TY - CONF A1 - Rhode, Michael T1 - Weld heat input effect on microstructure and hydrogen diffusion in thick-walled S690 submerged arc welded joints N2 - High-strength, low-alloy (HLSA) steels such as S690 are an attractive option for heavy industries such as offshore wind turbines and peripheral equipment due to their combination of excellent mechanical properties and weldability. The construction of these thick-walled structures requires highly efficient welding processes such as submerged arc welding (SAW). However, SAW faces challenges related to delayed hydrogen assisted cold cracking (HACC). Despite its importance, the effect of different diffusion coefficients on the cold cracking susceptibility of different microstructures within SAW-welded S690 steels is not fully understood. For this reason, the present study focuses on comparing the cold cracking susceptibility of thermomechanically rolled (TM) or quenched and tempered (QL) variants of S690 steel. Submerged arc welding was performed on both steel grades at different welding heat inputs. From these thick-walled welds, metallic membranes were extracted from the weld metal, the heat-affected zone (HAZ), and the two base metals. The specimens were subjected to electrochemical hydrogen permeation tests (according to ISO 17081) to determine the microstructure-specific hydrogen diffusion coefficients. In general, increased welding heat input and thickness decreased the hydrogen diffusion coefficients, i.e., the time required for hydrogen diffusion increased. In addition, the results showed that the TM grade exhibited slightly accelerated hydrogen diffusion coefficients compared to the QL grade, which is beneficial for hydrogen reduction and increases the HACC resistance. As a result, the microstructure-specific assessment of hydrogen diffusion in the BM, HAZ or WM of the SAW joint was less important for a given set of welding parameters compared to other welding processes such as gas metal arc welding (GMAW). The reason is that in multilayer SAW, the relatively large welding heat input and multiple annealing resulted in similar microstructures, resulting in very close hydrogen diffusion coefficients. From this point of view, it is sufficient to characterize the hydrogen diffusion coefficients of both the weld metal and the base material. T2 - 78th IIW Annual Assembly and International Conference CY - Genoa, Italy DA - 26.06.2025 KW - Hydrogen assisted cracking KW - Submerged arc welding KW - Diffusion KW - Electrochemical permeation KW - Microstructure PY - 2025 AN - OPUS4-63543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Trapping in T24 steel weld joints – Effects on activation energy for hydrogen diffusion during TDA N2 - Failure cases in the past decade exhibited severe cracking in T24 welds and showed that generally hydrogen-assisted cracking (HAC) occurring up to 200°C cannot be excluded. A basic understanding is necessary on how hydrogen diffusion is influenced by the weld process. In this regard, both weld microstructures HAZ and weld metal have particular influence on hydrogen diffusion compared to the base material. In general, hydrogen diffusion at a certain temperature is described by diffusion coefficients representing an effective value of combined lattice diffusion and effects of reversible hydrogen traps. Those traps are typically precipitates, interstitials, grain boundaries and so on. A common approach to describe the trap character and its effect on diffusion is the determination of so-called activation energy. This can be done by respective thermal desorption analysis (TDA) with linear heating. In the present study, different T24 as-welded microstructures (BM, HAZ, WM) were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by TDA with linear heating using a mass spectrometer for detection of ultra-low hydrogen amounts. The results showed that typically the as-welded HAZ had higher energy traps than the tempered base material. Nonetheless two important effects were ascertained: (1) it is strictly necessary to monitor the sample temperature due to its great impact on the hydrogen desorption peak temperature and (2) the real heating rate in the specimen vs. the applied heating rate has to be considered. Both influence the calculated activation energy, i.e. the assigned hydrogen trap character (moderate or strong trap), which changed up to a factor of two in terms of the calculated activation energy. This effect can be much more important compared to the microstructure effect itself. Hence, suitable experimental boundary conditions should be mandatory for the determination of hydrogen trap kinetics. T2 - Intermediate Meeting of IIW Commission C-II-A "Metallurgy of Weld Metal" CY - Trollhättan, Sweden DA - 06.03.2017 KW - Hydrogen KW - Trapping and diffusion KW - Thermal desorption analysis KW - Microstructure KW - Activation energy PY - 2017 AN - OPUS4-39401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Ti and Nb influence on the HAZ microstructures of weld-simulated high-strength structural steel S690QL N2 - High-strength low-alloyed (HSLA) steels with yield strength / proof stress ≥ 600 MPa are the basis of modern light-weight steel constructions. Indeed, the economic and ecological benefits strongly depend on their processability in terms of welding. In this context, the use of highly productive welding processes, suitable welding consumables is of vital interest and requires a fundamental understanding of the microstructural changes in the HSLA steel and especially the heat-affected zone (HAZ) of the welded joint. Microalloying elements, such as Ti or Nb, are essential to achieve the desired mechanical properties. In this context, the underlying standards (such as EN 10025-6) only specify maximum values, resulting in different manufacturer customized microalloy concepts. Furthermore, even small deviations can have a drastic effect expressed by an excessive hardening or softening despite identical welding conditions and filler metal. The reason is the different thermal stability of the Ti and Nb-related precipitates (typically carbides or carbon nitrides). As a result, it is difficult (or even impossible) to adequately predict the weldability. Against this background, different microalloying routes with varying Ti and Nb contents for a S690QL reference grade were systematically investigated in terms of lab-cast alloys close to realistic chemical compositions. To investigate the influence of the welding heat input on the HAZ microstructure formation, physical simulations were carried with specified peak temperatures and cooling times (by a dilatometry). The focus was the identification of the occurring phase transformations during cooling and the final HAZ microstructure. In this context, a double welding cycle was simulated to further identify the behavior of the so-called intercritical HAZ (where softening is likely to occur) in case of the common multi-layer welding for thick plates. The results showed: (1) microalloying has significant influence on the formation of the individual HAZ dependent on (2) the thermal stability of the Ti or Nb-precipitates and (3) synergistic effects of further elements such as Mo and their effect on phase transformations in the HAZ. The results represent a microstructure-based validation of welding processing of such HSLA-steels e.g. in terms of preferred microalloy and weld heat input combinations. T2 - 49th MPA Conference CY - Stuttgart, Germany DA - 06.10.2025 KW - High-strength steel KW - Microalloy elements KW - Welding KW - Weld simulation KW - Microstructure PY - 2025 AN - OPUS4-64319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steppan, Enrico A1 - Mantzke, Philipp A1 - Steffens, Benjamin A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Thermal desorption analysis for hydrogen trapping in microalloyed high-strength steels N2 - Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen-assisted cracking in microalloyed high-strength steels during fabrication and/or operation in industrial applications. In order to study these effects, electrochemically charged tensile specimens were tested to elucidate the degradation of their properties. The carrier gas hot extraction (CGHE) method, which functionally combines a mass spectrometer with a thermal desorption analysis (TDA) process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The mass spectrometer provided rapid and automatic determination of hydrogen concentration, whereas the TDA presented the activation energy within the respective test specimen at the specific temperature. Additionally, specimen temperature was carefully monitored to reduce the evaluation error for local effusion peaks. A quenching and deformation dilatometer was used for the analysis of typical heat-affected zones during the welding process for a high reproducibility of the homogenous microstructures that were studied. The present work shows the interaction between hydrogen and lattice defects in different microalloyed materials and heat-affected zones of weldable fine-grained steels. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. These preparations were made according to German standard DIN EN 10025-6 and to DIN EN 10149-2, respectively. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and microalloying elements such as Ti, Nb, Mo, Cr, and V. The two steel grades exhibited several types of traps: carbide formations, dislocations, and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in thermo-mechanically hot rolled steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot rolled steel revealed an increased interaction between hydrogen and precipitations. The higher carbon content in the quenched and tempered steel led to a higher interaction between hydrogen and iron carbide, specifically in the martensitic phase. Furthermore, the trapping behavior in heat-affected zones showed a significant increase in activation energy, especially in the coarse-grained microstructure. These previously mentioned various effects were studied to better understand the degradation of mechanical properties in these two steels. KW - Microalloyed steels KW - Hydrogen embrittlement KW - Heating KW - Chemical analysis KW - Microstructure KW - Heat-affected zone PY - 2017 DO - https://doi.org/10.1007/s40194-017-0451-z SN - 0043-2288 SN - 1878-6669 VL - 61 IS - 4 SP - 637 EP - 648 PB - Springer CY - Berlin Heidelberg AN - OPUS4-40190 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 - JOUR A1 - Buzolin, R.H. A1 - Richter, Tim A1 - Pixner, F. A1 - Rhode, Michael A1 - Schröpfer, Dirk A1 - Enzinger, N. T1 - Microstructure and texture characterisation of friction stir welded CoCrNi and CoCrFeMnNi multi-principle element alloys N2 - This work investigates the microstructure formed in friction stir welds of FCC alloys, focused on two multiprincipal alloys: a CoCrFeMnNi high-entropy alloy (HEA) and a CoCrNi medium-entropy alloy (MEA). A commercial stainless steel AISI 304 is used for comparison. The largest nugget was formed in the MEA, while the smallest was formed in the HEA. Grain refinement occurs in the stirred zone in all welds. Discontinuous dynamic recrystallisation is the predominant restoration mechanism during friction stir welding of the three investigated alloys. A sharp decrement in the Σ3 boundary fraction occurs in the stirred zone of the AISI 304 and HEA welds, while comparable values with the base metal are found for the MEA weld. The peak in the maximum index of crystallographic texture is observed on the advancing side of the stirred zone of the AISI 304 weld. A strong <001> θ-fibre texture is formed in the advancing side of the nugget in the AISI 304 from a well-established {123} <634> S-type texture in the base metal. Multiple crystallographic texture components without specific fibres are identified in most regions of the welds, indicating the complex shear path history during friction stir welding. KW - Microstructure KW - Multiple principal element alloy KW - Friction stir welding KW - Electron backscattered diffraction KW - Crystallographic texture PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572987 DO - https://doi.org/10.1016/j.mtcomm.2023.105870 VL - 35 SP - 1 EP - 14 PB - Elsevier Ltd. CY - Amsterdam (NL) AN - OPUS4-57298 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 - CONF A1 - Rhode, Michael T1 - Hydrogen trapping in T24 steel weld joints - microstructure influence vs. experimental design effect on activation energy for diffusion N2 - In general, hydrogen assisted cracking is a result of a critical combination of local microstructure, mechanical load and hydrogen concentration. In that connection, welded microstructures of low-alloyed creep-resistant steels can show different hydrogen trapping kinetics. That influences the adsorbed hydrogen concentration as well as the diffusion itself in terms of moderate or strong trapping. A common approach to describe trapping is by the activation energy that is necessary to release hydrogen from a specific trap site. In the present study, T24 base material and weld metal were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis(TDA) with linear heating using a mass spectrometer. The results showed a microstructure effect on hydrogen trapping kinetics at elevated temperatures. Additionally, it is necessary to monitor the specimen temperature. A comparison between idealized temperature profile and real specimen temperature showed that the calculated activation energy varied up to a factor of two. Thus, the assigned trap character(moderate or strong) changed. In case of high temperature peaks, this effect could be more important compared to the microstructure effect itself. T2 - 70th IIW Annual Assembly, Commission II-A CY - Shanghai, People's Republic of China DA - 25.06.2017 KW - Creep resisting materials KW - Welding KW - Hydrogen diffusion KW - Thermal desorption analysis KW - Microstructure KW - Experimental design PY - 2017 AN - OPUS4-40954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Mente, Tobias A1 - Steppan, E. A1 - Kannengießer, Thomas A1 - Steger, J. T1 - Hydrogen trapping in T24 Cr-Mo-V steel weld joints - microstructure effect vs. experimental influence on activation energy for diffusion N2 - Hydrogen-assisted cracking is a critical combination of local microstructure, mechanical load and hydrogen concentration. Welded microstructures of low-alloyed creep-resistant Cr-Mo-V steels show different hydrogen trapping kinetics. This influences the adsorbed hydrogen concentration as well as the diffusion by moderate or strong trapping. A common approach to describe hydrogen traps is by their activation energy that is necessary to release hydrogen from the trap. In the present study, Cr-Mo-V steel T24 (7CrMoVTiB10-10) base material and TIG weld metal were investigated. Electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis (TDA) with different linear heating rates. The results show two different effects. At first, the microstructure effect on trapping is evident in terms of higher hydrogen concentrations in the weld metal and increased activation energy for hydrogen release. Secondly, it is necessary to monitor the real specimen temperature. A comparison between the adjusted heating rate and the real specimen temperature shows that the calculated activation energy varies by factor two. Thus, the trap character in case of the base material changes to irreversible at decreased temperature. Hence, the effect of the experimental procedure must be considered as well if evaluating TDA results. Finally, realistic temperature assessment is mandatory for calculation of activation energy via TDA. KW - Creep-resistant steel KW - Hydrogen assisted cracking KW - Thermal desorption analysis KW - Welding KW - Microstructure KW - Diffusion PY - 2018 DO - https://doi.org/10.1007/s40194-017-0546-6 SN - 0043-2288 SN - 1878-6669 VL - 62 IS - 2 SP - 277 EP - 287 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-44505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Hydrogen diffusion in creep-resistant 9%-Cr P91 steel weld metal N2 - 9 %-Cr steel P91 is widely used in power plants due to the excellent creep-resistance. Components of this steel are typically welded and demand for careful welding fabrication, whereas a so-called post weld heat treatment (PWHT), must be conducted to increase the toughness and decrease the hardness of the martensitic as-welded (AW) microstructure. Before the PWHT, a hydrogen removal (or dehydrogenation) heat treatment is necessary as hardened AW martensitic microstructure is generally prone to delayed hydrogen assisted cracking (HAC). The microstructure and temperature dependent hydrogen diffusion is an important issue as it determines how long a potential crack-critical hydrogen concentration could remain in the microstructure. In this context, reliable hydrogen diffusion coefficients of P91 weld metal are rare. Hence, the diffusion behavior of P91 multi-layer weld metal was investigated in two different microstructure conditions: AW and further PWHT (760 °C for 4 h). Two different experimental techniques were used to cover a wide range of hydrogen diffusion temperatures: the electrochemical permeation technique (PT) at room temperature and the carrier gas hot extraction (CGHE) for a temperature range from 100 to 400 °C. From both techniques typical hydrogen diffusion coefficients were calculated and the corresponding hydrogen concentration was measured. It was ascertained that both heat treatment conditions show significant differences in hydrogen diffusivity. The biggest deviations were identified for room temperature. In this case, the AW condition shows significant hydrogen trapping and up to seven times lower diffusion coefficients. Additionally, PT investigations showed a preferred diffusion direction of hydrogen in the weld metal expressed by the diffusion coefficients and the permeability for both heat treatment conditions. The CGHE generally revealed lower diffusion coefficients for the AW microstructure up to 200 °C. In addition, the AW condition showed hydrogen concentrations up to 50 ml/100 g (considering electrochemical charging). Nonetheless, this hydrogen was not permanently (reversibly) trapped. Nonetheless, this temperature is approximately 100 °C below recommended dehydrogenation heat treatment (DHT). This has two main consequences: (I) in case of welding is interrupted or no DHT is conducted, a HAC susceptibility of hardened martensitic P91 weld metal cannot be excluded and (II) DHT can be conducted at temperatures around 200 °C below the recommended temperatures. T2 - IIW Annual Assembly, Meeting of Commission IX-C "Creep and heat resistant welds" CY - Bratislava, Slovakia DA - 07.07.2019 KW - Hydrogen KW - Diffusion KW - Weld metal KW - Microstructure KW - Post weld heat treatment PY - 2019 AN - OPUS4-48449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -