TY - JOUR A1 - Rhode, Michael A1 - Mente, Tobias A1 - Kannengießer, Thomas T1 - Parameters and challenges for reliable hydrogen determination in welded joints by carrier gas hot extraction N2 - For the hydrogen-based energy economy of tomorrow, the construction of the necessary infrastructure will play a central role. Most materials used to date, such as welded steels, can be prone to hydrogen embrittlement under certain conditions. This includes the classic delayed cold cracking during welding as well as degradation phenomena during service of components in hydrogen-containing environment. For the evaluation of any hydrogen effect, for example, on the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. In the case of weld seams, the carrier gas hot extraction (CGHE) according to ISO 3690 is meanwhile state-of-the-art. CGHE is based on accelerated hydrogen degassing due to the thermal activation of hydrogen at elevated temperatures. In addition to the quantification of hydrogen, thermal desorption analysis (TDA) with varying heating rates can be used to determine and evaluate the hydrogen trapping at microstructural defects in the material. For both techniques, experimental and metrological influences must be considered, which have a major effect on the result. For example, ISO 3690 suggests different sample geometries and minimum extraction times for CGHE. This study summarizes the results and experiences of numerous investigations at the Federal Institute for Materials Research and Testing (BAM) with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding the influence of the sample surface (polished/welded), measurement accuracy depending on the sample volume and the insufficient monitoring of the effect of PI control on the extraction temperature. A deviating extraction temperature from the target temperature can significantly falsify the measurement results. Based on the results, methods are shown which allow the desired extraction temperature to be reached quickly without physically interfering with the measuring equipment. This serves to significantly improve the reliability of the hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples is recommended for the heating procedure of choice to exclude possible undesired temperature influences before the measurement. The methods described can be transferred directly to industrial applications KW - Welding KW - Hydrogen measurement KW - ISO 3690 KW - Carrier gas hot extraction PY - 2024 DO - https://doi.org/10.37434/tpwj2024.04.01 SN - 0957-798X VL - 4 SP - 3 EP - 10 PB - International Association Welding AN - OPUS4-60071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael 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 - Richter, Tim T1 - Friction stir welding of a CoCrFeMnNi high entropy alloy compared to AISI 304 austenitic stainless steel: evolution of microstructure and mechanical properties N2 - High entropy alloys (HEA) are a new class of materials. In contrast to conventional alloys, HEA are single-phase alloys with at least five alloying elements. HEAs have enormous application potential due to (postulated) excellent structural property combinations from low to high temperatures. For HEA-application as structural materials in real components, a key issue is the suitability for joining processing. Requirements for the reliable and safe joining of these materials are crucial regarding economical component manufacture for future applications. In this context, friction stir welding (FSW) is a promising joining process due to the welding process temperature below the material melting point avoiding major issues, e. g. formation of (hard and brittle) intermetallic phases, which may have detrimental influences on the weld joint properties. This study presents elementary research about the FSW process influences on a CoCrFeMnNi-HEA with focus on the microstructure and mechanical properties. For that purpose, the FSW joint of the HEA is compared to that of an austenitic stainless steel AISI 304. The microstructures of the welds were investigated and characterized by means of light microscopy, SEM, EBSD and XRD. Hardness and tensile testing were applied to determine influences on the mechanical properties. Generally, a comparable weldability of HEA and AISI 304 in terms of metallurgical characteristics and resulting mechanical properties exhibited. For the weld joints of both materials typical characteristics regarding FSW were observed within the weld metal and thermo-mechanically influenced zone: fine-grained stirred zone with increased hardness and reduced fracture elongation compared with the respective base material. T2 - EUROMAT 2021 CY - Online meeting DA - 13.09.2021 KW - High entropy alloy KW - Friction stir welding PY - 2021 AN - OPUS4-53308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - HEA Processing - SURDIA - Current R&D at BAM N2 - This presentation summarizes the latest results on the BAM-Themenfeld project SURDIA on processing of high-entropy alloys (HEAs) at BAM. At first, the influence of machining by ultrasonic-assisted milling on the surface integrity is presented. Second, the weld processing by Tungsten Inert Gas (TIG) welding is presented and the results of the Friction Stir Welding (FSW), which is conducted at BAM for the first time. T2 - DFG SSP 2006 - Subgroup meeting on the synthesis and processing of CCAs/HEAs CY - Online meeting DA - 08.10.2021 KW - High-entropy alloy KW - Ultrasonic-assisted milling KW - Welding KW - Processing KW - Surface integrity PY - 2021 AN - OPUS4-53497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Rhode, Michael T1 - Friction stir welding of a CoCrFeMnNi high entropy alloy compared to AISI 304 austenitic stainless steel: evolution of microstructure and mechanical properties N2 - High entropy alloys (HEA) are a new class of materials. In contrast to conventional alloys, HEA are single-phase alloys with at least five alloying elements. HEAs have enormous application potential due to (postulated) excellent structural property combinations from low to high temperatures. For HEA-application as structural materials in real components, a key issue is the suitability for joining processing. Requirements for the reliable and safe joining of these materials are crucial regarding economical component manufacture for future applications. In this context, friction stir welding (FSW) is a promising joining process due to the welding process temperature below the material melting point avoiding major issues, e. g. formation of (hard and brittle) intermetallic phases, which may have detrimental influences on the weld joint properties. This study presents elementary research about the FSW process influences on a CoCrFeMnNi-HEA with focus on the microstructure and mechanical properties. For that purpose, the FSW joint of the HEA is compared to that of an austenitic stainless steel AISI 304. The microstructures of the welds were investigated and characterized by means of light microscopy, SEM, EBSD and XRD. Hardness and tensile testing were applied to determine influences on the mechanical properties. Generally, a comparable weldability of HEA and AISI 304 in terms of metallurgical characteristics and resulting mechanical properties exhibited. For the weld joints of both materials typical characteristics regarding FSW were observed within the weld metal and thermo-mechanically influenced zone: fine-grained stirred zone with increased hardness and reduced fracture elongation compared with the respective base material. T2 - Bachelor-, Master-, Doktoranden-Kolloquium CY - Magdeburg, Germany DA - 20.10.2021 KW - High Entropy Alloy KW - Friction stir welding KW - Austenitic stainless steel PY - 2021 AN - OPUS4-53608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Mente, Tobias T1 - Trapping and diffusion in high-pressure hydrogen charged CoCrFeMnNi high entropy alloy compared to austenitic steel 316L N2 - High entropy alloys (HEAs) have attracted considerable research attention as potential substitute materials for austenitic steels in high-pressure hydrogen environments. The corresponding hydrogen absorption, diffusion and trapping has received less scientific attention. Therefore, the CoCrFeMnNi-HEA was investigated and compared to an austenitic steel AISI 316L. Both were subjected to high-pressure hydrogen charging at 200 bar and 1000 bar. Thermal Desorption Analysis (TDA) was used to clarify the specific desorption behavior and hydrogen trapping. For this purpose, the underlying TDA spectra were analyzed in terms of a reasonable peak deconvolution into a defined number of peaks and the activation energies for the respective and predominant hydrogen trapping sites were then calculated. Both materials show comparable hydrogen diffusivity. However, there were significant differences in the absorbed hydrogen concentrations at both charging pressures. The calculated activation energies suggest strong hydrogen trapping in the CoCrFeMnNi-HEA. KW - High-entropy alloy KW - Hydrogen diffusion KW - Trapping KW - High-pressure charging KW - Thermal desorption analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611901 DO - https://doi.org/10.1016/j.ijhydene.2024.09.393 SN - 0360-3199 VL - 89 IS - 89 SP - 772 EP - 782 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-61190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael 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 - Richter, Tim T1 - Residual stresses in near-component specimens of a high and a medium entropy alloy due to tig and friction stir welding N2 - The new alloying concept of multi-element systems with defined entropy (HEA - High Entropy Alloy or MEA - Medium Entropy Alloy) is gaining increasing importance in materials research. Significantly improved properties or combinations of properties are shown by some HEA/MEA-systems. Thus, primarily the production and resulting microstructures of HEA as well as properties have been investigated so far. Furthermore, processing is a main issue to transfer HEA systems from the laboratory to real components. Since welding is the most important joining process for metals, it is crucial to investigate the influence of welding to guarantee component integrity. Welding leads to residual stresses, which significantly affect the component integrity. Hence, the focus of this study is the residual stress formation and distribution in a CoCrFeMnNi HEA and ternary CoCrNi MEA using two different welding processes: Tungsten Inert Gas (TIG) welding and soldi-state Friction Stir Welding (FSW). As a pathway for application of HEA in this investigation for the first-time residual stress analyses in realistic near-component specimens were performed. The residual stresses were determined by X-ray diffraction (XRD) on the surfaces of top and root weld side. The results were correlated with the local welding microstructures. The results show that both FSW and TIG generate significant tensile residual stresses on the weld surfaces in and transverse to the welding direction. In the case of FSW of the CoCrFeMnNi HEA, the longitudinal residual stresses are in the range of the yield strength of approx. 