Dislocation channel-veins and persistent slip bands (PSBs) are characteristic dislocation configurations that are of interest to both industry and academia. However, existing mathematical models are not adequate to describe the mechanism of the transition between these two states. In this thesis, a series of models are proposed to give a quantitative description to such a transition. The full problem has been considered from two angles. Firstly, the general motion and instabilities of arbitrary curved dislocations have been studied both analytically and numerically. Then the law of motion and local expansions are used to track the shapes of screw segments moving through channels, which are believed to induce dislocation multiplication by cross-slip. The second approach has been to investigate the collective behavior of a large number of dislocations, both geometrically necessary and otherwise. The traditional method of multiple scales does not apply well to describe the pile-up of two arrays of dislocations of opposite signs on a pair of neighbouring glide planes in two dimensional space. Certain quantities have to be more accurately defined under the multiple-scale coordinates to capture the much more localised resultant stress caused by these dislocation pairs. Through detailed calculations, one-dimensional dipoles can be homogenised to obtain some insightful results both on a local scale where the dipole pattern is the key diagnostic and on a macroscopic scale on which density variations are of most interest. Equilibria of dislocation dipoles in a two-dimensional regular lattice have been also studied. Some natural transitions between different patterns can be found as a result of geometrical instabilities.

An understanding of the damage evolution prior to crack initiation in advanced structural materials is of vital importance to the fatigue community in both academia and industry. Features known as the Persistent Slip Bands (PSBs) play an integral role in this damage evolution. Therefore, PSBs have been the focus of a lot of science-based investigations over the years. However, most existing studies in this area are restricted to analysis of PSBs in single crystal face centered cubic (FCC) materials. Moreover, these studies lack a quantitative analysis of the evolution of the fatigue damage (or PSBs) as a function of the material microstructure. This is especially true for relatively modern materials such as the Advanced High Strength Structural (AHSS) steels that are gaining a lot of importance in the automotive sector. Accordingly, the objective of this research is to quantitatively characterize evolution of PSBs in three AHSS steels having different microstructures as a function of number of fatigue cycles and strain amplitude. For this purpose strain controlled interrupted fatigue tests have been performed on two dual phase steels (DP-590 and DP-980) having different relative amounts of tempered martensite and a ferritic high strength low alloy steel (HR-590). Digital image analysis and Stereology have been used for unbiased quantitative characterization of the evolution of global geometry of the PSB colonies as function of number of fatigue cycles and strain amplitude. Evolution of PSB colonies has been couched in terms of variation of PSB colony volume fraction and total surface area unit volume, and total surface area of individual PSBs per unit volume and three-dimensional angular orientation distribution of the PSBs. For this purpose, new stereological techniques have been developed for estimation of the three-dimensional angular orientation distribution. The stereological data reveal that during strain controlled in these AHSS steels, volume fraction of the PSB colonies varies linearly with the their total surface area per unit volume. Detailed analysis of the stereological data leads to a simple geometric model for evolution of the PSB colonies in the three AHSS steels, which accounts for all observed data trends.

