The commercial polycrystalline superalloy RR1000 developed for turbine disc applications contains a large number of alloying elements. This complex alloy chemistry is required in order to produce appropriate microstructures and the required mechanical properties, such that the most important strengthener γʹ displays complex alloy chemistry. The broad aim of this project is to develop an approach to measuring the composition of γʹ precipitates at a broad range of length scales from nanometres to hundreds of nanometres, and subsequently develop a better understanding of the role of thermodynamics and diffusion kinetics on γʹ phase separation and precipitate growth. A solution of the absorption-corrected EDX spectroscopy to spherical particles was developed in our work, therefore enabling the quantitative analysis of precipitates' composition using an absorption-corrected Cliff-Lorimer approach. By performing this quantification, size-dependent precipitate compositional variations were obtained. Examination of this quantitative approach was compared to thermodynamic calculations of primary γ' precipitates possessing equilibrium compositions. Given the development of semi-quantitative compositional measurements for spherical γʹ precipitates and that cooling is one of the most common and critical regimes in physical metallurgy of Ni-based superalloys, this approach was then applied to study the local compositional variations that are induced in γ' precipitates when the alloy RR1000 undergoes different cooling rates. These measured compositions have been compared to detailed thermodynamic calculations and provide new experimental evidence of the importance of the dominant role of aluminium antisite diffusion in determining the low-temperature growth kinetics of fine-scale γ' precipitates. We have applied a similar analysis approach to study the compositional variations of γʹ cores within the class of secondary precipitates upon cyclic coarsening and reversal coarsening. It was shown that supersaturated Co in secondary γʹ exhibits an overall trend towards the equilibrium but Co content can significantly increase as γʹ coarsens. It was demonstrated that the limited elemental diffusivity in γ and γʹ compared to the observed coarsening rate in the coarsening regime results in the long-lasting Co supersaturation in γʹ and builds up elemental enhancements or depletions. These inhomogeneous elemental distributions produce compressive elastic constraints on large-scale secondary γʹ, therefore inducing morphological instability of these γʹ and causing the reversal coarsening. These results enable us to better understand the role that both thermodynamics and limited diffusion kinetics plays in controlling the complex microstructures of γ' precipitates.

A haute température, l’interdiffusion entre un superalliage et son revêtement protecteur (ß-NiAl ou ß- NiPtAl) dégrade à la fois la protection contre l’oxydation, par modification de la composition chimique du revêtement, et la microstructure du superalliage (3ième et 4ième générations) par formation de Zones de Réaction Secondaires (SRZ). Le but de cette étude a donc été (1) de développer des barrières de diffusion (BD) constituées d’une dense précipitation de phases a-W après traitement sous vide (BD simple) ou chromisation en phase vapeur (BD enrichie en chrome) (2) de mettre au point une méthode pour en étudier l’efficacité. Des mesures de concentration chimique (à partir de cartographies spectrales EDS), couplées à des ajustements des comportements en oxydation cyclique en utilisant le modèle « p-kp », et le développement d’un modèle « p-kp-ß » ont permis de montrer l’efficacité de la BD selon sa composition et la durée de vieillissement. Pour des longues durées de vieillissement, l’efficacité de la BD se réduit par la dissolution des précipités d’a-W dans les phases y’ et y formées à cause de la dégradation des propriétés protectrices du revêtement ß NiPtAl (augmentation de l’écaillage de l’oxyde formé et de la cinétique d’oxydation). Plusieurs causes probables de cette dégradation ont pu être déterminées, soit dues aux procédés (pollution au soufre) soit liées à la mise en place de la BD : augmentation de la transformation martensitique, enrichissement en tungstène et présence de précipités d’alpha chrome. Enfin, il a été montré que si l’initiation des SRZ est modifiée par l’ajout de la BD, leur cinétique de propagation ne l’est pas et est essentiellement dépendante de la composition de l’alliage. Un modèle de propagation des SRZ décrivant les évolutions chimiques locales de part et d’autres de l’interface « SRZ / superalliage » a été proposé. L’ajout de chrome à la BD permet d’inhiber la formation des SRZ, une couche riche en phases TCP remplace alors la SRZ. / At high temperature, interdiffusion between a superalloy and its protective coating (ß-NiAl or ß- NiPtAl) degrades the oxidation protection by modifying the chemical composition of the coating. It also degrades the 3rd et 4th generation superalloy microstructure due to the formation of Secondary Reaction Zones (SRZ). As a consequence, the aim of this study was (1) to develop diffusion barriers (DB) composed of a dense precipitation of a-W phases after a thermal treatment under vacuum (simple DB) or a vapour phase chromisation (Cr enriched DB), (2) to develop a method for quantifying the DB efficiency. Chemical concentration measurements (with EDS spectral maps) coupled with the « p-kp » modelling of the cyclic oxidation kinetics, and the development of the model « p-kp-ß » have permitted to study DB efficiency as a function of its composition and its high temperature ageing. For long ageing duration, the efficiency of the DB is reduced. Indeed, it is shown that the DB degrades the protection character of the ß-NiPtAl by increasing the oxide scale spallation and of its growth kinetic. This, in turns, accelerates the ß to y’ and y phases transformation and then increases the a-W precipitates dissolution. Some likely causes of this degradation have been determined, either due to the process (sulphur pollution) or intrinsic of the DB addition (increase of the martensitic transformation, enrichment in tungsten and a-Cr formation in the coating). Finally, it has been proved that DB addition modifies the SRZ initiation but not their propagation kinetic, which only depends on the superalloy local composition. A SRZ propagation model which describes local chemical evolutions on both sides of the « SRZ / superalloy » interface was proposed. The addition of chromium to the DB permits to inhibit the SRZ formation. In this case, a layer rich in TCP platelets replaces the SRZ.

Neste trabalho foi avaliada a influência das condições de processamento (pouring temperature and de vazamento e condições de isolamento térmico dos moldes cerâmicos) na formação de trincas nas palhetas de turbinas policristalinas, a base da superliga B1914, produzidas por microfusão. E devido à falta de informações sobre a superliga B1914 foram levantadas informações sobre o equilíbrio de fases (THERMOCALC) e foi realizada a caracterização microestrutural e mecânica deste material desta liga no estado bruto e tratada termicamente. Todas as palhetas vazadas a 1570, 1520 e 1470 °C em moldes sem isolamento e com isolamento parcial apresentaram trincas e outros defeitos de solidificação. Já as palhetas vazadas em moldes totalmente isolados estavam livres das trincas. No entanto foram identificados aglomerados de microporos na raíz de todas as palhetas. Os resultados de simulação de fração de fases mostraram que o equilíbrio de fases da superliga B1914 é constituído majoritariamente pelas fases γ e γ\' e pelas fases minoritárias MB2, M3B2 e sigma. A caracterização microestrutural da superliga B1914 confirmou os resultados de simulação e foram identificadas as fases gama (&#947) - dendritas e os precipitados da fase gama linha (&#947\') - no interior das dendritas e na região interdendrítica. As fases M3B2 e eram os microconstituintes do eutético. Os resultados de DTA e Scheil mostraram que o processo de solidificação, da superliga B1914, ocorreu fora de equilíbrio. Nos resultados obtidos a partir dos tratamentos térmicos, ficaram evidentes as dificuldades encontradas para solubilização das placas da fase &#947\'. A integridade estrutural dos corpos-de-prova foi comprometida pela presença de defeitos de solidificação (vazios). Tanto que os valores de LR e r obtidos nos ensaios estão muito abaixo dos valores encontrados na literatura. / This study was evaluated the influence of processing conditions (temperatures of casting conditions and thermal insulation of ceramic shells) in crack formation of equiaxed B1914 turbine blades produced by investment casting. Due to lack of information about B1914 alloy was performed microstructural and mechanical characterization of this alloy material in the raw state and treated. In shells uninsulated and partly insulated, after pouring was observed casting solidification defects. However the shells in a fully insulated were not observed casting crack formation. However were identified clusters of micropores in the root of all blades. The results of simulation phase fraction showed that the balance of phases in B1914 alloy is made mostly by γ and γ\' phases and the minority phases: MB2, M3B2 and sigma. The microstructural characterization of B1914 alloy confirmed the results of simulation and were identified: gamma (γ) - dendrites and gamma prime (γ\') - inside the dendrites and interdendritic regions. The M3B2 was found in eutectic. The results of DTA and Scheil showed that the process of solidification occurred in non-equilibrium. The results obtained from the thermal treatments showed difficulties to solubilize γ\' phase. The structural integrity of samples was compromised by the presence of solidification defects (pores). Both values of LR and εr obtained in the tests are much below the values found in literature.

This study develops a method to simulate a full-scale inertia friction weld with a sub-scale specimen and modifies a direct drive friction stir welder to perform the welding process. A torque meter is fabricated for the FSW machine to measure weld torque. Machine controls are modified to enable a force control during the IFW process. An equation is created to measure weld upset due to deflection of the FSW machine. Data obtained from a full-scale inertia friction weld are altered to account for the geometrical differences between the sub-scale and full-scale specimens. The IFW are simulated with the sub-scale specimen while controlling spindle RPM and matching weld power or weld RPM. The force used to perform friction welding is scaled to different values accounting for specimen size to determine the effects on output parameters including: HAZ, upset, RPM, torque, power and energy of the weld. Increasing force has positive effects to upset, torque, power and energy of the welds, while reducing the size of the HAZ.

A model was created to predict the thermo-mechanical fatigue crack growth rates under typical engine spectrum loading conditions. This model serves as both a crack growth analysis tool to determine residual lifetime of ageing turbine components and as a design tool to assess the effects of temperature and loading variables on crack propagation. The material used in the development of this model was a polycrystalline superalloy, Inconel 100 (IN-100). The first step in creating a reliable model was to define the first order effects that influence TMF crack growth in a typical engine spectrum. Load interaction effects were determined to be major contributors to lifetime estimates by influencing crack growth rates based upon previous load histories. A yield zone model was modified to include temperature dependent properties that controlled the effects of crack growth retardation and acceleration based upon overloads and underloads, respectively. Multiple overload effects were included in the model to create enhanced retardation compared to single overload tests. Temperature interaction effects were also considered very important due to the wide temperature ranges of turbine engine components. Oxidation and changing temperature effects were accounted for by accelerating crack growth in regions that had been affected by higher temperatures. Constant amplitude crack growth rates were used as a baseline, upon which load and temperature interaction effects were applied. Experimental data of isolated first order effects was used to calibrate and verify the model. Experimental data provided the means to verify that the model was a good fit to experimental results. The load interaction effects were described by a yield zone model, which included temperature dependent properties. These properties were determined experimentally and were essential in the model's development to include load and temperature contributions. Other interesting factors became apparent through testing. It was seen that specific combinations of strain rate and temperature would lead to serrated yielding, discovered to be the Portevin-Le Chatelier effect. This effect manifested itself as enhanced hardening, leading to unstable strain bursts in specimens that cyclically yielded while changing temperature.

In spite of its significance in industrial applications, the prediction of the influence of microstructure on the early stages of crack formation and growth in engineering alloys remains underdeveloped. The formation and early growth of fatigue cracks in the high cycle fatigue regime lasts for much of the fatigue life, and it is strongly influenced by microstructural features such as grain size, twins and morphological and crystallographic texture. However, most fatigue models do not predict the influence of the microstructure on early stages of crack formation, or they employ parameters that should be calibrated with experimental data from specimens with microstructures of interest. These post facto strategies are adequate to characterize materials, but they are not fully appropriate to aid in the design of fatigue-resistant engineering alloys. This thesis considers finite element computational models that explicitly render the microstructure of selected FCC metallic systems and introduces a fatigue methodology that estimates transgranular and intergranular fatigue growth for microstructurally small cracks. The driving forces for both failure modes are assessed by means of fatigue indicators, which are used along with life correlations to estimate the fatigue life. Furthermore, cracks with meandering paths are modeled by considering crack growth on a grain-by-grain basis with a damage model embedded analytically to account for stress and strain redistribution as the cracks extend. The methodology is implemented using a crystal plasticity constitutive model calibrated for studying the effect of microstructure on early fatigue life of a powder processed Ni-base RR1000 superalloy at elevated temperature under high cycle fatigue conditions. This alloy is employed for aircraft turbine engine disks, which undergo a thermomechanical production process to produce a controlled bimodal grain size distribution. The prediction of the fatigue life for this complex microstructure presents particular challenges that are discussed and addressed. The conclusions of this work describe the mechanistic of microstructural small crack. In particular, the fatigue crack growth driving force has been characterized as it evolves within grains and crosses to other grains. Furthermore, the computational models serve as a tool to assess the effects of microstructural features on early stages of fatigue crack formation and growth, such as distributions of grain size and twins.

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.

Co-20Cr-15W-10Ni alloy (L-605) is a cobalt-based superalloy combining high strength with keeping high ductility, biocompatible and corrosion resistant. It has been used successfully for heart valves for its chemical inertia, and this alloy is a good candidate for stent elaboration. Control of grain size distribution can lead to significant improvement of mechanical properties: in one hand grain refinement enhance the material strength, and on the other hand large grains provide the ductility necessary to avoid the rupture in use. Therefore, tailoring the grain size distribution is a promising way to adapt the mechanical properties to the targeted applications. The grain size can be properly controlled by dynamic recrystallization during the forging process. Therefore, the comprehension of the recrystallization mechanism and its dependence on forging parameters is a key point of microstructure design approach. The optimal conditions for the occurrence of dynamic recrystallization are determined, and correlation between microstructure evolution and mechanical behavior is investigated. Compression tests are carried out at high-temperature on Thermec-master Z and Gleeble forging devices, followed by gas or water quench. Mechanical behavior of the material at high temperature is analyzed in detail, and innovative methods are proposed to determine the metallurgical mechanisms at stake during the deformation process. Mechanical properties of the material after hot-working and annealing treatments are investigated. The grain growth kinetics of L-605 alloy is determined, and experimental results are compared with the static recrystallization process. Microstructures after hot deformation are evaluated using SEM-EBSD and TEM. Significant grain refinement occurs by dynamic recrystallization for high temperature and low strain rate (T≥1100 ◦ C, strain rate < 0.1s−1), and at high strain rate (strain rate > 10s−1). Dynamic recrystallization is discontinuous and takes place from the grain boundaries, leading to a necklace structure. The nucleation mechanism is most likely to be bulging from grain boundaries and twin boundaries. A new insight of the modeling of dynamic recrystallization taking as a starting point the experimental data is proposed. By combining the results from the mechanical behavior study and microstructure observation, the recrystallization at steady-state is thoroughly analyzed and provides the mobility of grain boundaries. The nucleation criterion for the bulging from grain boundaries is reformulated to a more general expression suitable for any initial grain size. Nucleation frequency can be deduced from experimental data at steady-state through modeling, and is extrapolated to any deformation condition. From this point, a complete analytical model of the dynamic recrystallization is established, and provides a fair prediction on the mechanical behavior and the microstructure evolution during the hot-working process.

Inconel 718 (IN 718) is widely used in applications, such as aircraft and power turbine components. Recently, fiber laser welding has become an attractive joining technique in industry for fabrication and repair of service-damaged components. However, a major limitation in the laser welding of IN 718 is that liquation cracking occurs. In the present work, autogenous fiber laser welding of IN 718 was used to study the effects of welding parameters and different pre-weld heat treatments on liquation cracking. Contrary to previous studies, a dual effect of heat input on cracking is observed. A rarely reported effect of heat input is attributed to process instability. Liquation cracking increases with pre-weld heat treatment temperatures that increase grain size and/or, possibly, intregranular boron segregation. The study shows that pre-weld heat treatment at 950oC can be used for repair welding of IN 718 without significant loss in cracking resistance.

Inconel 718 (IN 718) is widely used in applications, such as aircraft and power turbine components. Recently, fiber laser welding has become an attractive joining technique in industry for fabrication and repair of service-damaged components. However, a major limitation in the laser welding of IN 718 is that liquation cracking occurs. In the present work, autogenous fiber laser welding of IN 718 was used to study the effects of welding parameters and different pre-weld heat treatments on liquation cracking. Contrary to previous studies, a dual effect of heat input on cracking is observed. A rarely reported effect of heat input is attributed to process instability. Liquation cracking increases with pre-weld heat treatment temperatures that increase grain size and/or, possibly, intregranular boron segregation. The study shows that pre-weld heat treatment at 950oC can be used for repair welding of IN 718 without significant loss in cracking resistance.