300 MPa in the weld zone. T2 - ICRS11 – 11th International Conference on Residual Stresses CY - Nancy, France DA - 27.03.2022 KW - High Entropy Alloy KW - Medium Entropy Alloys KW - Welding microstructure KW - Residual stresses PY - 2022 AN - OPUS4-55444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröpfer, Dirk A1 - Rhode, Michael T1 - Local mechanical properties of TIG dissimilar metal welded CoCrFeMnNi high-entropy alloy to austenitic steel AISI 304 N2 - Multiple principal element alloys (MPEA) encompass the well-known high entropy alloys (HEAs). MPEA/HEA represent a new class of materials consisting of at least three alloying elements, each containing 5 to 35 at.-%. This alloying concept thus differs fundamentally from conventional materials such as steel or nickel alloys. For this purpose, the alloying elements are specifically selected, and the microstructures are adjusted in a single-phase and, in some cases, multi-phase manner. In particular, conflicting goals, such as the trade-off between strength and ductility in conventional steels, are overcome. In the last 20 years, however, the focus has been on material synthesis. With the increase in available material quantities, the focus is now on pro-cessing issues such as joining and welding processes. The weldability of MPEA has received very little atten-tion so far. Experience with dissimilar metal welds (DMWs) is completely lacking but is essential for the appli-cation of these materials in combination with conventional materials. The present study presents, comprehen-sive experimental results on the weldability of MPEA-DMWs. For that purpose, a Co20Cr20Fe20Mn20Ni20 HEA in cold-rolled and heat-treated condition was joined by means of tungsten inert gas welding (TIG) with the austenitic Cr-Ni steel AISI 304. The DMWs resulted in interesting mechanical properties. They were obtained by instrumented tensile tests as well as the local deformation in the weld area by using digital image correlation (DIC) technique. A significant softening in the heat-affected zone (HAZ) of the MPEAs as well as a slightly reduced tensile strength with a significant decrease of the elongation at fracture were found. The experiments provided proof in principle of the weldability of the MPEAs for DMWs with conventional materials that ensure a corresponding capability for mechanical loading. This allows further considerations on the application of these innovative materials. T2 - IIW Annual Assembly, Meeting of Commission C-II CY - Singapore DA - 18.07.2023 KW - High-entropy alloy KW - Welding KW - Microstructure KW - Mechanical properties KW - Dissimilar metal weld PY - 2023 AN - OPUS4-57978 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 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540645 DO - https://doi.org/10.1007/s40194-021-01218-9 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 - Wetzel, Annica A1 - Oczan, Ozlem A1 - Nietzke, Jonathan A1 - Richter, Tim A1 - Schröpfer, Dirk T1 - Hydrogen diffusion and local Volta potential in high- and medium-entropy alloys N2 - High-entropy alloys (HEAs) are characterized by a solid solution of minimum five and medium-entropy alloys (MEAs) of minimum three principal alloying elements in equiatomic proportions. They show exceptional application properties, such as high-strength and ductility or corrosion resistance. Future HEA/MEA-components could be exposed to hydrogen containing environments like vessels for cryogenic or high-pressure storage where the hydrogen absorption and diffusion in these materials is of interest. In our study, we investigated the HEA Co20Cr20Fe20Mn20Ni20 and the MEA Co33.3Cr33.3Ni33.3. For hydrogen ingress, cathodic charging was applied and diffusion kinetic was measured by high-resolution thermal desorption spectros-copy using different heating rates up to 0.250 K/s. Peak deconvolution resulted in high-temperature desorption peaks and hydrogen trapping above 280 °C. A total hydrogen concentration > 40 ppm was identified for the MEA and > 100 ppm for HEA. This indicates two important effects: (1) delayed hydrogen diffusion and (2) considerable amount of trapped hydrogen that must be anticipated for hydrogen assisted cracking phenomenon. Local electrochemical Volta potential maps had been measured for the hydrogen free condition by means of high-resolution Scanning Kelvin Probe Force Microscopy (SKPFM). T2 - Symposium on Materials and Joining Technology CY - Online meeting DA - 07.09.2020 KW - Hydrogen KW - High-entropy alloy KW - Diffusion KW - Scanning kelvin probe force microscopy KW - Corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511684 DO - https://doi.org/10.1088/1757-899X/882/1/012015 VL - 882 SP - 1 EP - 15 PB - IOP Publishing CY - Bristol AN - OPUS4-51168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Rhode, Michael A1 - Börner, Andreas T1 - Influence of modern machining processes on the surface integrity of high-entropy alloys N2 - High Entropy Alloys (HEAs) are a recent class of materials. In contrast to conventional alloys, HEAs consist of five alloying elements in equiatomic equilibrium. The high entropy effect is due, among other things, to the increased configuration entropy, which promotes solid solution formation. Many HEAs have enormous application potential due to excellent structural property combinations from very low to high temperatures. For the introduction of HEAs in real components, however, the question of the applicability of machining production technologies for component manufacture is of central importance. This has so far received Little attention in global materials research. Reliable and safe processing is essential for the demand of economical component production for potential areas of application, e.g. in power plant technology. For metals, milling is the standard machining process. This article presents the results of machining analyses. It focuses on the surface integrity resulting from the milling process on a Co20Cr20Fe20Mn20Ni20-HEA. For this purpose, investigations were carried out using ball nose end milling tools for conventional milling process in comparison to an innovative hybrid process available at BAM Berlin, Ultrasonic-Assisted Milling (USAM). USAM promises a lower Degradation of the surface properties due to lower loads on the workpiece surface during machining. For this purpose, basic milling parameters (cutting speed and tooth feed) were systematically varied and cutting forces were measured during the milling experiments. The subsequent Analysis of these forces allows an understanding of the mechanical loads acting on the tool and component surface. These loads cause topographical, mechanical and microstructural influences on the surface and consequently on the surface integrity. For their characterization, light and scanning electron microscopy were used, and the roughness and residual stresses via X-ray diffraction were measured. The results indicate significant advantages using USAM, especially due to reduced cutting forces compared to the conventional milling process. This causes lower mechanical loads on the tool and surface, combined with lower tensile residual stresses on and below the surface, and ultimately results in a significantly enhanced surface integrity. T2 - Symposium on Materials and Joining Magdeburg 2020 CY - Online meeting DA - 07.09.2020 KW - High entropy alloy KW - Machining KW - Ultrasonic machining PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512958 DO - https://doi.org/10.1088/1757-899X/882/1/012016 VL - 882 IS - 012016 SP - 1 EP - 11 PB - Institute of Physics CY - London AN - OPUS4-51295 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 - Buzolin, R. H. A1 - Richter, Tim A1 - Pixner, F. A1 - Rhode, Michael A1 - Schröpfer, Dirk A1 - Enzinger, N. T1 - Microstructure characterisation of multi-principal element alloys welds produced by electron beam welding N2 - This work explores the feasibility of producing bead-on-plate welds of a CrCoNi medium entropy alloy and a CrMnFeCoNi high entropy alloy using electron beam welding. The alloys were welded in two states: one in an as-cold-rolled condition and the other in an annealed condition. In addition, the materials are welded with two different parameters. The FCC microstructure of the welds is investigated using scanning electron microscopy assisted by energy-dispersive X-ray spectroscopy and electron-backscattered diffraction. The impact of the weld on the microstructure is discussed. The heat-affected zone is negligible for the annealed condition of both medium and high entropy alloys since there is no driving force for recrystallisation and the exposure time to high temperature is insufficient for grain coarsening. The texture formed in the fusion zone is also discussed and compared to the texture in the base metal and the heat-affected zone. Although the grain growth along the (100) crystallographic direction is preferential in all cases, the crystallographic texture type differs from each weld. Higher hardness values are measured in the medium entropy alloy’s base metal and fusion zone than in the high entropy alloy. KW - Multi-principal element alloy KW - Electron backscattered diffraction KW - Electron beam welding KW - High-entropy alloy KW - Microstructure characterization PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568129 DO - https://doi.org/10.1016/j.matdes.2023.111609 SN - 1873-4197 VL - 225 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Rhode, Michael T1 - Residual stresses in a high- and a medium-entropy alloy due to TIG and friction stir welding N2 - The new alloying concept of multi-element systems with defined entropy (HEA—high-entropy alloy; MEA—medium-entropy alloy) is gaining increasing importance in materials research. Significantly improved properties or combinations of properties are shown by some HEA/MEA systems. Thus, primarily the production and resulting microstructures of HEA, as well as its properties, have been investigated so far. Furthermore, processing is a main issue in transferring HEA systems from the laboratory to real components. Since welding is the most important joining process for metals, it is crucial to investigate the influence of welding to guarantee component integrity. Welding leads to residual stresses, which significantly affect the component integrity. Hence, the focus of this study is the residual stress formation and distribution in a CoCrFeMnNi HEA and ternary CoCrNi MEA using two different welding processes: tungsten inert gas (TIG) welding and solid-state friction stir welding (FSW). As a pathway for the application of HEA in this investigation, for the first time, residual stress analyses in realistic near-component specimens were performed. The residual stresses were determined by X-ray diffraction (XRD) on the surfaces of top and root weld side. The results were correlated with the local welding microstructures. The results show that both FSW and TIG generate significant tensile residual stresses on the weld surfaces in, and transverse to, the welding direction. In the case of FSW of the CoCrFeMnNi HEA, the longitudinal residual stresses are in the range of the yield strength of approx. 260 MPa in the weld zone. KW - High entropy alloy KW - Welding KW - Residual stresses KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567039 DO - https://doi.org/10.3390/jmmp6060147 SN - 2504-4494 VL - 6 IS - 6 SP - 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-56703 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 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 - CONF A1 - Schröpfer, Dirk T1 - Dissimilar metal joints of multiple principal element alloys friction stir welded to conventional austenitic steel 304 N2 - Multiple principal element alloys (MPEA) represent a class of materials consisting of at least three alloying elements, each with 5 to 35 atomic %. The MPEAs encompass the so-called high-entropy (HEA) and medium-entropy alloys (MEAs) and are fundamentally different from conventional materials like the Fe-based steel. Within the last 20 years, highly innovative MPEA with individually adjustable properties for industrial applications were identified. However, the focus has been on pure material synthesis. With the increase in available material quantities, the focus is now on processing issues such as joining and welding. In that connection, the weldability of MPEAs has received very little attention so far and experience in dissimilar metal welds (DMWs) is lacking so far but. The present study summarizes comprehensive experimental results on the weldability of MPEA-DMWs and their resulting microstructure. For this purpose, two equiatomic MPEAs, CoCrFeMnNi (HEA) and CoCrNi (MEA) in cold-rolled and annealed conditions were joined by solid-state friction stir welding (FSW) to an austenitic stainless steel 316L. The DMWs showed very interesting microstructure features. In addition, the mechanical-technological properties were obtained by instrumented tensile tests, and the local straining was determined in-situ by digital image correlation (DIC). A significant influence of the FSW processing on the mechanical performance was identified,in terms of the formation of FSW-specific defects like whitebands or tunnel defects. The experiments proofed the general (but currently limited) FS weldability of the MPEAs to conventional austenitic steel grade AISI 304. This enables targeted further considerations of these highly innovative MPEAs. T2 - AJP 2023: 3rd International Conference on Advanced Joining Processes 2023 CY - Braga, Portugal DA - 19.10.2023 KW - Multi-principal element alloys KW - Friction stir welding KW - Dissimilar metal weld (DMW) joint KW - Mechanical properties KW - Digital image correlation (DIC) PY - 2023 AN - OPUS4-58678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Development of a component test for assessment of delayed hydrogen assisted cracking susceptibility of thick walled submerged arc welded high strength offshore steels N2 - Offshore Wind Turbines (OWT) are a key factor in tomorrow's sustainable energy generation. The ever-increasing installation depth and weight of OWTs require suitable foundation concepts such as monopiles or tripods. Typically, mild steels such as S420ML are used with plate thicknesses of up to several hundred mm, resulting in high restraints in the welded joints. The large plate thickness requires high-efficiency welding processes such as submerged arc welding (SAW) with multiple wires. Due to the very high stiffness and plate thickness of the large-scale offshore structure, a susceptibility to time-delayed hydrogen assisted cracking (HAC) may occur. The evaluation of this crack susceptibility is very complex due to the component size and stiffness of real offshore structures. For this purpose, a near-component test geometry was developed to transfer the real stiffness conditions to laboratory (i.e. workshop) scale. The 350 kg mock-up studied consisted of heavy plates (thickness 50 mm, seam length 1,000 m) joined by a 22-pass submerged-arc weld. Additional stiffeners simulated the effect of high restraint or shrinkage restraint of the weld. Extreme scenarios of hydrogen absorption during welding were simulated by using flux in dry (HD < 5 ml/100g Fe) and wet (HD > 15 ml/100g Fe) conditions. Weld residual stresses were determined using a robotic X-ray diffractometer. Areas of critical tensile residual stress (at the level of the yield strength) were found in the weld metal and in the heat affected zone, suggesting that these weld sub-zones are the most critical in the case of hydrogen ingress. To identify possible delayed cracking, the welds were tested by phased array ultrasonic testing (PAUT) after welding, 6 h, 12 h, 24 h, and a maximum of 48 h. Summarized, no significant occurrence of HAC was detected, indicating the high crack resistance of the welded joint, i.e., a suitable combination of base material, welding consumable and parameters. T2 - MSE 2024: International Materials Science and Engineering Congress CY - Darmstadt, Germany DA - 24.09.2024 KW - Hydrogen KW - Offshore wind turbine KW - Component test KW - Submerged arc welding KW - Minimum waiting time PY - 2024 AN - OPUS4-61154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröpfer, Dirk T1 - Influence of welding stresses on relaxation cracking during heat treatment of a creep-resistant 13CrMoV steel, Part III N2 - Efficiency and flexibility are currently a major concern in the design of modern power plants and chemical processing facilities. The high requirements for economic profitability and in particular climate change neutrality are driving this development. Consequently, plant equipment and chemical reactor components are designed for higher operating pressure and temperature. Creep-resistant CrMo steels had been used as constructional materials for decades but came to operational limitations, for example the resistance against so-called high-temperature hydrogen attack in petrochemical reactors. For that purpose, 20 years ago V-modified CrMo steels had been developed for use in the petrochemical industry due to their very good creep-strength and hydrogen pressure resistance at elevated temperatures enabling long service life of the respective components. For example, the 13CrMoV9-10 steel is applicable for process temperatures of up to 482 °C and hydrogen pressures of up to 34.5 MPa. Due to the large dimensions and wall thickness of the reactors (wall thickness up to 475 mm) and the special alloy concept, reliable weld manufacturing of the components is extremely challenging. First, low toughness and high strength of the weld joint in the as-welded condition are critical regarding weld cracking. High welding residual stresses are the result of the highly restrained shrinkage of the component welds. For this purpose, the entire component must be subjected to Post-Weld Heat Treatment (PWHT) after completion of the welding operation. The aim is to increase the toughness of the weld joints as well as to reduce the welding induced residual stresses. Before and during PWHT, extreme caution is required to prevent cracking. Unfortunately, V-modified CrMo steels possess an increased susceptibility to cracking during stress relaxation the so-called stress relief cracking (SRC). Available literature studies have largely focused on thermal and metallurgical factors. However, little attention has been paid on the influence of the welding procedure on crack formation during PWHT considering actual manufacturing conditions. For that reason, we investigated in our previous studies (part I and II), the influence of heat control on the mechanical properties by simulating actual manufacturing conditions prevailing during the construction of petrochemical reactors using a special 3D- acting testing facility. The focus of part I was put on the influence of the welding heat control on mechanical stresses and the effect on cracking during PWHT. Part II was mainly dedicated to the metallurgical causes of SRC during PWHT and the interaction with the occurring mechanical stresses. It could be shown that not only high welding-induced stresses due to increased weld heat input cause higher susceptibility for SRC formation. It was further intensified by an altered precipitation behaviour in presence of mechanical stresses that are caused by the component related restraint. The present part III shows how residual stresses, which are present in such welded components and significantly influence the crack formation, can be transferred to the laboratory scale. As a result, the effect on the residual stresses on the SRC behaviour can be evaluated on simplified small-scale specimens instead of expensive mock-ups. For this purpose, experiments with test set-ups at different scales and under different rigidity conditions were designed and carried out. T2 - IIW Annual Assembly, Meeting of Commission II-A CY - Online meeting DA - 20.07.2020 KW - Welding KW - Creep-resistant steel KW - Residual stresses KW - Post weld heat treatment KW - Stress relief cracking PY - 2020 AN - OPUS4-51587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -