Les superalliages sont des matériaux clés en aéronautique. Ces matériaux sont utilisés pour la fabrication des pièces des parties chaudes des turboréacteurs d’avion. Les recherches pour une alternative des superalliages à base de Ni avec des caractéristiques supérieurs, ont abouti en 2006 à la découverte d’une nouvelle génération de superalliage à base de cobalt basée sur le système Co-Al-W avec une microstructure γ/γ' similaire aux superalliages à base nickel. Trois nuances d’alliages avec différent ratio Al/W ont été étudiées dans ce travail. L’objectif de ce travail a été dans un premier temps d’étudier l’évolution de la microstructure à 900 °C et de comprendre les mécanismes de transformation et de dissolution de la phase γ'. Pour cela des études en MEB et en MET ont été menées sur des échantillons recuits à 900 °C pendant divers temps. Nous avons montré que la phase γ' est une phase métastable et qu’elle se dissout au profit des phases Co3W et CoAl. Nous avons mis en évidence un mécanisme de dissolution par fractionnement des précipités γ' suivant les plan denses (111) et de fautesd’empilement donnant naissance à la phase D019. Dans un second temps nous avons étudié la cinétique de précipitation dans des alliages faiblement sursaturés. Les stades de germination, de croissance et de la coalescence ont été étudiés en se focalisant sur l’évolution temporelle de la composition des phases γ et γ ׳. Les données expérimentales ont été confrontées aux toutes dernières théories de germination, croissance et coalescence développées pour les alliages multicomposants non dilués, et qui prédisent l’évolution temporelle des compositions des phases γ et γ ׳. Ainsi, nous avons montré que l’évolution temporelle des paramètres cinétiques tels que la taille moyenne et la densité de particules durant la coalescence sont assez prochesde celles prévues par la théorie de coalescence de LSW. Grâce à la sonde atomique tomographique nous avons montré que la composition en W des phases γ et γ' décroit dans le temps. La décroissance de la teneur en W en particulier dans la phase γ' est observée pour la première fois dans ces alliages et elle est due aux effets de capillarité et de couplage des fluxde diffusion. Un très bon accord avec les nouvelles théories de germination, croissance et coalescence dans les ulticomposants a été démontré. Enfin à partir des modèles théoriques et de la base thermodynamique du système ternaire CoAlW nous avons déterminé l’énergie interfaciale dont les valeurs calculées sont comprises entre 30 et 48 mJ/m2. / Superalloys are key material in aerospace industry. These materials are used to manufacturing the high temperature part of aeroengines. Currently Ni-based superalloys are the most widely used materials for high temperature applications. Researches for a new generation of superalloys with better properties have lead in 2006 to the discovery of a new stable L12 ordered, Co3(Al,W) phase embedded in the disordered γ-Co solid-solution matrix. This work aims to study the evolution of the microstructure at 900 °C and understanding the mechanism of dissolution and transformation of the γ' phase. Three different alloys with different Al/W ratios are studied here. TEM and MEB analyses are carried out on samples aged at 900 °C forvarious time. We show that γ' is a metastable phase and it dissolves in favor of B2-CoAl and D019-Co3W phases. Moreover, we highlight a mechanism of dissolution by fragmentation along the {111} close packed planes and stacking faults giving rise to D019 phase. We also study the kinetics of precipitation in the low supersaturated alloys.The early stages of precipitation of the γ' phase in a model Co based superalloy have been investigated at 900 °C using electron microscopy and atom probe tomography in the low supersaturated alloys. Nucleation, growth and coarsening stages have been studied with a focus on the temporal evolution of the precipitate composition in the light of recent theoretical developments on phase separation in multicomponent alloys. The experimental data have been confronted to the theories of nucleation and coarsening recently developed for such alloys, which are valid for non-ideal and non-dilute systems, and predict the temporal evolution of both the matrix and precipitate compositions. The rate constant for the mean size evolution of the particles, as derived from experiments, has been compared to the one predicted by the mentioned coarsening theory that accounts for a more accurate description of the thermodynamics of the phases, as compared with more classical approaches. From this comparison the γ/γ' interfacialenergy was derived and found to range between 30 and 48 mJ/m2. The exponents for the temporal evolution of average particles size, number of particles per unit volume were found identical to those for binary alloys during the coarsening regime, as expected, and the temporal evolutions of compositions in both γ and γ' phases were found to evolve as predictedby theory. Indeed, the W content in the particles, measured from atom probe tomography (APT) experiments, was found to significantly decrease with time and the observed evolution is remarkably well described by the theory and therefore is shown to originate from the competition between diffusion and capillarity.

This thesis is about laser powder bed fusion (L-PBF) of the nickel-based superalloy: Alloy 247LC. Alloy 247LC is used mainly in gas turbine blades and processing the blades with L-PBF confers performance advantage over the blades manufactured with conventional methods. This is mainly because L-PBF is more suitable, than conventional methods, for manufacturing the complex cooling holes in the blades. The research was motivated by the need for academia and industry to gain knowledge about the processability of the alloy using L-PBF. The knowledge is essential in order to eventually solve the problem of cracking which is a major problem when manufacturing the alloy. In addition, dense parts with low void content should be manufactured and the parts should meet the required performance. Thus, the thesis answered some of the important questions related to process parameter-microstructure-defect relationships. The thesis presented an introduction in chapter 1. A literature review was made in chapter 2 to 4. In chapter 2, the topic of additive manufacturing was introduced followed by an overview of laser powder bed fusion. Chapter 3 focused on superalloys. Here, a review was made from the broader perspective of superalloys but was eventually narrowed down to the characteristics of nickelbased superalloys and finally Alloy 247LC. Chapter 4 reviewed the main research on L-PBF of Alloy 247LC. The methodology applied in the thesis was discussed in chapter 5. The thesis applied statistical design of experiments to show the influence of process parameters on the defects and microstructure, so a detail description of the method was warranted. This was given at the beginning of chapter 5 and followed by the description of the L-PBF manufacturing and the characterization methods. The main results and discussions, in chapter 6, included a preliminary investigation on how the process parameters influenced the amount of discontinuity in single track samples. This was followed by the results and discussions on the investigation of voids, cracks and microhardness in cube samples (detail presentation was given in the attached paper B). Finally, the thesis presented results of the microstructure obtainable in L-PBF manufactured Alloy 247LC. The initial results of the microstructure investigation were presented in paper A.

<div>Additively manufactured (AM) metals have been increasingly fabricated for structural applications. However, a major hurdle preventing their extensive application is lack of understanding of their mechanical properties. To address this issue, the objective of this research is to develop a computational model to simulate the creep behavior of nickel alloy 718 manufactured using the laser powder bed fusion (L-PBF) additive manufacturing process. A finite element (FE) model with a subroutine is created for simulating the creep mechanism for 3D printed nickel alloy 718 components.</div><div><br></div><div>A continuum damage mechanics (CDM) approach is employed by implementing a user defined subroutine formulated to accurately capture the creep mechanisms. Using a calibration code, the material constants are determined. The secondary creep and damage constants are derived using the parameter fitting on the experimental data found in literature. The developed FE model is capable to predict the creep deformation, damage evolution, and creep-rupture life. Creep damage and rupture is simulated as defined by the CDM theory.</div><div>The predicted results from the CDM model compare well with experimental data, which are collected from literature for L-PBF manufactured nickel alloy 718 of creep deformation and creep rupture, at different levels of temperature and stress. </div><div><br></div><div>Using the multi-regime Liu-Murakami (L-M) and Kachanov-Rabotnov (K-R) isotropic creep damage formulation, creep deformation and rupture tests of both the secondary and tertiary creep behaviors are modeled.</div><div>A single element FE model is used to validate the model constants. The model shows good agreement with the traditionally wrought manufactured 316 stainless steel and nickel alloy 718 experimental data collected from the literature. Moreover, a full-scale axisymmetric FE model is used to simulate the creep test and the capacity of the model to predict necking, creep damage, and creep-rupture life for L-PBF manufactured nickel alloy 718. The model predictions are then compared to the experimental creep data, with satisfactory agreement.</div><div><br></div><div>In summary, the model developed in this work can reliably predict the creep behavior for 3D printed metals under uniaxial tensile and high temperature conditions.</div>

During operational conditions of internal combustion turbines of turbojet engines, the impeller blades are stressed by load cycles which vary in time, temperature and stress. In the course of operation, the blades are exposed to a considerable number of degradation effects, particularly high-temperature corrosion, fatigue processes and creep. The presented work is aimed at the study of the structure cast nickel-base superalloy INCONEL 713 LC, creep tests exposured. The structural changes (degradation) was clasifikation by the help of image analyses. Operational conditions of heat parts, used in gas turbines and turbo-compressors, were simulated by creep tests of Inconel 713 LC nickel superalloy during a constant load of temperatures ranging from 750 up to 950C. Changes in the structure dependent upon time, temperature and stress applied were analysed by means of light and electron microscopy methods and image analyses after the fracture of test bars.

Un modèle phénoménologique 3D de visco-plasticité couplée avec les évolutions microstructurales et l'endommagement est proposé pour les superalliages monogranulaires base Nickel, les matériaux des aubes de turbine à haute pression de moteurs d'hélicoptères. L'anisotropie de la mise en radeaux, la croissance et la dissolution de la phase durcissante sont modélisés. Une variable tensorielle et sa loi d'évolution permettent la description de la variation de la largeur des couloirs de matrice. Ce travail s'appuie sur la décomposition en modes de Kelvin du tenseur d'élasticité. Cette décomposition conduit également à une description multi-critère mésoscopique de la visco-plasticité cubique. Une formulation en (visco-)plasticité cristalline a été également proposée. Une loi d'endommagement avec seuil de type dD/dt=... est formulée pour la modélisation du fluage tertiaire et pour la prévision de la ductilité en traction. Une expression originale du seuil d'endommagement rend compte des effets de vitesse sur l'amorçage de l'endommagement par visco-plasticité. Une étude expérimentale a été conduite sur le CMSX-4, l'alliage au centre de cette étude, parallèlement aux travaux de modélisation. Des essais de dissolution ont été réalisés afin de mesurer la variation de la fraction volumique des précipités avec la température. Les mécanismes de déformation du matériau ont été observés en fluage isotherme à 850°C et 1050°C selon les principales directions cristallines du triangle stéréographique standard et constituent une base d'identification pour le modèle, la réponse mécanique du matériau obtenue. Trois essais de traction ont été réalisés selon la direction <111>, deux à vitesse de chargement constante, le troisième à vitesse variable. Des essais cyclés thermiquement de type 150h-moteur ont été réalisées sur le banc MAATRE. Des analyses EBSD et MET ont été réalisés sur les échantillons orientés selon les directions cristallines <011>, <111> et <112> et testés à 850°C. Ces analyses ont montré que le mâclage est le principal mécanisme de déformation pour des déformations supérieures à $1-2%$ selon ces orientations cristallines en fluage à cette température et à haute contrainte (>400 MPa). Enfin, le modèle a été implanté dans le code à élément Finis ZéBuLon, sans ou avec endommagement, et des calculs de structures ont été réalisés / A 3D phenomenological model coupling viscoplasticity, microstructural evolutions and damage is proposed for Ni-based single crystal superalloys, which are widely used materials for high pressure turbine blade in helicopter engines. The anisotropy of the gamma'-rafting, the gamma'-coarsening and the dissolution of the hardening gamma' phase are modeled. A tensorial variable and its evolution law allow to describe the variation of the gamma channels. The modeling is based on the Kelvin decomposition of the elasticity tensor. This decomposition leads to a phenomenological multi-criterion description of the cubic visco-plasticity. A formulation based on the single crystal (visco-)plasticity framework is also proposed. A damage law of type dD/dt=… is introduced in order to model the tertiary creep stage and the ductility. A novel rate sensitive damage threshold is introduced in order to account for the rate sensitivity of the damage onset by visco-plasticity. An experimental study has been carried out on the CMSX-4 alloy, which is the material of main interest in this study, in parallel to the modeling work. Dissolution tests have been carried out to measure the gamma'-volume fraction variation with temperature. The deformation mechanisms of the CMSX-4 alloy have been observed by performing tensile creep tests at 1050°C and 850°C. These tests have also constituted a database for the model identification. Three tensile tests have been realized along the <111> crystal direction, two at constant strain rate and the third by varying the strain rate. Non-isothermal creep tests reproducing the 150h-type engine test have been performed on the MAATRE bench. EBSD and TEM analysis have been realized on the specimens oriented along the <011>, <011> and <112> crystal directions and crept at 850° C. These analysis have shown that micro-twinning governs the deformation along these crystal directions during creep at this temperature and at high stresses (> 400 MPa) for deformation in excess of 1-2%. Finally, the model (with and without damage) has been encoded in the ZéBuLoN Finite Element solver and structure computations have been performed.

The present doctoral thesis is focused on the effect of dwells on the low cycle fatigue behaviour of advanced high temperature materials. 10 minutes strain holds are introduced into the cyclic straining of cast Ni-based superalloy IN792-5A and cast intermetallic alloy TiAl-7Nb which were chosen as experimental material. Fatigue experiments were conducted in strain control mode with constant total strain amplitude and strain rate. IN792-5A was subjected to continuous cyclic loading test as well as fatigue tests either with tensile peak strain holds or compressive peak strain holds at temperature 800 °C. TiAl-7Nb was experimentally examined by continuous cyclic loading tests and also by fatigue test with tensile peak strain hold times at temperature 750 °C. Cyclic hardening/softening curves, cyclic stress-strain curves, Manson-Coffin curves and Basquin curves were obtained. Stress relaxation data were measured during hold times. Mean stress evolution was observed and documented. Microstructure of both alloys was observed in as-received state and also after cyclic loading by means of SEM and TEM. Surface relief investigation revealed cyclic plastic strain localisation as well as fatigue crack initiation sites. Fatigue crack propagation was described using fracture surface and longitudinal gauge section observations. Dislocation structures developed in the course of fatigue tests were studied and documented.

Anisotropic tertiary creep damage formulations have become an increasingly important prediction technique for high temperature components due to drives in the gas turbine industry for increased combustion chamber exit pressures, temperature, and the use of anisotropic materials such as metal matrix composites and directionally-solidified (DS) Ni-base superalloys. Typically, isotropic creep damage formulations are implemented for simple cases involving a uniaxial state of stress; however, these formulations can be further developed for multiaxial states of stress where materials are found to exhibit induced anisotropy. In addition, anisotropic materials necessitate a fully-developed creep strain tensor. This thesis describes the development of a new anisotropic tertiary creep damage formulation implemented in a general-purpose finite element analysis (FEA) software. Creep deformation and rupture tests are conducted on L, T, and 45°-oriented specimen of subject alloy DS GTD-111. Using the Kachanov-Rabotnov isotropic creep damage formulation and the optimization software uSHARP, the damage constants associated with the creep tests are determined. The damage constants, secondary creep, and derived Hill Constants are applied directly into the improved formulation. Comparison between the isotropic and improved anisotropic creep damage formulations demonstrates modeling accuracy. An examination of the off-axis creep strain terms using the improved formulation is conducted. Integration of the isotropic creep damage formulation provides time to failure predictions which are compared with rupture tests. Integration of the improved anisotropic creep damage produces time to failure predictions at intermediate orientations and any state of stress. A parametric study examining various states of stress, and materials orientations is performed to verify the flexibility of the improved formulation. A parametric exercise of the time to failure predictions for various levels of uniaxial stress is conducted.

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