TY - CONF A1 - Rhode, Michael A1 - Schaupp, Thomas A1 - Muenster, C. A1 - Mente, Tobias A1 - Boellinghaus, Thomas A1 - Kannengießer, Thomas T1 - "On how to influence your results" - A review on carrier gas hot extraction parameters for hydrogen determination in welded specimens N2 - Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in welded joints using a thermal conductivity device (TCD) for quantitative measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries and factors that additionally influence hydrogen determination. They are namely: specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PID-furnace controller as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up the reach the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by evaluation of the recorded data. Generally, independent temperature measurement with calibration specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA). T2 - IIW Annual Assembly and International Conference 2018, Meeting of Commission II-E CY - Nusa Dua, Bali Island, Indonesia DA - 15.07.2018 KW - Carrier gas hot extraction (CGHE) KW - Welding KW - ISO 3690 KW - Hydrogen KW - Experimental design PY - 2018 AN - OPUS4-45520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Sobol, Oded T1 - Additive manufacturing for components in hydrogen technologies N2 - With the introduction of a hydrogen-based energy and national economy, safety-relevant components for hydrogen technologies are becoming increasingly important. Characteristic of hydrogen technologies are, for example, harsh environmental conditions such as cryogenic or high-pressure storage, corrosion issues in fuel cells and electrolyzers, turbines, and many more. Additive manufacturing of components is becoming increasingly important and irreplaceable for the production of complex technical systems. Using the case studies of burners for gas turbines and electrodes and membranes for polymer (PEMFC) and solid oxide (SOFC) fuel cells, this article shows the potential of additive manufacturing of components. At the same time, however, the challenge of considering divergent mechanical properties depending on the direction of assembly in a "hydrogen-compatible" manner is also highlighted. Finally, the challenges posed by additive manufacturing and hydrogen for materials testing are highlighted under scenarios that are as realistic as possible. T2 - MPA-Workshop Hydrogen CY - Online meeting DA - 10.11.2022 KW - Additive manufacturing KW - Hydrogen KW - Technologies KW - Overview KW - Component PY - 2022 AN - OPUS4-56233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Kannengiesser, Thomas T1 - Call for interested people to contribute to series of comprehensive papers on welding and joining of components for sustainable energy systems N2 - Joining and welding technologies are of high importance for the manufacturing of components and parts used in sustainable energy generation, conversion, and transport. In that connection, offshore and on-shore installed wind turbines are of high interest for the generation of electrical energy as well as photo-voltaic systems (solar cells). The electricity can be either directly transported or conversed via power-to-gas e.g., to hydrogen. In that scope, electrolyzer up to MW-range are of interest as well as the conver-sion back to electricity via fuel cells. In addition, hydrogen is a key element of the decarburization of in-dustries as well as the mobility sector encompassing sea, air and land transportation driven by hydrogen or its derivates. Well-known examples cover the direct reduction of iron ore to replace the conventional blast furnace process up to gas turbines or fuel cells for home-end use. All mentioned technologies re-quire reliable components, which are to a high extend dependent on joining and especially welding pro-cessing of materials. Especially, the (petro-) chemical industry has many years of experience with both materials used in hydrogen applications. The challenge is e.g., the transition to mass production of sys-tem components of electrolyzers/fuel cells and for distribution grids. At this point, the scalability of cur-rently applied joining processes often limits the economic efficiency, whereas especially laser welding or additive manufacturing will be of high interest. In that connection, it is very important to provide answers by joint research of universities, institutes, and industrial companies. Very often, solutions are already available and “just” have to be investigated and adapted for the new application, like repair welding of NG pipelines. For that reason, we want to set up a series of comprehensive papers with the aforementioned title. The idea is to get an in-depth but manageable overview of the importance of joining technologies in sustaina-ble energy generation, conversion, and transport encompassing current processes, limitations, and fur-ther perspectives. In that connection, the additive manufacturing is gaining more and more attention. If applicable, current