As recentes descobertas de reservas de petróleo no pré-sal, representam uma grande oportunidade e desafio para a Petrobrás e demais indústrias de exploração e extração do petróleo. As exigências quanto aos materiais mais resistentes à corrosão e que conciliam boa resistência mecânica são cada vez maiores, devido aos constantes esforços dinâmicos que os equipamentos estarão sujeitos, pois os componentes estruturais serão submetidos à grande lâmina de água, ocorrência que as companhias exploradoras terão que superar. A otimização de materiais e equipamentos que podem melhorar a performance nas explorações do pré-sal tem sido a grande busca do setor nos últimos anos, muitos deles precisam ser testados e atestados quanto sua resistência à propagação de trincas, uma vez que, serão submetidos a oscilações devido as movimentações das marés e as condições de alta severidade a que serão expostos. Para suportar as condições de exposições com H2S, resistência a corrosão por pitting e resistência mecânica, porcas e parafusos têm sido fabricados com o Inconel 625, essas peças são estruturais e de extrema importância para a prospecção do petróleo. Após todas as etapas de fabricação, conformação, tratamento térmico e laminação a frio, o material foi caracterizado, realizou-se ensaio de metalografia que apresentou tamanhos de grão 7 e 8 conforme norma ASTM E112. Uma das premissas para a realização desse trabalho está nas condições que o material será exposto em situações acidentais, conforme informações da própria Petrobrás, em caso de vazamentos, os do tipo estruturais podem ser submetidos a temperaturas criogênicas de -100°C, -120°C e até -190°C devido ao vazamento de gases. Assim, o material foi caracterizado em temperaturas criogênicas através dos ensaios de tração, impacto e de CTOD. No ensaio de tração foi observado para as diferentes temperaturas criogênicas que apesar do aumento na resistência do material, da ordem de 787 MPa, o Inconel 625 manteve um alongamento acima de 40%. Nos resultados de Impacto a tenacidade se manteve acima de 200 J e não foi notada a curva de transição dúctil-frágil, mesmo para temperaturas tão baixas. No ensaio de CTOD utilizou-se corpos de prova de flexão (SENB) no ensaio de tenacidade à fratura, de acordo com a norma ASTM E1290.A componente plástica da abertura da boca do entalhe na temperatura de -190°C, pior caso, se manteve em 1,52 mm em média. Mediante a todos os resultados obtidos, pode-se afirmar que o aumento da resistência do Inconel 625 pelo processo de encruamento, não impossibilita sua aplicação para temperaturas criogênicas, mantendo sua capacidade de se deformar apreciavelmente antes de se romper. / Recently oil and gas discoveries in the Pre-Salt layer represent a huge exploration potential in Brazil, however, the technological challenges for the exploitation of these mineral resources are immense and therefore have motivated the development of studies looking for efficient methods and materials for their productions. The requirements about materials more corrosion resistance and mechanical resistance have been more frequently, as a result of high deep layer to explore the petroleum. The materials and equipment optimization to improve the performance in the pre-salt exploration have been the big search for oil and gas companies in the last years, but this materials must be testing in the crack propagation, because, this materials must resistance by oscillations, as consequence of ocean movements and others difficult situations that the materials must be support. To support H2S conditions, corrosion resistance by pitting corrosion and high mechanical resistance, bolts and nuts have been manufactured with Inconel 625, these products are structural and they are extreme importance to petroleum exploration. After all manufacturing operations, hot worked heat treatment and cold worked, the material was studied, and it was realized micrographic testing that result in grain size 7 and 8, in accordance ASTM E112 standard. One of premise to realized this paper are in the conditions that the material will be supported in accident situations, in agreement of Petrobras information, in the gases scape accidents, the structure materials can be exposed in cryogenically temperatures of -100°C, -120°C until -190°C. Therefore, the material was studied in cryogenically temperatures throw tensile testing, impact testing and CTOD. In the tensile testing was noted to different kind of cryogenically temperatures, same with more mechanical resistance, 787 MPa yield strength, the Inconel 625 has kept the 40% elongation. In the impact testing the notch toughness as kept above 200 J and it was not seen the transition ductile-Brittle in the low temperatures. In the CTOD testing was used bending test specimens (SENB) in the fracture toughness test for the Inconel 625, in agreement with the ASTM E1290 standard. The specimens was testing in tension and CTOD test in low temperatures: -100°C, -120°C and -190°C.The Clip gage displacement was recorded in the -190°C temperature with 1,52 mm average, this is the worse situation. Analyzing all the results, can be considered that the growth mechanical resistance of Inconel 625 by cold worked process, allow your application with cryogenically situations and the material has kept your ability to be well deformed before the crack.

As recentes descobertas de reservas de petróleo no pré-sal, representam uma grande oportunidade e desafio para a Petrobrás e demais indústrias de exploração e extração do petróleo. As exigências quanto aos materiais mais resistentes à corrosão e que conciliam boa resistência mecânica são cada vez maiores, devido aos constantes esforços dinâmicos que os equipamentos estarão sujeitos, pois os componentes estruturais serão submetidos à grande lâmina de água, ocorrência que as companhias exploradoras terão que superar. A otimização de materiais e equipamentos que podem melhorar a performance nas explorações do pré-sal tem sido a grande busca do setor nos últimos anos, muitos deles precisam ser testados e atestados quanto sua resistência à propagação de trincas, uma vez que, serão submetidos a oscilações devido as movimentações das marés e as condições de alta severidade a que serão expostos. Para suportar as condições de exposições com H2S, resistência a corrosão por pitting e resistência mecânica, porcas e parafusos têm sido fabricados com o Inconel 625, essas peças são estruturais e de extrema importância para a prospecção do petróleo. Após todas as etapas de fabricação, conformação, tratamento térmico e laminação a frio, o material foi caracterizado, realizou-se ensaio de metalografia que apresentou tamanhos de grão 7 e 8 conforme norma ASTM E112. Uma das premissas para a realização desse trabalho está nas condições que o material será exposto em situações acidentais, conforme informações da própria Petrobrás, em caso de vazamentos, os do tipo estruturais podem ser submetidos a temperaturas criogênicas de -100°C, -120°C e até -190°C devido ao vazamento de gases. Assim, o material foi caracterizado em temperaturas criogênicas através dos ensaios de tração, impacto e de CTOD. No ensaio de tração foi observado para as diferentes temperaturas criogênicas que apesar do aumento na resistência do material, da ordem de 787 MPa, o Inconel 625 manteve um alongamento acima de 40%. Nos resultados de Impacto a tenacidade se manteve acima de 200 J e não foi notada a curva de transição dúctil-frágil, mesmo para temperaturas tão baixas. No ensaio de CTOD utilizou-se corpos de prova de flexão (SENB) no ensaio de tenacidade à fratura, de acordo com a norma ASTM E1290.A componente plástica da abertura da boca do entalhe na temperatura de -190°C, pior caso, se manteve em 1,52 mm em média. Mediante a todos os resultados obtidos, pode-se afirmar que o aumento da resistência do Inconel 625 pelo processo de encruamento, não impossibilita sua aplicação para temperaturas criogênicas, mantendo sua capacidade de se deformar apreciavelmente antes de se romper. / Recently oil and gas discoveries in the Pre-Salt layer represent a huge exploration potential in Brazil, however, the technological challenges for the exploitation of these mineral resources are immense and therefore have motivated the development of studies looking for efficient methods and materials for their productions. The requirements about materials more corrosion resistance and mechanical resistance have been more frequently, as a result of high deep layer to explore the petroleum. The materials and equipment optimization to improve the performance in the pre-salt exploration have been the big search for oil and gas companies in the last years, but this materials must be testing in the crack propagation, because, this materials must resistance by oscillations, as consequence of ocean movements and others difficult situations that the materials must be support. To support H2S conditions, corrosion resistance by pitting corrosion and high mechanical resistance, bolts and nuts have been manufactured with Inconel 625, these products are structural and they are extreme importance to petroleum exploration. After all manufacturing operations, hot worked heat treatment and cold worked, the material was studied, and it was realized micrographic testing that result in grain size 7 and 8, in accordance ASTM E112 standard. One of premise to realized this paper are in the conditions that the material will be supported in accident situations, in agreement of Petrobras information, in the gases scape accidents, the structure materials can be exposed in cryogenically temperatures of -100°C, -120°C until -190°C. Therefore, the material was studied in cryogenically temperatures throw tensile testing, impact testing and CTOD. In the tensile testing was noted to different kind of cryogenically temperatures, same with more mechanical resistance, 787 MPa yield strength, the Inconel 625 has kept the 40% elongation. In the impact testing the notch toughness as kept above 200 J and it was not seen the transition ductile-Brittle in the low temperatures. In the CTOD testing was used bending test specimens (SENB) in the fracture toughness test for the Inconel 625, in agreement with the ASTM E1290 standard. The specimens was testing in tension and CTOD test in low temperatures: -100°C, -120°C and -190°C.The Clip gage displacement was recorded in the -190°C temperature with 1,52 mm average, this is the worse situation. Analyzing all the results, can be considered that the growth mechanical resistance of Inconel 625 by cold worked process, allow your application with cryogenically situations and the material has kept your ability to be well deformed before the crack.

The aim of this thesis was to investigate if the robotized welding method FSW (Friction Stir Welding) could be applied for joining a rotating structure in an aero engine at Volvo Aero Corporation. FSW is expected to introduce less defects than today’s welding methods and could therefore be suitable for critical aero components. The material is the nickel based alloy Inconel 718, however a material experimentation is outside the scope of this report.The main goal of this study is to verify if the ESAB ROSIO robot based FSW-system has a suitable work space to be able to weld the rotating structure, and if the welding tool has accessibility to the joints. The FSW-process needs a rigid fixture, and a number of fix-ture concepts are presented based on a proposed weld sequence. A final fixture design is proposed, which requires a new design of the structure.The accessibility studies were performed in the robot simulations software Robot Stu-dio. This showed that the robot was unable to weld the proposed model in all areas in the original design. If the robot and the rotating structure can be redesigned the access will be achieved as shown in Robot Studio simulations.In order to be implemented in real production a number of further actions need to be taken and the result of this study can be a basis for these.

L'optimisation de la durée de vie des disques de turbines conçus en superalliage à base de nickel, tel que l'Inconel 718 DA, constitue une vraie problématique industrielle. En effet, lors d'essais de fatigue oligocyclique à chaud sur des éprouvettes prélevées sur ces disques, il a été constaté que la durée de vie dépendait de la zone de prélèvement testée. Cette dispersion inattendue des résultats s'avère être un facteur très important d'un point de vue industriel car le dimensionnement des pièces étant conservatif, il est établi à partir des valeurs de durée de vie les plus faibles ce qui conduit à une pénalisation forte en termes de performance du point de vue de la conception. Le but de cette étude est donc d'expliciter la relation entre les paramètres de forgeage, les propriétés microstructurales et donc les durées de vie afin de proposer des pistes pour réduire la dispersion des résultats de fatigue pour optimiser ainsi le dimensionnement des structures. Dans un premier temps, l'étude de l'effet des paramètres de forgeage a été réalisée grâce au logiciel Forge2®. Cette étape a permis de mettre en évidence les paramètres de forgeage influant sur la microstructure et de définir des gammes de forgeage sur des lopins expérimentaux. Les mécanismes d'initiation et les modes d'endommagement ont été identifiés pour chaque microstructure de l'alliage. Il s'avère que, dans le cas des matériaux testés, deux mécanismes d'amorçage sont observés : un amorçage sur particule interne avec formation de « fish-eye » et un amorçage sur grain sub-surfacique. Une corrélation directe avec la microstructure et le domaine de durée de vie a pu être établie. L'effet du rapport entre la queue de distribution de taille de grains et la taille des particules a pu être mis en évidence, ainsi que la nocivité de la présence de joints Σ3 dans des gros grains. / Optimization of turbine discs in superalloy Nickel based durability is a real industrial challenge. The different regions of a wrought Inconel 718 DA superalloy turbine disk may present a wide range of behavior in fatigue life due to the variability of the microstructure. To improve the fatigue dimensioning, it is necessary to understand the relation between the forging parameters, the microstructure and the fatigue behavior. Firstly, the effect of the forging parameters on the microstructure was realized thanks to simulation calculation via Forge2® and experimental forging were realized. Secondly, fatigue tests under strain control conditions were performed at 450°C for all microstructures. Initiation mechanisms and fracture behavior are identified for each microstructure of this superalloy. Grain size and phases distributions were characterized in the specimens and related to fatigue failure initiation modes. The 3D distribution of the Titanium nitrides was also investigated using synchrotron laminography both in terms of size and spatial distribution. Fatigue crack initiation was seen to occur on large grains in stage I for the larger grain material whereas for the material with slightly smaller grains initiation from internal nitrides caused failure via so-called fish-eye cracks. A relation between the microstructure heterogeneities and the durability is established. Indeed, the initiation mechanism, which depends on the grain size distribution compare to the particles size, impacts the durability. The presence of Σ3 boundaries in large grains proves to be harmful.

This thesis aims to investigate the manufacturability of nickel-based superalloys, IN625 and IN718, using the laser powder bed fusion (LPBF) process. The study provides a better understanding of the process-structure-property of nickel-based superalloys, their fatigue life, and subsequent post-processing. First, the process-structure-property was investigated by selecting a wide range of process parameters to print coupons for IN625 and IN718. Next, a subset of process parameters was defined that would produce high relative density (>99%), low surface roughness (~2 μm), and a low tensile RS. Second, a multi-scale finite element model was constructed to predict the temperature gradients, cooling rates, and their effect on RS. At constant energy density, RS is affected by scan speed, laser power, and hatch spacing, respectively. Third, the optimum set of parameters was used to manufacture and test as-built and shot-peened samples to investigate the fatigue life without costly heat treatment processes. It was found that shot peening resulted in a fatigue life comparable to wrought heat-treated unnotched specimen. Additionally, IN625 had a better fatigue life compared to IN718 due to higher dislocations density as well as the absence of γ´ and γ´´ in IN718 due to the rapid cooling in LPBF. Finally, the effect of post-processing on dimensional accuracy and surface integrity was investigated. A new approach using low-frequency vibration-assisted drilling (VAD) proved feasible by enhancing the as-built hole accuracy while inducing compressive in-depth RS compared to laser peening, which only affects the RS. These favorable findings contributed to the scientific knowledge of LPBF of nickel-based superalloys by determining the process parameters optimum window and reducing the post-processes to obtain a high fatigue life, a better dimensional accuracy, and improved surface integrity. / Thesis / Doctor of Philosophy (PhD)

Ces travaux de thèse concernent l’étude du comportement thermo-physique de mélanges de polymères biosourcés chargés de poudre d’Inconel 718 mis en forme par Moulage par Injection de poudre Métallique. Des matériaux et procédés innovants pouvant permettre une amélioration du procédé ont été étudiés. L’utilisation de polyéthylène glycol (PEG), choisi pour ses propriétés de solubilité dans l’eau, et de polymères biosourcés, pour diminuer l’impact environnemental, ont été choisi. Les nuances de polymères biosourcés ont été choisies adaptées aux conditions du procédé de moulage par injection, il s’agit d’acide polylactique et de polyhydroalcanoates. De même, l’utilisation du CO2 à l’état supercritique comme solvant, a pour objectif de diminuer le temps de déliantage ainsi que d’augmenter la qualité des composants réalisés. Les résultats obtenus ont montré une dégradation du PEG et de l’acide stéarique lors des cycles de mélangeage de de moulage par injection dans les conditions d’utilisation des polymères biosourcés. L’utilisation des mélanges chargés composés de polymères biosourcés ont permis d’améliorer l’homogénéité des composants injectés, mais ont engendré des défauts lors de l’étape de déliantage. Ces défauts ont pu être éliminés par l’utilisation de CO2 à l’état supercritique comme solvant du PEG. Ce dernier procédé a permis une diminution importante du temps de déliantage ainsi qu’une amélioration de la qualité des composants finaux. Les composants densifiés possèdent les propriétés mécaniques correspondantes à l’Inconel 718. / The works done during this PhD focuses on the study of the thermo-physical behavior of bio sourced polymer blends loaded with Inconel 718 powder (feedstock) to be shaped by the Metal Injection Molding process (MIM). First, a review of the researches related to the MIM process was conducted to identify innovative materials and processes that can improve the MIM process. Thus, the use of polyethylene glycol (PEG), selected for its properties of solubility in water, and bio sourced polymers, in order to reduce the environmental impact, were selected. The bio sourced polymers have been selected in accordance with the conditions of the injection molding process, and the choice was made to use polylactic acid (PLA) and polyhydroalkanoates (PHA and PHBV). Similarly, the supercritical CO2 as solvent was chosen to reduce the time of binder removal as well as increasing the quality of components produced. Thermo-physical, mechanical and rheological characterizations were made to determine the behavior of the different feedstock formulations. The results showed a degradation of the PEG and of the stearic acid under the conditions of use of the biopolymers, during the mixing and the injection stages. The use of feedstock made of bio sourced polymers have improved the homogeneity of the injected components, but they have generated defects during the debinding step. These defects have been eliminated by the use of CO2 in the supercritical state as solvent of the PEG. This method has significantly decrease the time of binder removal and improved the quality of the final components. Finally, densified components have the mechanical properties corresponding to Inconel 718.

As recentes descobertas de petróleo e gás na camada do Pré-sal representam um enorme potencial exploratório no Brasil, entretanto, os desafios tecnológicos para a exploração desses recursos minerais são imensos e, consequentemente, têm motivado o desenvolvimento de estudos voltados a métodos e materiais eficientes para suas produções. Os tubos condutores de petróleo e gás são denominados de elevadores catenários ou do inglês \"risers\", e são elementos que necessariamente são soldados e possuem fundamental importância nessa cadeia produtiva, pois transportam petróleo e gás natural do fundo do mar à plataforma, estando sujeitos a carregamentos dinâmicos (fadiga) durante sua operação. Adicionalmente, um dos problemas centrais à produção de óleo e gás das reservas do Pré-Sal está diretamente associado a meios altamente corrosivos, tais como H2S e CO2. Uma forma mais barata de proteção dos tubos é a aplicação de uma camada de um material metálico resistente à corrosão na parte interna desses tubos (clad). Assim, a união entre esses tubos para formação dos \"risers\" deve ser realizada pelo emprego de soldas circunferenciais de ligas igualmente resistentes à corrosão. Nesse contexto, como os elementos soldados são considerados possuir defeitos do tipo trinca, para a garantia de sua integridade estrutural quando submetidos a carregamentos cíclicos, é necessário o conhecimento das taxas de propagação de trinca por fadiga da solda circunferencial. Assim, neste trabalho, foram realizados ensaios de propagação de trinca por fadiga na região da solda circunferencial de Inconel® 625 realizada em tubo de aço API 5L X65 cladeado, utilizando corpos de prova do tipo SEN(B) (Single Edge Notch Bending) com relações entre espessura e largura (B/W) iguais a 0,5, 1 e 2. O propósito central deste trabalho foi de obter a curva da taxa de propagação de trinca por fadiga (da/dN) versus a variação do fator de intensidade de tensão (ΔK) para o metal de solda por meio de ensaios normatizados, utilizando diferentes técnicas de acompanhamento e medição da trinca. A monitoração de crescimento da trinca foi feita por três técnicas: variação da flexibilidade elástica (VFE), queda de potencial elétrico (QPE) e análise de imagem (Ai). Os resultados mostraram que as diferentes relações B/W utilizadas no estudo não alteraram significantemente as taxas de propagação de trinca por fadiga, respeitado que a propagação aconteceu em condições de escoamento em pequena escala na frente da trinca. Os resultados de propagação de trinca por fadiga permitiram a obtenção das regiões I e II da curva da/dN versus ΔK para o metal de solda. O valor de ΔKlim obtido para o mesmo foi em torno de 11,8 MPa.m1/2 e os valores encontrados das constantes experimentais C e m da equação de Paris-Erdogan foram respectivamente iguais a 1,55 x10-10 [(mm/ciclo)/(MPa.m1/2)m] e 4,15. A propagação de trinca no metal de solda deu-se por deformação plástica, com a formação de estrias de fadiga. / Recent oil and gas discoveries in the Pre-Salt layer represent a huge exploration potential in Brazil, however, the technological challenges for the exploitation of these mineral resources are immense and therefore have motivated the development of studies looking for efficient methods and materials for their productions. The oil and gas pipellines, called risers, are elements that are necessarily welded and have fundamental importance in the production chain, since they transport oil and natural gas from the sea bed to the platforms and are subject to dynamic loads (fatigue) during operation. Additionally, one of the central problems in the production of oil and gas in the Pre-Salt reserves is directly associated with a highly corrosive media, such as H2S and CO2. A cheaper way to protect the pipelines from these medias is applying a protective layer of a corrosion resistant metal on the inner diameter of these pipes, creating a cladded pipe. Thus, a joining process of these pipes to form the risers must be carried out by the use of girth welds with a corrosion resistance material similar to the clad metal. As the welded structures are seen as potential location of \"crack like\" defects, to ensure the structural integrity of such component when subjected to repetitive loading conditions, it is necessary to know the fatigue crack growth rates for the girth weld. Therefore, in this work it was carried out fatigue crack propagation tests in the weld region of an API 5L X65 cladded pipe with Inconel® 625, girth welded using Inconel® 625 electrodes. From the welded region, Single Edge Notch Bending specimens, SEN(B), were removed with different thickness and width ratios (B/W= 0.5, 1, and 2). From the fatigue tests, the crack propagation rates (da/dN) as function of the variation of the stress intensity factor (ΔK), were determined for the weld metal, using different crack size measurement techniques: the elastic compliance (EC), electric potential drop (EPD) and image analysis (IA). The results showed that the different B/W ratios used in study did not modified significantly the fatigue crack growth rates, considering that crack propagation took place under small scale yielding conditions. The results of fatigue crack growth tests allowed to obtain the regions I and II of da/dN x ΔK curves for the weld metal. The ΔKth value obtained for the weld metal was around 11,8 MPa.m1/2 and the found values of the experimental constants C and m of Paris-Erdogan\'s equation were respectively equal to 1,55 x10-10 [(mm/cycle)/( MPa.m1/2)m] and 4.15. The micromechanism of fatigue crack growth took place by plastic deformation, with the formation of fatigue striations.

L’Inconel 718 est utilisé dans les disques de turbine des moteurs d’avion, de par sa haute résistance à la corrosion, à l’oxydation, au fluage et sa haute résistance mécanique à très haute température. Le nombre total de cycles de ces composants mécaniques s’élève à 109~1010 durant sa vie. Ils subissent des chargements de grande amplitude à faible fréquence, comme les forces centrifuges ou les contraintes thermiques mais aussi des chargements de faibles amplitudes à très haute fréquence, du aux vibrations des pales. Dans ce travail, on se propose d’étudier la fatigue à très grand nombre de cycles (VHCF) de l’Inconel 718 en utilisant des machines de fatigue ultrasonique, fonctionnant à 20KHz. Le système d’acquisition utilise des cartes NI et le logiciel LabView pour superviser la fréquence, la température, les déplacements durant toute la durée des tests. Des capteurs laser Keyence utilisant deux sondes pour les faces supérieure et inférieure de l’éprouvette permettent de capturer la fréquence et les modes de vibration. La différence entre les valeurs moyennes mesurées permet d’accéder à l’allongement de l’éprouvette, dû à l’auto-échauffement.3 types de matériaux avec différents traitements thermiques, AR, DA et DAHQ de l’ONERA et SAFRAN sont comparés. La différence au niveau de la taille de grain, de la phase, des précipités, … est analysée par micrographie métallographique en utilisant un microscope optique (MO) et un microscope électronique à balayage (MEB). Le comportement en traction quasi-statique et sous chargement cyclique contrainte-déformation est aussi proposé. La transition entre durcissement et adoucissement cyclique apparait à l’issue du traitement thermique. Finalement, les surfaces de ruptures sont observées en utilisant des caméras optiques et un MEB afin d’identifier les mécanismes de ruptures de l’Inconel 718 dans le domaine de la fatigue à très grand nombre de cycles. / Inconel 718 is widely used in turbine disk of aeronautic engines, due to its high resistance to corrosion, oxidation, thermal creep deformation and high mechanical strength at elevated temperature. The total cycle of these mechanical components is up to 109~1010 during its whole lifetime. It endures high-amplitude low-frequency loading including centrifugal force or thermal stress, and also low-amplitude high-frequency loading came from vibration of blade.In this work, the very high cycle fatigue (VHCF) behaviour of Inconel 718 with self-heating phenomenon without any cooling is studied using ultrasonic fatigue system at 20KHz. Acquisition system is improved using NI capture card with LabView for monitoring the frequency, temperature, displacement and so on during all the tests. Keyence laser sensor with two probes at the top and bottom surfaces of the specimens is used to reveal the frequency and vibration mode. The difference of mean values between these two probes is the elongation of the specimen caused by self-heating phenomenon.Three sets of materials with different heat treatment, As-Received (AR), Directly Aged (DA) and Directly Aged High Quality (DAHQ) from ONERA and SAFRAN are compared. The difference of grain size, phase, precipitate particle, etc. is investigated by metallographic micrograph using optical microscope (OM) and scanning electron microscope (SEM). Quasi-static uniaxial tensile property and cyclic stress-strain response is also proposed. The transition from cyclic hardening to cyclic softening appears after aged heat treatment. Finally, fracture surfaces are observed using optical camera and scanning electron microscope in order to identify the mechanism of fracture of Inconel 718 in the VHCF domain.

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.

L'Inconel 718 est un superalliage base nickel très utilisé pour produire les disques de turboréacteurs. Typiquement, une gamme de forgeage à chaud se compose de plusieurs étapes de déformation et de recuit. La présence des particules de seconde phase (particules de phase delta dans l'Inconel 718) permet en principe de limiter la croissance de grains pendant les étapes de recuit grâce au phénomène d'ancrage de Zener. Néanmoins, l'hétérogénéité microstructurale (distribution des particules, écrouissage, composition chimique) peut favoriser une croissance anormale des grains pendant le recuit. Ce phénomène est connu industriellement sous la terminologie d'"éclatement de grains". Les objectifs de la thèse étaient d'identifier les mécanismes responsables de l'éclatement des grains qui peut survenir durant les étapes de recuit sur les pièces forgées en Inconel 718, de les modéliser, et de simuler numériquement le phénomène. Les mécanismes physiques à l'origine du phénomène sont d'abord étudiés expérimentalement grâce à la caractérisation (par MEB et EBSD) des pièces forgées. L'influence des particules de seconde phase et de l'énergie stockée (estimée par des mesures de désorientations intragranulaires) est notamment étudiée. A partir des observations réalisées, une explication est proposée : le phénomène apparaît lorsque les forces motrices pour la migration des joints de grains dépassent la force de freinage de Zener ; ceci peut se produire lorsque la microstructure contient de l'énergie stockée, distribuée de manière hétérogène. Des essais de torsion à chaud sont mis en place pour reproduire, en laboratoire, le même phénomène, étudier la sensibilité aux paramètres thermomécaniques, et tester les hypothèses émises concernant les mécanismes. Les mécanismes ainsi identifiés comme responsables de l'éclatement de grains sont enfin simulés au moyen d'un modèle numérique en 2D. Le modèle numérique en champ complet est basé sur la méthode des éléments finis, et utilise le formalisme level-set pour décrire les joints de grains. La simulation de l'évolution microstructurale prend en compte à la fois les forces motrices des joints de grains liées à la capillarité et à l'énergie stockée, et l'interaction des joints de grains avec les particules de seconde phase. Ainsi, l'effet de la distribution de l'énergie stockée (estimée à partir de données expérimentales) a pu être étudié numériquement dans des microstructures avec particules. / Inconel 718 is a nickel base superalloy commonly used to manufacture the rotating disks of turbojet engines. Such disks are generally produced by hot forging, which involves a sequence of different deformation and annealing steps. The presence of second phase particles (delta phase in Inconel 718) is commonly exploited to limit grain growth during annealing via the Zener pinning phenomenon. Nonetheless, microstructure heterogeneity (with regards to second phase particles, hardening, texture and chemical composition) can lead to inhomogeneous grain growth during annealing. The objectives of this PhD work were to understand, model and simulate numerically the phenomenon of inhomogeneous grain growth that can occur in Inconel 718 turbine disks during the annealing steps of hot forging sequences. The physical mechanisms which may explain the occurrence of the phenomenon are investigated experimentally by performing SEM and EBSD analyses of Inconel 718 industrial pieces. The focus is placed on the influence of second phase particles and strain energy (estimated from intragranular misorientations) on the occurrence of the phenomenon. From those observations, it is inferred that the phenomenon occurs when the grain boundary driving forces overcome the Zener pinning forces; this is achieved when stored energy is present and heterogeneously distributed. Moreover, hot torsion tests are carried out to reproduce the phenomenon in laboratory, to evaluate its sensibility to thermomechanical parameters and to test the previously postulated mechanism. The validity of this mechanism is finally demonstrated by modelling numerically the phenomenon in 2D. The full field numerical model is based on a level set description of the grain boundaries in a finite element context. Microstructure evolution is simulated explicitly taking into account Zener pinning, capillarity and stored energy driven grain growth in a single framework. The effect of strain stored energy distributions (estimated from experimental data) in pinned microstructures is investigated focusing on the conditions leading to inhomogeneous grain growth.