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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.
Offshore wind turbines are an important goal in national energy strategies worldwide. Foundation structures are manufactured from submerged arc welded (SAW) plates with thicknesses up to 200 mm. In that connection, high-strength steels like the S420G2+M are more and more applied offering the possibility for increased stability and load-bearing capacity of the foundations. These offshore steel grades can show a susceptibility for delayed hydrogen assisted cold cracking of the weld joints. For that purpose, a minimum waiting time (MWT) of up to 48 h (dependent on applied standards) is recommended before non-destructive testing is allowed and conducted. But this concept is based on older steel grades that have been used for three or more decades. Nowadays, the metallurgical improvements (clean steels, proper rolling, and heat treatment) of base materials and well as welding consumables must be anticipated. Hence, the MWT concept should be critically discussed as it is assumed to be very conservative. For that reason, the focus of this study was to investigate the diffusion behavior in S420G2+M steel and its multi-layer SAW joint. Electrochemical permeation experiments were carried at room temperature. Boundary conditions were anticipated in terms of using different sample thicknesses. From the experimental data, hydrogen diffusion coefficients and absorbed diffusible hydrogen concentrations had been calculated. It was shown that hydrogen diffusion in the base material is increased compared to the weld metal. In addition, the sample thickness had a significant on the calculated diffusion coefficients. The minimum and maximum diffusion coefficients had been used for numerical modelling of the hydrogen diffusion in the welding joint. It became clear that a MWT must be always regarded together with a critical initial diffusible hydrogen concentration for the evaluation of a possible delayed cracking as diffusion times were mostly > 48 h due to the thick plates.
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.
Joining processes for components in hydrogen technologies: Current need and future importance
(2022)
This presentation gives an overview on the importance of joining processes for component fabrication in hydrogen technologies. For that reason, the current need and future research and developement activites are highlighted for the three technological fields: hydrogen storage, transport and use (in terms of the emerging field of additive manufacturing). Finally, some remarks are given for necessary changes in the standardization.
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.
This study gives an overview on the important field of joining processes for component fabrication in hydrogen technologies. For that reason, the current need and future research and developement activites are highlighted for the different technological field of hydrogen generation, storage, transport and use. In addition, the emerging field of additive manufacturing is included. Finally, some remarks are given for necessary changes in the standardization and its challenges.
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.
Metals that are exposed to high pressure hydrogen gas may undergo detrimental failure by embrittlement. Understanding the mechanisms and driving forces of hydrogen absorption on the surface of metals is crucial for avoiding hydrogen embrittlement. In this study, the effect of stress-enhanced gaseous hydrogen uptake in bulk metals is investigated in detail. For that purpose, a generalized form of Sievert's law is derived from thermodynamic potentials considering the effect of microstructural trapping sites and multiaxial stresses. This new equation is parametrized and verified using experimental data for carbon steels, which were charged under gaseous hydrogen atmosphere at pressures up to 1000 bar. The role of microstructural trapping sites on the parameter identification is critically discussed.
The steel grade 20MnMoNi5-5 (according to German DIN standard or 16MND5 according to French AFNOR standard) is widely applied in (weld) fabrication of reactor pressure vessel components. Thus, a wide range of welding technologies (like submerged arc welding (SAW) or tungsten inert gas (TIG)) is used resulting in different heat affected zone (HAZ) microstructures. During weld fabrication, the weld joints may take up hydrogen. Especially, the HAZ shows an increased susceptibility for a degradation of the mechanical properties in presence of hydrogen. In addition, the hydrogen-assisted degradation of mechanical properties is influenced by three main local factors: hydrogen concentration, microstructure, and load condition. Hence, the base material (BM) and two different simulated non-tempered as-quenched HAZ microstructures were examined using hydrogen-free and hydrogen-charged tensile specimens. The results indicate that the effect of hydrogen on the degradation is significantly increased in case of the HAZ compared to the BM. In addition, hydrogen has remarkable effect in terms of reduction of ductility. It was ascertained that the degradation of the mechanical properties increases in the order of BM, bainitic HAZ, and the martensitic HAZ. Scanning electron microscope (SEM) investigation showed a distinct change of the fracture topography depended on the microstructure with increasing hydrogen concentration in case of the as-quenched HAZ microstructures.
Carrier gas hot extraction (CGHE) technique was used for measurement of hydrogen in press-hardened (and as delivered) condition of 22MnB5 steel primarily coated with a thin layer of Al–Si. The CGHE technique was applied using different temperature programs: isothermal heating, temperature step, and linear heating in solid state. The effusing hydrogen was measured using thermal conductivity device (TCD) and high resolution mass spectroscopy (MS). Single isothermal heating at 400 and 900 °C allowed determining absolute value of effusing hydrogen. The linear heating, also known as thermal desorption analysis (TDA), revealed temperature dependent hydrogen effusion peaks. The deconvolution of the TDA spectra by peak fitting allowed the calculation of hydrogen desorption energies for each peak. The results showed good agreement between hydrogen concentrations measured with MS and TCD. In addition, the as-received ferrite-perlite microstructure showed only hydrogen effusion above 400 °C. The subsequent press hardening process leads to hydrogen uptake in the microstructure. In general, the press-hardened 22MnB5 revealed a hydrogen concentration of 0.4 to 0.5 ppm. The biggest concentration was released at isothermal holding at 400 °C indicating reversibly trapped hydrogen. TDA results with different heating rates confirmed mostly diffusible and reversible trapped hydrogen due to calculated activation energies in the range from 4 to 20 kJ mol-1; it was ascertained that nearly 90 % of the hydrogen left the specimens below 400 °C. Melt extraction (ME) was performed to measure the total hydrogen amount (including the diffusible and trapped hydrogen) and showed that above 900 °C up to 1 ppm hydrogen is trapped.
Low-alloyed CrMoV steels, such as T24, are widely used for welded components in fossil power stations due to their excellent creep-strength. Spectacular failure cases in the recent years exhibited severe cracking in T24 welds. The results showed that hydrogen-assisted cracking (HAC) occurring up to 200 degree Celsius cannot be excluded. Hence, a basic understanding is necessary on how hydrogen affects the material properties of welded microstructures. In this regard, each weld microstructure (HAZ and weld metal) has influence on the HAC susceptibility and respective hydrogen diffusion. Thus, the present contribution summarizes different results obtained from experiments with grades T24 (CrMoV alloy) and T22 (CrMo) and thermally simulated HAZ. Tensile tests were conducted with hydrogen charged specimens and compared to hydrogen-assisted stress corrosion cracking results obtained from slow strain rate tests (SSRT) up to 200 degree Celsius. Electrochemical permeation and degassing experiments were performed to identify a particular weld microstructure influence on hydrogen diffusion and trapping (especially in the HAZ). The results showed that T24 base material has improved resistance to hydrogen-assisted degradation/cracking. In contrast, the as-welded HAZ had remarkably increased susceptibility (tesnile tests at hydrogen concentration of 1 to 2 ppm). SSRT experiments confirmed this at elevated temperatures for both the T24 and the T22. Hence, the evaluation of a particular degradation of the mechanical properties should be performed independently for each weld microstructure. In addition, the HAZ showed decreased diffusion coefficients (at room temperature) of approximately one magnitude compared to the base materials. Trapped hydrogen was determined in the T24 at temperatures up to 120 degree Celsius compared to 75 degree Celsius in the T22. This has to be considered in case of changing operational temperatures, e.g. in the case of start-up and shutdown processes of boiler components.
Laboratory experiments on press hardened steels in different delivered states exposed to hydrogen
(2015)
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).
Low-alloyed heat-resistant steels have a fundamental contribution to the currently applied steel grades in pressurized and temperature loaded components like membrane walls(water walls)or pressure vessels. Here, the main advantages of the low-alloy concept can be used in terms of superior high temperature mechanical properties, workability and decreased amounts of expensive alloy elements. The main challenge for the future is to further increase the power plant thermal efficiency independent of the type of power plant concept, i.e. fossil-fired or nuclear power plant, where the material selection can directly affect reduction of CO2 emissions.
In power plant design, welding is the most applied manufacturing technique in component construction. The necessary weld heat input causes metallurgical changes and phase transitions in the heat affected zone (HAZ) of the base materials and in the deposited weld metal. The weld joint can absorb hydrogen during welding or in later service - This absorption can cause degradation of mechanical properties of the materials, and in certain loading conditions, hydrogen-assisted cold cracks can occur. This cracking phenomenon can appear time delayed due to the temperature dependency of the hydrogen diffusion and
the presence of a “critical” hydrogen concentration. Additionally, each specific weld microstructure shows a certain hydrogen diffusion and solubility that contribute to susceptibility of the cracking phenomenon. Therefore hydrogen cannot be neglected as possible failure effect, which was identified recently in the case of T24 creep-resistant tubeto-tube weld joints. It is necessary to identify and assess the hydrogen effect in weld joints of low-alloyed steel grades for to improve further early detection of possible failures.
For each specific weld joint microstructure, it is necessary to separate the interdependencies between mechanical load and the hydrogen concentration. The
diffusivity and solubility must be considered to identify hydrogen quantities in the material at any given time. In this case, the effects of mechanical loading were dealt with independently. For the characterization of the mechanical properties, hydrogen charged tensile specimens were investigated for the base materials and thermally simulated HAZ
microstructures. The hydrogen diffusion was characterized with the permeation technique at room temperature and at elevated temperature ranges up to 400°C - It was investigated by interpreting the hydrogen effusion behavior with carrier gas hot extraction technique (CGHE). For realistic determination of the hydrogen diffusion coefficients, an improved
method was developed encompassing accelerated specimen heating and hydrogen determination via mass spectrometer (MS). Simultaneously, the corresponding temperature
dependent trapped and total hydrogen concentrations were determined.
The determined experimental results showed increased susceptibility to the hydrogen affected
degradation of the HAZ compared to the base material, which is independent of the investigated alloy composition. In particular, the martensitic coarse grain HAZ is the most susceptible microstructure to hydrogen-affected degradation. The results of the tensile
tests allowed the definition of consistent microstructure specific failure criteria (envelope curves) versus quantified hydrogen concentrations for the reactor pressure vessel 16MND5 steel (20MnMoNi-5-5) and the creep-resistant T24 steel (7CrMoVTiB10-10). The procedure of quantifying hydrogen concentrations in HAZ microstructures is novel and supports a new method of analysis for hydrogen degradation effects. Further investigations with the T22
steel (10CrMo9-10), as compared to the creep-resistant T24 steel (7CrMoVTiB10-10),
confirmed the beneficial effect of Vanadium as an alloying element to improve the resistance to degradation. In general, Mn-Mo-Ni base material grades show a higher resistance compared to Cr-Mo steels that do not include Vanadium alloying.
The investigations showed the decreased diffusion coefficient of the HAZ microstructure compared to the base material microstructure. This is caused by the stronger trapping effects that are present which simultaneously increase the hydrogen solubility as well. In
general, trapping effects above 100°C are negligible. It is noted that after testing the T24 grade, these trapping effects were observed above 100°C and must be considered. At elevated temperatures, the calculated hydrogen diffusion coefficients are sometimes greater than those in literature. This is primarily due to the unique applied specimen heating procedure resulting in a varied hydrogen effusion from the specimen.
The significance of the obtained results can be characterized in three perspectives. First, the direct comparison of the degradation was possible in terms of microstructure-specific hydrogen effects on the mechanical properties. Second, consistent failure criteria were established to quantify degradation vs. the hydrogen concentration. Third, the determination of more accurate hydrogen diffusion coefficients is now available.
From a scientific point of view, important contributions were made to further interpret the hydrogen effects on the macroscopic mechanical properties, with respect to the alloy composition and the microstructure. From a procedural standpoint, the mentioned deviation in the elevated temperature diffusion coefficients can be caused by the calculation method. This can be an explanation for the reported data scatter in the references.
In terms of an economic view, the presented experimental results contribute to a safe and reliable weld workability of the steel grades. Thus, the identified temperature levels of hydrogen trapping can be applied in the definition of minimum preheat, interpass or postheat temperatures. In addition, recommendations for suitable dehydrogenation heat treatment (DHT) procedures, with accurate temperature values and holding times, can be derived from these results. In the future, the application of the mechanical and diffusion data is intended to support numerical analysis methods to provide an improved prediction of hydrogen effects on material degradation in weld microstructures.
Modeling of Hydrogen-Assisted Cracking (HAC) in Duplex Stainless Steels (DSS):
- Hydrogen causes significant degradation in DSS and consequently HAC
- Mechanisms of HAC have not been fully understood in two-phase microstructures
- Mesoscale numerical modeling for HAC in DSS was created, coupled to the macroscale, enabling simulation of HAC in both phases independent from predefined crack paths
Hydrogen-assisted cracking (HAC) represents a significant failure risk for (high strength) creep resistant low-alloyed steel components in fossil-fired power plant applications at temperatures of up to and above 200 °C. This particularly applies to respective start-up and shut-down processes associated with alternating service-conditions in terms of load flexible power plants. For quantitative determination of localized crack critical hydrogen concentrations, the temperature dependent hydrogen diffusion coefficients have to be determined as exactly as possible.
However, available literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels with similar microstructures. Additionally, the available diffusion data seem not to be very reliable and their scatter increases with decreasing temperature. One reason is that the experimental boundary conditions can have a major impact on the determination of respective effective diffusion coefficients. Hence, the scope of this study is to evaluate the influence of the experimental boundary conditions on the derived diffusion coefficients. In addition, different methods for calculating diffusion coefficients are discussed. To elucidate such influences and to draw a line to practical application, the diffusion and trapping behavior in the creep resistant steel 7CrMoVTiB10 10 has been studied.
For such purpose, hydrogen charged specimens were isothermally degassed at different temperatures using carrier gas hot extraction (CGHE). Based on experimental data, a numerical model has been developed by which the hydrogen transport behavior and the respective hydrogen distribution during CGHE can be assessed.
It is demonstrated that the specimen heating rate has a large influence on the calculated diffusion coefficients under assumption of isothermal degassing which elsewhere has been underestimated in the assessment of diffusion data in creep-resistant steels. The numerical results suggest that calculation methods for diffusion coefficients are limited if compared to experimental results. It also turned out that the sample preparation time before CGHE can enormously influence determined diffusion coefficients. Consequently, non-homogeneous hydrogen concentration profiles have to be anticipated in the simulations to arrive at characteristic effusion curves consistent to respective CGHE experiments. In turn, validated diffusion coefficients are now available for the low-alloyed Cr-Mo-V steel, which can be helpful to calculate appropriate hydrogen removal heat treatment procedures.
In the field of modelling hydrogen assisted cracking (HAC) phenomenon, hydrogen diffusivity is an important input parameter for numerical simulation. In terms of hydrogen diffusion coefficients, they have great impact on realistic assessment of the evolution of possible crack critical hydrogen concentrations. In addition, the chemical compositions of steels can have a strong effect on hydrogen diffusion. Unfortunately, literature provides a wide range of available hydrogen diffusion coefficients even for similar microstructures and equal temperatures. The scattering of the data can lead to significant deviations in the results of simulating the evolving hydrogen concentrations due to hydrogen uptake (by fabrication or service). Thus, the application of such data to crack-models or for component life tie predictions can be realized up to the present only by considering envelope curves of such value, corresponding to a work or bench case scenario, respectively. For improved reliability of numerical simulaitons, it is necessary to minimize the mentioned deviation of these data. Hence, this work focuses on the validation of hydrogen diffusion coefficients obtained from permeation experiments at room temperature. Two baintic steels with different alloying concepts were investigated, the creep-resistant 7CrMoVTiB10-10 and the reactor pressure vessel grade 20MnMoNi4-5. A numerical model is presented for simulation of the corresponding hydrogen diffusion during permeation experiments using the finite element software ANSYS. Three different diffusion coefficients (obtained from different common calculation methods) are considered and compared to numerical results. The vases of thes calculation methods are permeation transients which are a direct measure for hydrogen. The results of the simulated hydrogen diffusion coefficients show that only one procedure for calculation of diffusion coefficitnes is suitable in comparision to the experimental values. Thus, it is suggested to use this method for analysis of experimental results in case of hydrogen diffusion during permeation experiments. Furthermore, this work supplies validated values for the hydrogen diffusion coefficients of both steel grades.
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 the presence of hydrogen increases significantly with increasing yield strength. In case of missing knowledge about how and the amount of hydrogen that 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 economical benefits. This work presents the influence of welding parameters on the diffusible hydrogen content in both (1) single-pass and (2) multi-layer welds. Different
hydrogen concentrations were detected by varied contact tube distance, wire feed speed, arc length, and 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 has been reduced. Whereby, differences in hydrogen concentrations between both arc types are present.
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.
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).