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As a chemical metrology tool time-of-flight secondary ion mass spectrometry (ToF-SIMS) has become a very popular technique to monitor the elemental, isotopic and molecular distribution in two or three dimensions. Its reduced sampling depth, high sensitivity, great structural specificity and the direct detection of hydrogen thereby increase the emergence of ToF-SIMS for material and analytical surface science, particularly due to recent instrumental developments improving mass, depth and lateral resolution. For basic surface science, adsorption processes and surface reactivity thus can be investigated in high detail on organic as well as inorganic samples. The use of multivariate data analysis in addition can effectively assist to identify trends in the complex SIMS raw data set and define key co-variances between certain samples or mass spectra. In this contribution the essence of ToF-SIMS is illustrated by discussing two highly relevant energy applications. First, for piezoelectric electroceramics oxygen exchange active zones have been visualized to determine the impact of external field-load to the oxygen vacancy distribution between anode and cathode. As a second case study the interaction of hydrogen species with the microstructure of a duplex stainless steel was investigated. It was concluded that ToF-SIMS has a valuable essence for detailing hydrogen related degradation mechanisms.
Deuterium permeation and cracking in duplex steels as viewed by ToF-SIMS and HR-SEM with data fusion
(2016)
Better understanding of hydrogen assisted degradation and trapping mecha-nisms requires sufficient imaging techniques for respective hydrogen-microstructure interaction studies, in particular with multi-phase metallic micro-structures [1]. The present work is focusing on the elucidation of deuterium be-havior in two austenitic-ferritic duplex stainless steels (DSS) under the assumption that deuterium behaves in many ways similarly to hydrogen [2]. For case studies standard 2205 and lean 2101 DSSs were chosen due to the extensive use of these steels in industry [3]. The analyses were conducted by using a novel in-situ permeation and Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging technique or by ex-situ ToF-SIMS imaging following electrochemical charging experiments. Another pioneering procedure was data fusion (including chemometry) of results of powerful laterally resolved chemical analysis and high resolution structural characterization techniques .
Results for the ex-situ observations showed a different influence of deuterium loading on the two steel grades as well as different damage mechanisms in each phase. Formation of sub-surface blisters between the ferrite and austenite were obtained in both the standard and the lean DSS. In both steels, an increased deuterium concentration was observed around deformed regions such as cracks, confirming that they originate from the presence of deuterium [4]. The formation of parallel cracks was obtained only in the austenite within the standard duplex whereas in the lean duplex the highest intensity of deuterium was obtained in the austenite along the ferrite-austenite interphase.
In comparison, application of the novel in-situ permeation technique enabled to register and record the deuterium permeation through the material and the respective saturation sequence of the two phases as well as the interfaces. Faster diffusion of the deuterium was observed in the ferrite and a direct proof for deuterium enrichment at the austenite-ferrite interface has been given [1]. The integration of the specified techniques gives a better insight into the processes leading to hydrogen induced failure. These two experimental techniques provide very valuable tools for elucidation of respective metallurgical failure mechanisms that can be used for the validation of respective numerical models for hydrogen assisted cracking (HAC).
Hydrogen has great potential on the path towards decarbonization of the energy and transport sectors and can mitigate the urgent issue of global warming. It can be sustainably produced through water electrolysis with potentially zero emissions, and efficiently used (e.g., in fuel cell systems). Despite its environmental advantages, hydrogen-metal interactions could result in the degradation of the mechanical properties of several structural materials. In order to determine the magnitude of the material degradation in relation to hydrogen exposure, extensive material testing is required. The standardized procedure for in-situ testing for the quantification of the impact of compressed gaseous hydrogen (CGH2) relies on the utilization of an autoclave around the tested specimen. Such test set-up is complex, expensive, time-consuming and requires special equipment, trained personnel, and strict safety procedures. A relatively recent method to circumvent these issues and provide affordable results consists of using hollow specimens, thus applying the hydrogen pressure inside rather than outside the specimen. It allows to reduce the volume of hydrogen by several orders of magnitude and to perform the tests more efficiently and in a safer manner. This study focuses on evaluating the tensile properties of X65 vintage pipeline steel tested in a high-pressure hydrogen environment using hollow specimens. Tests are performed in 6 MPa H2 and Ar at the nominal strain rate of 10−6 s−1 to evaluate the reduced area at fracture and the elongation loss. The effect of surface finishing on crack initiation and propagation is investigated by comparing two different manufacturing techniques. In this way, this study provides insights into the applicability of a novel, reliable, and safe testing method which can be used to assess the hydrogen-assisted ductility loss in metallic materials.
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.