TY - CONF A1 - Rhode, Michael A1 - Czeskleba, Denis A1 - Kannengießer, Thomas A1 - Mente, Tobias T1 - Reliable hydrogen determination in metallic materials and their weld joints: Parameters and challenges N2 - In the course of tomorrow's hydrogen-based energy transition, the construction of the corresponding infrastructure will play a central role. The majority of materials used to date are typically welded for component fabrication. In that context, steels are widely applied and can be prone to hydrogen embrittlement. This includes the classical delayed cold cracking during welding processing as well as embrittlement phenomena during operation. For the evaluation of any hydrogen effect on, for example, the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. In the case of welds, for example, according to ISO 3690, this is the isothermal carrier gas hot extraction (CGHE). CGHE is based on accelerated hydrogen degassing due to thermal activation of hydrogen at elevated temperatures. In addition to the pure quantification of hydrogen, thermal desorption analysis (TDA) with varied heating rates can be used to determine and evaluate the bonding state at microstructural defects in the material. For both techniques, experimental and measurement influences have to be considered, which have a great effect on the result. For CGHE, for example, ISO 3690 suggests different sample geometries as well as minimum extraction times. The present study summarizes results and experiences of numerous investigations with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding: the influence of the sample surface (polished/welded), measurement accuracies depending on the sample volume as well as the insufficient monitoring of the effect of the PI controller on the extraction temperature. In particular, a deviating extraction temperature to the set temperature, can significantly falsify the measurement results. Based on the results, methods are shown to quickly reach the desired extraction temperature without having to physically interfere with the measurement equipment. This serves to substantially improve the reliability of hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples for the selected heating procedure is advisable to exclude possible unwanted temperature influences already before the measurement. In addition (and way more important), the methods described can be transferred directly to industrial applications. T2 - 47th MPA-Seminar CY - Stuttgart, Germany DA - 10.10.2023 KW - Hydrogen assisted cracking KW - Carrier gas hot extraction KW - Welding KW - ISO 3690 KW - Metals PY - 2023 AN - OPUS4-58677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Erxleben, Kjell A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Hydrogen determination in welded metallic materials: Necessity and challenges N2 - In the course of tomorrow's hydrogen-based energy transition, the construction of the corresponding infrastructure will play a central role. The majority of materials used to date are typically welded for component fabrication. In that context, steels are widely applied and can be prone to hydrogen embrittlement. For the evaluation of any hydrogen effect on, for example, the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. According to ISO 3690, carrier gas hot extraction (CGHE) can be used. In addition to the pure quantification of hydrogen, thermal desorption analysis (TDA) with varied heating rates can be used to determine and evaluate the bonding state at microstructural defects in the material. For both techniques, experimental and measurement influences have to be considered, which have a great effect on the result. For CGHE, for example, ISO 3690 suggests different sample geometries as well as minimum extraction times. The present study summarizes results and experiences of numerous investigations with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding: the influence of the sample surface (polished/welded), measurement accuracies depending on the sample volume. In particular, a deviating extraction temperature to the set temperature, can significantly falsify the measurement results. Based on the results, methods are shown to quickly reach the desired extraction temperature without having to physically interfere with the measurement equipment. This serves to substantially improve the reliability of hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples for the selected heating procedure is advisable to exclude possible unwanted temperature influences already before the measurement. In addition (and way more important), the methods described can be transferred directly to industrial applications. T2 - Eurocorr 2023 - The European Corrosion Congress CY - Brussels, Belgium DA - 27.08.2023 KW - Hydrogen KW - Carrier gas hot extraction KW - Welding KW - ISO 3690 KW - Measurement PY - 2023 AN - OPUS4-58305 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 - JOUR A1 - Rhode, Michael A1 - Schaupp, Thomas A1 - Münster, C. A1 - Mente, Tobias A1 - Kannengießer, Thomas A1 - Böllinghaus, Thomas T1 - Hydrogen determination in welded specimens by carrier gas hot extraction - a review on the main parameters and their effects on hydrogen measurement N2 - Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in weld joints using a thermal conductivity detector (TCD) for hydrogen 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 (ISO 3690 type B and small cylindrical samples), 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 PI-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 to 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 dummy specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA). KW - Hydrogen KW - Carrier gas hot extraction KW - Experimental design KW - Thermal conductivity device PY - 2019 U6 - https://doi.org/10.1007/s40194-018-0664-9 SN - 0043-2288 VL - 63 IS - 2 SP - 511 EP - 526 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schaupp, Thomas A1 - Rhode, Michael A1 - Yahyaoui, Hamza A1 - Kannengießer, Thomas T1 - Hydrogen distribution in multi-layer welds of steel S960QL N2 - High-strength low-alloyed (HSLA) steels with yield strength ≥ 690 MPa have increasing im-portance in steel construction and civil engineering. However, weld processing of those steels is a major challenge. The susceptibility for degradation of mechanical properties of weld joints sig-nificantly increases in presence of hydrogen and can result in hydrogen assisted cracking (HAC). Generally, risk for HAC increases with increasing yield strength of HSLA steels. To min-imize the incidence of HAC, it is essential to gain knowledge about both the (1) absorbed hydro-gen amount and its distribution in the weld seam and (2) options to lower the amount of intro-duced hydrogen. Existing standards recommend heat treatment procedures (interpass tempera-ture or post weld heat treatment) to reduce the diffusible hydrogen concentration in weldments. In this context, different weld seam geometries should be considered. For HSLA steel fabrication weld processing with seam opening angles of 45° to 60° is typical. Modern weld technologies allow welding with seam opening angles of 30° - reduced welding time and costs. In the present study, the hydrogen distribution in multi-layer welds of a 960 MPa HSLA steel was analysed. Influence of different seam opening angles as well as heat input, interpass temperature and post weld heat treatments were investigated. The welded samples were quenched in ice water imme-diately after welding and subsequently stored in liquid nitrogen. After defined warming up, small specimens were machined from the weld seam by water jet cutting. The diffusible hydrogen concentration was measured by carrier gas hot extraction with coupled mass spectrometer. The results showed, that low heat input and post weld heat treatment procedures can lower hydrogen concentrations in welds. Furthermore, a gradient of the hydrogen concentration was identified with increasing weld pool depth. By varying the seam opening angles different hydrogen concen-trations were measured. T2 - 3rd International Conference on Metals & Hydrogen CY - Ghent, Belgium DA - 29.05.2018 KW - Hydrogen KW - Welding KW - High-strength steels KW - Heat treatment KW - Carrier gas hot extraction PY - 2018 AN - OPUS4-45076 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Mente, Tobias A1 - Münster, C. A1 - Kannengießer, Thomas T1 - Specimen temperature during CGHE and influence on hydrogen determination N2 - Hydrogen determination in weld seams is standardized in ISO 3690. In accordance to this standard, a defined time for hydrogen collection has to be anticipated for different extraction temperatures. In other words, the temperature is the most important value that has to be monitored in addition to the aimed hydrogen determination. The specimen geometry has influence on the real sample temperature during CGHE vs. the adjusted furnace temperature. This presentation gives a short summary on possible influences on the "correct" hydrogen determination temperature during carrier gas hot extraction (CGHE) using infrared radiation driven furnace. The main findings are: (1) specimen surface is important in terms of polished or oxidized condition, (2) specimen geometry is important for fast heating, (3) PID-values of control software are a considerable influence to accelerate the heating process depite thick specimens and (4) independent sample temperature determination before CGHE is strongly recommended. T2 - Intermediate Meeting of IIW Subcommission II-E CY - Genoa, Italy DA - 05.03.2018 KW - Hydrogen KW - Welding KW - Carrier gas hot extraction KW - Temperature KW - Measurement PY - 2018 AN - OPUS4-44427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rhode, Michael A1 - Münster, C. A1 - Mente, Tobias A1 - Böllinghaus, Thomas ED - Somerday, B.P. ED - Sofronis, P. T1 - Influence of experimental conditions and calculation method on hydrogen diffusion coefficient evaluation at elevated temperatures N2 - Literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels used in power plants. In fact, experimental boundary conditions and calculation methods have influence on the determination of these coefficients. The diffusion and trapping behavior in creep-resistant steel 7CrMoVTiB10-10 has been studied. Based on experimental carrier gas hot extraction (CGHE) data, a numerical model has been developed to describe the hydrogen transport and respective hydrogen distribution at elevated temperatures. The numerical results suggest that common calculation methods for diffusion coefficients are limited for experimental data analysis. The sample preparation time before CGHE experiment influences the determined diffusion coefficients with the consequence that non-homogeneous hydrogen concentration profiles have to be considered in the simulations. KW - Temperature effect KW - Hydrogen diffusion KW - Creep-resistant steel KW - Hydrogen assisted cracking KW - Carrier gas hot extraction PY - 2017 SN - 978-0-7918-6138-7 U6 - https://doi.org/10.1115/1.861387_ch56 SP - 495 EP - 503 PB - ASME CY - New York, USA ET - 1 AN - OPUS4-42502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weczera, S. A1 - Rhode, Michael A1 - Sunderkoetter, C. A1 - Plath, A. A1 - Jüttner, S. T1 - Laboratory experiments on press hardened steels in different delivered states exposed to hydrogen N2 - The legal and economical demands in the automotive industry lead to increasing efforts reducing the CO2 emissions. A way to achieve that goal is to reduce the total weight of the car and therefore the fuel consumption. With the application of high strength steels in car body manufacturing it is possible to decrease the sheet thickness of the used materials and therefore the weight of the automobile. Components made of high strength steels can be produced by cold forming as well as by hot forming. In high strength steel the hydrogen content plays a crucial role for the component behavior. It is known that the hydrogen diffusivity and solubility are based on several factors, for example increasing dislocation density by cold working processes, vacancies, chemical composition and grain boundaries. The understanding and the control of the interaction between hydrogen and the high strength press hardened steels is an important factor for the application of the materials. The scope of this work is the determination of hydrogen diffusion and permeability kinetics in press hardened steel samples. An electrochemical hydrogen permeation method was applied on boron-manganese steel grades with different rolling reduction in initial ferrite/pearlite matrix as well as for the as-quenched martensite microstructure. The diffusible hydrogen contents of the specimens were measured using the carrier gas hot extraction technique (CGHE). T2 - CHS2 2015 - 5th International conference on hot sheet metal forming of high-performance steel CY - Toronto, Ontario, Canada DA - 31.05.2015 KW - Automotive KW - High strength steel KW - Hydrogen KW - Measurement KW - Carrier gas hot extraction KW - Press-hardened KW - Martensite KW - 22MnB5 KW - Permeation PY - 2015 VL - 5 SP - 45 EP - 54 PB - Verlag Wissenschaftliche Scripten CY - Auerbach, Germany AN - OPUS4-33468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dabah, Eitan A1 - Kannengießer, Thomas A1 - Mente, Tobias A1 - Beyer, Katrin A1 - Brauser, Stephan T1 - Quantification of hydrogen effective diffusion coefficients and effusion behavior in duplex stainless steel weld metals N2 - Modern methods like carrier gas hot extraction enable the quantification of dissolved hydrogen as well as the determination of the hydrogen trapping and diffusion behavior. This method was applied in order to compare for the first time the hydrogen diffusion and trapping behavior in electrochemically charged and welded duplex stainless steel (1.4462). Characteristic extraction temperatures (400, 650, and 900 °C) were used to quantify the amounts of diffusible hydrogen and trapped hydrogen for the base material and the weld metal, and in order to calculate the effective diffusion coefficients corresponding to the specific temperature. The comparison of the charging methods showed that electrochemically charged samples have a higher content of diffusible hydrogen than the welded samples. In addition, the effusion times increase in welded samples, which indicate a higher amount of trapped hydrogen. In electrochemically charged weld samples, a significant lower concentration of hydrogen was determined than in the base material. In addition, the effective diffusion coefficients were calculated for every microstructure and charging method. It was found that the base material has a higher effective hydrogen diffusion coefficient than that of the weld metal. This effect is due to the tortuous path of hydrogen diffusion in the weld metal. KW - Carrier gas hot extraction KW - Diffusion KW - Effusion KW - Hydrogen KW - Trapping PY - 2013 U6 - https://doi.org/10.1007/s40194-013-0051-5 SN - 0043-2288 SN - 1878-6669 VL - 57 IS - 4 SP - 561 EP - 567 PB - Springer CY - Oxford AN - OPUS4-29417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Solórzano, E. A1 - Beyer, Katrin A1 - Kannengießer, Thomas T1 - The advantage of using in-situ methods for studying hydrogen mass transport: Neutron radiography vs. carrier gas hot extraction N2 - Neutron radiography (NR) is compared with the commonly used carrier gas hot extraction (CGHE) technique. We performed isothermal hydrogen effusion experiments at 623 K to study the mass transport kinetics. The investigated material was technical iron. The quantification of the hydrogen mass flow is done for NR by using concentration standards. The temporal hydrogen concentration evolution in the sample coincides well for both methods, i.e. NR and CGHE, and is in good agreement with literature. The advantages of the NR method are the non-destructive nature of measuring and the in-situ determination of hydrogen concentrations with high spatial and temporal resolution. Remaining hydrogen inside the sample can be identified directly by the NR method. KW - Hydrogen diffusion KW - In-situ KW - Neutron radiography KW - Carrier gas hot extraction KW - Imaging PY - 2013 U6 - https://doi.org/10.1016/j.ijhydene.2013.08.145 SN - 0360-3199 VL - 38 IS - 34 SP - 14725 EP - 14729 PB - Elsevier CY - Oxford AN - OPUS4-29413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -