SN - 0043-2288 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-59521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudziak, Mateusz A1 - Bhatia, Riya A1 - Dey, R. A1 - Falkenhagen, Jana A1 - Ullrich, M. S. A1 - Thomsen, C. A1 - Schartel, Bernhard T1 - Wastewater phosphorus enriched algae as a sustainable flame retardant in polylactide N2 - Revolutionizing our polymer industry for adaption to a sustainable carbon circular economy has become one of today’s most demanding challenges. Exploiting renewable resources to replace fossil-fuel—based plastics with biopolymers such as poly(lactic acid) (PLA) is inevitable while using waste streams as a raw material resource at least is promising. When it comes to using PLA as technical polymer, its high flammability must be addressed by flame retardants compatible with the thermoplastic processing of PLA and its compostability. This study proposes microalgae enriched with phosphorus from wastewater (P-Algae) as an elegant way towards a kind of sustainable organophosphorus flame retardant. The concept is demonstrated by investigating the processing, pyrolysis, flammability, and fire behavior of PLA/P-Algae, while varying the P-Algae content and comparing P-Algae with four alternative bio-fillers (phosphorylated lignin, biochar, thermally treated sewage sludge, and metal phytate) with different P-contents as meaningful benchmarks. KW - PLA KW - Flame Retardancy KW - Phosphorylated Algae KW - Wastewater flame retardants KW - Zink phytate KW - Phosphorylated lignin KW - Thermally treated sludge PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604150 DO - https://doi.org/10.1016/j.polymdegradstab.2024.110885 SN - 1873-2321 SN - 0141-3910 VL - 227 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-60415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Schweißen im Wasserstoffanlagen- und Behälterbau - Eine Kurzübersicht N2 - Wasserstoff erfüllt die zentrale Rolle für die Umwandlung der bisherigen fossil-basierten Energieerzeugung und -nutzung auf eine dekarbonisierte, nachhaltige Form. Dazu muss der Wasserstoff erzeugt, gespeichert, transportiert werden, bevor er wieder der Nutzung zugeführt wird. Hierzu sind entlang der gesamtem Prozesskette Wasserstofftechnologien notwendig, die einen sicheren Betrieb erfordern. Hierbei kommt dem schweißtechnischen Anlagen- und Behälterbau wesentliche Bedeutung zu, insbesondere (aber nicht ausschließlich) für Speicherung und Transport des Wasserstoffes. Der vorliegende Beitrag gibt einen kurzen Überblick, wo und wie die konventionelle Schweißtechnik hierzu wichtige Beiträge leistet. Die additive Fertigung, also das „Drucken“ von Bauteilen wird dabei zunehmend wichtiger, entlang der gesamtem Prozesskette der Wasserstofftechnologien. Gleichwohl darf nicht unterschätzt werden, dass auch wesentlicher Bedarf an der Erweiterung und teilweiser Neufassung von bestehenden Regel- und Normenwerken besteht. T2 - 51. Sondertagung "Schweißen im Behälter- und Anlagenbau" CY - Munich, Germany DA - 01.03.2023 KW - Wasserstoff KW - Anlagenbau KW - Schweißen KW - Studie KW - Pipeline PY - 2023 SN - 978-3-96144-219-5 VL - 387 SP - 83 EP - 88 PB - DVS Media GmbH CY - Düsseldorf AN - OPUS4-57075 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hallier, Dorothea C. A1 - Smales, Glen Jacob A1 - Seitz, H. A1 - Hahn, Marc Benjamin T1 - Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine N2 - Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. KW - BioSAXS KW - Bio-SAXS KW - Cosolute KW - Ectoine KW - G5P KW - GVP KW - Radiation damage KW - Radical Scavenger KW - Single-stranded DNA-binding proteins KW - X-ray scattering KW - DNA KW - ssDNA KW - Protein KW - SAXS KW - Small-angle xray scattering KW - McSAS3 KW - Dosimetry KW - Microdosimetry KW - Geant4 KW - Geant4-DNA KW - Topas KW - Topas-MC KW - Monte-Carlo simulations KW - Particle scattering simulations KW - Topas-nBio KW - OH Radical KW - OH radical scavenger KW - LEE KW - Ionizing radiation damage KW - Protein unfolding KW - Ectoin PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568909 DO - https://doi.org/10.1039/d2cp05053f SN - 1463-9076 SN - 1463-9084 VL - 25 IS - 7 SP - 5372 EP - 5382 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-56890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Richter, Tim A1 - Mente, Tobias A1 - Mayr, P A1 - Nitsche, A T1 - Hydrogen effect on mechanical properties and cracking of creep‑resistant 9% Cr P92 steel and P91 weld metal N2 - Martensitic 9% Cr steels like P91 and P92 can show an increased susceptibility to delayed hydrogen-assisted cracking. The focus of this study was the microstructure and heat treatment efect on the mechanical properties of P92 base material and P91 multi-layer weld metal in both as-welded and post weld heat treated (PWHT) condition. Tensile tests with hydrogen free reference samples and electrochemically hydrogen charged samples were carried out; the mechanical properties were assessed