Les alliages de titane β-métastable sont largement utilisés dans l’industrie aéronautique pour leurs propriétés mécaniques élevées, leur faible densité et bonne résistance à la corrosion. Dans ces alliages, et contrairement aux alliages α ou α/β, environ 40 % de phase β sont retenus à température ambiante. Cette phase, à la structure cubique centrée, est connue pour présenter une anisotropie élastique élevée, qui influence significativement les mécanismes de déformation opérant à l’échelle de la microstructure. Les travaux de thèse détaillés dans ce manuscrit visent à mieux comprendre le lien entre la durabilité de l’alliage Ti-5Al-5Mo-5V-3Cr sous sollicitations cycliques, un enjeu important pour les équipements aéronautiques, et l’anisotropie élastique de la phase β.Ce point central a tout d’abord fait l’objet d’une étude dédiée, dans le but de permettre une description satisfaisante de l’élasticité cristalline de la phase β. Pour cela, et à l’aide de différentes microstructures modèles, la contribution de la phase α a pu être isolée. La caractérisation de la texture cristallographique associée à la mesure du module d'Young par méthode de résonance dynamique a permis de passer en revue les différents jeux de constantes d’élasticité de la phase β proposés dans la littérature et de conclure par le choix le plus adapté. Enfin, une prise en compte de la contribution liée à la précipitation α a permis de modéliser les propriétés du matériau dans l’état microstructural utilisé industriellement.Les mécanismes de déformation plastique et d’endommagement actifs sous sollicitations monotones et cycliques ont ensuite été caractérisés en lien avec l’orientation cristallographique locale des deux phases. Cette étape a permis d’étudier l’influence de l’anisotropie élastique de la phase β sur le comportement mécanique ainsi que d’identifier les configurations microstructurales favorisant l'endommagement de cet alliage. Les conséquences sur la durabilité de l’alliage Ti-5Al-5Mo-5V-3Cr sont finalement discutées. / Β-metastable titanium alloys are widely used in the aerospace industry due to the combination of superior mechanical properties with a low density and a good corrosion resistance. In contrast with α or α/β alloys, 40 % of β phase are retained at room temperature in these alloys. This phase, with a body-centered cubic structure, is known to exhibit a high elastic anisotropy. A significant influence is expected on the deformation processes operating at the microstructure scale. The PhD work detailed in the present manuscript focuses on the relationship between durability of Ti-5Al-5Mo-5V-3Cr under cyclic loadings, which is a critical concern for aerospace components, and the elastic anisotropy of the β phase. Elastic anisotropy was first studied in order to enable a proper description of crystalline elasticity in the the β phase. Different academic microstructures were designed to isolate the contribution of the α phase. A characterization of the crystallographic texture using the EBSD technique combined with estimation of Young’s modulus using the dynamic resonance method enabled to review and criticize the elastic constants datasets available in the literature for the β phase. Finally, the contribution of the α precipitation was re-introduced in order to model the properties of the alloy with an industrially used microstructure.The plastic deformation and damage processes operating under monotonic and cyclic loadings were then characterized by considering the local crystallographic orientation of both phases. This enabled to study the influence of elastic anisotropy on the mechanical behavior at multiple scales as well as to identify the microstructural arrangements favoring damage. The consequences on durability of the Ti-5Al-5Mo-5V-3Cr alloy under fatigue loading are finally discussed.

<p>The properties and microstructure of Ti-5Al-5V-5Mo-3Cr were characterized under various stress states after the following heat treatments: 1) annealing above the β transus, followed by cooling at various rates and ageing for different times; 2) solution heat treatment in the α-β range, fan-cooling and ageing for various temperatures and times.</p> <p>Heat treatment above the ptransus temperature causes complete recrystallization of the as-forged microstructure. The as-cooled microstructure consists of equiaxed β grains with an average grain size of 200μm. Water quenching from above the β transus results in precipitation of a dispersion of nano-sized ω phase; while the fan-cooled microstructure contains nano-sized ω and α precipitates. Ageing of the fan-cooled microstructure at 790°C or 600°C precipitates sub micron acicular α throughout the β grains. The tensile properties of this condition could not be determined using standard tensile specimens due to brittle failure at the grips.</p> <p>Controlled cooling from above the β transus to the ageing temperature at slower rates produces a coarser α+β microstructure. Acicular α laths are produced with cooling rates of 1°C/min, while lamellar α develops at cooling rates of 3.4°C/min. The β annealed and fan-cooled condition is characterized by relatively low strength (~850MPa) and low ductility (~6% elong.).The fracture mode is by intensely localized slip and the creation of transgranular cracks. Localization of slip is attributed to shearing of the nano-scale ω precipitates by dislocations. A linear relationship between the grain size, d⁻¹/² , and the yield and fracture stresses was established, as described by the Hall-Petch relation. With controlled cooling, the strength and ductility improve by precipitation of lamellar α within the β matrix. Improvements in ductility and strength are achieved by reducing the slip length.</p> <p>Solution heat treatment below the β transus and fan-cooling results in complete dissolution of the as-forged acicular α phase. Solutionizing at 50°C below the ptransus yields a volume fraction of 16.5% primary α in a matrix of retained β. Low angle grain boundaries and globular primary α, each measuring 2-4μm average in diameter, are uniformly distributed throughout the retained β matrix. The tensile strength in this condition is relatively low, i.e. (900MPa) and the ductility relatively high (~16% elong.). With ageing in the 500°C to 600°C temperature range, precipitation of α within the retained β begins within 5 minutes of the start of ageing. Precipitating is heterogeneously nucleated at dislocations and grain boundaries. The yield and ultimate tensile strengths reach values of roughly 1200 and 1300MPa, respectively, and remain relatively constant for up 48 hours ageing</p> <p> The fracture stresses for the solution treated condition and for material subsequently aged at 500°C and 600°C are quite similar in magnitude. This similarity is due to the fact that the fracture mechanism, which controls the fracture stress, is the same for all these conditions. The fracture mechanism for all the solution treated conditions begins with shear decohesion of the primary α/β interfaces.</p> <p>For each condition, the damage mechanisms and final fracture modes were evaluated and rationalized on the basis of microstructural features. The yield and fracture stresses for the various conditions were calculated and plotted on a two-principal stress axis coordinate system, thus creating the failure envelope for Ti-5553. For the β annealed and fan cooled and for the α-β solution heat treated and aged conditions the yield and fracture envelopes are two concentric ellipses in good agreement with the shear strain energy (van Mises) model for failure.</p> <p>The fracture toughness and stress corrosion cracking behaviour for the STA condition were evaluated and compared against other β titanium alloys.</p> / Thesis / Doctor of Philosophy (PhD)

Fusarium head blight (FHB), caused mainly by Fusarium graminearum (teleomorph: Gibberella zeae), is one of the most damaging diseases of wheat. A ‘Brio’/‘TC 67’ spring wheat population was used to map quantitative trait loci (QTLs) for resistance to FHB, and to study the association of morphological and developmental characteristics with FHB resistance. Interval mapping (IM) detected a major QTL on chromosome 5AL for resistance to disease severity (type II resistance) and Fusarium-damaged kernels (FDK) under greenhouse and field conditions, respectively. Inconsistent QTL(s) was also detected on chromosome 5BS for disease severity and index using field data. The associations of plant height and number of days to anthesis were negative with disease incidence, severity, index, and deoxynivalenol (DON) accumulation data under field conditions. However, number of days to anthesis was positively correlated with disease severity (greenhouse) and FDK (field). Awnedness had a negative effect on FHB, namely the presence of awns resulted in less disease in the population. Spike threshability also affected FHB so that the hard threshable genotypes represented lower disease. Phylogenetic relationships of putative F. graminearum isolates from different sources were characterized using Tri101 gene sequencing data. Canadian and Iranian isolates clustered in F. graminearum lineage 7 (=F. graminearum sensu stricto) within the F. graminearum clade while the isolates received from CIMMYT, Mexico were placed in F. graminearum lineage 3 (=Fusarium boothii) within the Fg clade or Fusarium cerealis. The PCR assay based on the Tri12 gene revealed the presence of the NIV, 3-ADON, and 15-ADON chemotypes with 15-ADON being the predominant chemotype. While we did not find the NIV chemotype among the Canadian isolates, it was the predominant chemotype among the Iranian isolates. High variation in aggressiveness was observed among and within Fusarium species tested, with the isolates of F. graminearum sensu stricto being the most aggressive and the NIV chemotype being the least aggressive. The interactions between Fusarium isolates and wheat genotypes from different sources were investigated by inoculating isolates of F. graminearum sensu stricto and F. boothii on wheat genotypes. Significant differences were observed among the genotypes inoculated by single isolates. Results also showed significant interactions between Fusarium isolates and wheat genotypes. The F. boothii isolates from CIMMYT produced low disease symptom and infection on wheat genotypes regardless of the origin of the genotypes while F. graminearum sensu stricto isolates from Canada and Iran resulted in higher FHB scores.

Fusarium head blight (FHB), caused mainly by Fusarium graminearum (teleomorph: Gibberella zeae), is one of the most damaging diseases of wheat. A ‘Brio’/‘TC 67’ spring wheat population was used to map quantitative trait loci (QTLs) for resistance to FHB, and to study the association of morphological and developmental characteristics with FHB resistance. Interval mapping (IM) detected a major QTL on chromosome 5AL for resistance to disease severity (type II resistance) and Fusarium-damaged kernels (FDK) under greenhouse and field conditions, respectively. Inconsistent QTL(s) was also detected on chromosome 5BS for disease severity and index using field data. The associations of plant height and number of days to anthesis were negative with disease incidence, severity, index, and deoxynivalenol (DON) accumulation data under field conditions. However, number of days to anthesis was positively correlated with disease severity (greenhouse) and FDK (field). Awnedness had a negative effect on FHB, namely the presence of awns resulted in less disease in the population. Spike threshability also affected FHB so that the hard threshable genotypes represented lower disease. Phylogenetic relationships of putative F. graminearum isolates from different sources were characterized using Tri101 gene sequencing data. Canadian and Iranian isolates clustered in F. graminearum lineage 7 (=F. graminearum sensu stricto) within the F. graminearum clade while the isolates received from CIMMYT, Mexico were placed in F. graminearum lineage 3 (=Fusarium boothii) within the Fg clade or Fusarium cerealis. The PCR assay based on the Tri12 gene revealed the presence of the NIV, 3-ADON, and 15-ADON chemotypes with 15-ADON being the predominant chemotype. While we did not find the NIV chemotype among the Canadian isolates, it was the predominant chemotype among the Iranian isolates. High variation in aggressiveness was observed among and within Fusarium species tested, with the isolates of F. graminearum sensu stricto being the most aggressive and the NIV chemotype being the least aggressive. The interactions between Fusarium isolates and wheat genotypes from different sources were investigated by inoculating isolates of F. graminearum sensu stricto and F. boothii on wheat genotypes. Significant differences were observed among the genotypes inoculated by single isolates. Results also showed significant interactions between Fusarium isolates and wheat genotypes. The F. boothii isolates from CIMMYT produced low disease symptom and infection on wheat genotypes regardless of the origin of the genotypes while F. graminearum sensu stricto isolates from Canada and Iran resulted in higher FHB scores.

<div>In this thesis, the role of location-specific microstructural features in the fatigue performance of the safety-critical aerospace components made of Nickel (Ni)-base superalloys and linear friction welded (LFW) Titanium (Ti) alloys has been studied using crystal plasticity finite element (CPFE) simulations, energy dispersive X-ray diffraction (EDD), backscatter electron (BSE) images and digital image correlation (DIC).</div><div><br></div><div>In order to develop a microstructure-sensitive fatigue life prediction framework, first, it is essential to build trust in the quantitative prediction from CPFE analysis by quantifying uncertainties in the mechanical response from CPFE simulations. Second, it is necessary to construct a unified fatigue life prediction metric, applicable to multiple material systems; and a calibration strategy of the unified fatigue life model parameter accounting for uncertainties originating from CPFE simulations and inherent in the experimental calibration dataset. To achieve the first task, a genetic algorithm framework is used to obtain the statistical distributions of the crystal plasticity (CP) parameters. Subsequently, these distributions are used in a first-order, second-moment method to compute the mean and the standard deviation for the stress along the loading direction (σ_load), plastic strain accumulation (PSA), and stored plastic strain energy density (SPSED). The results suggest that an ~10% variability in σ_load and 20%-25% variability in the PSA and SPSED values may exist due to the uncertainty in the CP parameter estimation. Further, the contribution of a specific CP parameter to the overall uncertainty is path-dependent and varies based on the load step under consideration. To accomplish the second goal, in this thesis, it is postulated that a critical value of the SPSED is associated with fatigue failure in metals and independent of the applied load. Unlike the classical approach of estimating the (homogenized) SPSED as the cumulative area enclosed within the macroscopic stress-strain hysteresis loops, CPFE simulations are used to compute the (local) SPSED at each material point within polycrystalline aggregates of 718Plus, an additively manufactured Ni-base superalloy. A Bayesian inference method is utilized to calibrate the critical SPSED, which is subsequently used to predict fatigue lives at nine different strain ranges, including strain ratios of 0.05 and -1, using nine statistically equivalent microstructures. For each strain range, the predicted lives from all simulated microstructures follow a log-normal distribution; for a given strain ratio, the predicted scatter is seen to be increasing with decreasing strain amplitude and are indicative of the scatter observed in the fatigue experiments. Further, the log-normal mean lives at each strain range are in good agreement with the experimental evidence. Since the critical SPSED captures the experimental data with reasonable accuracy across various loading regimes, it is hypothesized to be a material property and sufficient to predict the fatigue life.</div><div><br></div><div>Inclusions are unavoidable in Ni-base superalloys, which lead to two competing failure modes, namely inclusion- and matrix-driven failures. Each factor related to the inclusion, which may contribute to crack initiation, is isolated and systematically investigated within RR1000, a powder metallurgy produced Ni-base superalloy, using CPFE simulations. Specifically, the role of the inclusion stiffness, loading regime, loading direction, a debonded region in the inclusion-matrix interface, microstructural variability around the inclusion, inclusion size, dissimilar coefficient of thermal expansion (CTE), temperature, residual stress, and distance of the inclusion from the free surface are studied in the emergence of two failure modes. The CPFE analysis indicates that the emergence of a failure mode is an outcome of the complex interaction between the aforementioned factors. However, the possibility of a higher probability of failure due to inclusions is observed with increasing temperature, if the CTE of the inclusion is higher than the matrix, and vice versa. Any overall correlation between the inclusion size and its propensity for damage is not found, based on inclusion that is of the order of the mean grain size. Further, the CPFE simulations indicate that the surface inclusions are more damaging than the interior inclusions for similar surrounding microstructures. These observations are utilized to instantiate twenty realistic statistically equivalent microstructures of RR1000 – ten containing inclusions and remaining ten without inclusions. Using CPFE simulations with these microstructures at four different temperatures and three strain ranges for each temperature, the critical SPSED is calibrated as a function of temperature for RR1000. The results suggest that critical SPSED decreases almost linearly with increasing temperature and is appropriate to predict the realistic emergence of the competing failure modes as a function of applied strain range and temperature.</div><div><br></div><div>LFW process leads to the development of significant residual stress in the components, and the role of residual stress in the fatigue performance of materials cannot be overstated. Hence, to ensure fatigue performance of the LFW Ti alloys, residual strains in LFW of similar (Ti-6Al-4V welded to Ti-6Al-4V or Ti64-Ti64) and dissimilar (Ti-6Al-4V welded to Ti-5Al-5V-5Mo-3Cr or Ti64-Ti5553) Ti alloys have been characterized using EDD. For each type of LFW, one sample is chosen in the as-welded (AW) condition and another sample is selected after a post-weld heat treatment (HT). Residual strains have been separately studied in the alpha and beta phases of the material, and five components (three axial and two shear) have been reported in each case. In-plane axial components of the residual strains show a smooth and symmetric behavior about the weld center for the Ti64-Ti64 LFW samples in the AW condition, whereas these components in the Ti64-Ti5553 LFW sample show a symmetric trend with jump discontinuities. Such jump discontinuities, observed in both the AW and HT conditions of the Ti64-Ti5553 samples, suggest different strain-free lattice parameters in the weld region and the parent material. In contrast, the results from the Ti64-Ti64 LFW samples in both AW and HT conditions suggest nearly uniform strain-free lattice parameters throughout the weld region. The observed trends in the in-plane axial residual strain components have been rationalized by the corresponding microstructural changes and variations across the weld region via BSE images. </div><div><br></div><div>In the literature, fatigue crack initiation in the LFW Ti-6Al-4V specimens does not usually take place in the seemingly weakest location, i.e., the weld region. From the BSE images, Ti-6Al-4V microstructure, at a distance from the weld-center, which is typically associated with crack initiation in the literature, are identified in both AW and HT samples and found to be identical, specifically, equiaxed alpha grains with beta phases present at the alpha grain boundaries and triple points. Hence, subsequent fatigue performance in LFW Ti-6Al-4V is analyzed considering the equiaxed alpha microstructure.</div><div><br></div><div>The LFW components made of Ti-6Al-4V are often designed for high cycle fatigue performance under high mean stress or high R ratios. In engineering practice, mean stress corrections are employed to assess the fatigue performance of a material or structure; albeit this is problematic for Ti-6Al-4V, which experiences anomalous behavior at high R ratios. To address this problem, high cycle fatigue analyses are performed on two Ti-6Al-4V specimens with equiaxed alpha microstructures at a high R ratio. In one specimen, two micro-textured regions (MTRs) having their c-axes near-parallel and perpendicular to the loading direction are identified. High-resolution DIC is performed in the MTRs to study grain-level strain localization. In the other specimen, DIC is performed on a larger area, and crack initiation is observed in a random-textured region. To accompany the experiments, CPFE simulations are performed to investigate the mechanistic aspects of crack initiation, and the relative activity of different families of slip systems as a function of R ratio. A critical soft-hard-soft grain combination is associated with crack initiation indicating possible dwell effect at high R ratios, which could be attributed to the high-applied mean stress and high creep sensitivity of Ti-6Al-4V at room temperature. Further, simulations indicated more heterogeneous deformation, specifically the activation of multiple families of slip systems with fewer grains being plasticized, at higher R ratios. Such behavior is exacerbated within MTRs, especially the MTR composed of grains with their c-axes near parallel to the loading direction. These features of micro-plasticity make the high R ratio regime more vulnerable to fatigue damage accumulation and justify the anomalous mean stress behavior experienced by Ti-6Al-4V at high R ratios.</div><div><br></div>