Si l'amorçage des fissures de fatigue est aujourd'hui bien compris dans le cas de monocristaux de métaux purs, ce phénomène s'avère plus complexe à cerner et à prédire dans le cas d'alliages métalliques polycristallins tels que l'acier AISI 316LN.D'un point de vue expérimental, notre étude s'est concentrée sur la caractérisation du comportement mécanique et l'étude, à différentes échelles, des phénomènes liés à l'amorçage des fissures de fatigue oligocyclique dans l'acier 316LN. Pour des niveaux de déformation appliquée de Δε/2 = 0,3 et 0,5%, l'adoucissement cyclique observé au cours des essais coïncide avec l'organisation des dislocations sous forme de bandes. Ces bandes sont liées à l'activation des systèmes de plus haut facteur de Schmid. Elles portent la majeure partie de la déformation et provoquent en surface des intrusions et extrusions favorisant l'apparition et la coalescence de fissures.D'un point de vue modélisation, nous avons proposé un nouveau modèle de plasticité cristalline intégrant des dislocations géométriquement nécessaires (GND) directement calculées à partir du second gradient de la rotation élastique. Implémenté dans les codes d'éléments finis AbaqusTM et Cast3mTM, ce modèle s'inspire des travaux sur le monocristal en transformations finies de Peirce et al. (1983) et de Teodosiu et al. (1993). Adapté au cas des polycristaux par Hoc (1999) et Erieau (2003), il a été enrichi par l’introduction GND selon la théorie proposée par Acharya et Bassani (2000). Les simulations réalisées sur des différents types d'agrégats (2D extrudé et 3D) montrent que la prise en compte de GND permet :- de reproduire les effets de taille de grains au niveau macroscopique et local,- de décrire plus finement les champs de contraintes calculés.Ces simulations ont permis de mettre en évidence l'influence des matrices d'élasticité et d'écrouissage sur les valeurs et l'évolution des contraintes macroscopique effective et cinématique moyenne et le rôle important des conditions aux limites lors des calculs d'agrégats. / If fatigue crack initiation is currently quite well understood for pure single crystals, its comprehension and prediction in cases of polycrystal alloys such as AISI 316LN stainless steel remain complicated.Experimentally our study focuses on the characterisation of the mechanical behaviour and on the study at different scales of the phenomenon leading to low cycle fatigue crack initiation in 316LN stainless steel. For straining amplitudes of Δε/2 = 0,3 and 0,5%, the cyclic softening observed during testing has been related to the organisation of dislocations in band structures. These bands, formed due to the activation of slip systems having the greatest Schmid's factor, carry the most part of the deformation. Their emergence at free surfaces leads to the formation of intrusions and extrusions which help cracks initiate and spread.Numerically we worked on the mesoscopic scale, proposing a new model of crystalline plasticity. This model integrates geometrically necessary dislocations (GND) directly computed from the lattice curvature. Implemented in the finite element code AbaqusTM and Cast3mTM, it is based on single crystal finite deformations laws proposed by Peirce et al. (1983) and Teodosiu et al. (1993). Extended for polycrystals by Hoc (2001) and Erieau (2003), it has been improved by the introduction of GND (Acharya and Bassani, 2000). The simulations performed on different types of aggregates (2D/3D) have shown that taking GND into account enables:- the prediction of the grain size effect on a macroscopic and on a local scale,- a finer computation of local stress field.The influence of the elasticity and interaction matrices on the values and the evolution of the isotropic and kinematic mean stresses has been shown. The importance of boundary conditions on computed mechanical fields could also be pointed out.

Further understanding of mesoscale slip mechanics is crucial to future development of polycrystalline metals with improved performance. The research contained within this thesis aims to characterize localized mesoscale slip on slip bands further through two studies. First, a comprehensive comparison of slip system identification techniques was carried out to further validate each method as well as compare advantages and disadvantages of each. Second, slip bands in the presence of grain boundaries were studied to better characterize the dislocation content and behavior. In the first study, the use of SEM-DIC, AFM, ECCI, and HR-EBSD to characterize slip-system activity was assessed on the same material volume of Ti-7Al. This study presents a robust comparison of the various methods for the first time, including an assessment of their advantages and disadvantages, and how they can be used effectively in a complementary manner. The analysis of the different approaches was carried out in a blind manner independently at three different universities. A Ti-7Al specimen was deformed in uniaxial tension to approximately 3% axial strain, and the active slip systems were independently identified using (i) trace analysis; (ii) in-SEM digital image correlation, (iii) observations of residual dislocations from ECCI, and (iv) long-range rotation gradients through HR-EBSD, with consistent trace identification in all cases. Displacement data from AFM was used to augment the SEM-DIC displacement data by providing complementary out of plane displacement information. Furthermore, short-range dislocation gradients (measured by DIC) provided insight into the residual geometrically necessary dislocation (GND) content, and was consistent with the GND content extracted from EBSD data and ECCI images, confirming the presence of residual GNDs on the dominant slip systems resulting in visible slip bands. These approaches can be used in tandem to provide multi-modal information on slip band identification, strain and orientation gradients, out-of-plane displacements, and the presence of GNDs and SSDs, all of which can be used to inform and validate the development of dislocation-based crystal plasticity and strain gradient models. In the second study, shear strain profiles along slip bands in a modified Rolls-Royce nickel superalloy (RR1000) were analyzed for a tensile sample deformed by 2%. The strain increased with distance away from a grain boundary (GB), with maximum shear strain towards the center of the grain, indicating that dislocation nucleation generally occurred in the grain interior. The strain gradients in the neighborhood of the GBs were quantified and generally correlated with rotation about the active slip system line direction. This leads to an ability to determine the active slip system in these regions. The dislocation spacing and pileup stresses were inferred. The dislocation spacing closely follows an Eshelby analytical solution for a single ended pileup of dislocations under an applied stress. The distribution of pileup stress values for GBs of a given misorientation angle follows a log-normal distribution, with no correlation between the pileup stress and the GB misorientation angle. Furthermore, there is no observed correlation between various transmissivity factors and slip band pileup stress. Hence it appears that the obstacle strength of any of the observed GBs is adequate to facilitate the dislocation pileups present in the slip bands. However, slip band transmission does correlate with transmissivity factors, with the current study focusing on the Luster and Morris m'-factor. Observation of strain profiles of transmitted bands indicate dislocation nucleation locations.

Il existe actuellement une demande croissante pour le développement de méthodes expérimentales rapides et fiables permettant d'estimer la résistance à la fatigue dans le domaine de la fatigue à grands nombres de cycles. En ce sens, la fatigue ultrasonique apparue dans les années cinquante est très intéressante pour les industriels. En effet, la fréquence typique de ces essais est de 20 kHz ce qui permet d'atteindre le domaine des très grandes durées de vie en des temps d'essais raisonnables (109 cycles sont atteints en 14 h). Cependant ces essais posent le problème de l'effet de la fréquence et plus généralement de la validité des résultats obtenus pour estimer la durée de vie de structures chargées à des fréquences très inférieures à 20 kHz. L'objectif de ce travail est d'évaluer l'effet de la fréquence du chargement sur les mécanismes précurseurs de l'initiation de fissures et plus précisément sur les mécanismes de microplasticité à l'échelle du grain. Ce travail de thèse s’intéresse au cas du cuivre pur polycristallin sollicité en traction-compression alternée et symétrique. Pour mettre en évidence un effet de la fréquence, les courbes de Wöhler ont été construites à différentes fréquences. L’étude s’est ensuite focalisée sur les mécanismes de microplasticité précurseurs de l’initiation de fissures et plusieurs critères ont été examinés : les morphologies des bandes de glissement et leurs positions en lien avec la microstructure, les seuils d’apparition des bandes de glissement, le développement de ces bandes avec le nombre de cycles, la répartition de la microplasticité dans les grains, les valeurs d’énergie dissipée au cours d’un cycle. Le glissement dévié et la production-diffusion de lacunes sont deux mécanismes qui interviennent dans la formation des bandes de glissement et des extrusions en surface. Leurs rôles respectifs sur les effets de fréquence observés sont discutés. / Nowadays there is a growing demand for the development of fast and robust fatigue life prediction methods in the very high cycle fatigue domain. In this way, ultrasonic fatigue technique which appeared in 1950 is very interesting for manufacturers. Because the typical frequency of these tests is 20 kHz, this technique is efficient to perform tests up to a very high number of cycles in a reasonable time (109 cycles are reached in 14 h). However, the frequency domain of these fatigue tests facilities raises the issue of the effect of frequency and more generally the validity of the obtained results for estimating fatigue life of structures loaded at frequencies three or four order of magnitude below ultrasonic frequencies. The objective of this work is to evaluate the effect of the loading frequency on the precursors of fatigue damage, namely the microplasticity at the grain scale. This thesis work deals with the case of polycrystalline pure copper loaded in fully reversed tensioncompression. To show the effect of frequency, the Wöhler or S-N curves were constructed at different frequencies. Then, the study focused on the mechanisms of microplasticity preceding crack initiation and several criteria were investigated: the morphologies of the slip bands and their locations in the microstructure, the thresholds of appearance of the slip bands, the evolution of the slip bands amount with the number of cycles, the distribution of the microplasticity in the grains, the dissipated energy during a fatigue cycle. Cross slip and vacancies production and diffusion are two mechanisms which play a part in the formation of slip bands and extrusions in surface. Their respective roles on the effects of frequency observed are discussed

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.

Metal fatigue is a recurring problem for metallurgists and materials engineers, especially in structural applications. It has been responsible for many disastrous accidents and tragedies in history. Understanding the micro-mechanisms during cyclic deformation and combating fatigue failure has remained a grand challenge. Environmental effects, like temperature or a corrosive medium, further worsen and complicate the problem. Ultimate design against fatigue must come from a materials perspective with a fundamental understanding of the interaction of microstructural features with dislocations, under the influence of stress, temperature, and other factors. This research endeavors to contribute to the current understanding of the fatigue failure mechanisms. Cast aluminum alloys are susceptible to fatigue failure due to the presence of defects in the microstructure like casting porosities, non-metallic inclusions, non-uniform distribution of secondary phases, etc. Friction stir processing (FSP), an emerging solid state processing technique, is an effective tool to refine and homogenize the cast microstructure of an alloy. In this work, the effect of FSP on the microstructure of an A356 cast aluminum alloy, and the resulting effect on its tensile and fatigue behavior have been studied. The main focus is on crack initiation and propagation mechanisms, and how stage I and stage II cracks interact with the different microstructural features. Three unique microstructural conditions have been tested for fatigue performance at room temperature, 150 °C and 200 °C. Detailed fractography has been performed using optical microscopy, scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD). These tools have also been utilized to characterize microstructural aspects like grain size, eutectic silicon particle size and distribution. Cyclic deformation at low temperatures is very sensitive to the microstructural distribution in this alloy. The findings from the room temperature fatigue tests highlight the important role played by persistent slip bands (PSBs) in fatigue crack initiation. At room temperature, cracks initiate along PSBs in the absence of other defects/stress risers, and grow transgranularly. Their propagation is retarded when they encounter grain boundaries. Another major finding is the complete transition of the mode of fatigue cracking from transgranular to intergranular, at 200 °C. This occurs when PSBs form in adjacent grains and impinge on grain boundaries, raising the stress concentration at these locations. This initiates cracks along the grain boundaries. At these temperatures, cyclic deformation is no longer microstructure- dependent. Grain boundaries don’t impede the progress of cracks, instead aid in their propagation. This work has extended the current understanding of fatigue cracking mechanisms in A356 Al alloys to elevated temperatures.

Low cycle fatigue is an important valving parameter of materiale which are exposed random alternate strain during their operation. The alternate strain in that material is caused by temperature fluctuations during operation and outages such as aircraft engines. Tests of low cycle fatigue were performed on samples of superalloy Inconel 738LC at stable room temperature at 23°C. The actual experiment took place at certain intervals, consisting of cycling itself, and observing changes in surface relief by light and electron microscopy. There was observed significant surface relief at an early stage of low cycle fatigue. We compared results of measurement with other different observation methods.

Superaustenitická korozivzdorná ocel typu 22Cr25NiWCoCu určená pro vysokoteplotní aplikace v energetickém průmyslu byla studována za podmínek nízkocyklové únavy při pokojové a zvýšené teplotě. Jednotlivé vzorky byly podrobeny různým zátěžným procedurám, což umožnilo studium materiálové odezvy spolu s mechanismem poškození. Křivky cyklického zpevnění/změkčení, cyklického napětí a Coffin-Mansonovy křivky byly vyhodnoceny. Únavová životnost materiálu byla diskutována s ohledem na uplatňované mechanismy poškození, které se vyvinuly za specifických zátěžných podmínek. Standardní izotermální únavové experimenty byly provedeny při pokojové a zvýšené teplotě. Hysterezní smyčky zaznamenané během cyklického zatěžování byly analyzovány pomocí zobecněné statistické teorie hysterezní smyčky. Pro různé amplitudy napětí byla určena jak distribuce hustoty pravděpodobnosti interních kritických napětí (dále PDF), tak rovněž zjištěn její vývoj během cyklického namáhání. Zjištěné průběhy PDF byly korelovány s vývojem povrchového reliéfu a vnitřního dislokačního uspořádání zdokumentované pro obě teploty pomocí rastrovací elektronové mikroskopie (SEM) vybavené technikou fokusovaného iontového svazku (FIB), která umožnila rovněž efektivní studium nukleace povrchových únavových trhlin. Při cyklickém zatížení při pokojové teplotě byla pozorována lokalizace cyklické plastické deformace do perzistentních skluzových pásů (PSP). V místech, kde tyto PSP vystupují na povrch materiálu byly pozorovány perzistentní skluzové stopy (PSS) tvořené extruzemi a intruzemi. Postupné prohlubování intruzí, zejména na čele nejhlubší intruze, vede k iniciaci únavové trhliny. Odlišný mechanismus tvorby trhlin byl zjištěn při únavové zkoušce při zvýšené teplotě, kde zásadní roli hrál vliv prostředí. Rychlá oxidace hranic zrn a jejich následné popraskání představuje dominantní mechanismus v I. stádiu nukleace trhlin. Aplikace desetiminutové prodlevy v tahové části zátěžného cyklu vedlo k vývoji vnitřního (kavitačního) poškozování. Mechanismy vnitřního poškozování byly studovány na podélných řezech rovnoběžných s napěťovou osou zkušebních vzorků. Trhliny a jejich vztah k hranicím zrn a dvojčat byly studovány pomocí difrakce zpětně odražených elektronů (EBSD). Vliv prodlevy na únavovou životnost byl korelován s vývojem povrchového reliéfu a vnitřního poškození. Vzorky z uvedené oceli byly rovněž podrobeny zkouškám termomechanické únavy (TMF), při nichž se v čase mění jak zátěžná síla tak i teplota. Termomechanické únavové zkoušky v režimu soufázném (in-phase) a protifázném (out-of-phase) byly provedeny jak s prodlevou, tak i bez ní. Ve všech případech bylo pozorováno rychlé cyklické zpevnění bez ohledu na použitou amplitudu deformace, u vzorků testovaných v out-of-phase režimu byla zjištěna tendence k saturaci. Zkoumáním povrchového reliéfu za pomocí technik SEM a FIB byla odhalena přednostní oxidace hranic zrn a následné praskání těchto hranic kolmo k ose zatížení. Prodlevy v cyklech při maximálním napětí vedly ke zvýšení amplitudy plastické deformace a následně ke creepovému poškození ve formě vnitřních kavit a trhlin. Interkrystalické šíření trhlin bylo pozorováno na vzorcích testovaných v režimu in-phase. Vývoj poškození v režimu out-of-phase nebyl principiálně ovlivněn zařazením prodlevy do zátěžného cyklu. Charakteristickým znakem namáhání v režimu out-of-phase je nukleace několika trhlin v homogenní oxidické vrstvě jdoucích napříč zrny kolmo k ose zatěžování.