Le système barrière thermique, permettant la protection des aubes mobiles des turbines aéronautiques, est un système dont l'élaboration est complexe et nécessite de nombreuses étapes. L'utilisation du spark plasma sintering (SPS) a permis de réaliser des systèmes barrière thermique complets en une étape unique. Au-delà des possibilités industrielles de cette méthode, le SPS s'est avéré un outil de recherche précieux pour rapidement tester un vaste champ de compositions et d'ajouts d'éléments réactifs. Les premier essais et la modélisation de la diffusion dans le SPS ont permis de prévoir les phases du revêtement suite à l'étape de SPS. Les travaux se sont ensuite focalisés sur l'optimisation d'une composition de sous couche γ-γ' riche en platine dopée avec des éléments réactifs sur un substrat d'AM1. L'analyse chimique des revêtements SPS a révélé des taux de pollutions en soufre et carbone extrêmement faibles. Au vu de l'influence néfaste de ces éléments sur la tenue en oxydation cyclique ces analyses mettent en valeur la qualité des revêtements élaborés. Les performances des sous couches dopées, avec notamment du hafnium, de l'yttrium et du zirconium ont été évaluées lors d'essais de cyclage thermique à 1100°C sous air. La composition de revêtement γ-γ' la plus prometteuse a ensuite été comparée au système industriel β-(NiPt)Al avec la même barrière thermique de zircone yttriée déposée par EBPVD et le même substrat d'AM1. Les résultats obtenus montre une meilleure durée de vie des systèmes TBC avec sous couches γ-γ'. Par contre la remontée importante des éléments du superalliage dans le revêtement influence la durée de vie du système TBC comme cela a été montré par des dépôts conduits sur d'autres nuances de superalliages à base de nickel. Ces résultats montrent que pour les revêtements γ-γ' la prise en compte du revêtement dans le développement d'un superalliage est essentielle. / To protect turbines blades from excessive oxidation and to lower the temperature at the blade surface, a multilayer coating system has been developed in the past, i.e. the thermal barrier coating. The fabrication of TBC is expensive and demands numerous process steps. In this study, bond coatings have been fabricated by spark plasma sintering in a single step. This fast fabrication process permits to test a large range of bond coating compositions with different reactive elements such as Zr, Y and Hf on AM1 nickel base superalloy. From the first results, the data related to the diffusion during the SPS were calculated to predict the coating phases. Impurities levels were measured after SPS fabrication. Sulphur and carbon concentration were very low. These results highlight the great quality of coating made by spark plasma sintering, more particularly with a top coat also made by SPS. Then, a composition of γ-γ’ coating has been optimized for high life span during thermal cycling. The thermal cycling at 1100°C of TBC system with this optimized γ-γ’ bond coatings give better life span than the conventional system with β-(Ni,Pt)Al phase bond coating. After long thermal cycling, >1000*1h cycles, chemical elements from the substrate can diffuse in the thermally grown oxide, leading to its delamination. Thus, for increasing the life span of the whole system the bond coating has to be considered during the superalloy development.

L'alliage N19 est un superalliage base nickel, élaboré par métallurgie des poudres, qui a été développé récemment en vue d'une application pour disques de turbine aéronautique. L'objectif de cette étude est d'optimiser la microstructure de cet alliage en agissant sur les paramètres de traitements thermiques pour améliorer les propriétés mécaniques de l'alliage. Une bonne compréhension des relations entre les paramètres de traitements thermiques et la microstructure, d'une part, et, des relations entre la microstructure et les propriétés mécaniques, d'autre part, est donc nécessaire. De nombreux traitements thermiques ont été appliqués à l'alliage N19 pour évaluer l'effet de la température de mise en solution, des conditions de refroidissement et de la température de revenu sur la taille de grains, et sur la taille et la distribution des précipités gamma prime. L'observation des microstructures en microscopie électronique à balayage et en transmission a permis d'évaluer l'effet des différentes étapes du traitement thermique sur les caractéristiques microstructurales de l'alliage. L'effet de ces modifications microstructurales sur la vitesse de propagation de fissure en fatigue-fluage à 650°C a été étudié. Les résultats de ces essais de propagation de fissure en fatigue-fluage ont été analysés à l'aide d'essais de comportement en fatigue-relaxation. Une synthèse des différentes propriétés mécaniques de l'alliage en fonction des paramètres de traitements thermiques et des caractéristiques microstructurales a été proposée. / The N19 alloy is a powder metallurgy nickel-based superalloy which has recently been developed for aircraft engine turbine disks. The aim of this study is to optimize the N19 microstructure through the adjustment of the heat treatment parameters in order to enhance the mechanical properties of this alloy. A good understanding of the relationships between the heat treatment parameters and the microstructure, and between the microstructure and the mechanical properties is required. Numerous heat treatments were applied to the alloy to investigate the effect of the solutionizing temperature, the cooling path, and the ageing temperature on the grain size, and on the gamma prime precipitates size and distribution. The observation of the microstructures using scanning electron microscopy and transmission electron microscopy supports the analysis of the heat treatment parameters effects on the microstructural features of the alloy. The effect of the microstructural modifications on the creep fatigue crack growth rate at 650°C was studied. The results of the creep fatigue crack growth tests were analyzed using cyclic stress-relaxation tests. A synthesis of the various mechanical properties of the alloy according to the heat treatment parameters and microstructural features is proposed.

Lors de la phase de certification d’un turbomoteur, le motoriste doit démontrer que la perte d’une pale de rotor ne conduit pas au "Knocking-Off", c’est à dire à la rupture en cascade des pales suiveuses. Cette démonstration est faite en général par un essai au banc coûteux car partiellement destructif. Grâce à l’amélioration des moyens de calcul, il devient possible de simuler la réponse transitoire de la structure soumise à ce type de chargement très complexe. En tant que point d’entrée sur la simulation, la connaissance du comportement des matériaux est primordiale. Or, peu d’études sont publiées sur le comportement dynamique des superalliages à base nickel monocristallins et, de surcroît, à des températures élevées de l’ordre de 1000°C. Pour prédire efficacement les conséquences d’impacts sur des pales de turbines, des travaux expérimentaux et numériques ont été réalisés sur un monocristal couramment utilisé par Turbomeca. Des essais de compression dynamique à haute température sur barres de Hopkinson permettent d’estimer le seuil de plasticité et l’écrouissage du matériau en fonction de l’orientation du cristal, de la vitesse de déformation et de la température. Les paramètres d’une loi visco-plastique anisotrope sont identifiés pour modéliser efficacement le comportement macroscopique du MC2 sous des chargements intenses et fortement multi-axiaux. Une campagne d’essais balistiques au banc de Safran Snecma a été réalisée sur des plaques et des pales monocristallines à hautes températures. Afin de prendre en compte la fragmentation des profils dans les calculs de perte de pale, un critère en déformation plastique dépendante du taux de triaxialité des contraintes est calibré puis validé par confrontation aux essais de tirs sur plaques. Des mesures de stéréo-corrélation postmortem et des enregistrements à la caméra rapide permettent de valider les simulations. Une pratique de modélisation de la perte d’une pale avec l’outil LS-Dyna a été établie et appliquée à un cas industriel de perte de pale en service. Enfin, en vue de justifier le découplage temporel entre les dommages primaires, liés aux impacts directs sur les premières pales suiveuses, et secondaires, liés aux effets de l’excentration, une approche de dynamique d’ensemble de ligne d’arbre a été développée puis validée. / During the certification process of a turbo engine, the engine manufacturer has to demonstrate that the loss of a rotor blade does not lead to the "knocking-off" phenomenon, in other words to the cascading failure of the successive blades. Generally, this demonstration is carried out through a costly rig test driving to the partial destruction of the engine. Thanks to the improvement of computational resources, it is now possible to simulate the transient response of the structure subjected to this complex loading. The knowledge of material behavior turns out to be the essential starting point for the simulation. However, only a few studies have been published on the dynamic behavior of nickel-based single crystal superalloys at high temperature reaching 1000°C. With a view to efficiently predicting the consequences of impacts on turbine blades, experimental and numerical works have been conducted on a single crystal frequently used by Turbomeca. High-temperature dynamic compressive tests on Split Hopkinson Pressure Bars (SHPB) have enabled to estimate the material plasticity level and hardening, depending on the crystal orientation, strain rate and temperature. The parameters of a viscoplastic anisotropic law have been identified to effectively model the MC2 macroscopic behavior under highly intense and multiaxial loading. At Safran Snecma Villaroche, ballistic tests have been undertaken on both single crystal plates and blades under high temperatures. In order to consider the fragmentation of profiles in blade-off simulations, a plastic strain criterion depending on stress triaxiality has been calibrated and validated by comparison with the impacts on blades. Post-mortem digital images correlation measurements and high-speed camera recordings have confirmed these simulations. Using LS-Dyna solver, a blade-off modeling strategy has been created and applied to an actual blade-off industrial case. Finally, a rotordynamics approach has been developed and validated with the aim of separately analyzing the primary damage, caused by direct impacts on the first following blades, and the secondary damage due to the effects of unbalance on a flexible rotor.

Yttria-stabilized zirconia-based thermal barrier coating systems are the most widely used commercial coatings in the industry, with practical applications in aircraft engines and land-based power turbines. The purpose of thermal barriers is primarily to protect the substrate from high temperatures and also to increase its oxidation resistance. Currently, concerning the relatively frequent volcanic eruptions and increasing air traffic intensity in desert areas, increased attention is being paid to the development of new thermal and environmental coatings that will withstand the so-called CMAS attack and still successfully meeting the strictest requirements of the aerospace industry. Two newly developed experimental coatings consisting of three successive layers have been developed for this work. The upper two layers are thermal insulating ceramic coatings, where two different uppermost coatings were deposited. The first uppermost layer of the coating is a mixture of mullite and hexacelsian in a ratio of 70/30 wt. %. The second upper most type of coating consists of Al6Si2O13 + MgAl2O4 + BaCO3 in a ratio of 6:3:1 wt. %. The interlayer is made of the commercially utilized yttria-stabilized zirconia. The metallic CoNiCrAlY coating, which is directly deposited on the nickel-based superalloy MAR-M247, fulfils a compensatory function between the mechanical properties of the nickel superalloy and the ceramic coating. The thermal and environmental barrier system was deposited using air plasma spraying (APS) technology. The main objective of this work was to evaluate the effect of the newly developed thermal and environmental barrier coating, which has a high potential for the protection of component surfaces in an aggressive environment, on isothermical and thermomechanical fatigue behaviour of nickel-based superalloy MAR-M247. Low cycle fatigue tests were performed in strain control mode with constant strain amplitude on both uncoated and TEBC coated superalloy. Fatigue hardening/softening curves, cyclic stress-strain curves and fatigue life curves in the representation of total strain amplitude, plastic strain amplitude and stress amplitude on the number of cycles to failure were obtained. Microstructural analysis of MAR-M247 superalloy and a newly developed experimental coating was performed in a scanning electron microscope. The fatigue crack initiation sites were identified and the process of fatigue crack propagation was described. The dislocation arrangement after fatigue loading of MAR-M247 was investigated in a transmission electron microscope. The findings of isothermical and thermomechanical low cycle fatigue behaviour of uncoated and TEBC coated MAR-M247 superalloy and identification of damage mechanisms presented in this dissertation will improve the estimation of safe-life that is particularly relevant to aircraft engines components.

Multiple step tests under cyclic strain control have been performed using cylindrical specimens of cast polycrystalline Inconel 738LC superalloy at 23, 700, 500, 800 and 900 °C in laboratory atmosphere to obtain cyclic stress-strain curves. During cyclic straining of specimen were obtained cyclic hardening-softening curves. Their progress changed with temperature and strain amplitude. Evaluated cyclic stress-strain curves are shifted to lower stresses with increasing temperature. Surface relief was observed in fatigued specimens under SEM and metalography under optic microscopy. Slip markings were studied on specimen surface fatigued at 700 °C .Stress-strain response is compared and discussed in relation to the surface observations - persistent slip markings.

No description available.

Alloy 617 displays a ductility dip during straining at exactly 1000˚C, leading to brittle fracture. A sudden decrease in ductility appearing during Gleeble hot ductility tests of Ni-based superalloys is a well-known phenomenon, while its cause is unknown. Many mechanisms have been established as possible contributors to the issue, and in later years not one, but the simultaneous presence of several of these mechanisms were confirmed as the cause. The ductility dip leads to solid state cracking and a specific solid state cracking phenomenon known as ductility dip cracking is specifically common in Ni-based superalloys. Ductility dip cracking is identified by intergranular cracks and the occurrence of specific precipitates, among other things. This work investigates the possibility that the decreased ductility is due to ductility dip cracking. Furthermore, other possible explanations are investigated. Visual examination was conducted through LOM, SEM and chemical analysis using EDS technique. Combined with thermodynamic calculations, the existence of Cr-rich M23C6 carbides, Ti(N,C) and Mo-rich particles, most likely M3B2, were confirmed. Further, it is established that the ductility dip is related to the lack of dynamic recrystallization at 1000˚C. It is not confirmed that the ductility dip in alloy 617 is due to ductility dip cracking. / Nickelbaslegeringen 617 uppvisar en minskning i duktilitet under Gleeble-dragprovning vid exakt 1000˚C vilket leder till sprött brott. En plötslig sänkning av duktiliteten vid varmdragning av Ni-baserade superlegeringar är ett välkänt fenomen, dock är orsaken inte fastställd. Många mekanismer har bekräftats som bidrag till problemet och under de senaste åren har den simultana närvaron av fler av dessa mekanismer bekräftats som orsaken. Sänkningen i duktilitet leder till sprickbildning i fast fas och en specifik typ av sprickbildning känd som ”ductility dip cracking” är speciellt förekommande i Ni-bas legeringar. Denna identifieras bland annat genom intergranulära sprickor och närvaron av specifika utskiljningar. Detta arbete undersöker möjligheten att duktilitetssänkningen beror på  ”ductility dip cracking”. Dessutom undersöks fler tänkbara förklaringar. Visuell granskning genomfördes via LOM och SEM och analys av sammansättningar via EDS-analys. I kombination med termodynamiska simuleringar blev förekomsten av Cr-rika M23C6 karbider, Ti(N,C) och Mo-rika partiklar, troligtvis M3B2, bekräftad. Fortsatt är det bekräftat att duktilitetssänkningen är relaterat till avsaknaden av rekristallisation vid 1000˚C. Det är inte bekräftat i detta arbete att duktilitetssänkningen i legering 617 beror av ”ductility dip cracking”.

No description available.

L’alliage L-605 est un superalliage base cobalt combinant une haute résistance et une bonne ductilité, de plus il est biocompatible et présente une bonne résistance a la corrosion. Dû a son inertie chimique dans le corps humain, ce matériau a été utilise avec succès pour fabriquer des valves cardiaques et des stents. Le contrôle de la microstructure peut influencer grandement les propriétés mécaniques : notamment un raffinement des grains est susceptible d’augmenter d’avantage la résistance et serait intéressant pour permettre de fabriquer des stents selon une architecture plus fine. L’ajustement de la distribution de taille de grains à travers le phénomène de recristallisation lors de la déformation à chaud apparait comme une solution pratique pour ajuster les propriétés mécaniques du matériau. Pour contrôler la microstructure et choisir les conditions de procédé optimales, les mécanismes mis en jeu lors de la recristallisation dynamique et l’effet des conditions de déformation sur la taille de grain doivent être compris et prévisibles par des outils théorique. Les propriétés mécaniques du matériau à haute température sont déterminées par des essais de compression à chaud. L’évolution microstructurale du matériau lors de la compression est analysée par microscopie optique et électronique (EBSD, TEM). Le phénomène de recristallisation dynamique continue est mis en évidence, et procède par nucléation de nouveaux grains aux joints de grain. La corrélation entre le comportement mécanique à chaud et l’évolution microstructurale est déterminée expérimentalement. Les conditions optimales de déformation impliquant la recristallisation dynamique sont déterminées, et la microstructure résultante est étudiée en détail. De nouveaux outils théoriques permettant de prévoir les conditions de recristallisation et d’extraire les paramètres physiques du matériau a partir des données expérimentales sont proposés. Enfin, la recristallisation dynamique est modélisée analytiquement, et permet de prédire le comportement mécanique et l’évolution de la taille de grain lors de la déformation. / 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.

The present dissertation reports the findings of a study of cracking behavior of a newly developed superalloy, Allvac 718Plus during high power beam welding and post-weld heat treatment. Microstructures of the base alloy, heat affected zone (HAZ) and fusion zone (FZ) of welded and post-weld heat treated (PWHT) coupons were examined by the use of standard metallographic techniques involving optical microscopy, analytical scanning electron microscopy (SEM) and analytical transmission electron microscopy. Moreover, grain boundary segregation behavior of boron atoms during pre-weld heat treatments was evaluated using secondary ion mass spectroscopic system. In the first phase of the research, 718Plus was welded using a low and high heat input CO2 laser to assess its weld cracking response. Detailed examination of the welds by analytical electron microscopic technique revealed the occurrence of cracking in the HAZ of low heat input welds, while their FZ was crack free. However, both the FZ and HAZ of high heat input welds were crack-free. Resolidified constituents were observed along the cracked grain boundaries of the lower heat input welds, which indicated that HAZ cracking in this newly developed superalloy was associated with grain boundary liquation. However, despite a more extensive liquation of grain boundaries and grain interior in the HAZ of high heat input welds, no cracking occurred. This was attributed to the combination of lower welding stresses generated during cooling, and relaxation of these stresses by thick intergranular liquid. Although HAZ cracking was prevented by welding with a high heat input laser, it resulted in a significant damage to the parent microstructure through its extensive liquation. Thus, the use of low heat input welding is desirable. However, this resulted in HAZ cracking which needs to be minimized or eliminated. Therefore, during the second phase of this research, the effects of pre-weld thermal processing on the cracking response of 718Plus were investigated. Results from the quantification of the cracking of the alloy showed that HAZ cracking may be significantly reduced or eliminated through an adequate selection of pre-weld thermal cycle. In the third stage of this research, crack-free welds of 718Plus were post-weld heat treated using standard thermal schedules. A significant solid state cracking of the alloy occurred during the PWHT. The cracking was attributed to the presence of embrittling phases on HAZ grain boundaries, coupled with aging contraction stresses that are generated by a considerable precipitation of gamma prime phase during aging.