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Metallic materials, predominantly steels, are the most common structural materials in the various components along the hydrogen supply chain. Ensuring their sustainable and safe use in hydrogen technologies is a key factor in the ramp-up of the hydrogen economy. This requires extensive materials qualification, however, most of the accepted; and standardized test methods for determining the influence of gaseous hydrogen on metallic materials describe complex and costly procedures that are only available to a very limited extent worldwide. The hollow specimen technique is a simple, rapid, and economical method designed to overcome the limitations of the current methods for the qualification of metallic materials under high-pressure hydrogen gas. However, this technique is not yet standardized. The TransHyDE-H2Hohlzug project is presented in this article, along with the main steps required to optimize the hollow specimen technique. This includes closing knowledge gaps related to the specimen geometry, surface quality, and gas purity in dedicated working packages, thus contributing to a comprehensive standardization of the technique for tests in high-pressure hydrogen gas.
The high potential of hydrogen as a key factor on the pathway towards a climate neutral economy, leads to rising demand in technical applications, where gaseous hydrogen is used. For several metals, hydrogen-metal interactions could cause a degradation of the material properties. This is especially valid for low carbon and highstrength structural steels, as they are commonly used in natural gas pipelines and analyzed in this work.
This work provides an insight to the impact of hydrogen on the mechanical properties of an API 5L X65 pipeline steel tested in 60 bar gaseous hydrogen atmosphere. The analyses were performed using the hollow specimen technique with slow strain rate testing (SSRT). The nature of the crack was visualized thereafter utilizing μCT imaging of the sample pressurized with gaseous hydrogen in comparison to one tested in an inert atmosphere.
The combination of the results from non-conventional mechanical testing procedures and nondestructive imaging techniques has shown unambiguously how the exposure to hydrogen under realistic service pressure influences the mechanical properties of the material and the appearance of failure.
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.
The Tsumeb Mine in Namibia represents one of the best-preserved mining sites in the world and is rapidly gaining cross-disciplinary interest among cultural and engineering scientists. Most of the open pit and the shaft mining equipment are still in place, including the ore processing units and the local power plant. The mining area thus deserves recognition as an industrial world heritage site, especially due to the rarity of such locations on the African continent. The Shaft #1 headgear, built in 1924, represents one of the oldest known riveted steel headgears of the Promnitz design worldwide. In contrast to similar steel structures located in the northern hemisphere, it has been exposed to a different rural semi-arid climate since it is located in the Otavi Mountain Land, characterized by semi-annual change of rainy and dry seasons. Parts of the Shaft #1 headgear have remained largely untouched for more than 70 years. Besides its outstanding heritage value, it thus also represents an interesting object for studying the composition of corrosion layers formed on mild steel surfaces when exposed to continental and industrial mining atmospheres. To find a suitable transparent corrosion prevention coating, various on-site coating samples were evaluated after 11 months of outdoor exposure, including Owatrol Oil®, which is based on natural oil and alkyd resin with strong wicking potential. The substance is frequently applied for the conservation of single components but is not yet widely used on large steel structures in the field of industrial heritage conservation. However, it represented the most stable anti-corrosion coating under the local atmospheric conditions in the on-site tests. Thus, the suitability of Owatrol Oil® as a transparent coating for corrosion protection of riveted mild steel structures in such climates was further investigated as a more recent approach for the conservation of large steel structures. Since the protective coatings are exposed to strong UV radiation in the local climate, the addition of a specific UV stabilizer mixture was also tested. For such laboratory tests, two mild steel samples were taken. The first one originated from a diagonal strut of the 1920s and the second one from a handrail mounted in the early 1960s. Using corresponding high-resolution scanning electron microscopy (HR-SEM) and energy-dispersive X-ray spectroscopy (EDX) it was found that the corrosion layers are predominantly composed of lepidocrocite and goethite. A weathering program simulating the specific environmental conditions at Tsumeb in a UV climate chamber was developed and the corrosion resistance of the mild steel surface was subsequently evaluated by potentiodynamic measurements. Such tests proved to be a fast and reliable procedure for ranking the corrosion resistance of the old mild steels. It was found that the long-term corrosion layers already provide significant protection against further corrosion in the simulated environment. However, the study also showed that this can be further improved by the application of the Owatrol Oil® as a protective coating that also seals crevices. The addition of the UV stabilizers, however, led to a significant deterioration in corrosion protection, even in comparison to that of the uncoated long-term corrosion layers on the surface. Regular overcoating seems more advisable for the long-term preservation of the Shaft #1 headgear than modifying the Owatrol Oil® Coating with the tested UV-stabilizing additives.
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.
Due to the increasing global demand for pure silver, native wire silver aggregates in very high purities are gaining more industrial attention. Up to the present, no substantial metallurgical Investigation of natural wire silver exists in the accessible literature. To convey urgently needed cross-disciplinary fundamental knowledge for geoscientists and metallurgical engineers, twenty natural wire silver specimens from eight different ore deposits have been investigated in detail for the first time by EBSD (Electron Back Scattering Diffraction), supported by light microscopy and micro-probe analyses. The improved understanding of the natural silver wire microstructure provides additional Information regarding the growth of natural silver aggregates in comparison to undesired artificial growth on electronic devices. Clear evidence is provided that natural silver curls and hairs exhibit a polycrystalline face-centered cubic microstructure associated with significant twinning. Although the investigated natural wire silver samples have relatively high purity (Ag > 99.7 wt.-%), they contain a variety of trace elements such as, S, Cu, Mn, Ni, Zn, Co and Bi, As and Sb. Additionally, Vickers micro-hardness measurements are provided for the first time which revealed that natural silver wires and curls are softer than it might be expected from conversion of the general Mohs hardness of 2.7.