Les alliages à base Nickel polycristallins sont largement utilisés pour les pièces aéronautiques soumises à des sollicitations extrêmes en service. Des objectifs toujours plus ambitieux en termes de rendement énergétique des moteurs d’avions ont conduit les constructeurs à augmenter leur température de fonctionnement. Les nuances utilisées jusqu’alors dans les parties chaudes, tels que l’Inconel 718, n’ont pas une tenue mécanique suffisante à ces températures. Le René 65 est un nouvel alliage à microstructure γ-γ’ élaboré spécifiquement pour ces applications. Il a été retenu par Safran Aircraft Engines comme constituant des disques de turbine basse pression du nouveau turboréacteur LEAP. Pour garantir la bonne tenue des disques, une microstructure fine et homogène est requise. Le procédé de forgeage de ces pièces est une séquence d’étapes de déformation à chaud et de traitements thermiques, durant lesquelles la microstructure évolue. Si les phénomènes physiques gouvernant les évolutions microstructurales sont connus, leurs mécanismes exacts et leurs cinétiques varient d’un alliage à l’autre.Des essais de déformation à chaud ont été réalisés en laboratoire dans différentes conditions de température, vitesse et taux de déformation représentatifs des procédés industriels. L’étude précise des mécanismes de recristallisation dynamique, ainsi que de leurs cinétiques, constitue la première partie de ce travail. La caractérisation fine des microstructures déformées a permis de mettre en évidence un nouveau mécanisme de recristallisation, dit de recristallisation en hétéroépitaxie, qui se superpose aux autres mécanismes conventionnels. L’interaction entre ces différents mécanismes ainsi que leurs cinétiques relatives ont été établies dans une vaste gamme de conditions de déformation. Il est démontré que ce mécanisme de recristallisation s'applique également à d'autres alliages γ-γ’. La deuxième partie de l’étude est consacrée à la stabilité des microstructures déformées lors de leur exposition à haute température. L'alliage René 65, comme d’autres alliages à base Nickel, est sensible à un phénomène indésirable dit de croissance sélective de grains. Ses conditions de déclenchement ont été déterminées, de manière à délimiter une fenêtre de forgeage critique. Les mécanismes microstructuraux à l’origine de ce phénomène ont été discutés, ainsi que la possibilité d’une solution préventive. / Polycrystalline Nickel-based alloys are widely used as components for rotative parts of jet engines submitted to extreme conditions. Endlessly increasing objectives in terms of energy efficiency have led the engine manufacturers to increase their service temperature. As a consequence, Inconel 718 and similar alloys -that were used until now- cannot withstand such severe conditions anymore, and lack mechanical resistance at the increased temperature. René 65 is a new γ-γ’ superalloy which has been designed specifically for that purpose by General Electric. It has been selected by Safran Aircraft Engines as the material for low-pressure turbine disks in the new LEAP engine. To reach the desired mechanical properties, a fine and homogeneous microstructure is required. The forging process is a complex sequence which involves various hot deformation stages and thermal treatments, during which the microstructure evolves. Although the underlying mechanisms governing the microstructure evolutions are quite known, their specific mechanism and kinetics may vary depending on the alloy.Interrupted compression tests were conducted at laboratory scale under thermomechanical conditions (temperature, strain and strain rate) in accordance with the industrial process. In the first part, the focus is placed on the dynamic recrystallization mechanisms. Accurate characterization of the deformed microstructures has enabled to highlight a new recrystallization mechanism which superimposes with more conventional ones. It was named heteroepitaxial recrystallization. The interactions between those mechanisms as well as their relative kinetics have been established in a wide range of deformation conditions. . It is demonstrated that this mechanism occurs in other γ-γ’ Nickel-based alloys. The second part of the study is dedicated to the stability of deformed microstructures when exposed to high temperature thermal treatments. René 65, as many other Nickel-based alloys, is subjected to the undesirable phenomenon of selective grain growth, which leads to very heterogeneous microstructures containing abnormally large grains in a fine matrix. Critical deformation conditions leading to heterogeneous microstructures during subsequent annealing have been determined in an aim to identify the critical forging window which should be avoided. The microstructural mechanisms responsible of this phenomenon have been investigated, and the possibility of a preventive solution is discussed.

Ce travail de thèse est consacré principalement à l’étude des relations entre la microstructure, le procédé de grenaillage et les champs de contraintes résiduelles dans le superalliage à base de nickel N18. Pour mettre en exergue le rôle de la microstructure, nous avons tout d’abord fabriqué quatre microstructures modèles de tailles de grains gamma et de précipités gamma' significativement différentes par différents chemins thermiques. Les échantillons ont été ensuite grenaillés par ultrason et enfin soit traités thermiquement ou sollicités en fatigue à chaud. Nous avons étudié les changements microstructuraux et mécaniques induits par chaque étape en s'appuyant sur différentes techniques de caractérisation (MEB, dureté, essais de traction et de fatigue). Nous montrons que la dureté et les propriétés en traction avant grenaillage ainsi que les modifications microstructurales et de dureté après grenaillage sont principalement dépendantes de la taille de précipités gamma'. Des mesures in situ de résistivité électrique ont permis de suivre les cinétiques de dissolution et de précipitation de la phase gamma' au cours de traitements thermiques. Les cinétiques ont été comparées à un modèle de précipitation développé pour l’alliage N18. Dans la suite, nous avons déterminé finement les contraintes résiduelles par diffraction des rayons X en laboratoire avec la méthode des « sin² psi » et au synchrotron avec la microdiffraction Laue couplée à des mesures d’énergies. La sensibilité de la microdiffraction a permis d’appréhender le rôle de la microstructure sur les champs de déformations et de contraintes à l’échelle du micromètre et de différencier la contribution des phases gamma et gamma', qui constitue l’une des principales difficultés de ce travail d’exploitation. Avant grenaillage, la déformation déviatorique est inférieure à 2 x 10-4 quelle que soit la taille de précipités gamma'. À l’issue du grenaillage, un décalage des profils de déformations et de contraintes de 100 µm est observé lorsque l'on compare la microstructure contenant de fins précipités gamma' (200 nm) à celle contenant des précipités gamma' grossiers (2000 nm). Les profils de contraintes obtenus avec la microdiffraction Laue montrent des différences significatives en comparaison à l’état de contraintes planes attendu à cœur de l’échantillon. Enfin, nous montrons qu’à l’issue d’un maintien isotherme ou d’un essai de fatigue interrompu, les déformations déviatoriques introduites par de grenaillage sont relaxées ou redistribuées / This thesis is mainly devoted to the study of the relation between microstructure, shot-peening process and residual stress fields in a N18 nickel-based superalloy. To highlight the effect of the microstructure, four simplified microstructures with significantly different gamma grain and gamma' precipitate sizes were designed using different heat treatments. Samples were then subjected to ultrasonic shot-peening and finally either to isothermal holding or to low-cycle fatigue test. Microstructural and mechanical modifications induced by each step were studied using different characterization techniques (SEM, hardness, tensile and fatigue tests). Hardness and tensile properties prior to shot-peening as well as microstructural and hardness modifications after shot-peening mainly depend on the gamma' precipitate size. In situ electrical resistivity measurements were used to follow gamma' dissolution and precipitation kinetics during heat treatments. The kinetics was compared to a model developed for the N18 alloy. Afterward, residual stresses were determined by conventional X-ray diffraction with the « sin² psi » method and synchrotron Laue microdiffraction coupled with energy measurements. The sensitivity of the microdiffraction technique allowed to understand the effect of the microstructure on strain and stress fields at the micrometer scale and to separate the contribution of gamma phase from that of gamma' phase, which is one of the major difficulties of this analysis. Prior to shot-peening, the deviatoric strain is less than 2 x 10-4 regardless of the gamma' precipitate size. After shot-peening, a shift of 100 µm on strain and stress profiles was observed between microstructures with fine gamma' precipitates (200 nm) and coarse gamma' precipitates (2000 nm). Stress profiles obtained with Laue microdiffraction method showed significant differences compared to the plane stress state expected in the sample. Finally, the deviatoric strains introduced by shot-peening are relaxed or redistributed after an isothermal holding or an interrupted fatigue test

This work deals with the issue of defects generation during the separation of the castings from a nickel-based superalloy, Inconel 738LC. The technology of investment casting is presented, followed by a description of metallurgy of superalloys, their physical and mechanical properties, as well as their technical applications. The machinability of superalloys and method of castings separation were also described as well as some of the casting defects that were reported to have impact on the generation of the defects after cutting. In the experimental part, the material microstructure and casting defects were analyzed. The experimental machining part consisted first of a comparative study of the friction sawing and plasma arc cutting technology at the standard operating conditions actually used in production. Second, an optimization study for the friction sawing was carried out, with a special focus on the suitability of an alternative cutoff wheel for the chosen application. Application of this wheel allows reducing the security distance between the cut and the part, thus reducing the production cost of the part.

Les turbines aéronautiques et terrestres utilisent comme matériaux de structure les superalliages à base nickel. Ils sont confrontés en utilisation à des environnements agressifs à très hautes températures, conduisant à l'usure et la corrosion, et à des sollicitations mécaniques qui entraînent fatigue et fluage. Pour permettre l'utilisation de ces matériaux dans des conditions toujours plus sévères de fonctionnement et augmenter la durée de vie des pièces, divers traitements de nitruration ont été proposés pour durcir la surface tout en conservant ou en améliorant la tenue mécanique et la résistance chimique. Les modifications induites par la nitruration, leur stabilité et l'influence de la microstructure initiale sont encore mal comprises dans ces matériaux complexes. Au cours de ces travaux, nous avons étudié les effets d'une nitruration assistée plasma en fonction de la microstructure et de la composition chimique des alliages. Différents types de superalliages à base nickel ont été choisis, de microstructures variées, comprenant éventuellement des précipités de type Ni3(Al,Ti,Nb) et/ou Ni3 (Nb). Nous avons alors caractérisé les modifications induites par l'introduction de l'azote dans les matériaux suite à un traitement de nitruration à basse température (400°C) : expansion de la maille, génération de contraintes résiduelles, comportement des précipités, formation de nitrures, plasticité, anisotropies... Les résultats obtenus suggèrent des effets différents selon la composition des précipités. Ces modifications structurales et leurs évolutions ont ensuite été étudiées lors d'un recuit à plus haute température (650°C) afin d'étudier la stabilité des couches formées. / Nickel-based superalloys are commonly used in pressurized water heat exchangers or in the hottest sections of aeroengines or industrial gas turbines, where they are subjected to high temperature and severe mechanical solicitations (fatigue, creep). To allow use of those materials in more and more difficult operating conditions and to improve their duration, different nitriding treatments have been proposed to harden the surface while maintaining or improving their mechanical strength and chemical resistance. However, modifications induced by nitriding, resulting stability in time and influences of the initial microstructure are still poorly understood in these complex materials. In this work, we investigated the behavior of plasma nitriding on superalloys according to their initial microstructure and chemical composition. Thus, different types of Nickel-based superalloys were selected with various microstructures, possibly including precipitates like Ni3(Al, Ti, Nb) and/or Ni3(Nb). Then, we have characterized the modifications induced by nitrogen introduction in the materials after nitriding treatment at low temperature (400°C): lattice expansion, generation of residual stress, precipitates behavior, nitrides formation, plasticity, anisotropy... The results suggest different behaviors depending on the composition of precipitates. Finally, these structural modifications and their evolutions have been studied during an annealing at higher temperature (650°C) in order to study the stability of the nitrided layers.

La prévision de la durée de vie des composants des centrales REP, en particulier les générateurs de vapeur, est cruciale. De nombreux travaux ont été menés pour comprendre les mécanismes de détérioration des composants par corrosion sous contrainte. Ces mécanismes restent mal connus. La couche d'oxyde doit jouer un rôle prépondérant. Une méthodologie, associant les techniques ToF-SIMS in situ et XPS, a été développée pour déterminer les cinétiques d'oxydation et comprendre les mécanismes de croissance des couches d'oxyde. La cinétique, la composition et la stratification des couches d'oxyde formées dans l'eau à haute température sur l'alliage 600 ont été comparées à des couches d'oxyde modèles formées in situ dans les bâtis XPS et ToF-SIMS en milieu gazeux à 300°C sous faible pression d'oxygène. On montre ainsi que l'oxydation en milieu gazeux à 300°C est un bon modèle pour simuler l'oxydation en milieu primaire. Une méthodologie originale a ensuite été mise au point à l'aide du ToF-SIMS pour déterminer les mécanismes de transport des espèces. Des échantillons préalablement oxydés en phase gazeuse ou dans l'eau à haute température ont été, dans une deuxième étape, réoxydés in situ dans le bâti ToF-SIMS à la même température, sous basse pression d'oxygène isotopique 18. Il apparait que la croissance de l'oxyde est localisée à l'interface métal/oxyde du fait de la diffusion des anions O2-, des phénomènes d'échange isotopique se produisant simultanément à l'oxydation. Le coefficient de diffusion de l'oxygène a pu être déterminé à l'aide d'un modèle approprié développé au cours de ce travail. / The lifetime prediction of pressurized water reactor (PWR) components, especially the steam generators (SG), is of high interest. Several works have been dedicated to the understanding of the stress corrosion cracking (SCC) mechanisms. However these mechanisms are still relatively poorly understood. The oxide layer should play an important role. A methodology, combining in situ ToF-SIMS and XPS techniques, has been developed to determine the oxidation kinetics and to understand the oxide layer growth mechanisms. Kinetics, composition and stratification of the oxide layers, formed in high temperature water on Alloy 600, were compared to model oxide layers formed in situ at 300°C under a low oxygen pressure. It shows that thermal oxidation under low oxygen pressure is a suitable model to simulate the oxidation in high temperature water. Finally, an original methodology based on ToF-SIMS has been developed to determine the transport mechanisms governing the oxide growth. Samples previously oxidized under a low oxygen pressure or in high temperature water, are, in a second step, re-oxidized in situ in the ToF-SIMS chamber at the same temperature under low oxygen isotope 18 pressure. It appears that the oxide growth is located at the metal/oxide interface due to the diffusion of O2- anions, isotopic exchange phenomena occuring simultaneously with oxidation. The oxygen diffusion coefficient was determined using an appropriate model developed in this work.

Indiana University-Purdue University Indianapolis (IUPUI) / 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. 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. 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. 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. 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. 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.

This diploma thesis is focusing on possibilities of influencing casting’s structure of nickel superalloy Inconel 713LC by force effects caused by vibration and rotation during crystallization. In this research were cast three test castings of turbine wheels with different solidification conditions that have affected the size and distribution of the grains. The aim was to compare the different microstructure and macrostructure of castings and then compare the dependence of grain refinement on mechanical properties. Changes in the structure were analyzed by means of light and electron microscopy methods after the fracture of test bars.

This project was ordered by Sandvik Materials Technology and was performed by a group of students at Uppsala university. The purpose of the project was to study precipitation behavior and structure stability in six advanced heat resistant alloys. Each sample were subjected to a creep rupture test in 600 or 700°C depending on the alloy type. Two parts of each alloy where examined; one part which had been affected by creep and another part which was unaffected by creep. A literature study was performed first to gain knowledge of the scientific theory utilized in this project, namely creep, precipitation hardening, and about the different materials which were analyzed. Preliminary results for the phase composition of the materials were obtained from a Thermo-Calc (TC) simulation. The SEM-images showed nothing noteworthy for any sample due to the roughness of the sample surfaces. The EDS-analysis showed chromium depletion in the centers of the aged samples of HT9 and Sanicro® 75X. Other minority phases such as Cr23C6 in Sanicro®70, P-phase and a titanium nitride phase in sanicro® 60X, VB in Esshete 1250 and Sigma-phase in 4C54 were identified using EDSmapping. It was found that when using XRD to analyze the phase compositions of small samples it is impractical to have the samples cast in bakelite beforehand. The XRD-results obtained in this project showed that more than 90% of the XRD diffractogram for every sample was graphite, which made the identification of minority phases impossible. The quality of the LOM-images varied greatly between samples, for 4C54 grain sizes were measured in all images, for Esshete 1250 grain sizes were measured for the crept sample, and for Sanicro® 60X measurements could only be taken from one image. Most of the sample preparation was insufficient to achieve the test results necessary for complete microstructural analysis and phase analysis of the samples. The mistakes in the practical steps of the project were noted and improvements for these mistakes are presented in the conclusion.

The present diploma thesis is focused on the effect of AlCr layer on the low cycle fatigue behaviour of cast polycrystalline superalloy IN713LC at 800°C. Protective layer is made by chemical vapour deposition followed by heat treatment. Fatigue tests were conducted in strain control mode with constant total strain amplitude and strain rate. The fatigue behaviour is assessed by cyclic hardening/softening curves, cyclic stress-strain curves, Manson-Coffin curves and Basquin curves. Microstructure was observed in as-received state and also after cyclic loading by means of optical microscopy and SEM.

No description available.