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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).
Hydrogen generally causes lattice distortions and phase transformations when introduced into a metallic crystal lattice. For the investigations reported in this contribution, hydrogen thermal desorption analysis has been carried out to observe the influence of hydrogen desorption on the lattice of super martensitic stainless steel during continuous heating. The lattice expansion parameter and the phase transformations have been monitored during the thermal desorption process, and the influence of hydrogen on such characteristics has been evaluated. It was found that hydrogen has a significant influence on both the lattice parameter and on the thermal expansion. However, hydrogen has no influence on phase transformation during thermal desorption. The hydrogen's desorption behavior in this process was also observed and it turned out that hydrogen desorbs in two stages, i.e., firstly diffusible hydrogen and trapped hydrogen afterward.
Quite a number of models for hydrogen distribution in steels and welds have been developed in the past 20 years. They reach from simple analytical models to more complex two and three dimensional finite element simulations. So far, these models have been used to simulate hydrogen distribution in homogeneous microstructure. This paper contributes to numerical simulation of hydrogen distribution in heterogeneous microstructure, e. g. in a duplex stainless steel microstructure consisting of two phase fractions. Under appropriate conditions, such as cathodic protection, it is possible that hydrogen is absorbed leading to material embrittlement and possibly initiating hydrogen assisted cracking. In order to avoid hydrogen assisted cracking in duplex stainless steels, it is of great interest to know more about the diffusion behavior of the ferrite and austenite phase. A numerical model has been developed that operates on the mesoscale and enables simulation of hydrogen transport in the various phases of a metallic material. As a first application of this model, hydrogen distribution in a duplex stainless steel 1.4462, consisting of approximately equal portions of ferrite and austenite, was simulated using the finite element program package ANSYS. The results reflect the dependency of hydrogen distribution on the microstructural alignment of the ferrite and austenite phase fractions. Crack-critical areas can thus be identified, provided the critical strain-hydrogen combination is known for the respective microstructural phase.
Quite a number of numerical models for hydrogen-assisted cracking in different kind of steels are existing reaching from simple analytical models to more complex two- and three-dimensional finite element simulations. These numerical models have been used to simulate the processes of hydrogen-assisted cracking in homogeneous microstructure. This paper contributes to numerical simulation of hydrogen-assisted cracking in heterogeneous microstructure, e.g., in a duplex stainless steel microstructure consisting of two phase fractions. If hydrogen is absorbed during welding or during service, i.e., due to cathodic protection, hydrogen is leading to material embrittlement and leads to hydrogen-assisted cracking. In order to improve understanding of the mechanisms of hydrogen-assisted cracking in duplex stainless steels, a numerical model has been created that operates at the mesoscale and enables simulation of stress–strain distribution as well as cracking in the various phases of a metallic material. Stress–strain distribution and hydrogen-assisted cracking in the duplex stainless steel 1.4462, consisting of approximately equal portions of ferrite and austenite, was simulated using the finite element program ANSYS. It was shown by numerical simulation that higher local stresses and strains are present at ferrite and austenite than the global stresses and strains in the duplex stainless steel, while the highest plastic deformations occur at austenite and the highest stresses can be found in small ferrite bars surrounded by ductile austenitic islands. By analyzing the stress–strain distribution in the duplex microstructure, crack critical areas in the ferrite can be identified. Hydrogen-assisted cracking was modeled assuming high hydrogen concentrations and regarding the local mechanical load in each phase of the duplex stainless steel. The mesoscale model qualitatively reflects the crack initiation and propagation process in the ferritic and austenitic phase of the duplex stainless steel.
Welded components of P91 9% Cr steel demand for careful welding fabrication with necessary post weld heat treatment (PWHT). Before the PWHT, a hydrogen removal heat treatment is necessary for avoidance of hydrogen assisted cracking (HAC). In this context, the microstructure and temperature-dependent hydrogen diffusion is important, and reliable diffusion coefficients of P91 weld metal are rare. For that reason, the diffusion behavior of P91 multi-layer weld metal was investigated for as-welded (AW) and PWHT condition by electrochemical permeation experiments at room temperature and carrier gas hot extraction (CGHE) from 100 to 400 °C. Hydrogen diffusion coefficients were calculated, and the corresponding hydrogen
concentration was measured. It was ascertained that both heat treatment conditions show significant differences. At room
temperature the AW condition showed significant hydrogen trapping expressed by to seven times lower diffusion coefficients. A preferred diffusion direction was found in perpendicular direction expressed by high permeability. The CGHE experiments
revealed lower diffusion coefficients for the AW condition up to 400 °C. In this context, a hydrogen concentration of approximately 21 ml/100 g was still trapped at 100 °C. For that reason, a certain HAC susceptibility of as-welded P91 weld metal cannot
be excluded, and hydrogen removal should be done before PWHT.
Effect of Tensile Loading and Temperature on the Hydrogen Solubility of Steels at High Gas Pressure
(2023)
The hydrogen solubility in ferritic and martensitic steels is affected by hydrostatic stress, pressure, and temperature. In general, compressive stresses decrease but tensile stresses increase the hydrogen solubility. This important aspect must be considered when qualifying materials for high‐pressure hydrogen applications (e.g., for pipelines or tanks) by using autoclave systems. In this work, a pressure equivalent for compensating the effect of compressive stresses on the hydrogen solubility inside of closed autoclaves is proposed to achieve solubilities that are equivalent to those in pipelines and tanks subjected to tensile stresses. Moreover, it is shown that the temperature effect becomes critical at low temperatures (e.g., under cryogenic conditions for storing liquid hydrogen). Trapping of hydrogen in the microstructure can increase the hydrogen solubility with decreasing temperature, having a solubility minimum at about room temperature. To demonstrate this effect, the generalized law of the hydrogen solubility is parameterized for different steels using measured contents of gaseous hydrogen. The constant parameter sets are verified and critically discussed with respect to the high‐pressure hydrogen experiments.
Hydrocarbons fuel our economy. Furthermore, intermediate goods and consumer products are often hydrocarbon-based. Beside all the progress they made possible, hydrogen-containing substances can have severe detrimental effects on materials exposed to them. Hydrogen-assisted failure of iron alloys has been recognised more than a century ago. The present study aims to providing further insight into the degradation of the austenitic stainless steel AISI 304L (EN 1.4307) exposed to hydrogen. To this end, samples were electrochemically charged with the hydrogen isotope deuterium (2H, D) and analysed by scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). It was found that deuterium caused a phase transformation from the original γ austenite into ε- and α’-martensite. Despite their low solubility for hydrogen, viz. deuterium, the newly formed phases showed high deuterium concentration which was attributed to the increased density of traps. Information about the behaviour of deuterium in the material subjected to external mechanical load was gathered. A four-point-bending device was developed for this purpose. This allowed to analyse in-situ pre-charged samples in the ToF-SIMS during the application of external mechanical load. The results indicate a movement of deuterium towards the regions of highest stress.
The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed.
To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place.
By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and
deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules.