Since hydrogen is an alternative energy source and has both economic and environmental benefits, it has received more attention. To use hydrogen a certain condition must be met, safe pressurized containers which are often made of metal. The metal isrequired due to the high mechanical strength and reasonable cost. The problematic part is that hydrogen affects the mechanical properties of the material. Using metal in an environment with hydrogen will break down and lead to Hydrogen Environmental Embrittlement (HEE). If hydrogen will be used safely, understanding its effect on high-strength steel is necessary. Many studies have been done on hydrogen embrittlement, but it is not sufficient and therefore studies are still ongoing. The goal is to create further understanding of when components exposed to hydrogen in their service environment, in terms of mechanical, fracture surface and microstructural aspects. There are two types of stainless steel that was examined, 304 stainless steel (304 SS) and 316L stainless steel (316L SS), all specimens are cylindrical. The study mainly focused on mainly experimental aspects with some simulations. To charge the samples with hydrogen, a cathodic charging method was chosen. For fast strain rate, samples were loaded from 12 to 48 hours while slow strain rate was not preloaded. Measurement and Digital image correlation (DIC) were used due to slippage during tensile testing, it would also provide the actual engineering stress-strain curve. To see the microstructure, it was sanded, polished and etched. A special container was created to test the slow strain rate. This was done through several different tests. Both types of steel were affected by hydrogen, the yield strength and ductility were reduced. Charging at the slow strain rate leads to extreme embrittlement compared to the high strain rate. The grain boundaries had decreased in size after being charged with hydrogen. The 304 SS grains were more difficult to detect compared to the 316L SS. Different types of factors can affect the result, for the slow strain rate, hydrogen was present all the way until it reached its breaking point and after it started diffusion. Meanwhile, the hydrogen diffusion started at a high strain rate when it was taken out from charging in the container. During the time it takes to place the sample in the tensile testing machine and do the tensile test, the hydrogen diffuses, and it results in less brittleness. Keywords: Hydrogen embrittlement, tensile test, DIC, metallographic. / Eftersom väte är en alternativ energikälla och har både ekonomiska och miljömässiga fördelar har det fått mer uppmärksamhet. För att använda väte måste vissa villkor uppfyllas, det krävs säkra trycksatta behållare som ofta är gjorda av metall. Metall används på grund av kravet på hög mekanisk hållfasthet och rimliga kostnader. Den problematiska delen är att väte påverkar de mekaniska egenskaperna hos materialet. Genom att använda metall i en miljö med vätgas kommer att brytas ned och leda till vätmiljöförsprödning. Om väte kommer att användas på ett säkert sätt är förståelsen för dess effekt på höghållfast stål nödvändig. Det har gjorts många studier om väteförsprödning men det är inte tillräcklig och därför pågår undersökningar fortfarande. Målet är att skapa ytterligare förståelse för när komponenter som utsätts för väte i deras servicemiljö, när det gäller mekaniska, sprick ytan och mikrostrukturella aspekter. Det finns två typer av rostfritt stål som undersöktes, 304 rostfritt stål (304 SS) och 316L rostfritt stål (316L SS), alla prov är cylindriska. Studien fokuserade huvudsakligen på huvudsakligen experimentella aspekter med vissa simuleringar. För att ladda proverna med väte valdes en katodisk laddningsmetod. För snabb töjnings hastighetladdades proverna från 12 till 48 timmar medan långsam töjnings hastighet förladdades inte. Mätning och Digital bildkorrelat (DIC) användes på grund av glidning under dragprovning, dettaskulle ge den korrekta ingenjörs spänning-töjningskurvan. För att se mikrostrukturen så slipades, polerades och etsning utfördes. En speciell behållare skapades för att testa den långsamma töjnings hastighet. Detta gjordes genom flera olika tester. Båda typerna av stål påverkades av väte, avkastningsstyrkan och duktiliteten minskades. Laddning med den långsamma töjnings hastighet leder till extrem försprödhet jämfört med den höga töjnings hastighet. Korngränserna hade minskat sin storlek efter att de laddats med väte. 304 SS-kornen var svårare att upptäcka i jämförelse med 316L SS. Olika typer av faktorer kan påverka resultatet, för långsam töjnings hastighet var väte närvarande hela vägen tills det har nått sin brytpunkt och efter det började diffusion. Under tiden startade vätediffusionen med högt töjnings hastighet när den kom ut laddar behållaren. Under den tid det tar att placera provet i dragprovningsmaskinen och göra dragprovningen så diffuserar vätet och det leder till mindre sprödhet. Nyckelord: Väteförsprödning, dragprovning, DIC, metallografisk.

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[pt] A exposição de aços a condições de geração de hidrogênio, como em ambientes que contenham H2S ou sob proteção catódica, pode provocar o aumento do teor de hidrogênio na sua superfície, fragilizando o material. Foi desenvolvido um estudo com o objetivo de comparar o comportamento das microestruturas de dois diferentes aços inoxidáveis, um austenítico de classe P550 e um duplex S31803, com relação à permeação e consequente fragilização pelo hidrogênio. Os aços foram testados nas condições com e sem solda autógena utilizando os mesmos parâmetros de soldagem. Foram realizados análise microestrutural por MO, MEV e MET, ensaios de tração, ensaios de BTD com os corpos de prova imersos em solução de água do mar sintética e sob aplicação de potencial catódico de -1200 mV SCE, com o objetivo de simular condições de serviço e fractografia por MEV dos corpos de prova ensaiados por BTD. Observou-se que ambas as classes de aços sofreram alguma fragilização, no entanto, com relação à perda de ductilidade em função da redução de área dos corpos de prova, esta ocorreu de forma mais pronunciada para o aço inoxidável duplex. Foi observado que o aço austenítico no metal de base continha maior densidade de maclas do que o metal de solda, resultando em maior fragilização. Além disto, no metal de base, observou-se mais alta densidade de discordâncias e de precipitados. O aço duplex, por outro lado, apresentou fragilização muito maior do que o austenítico em ambas as condições quando permeado pelo hidrogênio. No entanto, esta fragilização foi mais pronunciada na condição de como soldado. Atribuiu-se este comportamento à ferritização parcial da estrutura e à formação de austenita Widmanstätten. As análises fractográficas sugerem a alteração do mecanismo de fratura dos corpos de prova de dúctil, quando ensaiados ao ar, para frágil, na condição de ensaio com geração de hidrogênio. Esta observação fundamenta-se no fato de que as superfícies de fratura de todos os corpos de prova ensaiados ao ar são formadas predominantemente por dimples (dúctil), enquanto no ensaio com geração de hidrogênio, as superfícies de fratura se apresentam com aspecto frágil de diferentes formas para cada aço. / [en] Steel exposure to hydrogen generation conditions, such as in environments containing H2S or under cathodic protection, can cause an increase in the hydrogen content on the surface which leads to the material embrittlement. A comparative study was carried out on the structure behavior of two different stainless steels, an austenitic class P550 and a duplex S31803, concerning permeation and consequent hydrogen embrittlement. The steels were tested in conditions with and without autogenous welding using the same welding parameters. It was performed microstructural analysis by OM, SEM and TEM, tensile tests, BTD tests with the specimens immersed in a synthetic seawater solution and under application of a cathodic potential of -1200 mV SCE, in order to simulate service conditions, and surface fractography of these specimens by SEM. It was observed that both grades of steel suffered some fragility. However, the loss of ductility due to the reduction of the area of the specimens occurred in a more pronounced way for the duplex stainless steel. It was also observed that the austenitic steel in the base metal contained a higher density of twinnings than the weld metal, resulting in greater embrittlement. In addition, a higher density of dislocations and precipitates was observed in the base metal. On the other hand, duplex steel showed much more significant embrittlement than austenitic in both conditions when permeated by hydrogen. However, this weakness was more pronounced in the as welded condition. This behavior was attributed to the partial ferritization of the structure and the formation of Widmanstätten austenite. Fractographic analyzes suggest that the fracture mechanism morphology changed from ductile to brittle when the specimens were tested in the air and hydrogen condition respectively. This observation is based on the fact that the fracture surfaces of all samples tested in the air consisted predominantly of dimples (ductile). In contrast, in the test with hydrogen generation, the fracture surfaces appear with different brittle morphologies for each steel.

In this work, Slow Strain Rate Test (SSRT) testing, Light Optical Microscopy (LOM) and Scanning Electron Microscopy (SEM) were used to study the effect of microstructure, corrosive environments and cathodic polarisation on stress corrosion cracking (SCC) of two grades of high strength steels, Type A and Type B. Type A is manufactured by quench and tempered (Q&T) method. Type B, a normalize steel was used as reference. This study also supports electrochemical polarisation resistance method as an effective testing technique for measuring the uniform corrosion rate. SSRT samples were chosen from base metal, weld metal and Heat Affected Zone (HAZ). SSRT tests were performed at room temperature under Open Circuit Potential (OCP) and cathodic polarisation using 4 mA/cm2 in 1 wt% and 3.5 wt% NaCl solutions. From the obtained corrosion rate measurements performed in 1 wt% and 3.5 wt% NaCl solutions it was observed that increased chloride concentration and dissolved oxygen content enhanced the uniform corrosion for all tested materials. Moreover, the obtained results from SSRT tests demonstrate that both Q&T and normalized steels were not susceptible to SCC in certain strain rate (1×10-6 s-1) in 1 wt% and 3.5 wt% NaCl solutions under OCP condition. It was confirmed by a ductile fracture mode and high reduction in area. The weld metal of Type A with acicular ferrite (AF), pro-eutectoid (PF) and bainite microstructure showed higher susceptibility to hydrogen assisted stress corrosion cracking compared to base metal and HAZ. In addition, typical brittle intergranular cracking with small reduction in area was observed on the fracture surface of the Type A due to hydrogen charging.

Hydrogen embrittlement can manifest itself as hydride formation in structures when in contact with hydrogen-rich environments, e.g. in space and nuclear power applications. To supplant experimentation, modeling of such phenomena is beneficial to make life prediction reduce cost and increase the understanding. In the present work, two different approaches based on phase field theory are employed to study the precipitation kinetics of a second phase in a metal, with a special focus on the application of hydride formation in hexagonal close-packed metals. For both presented models, a single component of the non-conserved order parameter is utilized to represent the microstructural evolution. Throughout the modelling the total free energy of the system is minimized through the time-dependent Ginzburg-Landau equation, which includes a sixth order Landau potential in the first model, whereas one of fourth order is used for the second model. The first model implicitly incorporates the stress field emanating from a sharp crack through the usage of linear elastic fracture mechanics and the governing equation is solved numerically for both isotropic and anisotropic bodies by usage of the finite volume method. The second model is applied to plate and notched cantilever geometries, and it includes an anisotropic expansion of the hydrides that is caused by the hydride precipitation. For this approach, the mechanical and phase transformation aspects are coupled and solved simultaneously for an isotropic material using the finite element method. Depending on the Landau potential coefficients and the crack-induced hydrostatic stress, for the first model the second-phase is found to form in a confined region around the crack tip or in the whole material depending on the material properties. From the pilot results obtained with the second model, it is shown that the applied stress and considered anisotropic swelling induces hydride formation in preferential directions and it is localized in high stress concentration areas. The results successfully demonstrate the ability of both approaches to model second-phase formation kinetics that is triggered by flaw-induced stresses and their capability to reproduce experimentally observed hydride characteristics such as precipitation location, shape and direction. / <p>Note: The papers are not included in the fulltext online.</p><p>Paper I and II in thesis as manuscripts.</p>

Safe, effective hydrogen fuel cells are one of the contenders for the next shift in mobile power technology. One of the solutions to the inherent risks of high pressure hydrogen fuel cells is an outer low pressure container with an inner high pressure containers containing a micro-electromechanical systems (MEMS) valve which regulating the pressure. These MEMS valves consist of several etched Si-chips stacked and bonded, which shall withstand the pressure and temperature range in the high pressure fuel cell as well as the embrittlement caused by the hydrogen gas. Hydrogen embrittlement is a phenomena where materials, mostly metals, lose their ductility due to diffusion of hydrogen atoms into their grain boundaries. A suitable method for stacking the chips is needed and thus a literature study was conducted. Several chip-to-chip bonding methods were investigated in the purpose of finding the most suitable methods tolerating temperatures between -40 to 85°C, pressure up to 1000 bar, hermetically sealing, withstanding hydrogen embrittlement and still bond with particulate contaminations caused by testing each chip. The method found to be best fitting for the purpose was anodic bonding with an alkali glass. Alternatively anodic bonding with a ceramic glass system could be considered if technique from alkali glass is adaptable.

The aviation industry plays a significant role in global connectivity and economic growthbut has substantial negative environmental impacts, particularly in terms of carbondioxide emissions. According to a study by the European parliament, the aviationindustry accounts for 0,4 % of greenhouse gas emissions within the EU and 3,4% forinternational flights. In response to these environmental issues, liquid hydrogen is seenas a promising choice, offering efficiency as a clean energy source, especially whenproduced through electrolysis, as well as higher energy density per volume, making itattractive for the aviation industry where energy and weight optimization are crucial. However, the challenge of using hydrogen as fuel lies in designing a tank that canwithstand extreme conditions, such as low temperature and high pressure , while alsominimizing the risk of flammability and explosion. Additionally the right materials mustbe chosen to resist hydrogen embrittlement. This project aims to design a hydrogentank for aircraft that meets the requirements specified in this study. This will be achievedthrough a literature review, numerical simulations with SolidWorks FEM to test differenttank shapes and materials, and the use of Python code to calculate different spatialparameters.The results indicate that a cylindrical shape is the most optimal choice for the tank, andfour materials have been identified as suitable, with aluminum alloys showing moreadvantages compared to stainless steel due to reduced weight with similar strength.

Les systèmes de maintien situés sur les structures assemblages-combustibles des réacteurs nucléaires à eau sous pression (REP) sont constitués d'un empilement de lames qui agissent à la fois, comme élément accommodant les incompatibilités thermiques résultant des différences de coefficients de dilatation Acier, alliages de zirconium et principalement, comme système permettant de limiter les effets hydrodynamiques induits par le passage du fluide caloporteur à travers les assemblages. Actuellement, l'alliage 718 est le matériau constitutif de ces ressorts à lames. Il présente les performances en service nécessaires et suffisantes pour répondre aux sollicitations de ces systèmes ainsi qu'aux exigences des autorités de sûreté (dans les conditions actuelles de fonctionnement des REP). Or, dans le cadre de l'augmentation des performances générales des assemblages combustibles, l'emploi d'autres matériaux, dont les propriétés de relaxation sous flux neutronique sont supérieures à celles du 718, est envisagé par AREVA. Les matériaux étudiés sont principalement des superalliages base Ni, tels que les nuances 625+ et 725 qui à l'instar de l'alliage 718 durcissent par précipitation de phases secondaires, ainsi que des nuances d'alliage 718 riche en Molybdène. Cependant, bien que ces nouveaux matériaux présentent une relaxation sous flux neutronique améliorée, ils doivent répondre également à un cahier des charges strict, propre à leur utilisation en centrale : des propriétés mécaniques équivalentes, une bonne résistance à la corrosion sous contrainte (CSC) et une bonne résistance à la fragilisation par l'hydrogène (FPH) en milieu primaire de REP. Chacune de ces propriétés a été étudiée avec attention dans le double but de comparer ces matériaux entre eux et afin de cerner les paramètres clés contrôlant leur différence de comportement aussi bien en CSC qu'en FPH / Hold-down systems used in the fuel assembly of Nuclear Pressurized Water Reactor (PWR) are constituted by stiff springs. The role of the hold-down springs is to ensure the bond between the fuel assembly and the lower plate of the intern structure of the core, thus holding down the assembly on the bottom plate of the reactor, during all the exploitation and maintenance periods. Nowadays, alloy 718 is the constitutive material of these hold-down springs. Its properties in terms of mechanical behaviour, corrosion resistance… fill in the specifications required for such application in the present service conditions. However, in order to improve the common efficiency of fuel assemblies, the upgrading of their design as well as the use of new materials are advocated by the nuclear power plant company, AREVA. Though other Ni-base superalloys known for their good behaviour under neutronic radiation can be proposed as new materials, those superalloys must fill in all the application specifications in order to substitute alloy 718. So, sufficient mechanical properties, good resistance to Stress Corrosion Cracking (SCC) and good resistance to Hydrogen Embrittlement (HE) are also required to allow the replacement. All of these properties are carefully studied with the double aim to characterize and compare different superalloys, and to determine key parameters governing the SCC and HE behaviours of such alloys in primary water of PWR

This research focused on a comprehensive microstructural and mechanical property characterisation study of the Ni-Fe-Cr alloys 718 and 945X. The aim of the project was to better understand the relationship between performance and microstructure of existing (Alloy 718) and newly developed (Alloy 945X) high strength nickel alloys focusing on downhole applications. The main difference between the two alloys is that alloy 945X has lower Nb content than alloy 718, which may minimise the tendency to form delta when combined with correct processing. Previous studies have related the hydrogen embrittlement in alloy 718 with the collection of hydrogen by delta phase. Microstructural characterisation of the new alloy 945X after long term isothermal exposure up to 120 hours in the temperature range 650◦C to 900◦C was conducted with scanning electron microscopy (SEM), to generate a time-temperature-transformation (TTT) diagram. The TTT diagram was used as a road map for designing two isothermal heat treatments of alloy 945X on tensile specimens. Then, the effect of hydrogen charging on the tensile properties and microstructure of the 'as-received' and these two variant heat treatments was investigated. Fractographic analysis showed that, in the presence of hydrogen, intergranular fracture occurred for all the heat treatments, regardless the presence of delta phase at grain boundaries. There was no simple correlation between the volume fraction of delta-phase and susceptibility to hydrogen assisted embrittlement. Rather, it was demonstrated that the morphology and distribution of delta-phase along grain boundaries plays a key role and the other precipitate phases also have an influence through their effect on the ease of strain localisation. This study also examined the hydrogen embrittlement sensitivity of nickel alloy 718 given four different heat treatments to obtain various microstructural states. Each heat treatment leads to differences in the precipitate morphologies of γ', γ'' and delta phases. Material characterisation and fractography of the examined heat treatments were performed using a high resolution FEG-SEM. Three specimens of each condition were pre- charged with hydrogen and tensile properties were compared with those of non-charged specimens. It was observed that hydrogen embrittlement was associated with intergranular and transgranular microcrack formation, leading to an intergranular brittle fracture. delta phase may assist the intergranular crack propagation, and this was shown to be particularly true when this phase is coarse enough to produce crack initia- tion, but this is not the only factor determining embrittlement. Other microstructural features play a role, as does the strength of the material. Finally, the evolution of delta-(Ni3Nb) phase in alloy 718 from the early stages of precipitation, with a particular focus on identifying the grain boundary characteristics that favour precipitation of grain boundary delta phase was investigated. Results showed that delta phase was firstly formed on Σ3 boundaries after 5 hours at the examined temperature (800◦C). Increasing ageing time at 800◦C was observed to lead to an increase in size and precipitation of phases γ'-γ''-delta, an increase in fraction of the special CSL boundaries and an evolution in the morphology of twins and the growth of grains.

Chemo-mechanics studies the material behavior and phenomena at the interface of mechanics and chemistry. Material failures due to coupled chemo-mechanical effects are serious roadblocks in the development of renewable energy technologies. Among the sources of renewable energies for the mass market, hydrogen and lithium-ion battery are promising candidates due to their high efficiency and easiness of conversion into other types of energy. However, hydrogen will degrade material mechanical properties and lithium insertion can cause electrode failures in battery owing to their high mobilities and strong chemo-mechanical coupling effects. These problems seriously prevent the large-scale applications of these renewable energy sources. In this thesis, the atomistic and continuum modeling are performed to study the chemical-mechanical failures. The objective is to understand the hydrogen embrittlement of grain boundary engineered metals and the lithium insertion-induced fracture in alloy electrodes for lithium-ion batteries. Hydrogen in metallic containment systems such as high-pressure vessels and pipelines causes the degradation of their mechanical properties that can result in sudden catastrophic fracture. A wide range of hydrogen embrittlement phenomena was attributed to the loss of cohesion of interfaces (between grains, inclusion and matrix, or phases) due to interstitially dissolved hydrogen. Our modeling and simulation of hydrogen embrittlement will address the question of why susceptibility to hydrogen embrittlement in metallic materials can be markedly reduced by grain boundary engineering. Implications of our results for efficient hydrogen storage and transport at high pressures are discussed. Silicon is one of the most promising anode materials for Li-ion batteries (LIB) because of the highest known theoretical charge capacity. However, Si anodes often suffer from pulverization and capacity fading. This is caused by the large volume changes of Si (~300%) upon Li insertion/extraction close to the theoretical charging/discharging limit. In particular, large incompatible deformation between areas of different Li contents tends to initiate fracture, leading to electro-chemical-mechanical failures of Si electrodes. In order to understand the chemo-mechanical mechanisms, we begin with the study of basic fracture modes in pure silicon, and then study the diffusion induced deformation and fracture in lithiated Si. Results have implications for increasing battery capacity and reliability. To improve mechanical stability of LIB anode, failure mechanisms of silicon and coated tin-oxide nanowires have been studied at continuum level. It's shown that anisotropic diffusivity and anisotropic deformation play vital roles in lithiation process. Our predictions of fracture initiation and evolution are verified by in situ experiment observations. Due to the mechanical confinement of the coating layers, our study demonstrates that it is possible to simultaneously control the electrochemical reaction rate and the mechanical strain of the electrode materials through carbon or aluminum coating, which opens new avenues of designing better lithium ion batteries. This thesis addresses the nano-chemo-mechanical failure problems in two green energy-carrier systems toward improving the performance of Li-ion battery anode and hydrogen storage system. It provides an atomistic and continuum modeling framework for the study of chemo-mechanics of advanced materials such as nano-structured metals and alloys. The results help understand the chemical effects of impurities on the mechanical properties of host materials with different metallic and covalent bonding characteristics.