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Hydrogen absorption and diffusion in T24 steel weld joints and effect on mechanical properties
(2018)
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.
Hydrogen absorption and diffusion in T24 steel weld joints and effect on mechanical properties
(2018)
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.
Aircraft main landing gear (MLG) components are commonly manufactured from low-alloyed, martensitic, ultra-high strength steels (UHSS) that have to be coated for corrosion protection, representing an expensive and environmentally harmful production step. To avoid already partly banned corrosion protection plating, the new high-alloyed UHSS, Ferrium S53 (UNS S10500), has been designed to replace lowalloyed legacy materials and has been subjected to a limited field test over five years. As with the legacy alloys, UNS S10500 has a fully hardened martensitic microstructure known to be susceptible to hydrogen assisted cracking, per se. Containing about 10 wt% Cr, steels such as S10500 are at the lower limit for corrosion resistant alloys. Similar to super-martensitic stainless steels used in the oil and gas industry, a common failure sequence in marine environments represents pitting and subsequent hydrogen assisted stress corrosion cracking (HASCC). For addressing such phenomena quantitively, as required for respective lifetime assessments of MLG components and systems, the tolerance of such materials dependent on the absorbed hydrogen concentration must be evaluated quantitatively. However, there is a lack of such valuable materials data, as well as of the fractographic behavior dependent on the hydrogen concentration that might be absorbed during HASCC. To provide an improved understanding of the hydrogen dependent mechanical and fractographic behavior, samples of the legacy AISI 4340 and the new S10500 MLG steels have electrochemically been hydrogen-saturated and subjected to tensile testing. In contrast to a previous study, this contribution for the first time focuses on materials that have been salvaged from real service used landing gear components. In this study, it has been demonstrated that the service-applied S10500 steel has not only a higher strength, but also an improved ductility in comparison to the legacy AISI 4340 steel after similar service durations that provides a higher tolerance against hydrogen concentrations that might be absorbed during potential pitting and HASCC in marine environments. In addition, it has been found that the absorbed hydrogen concentration significantly affects the fracture behavior. Interestingly, hardening of the hydrogen charged low-alloyed AISI 4340 steel changes the fracture topography from trans- toward intergranular, while hardening of the S10500 steel turned the fracture topography from inter- to transgranular at respectively high hydrogen concentrations.
Spectacular failure cases of fossil power stations in the recent years exhibited severe cracking in T24 welds. The results show that hydrogen-assisted cracking up to 200 °C cannot be excluded. Hence, it is important to gain a basic understanding on how hydrogen might affect the basic material properties in the respective weld microstructures. The present study focuses on hydrogen degradation of the respective weld microstructures, i.e., the weld metal and the coarse grained heat affected zone, where actually cracking appeared in practice. Tensile tests were carried out for coarse grain heataffected zone (CGHAZ) and the weld metal in uncharged and electrochemically hydrogen-charged condition. It turned out that both microstructures show distinct tendency for gradual degradation of mechanical properties in the presence of increasing hydrogen concentration. Already for a hydrogen concentration about and above 2 ml/100 g Fe, a significant ductility reduction has been observed. SEM investigations revealed that the fracture topography changes from ductile topography in uncharged condition to intergranular topography for the CGHAZ and to ductile-brittle mix for the weld metal (WM) in hydrogen charged condition. Ti-rich inclusions were identified as central regions of quasi-cleavage fracture areas in the WM. An approximation procedure is applied to quantify the degradation intensity.
Quantitative investigations of hydrogen dependent properties of aircraft landing gear materials have only scarcely been carried out in the past. They are essential for respective component life time assessments. To better understand the behavior of these landing gear materials in a hydrogen rich environment, specimens were charged in the condition as delivered with known concentrations of hydrogen and then mechanically tested to evaluate the degradation effects. The present contribution is focused on evaluating the hydrogen concentration dependent material properties and the respective fracture topographies of the two investigated steels, and then continued by the comparison of the results with other previously investigated martensitic steels in order to better understand the thresholds for these materials to maintain structural integrity.
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.
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).
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.
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.
High-entropy alloys (HEAs) are characterized by a solid solution of minimum five and medium-entropy alloys (MEAs) of minimum three principal alloying elements in equiatomic proportions. They show exceptional application properties, such as high-strength and ductility or corrosion resistance. Future HEA/MEA-components could be exposed to hydrogen containing environments like vessels for cryogenic or high-pressure storage where the hydrogen absorption and diffusion in these materials is of interest. In our study, we investigated the HEA Co20Cr20Fe20Mn20Ni20 and the MEA Co33.3Cr33.3Ni33.3. For hydrogen ingress, cathodic charging was applied and diffusion kinetic was measured by high-resolution thermal desorption spectros-copy using different heating rates up to 0.250 K/s. Peak deconvolution resulted in high-temperature desorption peaks and hydrogen trapping above 280 °C. A total hydrogen concentration > 40 ppm was identified for the MEA and > 100 ppm for HEA. This indicates two important effects: (1) delayed hydrogen diffusion and (2) considerable amount of trapped hydrogen that must be anticipated for hydrogen assisted cracking phenomenon. Local electrochemical Volta potential maps had been measured for the hydrogen free condition by means of high-resolution Scanning Kelvin Probe Force Microscopy (SKPFM).