and supported by detailed fractographic analysis. Finally, a hydrogen and microstructure-dependent fracture criterion is established. All investigated microstructures showed a hydrogen-infuenced degradation of the mechanical properties compared to the hydrogen-free reference samples. The as-welded martensitic P91 weld metal had the highest degree of degradation in the presence of hydrogen. The P91 PWHT weld metal and the P92 base material had comparable properties. From that point of view, a signifcantly increased risk for hydrogen-assisted cold cracking during welding fabrication of P91 weld joints must be considered before any heat treatment is conducted. T2 - IIW Annual Assembly, Meeting of Commission IX-C CY - Tokyo, Japan DA - 16.07.2022 KW - Creep-resisting materials KW - Welding KW - Hydrogen assisted cracking KW - Hydrogen embrittlement KW - Mechanical properties PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564070 DO - https://doi.org/10.1007/s40194-022-01410-5 SN - 0043-2288 SP - 1 EP - 12 PB - Springer Nature CY - Basel (CH) AN - OPUS4-56407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Weber, Kathrin A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Elucidation of orientation relations between Fe-Cr alloys and corrosionproducts after high temperature SO2 corrosion N2 - The early stages of corrosion of Fe-Cr-model alloys (2 and 9 % Cr) were investigated after exposure at 650 °C in0.5 % SO2containing gas by electron backscattered diffraction (EBSD) and transmission electron microscopy(TEM). The impact of the grain orientation of the base alloy on the orientation relations of the corrosion productsis presented. After 2 min–5 min exposure the formation of a multi-layered corrosion zone was discovered. Aclear orientation relationship between ferrite and the (Fe,Cr)3O4 spinel could be demonstrated. The obtainedresults show the importance of the grain orientation on oxidation resistance. KW - Iron KW - TEM KW - SEM KW - High temperature corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508911 DO - https://doi.org/10.1016/j.corsci.2020.108809 VL - 174 SP - 1 EP - 11 PB - Elsevier AN - OPUS4-50891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drexler, A.-K. A1 - Konert, Florian A1 - Nietzke, Jonathan A1 - Hodžić, E. A1 - Pastore, S. A1 - Domitner, J. A1 - Rhode, Michael A1 - Sommitsch, C. A1 - Böllinghaus, Thomas T1 - Effect of Tensile Loading and Temperature on the Hydrogen Solubility of Steels at High Gas Pressure N2 - The hydrogen solubility in ferritic and martensitic steels is affected by hydrostatic stress, pressure, and temperature. In general, compressive stresses decrease but tensile stresses increase the hydrogen solubility. This important aspect must be considered when qualifying materials for high‐pressure hydrogen applications (e.g., for pipelines or tanks) by using autoclave systems. In this work, a pressure equivalent for compensating the effect of compressive stresses on the hydrogen solubility inside of closed autoclaves is proposed to achieve solubilities that are equivalent to those in pipelines and tanks subjected to tensile stresses. Moreover, it is shown that the temperature effect becomes critical at low temperatures (e.g., under cryogenic conditions for storing liquid hydrogen). Trapping of hydrogen in the microstructure can increase the hydrogen solubility with decreasing temperature, having a solubility minimum at about room temperature. To demonstrate this effect, the generalized law of the hydrogen solubility is parameterized for different steels using measured contents of gaseous hydrogen. The constant parameter sets are verified and critically discussed with respect to the high‐pressure hydrogen experiments. KW - Hydrogen KW - Solubility KW - Temperature KW - Tensile loading KW - Analytical calculation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586701 DO - https://doi.org/10.1002/srin.202300493 SN - 1611-3683 SP - 1 EP - 9 PB - Wiley AN - OPUS4-58670 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, Maha A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Erroneous or Arrhenius: A Degradation Rate-Based Model for EPDM during Homogeneous Ageing N2 - To improve the predictive capability of long-term stress relaxation of elastomers during thermo-oxidative ageing, a method to separate reversible and irreversible processes was adopted. The separation is performed through the analysis of compression set after tempering. On the Basis of this separation, a numerical model for long-term stress relaxation during homogeneous ageing is proposed. The model consists of an additive contribution of physical and chemical relaxation. Computer simulations of compression stress relaxation were performed for long ageing times and the results were validated with the Arrhenius treatment, the kinetic study and the time-temperature superposition technique based on experimental data. For chemical relaxation, two decay functions are