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This master’s thesis work is a study of oxidation and degradation of nickel-base alloys at high temperatures. The materials studied are designed for use in critical gas turbine components such as turbine blades and vanes. Some of the alloys are used today, whereas others have not yet entered commercial application. In order to maximize the efficiency of gas turbines, there is an ambition to maximize the operating temperatures. There is therefore a demand for materials which can withstand the damage mechanisms active at high temperatures. Among these damage mechanisms are oxidation and microstructural degradation. To investigate the oxidation resistance of 7 different monocrystalline and polycrystalline alloys, samples have been exposed isothermally in still air at temperatures between 850 and 1000°C, for exposure times of up to 20000h. Two of the alloys were also exposed cyclically at 950°C. Oxidation during the heat treatment resulted in significant weight changes, which were measured after each cycle for cyclically exposed samples and after completed heat treatment for isothermally exposed samples. The weight change data was used to evaluate the relative oxidation resistance of the alloys. The ranking of the alloys with respect to oxidation resistance was generally in agreement with the oxidation resistance predicted by a simple consideration of the Cr and Al contents of the alloys. However, the single-crystal alloy PWA1483 displayed better oxidation resistance than predicted from its chemical composition. Metallographic analysis of the samples indicated that the oxide scales formed consisted of several different types of oxides. The oxide scales were mainly composed of Cr2O3 and Al2O3. Fragments of the oxide scales spalled off, primarily during cooling but also in some cases during the long-term heat treatments. Spalling of the oxide scale accelerated the oxidation process, since the ability of the oxide scale to impede diffusion decreased with its decrease in thickness. Oxidation caused depletion of Al and thereby local dissolution of the aluminum-rich γ′ particles, which are of vital importance to the mechanical properties of the material. A γ′ depleted zone thereby formed underneath the oxide scale. In this zone nitrides and needle-like particles, believed to be topologically close packed μ phase, precipitated during heat treatment. Recrystallization in the depletion zone was observed in some of the monocrystalline materials. MC carbides (M=metal) present in the virgin material decomposed during heat treatment and M23C6 carbides were formed. The γ′ particles coarsened during heat treatment, which resulted in decreased hardness. The hardness decreased with exposure temperature up to 950°C, as expected due to the increased coarsening rate. At 1000°C an unexpected increase in hardness was observed for all sample materials except one. A possible explanation for this hardness increase is redistribution of γ′, by dissolution of γ′ during heat treatment and reprecipitation during cooling as much finer particles. A fine dispersion of γ′ is expected to contribute more to the hardness than a corresponding volume of γ′ in the form of larger particles. For some of the sample series, clear correlations between hardness and γ′ particle size or exposition time were found. These relationships could potentially be used to estimate the exposure temperature of service-exposed material. A numerical model was implemented in Matlab to describe the process of oxide growth and spalling, cycle by cycle. The model was successfully adapted to experimental data from the cyclic oxidation measurements. The general applicability of the model to cyclic oxidation data at different temperatures and cycle frequencies was not investigated. At long times of cyclic exposure, the net weight loss of the samples could be well approximated as a linear function of the number of cycles. However, during the last few cycles the amount of oxide spalled in each cycle suddenly decreased. This change in spallation behavior was mainly observed for the samples cooled in air between every cycle and to a much smaller extent for the samples cooled in water. The proposed explanation is that spalling occurred preferentially at a weak subscale interface and that the spalling propensity decreased with decreasing area of this weak interface. The deviating results of the last few cycles were not included in the modeling of the cyclic oxidation process.

No description available.

No description available.

No description available.

Les pales de turbine Haute Pression des turbines d'hélicoptères sont soumises à des sollicitations cycliques, thermiques et mécaniques, complexes. L'objectif de ce travail est de caractériser l'influence du cyclage thermique sur le comportement et l'endommagement en fluage de systèmes MCrAlY/superalliage à base de nickel et d'étudier les interactions entre le substrat et le revêtement à haute température. Dans un premier temps, des essais de vieillissement et de fluage isothermes ont été menés afin d'évaluer les dégradations environnementales et mécaniques de systèmes superalliage monocristallin CMSX-4/revêtement NiCoCrAlYTa, déposé selon différents procédés (codéposition électrolytique, projection HVOF). Ces essais de vieillissement isotherme et l'analyse microstructurale qui a été réalisée ont notamment permis d'évaluer le pouvoir protecteur des revêtements entre 950 et 1150°C. Des diagrammes d’occurrence de phases représentatifs de l'état de dégradation de ces revêtements ont été construits et ont montré une équivalence des deux procédés vis-à-vis de la protection du superalliage. Les essais de fluage isotherme ont ensuite confirmé cette équivalence et ont constitué une référence pour les essais de fluage cyclés thermiquement. La comparaison des essais de vieillissement et fluage isothermes a également montré que l’épaisseur de la zone d’interdiffusion entre le superalliage et le revêtement était indépendante de l’application d’une contrainte. Dans un second temps, une étude approfondie de l'influence du cyclage thermique sur le comportement en fluage à 1150°C des superalliages a été menée tout d'abord sur le superalliage MC2, pour évaluer l'effet des paramètres qui caractérisent les cycles thermiques (durée du palier à haute température, vitesses de refroidissement, effet de la température basse du cycle). L'effet du cyclage sur la vitesse de déformation et sur la durée de vie à rupture a été confirmé, et le rôle de la répétition des cycles thermiques sur l'accélération prématurée de l'endommagement de la structure du substrat et la déformation accrue a été mis en évidence. Enfin, le comportement en fluage cyclé thermiquement du système CMSX-4/NiCoCrAlYTa déposé par codéposition électrolytique a été caractérisé aux températures 1050 et 1150°C. Pour ces différentes conditions, particulièrement à 1150°C, il a de nouveau été montré sur ce matériau que les séquences rapides et successives de dissolution - re-précipitation de la phase γ' induisaient une accélération et une généralisation dans le substrat de la déstabilisation de la morphologie en radeaux. Dans une moindre mesure, il a également été montré que le cyclage thermique affecte la zone d'interdiffusion plus en profondeur dans le substrat. / Turbine blades of helicopters are subjected to complex thermal and mechanical cycles. The purpose of this work is to characterize the influence of the thermal cycling on high temperature creep behaviour and damage of MCrAlY coating / single crystal nickel-based superalloys systems, and to study the interactions between the superalloy and the coating. Firstly oxidation and isothermal creep tests have been performed to measure the environmental and mechanical resistance of systems made of CMSX-4 superalloy / NiCoCrAlYTa coating deposited by several processes (Tribomet process and HVOF spraying). Microstructure and chemical composition of both coatings were examined after oxidation and creep testing and quite similar observations were made for both coating processes. The combination of phases and chemical analysis after oxidation testing allowed the establishment of an occurrence diagram of phases for both coating processes, according to temperature and duration of exposure. The obtained diagrams seemed similar for both processes. Finally both processes appeared to be equivalent for the protection of CMSX-4 superalloy in isothermal oxidation and creep conditions. Moreover the growth of the inderdiffusion zone between coating and superalloy is independent of the stress. Secondly the influence of thermal cycling parameters on creep properties of the MC2 single crystal nickel-based superalloy has been studied at 1150°C and 80MPa.We have demonstrated that thermal cycling creep was more damaging than isothermal creep in terms of creep lifetime and rates. Furthermore, the number of low temperature incursions and low cooling and heating rates have severe detrimental effect on creep resistance, whereas the low temperature value of the thermal cycle is not significant. These results specify the role of re-precipitation and dissolution of γ’ particles during thermal cycling creep. Finally the effect of thermal cycling on high temperature creep of thin-walled and coated CMSX-4 single crystal superalloy was evaluated by performing thermal cycling and isothermal creep tests at 1050°C and 1150°C. The deleterious effect of thermal cycling on the creep behavior and lifetime has been confirmed, particularly for the condition at 1150°C and 80 MPa. Furthermore, the number of low temperature incursions has severe detrimental effect on creep resistance on account of the rafted microstructure destabilization induced by these sequences. These results confirm the role of re-precipitation and dissolution of γ’ particles during thermal cycling creep. Thermal cycling infers also on destabilization of subcoating zone in the superalloy but this effect seems to be secondary.

