The aim of this thesis is to provide microstructural and mechanical characterisation of α-β titanium alloys exposed to a range of thermo-mechanical conditions, in particular under-going high rate deformation at elevated temperatures, representative of the Linear Friction Welding (LFW) manufacturing process. Three α-β titanium alloys provided by Rolls-Royce are studied: Ti-64 blade, disc and Ti-6246 disc. Ti-64 and Ti-6246 show complex deformation behaviour with strain, strain rate and temperature, especially near the transus temperature, where the low temperature α phase is transformed into the high temperature β phase. The microstructure and mechanical properties evolve in an interconnected fashion, and understanding this mutual influence is necessary to better predict the behaviour of these alloys. Characterisation of the mechanical properties was performed through uniaxial compression tests at strain rates from 0.001 to 3000 s^-1, using an Instron screw-driven machine at quasi-static rates, a servo-hydraulic machine at medium rates and a Split-Hopkinson Pressure Bar and a drop-weight tower at high strain rates. The tests were performed over a range of temperatures from room temperature to 1300 °C. The main focus was on high strain rate and high temperature tests, with the development of a gravity driven direct impact Hopkinson bar, referred as a drop-weight system, which is intended to evaluate the mechanical response of metals to high strain rate loading at temperatures up to c. 1300 °C. The design and principles of operation of the system are presented, along with calibration and validation data. Preliminary tests were performed on stock Ti-64, heated at two rates: 1 and 20 °C s^-1. The evolution of the mechanical properties was analysed, focussing on the strain rate, temperature and phases dependencies. Characterisation of the microstructure was realised by performing interrupted compression tests, first at room temperature, three plastic strains, 4%, 10% and 20%, and two different strain rates, 0.001 and 2000 s^-1; then at 4% plastic strain, a strain rate of 2000 s^-1 and three elevated temperatures, 700, 900 and 1100 °C. A better understanding of the microstructure evolution with strain, strain rates and temperature, including the macrotexture and microtexture of the specimens, was obtained using Electron Backscatter Diffraction (EBSD) to characterise the texture of the undeformed and deformed materials. The better understanding of the flow stress and microstructural evolution of both Ti-64 and its individual α and β phases with various strain rates and temperatures is intended to be used in the development of more accurate models representing the behaviour of these alloys. Predicting the microstructure evolution and then the mechanical properties of a material is essential to optimise the final mechanical properties of the alloys when welded by manufacturing processes such as the LFW process.

High chromium ferritic steels such as Grade 91 and Grade 92 are extensively used in the power plant industry. Components made from these types of steels, including headers, steam pipes and tubes, are required to provide reliable service at high pressures (20-30 MPa) and temperatures (550-610°C) for several decades. However, in order to further improve the thermal efficiency of the power plant, the future operation temperature for the ferritic steels needs to be elevated to 650°C. Therefore, the current research project focuses on the examination of recently developed MarBN type steels (Martensitic steel strengthened by Boron and Nitrides) and four Grade 92 derivatives in order to evaluate their suitability for 650°C application, and also to assess their creep strength from a microstructural point of view.

La compréhension et la simulation des mécanismes de déformation dans la croûte supérieure sont des enjeux scientifiques et techniques importants. La calcite étant un minéral commun de la croûte supérieure se déformant essentiellement par maclage sous 200 °C, c'est pour cette raison que l'on s'intéresse plus particulièrement au maclage de la calcite dans le cadre de cette thèse. L'utilisation du maclage de la calcite n'en est pas à son coup d'essai et de nombreuses méthodes d'inversions existent que ce soit pour remonter aux tenseurs des contraintes comme aux tenseurs des déformations. Cette thèse propose une nouvelle méthode d'inversion basée sur l'inversion d'Etchopar permettant de reconstruire 5 sur 6 paramètres du tenseur des contraintes avec une quantification fine des incertitudes. Cette méthode permet de détecter automatiquement l'existence d'un ou de plusieurs évènements tectoniques enregistrés par le maclage de la calcite. Un deuxième volet de la thèse consiste en l'amélioration de la méthode d'acquisition des données de macles en utilisant un EBSD (electron backscatter diffraction). En effet, l'utilisation traditionnelle de la platine universelle a des limitations techniques et amène aussi à un doute visuel sur l'appréciation du statut non-maclé de certains plans, en plus du côté long et fastidieux. Le dernier volet de la thèse consiste à déterminer le seuil de maclage de la calcite pour différentes tailles de grains à l'aide de tests mécaniques sous une presse uniaxiale. Qui plus est, le suivi en continu des déformations sur les monocristaux de calcite a permis de mettre en évidence le comportement macroscopique d'un cristal de calcite et la séquence de maclage. / The understanding and modelling of deformation mechanics in the upper crust are important scientific and technical issues. The calcite is a common mineral in the upper crust and mainly deforms by twinning under 200°C. That is why we are interested by calcite twinning as part of this thesis. It is not the first time that calcite twinning is used to reconstruct paleostress or paleostrain tensors. This thesis propose a new inversion method based on the Etchecopar’s one allowing to reconstruct 5 among 6 parameters of the stress tensor with an accurate quantification of the uncertainties. This method allows to automatically detect the realness of one or several tectonic events recorded by calcite twinning. A second part of the thesis consists in the improvement of the data acquisition by using EBSD (electron backscatter diffraction). In fact, the traditional use of the universal stage has technical limitations and brings some optical doubt about the untwinned status of few planes in addition to the long and tedious side. The last part of the thesis consists in the establishing the threshold of calcite twinning for different grain sizes by mechanical tests under a uniaxial press. Moreover, the continuous monitoring of the experiments using single crystals of calcite allowed to highlight the macroscopic behavior of a single crystal and the sequence of twinning.

X / A combined experimental and computational investigation of the deformation behavior of pure magnesium single crystal at the micron length scale has been carried out. Employing the recently exploited method of microcompression testing, uniaxial microcompression experiments have been performed on magnesium single crystals with [0001], [2-1-12], [10-11], [11-20] and [10-10] compression axes. The advantage of the microcompression method over conventional mechanical testing techniques is the ability to localize a single crystalline volume which is characterizable after deformation. The stress-strain relations resulting from microcompression experiments are presented and discussed in terms of orientation dependent slip activity, twinning mechanisms and an anisotropic size effect. Such a mechanistic picture of the deformation behavior is revealed through SEM, EBSD and TEM characterization of the deformation structures, and further supported by 3D discrete dislocation dynamics simulations. The [0001], [2-1-12], and [10-11] compression axes results show dislocation plasticity. Specifically, the deformation due to [0001] compression is governed by pyramidal slip and displays significant hardening and massive unstable shear at stresses above 500MPa. In the case of the two orientations with compression along an axis 45 degrees to the basal plane, unsurpringly it is found that basal slip dominates the deformation. In contrast, compression along the [11-20] and [10-10] directions show deformation twinning in addition to dislocation plasticity. In the case of compression along [11-20], the twinning leads to easy basal slip, while the twin resultant during compression along [10-10] does not lead to easy basal slip. In all cases, a size effect in the stress-strain behavior is observed; the flow stress increases with decreasing column diameter. Furthermore, the extent of the size effect is shown to depend strongly on the number of active slip systems; compression along the [0001] axis is associated with 12 slips systems and displays a saturation of the size effect at a diameter of 10μm, while the other orientations still show a significant size effect at this diameter. The experimental evidence of an orientation-dependent deformation behavior in flow stress has been investigated by 3D discrete dislocation dynamics simulations. Here, the code TRIDIS was modified for hcp structure and c/a ratio of Mg. By matching the simulation results to experimental results, some proper constitutive material parameters such as initial dislocation density, dislocation source length, the critical resolved shear stress were suggested. For the case of [0001] and [2-1-12] orientation, dislocation feature in the pillar during the deformation was exhibited and strain burst was discussed.

abstract: Shock loading is a complex phenomenon that can lead to failure mechanisms such as strain localization, void nucleation and growth, and eventually spall fracture. The length scale of damage with respect to that of the surrounding microstructure has proven to be a key aspect in determining sites of failure initiation. Studying incipient stages of spall damage is of paramount importance to accurately determine initiation sites in the material microstructure where damage will nucleate and grow and to formulate continuum models that account for the variability of the damage process due to microstructural heterogeneity, which is the focus of this research. Shock loading experiments were conducted via flyer-plate impact tests for pressures of 2-6 GPa and strain rates of 105/s on copper polycrystals of varying thermomechanical processing conditions. Serial cross sectioning of recovered target disks was performed along with electron microscopy, electron backscattering diffraction (EBSD), focused ion beam (FIB) milling, and 3-D X-ray tomogrpahy (XRT) to gain 2-D and 3-D information on the spall plane and surrounding microstructure. Statistics on grain boundaries (GB) containing damage were obtained from 2-D data and GBs of misorientations 25° and 50° were found to have the highest probability to contain damage in as-received (AR), heat treated (HT), and fully recrystallized (FR) microstructures, while {111} Σ3 GBs were globally strong. The AR microstructure’s probability peak was the most pronounced indicating GB strength is the dominant factor for damage nucleation. 3-D XRT data was used to digitally render the spall planes of the AR, HT, and FR microstructures. From shape fitting the voids to ellipsoids, it was found that the AR microstructure contained greater than 55% intergranular damage, whereas the HT and FR microstructures contained predominantly transgranular and coalesced damage modes, respectively. 3-D reconstructions of large volume damage sites in shocked Cu multicrystals showed preference for damage nucleation at GBs between adjacent grains of a high Taylor factor mismatches as well as an angle between the shock direction and the GB physical normal of ~30°-45°. 3-D FIB sectioning of individual voids led to the discovery of uniform plastic zones ~25-50% the size of the void diameter and plastic deformation directions were characterized via local average misorientation maps. Incipient transgranular voids revealed from the sectioning process were present in grains of high Taylor factors along the shock direction, which is expected as materials with a low Taylor factor along the shock direction are susceptible to growth due their accomodation of plastic deformation. Fabrication of square waves using photolithography and chemical etching was developed to study the nature of plasticity at GBs away from the spall plane. Grains oriented close to <0 1 1> had half the residual amplitudes than grains oriented close to <0 0 1>. / Dissertation/Thesis / Doctoral Dissertation Mechanical Engineering 2015

L'objectif principal de cette thèse est de caractériser et d'analyser les phénomènes de recristallisation et de croissance des grains qui se produisent dans les métaux hexagonaux. On considère ici surtout le titane et le zirconium. pour cette raison, plusieurs expériences ont été préparées et réalisées à l'aide de la technique EBSD (la diffraction d'électrons rétrodiffusés). En même temps, un logiciel spécial utilisant l'approche de simulation et qui est basé sur le modèle Monte Carlo Potts a été conçu afin de faciliter l'analyse expérimentale. Sur la base de données expérimentales et des résultats des simulations, les modèles physiques et les hypothèses concernant les processus de recristallisation et de croissance des grains étudiés ont été proposés et vérifiés de manière positive. / The main aim of this thesis is to describe and analyse recrystallization and grain growth phenomena taking place in hexagonal metals, in particular cold-rolled titanium and channel-die compressed zirconium were considered. For that reason, several experiements were prepared and carried out using EBSD (Electron Backstartter Diffraction) technique. In addition, a special software based on Monte Carlo Potts model was developed in order to facilitate experiemental analysis using simulation approach. Based on the obtained experiemental data and simulation results, physical models and hypotheses concerning the investigate recrystallization and grain growth processes were proposed and positively verified.