challenges in the adaption or creation of new standards/regulations shall be addressed. T2 - IIW Intermediate Meeting, Com. II-A CY - Incheon, Republic of Korea DA - 12.03.2024 KW - Hydrogen KW - Welding KW - Comprehensive study KW - Component manufatcturing KW - Additive manufacturing PY - 2024 AN - OPUS4-59676 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 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Konert, Florian A1 - Sobol, Oded A1 - Böllinghaus, Thomas A1 - Merz, Benjamin T1 - Hollow specimens as simplified approach for testing metallic materials under high pressure hydrogen development and utilization N2 - The hydrogen economy requires large-scale storage and transportation options like long-distance transmission pipelines. The applied materials (typically steels) must be carefully tested under different conditions (pressure, temperature, impact of impurities, etc.) for their suitability and service with hydrogen. In combination with mechanical load, as occurs in every gas network, hydrogen can induce degradation of the mechanical properties and promote finally resulting in embrittlement, i.e., the formation of cracks. The conventional testing procedures consist of autoclaves in which samples are strained under pressurized hydrogen. The test apparatus requires large amounts of hydrogen and thus a high level of safety and costs. In very specific cases, these tests might be replaced by simplified electrochemical charging. However, these test alternatives raise several questions regarding the equivalency of both testing scenarios. In the early 1980’s the idea of a so-called hollow tensile sample raised and was reinitiated 2021 in ISO TC 164 by T. Ogata (NIMS, Japan) and further developed (e.g. by Fraunhofer IWM, Germany). The idea was: the sample itself represents the autoclave instead of charging a sample from outside. For that reason, a hole is drilled through the sample and the inner surface is pressurized by hydrogen gas during the mechanical testing. Indeed, this represents the main advantage as no expensive pressure-resistant autoclave equipment for large H-volumes is necessary, which significantly reduces the safety-related issues and thus the high costs. In the following, we show recent activities at BAM Berlin on adaption of the hollow-specimen technique for slow strain rate testing (SSRT). The current research activities are focussed on macroscopic influences like the sample geometry, minimum necessary dimensions, and microscopic influences e.g., on the surface by the processing method (drill hole quality and geometric precision) as well as the gas pressure effect (mechanical deformation of surface in different media). T2 - FEMS EUROMAT 2023 CY - Frankfurt a. M., Germany DA - 04.09.2023 KW - Hydrogen KW - Hollow tensile specimen KW - High-pressure KW - Mechanical properties KW - Testing PY - 2023 AN - OPUS4-58220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Boellinghaus, Thomas T1 - Hydrogen absorption and diffusion in T24 steel weld joints and effect on mechanical properties N2 - The present contribution summarizes results obtained from experiments with low-alloyed boiler steel grades T24 (CrMoV alloy), T22 (CrMo) and thermally simulated T24 HAZ microstructure and pure weld metal. The hydrogen absorption and diffusion behavior was investigated by permeation experiments and thermal desorption analysis (TDA). The results showed significant weld microstructure influence on diffusion by hydrogen trapping. Trapped hydrogen was determined in the T24 BM at temperatures up to 120 °C compared to 75 °C in the T22. In addition, the T24 HAZ showed decreased diffusion coefficients (at room temperature) of approximately one magnitude compared to the BM. For the mechanical properties, tensile tests were conducted with electrochemically hydrogen charged specimens and compared to results obtained from slow strain rate tests (SSRT) in high-temperature water up to 200 °C. The as-welded HAZ had remarkably increased susceptibility compared to the BM already at low hydrogen concentration of 1-2 ppm. The SSRT were conducted for free corrosion and acidic environment and confirmed this behavior at elevated temperatures for both HAZ microstructures of T24 and T22. Summarized, each weld microstructure has specific diffusion coefficients and shows different susceptibility to degradation of the mechanical properties, i.e. delayed hydrogen assisted cracking or stress corrosion cracking. T2 - NACE Italia - 2nd Conference & Expo 2018 CY - Genoa, Italy DA - 28.05.2018 KW - Hydrogen KW - Stress corrosion cracking KW - Welding KW - Creep-resistant steel KW - T24 / 7CrMoVTiB10-10 PY - 2018 AN - OPUS4-45080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Richter, T. A1 - Mayr, P. A1 - Nitsche, A. A1 - Mente, Tobias A1 - Böllinghaus, Thomas 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 - TY - CONF A1 - Rhode, Michael A1 - Mente, Tobias T1 - Hydrogen embrittlement of steels N2 - Hydrogen assisted cracking of metals is a serious issue in the safety of components, espcially in case of welding. The current presentation gives an overview on specialized testing procedures at Department 9 including the quantitative determination of hydrogen. T2 - HYDROGENIUS BAM Joint Hydrogen Symposium CY - Online meeting DA - 06.07.2021 KW - Hydrogen KW - Embrittlement KW - Degradation KW - Carrier gas hot extraction KW - Welding PY - 2021 AN - OPUS4-53049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Kannengießer, Thomas A1 - Schaupp, Thomas A1 - Mente, Tobias T1 - Hydrogen in weld joints - An underestimated risk? - Utilization potential of gas analytics versus safety of welded components N2 - Hydrogen was once called “the versatile embrittler” [1], which summarizes very well the effect on reduction of ductility and/or toughness in technical alloys like steel. In that connection, welding is one of the most important component fabrication technologies. During welding, hydrogen can be transferred to the weld pool from manifold sources (like contaminations, residuals at the surface, etc.). As hydrogen embrittles a material, the safety of welded components with hydrogen is always a critical issue. Weld heat input causes additional changes in the microstructure like grain growth or partial dissolution of precipitates and many more. All these things influence the mechanical properties and also represent hydrogen traps. These traps decrease the hydrogen diffusion compared to the ideal lattice. The result can be so-called delayed hydrogen assisted cracking (HAC) of the weld joint due to the significantly decreased diffusivity by trapped hydrogen. This is often an underestimated risk as those cracks can appear in the weld joint even after some days! It is essential to know about hydrogen ingress during welding and the microstructure specific hydrogen diffusion. Both are depended on weld parameter influence and the chemical composition of the base material and weld metal. For that purpose, gas analytic methods like solid-state carrier gas hot extraction (CGHE) are useful tools to: (1) identify detrimental hydrogen concentrations from weld joints, (2) binding energies from hydrogen traps by thermal desorption analysis or (3) high-temperature diffusion coefficients. Those values are extremely important for welding practice in terms of recommendations on realistic hydrogen removal heat treatment (HRHT) after welding. Considering the increasing use of “digital” experiments, the data is also needed for reliable numerical simulations of HAC process or HRHT-effectiveness. The present contribution gives an overview on the influence of hydrogen on weld joints, the necessity, methods and standards for hydrogen determination (CGHE) with the aim of fabrication of safe welded and crack-free components. [1] R. A. Oriani (1987), Corrosion 43(7):390-397. doi: 10.5006/1.3583875 T2 - 20. Tagung Festkörperanalyse - FKA20 CY - Vienna, Austria DA - 01.07.2019 KW - Hydrogen KW - Welding KW - Gas analytic PY - 2019 AN - OPUS4-48402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Schaupp, Thomas A1 - Kannengießer, Thomas T1 - Influence of welding parameters on diffusible hydrogen content in high-strength steel welds using modified spray arc N2 - In order to satisfy the growing requirements towards lightweight design and resource efficiency in modern steel constructions, e.g. mobile cranes and bridges, high-strength steels with typical yield strength ≥ 690 MPa are coming into use to an increasing extent. However, these steels require special treatment in welding. The susceptibility for degradation of the mechanical properties in presence of hydrogen increases significantly with increasing yield strength. In case of missing knowledge about how and which amount of hydrogen is uptaken during welding, hydrogen assisted cracking (HAC) can be a negative consequence. Moreover, modern weld technology like the modified spray arc process enables welding of narrower weld seams. In this context, a reduced number of weld beads, volume and total heat input are technical and economic benefits. This work presents the influence of welding parameters on the diffusible hydrogen content in both singlepass and multi-layer welds. Different hydrogen concentrations were detected by varied contact tube distance, wire feed speed, arc length as well as varied arc type (transitional arc and modified spray arc). The results show, that all welding parameters have significant influence on the diffusible hydrogen concentration in the single-pass welds. By increasing the number of weld beads in case of multi-layer welding, the hydrogen concentration have been substantially reduced. Whereby, differences in hydrogen concentrations between both arc types are present. T2 - 70th IIW Annual Assembly, Commission II-A CY - Shanghai, People's Republic of China DA - 25.06.2017 KW - Hydrogen KW - MAG Welding KW - High-strength steels KW - Process parameters PY - 2017 AN - OPUS4-40953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -