This research focused on a comprehensive microstructural and mechanical property characterisation study of the Ni-Fe-Cr alloys 718 and 945X. The aim of the project was to better understand the relationship between performance and microstructure of existing (Alloy 718) and newly developed (Alloy 945X) high strength nickel alloys focusing on downhole applications. The main difference between the two alloys is that alloy 945X has lower Nb content than alloy 718, which may minimise the tendency to form delta when combined with correct processing. Previous studies have related the hydrogen embrittlement in alloy 718 with the collection of hydrogen by delta phase. Microstructural characterisation of the new alloy 945X after long term isothermal exposure up to 120 hours in the temperature range 650◦C to 900◦C was conducted with scanning electron microscopy (SEM), to generate a time-temperature-transformation (TTT) diagram. The TTT diagram was used as a road map for designing two isothermal heat treatments of alloy 945X on tensile specimens. Then, the effect of hydrogen charging on the tensile properties and microstructure of the 'as-received' and these two variant heat treatments was investigated. Fractographic analysis showed that, in the presence of hydrogen, intergranular fracture occurred for all the heat treatments, regardless the presence of delta phase at grain boundaries. There was no simple correlation between the volume fraction of delta-phase and susceptibility to hydrogen assisted embrittlement. Rather, it was demonstrated that the morphology and distribution of delta-phase along grain boundaries plays a key role and the other precipitate phases also have an influence through their effect on the ease of strain localisation. This study also examined the hydrogen embrittlement sensitivity of nickel alloy 718 given four different heat treatments to obtain various microstructural states. Each heat treatment leads to differences in the precipitate morphologies of γ', γ'' and delta phases. Material characterisation and fractography of the examined heat treatments were performed using a high resolution FEG-SEM. Three specimens of each condition were pre- charged with hydrogen and tensile properties were compared with those of non-charged specimens. It was observed that hydrogen embrittlement was associated with intergranular and transgranular microcrack formation, leading to an intergranular brittle fracture. delta phase may assist the intergranular crack propagation, and this was shown to be particularly true when this phase is coarse enough to produce crack initia- tion, but this is not the only factor determining embrittlement. Other microstructural features play a role, as does the strength of the material. Finally, the evolution of delta-(Ni3Nb) phase in alloy 718 from the early stages of precipitation, with a particular focus on identifying the grain boundary characteristics that favour precipitation of grain boundary delta phase was investigated. Results showed that delta phase was firstly formed on Σ3 boundaries after 5 hours at the examined temperature (800◦C). Increasing ageing time at 800◦C was observed to lead to an increase in size and precipitation of phases γ'-γ''-delta, an increase in fraction of the special CSL boundaries and an evolution in the morphology of twins and the growth of grains.

Les composants des industries de l'aéronautique, du spatial ou de l'énergie sont souvent en fonctionnement dans des environnements sévères où les températures et les pressions peuvent atteindre des valeurs importantes. Les matériaux traditionnels sont alors remplacés par des superalliages dits réfractaires, l'Inconel 718 est un de ces matériaux. Ils sont en particulier caractérisés par la conservation de leurs propriétés mécaniques à hautes températures. L'Inconel 718 est un alliage à base nickel, réputé comme difficile à usiner. Cette difficulté de mise en forme, liée à ses caractéristiques physiques et mécaniques, impose généralement une utilisation très importante de fluides de coupe ; ceux-ci représentent une fraction significative du coût de la pièce usinée. L'objectif est alors de migrer vers l'usinage à sec et grande vitesse. Cependant, du fait des caractéristiques mécaniques et du caractère réfractaire de l'Inconel 718, les surfaces générées peuvent être affectées thermiquement durant l'opération d'usinage avec la mise en place de contraintes résiduelles en traction néfastes pour la tenue en service des pièces usinées. Au travers des travaux présentés, nous nous proposons de montrer la faisabilité de l'usinage à sec de l'Inconel 718 et ses conséquences sur l'intégrité des surfaces réalisées. Des essais de tournage sous lubrification et à sec ont été réalisés dans des conditions de semi-finition avec un outil en carbure de tungstène revêtu. Les surfaces et sous surfaces ont été observées et qualifiées par un ensemble de moyens : microscope à interférométrie, microscope électronique à balayage, microduromètre, goniomètre rayons X pour l'analyse des contraintes résiduelles. L'analyse de l'intégrité des surfaces a permis de mettre en évidence les principaux facteurs influents. La qualité des surfaces produites dépendant de la maîtrise de la température de coupe, une technique de mesure des températures a alors été développée pour une opération de fraisage ; elle est basée sur la technologie des thermocouples. Les essais menés ont permis de déterminer la température en surface et en sous surface ; ces informations sont des éléments importants de validation d'un modèle thermique de la coupe. Enfin, à la suite d'essais de fraisage périphérique et de la mesure des efforts pour différentes conditions de coupe, nous présentons une comparaison entre ces résultats expérimentaux et une modélisation du procédé. La modélisation correspond à une approche thermomécanique de la coupe. En termes d'efforts, la comparaison est tout à fait satisfaisante ; un prolongement de cette approche pour valider l'aspect thermique, est toutefois envisagé.

Additive manufacturing (AM) is the name given to the technology of building 3D parts by adding layer-by-layer of materials, including metals, plastics, concrete, etc. Of the different types of AM techniques, electron beam melting (EBM), as a powder bed fusion technology, has been used in this study. EBM is used to build parts by melting metallic powders by using a highly intense electron beam as the energy source. Compared to a conventional process, EBM offers enhanced efficiency for the production of customized and specific parts in aerospace, space, and medical fields. In addition, the EBM process is used to produce complex parts for which other technologies would be either expensive or difficult to apply. This thesis has been divided into three sections, starting from a wider window and proceeding to a smaller one. The first section reveals how the position-related parameters (distance between samples, height from build plate, and sample location on build plate) can affect the microstructural characteristics. It has been found that the gap between the samples and the height from the build plate can have significant effects on the defect content and niobium-rich phase fraction. In the second section, through a deeper investigation, the behavior of Alloy 718 during the EBM process as a function of different geometry-related parameters is examined by building single tracks adjacent to each other (track-by-track) andsingle-wall samples (single tracks on top of each other). In this section, the main focus is to understand the effect of successive thermal cycling on microstructural evolution. In the final section, the correlations between the main machine-related parameters (scanning speed, beam current, and focus offset) and the geometrical (melt pool width, track height, re-melted depth, and contact angle) and microstructural (grain structure, niobium-rich phase fraction, and primary dendrite arm spacing) characteristics of a single track of Alloy 718 have been investigated. It has been found that the most influential machine-related parameters are scanning speed and beam current, which have significant effects on the geometry and the microstructure of the single-melted tracks.

Fundação de Amparo a Pesquisa do Estado de Minas Gerais / The nickel-based superalloys have a high mechanical strength which remains at elevated temperature, high creep and fatigue resistances and excellent oxidation resistance. This makes these alloys highly recommended for use in high temperature working environments such as mechanical components for the aerospace industry. However, these characteristics are major problems when machining them, as it promotes high heat generation in the flow zone, resulting in the development of high wear rates on the cutting tools. In order to reduce the problems caused by the high temperatures generated, the application of a cutting fluid, when possible, is essential to reduce friction at the chip-tool-workpiece interfaces and lower the temperatures in the cutting zone. Seeking to further increase in the efficiency of cutting fluids during machining of nickel alloys, this work presents a study of the influence of solid lubricants, graphite and molybdenum disulphide (MoS2) mixed to a vegetal based cutting fluid, applied by conventional method (flooding) and minimal quantity of fluid - MQF in turning of Inconel 718 with carbide and ceramic (mixed, whisker and SiAlON) tools. When turning with cemented carbide tools the addition of graphite to the cutting fluid provided the best results, while with ceramic tools MoS2 presented the best performance. The life of the carbide tool had an average increase above 200% in conventional flooding application of cutting fluid when compared to MQF, regardless the addition of solid lubricant. The addition of solid lubricants promoted an increase in the life of whisker and SiAlON tools. The flank wear was dominant for cemented carbide tools and SiAlON ceramics, while for whisker and mixed ceramics the notch wear was predominant. Attrition and diffusion wear mechanism were observed in all evaluated conditions. The addition of solid lubricant to the cutting fluid provided significant improvements in the surface roughness values for most of the evaluated conditions. However, there were no significant changes in the machining forces and cutting temperature. The residual stress was tensile and compression, depending on the fluid application method. Overall, the addition of solid lubricant showed no significant differences. / As superligas à base de níquel apresentam alta resistência mecânica que se mantém em elevadas temperaturas, altas resistência à fluência e à fadiga e excelente resistência a oxidação. Isso torna estas ligas altamente recomendadas para utilização em ambientes que trabalham a altas temperaturas, como por exemplo na fabricação de componentes mecânicos para a indústria aeroespacial. Entretanto, esta característica representa um grande problema quando elas são usinadas, pois promove elevada geração de calor na zona de fluxo, implicando no desenvolvimento de altas taxas de desgaste da ferramenta de corte. A fim de reduzir os problemas causados pelas altas temperaturas geradas, a aplicação de um fluido de corte, quando possível, é essencial, proporcionando redução do atrito na interface cavaco-ferramenta-peça e menores temperaturas na zona de corte. Na busca de aumentar ainda mais a eficiência dos fluidos de corte na complexa usinagem das ligas de níquel, este trabalho apresenta um estudo da influência dos lubrificantes sólidos grafite e bissulfeto de molibdênio (MoS2) misturado a um fluido de corte de base vegetal, aplicados pelo método convencional (jorro) e mínima quantidade de fluído MQF, no torneamento do Inconel 718, com ferramentas de metal duro e cerâmicas (mista, whisker e SiAlON). No torneamento com ferramentas de metal duro a adição de grafite ao fluido de corte proporcionou os melhores resultados, enquanto que no torneamento com ferramentas cerâmicas, foi o MoS2 que apresentou melhor desempenho. A vida da ferramenta de metal duro teve um incremento acima de 200% na usinagem convencional (jorro) quando comparado com a usinagem por MQF, sem considerar a adição do lubrificante sólido. A adição de lubrificantes sólidos promoveu um incremento na vida das ferramentas whisker e SiAlON. O desgaste de flanco foi predominante para as ferramentas de metal duro e cerâmica SiAlON, enquanto que nas cerâmicas whisker e mista o desgaste de entalhe foi predominante. Os mecanismo de desgaste de attrition e difusão foram observados em todas as condições avaliadas. A adição de lubrificante sólido ao fluido de corte proporcionou melhorias significativas nos valores da rugosidade para a maioria das condições avaliadas. No entanto, não se observou mudanças significativas nas forças e temperatura de usinagem. As tensões residuais foram de tração e compressão, dependendo do método de aplicação do fluido. No geral, a adição do lubrificante sólido não apresentou diferenças significativas. / Doutor em Engenharia Mecânica

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The challenges faced in today’s industry require materials capable of working in chemically aggressive environments at elevated temperature, which has fueled the development of oxidation resistant materials. All-Oxide Ceramic Matrix Composites (OCMC) are a promising material family due to their inherent chemical stability, moderate mechanical properties, and low weight. However, limited information exists regarding their behavior when in contact with other high-temperature materials such as superalloys. In this work three sets of tribological tests were performed: two at room temperature and one at elevated temperature (650 °C). The tests were performed in a pin-on-disk configuration testing Inconel 718 (IN-718) pins against disks made with an aluminosilicate geopolymeric matrix composite reinforced with alumina fibers (N610/GP). Two different loads were tested (85 and 425 kPa) to characterize the damage on both materials. Results showed that the pins experienced ~ 100 % wear increase when high temperature was involved, while their microstructure was not noticeably affected near the contact surface. After high temperature testing the OCMC exhibited mass losses two orders of magnitude higher than the pins and a sintering effect under its wear track, that led to brittle behavior. The debris generated consists of alumina and suggests a possible crystallization of the originally amorphous matrix which may destabilize the system. The data suggests that while the composite’s matrix is stable, wear will not develop uncontrollably. However, as soon as a critical load/temperature combination is attained the matrix is the first component to fail exposing the reinforcement to damage which drastically deteriorates the integrity of the component.

This thesis is on fatigue crack growth experiments and assessments of fatigue crack growth rates. Both constant and variable amplitude loads in two different materials are considered; a nickel based super-alloy Inconel 718 and a stainless steel 316L. The considered load levels extend from small scale yielding (SSY) to large scale yielding (LSY) for both materials. The effect of different load schemes on the fatigue crack growth rates is investigated on Inconel 718 and compact tension specimens in Paper A. It is concluded that load decreasing schemes give a to high Paris law exponent compared to constant or increasing load amplitude schemes. Inconel 718 is further analyzed in Paper B where growth rates at variable amplitude loading in notched tensile specimens are assessed. The predictions are based on the fatigue crack growth parameters obtained in Paper A. The crack closure levels are taken into consideration and it is concluded that linear elastic fracture mechanics is incapable of predicting the growth rates in notches that experience large plastic cyclic strains. Even if crack closure free fatigue parameters are used and residual stresses due to plasticity are included. It is also concluded that crack closure free and nominal fatigue crack growth data predict the growth rates equally well. However, if the crack closure free parameters are used, then it is possible to make a statement in advance on the prediction in relation to the experimental outcome. This is not possible with nominal fatigue crack growth parameters. The last three papers consider fatigue crack growth in stainless steel 316L. Here the load is defined as the crack tip opening displacement parameter. Paper C constitutes an investigation on the effect of plastic deformation on the potential drop and consequently the measured crack length. It is concluded that the nominal calibration equation obtained in the undeformed geometry can be used at large plastic deformations. However, two conditions must be met: the reference potential must be taken in the deformed geometry and the reference potential needs to be adjusted at every major change of plastic deformation. The potential drop technique is further used in Paper D and Paper E for crack length measurements at monotonic LSY. Constant amplitude loads are considered in Paper D and two different variable amplitude block loads are investigated in Paper E. The crack tip opening displacement is concluded in Paper D to be an objective parameter able to characterize the load state in two different geometries and at the present load levels. Furthermore, if the crack tip opening displacement is controlled in an experiment and the local load ratio set to zero, then only monotonic LSY will appear due to extensive isotropic hardening, i.e. elastic shake-down. This is also the reason why the linear elastic stress-intensity factor successfully could merge all growth rates, extending from SSY to monotonic LSY along a single line in a Paris law type of diagram, even though the generally accepted criteria for SSY is never fulfilled. For the variable amplitude loads investigated in Paper E, the effect of plastic deformation on measured potential drop is more pronounced. However, also here both the crack tip opening displacement parameter and the linear elastic stress-intensity factor successfully characterized the load state. / <p>QC 20130108</p>