introduced each with an activation energy and a degradative process. The first process with the lower activation energy dominates at lower ageing times, while the second one with the higher activation energy at longer ageing times. A degradation-rate based model for the evolution of each process and ist contribution to the total system during homogeneous ageing is proposed. The main advantage of the model is the possibility to quickly validate the interpolation at lower temperatures within the range of slower chemical processes without forcing a straight-line extrapolation. KW - Kinetic study KW - Arrhenius KW - TTS KW - Modeling KW - Chemical processes KW - Stress relaxation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512931 DO - https://doi.org/10.3390/polym12092152 SN - 2073-4360 VL - 12 IS - 9 SP - 1 EP - 21 AN - OPUS4-51293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, Maha A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Understanding the recovery behaviour and the degradative processes of EPDM during ageing N2 - Recovery is an important measure for seal applications representing to which extent the elastomer regains its initial shape after deformation and release of an applied force. Compression set (CS) indicates the degree of recovery. Ethylene propylene diene rubber (EPDM) was aged at 75 ◦C, 100 ◦C, 125 ◦C and 150 ◦C for different ageing times up to five years and compression set measurements were performed at different times after disassembly and after additional tempering. Short- and long-term recovery up to one year after release for samples aged at 125 ◦C and 150 ◦C was also studied. To assess the curvature in the Arrhenius diagram that may occur due to non-sufficiently aged specimens, a degradation-rate based model was fitted to the CS data after tempering. For each ageing temperature, two decay fit functions were proposed, each with an activation energy and a corresponding degradative process. The influence of ageing on the leak-tightness after fast small partial release is investigated and estimated through the analysis of the shift factors from time temperature superposition (TTS) of CS measurements at different times after disassembly. Shift factors of CS measurement after 1 s and after additional tempering are in good agreement. KW - Compression set KW - Ageing KW - Recovery KW - Degradative processes KW - Leakage rate PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573699 DO - https://doi.org/10.1016/j.polymertesting.2023.107987 SN - 0142-9418 VL - 121 SP - 107987 PB - Elsevier Ltd. AN - OPUS4-57369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vega Puga, E. A1 - Wachtendorf, Volker A1 - Kömmling, Anja A1 - Brendelberger, S. A1 - Jaunich, Matthias A1 - Sattler, C. T1 - Lifetime prediction and degradation assessment of FKM and FFKM O-rings under high temperature thermo-oxidative ageing N2 - To support the development of solar reactor technologies for hydrogen production, this study investigates the thermo-oxidative degradation mechanisms of fluorinated elastomers and predicts their lifetimes at high temperatures (200–300 ◦C) consistent with the application requirements. An accelerated ageing programme is conducted with FKM and FFKM O-rings and flat samples for up to 21 days. Optical microscopy is used to analyse the exposed seals’ morphological changes, while IR microscopy is utilised to investigate the underlying chemical degradation mechanisms of both elastomers. Findings suggest that FKM’s degradation arises from dehydrofluorination of the polymer, followed by chain scission and backbone cleavage as a result of the oxidation of newly formed C=C double bonds. FFKM’s degradation is primarily associated with chain scission, but there is also indication that post-curing processes may occur during material ageing. Furthermore, hardness, equilibrium compression set (CS), continuous compression stress relaxation (CSR) and leakage rate tests are used to evaluate changes in the mechanical properties and sealing performance of the elastomers. Equilibrium CS data is extrapolated using time-temperature shifts (TTS) and used to derive an end-of-life criterion of 75 % equilibrium CS, which correlates to leakage rates higher than a predetermined threshold. Service lifetime predictions of FKM and FFKM O-rings at several temperatures are performed and a seal operating temperature of 200 ◦C is suggested, which ensures reasonable O-ring replacement intervals of more than half a year in the solar reactor for both considered materials. KW - Fluoroelastomer KW - Perfluoroelastomer KW - Thermo-oxidative ageing KW - Lifetime prediction KW - Compression set PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630112 DO - https://doi.org/10.1016/j.polymertesting.2025.108820 SN - 1873-2348 VL - 147 SP - 1 EP - 17 PB - Elsevier BV CY - Amsterdam AN - OPUS4-63011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wetzel, Annica A1 - Hans, Ann-Kathrin A1 - von der Au, Marcus A1 - Brand, Izabella A1 - Wittstock, Gunther A1 - Özcan Sandikcioglu, Özlem A1 - Witt, Julia T1 - Long-term corrosion studies of CrCoNi and CrMnFeCoNi in sulfuric acid N2 - This study investigates the long-term corrosion behavior of CrCoNi and CrMnFeCoNi MPEAs over 28 d in 1 M H2SO4. Corrosion progression and passive film evolution were analyzed using open circuit potential measurements, electrochemical impedance spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy. Unlike short-term polarization tests, where CrCoNi exhibited intergranular corrosion, long-term immersion resulted in a stable, Cr-rich passive oxide layer. In contrast, CrMnFeCoNi formed a porous mixed oxide layer, increasing its susceptibility to degradation and revealing a distinct corrosion mechanism. X-ray photoelectron spectroscopy tracking at weekly intervals showed that prolonged immersion led to the transformation of sulfide/sulfite species into a sulfate-containing surface film. This effect was only detectable in long-term corrosion studies. These findings provide new insights into the time-dependent degradation mechanisms of MPEAs and demonstrate that corrosion mechanisms differ significantly from short-term polarization tests. This highlights the need for long-term studies to properly assess material stability in practical applications. KW - Long-term corrosion KW - Multi-principal element alloys (MPEAs) KW - X-ray photoelectron spectroscopy (XPS) PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636895 DO - https://doi.org/10.1038/s41529-025-00637-z SN - 2397-2106 VL - 9 IS - 1 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-63689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wallis, Theophilus A1 - Darvishi Kamachali, Reza T1 - Grain boundary structural variations amplify segregation transition and stabilize co-existing spinodal interfacial phases N2 - Grain boundaries (GBs)’s role in determining the functional and mechanical properties of polycrystalline materials is inscribed in both their structure and chemistry. Upon solute segregation, the structure and composition of a GB can change concurrently. We study the co-evolution of GB’s structure and segregation by enhancing the density-based phase-field model to account for the in-plane structural variations in the GB. Significant mutual coupling is revealed between the GB’s chemical and structural states during Mn segregation in Fe-Mn alloys. We found that the structural degrees of freedom in a GB (the ability of the GB structure to respond to the chemical variation) amplifies Mn segregation transition, even when the GB structure stays unchanged. When the GB structure is not uniform, that is the usual case, the coupling between GB structure and segregation evolution also enables the spinodally formed low- and high-Mn phases (upon segregation transition) to co-exist within the GB region. These findings explain the stabilizing mechanism of pronounced interfacial segregation fluctuations, experimentally evidenced in Fe-Mn GBs, and give new insights on the structural sensitivity of GBs’ segregation phenomena and the mutual chemo-structural interplay. KW - Grain boundary engineering KW - Segregation engineering KW - Grain boundary structure KW - Fe-Mn steels PY - 2022 DO - https://doi.org/10.1016/j.actamat.2022.118446 SN - 1359-6454 VL - 242 PB - Elsevier Ltd. AN - OPUS4-56160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stohl, Leonie A1 - Manninger, Tanja A1 - von Werder, Julia A1 - Dehn, F. A1 - Gorbushina, Anna A1 - Meng, Birgit T1 - Bioreceptivity of concrete - A review N2 - Materials that support natural biodiversity on their surfaces can compensate for human activities that have a negative impact on nature and thus contribute to a carbon-neutral and nature-positive world. Specifically designing bioreceptive materials which favor the growth of biofilms on their surface is an approach complementing conventional, macroscopic green façades. But what exactly characterizes a bioreceptive substrate and how do biofilm and substrate interact? How and why does a spontaneous colonization and the formation of biofilms take place? What are biofilms and how can they be established in a laboratory setting? How can this existing knowledge be transferred to the artificial stone concrete so that this material can be tuned to increase (or decrease) its bioreceptivity? This review paper aims at summarizing the existing state of knowledge on bioreceptive concrete and pointing out inconsistencies and contradictions which can only be removed by more interdisciplinary research in the field. KW - Bioreceptivity KW - Biofilm KW - Green facades KW - Developing building materials KW - Surface interactions KW - Concrete PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581685 DO - https://doi.org/10.1016/j.jobe.2023.107201 SN - 2352-7102 VL - 76 SP - 1 EP - 17 PB - Elsevier AN - OPUS4-58168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -