An extensive review of probabilistic techniques in fatigue analysis indicates that there is a need for new microstructure-sensitive methods in describing the effects of notches on the fatigue life reduction in cyclically loaded components. Of special interest are notched components made from polycrystalline nickel-base superalloys, which are used for high temperature applications in aircraft gas turbine engine disks. Microstructure-sensitive computational crystal plasticity is combined with novel probabilistic techniques to determine the probability of failure of notched components based on the distribution of slip within the notch root region and small crack initiation processes. The key microstructure features of two Ni-base superalloys, a fine and coarse grain IN100, are reviewed and the method in which these alloys are computationally modeled is presented. Next, the geometric model of the notched specimens and method of finite element polycrystalline reconstruction is demonstrated. Shear-based fatigue indicator parameters are used to characterize the shear-based, mode I formation and propagation of fatigue cracks. Finally, two different probabilistic approaches are described in this work including a grain-scale approach, which describes the probability of forming a crack on the order of grain size, and a transition crack length approach, which describes the probability of forming and propagating a crack to the transition crack length. These approaches are used to construct cumulative distribution functions for the probability of failure as a function of various notch root sizes and strain load amplitudes.

Inconel 738 (IN 738), like other precipitation-hardened nickel-base superalloys that contain a substantial amount of Al and Ti, is very difficult to weld due to its high susceptibility to heat-affected zone (HAZ) cracking during conventional fusion welding processes. The cause of this cracking, which is usually intergranular in nature, has been attributed to the liquation of various phases in the alloy, subsequent wetting of the grain boundaries by the liquid and decohesion along one of the solid-liquid interfaces due to on-cooling tensile stresses. To address the problem of liquation cracking in weldments, recent developments in welding research have resulted in supposedly exclusive solid-state friction joining processes, such as linear friction welding (LFW), for joining crack susceptible structural alloys. The objective of this work was therefore to investigate the weldability of the difficult-to-weld IN 738 superalloy by LFW and to analyze the resulting microstructural changes in the alloy due to the welding process. LFW was performed on Linear Friction Welding Process Development System (PDS) at the Aerospace Manufacturing Technology Centre of the Institute for Aerospace Research, National Research Council (NRC) of Canada. In order to study and decouple the effect of non-equilibrium thermal cycle and imposed compressive stress during the joining, physical simulation of the LFW process was performed by using Gleeble 1500-D Thermo-Mechanical Simulation System at the University of Manitoba. Detailed microstructural study of welded and Gleeble-simulated materials was carried out. Correlation between the simulated microstructure and that of the weldments was obtained, in that, a significant grain boundary liquation was observed in both the simulated specimens and actual weldments due to non-equilibrium reaction of second phase particles, including the strengthening gamma prime phase. These results show that in contrast to the general assumption of LFW being an exclusively solid-state joining process, intergranular liquation, caused by non-equilibrium phase reaction(s), occurred during the process. However, despite a significant occurrence of liquation in the alloy, no HAZ cracking was observed. Nevertheless, the result showed that crack-free welding by linear friction welding is not due to preclusion of grain boundary liquation as has been commonly assumed and reported. Instead, resistance to cracking can be related to the counter-crack-formation effect of the imposed strain and to a concept observed and reported for the first time in this work, which is strain-induced rapid solidification. Furthermore, microstructural evolution during joining cannot be understood without considering the concept of non-equilibrium liquation reaction and strain-induced rapid solidification of the metastable liquid, which are carefully elucidated in this thesis.

Inconel 738 (IN 738), like other precipitation-hardened nickel-base superalloys that contain a substantial amount of Al and Ti, is very difficult to weld due to its high susceptibility to heat-affected zone (HAZ) cracking during conventional fusion welding processes. The cause of this cracking, which is usually intergranular in nature, has been attributed to the liquation of various phases in the alloy, subsequent wetting of the grain boundaries by the liquid and decohesion along one of the solid-liquid interfaces due to on-cooling tensile stresses. To address the problem of liquation cracking in weldments, recent developments in welding research have resulted in supposedly exclusive solid-state friction joining processes, such as linear friction welding (LFW), for joining crack susceptible structural alloys. The objective of this work was therefore to investigate the weldability of the difficult-to-weld IN 738 superalloy by LFW and to analyze the resulting microstructural changes in the alloy due to the welding process. LFW was performed on Linear Friction Welding Process Development System (PDS) at the Aerospace Manufacturing Technology Centre of the Institute for Aerospace Research, National Research Council (NRC) of Canada. In order to study and decouple the effect of non-equilibrium thermal cycle and imposed compressive stress during the joining, physical simulation of the LFW process was performed by using Gleeble 1500-D Thermo-Mechanical Simulation System at the University of Manitoba. Detailed microstructural study of welded and Gleeble-simulated materials was carried out. Correlation between the simulated microstructure and that of the weldments was obtained, in that, a significant grain boundary liquation was observed in both the simulated specimens and actual weldments due to non-equilibrium reaction of second phase particles, including the strengthening gamma prime phase. These results show that in contrast to the general assumption of LFW being an exclusively solid-state joining process, intergranular liquation, caused by non-equilibrium phase reaction(s), occurred during the process. However, despite a significant occurrence of liquation in the alloy, no HAZ cracking was observed. Nevertheless, the result showed that crack-free welding by linear friction welding is not due to preclusion of grain boundary liquation as has been commonly assumed and reported. Instead, resistance to cracking can be related to the counter-crack-formation effect of the imposed strain and to a concept observed and reported for the first time in this work, which is strain-induced rapid solidification. Furthermore, microstructural evolution during joining cannot be understood without considering the concept of non-equilibrium liquation reaction and strain-induced rapid solidification of the metastable liquid, which are carefully elucidated in this thesis.

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Primary water stress corrosion cracking (SCC) of metals in pressurized water reactors (PWRs) is known to be one of the most challenging and cost intensive modes of failure in the nuclear industry. Even though it is known that cracking in Ni-base alloys proceeds mainly intergranular (IG), the initiation and propagation of cracks in ductile metals are not yet understood and a much-desired accurate prediction of SCC related failure seems unobtainable. In this thesis, a combination of microcantilever fracture experiments, scanning electron- (SEM) and transmission electron microscopy (TEM) techniques was employed to study and compare the failure of oxidized grain boundaries of Ni-base Alloy 600 with high and low intergranular carbide coverage and different sample history. A new technique for lifting-out whole cantilevers after testing and for performing 3D focussed ion beam sequencing (3D FIB-SEM) while preserving a thin central region of the cantilever for further TEM sample preparation was developed and is presented. In lieu with recent efforts of the main project sponsor Électricité de France (EDF) to build a predictive model for IGSCC based on localized/microscopic information, one of the main objectives was the extraction of the stress at failure of individual oxidized GBs. Supported by finite element simulations, microcantilever fracture tests revealed that surface oxides on top of individual GBs have the capability to alter the mechanical response by delaying/suppressing the onset of failure. An overestimation of the failure stress (> 230 MPa) was observed, proving that the presence of the surface oxide on top of the test structures cannot be neglected. The failure stress on both samples, tested without influence of the surface oxide, was found to cover a range of 300 - 600 MPa, which agreed well with finite element simulations of the tests and further demonstrates the reliability of the obtained data. The second objective was to gain a better understanding of the observed fracture behaviour and the role of local microstructure. Using the gathered microscopy data, it was found that the crack clearly favours a progression along the IG oxide-metal interface in the presence of carbide precipitates. Electron energy loss spectroscopy (EELS) revealed that the observed crack path can be linked to compositional and density variations of the IG oxide. In the presence of carbides the oxide was layered. An oxide close to the stoichiometry of chromia was located at the original GB and next to the carbides. Next to this Cr-rich oxide, Fe-rich mixed spinel oxides of varying composition and density were found. An explanation for density variations based on the possible formation of defective spinel oxides of the type A²⁺B³⁺₂O₄, due to an unavailability of certain cation species is presented. No clear interface preference was observed in the absence of precipitation, where the IG oxide was found to be thin and often incomplete with Cr-richer oxides preferentially located at the original GB. While these observations were consistent on both samples (high and low carbide coverage), bigger void-like defects were located at the Fe-richer oxide-metal interface of the cold worked sample with high IG carbide precipitation only. These weak spots seemed to be the preferred path for crack propagation on this sample. The sample with low intergranular carbide coverage showed no obvious porosities at this interface but a Cr- depleted region was seen. Introducing a multi-faceted investigation strategy, supported by finite element simulations, the presented thesis provides the most accurate determination of the failure stress of oxidized GBs on Alloy 600 to date and and adds new valuable insights to our understanding of IGSCC and the future prediction of SCC related failures.

Dans cette thèse, nous nous sommes intéressés aux propriétés semi-conductrices des oxydes formés sur les alliages base nickel en milieu primaire des REP. L'objectif étant de mettre en évidence les effets de la pression partielle en hydrogène, de la nature de l'alliage et de l'état de surface sur les types de semi-conductions et les énergies de bandes interdites. La technique photoélectrochimique a été employée pour caractériser ces propriétés semi-conductrices. D'autres techniques de caractérisation complémentaires ont été également utilisées telles que le MEB-FEG, la diffraction des rayons X, la spectroscopie Raman et l'XPS. Les essais de corrosion ont été effectués en milieu primaire simulé (autoclave en titane, température 325°C, durée 500 heures). Des échantillons d'alliages 600 et 690 de polissage 1 µm diamant, ont été oxydés aux P(H2) < 0,01 ; 0,3 et 6,5 bar. L'état de surface ne concernait que l'alliage 600 oxydé à P(H2) = 0,3 bar. Nous avons utilisé une nouvelle méthode d'ajustement numérique pour la détermination des gaps. Les résultats obtenus montrent que seule la pression d'hydrogène affecte le type de semi-conduction des oxydes présentés par les hautes énergies, il passe du type-n (P(H2) < 0,01) en type proche de l'isolant (P(H2) = 0,3 et 6,5 bar). Un comportement du type-n a été enregistré à basse énergie quels que soit les paramètres d'étude. Les énergies de bande interdites des oxydes NiO, Cr2O3 et NiFe2O4 ont été révélées. / In this thesis, we are interested in semiconducting properties of oxides formed on nickel base alloys. The aim is to demonstrate the effects of hydrogen partial pressure, the nature of the alloy and the surface conditions on the semi-conduction type and the band gap energies. Photoelectrochemical technique was used to characterize the semiconducting properties. Other complementary techniques were also used such as FEG-SEM, X-ray diffraction, Raman spectroscopy and XPS. Corrosion tests were performed in simulated primary medium (titanium autoclave, temperature 325°C, duration 500 hours). Samples of alloys 600 and 690 of 1 µm diamond polishing were oxidized at P(H2) < 0,01 ; 0,3 et 6,5 bar. The surface conditions concerned only the alloy 600 oxidized at P(H2) = 0,3 bar. We used a new method for fitting energy spectra to obtain the band gap energies. The obtained results show that only the hydrogen pressure affects the semiconducting type of oxides presented by the high energies, it shift from n-type (P(H2) < 0,01 bar) to insulating type (P(H2) = 0,3 and 6,5 bar). An n-type behavior was recorded at low energy whatever the study parameters. Band gaps energies of NiO, Cr2O3 and NiFe2O4 were revealed.

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Les métaux déposés base nickel sont utilisés pour assembler des composants du circuit primaire des centrales nucléaires à Réacteurs à Eau sous Pression (REP). Un nombre croissant de cas de fissuration par Corrosion Sous Contrainte (CSC) des soudures en alliages base nickel 182 et 82 est rapporté dans le retour d'expérience international ce qui motive le développement d'un modèle permettant de prévoir la fissuration par CSC de ces matériaux. Ce mécanisme de dégradation fait intervenir des paramètres matériaux, mécaniques ou environnementaux qui peuvent interagir entre eux. L'objectif de cette étude est de mieux comprendre les mécanismes physiques locaux (aux joints de grains) impliqués dans l'amorçage de fissures de CSC. Un essai de traction sur une éprouvette en alliage 182 préalablement oxydée en milieu primaire simulé a mis en évidence une dispersion de la sensibilité à l'oxydation des différents joints de grains. L'analyse couplée entre oxydation et fissuration a permis, à l'aide de calculs de micro-mécanique sur un agrégat polycristallin synthétique, de proposer un critère de rupture des joints de grains oxydés défini par un couple profondeur d'oxydation/ contrainte locale critique. Compte tenu du rôle clé que tient l'oxydation intergranulaire dans le mécanisme de fissuration par CSC et de la dispersion observée entre les différents joints de grains, une cinétique d'oxydation intergranulaire des alliages base nickel 182 et 82 a été identifiée prenant en compte la précipitation de carbures de chrome, la température ou encore la teneur en hydrogène dissous. Ce modèle cinétique permet d'aborder statistiquement l'oxydation des joints de grains et est intégré à un modèle d'amorçage local. Dans ce dernier l'amorçage, défini par la fissuration de l'oxyde intergranulaire est suivi d'une phase de propagation lente puis rapide jusqu'à une certaine profondeur de fissure. Des hypothèses simplificatrices ont été faites lors de l'identification des lois embarquées dans le modèle de CSC. Toutefois, celles-ci s'avèreront utiles pour cibler les conditions des futurs essais à mener afin de conforter l'identification des différents paramètres. / Nickel base welds are widely used to assemble components of the primary circuit of Pressurized Water Reactors (PWR) plants. International experience shows an increasing number of Stress Corrosion Cracks (SCC) in nickel base welds 182 and 82 which motivates the development of models predicting the time to SCC initiation for these materials. SCC involves several parameters such as materials, mechanics or environment interacting together. The goal of this study is to have a better understanding of the physical mechanisms occurring at grains boundaries involved in SCC. In-situ tensile test carried out on oxidized alloy 182 evidenced dispersion in the susceptibility to corrosion of grain boundaries. Moreover, the correlation between oxidation and cracking coupled with micro-mechanical simulations on synthetic polycrystalline aggregate, allowed to propose a cracking criterion of oxidized grain boundaries which is defined by both critical oxidation depth and local stress level. Due to the key role of intergranular oxidation in SCC and since significant dispersion is observed between grain boundaries, oxidation tests were performed on alloys 182 and 82 in order to model the intergranular oxidation kinetics as a function of chromium carbides precipitation, temperature and dissolved hydrogen content. The model allows statistical analyses and is embedded in a local initiation model. In this model, SCC initiation is defined by the cracking of the intergranular oxide and is followed by slow and fast crack growth until the crack depth reaches a given value. Simplifying assumptions were necessary to identify laws used in the SCC model. However, these laws will be useful to determine experimental conditions of future investigations carried out to improve the calibration used parameters.

The topic of this thesis is the formation of microporosity in cast test bars of nickel-base superalloy Inconel 713LC during solidification. The theoretical part consists of nickel alloys, their macrostructure, the method of casting and crystallization of nickel-based superalloys. The second part is devoted to the design of casting conditions, the production of shell molds, the size and shape of grains, evaluation of microporosity by various available methods, comparing the influence of grain size and the proportion of microporosity on the resulting values of the mechanical tests. Experiments were carried out in cooperation with PBS Velká Bíteš and ÚST foundry department.

The focus of this master’s thesis is on the heat treatment of Ni-base alloys, specifically the risk of intermetallic σ-phases during different stages of heat treatment. The alloy studied is Sanicro®28, a super-austenitic stainless steel produced by Alleima AB. The problem at hand is that the quench-annealing stage is in high demand at the manufacturing facility, and the goal is to investigate if it can be removed from the manufacturing route. During forging, the outer surface and bar-ends can reach low temperatures, posing a high risk of σ-phase precipitation. Additionally, a necklace structure with large grains surrounded by fine re-crystallization is often observed at the surface of forged superalloys/Ni-base alloys. Today, this forged structure is re-crystallized and σ-phase dissolved during the quench-annealing stage. An alternative to quench-annealing after forging is to re-heat the bar using a Car Wagon Furnace(CWF). The thesis includes two laboratory experiments simulating two stages of heat treatment, the CWF and induction furnaces/soaking. The samples subjected to simulated CWF treatment showed re-crystallization throughout the entire structure. Annealing in CWF removes the large grains in surface positions. The time in the CWF also showed to be sufficient to dissolve σ-phase present from forging. Samples heated to the induction furnace set temperature do not contain precipitates, while temperatures below the induction set temperature induce σ precipitation to varying degrees. The key findings of the thesis are as follows: • Re-heating in a CWF right after forging is enough to dissolve σ-phase at half-radius and surface locations. • Quench-annealing stage could be removed by changing the route to a CWF after forging. • If temperatures fall below the σ-maximum stability temperature during induction furnace heating cycles, σ-phase precipitation occurs.