Les aubes de turbine haute pression en superalliage monocristallin sont refroidies, à la fois par un réseau de canaux internes, ainsi que par des perforations débouchantes. Soumises à des cycles thermo-mécaniques complexes, elles subissent des endommagements de type fatigue, fluage et oxydation. Pour valider les chaînes de prévision de durée de vie en conditions réelles d'utilisation, il a été nécessaire d’étudier des configurations d’essais technologiques reproduisant les conditions d'un cycle moteur en laboratoire. Pour cela, une installation d'essai de fatigue à gradient thermique de paroi est développée. Le gradient thermique est généré par chauffage de la surface externe et refroidissement interne par une circulation d’air. L’installation a ainsi permis la réalisation d'essais selon une complexité croissante, allant de l’essai isotherme jusqu'au cycle thermo-mécanique complexe, sur éprouvette tubulaire lisse ou multi-perforée. Afin d’analyser finement ces essais, deux méthodes de mesures sont étudiées. La méthode du potentiel électrique pour la détection et le suivi de fissure appliquée à des géométries complexes et la corrélation d’images, dont l’utilisation est étendue à la haute température. Le point-clé de la modélisation de ces essais est l'estimation du champ thermique. L'impossibilité de le mesurer sur éprouvette, a conduit à le déterminer numériquement, notamment par des simulations couplées aéro-thermiques. La chaîne de prévision de durée de vie intégrant l'aspect non-local, a ainsi pu être confrontée aux mesures expérimentales en termes de réponse mécanique, localisation de l'endommagement et durée de vie à amorçage. / Monocrystalline high pressure turbine blades are booth cooled by an internal channel network and side-wall crossing holes. As they undergo complex thermo-mechanical cycles they suffer fatigue, creep and oxidation damages. In order to validate lifetime prediction chain under real conditions of use, the study of technological test configurations reproducing turbine cycle conditions was necessary. For that, a thermal gradient mechanical fatigue facility is developed. Thermal gradient is generated through an external surface heating and an internal air cooling. As a result, tests could be conducted following a growing complexity on smooth and multi-perforated tubular specimens going from isothermal test up to thermo-mechanical complex cycle. The need of in-depth analysis of these tests led to the study of two measurement methods. The electrical potential drop method for crack detection and crack following applied to complex shapes and digital image correlation which use was extended to high temperatures. Simulation key issue is the thermal field estimation. Measurement complexity led us to numerically determine it by various methods including aero-thermal coupled calculations. Finally lifetime prediction chain including non-local coverage was confronted with experimental measurements in terms of mechanical response, damage localisation and crack initiation lifetime.

Ce manuscrit de thèse présente les résultats de travaux concernant les effets des transitoires thermiques sur la précipitation des phases intermétalliques dans le superalliage base nickel Inconel 718® et les conséquences de cette précipitation sur les propriétés mécaniques de cet alliage. Ces travaux se concentrent sur une approche couplée capable de décrire l’évolution de la précipitation de la phase γ'' et ses conséquences sur la limite d’élasticité de l’Inconel 718®. L’état de précipitation est modélisé grâce à l’implémentation des équations de la théorie classique de germination et de croissance, modifiées afin de prendre en compte la géométrie en plaquette des précipités γ''. Ce modèle de précipitation est ensuite validé par des données expérimentales issues de la littérature mais également d’observations au microscope électronique en transmission et d’essais de diffusion de neutrons aux petits angles. La distribution de taille de la phase γ'' ainsi simulée est utilisée comme donnée d’entrée d’un modèle de prédiction de la limite d’élasticité précipitation-dépendant. Ces limites d’élasticité simulées sont enfin comparées à des résultats expérimentaux issus d’essais de traction. Une maquette de soudage a ensuite été réalisée afin de tester le modèle de prévision de limite d’élasticité pour des transitoires thermiques, dans un cas industriel. / This thesis manuscript presents the results of work concerning the effects of thermal transients on the precipitation of intermetallic phases in the nickel-based superalloy Inconel 718® and the consequences of this precipitation on the mechanical properties of this alloy. This work focuses on a coupled approach capable of describing the evolution of the precipitation of the γ'' phase and its consequences on the yield strength of the Inconel 718®. The precipitation state is modeled thanks to the implementation of the equations of the classical germination and growth theory, modified to take into account the platelet geometry of the γ'' precipitates. This precipitation model is then validated by experimental data from the literature but also from transmission electron microscope observations and small angle neutron scattering tests. The size distribution of the γ'' phase thus simulated is used as the input data of a model for predicting the precipitation-dependent elasticity limit. These simulated elasticity limits are finally compared with experimental results from tensile tests. A welding model was then made to test the elastic yield prediction model for thermal transients in an industrial case.

O uso do cálculo termodinâmico e consequentemente base de dados desenvolvidas para esse propósito é hoje uma das ferramentas fundamentais para o aprimoramento e desenvolvimento de superligas a base de níquel. A proposta deste trabalho foi avaliar a confiabilidade de uma base de dados comercial, específica para superligas a base de níquel, utilizada em softwares de cálculos termodinâmicos computacionais. Comparou-se os dados experimentais da superliga Inconel 713LC com informações obtidas através do calculo termodinâmico para a composição química específica da superliga estudada. As amostras da superliga comercial Inconel 713LC foram retiradas de barras da liga fundida a vácuo (VIM). Os tratamentos térmicos foram realizados sob atmosfera de argônio em cápsulas de quartzo nas temperaturas de 600?C, 900?C e 1250 ?C nos tempos de 10h, 24h, 50h, 100h, 250h, 500h, 1000h e 2000 horas, de acordo com a temperatura de tratamento utilizada, visando acompanhar o desenvolvimento microestrutural até alcançar a condição de equilíbrio termodinâmico. Previamente, a amostra no estado bruto de fusão e as amostras após os tratamentos de equilíbrio foram caracterizadas microestruturalmente via microscopia eletrônica de varredura (MEV) e a composição das fases medidas por microanálise de energia dispersiva (EDS). As temperaturas das transformações de fases foram medidas por analise térmica diferencial (DTA). Nas amostras também foram realizadas medidas de microdureza para acompanhar indiretamente a evolução microestrutural da fase gama prime. Para os cálculos termodinâmicos foram utilizados o software Thermo-Calc® e a base de dados TTNi8 da empresa Thermotech Ltd®. / The computational thermodynamic simulation and the databases designed for this purpose are today one the most important tools to develop new nickel based superalloys. The aim of this work was to check the reliability of a commercial database, designed specifically for Ni-based superalloys. The experimental phase diagram data of Inconel 713LC, such as, liquidus and solidus temperatures as well as chemical phase compositions were compared with thermodynamic information extracted from computational simulations. Samples of a commercial superalloy Inconel 713LC were extracted from an ingot produced by Vacuum Induction Melting (VIM) and heat treated under argon in quartz capsules at 600?C, 900 ?C and 1250?C for 10h, 24h, 50h, 100h, 250h, 500h, 1000h and 2000h, according to the treatment temperature used, aiming at reaching the thermodynamic equilibrium conditions. The as-cast and all heat-treated samples were characterized by Scanning Electron Microscopy (SEM) and the chemical compositions of the phases were measured via Energy Dispersive X-ray Spectroscopy (EDS). Temperatures of phase transformations were determined by Differential Thermal Analysis (DTA). Microhardness measurements were performed to indirectly follow the microstructural evolution of gamma prime. The Thermo-Calc® software and the TTNi8 database from Thermotech Ltd® were used for thermodynamic calculations.