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Current interest in hydrogen gas as an energy source is growing due to its attractive properties such as high chemical energy density and the fact that its combustion produces water as by-product, qualifying this gas as an appealing clean energy source. In particular, the use of molecular hydrogen in automotive applications such as the hydrogen internal combustion engine (HICE) or hydrogen fuel cells is an excellent clean alternative.
Despite these promising opportunities, hydrogen gas has a distinct disadvantage as an everyday energy medium, that is, it is highly flammable. Hydrogen processing apparatuses should therefore be constantly monitored so that leaks are immediately detected. The implementation of direct sensing systems for H2(g) is thus a decisive factor for its application and acceptance as a clean energy source. Because the automotive market alone is already a mass market, these sensors do not only have to be reliable, robust and dimensionally small, but operation has to be simple and the device itself cost-effective. In addition, very low detection limits are a must as already escape of small quantities of H2(g) is directly related to public health and safety. Besides electrochemical or semiconductor sensors, optical sensors are especially appealing because the equipment is usually simple and accessible, easily miniaturized and measurements can be performed in situ and in real time.
If one cannot rely for instance on metallic palladium as interacting matrix, a major challenge for optochemical hydrogen sensors is to find a suitable material that fulfils all the requirements mentioned above and undergoes a dedicated indication reaction with H2(g). One such alternative can be Metal-Organic Frameworks (MOFs) which constitute a predefined, organized, mesoporous structure built up from metal ions and organic bridging ligands. With a myriad of building blocks being available, MOFs can be equipped with internal H2 reception sites that shall allow for selective and sensitive indication. For instance, if Pd ions are implemented in such a way that they express open metal sites (OMS), these OMS shall possess a strong affinity for hydrogen. If light absorbing and emitting organic ligands are additionally chosen, luminescent MOFs (LMOFs) can result that are perfect candidates for optical sensors, as changes at the analyte reception site can be effectively transduced into a measurable signal.
In this contribution, we intended to discuss the development of a new luminescent sensor material for the detection of the highly flammable H2(g). This sensor material is based on an LMOF assembled from Pd(II) and aromatic bridging ligands, the advent of hydrogen at the OMS in the LMOF producing distinct variations in the material’s optical properties.
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.
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.
In the course of tomorrow's hydrogen-based energy transition, the construction of the corresponding infrastructure will play a central role. In that context, large diameter long-distance transmission pipelines for hydrogen will be the backbone in the European Union with service pressures from 70 to 90 bar (e.g., depending on national regulations). It is a major goal to rededicate the existing LNG infrastructure despite the necessity of new pipelines. From that point of view repairing of such transmissions pipelines via welding can be necessary. For the LNG infrastructure, it is state of the art that repair welding is conducted at pipelines under service, i.e., the LNG is still flowing as pressurized gas in the steel pipes. The reason is that a shut-down of large diameter pipelines is not so easy or sometimes impossible. In fact, as long no oxygen enters the pipeline, there would be any combustion or (in the worst case) explosion. At the moment, it is entirely open if current repair welding procedures for LNG pipelines can be transferred to pure hydrogen pipelines. In opposite to LNG, hydrogen can be way easier absorbed to the pipeline steels and diffuses through the material. If it accumulates in susceptible regions, i.e., in the welded joint, hydrogen assisted embrittlement could occur. The planned welding procedure requires a so-called preheating and maintenance of the weld joint of up to 300°C for several hours. This temperature is way higher compared to the typical service temperature of max. 40 to 50°C at operational pressures of 100 bar. In accordance to API 941, these low-alloyed pipeline steels are subjected to short-term service loads, which they are not designed for. For that reason, a collaborative project between BAM and DVGW (German Association for Gas and Water professions) was initiated in 2022 to answer the following questions by experiments and numerical simulation of: (1) How many hydrogen is additionally absorbed during the heating of the material to max. 300°C under remaining operational pressures? (2) Is the hydrogen concentration sufficient to reach a critical condition? (3) Which material and weld microstructure is the most susceptible? (4) Is there a significant difference in the repair welding behavior of LNG pipelines that had been already in use for long-term? (5) Which welding parameters and joint dimensions must be ensured for safe repair welding repair of typical pipelines? For that reason, the present study gives an overview on the current practice in repair welding of in-service pipelines, the industrial importance of this topic for the hydrogen-based energy transition and summarizes first results.
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.
Fatigue crack propagation investigations have been performed in austenitic-ferritic duplex stainless steel H22N5M3 in air and during hydrogen charging, using various frequencies of loading. Strong differences of crack propagation velocity depending on the test conditions were noticed. Lower frequency with applied hydrogen charging led to the huge increase of crack propagation velocity compared to the tests performed in air. To understand such a behaviour in each case and characterize crack mode, the samples were observed using electron back-scattered diffraction (EBSD). It was shown that in air, the fatigue crack propagation involved plastic deformation and the resulting cracks had ductile character. The presence of hydrogen led to more brittle mode of cracking. This effect was also connected with frequency of loading: lower frequency, which assured longer time for hydrogen-crack tip interaction, resulted in the highest crack propagation velocity and the brittle cracking mode with lower amount of plastic deformation. The performed observations indicated that the path of the crack went mostly transgranularly through both austenite and ferrite phases. Phase and grain boundaries were not the preferred paths for crack propagation.
The hydrogen influence on the microstructure of the austenitic-ferritic Cr22-Ni5-Mo3 stainless steel was investigated. Cathodic hydrogen charging was performed electrochemically from aqueous solution of 0.1M H2SO4 with hydrogen entry promoter addition. The aim of this study was to reveal microstructural changes appearing during the hydrogen charging and particularly to clarify the occurrence of phase transformations induced by hydrogen. The specific changes in both phases of steel were observed. In the ferritic phase, strong increase of dislocation density was noticed. Longer time of hydrogen charging leaded also to the strips and twin plates formation in ferrite phase. In the austenitic phase, the generation of stacking faults, followed by the formation of α' martensite was remarked.
Molybdenum disulfide (MoS₂) is a well-known solid lubricant for tribosystems running in vacuum or dry gases. Problems arise due to its sensitivity to humidity, which is a drawback for its application under ambient conditions. However, by using a physical vapor deposition (PVD) process, deposition parameters can be optimized not only to gain a coatings structure with favorable frictional properties but also to minimize the sensitivity to attack by water molecules. Therefore, an improved tribological behavior even under moist conditions can be achieved. MoS₂coatings are also candidates for being applied at cryogenic temperatures. They already have proven their suitability, e.g., for sliding support elements between superconducting magnets of the nuclear fusion-experiment Wendelstein 7-X. However, these coatings were exclusively produced for this particular application and the utilization for more common tribosystems may be precluded due to cost considerations. In view of a wider range of applications, pure and Cr containing PVD-MoS₂ coatings with an optimized structure were tested under varying environments including hydrogen gas and cryogenic temperatures. Results of the most promising variant are presented in this paper.