The goal of this work is to understand how the wear and deformation mechanisms of hardmetalinserts change when the cobalt binder phase is replaced with a dierent metal or analloy. The focus is on inserts for steel turning. The work presented in this licentiate thesisconsists of the rst steps.Cobalt is the most common binder phase in hardmetal tools based on tungsten carbide asthe hard phase. Metallic cobalt powder, present during the manufacturing, has been associatedwith lung diseases and an increased risk for lung cancer if inhaled. Therefore it is importantto investigate alternative binders as one possible solution.This work studies binder phase alloys from the iron-nickel-cobalt system. These alloyscan be either austenitic, martensitic or a mixture of the two phases. By changing the binderphase composition to change the crystal structure it is possible to tailor the macroscopic mechanicalproperties of the material. It is also possible to tailor the composition in such a waythat the binder is transformation toughening, forming martensite as a response to mechanicaldeformation.The majority of inserts for steel turning are coated, and it is important to investigate if thehardmetals with alternative binder can be coated and if the coating adhesion is sucient forsteel turning.Four dierent alternative binder alloys and one reference with cobalt binder coated bychemical vapour deposition were investigated by scratch testing to determine the adhesion.The scratch test adhesion was sucient on all samples, but signicant variations in coatingadhesion were found.One alternative binder with 86wt%Ni and 14wt%Fe and a reference with cobalt binder manufacturedto mimic state of the art turning inserts were tested in steel turning. The alternativebinder grades had a lower resistance to plastic deformation and this was attributed to earlyaking of the coating due to a lower coating adhesion. Focused ion beam and scanning electronmicroscopy were used to study the deformation of the hard metal in the used cuttinginserts.

<p>  </p> <p>Stress corrosion cracking (SCC) is a longstanding critical materials challenge in austenitic stainless steels (AuSS). Recently, there has been mounting concern regarding the potential for Chloride-induced stress corrosion cracking (CISCC) along arc weld seams on austenitic stainless-steel canisters used as spent nuclear fuel (SNF) dry storage containers, due to the residual stress from the welding process and exposure to chloride-rich coastal air at storage sites. To ensure the safety of the SNF storage, fundamental understanding and mitigation methods of CISCC are critical in both engineering design and maintenance of the storage canisters before and after their deployment. With the recent development of high-resolution characterization and analysis techniques, a more robust and comprehensive understanding of the fundamental TGCISCC mechanism starts to be more accessible. In this thesis, comprehensive state-of-the-art techniques, including SEM, EBSD, HREBSD, FIB, ATEM, TKD, potential dynamic measurement, XRD, and nanoindentation will be used to further understand the mechanistic mechanism of TGCISCC in AuSS from macroscopic scale down to atomistic scale. </p>

Formable Advanced High-Strength Steels (AHSS) have a unique combination of strength and ductility, making them ideal in the effort to lightweight vehicles. The AHSS in this study, Quenched and Partitioned 1180, rely on the Transformation Induced Plasticity (TRIP) effect, in which retained austenite (RA) grains transform to martensite during plastic deformation, providing extra ductility via the transformation event. Understanding the factors involved in RA transformation, such as local strain and grain attributes, is therefore key to optimizing the microstructure of these steels. This research seeks to increase understanding of those attributes and the correlations between microstructure and RA transformation in TRIP steels. To measure local strain, the viability of using forescatter detector (FSD) images as the basis for DIC study is investigated. Standard FSD techniques, along with an integrated EBSD / FSD approach (Pattern Region of Interest Analysis System), are both analyzed. Simultaneous strain and microstructure maps are obtained for tensile deformation up to around 6% strain. The method does not give sub-grain resolution, and surface feature evolution prevents DIC analysis across large strain steps; however, the data is easy to obtain and provides a natural set of complementary information for the EBSD analysis. In-situ tensile tests combined with EBSD allow RA grain and neighboring attributes to be characterized and corresponding transformation data to be obtained. However, pseudo-symmetry of the ferrite (BCC) and martensite (BCT) phases prevents EBSD from accurately identifying all phases. Measuring the relative distortion of the crystal lattice, tetragonality, is one approach to identifying the phases. Unfortunately, small errors in the pattern center can cause significant errors in tetragonality measurement. Therefore, this research utilizes a new approach for accurate pattern center determination using a strain minimization routine and applies it to tetragonality maps for phase identification. Tetragonality maps based on dynamically simulated patterns result in the most accurate maps and can also be used to predict approximate local carbon content. Machine learning is then used on the collected data to isolate key attributes of RA grains and provide a decision tree model to predict transformation based on those attributes. Among the most relevant attributes found, RA grain area, RA grain shape aspect ratio, a “hardness” factor, and major axis orientation are included. Possible correlations between these factors and transformation improve understanding of relevant attributes and show the advantage that machine learning can have in unravelling complex material behavior.

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