L’Inconel 718 est un superalliage base nickel largement utilisé par les motoristes tels Safran Aircraft Engines pour l’élaboration des disques de turbine. Après forgeage des disques, un traitement de vieillissement appelé « Direct Aged » est appliqué. En service, le régime de croisière représente un temps de maintien sous chargement constant pour les disques. Bien que pas complètement compris, il est largement admis qu’un temps de maintien dans un cycle de fatigue a un effet néfaste sur le comportement en fissuration de l’Inconel 718 ainsi que d’autres superalliages. Cette étude porte donc sur la fissuration en fatigue-fluage dans l’Inconel 718 DA à 550°C et 650°C. Des essais sont menés pour des temps de maintien allant jusqu’à 1h. Des développements de la méthode de suivi de fissure par mesure de potentiel (DCPD) ont permis d’identifier la décharge-recharge (contribution de fatigue) d’un cycle de fatigue-fluage comme la partie la plus néfaste du cycle. L’application d’un temps de maintien amplifie cette contribution. Le temps de maintien induit également des fronts de fissure extrêmement courbes et tortueux, contrairement à de la fatigue pure. Une stratégie numérique a été développée, couplant la simulation 3D de la propagation et la méthode dite DCPD, permettant de réaliser des « essais numériques ». La propagation de fronts courbes et tortueux est simulée. Il a été démontré que le comportement en propagation est directement lié à la forme du front de fissure et son évolution. Des essais complexes ont été menés, sous vide, ou impliquant des surcharges. Lorsque l’effet du temps de maintien est annihilé, les morphologies complexes des fronts disparaissent. Elles sont alors associées à une inhibition locale de l’effet endommageant de l’environnement due à la plasticité et aux vitesses de déformation locales. Tous les essais présentés sont analysés en considérant l’effet de la vitesse de déformation locale qui influe largement le comportement en fissuration de l’Inconel 718. / Inconel 718 is a nickel-based superalloy widely used by aeroengines manufacturers like Safran Aircraft Engine to manufacture turbine disks. After forging, disks are given an ageing treatment called “Direct Aged”. In service, during cruise, these critical components handle hold-time periods at constant loading. It is well known, although not fully understood, that hold-time increases crack growth rates (CGR) in Inconel 718 as well as others superalloys. Therefore, this study focuses on crack propagation under hold-time conditions in DA Inconel 718, at 550°C and 650°C. Experiments were carried out for different hold-times, up to 1h. Developments on the crack monitoring technique (DCPD) led to the conclusion that the most damaging part of the cycle is load-reversal (fatigue contribution). This contribution is enhanced by the hold-time period. Holdtime leads to dramatically curved and tortuous crack front, contrary to pure fatigue cycles. A numerical framework was developed, combining crack growth and DCPD simulations, so that “numerical tests” can be carried out. Using this method, crack growth simulations were performed from curved and tortuous, experimentally reproduced, crack front. It was concluded that increased crack CGR under hold-time conditions are closely related to the crack front morphology and its evolution during propagation. More complex tests, with overloads or under vacuum, were carried out. When the hold-time effect is inhibited, complex morphologies vanish. Such morphologies were associated to local inhibition of the environmental damaging effect due to local high plastic strain and strain rates. The large variety of experiments, presented in this study, was then successfully analyzed considering the effect of local strain rates which greatly influence the crack growth behavior of Inconel 718.

Ce travail est une contribution à une étude de recherche et développent, proposée par Hydro Aluminium, dans le domaine des mécanismes d'endommagement de filières d'extrusion et. L'originalité du travail de thèse est basée sur le développement d'un alliage Inconel 718 optimisé pour l'application spécifique de filière d’extrusion, ce qui représente un saut technologique dans l'emploi de ce superalliage dans le domaine des outils. L'impact des paramètres du procédé d'extrusion, appelés paramètres extrinsèques, - tels que la vitesse d'extrusion, la longueur de billette, le chargement thermo-mécanique - sur le comportement mécanique du matériau a été analysé. Les cycles traction-compression sont simulés à l'aide d’essais isothermes de fatigue oligocyclique (LCF) qui donnent des informations sur les différents mécanismes d'endommagement survenant dans la filière. Du point de vue scientifique, la sollicitation de fatigue oligocyclique isotherme (LCF) est considérée comme la plus représentative des conditions thermomécaniques agissant sur l'outil. Les résultats montrent que la vitesse de déformation et de temps de maintien ont un impact significatif sur la durés de vie en fatigue. Le développent du matériau, enfin, a été atteint en modifiant les paramètres intrinsèques au matériau - tels que la taille des grains et la morphologie des précipités intermétalliques. Des traitements thermiques alternatifs, permettant d'adapter le matériau aux conditions spécifiques imposées par le procédé d'extrusion, ont été formulés. Des essais de fatigue LCF supplémentaires, ont permit de comparer la réponse cyclique de ces nouvelles nuances à celle du traitement original. Un de ces traitement, élaboré au travers d’une approche pluridisciplinaire incluant les aspects métallurgie, chimie et mécanique, a été retenu comme la nouvelle procédure standard pour le traitement des matrices d'extrusion en Inconel 718. / This present work is a contribution to an extensive development study, promoted by Hydro Aluminium, in the field of the damage mechanisms of extrusion dies. The originality of the present work is based on the development of an optimized Inconel 718 alloy as bulk material for extrusion die., which corresponds to a new application of this alloy in the field of tools: The investigation of the impact of the so called “Material Extrinsic Parameters”, such as extrusion speed, billet length and thermo-mechanical loading on the mechanical behaviour of the material is proposed. The cyclic tensile and compressive stresses, acting on the die, are simulated by isothermal Low Cycle Fatigue (LCF) tests. Results show that strain rate and holding time have a significant impact on fatigue life. These considerations represent the “Input Data” for the design of an optimized Inconel 718 in order to adapt the material to the specific conditions imposed by the extrusion process. This objective is achieved by modifying the “Material Intrinsic Parameters” such as grain size or precipitates morphology through the formulation of alternative thermal treatments. Additional LCF tests, are carried out to compare the cyclic response of the alternative Inconel 718 grades. One of this treatment, elaborated by a multidisciplinary approach including metallurgical, chemical and mechanical experiments that has been implemented in the industrial production practice as the new standard procedure for the thermal treatment of the Inconel 718 extrusion dies.

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.

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.

Nickel based superalloys are currently being investigated for high temperature applications in advanced steam power plant operating at temperatures of 700˚C and above. Three nickel-based superalloys Inconel 617, Inconel 625 and Nimonic 263 alloys, which are of primary interest for boiler technology components such as furnace walls, superheater tubes, header and steam pipes, etc and for steam turbine technology components such as HP &IP cylinders, rotor forgings, casing and valve chest, blading, etc., have been evaluated for long and short term creep performance. Creep deformation processes occurring at high temperatures and stresses lead to the evolution of microstructures in the form of precipitation, precipitate coarsening and recovery effects. The deterioration in mechanical properties as a result of this microstructural change has been evaluated by hardness testing. This work discusses the microstructural evolution occurring in alloys in samples that have been creep exposed at a series of temperatures from 650°C to 775°C and for durations from 1000 to 45,000 hours using advanced FEGSEM, TEM, XRD and phase extraction techniques. The fractions and morphology of different phases, their locations during exposure to higher temperatures and probable creep fracture mechanism in these alloys are illustrated and discussed.

L'Inconel 718 est un superalliage base-nickel très utilisé pour la fabrication de pièces aéronautiques soumises à de fortes contraintes et de hautes températures. La maîtrise de la microstructure finale issue de la mise en forme à chaud est un des éléments clés pour le contrôle des propriétés mécaniques et pour répondre aux exigences strictes du secteur. Dans cette étude, l'évolution de la microstructure de l'Inconel 718 est étudiée au moyen d'essais de torsion suivis d'une trempe à l'eau (pour examiner les évolutions dynamiques) ou d'un maintien à la température de déformation puis d'une trempe à l'eau (pour examiner les évolutions post-dynamiques). Ces essais sont réalisés dans les domaines de température δ-supersolvus et δ-subsolvus et pour des vitesses de déformation de 10-2 à 0.1 s-1. Des analyses microstructurales par microscopie électronique à balayage et cartographie des orientations cristallographiques par EBSD sont réalisées pour suivre l'évolution de la fraction recristallisée, de la taille de grains recristallisés ainsi que de l'état de précipitation lors de la déformation et des maintiens pré- et post-déformation. Sur base de ces observations expérimentales, les principaux mécanismes métallurgiques actifs sont identifiés, puis modélisés : écrouissage, germination de nouveaux grains, migration de joints de grains, et interaction avec les particules de seconde-phases. Un modèle d'évolution microstructurale en champ moyen a été enrichi pour prendre en compte l'ensemble de ces mécanismes élémentaires et leur dépendance aux conditions thermomécaniques. Ce modèle permet de décrire, pour les domaines δ-subsolvus et δ-supersolvus, les cinétiques de recristallisation dynamique et post-dynamique de l'Inconel 718, les cinétiques de précipitation et dissolution de la phase δ, ainsi que l'évolution de la taille de grains. Il prédit également les courbes contrainte-déformation dans le domaine de température δ-supersolvus. / Inconel 718 is nickel-based Superalloy widely used in the aeronautic industry to manufacture aircraft parts subjected to extreme in-service conditions of high stresses at elevated temperatures. Controlling the microstructure after hot forming is a key element to control the mechanical properties of the final products and meet the tight specifications imposed by the aeronautic industry.In this work, the microstructure evolution of Inconel 718 was investigated via isothermal and iso-strain rate torsion tests followed by water quenching (to investigate dynamic evolution) or by annealing at deformation temperature then water quenching (to investigate post-dynamic evolution). These tests were conducted in both δ-Supersolvus and δ-Subsolvus temperature domains and for strain rates of 0.01 to 0.1 s-1.Scanning electron microscopy (SEM) and Electron Back Scattered Diffraction (EBSD) were used to characterize the microstructure and follow the evolution of the recrystallized fraction, the recrystallized grain size and the δ-phase precipitation after deformation and during pre-deformation and post-deformation annealing. Based on these experimental observations, the main metallurgical mechanisms have been identified and modelled: hardening, nucleation of new grains, grain boundaries migration and the δ-phase- recrystallization interaction.A two-site mean field approach having a low computational cost was chosen to model the microstructural evolution at different thermomechanical conditions. This model describes the main mechanisms taking place during hot forming of Inconel 718 in both δ-Supersolvus and δ-Subsolvus domains and predicts the recrystallization kinetics in both dynamic and post-dynamic regimes , the δ-phase precipitation and dissolution kinetics and the grain size evolution. The model predicts also the strain-stress curves at high temperatures in the absence of δ-phase particles.

Des influences de l’humidité sur le comportement à l’oxydation sous air de l’alliage Inconel 600 ont été étudiées à haute température (de 600°C à 900°C) pour différentes durées d’oxydation (de 24 heures à 150 heures). La cinétique d’oxydation a été étudiée par l’analyse thermogravimétrie : à une température relativement basse (de 600°C à 700°C), la cinétique suit une seule loi parabolique ; à plus haute température (de 800°C à 900°C), une évolution en deux étapes a été observée, chaque étape suit une loi parabolique. En présence de la vapeur d’eau (de 0% à 19% d’humidité absolue), à toutes les températures étudiées, la teneur de Cr en surface de l’oxyde est plus élevée que celle oxydée sans vapeur d’eau. L’oxydation à une même température, la prise de masse diminue en présence de la vapeur d’eau. La morphologie de la surface oxydée est étudie par MEB-FEG. Avec la présence d’humidité, la couche d’oxyde est plus compacte et homogène. En couplant avec la diffraction des rayons X en faible incidence (GIXRD), deux couches d’oxyde ont été observées dans la section transversale quand la température d’oxydation est plus de 700°C avec ou sans l’humidité: la couche externe contient principalement de la phase NiO et la couche interne contient de spinelle NiCr2O4 et de la phase Cr2O3. Les fractions de chaque phase dépendent des conditions d'oxydation (température, taux humidité, durée d’oxydation etc…). Les études de contraintes dans les couches d’oxydes ont été effectuées par la méthode classique des sin2ψ en diffraction des rayons pour les contraintes résiduelles, ainsi que par la méthode de déflexion in situ pour les contraintes de croissance. Les contraintes résiduelles dans les 2 couches oxydes sont en compression, tandis que le niveau de contraintes résiduelles de compression dans la couche NiO (<600 MPa) est moins important que celui dans la couche de NiCr2O4 (> 800 MPa). En présence de la vapeur d’eau, les contraintes résiduelles en compression augmentent de façon très importante. Les analyses et les évaluations des contraintes (résiduelles, croissance et thermique) ont été effectuées. Ces résultats indiquent que le mécanisme d'oxydation n’est pas seulement un processus chimique, mais un processus mécano-chimique complexe qui fait intervenir le comportement mécanique. Les analyses par SIMS et par XPS ont été réalisées sur des échantillons oxydés pour étudier le mécanisme de diffusion atomique et le rôle de l’humidité sur l’oxydation. / Humidity influences on the oxidation behavior of the alloy in air Inconel 600 were investigated at high temperature (600°C to 900°C) for various oxidation periods (24 hours to 150 hours) .The oxidation kinetics were studied by thermo gravimetric analysis: at a relatively low temperature (600°C to 700°C), the kinetics following a single parabolic law; at a higher temperature (800°C to 900°C), a two-stage evolution was observed, each step follows a parabolic law. In the presence of water vapor (from 0% to 19% absolute humidity) at all temperatures studied, the content of Cr in the oxide surface is higher than that oxidized without steam. Oxidation at the same temperature, the weight gain decreases in the presence of water vapor.The morphology of the oxidized surface is studied by FEG-SEM. With the presence of water vapor, the oxide layer is more compact and homogeneous. By coupling with the X-ray diffraction in low incidence (GIXRD), two oxide layers were observed in the cross section when the oxidation temperature is over 700°C with or without humidity: the outer layer contains mainly of the NiO phase and the inner layer contains spinel NiCr2O4 and Cr2O3 phase. The fractions of each phase depend on the oxidation conditions (temperature, humidity, oxidation period etc ...).Constraints studies in the oxide layers have been made by the classical method of ray diffraction sin2ψ to residual stresses as well as the in situ method for deflection of the growth stresses. Residual stresses in the two oxide layers are in compression, while the level of compressive residual stress in the NiO layer (<600 MPa) is less than that in the layer of NiCr2O4 (> 800 MPa). In the presence of water vapor, the compressive residual stress increases dramatically. The analyzes and assessments of constraints (residual, growth and thermal) were performed. These results indicate that the oxidation mechanism is not only a chemical process, but a complex chemical mechanical process involving the mechanical behavior. Analysis by SIMS and XPS were performed on samples oxidized to study the atomic scattering mechanism and the role of humidity on the oxidation.

Properties of samples and their coatings may be affected by the electron beam. This paper deals with the analysis of the microstructure, phase and chemical composition and the determination of mechanical characteristics of inconel steel substrate and CoNiCrAlY coatings deposited via different types of thermal spraying (HVOF, cold spray), in combination with modifications by the electron beam technology. During the study it was found that the deposition did not change the chemical composition. Further it was found that the interaction of the electron beam with the material did not change the chemical composition, but there is a change in the structure and a reduction of porosity and surface roughness, resulting in a change of mechanical properties such as decreasing hardness or increase of the modulus of elasticity.

No description available.

Analyse des interactions entre les processus d'oxydation et les mécanismes de déformation conduisant à un mode de propagation des fissures soit transgranulaire ductile, soit intergranulaire fragile, le dernier mode étant associé à une propagation beaucoup plus rapide des fissures. Proposition de différents modèles phénoménologiques permettant de relier le mode d'oxydation au mode de déformation, ainsi que le mode d'oxydation au mode de propagation des fissures.