Syfte Syftet med föreliggande studie var att undersöka böjhållfastheten hos IPS e.max CAD före och efter termocykling med 10 000 respektive 15 000 cykler. Material och metod Trettio provkroppar framställdes från fem stycken IPS e.max CAD LT-block. Provkropparna var indelade i två testgrupper (GT10 och GT15), och en kontrollgrupp (GK), á 10 provkroppar i varje. Provkropparna utformades enligt måtten L 17,9 ± 0,03 mm x B 2,5 ± 0,03 mm x H 2,5 ± 0,03 mm. Samtliga provkroppar kristalliserades och grupp GK förvarades i rumstemperatur, resterande två grupper, GT10 och GT15 termocyklades i 10 000 respektive 15 000 cykler.Därefter utfördes ett trepunkts böjhållfasthetstest. Resultaten analyserades med One-way ANOVA, Tukey’s test med signifikansnivån α= 0,05 i statistikprogrammet SPSS. Resultat Resultaten visade att det inte fanns någon signifikant skillnad mellan grupp GK och GT10 (p>0,05) respektive mellan grupp GT10 och GT15 (p>0,05). Grupp GT15 hade högst medelvärde (516 MPa) och grupp GK hade lägst medelvärde (450 MPa). Signifikant skillnad fanns mellan grupp GK och GT15 (p<0,05). Grupp GT15 hade en signifikant högre böjhållfasthet (~470-637 MPa) jämfört med grupp GK (~406-494 MPa). Slutsats Inom föreliggande studies begränsningar kan följande slutsatser dras: Termocykling med 10 000 cykler påverkar inte böjhållfastheten, däremot ger ökat antal cykler (15 000) högre böjhållfasthet. / Purpose  The purpose of the present study was to investigate the flexural strength of IPS e.max CAD beforeand after thermal cycling with 10,000 and 15,000 cycles, respectively.  Material and method  Thirty specimens were prepared from five IPS e.max CAD LT blocks, divided into two test groups (GT10 and GT15), and one control group (group GK) (n=10). The specimens were designed with the dimensions L 17.9 ± 0,03 mm x W 2.5 ± 0,03 mm x H 2.5 ± 0,03 mm. All specimens were crystallized and group GK was kept in room temperature, the remaining two groups, GT10 and GT15 were thermocycled with 10,000 and 15,000 cycles respectively. A three-point flexural strength test was performed. The results were analyzed with One-way ANOVA, Tukey's test with a significance level α = 0.05 in the statistical program SPSS.  Results  The results showed that there was no significant difference between groups GK and GT10 (p> 0.05), and between groups GT10 and GT15 (p> 0.05). It was also observed that group GT15 had the highest average (516 MPa) and group GK had the lowest average (450 MPa). There was a significant difference between groups GK and GT15 (p <0.05). Group GT15 had a significantly higher flexural strength (~ 470-637 MPa) compared to group GK (~406-494 MPa).  Conclusion  Within the limitations of the present study, the following conclusions can be drawn:Thermal cycling comprising 10,000 cycles do not affect the flexural strength, however, increasing the number of cycles (15,000) will give higher flexural strength.

Syfte: Syftet med föreliggande in vitro-studie är att undersöka passformen på ett 3D-printat polymerbaserat material för stabiliseringsskenor över tid, framställt i två olika printningsvinklar.  Material och metod: 16 provkroppar tillverkades av Keysplint soft® Clear for Carbon® Printers och delades in i två grupper beroende på printningsvinkel. Åtta provkroppar printades i 0° och åtta printades i 10°. Provkropparna genomgick termocykling på 10 000 cykler och passformen utvärderades med replikatekniken där gruppernas medelvärden jämfördes i fem parametrar mot respektive referensvärde i CAD-inställningen. Statistisk analys gjordes med One-Way ANOVA, Tukey’s test och signifikansnivån sattes till α = 0,05.  Resultat: Signifikant skillnad fanns för grupperna 0° och 0°TC i två av fem parametrar. Det fanns ingen signifikant skillnad före och efter termocykling för provkroppar printade i 10°. Signifikant skillnad hittades i tre parametrar mellan grupperna 0° och 10°. Slutsats: Inom föreliggande studies begränsningar kunde det påvisas att: 3D-printade stabiliseringsskenor med 0° printningsvinkel ger bättre passform än skenor med 10° printningsvinkel. 3D-printade stabiliseringsskenor med 10° printningsvinkel ger bättre passform över tid. / Aim: The purpose of this in vitro study is to evaluate the fit of a 3D-printed polymeric material for splint appliance over time with two different printing angles. Material and method: 16 specimens were manufactured by Keysplint Soft® Clear for Carbon® Printers and were divided in two groups. Eight specimens were printed with a 0° angle and eight printed with a 10° angle. The specimens underwent a thermal cycling of 10 000 cycles and the fit was evaluated by the replica technique. The groups mean values were compared in five parameters against the reference value in the CAD-setting. Statistical analysis was done with One-way ANOVA, Tukey’s test and significance level was set to α = 0,05. Results: Significant differences were found between groups 0° and 0°TC in two out of the five parameters. No significant differences were found before and after thermal cycling for specimens printed with a 10° angle. Significant differences were found in three parameters between groups 0° and 10°. Conclusion: Within the limitations of this study the conclusions are: 3D-printed splint appliance indicates a better fit printed with 0° angle than with 10° angle. 3D-printed splint appliance printed with the 10° angle indicates a better fit over time.

An exhaust manifold of a truck engine is subjected to tough conditions. As the truck is started, operated and shut down, it becomes subjected to thermal cycling up to around 800°C. At such high temperatures, corrosion, fatigue and creep are active degradation mechanisms. As can be imagined, the interplay between the three complicates materials selection. It is desired to have a versatile grade of high durability which is not too expensive. At the moment, a ferritic, ductile cast iron designated SiMo51 is used for the application. However, due to the rough conditions, it is considered to be on the verge of its operational limit. As a consequence, there is an ongoing search for candidate materials. In this study, the ductile cast irons SiMo51, SiMo1000, D5S and the cast steel HK30 have been included. In the past, there have been several studies describing corrosion and fatigue of the cast materials used for exhaust manifolds. However, on the subject of creep of cast materials, little is known. The present study aims to reveal creep tendencies of cast materials and to do it in several ways. More precisely, three creep-testing methods were employed: the conventional constant-load creep-test, the “Sequential tensile test (STT)” and “Stress relaxations with thermal cycling (SRTC)”. The first one is the traditional one. It is tedious, usually lasting months or years. The second one is a tensile test in which the strain rate is changed in sequences as specimen deformation proceeds. Here, the idea is that a slow tensile test is not different from a conventional creep test. In the third one, stress relaxations are provoked as a specimen is thermally cycled in a locked state. Since stress relaxations are a consequence of creep deformation, the relaxation data gathered from isothermal holds can be directly compared to results from the isothermal constant-load creep-test and STT. When thermally cycled in a locked state, the materials display a loop character in σ, ε and T which provides extensive information about the mechanical properties over the selected temperature interval. In a logarithmic Norton plot, the creep strain rate is plotted as a function of stress. By plotting STT-data in such Norton plots, it was shown that the creep behaviour of the included materials is well represented by Norton’s law. Furthermore, it was found that the creep strain rates and stress relaxations, measured during isothermal holds in SRTC, in several cases show perfect coincidence with tensile test data obtained through STT. At 700°C, data from all three tests were inserted in the same Norton plot. At higher stress levels, the SRTC-curve follows the STT-curve and at lower stresses, when the creep regime is entered, it bends down and unites with data obtained by the constant-load creep tests. Additionally, it was seen that a relatively high degree of pre-deformation can give a critical stress below which creep deformation stops completely. / <p>The Financier is Scania CV. </p>

Les pales de turbine Haute Pression des turbines d'hélicoptères sont soumises à des sollicitations cycliques, thermiques et mécaniques, complexes. L'objectif de ce travail est de caractériser l'influence du cyclage thermique sur le comportement et l'endommagement en fluage de systèmes MCrAlY/superalliage à base de nickel et d'étudier les interactions entre le substrat et le revêtement à haute température. Dans un premier temps, des essais de vieillissement et de fluage isothermes ont été menés afin d'évaluer les dégradations environnementales et mécaniques de systèmes superalliage monocristallin CMSX-4/revêtement NiCoCrAlYTa, déposé selon différents procédés (codéposition électrolytique, projection HVOF). Ces essais de vieillissement isotherme et l'analyse microstructurale qui a été réalisée ont notamment permis d'évaluer le pouvoir protecteur des revêtements entre 950 et 1150°C. Des diagrammes d’occurrence de phases représentatifs de l'état de dégradation de ces revêtements ont été construits et ont montré une équivalence des deux procédés vis-à-vis de la protection du superalliage. Les essais de fluage isotherme ont ensuite confirmé cette équivalence et ont constitué une référence pour les essais de fluage cyclés thermiquement. La comparaison des essais de vieillissement et fluage isothermes a également montré que l’épaisseur de la zone d’interdiffusion entre le superalliage et le revêtement était indépendante de l’application d’une contrainte. Dans un second temps, une étude approfondie de l'influence du cyclage thermique sur le comportement en fluage à 1150°C des superalliages a été menée tout d'abord sur le superalliage MC2, pour évaluer l'effet des paramètres qui caractérisent les cycles thermiques (durée du palier à haute température, vitesses de refroidissement, effet de la température basse du cycle). L'effet du cyclage sur la vitesse de déformation et sur la durée de vie à rupture a été confirmé, et le rôle de la répétition des cycles thermiques sur l'accélération prématurée de l'endommagement de la structure du substrat et la déformation accrue a été mis en évidence. Enfin, le comportement en fluage cyclé thermiquement du système CMSX-4/NiCoCrAlYTa déposé par codéposition électrolytique a été caractérisé aux températures 1050 et 1150°C. Pour ces différentes conditions, particulièrement à 1150°C, il a de nouveau été montré sur ce matériau que les séquences rapides et successives de dissolution - re-précipitation de la phase γ' induisaient une accélération et une généralisation dans le substrat de la déstabilisation de la morphologie en radeaux. Dans une moindre mesure, il a également été montré que le cyclage thermique affecte la zone d'interdiffusion plus en profondeur dans le substrat. / Turbine blades of helicopters are subjected to complex thermal and mechanical cycles. The purpose of this work is to characterize the influence of the thermal cycling on high temperature creep behaviour and damage of MCrAlY coating / single crystal nickel-based superalloys systems, and to study the interactions between the superalloy and the coating. Firstly oxidation and isothermal creep tests have been performed to measure the environmental and mechanical resistance of systems made of CMSX-4 superalloy / NiCoCrAlYTa coating deposited by several processes (Tribomet process and HVOF spraying). Microstructure and chemical composition of both coatings were examined after oxidation and creep testing and quite similar observations were made for both coating processes. The combination of phases and chemical analysis after oxidation testing allowed the establishment of an occurrence diagram of phases for both coating processes, according to temperature and duration of exposure. The obtained diagrams seemed similar for both processes. Finally both processes appeared to be equivalent for the protection of CMSX-4 superalloy in isothermal oxidation and creep conditions. Moreover the growth of the inderdiffusion zone between coating and superalloy is independent of the stress. Secondly the influence of thermal cycling parameters on creep properties of the MC2 single crystal nickel-based superalloy has been studied at 1150°C and 80MPa.We have demonstrated that thermal cycling creep was more damaging than isothermal creep in terms of creep lifetime and rates. Furthermore, the number of low temperature incursions and low cooling and heating rates have severe detrimental effect on creep resistance, whereas the low temperature value of the thermal cycle is not significant. These results specify the role of re-precipitation and dissolution of γ’ particles during thermal cycling creep. Finally the effect of thermal cycling on high temperature creep of thin-walled and coated CMSX-4 single crystal superalloy was evaluated by performing thermal cycling and isothermal creep tests at 1050°C and 1150°C. The deleterious effect of thermal cycling on the creep behavior and lifetime has been confirmed, particularly for the condition at 1150°C and 80 MPa. Furthermore, the number of low temperature incursions has severe detrimental effect on creep resistance on account of the rafted microstructure destabilization induced by these sequences. These results confirm the role of re-precipitation and dissolution of γ’ particles during thermal cycling creep. Thermal cycling infers also on destabilization of subcoating zone in the superalloy but this effect seems to be secondary.

L’avion plus électrique demande des modules de puissances de plus en plus performants dans les domaines de la fiabilité et de la maîtrise de la durée de vie restante. Le remplacement des systèmes hydrauliques et pneumatiques par des actionneurs électriques et leurs convertisseurs associés est, aujourd’hui, un moyen efficace de réduire les coûts de maintenance et la consommation de carburant. L’ajout de composantes électriques est également un bon moyen d’augmenter la fiabilité des systèmes. La fiabilité est toujours étudiée à partir de contraintes cycliques accélérées. La tendance actuelle est d’embarquer des fonctions de suivi de l’état de santé dans les modules de puissance pour permettre la prédiction de la durée de vie restante. Cette approche implique des modifications du circuit afin de mettre en place des capteurs et est souvent dédiée à un mode de défaillance en particulier. Cette thèse propose une approche par apprentissage du suivi de l’état de santé de modules de puissance à base de MOSFET en carbure de silicium. Une large étude bibliographique a permis de créer et de réaliser un banc de test instrumenté permettant de mettre en œuvre des défaillances attendues dans les modules de puissance mais aussi d’enregistrer un grand nombre de paramètres électriques au cours de la vie du module. Ces paramètres montrent une évolution au cours du vieillissement du module en fonction des modes de défaillances. Un modèle de réseaux neuronaux s’appuie sur la dérive de ces paramètres pour établir le pronostic de durée de vie restante d’un module de puissance à chaque instant de son utilisation normale / More electrical aircraft requires power modules of higher performances, especially in terms of reliability with a control of lifetime. The replacement of hydraulic and pneumatic systems by electric actuators and their associated converters is the present trend to reduce maintenance cost and fuel consumption. Adding more electric components is also thought as a good way to increase reliability in systems. Reliability is still analysed from accelerated stress cycles. A large volume of data must be obtained in various conditions to assert a pertinent extrapolation of remaining lifetime during operation. A trend is to embed some condition monitoring functions in power modules to help predict the remaining lifetime. This approach is the field of hardware developments with respect to sensors and decorrelation methods but mainly dedicated to one particular failure. This thesis presents a learning approach of silicon carbide MOSFET based power modules condition monitoring. A large literature study has led to the elaboration of a test plan and an instrumented test bench. This test bench allows an accelerated lifespan of power module and an on-line recording of several electrical parameters. These parameters shows a drift according to the power module ageing. A neural network model based on these parameters drifts has been constructed to estimate the remaining useful lifetime of a power module in normal operation

Este estudo in vitro teve como objetivo determinar a infiltração marginal e resistência à remoção por tração de coroas totalmente metálicas, cimentadas com cimento de fosfato de zinco e que foram submetidas à abertura oclusal para tratamento endodôntico. Foram usados 20 dentes molares (Banco Permanente de Dentes Humanos da FOUSP). Os dentes foram fixados sobre uma base acrílica de secção circular e foram torneados configurando preparos para coroas totais com dimensões de altura e diâmetro padronizadas. Coroas metálicas em Ni Cr foram fundidas através da técnica de enceramento direto e cimentadas com cimento de fosfato de zinco com carga axial de 5 Kg por 10 minutos. Os corpos de prova foram divididos em: Grupos Controle GC1 e GC2, que utilizaram os mesmos corpos de prova, e Grupo Experimental (GE). Todos os corpos de prova foram mantidos em água destilada para que não se desidratassem. Os espécimes dos grupos GC1 e GC2 foram mantidos sem nenhuma intervenção e os do grupo GE foram perfurados com broca de carbide de tungstênio, simulando uma cirurgia de acesso endodôntico. As amostras dos grupos GC2 e GE foram submetidas à ciclagem térmica de 700 ciclos entre 5º e 55º C. Em seguida foram mantidos em uma solução de azul de metileno 0,5%, ph 7,2 por 4 horas a 37º C. Foram submetidos ao ensaio mecânico de tração das coroas em uma máquina universal de ensaios Kratos SV 100, regulada para trabalhar a uma velocidade de ensaio de 0,5 mm/minuto. Os resultados obtidos foram submetidos à análise estatística pelos testes t de Student e as infiltrações avaliadas pela correlação linear de Spearman. A análise inferencial dos resultados dos testes de tração demonstrou com um nível de significância p=0,108, entre os grupos GC1 e GC2, e p=0,502, entre os grupos GC2 e GE, não haver diferença estatisticamente significante. As médias dos valores obtidos nos testes de tração e os seus respectivos desvios padrão foram: GC1 13,96+/-4, 48, GC2 11,26+/-2,269 e GE 10,09+/-4,86 (valores em Kgf). A análise visual subjetiva da infiltração nos corpos de prova indicou que o grupo GE apresentou o maior grau de infiltração marginal com presença do corante atingindo o terço oclusal das paredes axiais (mediana dos scores 3). O grupo GC2 apresentou infiltração marginal no terço médio (mediana dos scores 2). O grupo GC1 apresentou infiltração marginal no terço cervical e médio (mediana dos scores 1). / This in vitro study had the objective to determine the marginal microleakage and the retentive strength of totally metallic crowns, cemented with zinc phosphate cement and subjected to occlusal access for endodontic treatment. 20 human molars (Banco Permanente de Dentes Humanos da FOUSP) have been used for the experiment. The teeth were fixed on a circular acrylic section base and were prepared with standardized dimensions. Metallic crowns in Ni Cr were cast with the direct waxing technique and cemented with zinc phosphate cement with vertical load of 5 kg for 10 minutes. The specimens were divided in groups: Group Control 1 (GP1), Group Control 2 (GP2) and Group Experimental (GE). All the specimens were kept on distillated water so that they wouldn’t dehydrate. The specimens of the groups GC1 and GC2 were kept without any intervention and the ones of the group GE were drilled with a tungstein carbide bur, simulating an endodontic access surgery. Next, the samples of groups GC2 and GE were subjected to a thermal cycling of 700 cycles between 5º and 55º C. To verify the existence of micro infiltration, it was used the methylene blue dye test, 0,5%, ph 7,2 for 4 hours at 37ºC. The specimens were subjected to the load of tension in a universal tensile testing machine Kratos SV 100 at speed 0,5 mm/min. Statistical analyses with t tests showed no significant difference between crown retention before and after endodontic access preparation (p=0,108). The mean displacement forces were: GC1 13,96+/-4,48, GC2 11,26+/-2,269 e GE 10,09+/-4,86 (value in Kgf). With the Spearman’s evaluation test the microleakage was measured. The results showed a greater median of score in GE (score 3). The GC2 and GC1 showed median scores 2 and 1 in order.

Este estudo apresenta uma abordagem para a avaliação do comportamento de um ferro fundido branco de alto cromo e um aço ferramenta AISI D2 submetido a ciclos térmicos. Para a realização do estudo foi desenvolvido um procedimento para ensaios de fadiga térmica submetidos a números de ciclos variados, usando para aquecimento um sistema indutivo e para resfriamento um tanque de água. Devido a complexidade dos fenômenos envolvidos, um modelo de elementos finitos foi elaborado para a solução do campo de temperaturas e tensões superficiais atuantes. O controle da tensão superficial atuante foi realizado por meio da mudança de geometria do corpo de prova, sendo esta geometria resultante de teste por simulação computacional. Os corpos de prova foram caracterizados quando a sua microdureza e fração volumétrica de carbonetos antes do ensaio e após ensaio foram caracterizados quanto a sua microdureza, número e profundidade das trincas. O regime de propagação durante os primeiros 50 ciclos foi controlado por mecanismo de fadiga de baixo ciclo, exibindo as maiores velocidade de propagação das trincas e o regime de propagação depois dos 50 ciclos foram controlados por mecanismos de fadiga de alto ciclo. A nucleação das trincas ocorreu predominantemente pela interface matriz/carboneto e pelo próprio carboneto, sendo a propagação das trincas predominantemente pela interconexão de carbonetos fraturados na superfície do material e predominantemente na interface matriz carboneto em camadas mais profundas do corpo de prova. Os resultados obtidos mostraram uma boa correlação entre o ensaio e o modelo numérico, permitindo uma maior confiabilidade para execução do modelo mecânico subsequente. Baseado nos resultados foi possível propor uma metodologia para a avaliação de ambos materiais submetidos a ciclos térmicos. / This study presents an approach to evaluate the behavior of high chromium white cast iron and AISI D2 tool steel submitted at thermal cycles. It was developed a procedure for a thermal fatigue test in different times of cycles were done, using induced heating and water cooling. Due to the complexity of the phenomena involved, a FEM study was performed for solving the temperatures and superficial stresses fields. The control of superficial stress was done by changing the geometry of the test specimens, what was defined by computational simulation. The test specimens were evaluated the microstructure, microhardness and carbides contends before the test. After the test were evaluated microhardness, amount and depth of thermal fatigue cracks. The propagation during the earlier cycles was defined by mechanics of low cycle instead of after 100 cycles that was defined by mechanics of high cycle fatigue. This mechanics was observed by crack velocity analyses in both periods. The nucleation of thermal fatigue cracks initiate mostly at the matrix/carbide interface or at the carbide itself, being the cracks propagation was mainly by the interconnection of fractured carbides at surface and mainly at the interface matrix/carbide in the inner layer of the specimens test. The results obtained showed an adherence between the test and the numerical model, allowed a greater reliability to the subsequent mechanical model. Based on the results was possible propose a methodology for evaluation of both materials subjected a thermal cycles.

La résistance à l'écaillage d'un système barrière thermique est fonction de la composition et microstructure des matériaux constituant le système, ainsi que des procédés utilisés pour son élaboration. Cette thèse s'intéresse à l'influence d'une couche de platine déposée à la surface du dépôt NiCoCrAlYTa (sous-couche) sur le comportement en oxydation du système barrière thermique. Une étude approfondie est d'abord menée afin d'identifier les atouts et points faibles en oxydation cyclique d'un système comprenant un revêtement NiCoCrAlYTa. La formation d'une couche d'oxyde composée non exclusivement d'alumine et l'importante rugosité de la sous-couche, favorisant les défauts au sein de la barrière thermique, accélèrent l'écaillage de la barrière thermique. Parallèlement, la présence de carbures de tantale au sein du dépôt ne suffit pas à stopper le titane qui diffuse depuis le superalliage jusqu'à la couche d'oxyde et dégrade le système. Le platine ayant déjà démontré son effet très bénéfique sur les dépôts aluminures de nickel, il apparaît comme prometteur pour améliorer le comportement en oxydation du revêtement NiCoCrAlYTa. L'étude de son influence débute par une analyse fine de deux sous-couches NiCoCrAlYTa modifié platine : la première comprend un revêtement NiCoCrAlYTa obtenu par co-dépôt électrolytique, la seconde un dépôt NiCoCrAlYTa élaboré par projection plasma sous vide. Cette caractérisation, par diffraction des rayons X et microscopie électronique à balayage et en transmission, met en évidence la présence de martensite en surface du revêtement, conséquence de la diminution de l'activité de l'aluminium par le platine. Elle révèle également la forte influence du procédé utilisé pour l'élaboration du dépôt NiCoCrAlYTa sur la microstructure obtenue après le traitement thermique de diffusion. Des essais d'oxydation isotherme et de préoxydation sont ensuite réalisés sur la sous-couche dont le revêtement NiCoCrAlYTa est élaboré par co-dépôt électrolytique. Les couches d'oxydes formées sont analysées par diffraction des rayons X, spectroscopie Raman et fluorescence. Grâce à l'ajout de platine, qui entraîne l'augmentation de la teneur en aluminium dans la zone externe du revêtement, l'oxydation sélective de l'aluminium est favorisée. Cela se traduit par une diminution de la cinétique d'oxydation et une augmentation de la résistance à l'écaillage de la couche d'oxyde. Cependant, les carbures de tantale se décomposent lors du traitement thermique de diffusion puis lors de l'oxydation, laissant le titane libre de diffuser depuis le superalliage jusqu'à l'oxyde. De l'oxyde de titane est en effet détecté par spectroscopie Raman en petite quantité dans de la couche d'oxyde (avec l'AM3 comme substrat). Un autre point important sur la composition du superalliage est la présence d'élément réactif qui permet de diminuer la croissance de la couche d'oxyde. Concernant les essais de préoxydation, les résultats obtenus indiquent la nécessité d'une faible pression partielle d'oxygène afin de promouvoir la formation d'alumine-a. Le platine, quant à lui, ne favorise pas la formation d'alumine de transition. Des essais d'oxydation cyclique sur des systèmes barrière thermique sont ensuite menés. L'effet bénéfique du platine sur l'oxydation sélective de l'aluminium est confirmé, ce qui entraîne une augmentation de la durée de vie en cyclage. Cependant, la décomposition des carbures de tantale est de nouveau observée. Une diffusion très importante de titane depuis le superalliage jusqu'à l'oxyde est ainsi notée pour les systèmes barrière thermique comprenant une sous-couche modifiée platine avec un dépôt NiCoCrAlYTa obtenu par projection plasma sous vide. Dans le cas de système avec une sous-couche modifiée platine comprenant un dépôt NiCoCrAlYTa élaboré par co-dépôt électrolytique, le problème majeur est la présence de pores en surface et d'une certaine porosité à l'intérieur du revêtement. L'oxydation des pores en surface ainsi que le cyclage thermique provoque la pénétration de l'oxyde puis sa propagation catastrophique dans le revêtement. Les résultats obtenus permettent de dégager les points importants de l'élaboration d'un système barrière thermique. Il est alors recommandé que le superalliage contienne un élément réactif mais peu de titane. Le dépôt NiCoCrAlYTa nécessaire à la fabrication de la sous-couche doit être dense et la préparation de surface, avant et après le dépôt de platine, doit permettre d'obtenir une faible rugosité de surface avant le dépôt de la barrière thermique. Enfin, les paramètres (température, pression partielle d'oxygène, sablage) lors de la première oxydation du système doivent être contrôlés de manière à favoriser la formation d'alumine-a. / The resistance to spallation of a thermal barrier coating system depends on the composition and the microstructure of the materials constituting the system, as well as on the processes used for its manufacturing. This PhD is interested in the influence of a Pt layer deposited on the surface of the NiCoCrAlYTa coating (bond coating) on the oxidation behavior of the thermal barrier coating system. A thorough study is first carried out in order to define the assets and the weak points under cyclic oxidizing conditions of a system composed of a NiCoCrAlYTa coating. The formation of an oxide layer not only composed of alumina and the great roughness of the bond coating, favoring defects within the thermal barrier, speed up the thermal barrier spallation. At the same time, the presence of tantalum carbides within the coating is not sufficient to prevent titanium from diffusing from the bond coating toward the oxide layer and from degrading the system. Platinum having already demonstrated its beneficial effect on nickel aluminide coatings, it seems promising in order to improve the oxidation resistance of the NiCoCrAlYTa coating. The study of its influence starts by a thorough analyses of two Pt-modified NiCoCrAlYTa bond coatings: the first one is composed of a NiCoCrAlYTa coating made by composite electroplating, the second one is composed of a NiCoCrAlYTa coating manufactured by vacuum plasma spray. This characterization, done using X-ray diffraction and secondary and transmission electron microscopy, highlights the presence of martensite at the coating surface, consequence of the decrease in the aluminium activity by platinum. It also reveals the strong influence of the process used to manufacture the NiCoCrAlYTa coating on the microstructure obtained after diffusion heat treatment. Preoxidation and isothermal oxidation tests are then carried out on the systems for which the NiCoCrAlYTa coating is made by composite electroplating. The oxide layers that formed are analyzed by X-ray diffraction, Raman spectroscopy and fluorescence. With Pt addition, that leads to an increase in the aluminium concentration in the external part of the coating, the selective oxidation of aluminium is favored. This results in a decrease in the oxidation kinetics and an increase in the resistance to spallation of the oxide layer. However, tantalum carbides decompose during the diffusion heat treatment and then during the oxidation, making the titanium free to diffuse from the superalloy toward the oxide. Indeed, titanium oxide is identified in small quantity in the oxide layer by Raman spectroscopy (with AM3 as substrate). Another relevant point on the superalloy composition is the presence of reactive elements that leads to a decrease in the oxide layer growth. Concerning the preoxidation tests, the obtained results indicate the necessity of a low oxygen partial pressure so as to promote the a-alumina formation. As for platinum, it does not favor the formation of transient alumina. Cyclic oxidation tests on thermal barrier coating systems are then carried out. The beneficial effect of platinum on the selective oxidation of aluminum is confirmed, that leads to longer lifetimes under thermal cycling. However, the tantalum carbides decomposition is observed once again. A great titanium diffusion from the superalloy toward the oxide is noticed for the thermal barrier coating systems composed of a platinum modified bond coating with a NiCoCrAlYTa deposit made by vacuum plasma spraying. In the case of systems composed of a Pt modified bond coating with a NiCoCrAlYTa deposit manufactured by composite electroplating, the main issue is the presence of pores at the surface and of a porosity within the coating. The pores oxidation at the surface as well as the thermal cycling result in the oxide penetration and then its disastrous propagation within the coating. The obtained results reveal the relevant points concerning the manufacturing of thermal barrier coating systems. It is recommended to use a reactive element containing superalloy that has very little titanium. The NiCoCrAlYTa coating required for the bond coating manufacturing has to be dense and the surface preparation, before and after the Pt deposit, has to lead to a surface with a low roughness before the deposition of the thermal barrier coating. Finally, the parameters during the first oxidation of the system (temperature, oxygen partial pressure, grit blasting), has to be done in order to favor a-alumina formation.

L’augmentation des températures de fonctionnement des turboréacteurs est un axe de développement privilégié dans l’industrie aéronautique. Une solution est l’amélioration des systèmes barrières thermiques. Ce travail de thèse s’intéresse au procédé de projection plasma de suspensions (SPS) qui permet d’envisager une amélioration significative des performances pour les prochaines générations de barrières thermiques, comparé au procédé d’évaporation sous faisceau d’électrons (EB-PVD). Le procédé SPS a en effet démontré une capacité à générer des microstructures colonnaires qui présentent un intérêt pour l’accommodation des contraintes thermo-mécaniques. Une étude microstructurale a conduit à l’identification des paramètres influant sur les variations de morphologies des revêtements (taille de colonnes, distribution de taille, compacité). Deux nuances optimisées en zircone yttriée (YSZ), nommées colonnaire et colonnaire compacte, ont été caractérisées de façon approfondie afin de déterminer les bénéfices du procédé SPS. Ces nuances se caractérisent par une conductivité thermique inférieure à 1 W.m-1.K-1, sur une plage de température allant de 25 à 1100 °C, soit des valeurs avantageuses par rapport à celles des revêtements EB-PVD (1,3 – 1,5 W.m-1.K-1). La durée de vie des dépôts SPS, estimée par cyclage thermique, est au moins équivalente à un dépôt YSZ réalisé par EB-PVD et cyclé en même temps. Le résultat le plus élevé obtenu, supérieur à 2000 cycles, est particulièrement prometteur. La capacité de fonctionnalisation du procédé SPS a par ailleurs permis la réalisation de systèmes multifonctionnels comprenant un dépôt colonnaire YSZ et un dépôt homogène Gd2Zr2O7 en surface. Cette architecture bicouche a pour objectif de pallier les infiltrations chimiques de type CMAS (CaO–MgO–Al2O3–SiO2) qui constituent un frein pour l’augmentation de la température de fonctionnement. Le caractère anti-CMAS du matériau Gd2Zr2O7 mis en forme par SPS a été évalué jusqu’à 1300 °C. / The increase of operating temperature of gas turbine engines is an issue of interest for the aeronautic industry. A solution is the enhancement of thermal insulation properties of thermal barrier coatings (TBCs). The present work is related to suspension plasma spraying process (SPS) that allows to consider significant improvements for the next generation of TBC systems, compared to the currently used process, namely electron beam physical vapor deposition (EB-PVD). Indeed, SPS process can produce columnar microstructures able to provide high thermo-mechanical compliance. A microstructural study led to identify parameters which impacted the coating morphology (column size, distribution, and compaction). Two optimized yttria-stabilized zirconia (YSZ) microstructures were carefully characterized to highlight SPS process advantages. Low thermal conductivities (< 1 W.m-1.K-1) were obtained within a large temperature range (25 °C – 1100 °C), compared to EB-PVD YSZ coatings (1,3 – 1,5 W.m-1.K-1). Thermal lifetime was estimated thanks to thermal cyclic fatigue tests. A similar level of thermal lifetime was reached with SPS coatings compared to EB-PVD one. Some SPS columnar coatings even showed more than 2000 cycles to failure. The ability of SPS to perform multifunctional systems, including a YSZ columnar structure with a homogeneous Gd2Zr2O7 coating on the top, was investigated. This architecture must provide a chemical protection to CMAS (CaO–MgO–Al2O3–SiO2) aggressions. These contaminants would impede the increase of temperature in next generation of gas turbine engines. The anti-CMAS behavior was assessed for SPS Gd2Zr2O7 coatings until 1300 °C.

Les procédés existant pour la fabrication de sous-couches et de systèmes barrière thermique pour les aubes mobiles des turbomachines sont complexes, onéreux, et, de leur reproductibilité dépend la durée de vie de ces systèmes. Cette étude montre la faisabilité d'obtention de sous-couches γ-Ni + γ'-Ni3Al enrichies en platine et de systèmes barrière thermique complets, par l'utilisation du procédé de Spark Plasma Sintering (SPS). Les paramètres du procédé SPS (pression, durée, température et nombre de paliers) ont été ajustés afin de fabriquer les différents types de systèmes. Des améliorations ont été apportées à l'outillage, en vue notamment de mieux appréhender la température de la pièce lors du cycle thermique et, d'empêcher la formation de carbures. Les propriétés microstructurales des revêtements obtenus sont caractérisées et mises en relation avec les paramètres d'élaboration. De plus, les propriétés d'usage (cinétique d'oxydation, résistance au cyclage thermique et à la corrosion par les aluminosilicates fondus, CMAS, conductivité thermique) ont été évaluées. Un large domaine de composition de sous-couches a pu être exploré, notamment par l'addition, par pulvérisation cathodique, d'éléments réactifs (Hf, Y, Si) et d'autres éléments (Ag, Au, Cu) ayant un effet sur le domaine de stabilité de la phase γ'. La possibilité de réaliser des systèmes barrière thermique mono et bi-couches céramiques en une seule étape par le procédé SPS est également démontrée. Un mode d'endommagement spécifique des systèmes barrière thermique élaborés par SPS a été mis en évidence lors d'essais de cyclage thermique et interprété avec l'aide de simulations numériques par éléments finis. Les nombreuses compositions et architectures réalisées au cours de cette étude, sont un encouragement à poursuivre les améliorations apportées au procédé pour l'obtention de systèmes plus complexes et plus fiables. / Fabrication of bond coatings and thermal barrier coating systems for aircraft engine turbine blades and vanes, rely on complex and costly processes, and the lifetime of the systems highly depends on their reproducibility. This work demonstrates the feasibility of platinum rich γ-Ni + γ'-Ni3Al bond coatings and complete thermal barrier coating systems using the Spark Plasma Sintering (SPS) process. Processing parameters (pressure, number, temperature and duration of dwells) have been finely tuned to fabricate the different types of systems. Some necessary adjustments to the equipments have been made to prevent the specimens from pollution, and to better control the samples temperature, and are discussed. The microstructure characteristics and their relation with process parameters have been investigated. Properties such as oxidation kinetics, thermal cycling resistance and CMAS (molten aluminosilicate) corrosion are evaluated. Physical vapor deposition have been used for bond coat doping with reactive elements (Hf, Y, Si) and elements that extend the γ' phase stability domain (Au, Ag, Cu). The possibility to fabricate complete thermal barrier coating systems with a mono or a bi-ceramic top coat layer in a single step is demonstrated. SPS thermal barrier coating systems exhibit a singular spalling behavior during thermal cycling. A finite-element numerical model has been developed and allows its understanding. The versatility of the SPS process has allowed the fabrication of a large number of bond coat compositions and thermal barrier coatings architectures. There is a strong incentive in developing this process for fabricating more reliable and competitive systems.