Les travaux présentés dans cette thèse sont réalisés dans le cadre du projet européen ACCENT et s’inscrivent dans la problématique de l’utilisation de la surveillance d’usinage dans la fabrication des pièces critiques de moteurs aéronautiques. L’objectif est de définir une technique de surveillance de l’usure de l’outil dans l’usinage de l’alésage central d’un disque haute pression réalisé en superalliage à base nickel. Trois grandes étapes peuvent être identifiées dans notre démarche : l’identification des modes de dégradation dans le perçage de l’Udimet® 720 LI, la définition de relations entre les différents types d’usure et les grandeurs physiques mesurées et finalement, la proposition de stratégies de surveillance basées sur les résultats précédents. Afin de répondre aux objectifs, un protocole expérimental a été défini. Les campagnes expérimentales nous ont permis de caractériser l’usure du foret et de définir une cartographie des modes de dégradation en fonction de conditions de coupe testées. Par ailleurs, l’impact des perturbations d’usinage (coupure de lubrification, modification du pourcentage d’émulsion du lubrifiant, défaut de position de l’outil par rapport à l’avant-trou, etc.) a été étudié. La deuxième partie consiste à identifier les relations entre les modes de dégradation et les signaux de surveillance enregistrés (efforts, couple, puissance, vibrations, etc.). Pour cela, nous avons privilégié deux pistes : une explication directe de l’évolution des signaux par des phénomènes physiques et une approche selon « la base de données », pour développer des modèles d’usures par des critères statistiques extraits sur les signaux. Cette analyse a aussi permis la détection de certaines perturbations d’usinage en utilisant les grandeurs physiques mesurées. Il s’agit notamment d’un défaut d’excentration de l’outil dans le porte-outil et d’un problème d’évacuation de copeaux. La troisième étape porte sur la sensibilité des signaux afin de détecter l’ensemble des phénomènes et la définition des stratégies de surveillance pouvant être mises en œuvre. Pour chaque relation définie, nous avons déterminé une probabilité de détection. Ensuite, nous avons utilisé les signaux en parallèle afin d’accroitre la robustesse de la détection. Les taux de probabilité ont été améliorés, en se basant sur l’hypothèse d’indépendance des signaux (sans calculer les biais existants). Enfin, l’association de l’approche phénoménologique à l’approche dite « statistique » a permis d’augmenter la robustesse de la surveillance. / The work presented in this thesis is a part of European project ACCENT and fits into the context of using process monitoring in the manufacture of critical parts for aircraft engines. The aim is to define a monitoring technique for the tool wear in the machining of the central bore of a high pressure disk made in nickel based superalloy. The major stages can be identified in our approach: identification of tool failure modes in drilling Udimet® 720 LI, defining the relationships between wear and measured physical quantities and finally, a proposal for monitoring strategies based on the previous results. In order to complete the objectives, an experimental protocol was defined. The experimental campaigns allowed us to characterize the drill wear and to define cartography of tool failure modes depending on cutting conditions tested. Moreover, the impact of machining disturbances (lubricant stop, change in percentage of lubricant emulsion, the position over the before hole, etc.) was studied. In the second part, the relations between the tool failure modes and monitoring signals recorded during the machining (forces, torque, power, vibrations, etc.) were identified. For this task, we focused on two directions: a straightforward explanation of signals evolution by physical phenomena and “black box” approach to develop wear models from a database obtained by statistical criteria extracts from the signals. This analysis also allowed the detection of certain machining disturbances using the physical quantities. These include an eccentricity of the tool in the tool holder and a chips evacuation problem. The third part concerns the signals sensitivity to detect the different phenomena and the definition of monitoring strategies which can be implemented. For each relation defined, a detection probability was determined. Further, we used signals in parallel to increase the robustness of detection. The probabilities were improved, with an assumption of independent signals (without calculating existing biases). Finally, the combination of the phenomenological approach to the so-called "statistical" has increased the robustness of the monitoring technique.

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, an alloy system bases on nickel as the matrix element with the addition of up to 10 more alloying elements including chromium, aluminum, cobalt, tungsten, molybdenum, titanium, and so on. Through the development and improvement of nickel-based superalloys in the past century, they are well proved to show excellent performance at the elevated service temperature. Owing to the combination of extraordinary high-temperature mechanical properties, such as monotonic and cyclic deformation resistance, fatigue crack propagation resistance; and high-temperature chemical properties, such as corrosion and oxidation resistance, phase stability, nickel-based superalloys are widely used in the critical hot-section components in aerospace and energy generation industries. The success of nickel-based superalloy systems attributes to both the well-tailored microstructures with the assistance of carefully doped alloying elements, and the intently developed manufacturing processes. The microstructure of the modern nickel-based superalloys consists of a two-phase configuration: the intermetallic precipitates (Ni,Co)3(Al,Ti,Ta) known as γ′ phase dispersed into the austenite γ matrix, which is firstly introduced in the 1940s.  The recently developed additive manufacturing (AM) techniques, acting as the disruptive manufacturing process, offers a new avenue for producing the nickel-based superalloy components with complicated geometries. However, γ′ strengthened nickel-based superalloys always suffer from the micro-cracking during the AM process, which is barely eliminated by the process optimization. On this basis, the new compositions of γ′ strengthened nickel-based superalloy adapted to the AM process are of great interest and significance. This study sought to design novel γ′ strengthened nickel-based superalloys readily for AM process with limited cracking susceptibility, based on the understanding of the cracking mechanisms. A two-parameter model is developed to predict the additive manufacturability for any given composition of a nickel-based superalloy. One materials index is derived from the comparison of the deformation-resistant capacity between dendritic and interdendritic regions, while another index is derived from the difference of heat resistant capacity of these two spaces. By plotting the additive manufacturability diagram, the superalloys family can be categorized into the easy-to-weld, fairly-weldable, and non-weldable regime with the good agreement of the existed knowledge. To design a novel superalloy, a Cr-Co-Mo-W-Al-Ti-Ta-Nb-Fe-Ni alloy family is proposed containing 921,600 composition recipes in total. Through the examination of additive manufacturability, undesired phase formation propensity, and the precipitation fraction, one composition of superalloy, MAD542, out of the 921,600 candidates is selected. Validation of additive manufacturability of MAD542 is carried out by laser powder bed fusion (LPBF). By optimizing the LPBF process parameters, the crack-free MAD542 part is achieved. In addition, the MAD542 superalloy shows great resistance to the post-processing treatment-induced cracking. During the post-processing treatment, extensive annealing twins are promoted to achieve the recrystallization microstructure, ensuring the rapid reduction of stored energy. After ageing treatment, up to 60-65% volume fraction of γ′ precipitates are developed, indicating the huge potential of γ′ formation. Examined by the high-temperature slow strain rate tensile and constant loading creep testing, the MAD542 superalloy shows superior strength than the LPBF processed and hot isostatic pressed plus heat-treated IN738LC superalloy. While the low ductility of MAD542 is existed, which is expected to be improved by modifying the post-processing treatment scenarios and by the adjusting building direction in the following stages of the Ph.D. research. MAD542 superalloy so far shows both good additive manufacturability and mechanical potentials. Additionally, the results in this study will contribute to a novel paradigm for alloy design and encourage more γ′-strengthened nickel-based superalloys tailored for AM processes in the future. / <p>Additional funding agencies: Agora Materiae Graduate School for multidisiplinary PhD students at Linköping University, and Stiftelsen Axel Hultgren.</p>

Nickel superalloys are used for high-temperature application in energetic and aerospace industry. They are exposed to aggressive environment at high temperatures with the interactions between fatigue and creep processes, high-temperature oxidation, corrosion and erosion. Lifetime extension of such strained parts while increasing the performance of particular machine is possible by applying protective surface coatings. The subject of this work is to investigate the fatigue failure mechanisms of superalloy Inconel 713LC at 800 °C and to compare these mechanisms between material with a protective coating based on Al-Si and material without coating. The location of initiation fatigue cracks, their propagation and the fatigue crack propagation rate in some areas were analyzed by optical microscopy, scanning electron microscopy and confocal laser scanning microscopy. Based on previous research it was found that the application of the coating AlSi has a positive effect on lifetime of alloy Inconel 713LC. These results were confirmed and estimated in the diploma thesis.

No description available.

Laser-material interaction of Nickel based superalloy Haynes 282 melt pools were studied for laser parameters similar to laser powder bed fusion (PBF-LB) without powder. The effect of power, speed, hatch distance and laser focus offset were analysed by characterizing different types of melt pool behaviour, including conduction, transition to keyhole, and keyhole mode. Focus offset parameter was found to modify the melting mode from keyhole to conduction type in experiments with and without powder. This change in melting mode is attributed to the variation in laser beam spot size for the same line energy. Such manipulation of type of melting with control of focus offset can be utilized as a method to optimize process parameters for novel materials in the PBF-LB process at high layer thickness. Based on the above study, cubes were built with refined process parameters utilizing powder layer thicknesses of 60- and 90-microns for improved productivity, using partial factorial design of experiment. The conduction mode of melting helped reducing defects, minimizing lack of fusion and keyhole porosity in specimens built with powder at 60- and 90-microns layer thickness. Effect of process parameters and indirect measure like area energy, on the melt pool overlap, defect level and dominant shape of the defects are presented. Optimizing the process parameters to identify the boundaries for building cubes with reduced porosity is also discussed. / Den Ni-baserade superlegeringen, Haynes 282, skannades med laserparametrar liknande de som används i laserpulverbäddfusion (PBF-LB), men utan pulver.Studien undersökte inverkan av effekt, hastighet, avstånd mellan två intilliggandeskanningspass och laserfokusförskjutning, vilket karakteriserades genom olikatyper av beteenden hos smältbadet, inklusive värmeledning, övergång frånvärmeledning till nyckelhål, och nyckelhål. Fokusförskjutningen visade sig ändrasmältbadets läge från nyckelhål till värmeledning. Denna förändring observeradesbåde i experiment utan pulver och i de med pulver. Förändringen beror påbreddningen av laserstrålens punktstorlek samtidigt som samma linjeenergibibehålls. Denna förändring i smältningstyp genom fokusförskjutning kananvändas som en metod för att optimera utforskningen av nya material i PBFLB-processen. Baserat på detta byggdes kuber med pulver med lagertjocklekar på 60 och 90mikrometer, användande olika processparametrar enligt en experimentell designbaserad på en central sammansatt design. Smältning genom värmeledning bidrogtill att minska defekter, minimera bindningsfel och nyckelhålsporositet i proversom byggts med pulver med lagertjocklekar på 60 och 90 mikrometer. Inverkanav processparametrarna och indirekta mått såsom areaenergi på smältbadetsöverlappning, defektnivå och den dominerande formen på defekter presenteras.Optimering av processparametrarna samt identifiering av parameterrymden föratt bygga kuber med minskad porositet undersöks också. / <p>Paper A is to be submitted, and paper C is acceptet and are not included in this licentiate thesis. We do  not have permission to publish paper B in the digital version.</p>

L'objectif de cette thèse est de mettre en évidence l'influence de la microstructure initiale sur le glissement intergranulaire lors du fluage à haute température d'un superalliage polycristallin à base de nickel. Dans ce but, plusieurs microstructures sont obtenues à partir de la microstructure de référence de l'alliage NR6, par application de traitements thermiques spécifiques. L'influence des paramètres microstructuraux sur les déformations locales est ensuite étudiée à l'aide d'une technique de microextensométrie couplée à une analyse par diffraction des électrons rétrodiffusés. Il est ainsi possible de relier microstructure, déformations locales et comportement macroscopique en fluage. Pour la microstructure de référence de l'alliage NR6, la déformation opère principalement par cisaillement des phases γ et γ'. Ce mécanisme est favorable au glissement intergranulaire. L'absence de précipités tertiaires de phase γ' favorise le contournement des précipités secondaires par les dislocations. Ceci permet de réduire le glissement intergranulaire mais est également néfaste pour la résistance à la déformation de l'alliage. La présence de joints de grains dentelés augmente la résistance au glissement intergranulaire mais diminue la résistance à la déformation intragranulaire en favorisant le contournement des précipités. Ainsi la résistance globale à la déformation n'est pas affectée. Enfin, l'augmentation de la taille de grains n'a d'influence ni sur les mécanismes de déformation mis en jeu ni sur l'amplitude du glissement. Cependant, la fraction moins élevée de joints de grains induit une diminution de la contribution du glissement intergranulaire à la déformation globale. / The aim of this study is to highlight the influence of initial microstructure on grain boundary sliding during high-temperature creep of a polycrystalline nickel-based superalloy. To reach this goal, several microstructures are produced from the reference microstructure of NR6 alloy by adequate heat treatments. The influence of microstructural parameters on local deformations is then studied thanks to a microextensometry technique coupled with an electron back-scattered diffraction analysis. It thereby enables linking microstructure, local deformations and macroscopic creep behaviour. In the case of NR6 alloy reference microstructure, deformation occurs mainly by γ and γ' phases cutting by dislocations. This mechanism is grain boundary sliding-favourable. The absence of tertiary γ' phase precipitates promotes secondary precipitates bypassing by dislocations. This results in a reduction of grain boundary sliding but is also harmful to the alloy creep resistance. Grain boundary serration improves grain boundary sliding resistance but diminishes intragranular deformation resistance by favouring precipitate bypassing. Then global deformation resistance is not changed. Finally, grain size increase has influence neither on activated deformation mechanisms nor on sliding amplitude. However, the decrease of grain boundary fraction leads to a reduction of grain boundary sliding contribution to overall strain.

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.