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 - Richter, Tim T1 - Characterization of Hydrogen Diffusion in a Thick-walled Submerged Arc Multi-Layer Weld Joint N2 - The energy production of the future will be dominated by CO2-emission free techniques like wind turbines and become essential in scope of the planned hydrogen economy. As onshore installation capacity is limited, the in-crease of the number of offshore wind turbines (OWT) is a major goal. In that connection, the OWTs continuously increase in size and weight and demand adequate foundations concepts like monopiles or tripods. These compo-nents are typically manufactured from welded mild steel plates with thickness up to 200 mm. The predominant welding technique is submerged arc welding (SAW) with up to five wires. In accordance with the standards, the occurrence of delayed hydrogen assisted cracking is anticipated by either a hydrogen removal heat treatment (HRHT) or a so-called minimum waiting time (MWT) before non-destructive testing (NDT) of the respective weld joint is allowed. The reason for the MWT is the necessary time for the hydrogen diffusion at ambient temperature due the high plate thickness. Both the effectiveness of a HRHT at elevated temperatures or the MWT at ambient temperature can be estimated by calculation of the diffusion time. This time depends on reliable hydrogen diffu-sion coefficients and these are rare in literature. For that reason, this study presents the hydrogen diffusion coef-ficients obtained from a multi-layer SAW joint of an offshore steel grade. Two different experimental techniques were used to identify the respective diffusion behavior: (1) hydrogen desorption experiments with a carrier gas hot extraction analyzer at elevated temperatures for the characterization of a HRHT and (2) the electrochemical permeation technique at ambient temperature for the characterization of an MWT. From both experiments, the respective diffusion coefficients were calculated. The obtained DCs are different from those reported in literature, i.e., the duration or applicability of a HRHT or MWT must be critically discussed. T2 - European Congress and Exhibition on Advanced Materials and Process - Euromat 2021 CY - Online meeting DA - 13.09.2021 KW - Welding KW - Offshore KW - Wind turbine KW - Hydrogen KW - Cracking PY - 2021 AN - OPUS4-53296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Rhode, Michael A1 - Boerner, Andreas A1 - Saliwan Neumann, Romeo A1 - Schneider, M. A1 - Laplanche, G. T1 - Influence of machining on the surface integrity of high- and medium-entropy alloys N2 - High- and medium-entropy alloys (HEAs) are a quite new class of materials. They have a high potential for applications from low to high temperatures due to the excellent combination of their structural properties. Concerning their application as components; processing properties, such as machinability, have hardly been investigated so far. Hence, machinability analyses with a focus on the influence of the milling process and its basic parameters (cutting speed, feed per cutting edge) on the resulting surface integrity of specimens from an equiatomic high- (CoCrFeMnNi) and a medium- (CoCrNi) entropy alloy have been carried out. A highly innovative milling process with ultrasonic assistance (USAM) was compared to conventional milling processes. Recent studies have shown that USAM has a high potential to significantly reduce the mechanical load on the tool and workpiece surface during milling. In this study, the basic machining and ultrasonic parameters were systematically varied. After machining, the surface integrity of the alloys was analyzed in terms of topography, defects, subsurface damage, and residual stresses. It was observed that USAM reduces the cutting forces and increases the surface integrity in terms of lower tensile residual stresses and defect density near the surfaces for the CoCrFeMnNi alloy. It was shown that the cutting forces and the metallurgical influence in the sub surface region are reduced by increasing the cutting speed and reducing the feed rate per cutting edge. With the CoCrNi alloy, the tool revealed severe wear. As a result, for this alloy no influence of the parameters on the machinability could be determined. KW - High Entropy Alloy KW - Medium Entropy Alloys KW - Ultrasonic assited machining PY - 2022 DO - https://doi.org/10.1016/j.matchemphys.2021.125271 SN - 0254-0584 VL - 275 SP - 125271 PB - Elsevier B.V. AN - OPUS4-53606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Richter, Tim A1 - Mayr, P. A1 - Nitsche, A. A1 - Mente, Tobias A1 - Böllinghaus, Thomas T1 - Hydrogen diffusion in creep-resistant 9% Cr P91 multi-layer weld metal N2 - Welded components of P91 9% Cr steel demand for careful welding fabrication with necessary post weld heat treatment (PWHT). Before the PWHT, a hydrogen removal heat treatment is necessary for avoidance of hydrogen assisted cracking (HAC). In this context, the microstructure and temperature-dependent hydrogen diffusion is important, and reliable diffusion coefficients of P91 weld metal are rare. For that reason, the diffusion behavior of P91 multi-layer weld metal was investigated for as-welded (AW) and PWHT condition by electrochemical permeation experiments at room temperature and carrier gas hot extraction (CGHE) from 100 to 400 °C. Hydrogen diffusion coefficients were calculated, and the corresponding hydrogen concentration was measured. It was ascertained that both heat treatment conditions show significant differences. At room temperature the AW condition showed significant hydrogen trapping expressed by to seven times lower diffusion coefficients. A preferred diffusion direction was found in perpendicular direction expressed by high permeability. The CGHE experiments revealed lower diffusion coefficients for the AW condition up to 400 °C. In this context, a hydrogen concentration of approximately 21 ml/100 g was still trapped at 100 °C. For that reason, a certain HAC susceptibility of as-welded P91 weld metal cannot be excluded, and hydrogen removal should be done before PWHT. KW - Creep resisting materials KW - Diffusion KW - Hydrogen KW - Weld metal KW - Post weld heat treatment KW - Microstructure PY - 2020 DO - https://doi.org/10.1007/s40194-019-00828-8 SN - 0043-2288 VL - 64 IS - 2 SP - 267 EP - 281 PB - Springer AN - OPUS4-50471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -