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A seamless pipe made of AISI 321 stainless steel represented a part of a transportation Pipeline system for hydrogen-containing hot gas in a hydrocarbon cracking unit. After a service period of approximately 21 months, a segment of such pipe demonstrated the cracks, causing leakage and respective fire. For clarification of a failure root cause, various metallurgical investigations combined with numerical simulations have been applied. The results revealed that the rupture of seamless pipe was evidently influenced by hydrogen assisted cracking (HAC). An increased susceptibility of the alloy to HAC had to be attributed to its sensitive microstructure which was related to the occurrence of slip bands with a high quantity in austenite grains, particularly in the specific region underneath the outer wall surface. In addition, the intensity of restraint resulting from the T-joint weld configuration caused respectively higher triaxial stresses in the confined area on the outer wall surface where the crack started. The numerical simulations of hydrogen diffusion revealed that a uniform hydrogen concentration profile over the pipe wall thickness was reached when the service period was more than 20 months. This duration agreed well to the timeto-failure of the actual component. Considering additionally that the final stage of rupture by overload was preceded by severe HAC, as confirmed by the respective intergranular fracture topography.
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.
In the present work, the influence of deuterium on the microstructure of a duplex stainless steel type EN 1.4462 has been characterized by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) supported by scanning electron microscopy (SEM), focused ion beam (FIB), electron back scattered diffraction(EBSD) and energy dispersive x-ray (EDX) investigations. Characterization has been carried out before and after electrochemical charging with deuterium which has been used as a tracer, due to its similar behavior to hydrogen in the steel microstructure. In a first approach, the distribution of the deuterium occurring at temperatures above 58 °C has been visualized. Further it turned out that sub-surface micro blisters are formed in the ferrite-austenite interface, followed by the formation of needle shaped plates and subsequent cracking at the ferrite surface. In the austenite phase, parallel cracking alongside twins and hexagonal close packed (martensitic) regions has been observed. In both phases and even in the apparent interface, cracking has been associated with high deuterium concentrations, as compared to the surrounding undamaged microstructure. Sub-surface blistering in the ferrite has to be attributed to the accumulation and recombination of deuterium at the ferrite-austenite interface underneath the respective ferrite grains and after fast diffusing through this phase. Generally, the present application of chemometric imaging and structural analyses allows characterization of hydrogen assisted degradation at a sub-micron lateral resolution.
Influence of Hydrogen Uptake and Diffusion in Structural Components in the Field of Renewable Energy
(2021)
Great efforts are invested worldwide in the development of efficient electrolysis processes, fuel cells technologies and hydrogen transport and storage infrastructures. This includes the exploitation of existing gas-grid infrastructure for the injection of hydrogen. Considering transport and storage facilities, the utilization of gaseous hydrogen can be divided into two main groups which are differentiating in the pressure regime. Fueling stations are operating in high pressure (>800 bar) and high purity and therefore use austenitic stainless steels in their compression systems. On the other hand, existing gas infrastructure where the natural gas is transported across long distances is usually operating with up to 300 bar. In this case the pipe-systems consist of several steel classes, mainly low alloyed steels in which the surface quality and the gas mixture are strongly varying.
Even though ingress of hydrogen can lead to catastrophic failures in all steels, its exact impact on the mechanical properties, as well as its interaction with the surface, microstructure and lattice and the underlying mechanisms remain unclear. Therefore, research on the impact of gaseous hydrogen in pressure vessels and pipes has clearly an integral part on the path to safe and sustainable use of the different components along the different chains. This becomes even more relevant considering the influence of impurities in the gas, e.g. sulfur and with the introduction of new production technologies, such as additive manufacturing, into the market.
Determination of these interactions and impact that might lead to the degradation of the properties can allow a safe use of steels in present and future hydrogen-based energy applications.
The following contribution gives an overview of the problem and introduction to the conventional and innovative tools used and developed nowadays to analyze it. For this purpose, materials were loaded with hydrogen by electrochemical means and under high pressure and elevated temperatures. The results presented provide an invaluable insight into the impact of hydrogen on the integrity of selected steels used in the two mentioned above applications. This work is part of an ongoing research in which mechanical, chemical, structural, and microstructural analyses tools are combined in-situ and ex-situ.
Um die Absorption von Wasserstoff und dessen Verhalten in den Werkstoffen beim Einsatz unter Druck-H2 sowie die H- abhängigen Materialeigenschaften zu definieren, entwickelt die BAM mit ihrer langjährigen Erfahrung adäquate Prüfkonzepte, die einsatzrelevante Bedingungen und reale Beanspruchungen (Temperatur, Wasserstoff und mech. Beanspruchung) hierarchisch berücksichtigen. Der Vortrag gibt eine Einführung in das Thema von wasserstoffunterstützen Materialschäden durch die Problematik der Einspeisung von Wasserstoff in bestehende Erdgasnetze. Ferner wird auf die Hochdruck-Infrastruktur (sowie H2-Tankstellen) und die Entwicklung von Prüfkonzepten für die Gasinfrastruktur unter Druckwasserstoffbeaufschlagung eingegangen.
Increasing environmental problems with conventional energy technology are stimulating the demand for alternative energy solutions. With air quality reaching catastrophic levels in large cities worldwide, Fuel Cell Electric Vehicles offer the ideal combination of clean power with the amenities of electric drives. Hydrogen use on vehicles, nevertheless, also raises some issues about safe handling. As fuel cells and hydrogen applications, including vehicles, approach technological maturity, developing their business cases becomes crucial in introducing them to the consumer markets.
The Joint European Summer School JESS 2021 addresses these issues by offering high quality graduate level courses on selected topics of vehicle technology, innovation & business development, safe handling of hydrogen, and modelling. This series of summer schools has been ongoing since 2004 and targets an audience of university students (MSc and PhD levels) and post-doctoral researchers. We also welcome more experienced researchers and engineers wishing to expand their general knowledge, for instance, to suit a newly acquired position or collect credits for Continuous Professional Development (CPD). The course content is tailored to the needs of a diverse audience: newcomers to the field, experienced students, and young professionals working at the forefront of fuel cell and hydrogen applications.
For almost 150 years it is known that hydrogen has a deleterious effect on the mechanical properties of metallic components. Nowadays, the problem of hydrogen assisted degradation is highly relevant in energy related fields due to the massive use of steel as a structural component in these applications and its sensitivity to hydrogen. Since the discovery of hydrogen assisted cracking (HAC), researchers studied intensively and suggested possible explanations and mechanisms in order to define how hydrogen is affecting the material. In general, it is considered that hydrogen changes the mechanical properties more in terms of ductility (deformation capacities) than in strength (load capacities). Hydrogen concentration is one of three crucial factors in the degradation process, together with the microstructure of the material and the internal/external mechanical load. The relatively high concentration of hydrogen resulting in this loss of ductility can originate during production or before service (e.g. welding processes) and during service (i.e. catholically protected systems to eliminate corrosion processes in sour environments).
In parallel to the theoretical work, tremendous efforts were, and are still, invested in searching for a proper method to elucidate, map and quantify the hydrogen in the microstructure, which is the basis for this work. For steels, the focus is mainly on the observations of diffusion processes and the interaction of hydrogen with the microstructure
in regions with high local stresses/strains (for example around evolving cracks). The challenge for reaching this goal arises from the fact that accurate indication of hydrogen by means of position, unlike heavier atoms, can be made only by mass spectrometry or by interaction with another element (e.g. silver decoration, special coating and resonant nuclear reaction by nitrogen). In addition to this, the difficulty recording the hydrogen behavior while it rapidly diffuses through the material, leaving only the unpredicted failure, should be taken into account.
Although using powerful characterization methods, models and computational simulations, the key to defining the mechanisms behind HAC is still under debate and not fully understood. The relationship between material and hydrogen is determined by three factors, i.e., the material structure and microstructure – determining the physical properties, the mechanical load applied on the material and the hydrogen concentration. It is well known that in order to have a complete definition of HAC these three factors must be examined locally with the minimal scale and the maximal resolution reachable. The major gap is the lack in such a characterization method or a technique by which one has the ability to detect and observe the hydrogen in the metallic microstructure. The commonly used techniques nowadays are capable of characterization of the microstructure without the ability to observe the hydrogen distribution. Global hydrogen concentration and localized hydrogen observation are possible by some techniques which are incapable of indicating a change in the structure or microstructure therefore a comprehensive overview can be gained only by combining several methods.
In the presented research, secondary ion mass spectrometry (SIMS) was adopted as the main tool to detect and locally map the hydrogen distribution in two types of duplex stainless steel grades: EN 1.4462 (standard 2205 duplex stainless steel) and EN 1.4162 (2101 lean duplex stainless steel). The term duplex stainless steel (DSS) refers to the austenitic-ferritic microstructure of the steel where the combination of physical and mechanical properties of the two phases is achieved. The DSS was selected as a case study for this work due to the wide use of this grade in many energy and the lack of knowledge on hydrogen behavior in two-phase containing microstructures. ToFSIMS was exploited in-situ and ex-situ in three experimental approaches during or following
an electrochemical charging procedure. This type of hydrogen charging was selected as it simulated a procedure of cathodic protection of most sub-water oil and gas extraction and delivery systems. The experimental procedures were:
1. Ex-situ charging followed by ToF-SIMS imaging for basic understanding of hydrogen distribution.
2. Ex-situ charging followed by in-situ mechanical loading to obtain information on hydrogen behavior around a propagating crack.
3. In-situ permeation of hydrogen through a steel membrane inside the ToF-SIMS to obtain information on diffusion behavior of hydrogen in a two-phase microstructure.
The comprehensive view of the effect of hydrogen on steel was gained by using supplementary methods, such as high resolution scanning electron microscopy (HR-SEM), focused ion beam (FIB) and electron back-scattered diffraction (EBSD). The state of the art in this work lies in applying both: in-situ experimental approaches and data treatment of the ToF-SIMS raw data. The data treatment includes the combination of data from several sources (data fusion).
The results for the ex-situ charging followed by static sample imaging and data fusion showed that when the analyzed surface is directly exposed to the electrolyte the degradation is pronounced differently in the ferrite, austenite and interface. The degradation mechanisms in the ferrite and austenite were reflected by the formation of cracks on the surface of both, where a high concentration of hydrogen was obtained. This result supports the assumption that hydrogen is attracted to highly deformed regions. The advantage of using in-situ charging/permeation in comparison to ex-situ charging is that the effect of hydrogen on the ferrite and austenite phases when the hydrogen is evolving from within the microstructure is realized, in comparison to when the analyzed surface is initially exposed directly to the electrolyte. In both experiments the ferrite was observed as a fast diffusion path for the hydrogen. The faster diffusion of hydrogen through the ferrite is expected due to the higher diffusion coefficient, however, a direct proof for the diffusion sequence in this scale was never shown. Most significant results were achieved by the ‘core’ experiments of this research. These experiments included the design of a novel dynamic mechanical loading device to apply an external load during SIMS imaging of a hydrogen precharged-notched sample. For the first time it was shown that plastic deformation induced by applying a mechanical load is resulting in a redistribution of hydrogen locally around the notch.
The following presentation provides an overview on some of the challenges with metallic materials used as structural materials in the energy sector for the transport and storage of hydrogen. The presentation contains explanations about the methodologies utilized to characterize the susceptibility of these materials for hydrogen.
Martensitic 9 %-Cr steels like P91 and P92 can show an increased susceptibility to delayed hydrogen assisted cracking. The focus of this study was the microstructure and heat treatment effect on the mechanical properties of P92 base material and P91 multi-layer weld metal in both as-welded and post weld heat treated (PWHT) condition.
Tensile tests with hydrogen free reference samples and electrochemically hydrogen charged samples were carried out, the mechanical properties were assessed and supported by dedicated fractographic analysis. In addition, hydrogen and microstructure dependent fracture criteria were calculated. All investigated microstructures showed a hydrogen influenced degradation of the mechanical properties compared to the hydrogen free reference samples. In that connection, the as welded martensitic P91 weld metal had the highest degree of degradation in presence of hydrogen. The P91 PWHT weld metal and the P92 base material had comparable properties. From that point of view, a significantly increased risk for hydrogen assisted cold cracking during welding fabrication of P91 weld joints must be considered before any heat treatment is conducted.