TY - JOUR A1 - Mege-Revil, Alexandre A1 - Rapontchombo-Omanda, Jessie A1 - Serrano Munoz, Itziar A1 - Cristol, Anne-Lise A1 - Magnier, Vincent A1 - Dufrenoy, Philippe T1 - Sintered Brake Pads Failure in High-Energy Dissipation Braking Tests: A Post-Mortem Mechanical and Microstructural Analysis N2 - The industrial sintering process used to produce metallic matrix pads has been altered to diminish the amount of copper used. Unfortunately, replacing a large part of the copper with iron seems to have reached a limit. In the high-energy, emergency-type rail braking used in this study, the materials are put to the very limit of their usage capacity, allowing us to observe the evolution of the microstructure and mechanical properties of sintered, metallic matrix pads. After the braking test, their compressive behaviour was assessed using digital image correlation (DIC), and their microstructure with scanning electron microscopy (SEM). The worn material has three flat layers with different microstructures and compressive behaviours. The bo􀁇om layer seems unmodified. Macroscopic and microscopic cracks run through the intermediate layer (2–15 mm depth). The top layer has stiffened thanks to resolidification of copper. The temperature reaches 1000 °C during the braking test, which also explains the carbon diffusion into iron that result in the weakening of iron–graphite interfaces in the pad. Finally, submicronic particles are detected at many open interfaces of the worn and compressed pad. Associated with the predominant role of graphite particles, this explains the weak compressive behaviour of the pads. KW - Friction braking KW - Sintering KW - Metallic matrix pad KW - Microstructure KW - Scanning electron microscopy (SEM) KW - Compressive test KW - Cracks KW - Digital image correlation (DIC) KW - Diffusion PY - 2023 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-587318 SN - 1996-1944 VL - 16 IS - 21 SP - 1 EP - 18 PB - MDPI AN - OPUS4-58731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Steurer, Florian T1 - Diffusion in high-pressure hydrogen charged multi-principal element alloys CoCrFeMnNi and CoCrNi vs. AISI 316L N2 - Multi-principal element alloys (MPEAs) are innovative materials that have attracted extensive research attention within the last decade. MPEAs are characterized by a solid solution of equiatomic metallic elements. Depending on the number of elements, they are also referred as high entropy alloys (HEAs with n ≥ 4 elements like CoCrFeMnNi) and medium-entropy alloys (MEA with n = 3 elements CoCrNi). Depending on the alloy concept, MPEAs show exceptional properties in terms of mechanical performance or corrosion resistance at extreme environments. In that connection, hydrogen and its challenges for the most metallic materials gets more and more important. MPEAs are candidate materials for the substitution of conventional materials like austenitic stainless steels e.g., at very high-pressure up to 1000 bar. Those pressures are typically reached in valves or compressors for refueling of tanks with operational pressure of 700 bar. So far, the susceptibility of HEA/MEAs to hydrogen assisted cracking (if any) and the especially the underlying hydrogen uptake and diffusion was not within the scientific scope and not investigated in detail yet. For that reason, we focused on the hydrogen absorption the characterization of the hydrogen diffusion and trapping at elevated temperatures in a CoCrFeMnNi-HEA (each element with 20 at.-%) and CoCrNi-MEA, each element with 33.3 at.-%). As reference grade, the commercially available austenitic stainless steel AISI 316L was investigated. High-pressure hydrogen charging was conducted at different pressures in autoclave environment with maximum value of 1,000 bar. Thermal desorption analysis (TDA) via carrier gas hot extraction with coupled mass spectrometry was used with a max. heating rate of 0.5 K/s up to 650 °C. The measured desorption spectra of the different samples were deconvoluted into a defined number of individual peaks. The individually calculated peak temperatures allowed the definition of activation energies for predominant trap sites in the respective materials as well as the percentage share of the totally absorbed hydrogen concentration. The results present for the first time the complex interaction of both MPEAs and high-pressure hydrogen charging. A deconvolution of four peaks was selected and a main desorption peak was identified the dominant hydrogen trap containing the biggest share of the absorbed hydrogen concentration. The chemical composition an austenitic phase of both MPEAs is responsible for delayed hydrogen diffusion and strong, but mostly reversible, trapping. The comparison with the 316L samples showed significantly higher activation energies in the MPEAs, whereas hydrogen was also trapped at very high extraction temperatures. The absorbed maximum hydrogen concentration at 1,000 bar was 130 ppm for the CoCrFeMnNi-HEA, 50 ppm for the CoCrNi-MEA and 80 ppm for the 316L. It is interesting that the CoCrFeMnNi-HEA has obviously a way higher trapping capability compared to the conventional austenitic 316L, which could be a major advantage in terms of resistance to hydrogen assisted cracking. T2 - 47th MPA-Seminar CY - Stuttgart, Germany DA - 10.10.2023 KW - High-entropy alloy KW - Hydrogen KW - Diffusion KW - Thermal desorption analysis KW - Multiple-principal element alloy PY - 2023 AN - OPUS4-58675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nietzke, Jonathan A1 - Rhode, Michael A1 - Mente, Tobias A1 - Kannengießer, Thomas T1 - Experimental and numerical characterization of hydrogen diffusion in thick-walled submerged arc welded joint of S420G2+M offshore steel grade N2 - Offshore wind turbines are an important goal in national energy strategies worldwide. Foundation structures are manufactured from submerged arc welded (SAW) plates with thicknesses up to 200 mm. In that connection, high-strength steels like the S420G2+M are more and more applied offering the possibility for increased stability and load-bearing capacity of the foundations. These offshore steel grades can show a susceptibility for delayed hydrogen assisted cold cracking of the weld joints. For that purpose, a minimum waiting time (MWT) of up to 48 h (dependent on applied standards) is recommended before non-destructive testing is allowed and conducted. But this concept is based on older steel grades that have been used for three or more decades. Nowadays, the metallurgical improvements (clean steels, proper rolling, and heat treatment) of base materials and well as welding consumables must be anticipated. Hence, the MWT concept should be critically discussed as it is assumed to be very conservative. For that reason, the focus of this study was to investigate the diffusion behavior in S420G2+M steel and its multi-layer SAW joint. Electrochemical permeation experiments were carried at room temperature. Boundary conditions were anticipated in terms of using different sample thicknesses. From the experimental data, hydrogen diffusion coefficients and absorbed diffusible hydrogen concentrations had been calculated. It was shown that hydrogen diffusion in the base material is increased compared to the weld metal. In addition, the sample thickness had a significant on the calculated diffusion coefficients. The minimum and maximum diffusion coefficients had been used for numerical modelling of the hydrogen diffusion in the welding joint. It became clear that a MWT must be always regarded together with a critical initial diffusible hydrogen concentration for the evaluation of a possible delayed cracking as diffusion times were mostly > 48 h due to the thick plates. T2 - 4th International Conference on Metals and Hydrogen - Steely & Hydrogen 2022 CY - Ghent, Belgium DA - 11.10.2022 KW - Hydrogen KW - Submerged arc welding KW - Diffusion KW - Minimum waiting time KW - Electrochemical permeation PY - 2022 SP - 1 EP - 11 CY - Ghent, Belgium AN - OPUS4-56075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Richter, Tim T1 - Hydrogen diffusion and desorption characteristics of a CoCrFeMnNi high entropy and a CoCrNi medium entropy alloy N2 - High-entropy alloys (HEAs) are innovative high-performance materials that have attracted more and more research attention. HEAs are characterized by a solid solution of typically five equiatomic metallic elements. In addition, medium-entropy alloys (MEA, with three elements) are of interest and become more and more important. Depending on the alloy concept, HEAs and MEAs show exceptional mechanical properties, especially high-strength and ductility combinations at both cryogenic and elevated temperatures combined with excellent corrosion resistance. Future structural HEA/MEA components can be exposed to potential applications with hydrogen containing environments like high-temperature water in pressurized nuclear reactors or aerospace structures. Other potential applications could be in materials for vessel walls in the field of cryogenic and high-pressure hydrogen storage. So far, the susceptibility of HEAs/MEAs to hydrogen assisted cracking (if any) and the hydrogen diffusion is not investigated in detail yet and can limit or extend possible applications of HEA/MEA as structural materials. In our work, we focused on the hydrogen absorption, diffusion, and distribution in a HEA (CoCrFeMnNi the original Cantor-alloy) and a MEA (CoCrNi). Cathodic hydrogen charging was carried out for the hydrogen ingress, and thermal desorption analysis (TDA) revealed complex hydrogen trapping in both alloy types up to 300 °C. The absorbed total hydrogen concentrations were > 100 ppm for the HEA and > 40 ppm for MEA. In addition, the assessment of the peak deconvolution is not trivial and must consider both experimental and microstructure influences. T2 - 4th International Conference on Metals and Hydrogen - Steely & Hydrogen 2022 CY - Ghent, Belgium DA - 11.10.2022 KW - Hydrogen KW - High-entropy alloy KW - Multiple principal element alloy KW - Thermal desorption analysis KW - Diffusion PY - 2022 SP - 1 EP - 11 CY - Ghent, Belgium AN - OPUS4-56076 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nietzke, Jonathan A1 - Rhode, Michael A1 - Richter, Tim T1 - Hydrogen diffusion and desorption characteristics of a CoCrFeMnNi high entropy and a CoCrNi medium entropy alloy N2 - Future structural components made of the novel high-entropy (HEA) or medium-entropy alloys (MEA) components can be potentially exposed to hydrogen containing environments like high-temperature water in pressurized nuclear reactors or aerospace structures. Further applications are vessels wall materials for cryogenic or high-pressure hydrogen storage. So far, the susceptibility of HEA/MEAs to hydrogen assisted cracking (if any) and the hydrogen diffusion is not investigated in detail yet and can limit or extend possible applications of HEA/MEA as structural materials. In our work, we focused on the hydrogen absorption, diffusion, and distribution in a HEA (Co20Cr20Fe20Mn20Ni20, the original Cantor-alloy) and a MEA (Co33.3Cr33.3Ni33.3). Conventional cathodic hydrogen charging was carried out for the hydrogen ingress in the materials. Thermal desorption analysis (TDA) via carrier gas hot extraction with coupled mass spectrometry revealed complex hydrogen trapping in both alloy types up to 300 °C. The absorbed total hydrogen concentrations were ≥ 70 ppm for the HEA and approximately 40 ppm for the MEA-type. Although both materials have different chemical composition, the TDA spectra were comparable. In addition, it was shown that the consideration of the sample geometry is an important influence on the sample temperature. It decreases the effective applied heating rate, which must be anticipated for each hydrogen peak after deconvolution of the spectra. This increases the activation energy and shifts the peak to lower temperatures. As a result, microstructure effects can be separated from experimental boundary conditions like the concentration gradient due to the charging process and later thermal activation. T2 - 4th International Conference on Metals and Hydrogen - Steely & Hydrogen 2022 CY - Ghent, Belgium DA - 11.10.2022 KW - High-entropy alloy KW - Diffusion KW - Hydrogen KW - Thermal desorption analysis KW - Trapping PY - 2022 AN - OPUS4-56007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Richter, Tim A1 - Mente, Tobias A1 - Mayr, P. A1 - Nitsche, A. T1 - Thickness and microstructure effect on hydrogen diffusion in creep‑resistant 9% Cr P92 steel and P91 weld metal N2 - Martensitic 9% Cr steels like P91 and P92 show susceptibility to delayed hydrogen assisted cracking depending on their microstructure. In that connection, effective hydrogen diffusion coefficients are used to assess the possible time-delay. Limited data on room temperature diffusion coefficients reported in literature vary widely by several orders of magnitude (mostly attributed to variation in microstructure). Especially P91 weld metal diffusion coefficients are rare so far. For that reason, electrochemical permeation experiments had been conducted using P92 base metal and P91 weld metal (in as-welded and heat-treated condition) with different thicknesses. From the results obtained, diffusion coefficients were calculated using to different methods, time-lag, and inflection point. Results show that, despite microstructural effects, the sample thickness must be considered as it influences the calculated diffusion coefficients. Finally, the comparison of calculated and measured hydrogen concentrations (determined by carrier gas hot extraction) enables the identification of realistic diffusion coefficients. KW - Creep-resistant steel KW - Diffusion KW - Hydrogen assisted cracking KW - Welding KW - Electrochemical permeation PY - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-540645 SN - 0043-2288 SP - 1 EP - 16 PB - Springer Nature Switzerland AG AN - OPUS4-54064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Richter, Tim A1 - Mente, Tobias A1 - Mayr, P. A1 - Nitsche, A. T1 - Thickness and microstructure effect on hydrogen diffusion in creep-resistant 9 % Cr P92 steel and P91 weld metal N2 - Martensitic 9 %-Cr steels like P91 and P92 show susceptibility to delayed hydrogen assisted cracking depending on their microstructure. In that connection, effective hydrogen diffusion coefficients are used to assess the possible time-delay. The small number of available diffusion coefficients varies already at room temperature by several orders of magnitude (mostly regarded as result of present microstructure). Especially P91 weld metal diffusion coefficients are rare so far. For that reason, electrochemical permeation experiments had been conducted using P92 base metal and P91 weld metal (in as-welded and heat-treated condition) with different thicknesses. The diffusion coefficients are calculated by two methods (time-lag and inflection point method) were performed. The results show that, despite of microstructural effects, the sample thickness must be considered as it influences the calculated diffusion coefficients. Finally, the comparison of calculated and measured hydrogen concentrations (determined by carrier gas hot extraction) enables the identification of realistic diffusion coefficients. T2 - IIW Annual Assembly, Meeting of Commission IX-C CY - Online meeting DA - 15.07.2021 KW - Creep-resistant steel KW - Diffusion KW - Electrochemical permeation KW - Hydrogen KW - Welding PY - 2021 AN - OPUS4-53048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Richter, Tim A1 - Mente, Tobias A1 - Mayr, P. A1 - Nitsche, A. T1 - Thickness and microstructure effect on hydrogen diffusion in creep-resistant 9 % Cr P92 steel and P91 weld metal N2 - Martensitic 9 %-Cr steels like P91 and P92 show susceptibility to delayed hydrogen assisted cracking depending on their microstructure. In that connection, effective hydrogen diffusion coefficients are used to assess the possible time-delay. The small number of available diffusion coefficients varies already at room temperature by several orders of magnitude (mostly regarded as result of present microstructure). Especially P91 weld metal diffusion coefficients are rare so far. For that reason, electrochemical permeation experiments had been conducted using P92 base metal and P91 weld metal (in as-welded and heat-treated condition) with different thicknesses. The diffusion coefficients are calculated by two methods (time-lag and inflection point method) were performed. The results show that, despite of microstructural effects, the sample thickness must be considered as it influences the calculated diffusion coefficients. Finally, the comparison of calculated and measured hydrogen concentrations (determined by carrier gas hot extraction) enables the identification of realistic diffusion coefficients. T2 - IIW Intermediate Meeting, Comm. IX-C "Welding of creep and heat-resistant materials" CY - Online meeting DA - 08.03.2021 KW - Hydrogen KW - Welding KW - Diffusion KW - Creep-resistant steel KW - Electrochemical permeation PY - 2021 AN - OPUS4-52239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Mente, Tobias A1 - Kannengießer, Thomas T1 - Diffusionsmessungen in UP-Mehrlagenschweißgut als effektives Tool gegen verzögerte Kaltrissbildung in Dickblechschweißungen N2 - Offshore-Windenergieanlagen bilden einen zentralen Bestandteil der zukünftigen Energieerzeugung. Hierzu notwendige Gründungs- und Turmstrukturen werden vorrangig aus UP-geschweißten Blechen aus hochfesten niedriglegierten Stählen mit Dicken bis zu 200 mm hergestellt. Die großen Blechdicken begünstigen hohe Schweißeigenspannungen und lange Diffusionswege für z. B. über den Schweißprozess eingebrachten Wasserstoff. Damit steigt das Risiko für eine wasserstoffunterstützte Kaltrissbildung (WKB) an. Zum sichereren Ausschluss von WKB in den geschweißten Komponenten wird in Abhängigkeit der Nahtgröße, Wärmeeinbringung und Stahlsorte eine Mindestwartezeit (MWZ) von bis zu 48 h empfohlen, bevor die zerstörungsfreie Prüfung durchgeführt wird. Es ist allerdings offen, ob die empfohlene MWZ zu konservativ ist. Einflüsse sind hier bspw. die schwierige Bewertung des Wasserstoffdiffusionsverhaltens im heterogenen UP-Mehrlagen-Schweißgut (SG) im Vergleich zum Grundwerkstoff (GW). Zudem sind nur sehr begrenzt H-Diffusionskoeffizienten für UP-Mehrlagen-SG als Grundlage zur Abschätzung des Zeitintervalls einer möglichen verzögerten Kaltrissbildung (somit MWZ) oder auch für Nachwärmprozeduren zur Wasserstoffreduktion (keine MWZ) verfügbar. Verlässliche H-Diffusionskoeffizienten sind daher ein adäquates Tool zur Bewertung des Risikos einer verzögerten WKB. Dieser Beitrag beschreibt Untersuchungen zur Charakterisierung der Wasserstoffdiffusionsverhalten in UP-Mehrlagen-SG eines 60 mm dicken Bleches einer Offshore-Stahlgüte. Dazu wurden Proben unterschiedlicher Dicke aus dem reinen Schweißgut extrahiert und über elektrochemische Permeation und Trägergasheißextraktion im Temperaturbereich bis 400 °C sehr interessante Ergebnisse zu den korrespondierenden Diffusionskoeffizienten erarbeitet. T2 - DVS Congress 2021 CY - Online meeting DA - 14.09.2021 KW - UP-Schweißen KW - Wasserstoff KW - Kaltriss KW - Permeation KW - Diffusion PY - 2021 SN - 978-3-96144-146-4 VL - 371 SP - 448 EP - 459 PB - DVS Media GmbH CY - Düsseldorf AN - OPUS4-53369 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Camin, B. A1 - Hansen, L. A1 - Heuser, M. A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Theisen, W. A1 - Fedelich, Bernard T1 - Refinement and Experimental Validation of a Vacancy Model of Pore Annihilation in Single-Crystal Nickel-Base Superalloys during Hot Isostatic Pressing N2 - Initially, as-cast and homogenized single crystals of nickel-base superalloy CMSX-4 are subjected to hot isostatic pressing at 1288 °C. Two series of experiments are conducted: under the same pressure of 103 MPa but with different durations, between 0.5 and 6 h, and under different pressures, between 15 and 150 MPa, but for the same time of 0.5 h. The porosity annihilation is investigated metallographically and by high-resolution synchrotron X-ray tomography. The obtained experimental results are compared with the predictions of the vacancy model proposed recently in the group. Herein, the model is further refined by coupling with X-ray tomography. The model describes the evolution of the pore arrays enclosed in the 3D synchrotron tomograms during hot isostatic pressing and properly predicts the time and stress dependences of the pore annihilation kinetics. The validated model and the obtained experimental results are used for selecting the optimal technological parameters such as applied pressure and processing time KW - Superalloys KW - HIP KW - Single-Crystal KW - Diffusion PY - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-526859 VL - 23 IS - 7 SP - 211 AN - OPUS4-52685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -