Creep resistance is an important design criterion at high temperatures especially when continuous attempts are made to increase the efficiencies by increasing the operating temperatures. Alumina is an important high temperature material and in addition to that it is used in wide variety of applications such as substrates for electronic packaging, spark plugs, envelopes for sodium vapour lamps, cutting tools (when reinforced with silicon carbide) and in artificial joint prostheses. Studies on creep in alumina. have started as early as 1961. There are differing mechanisms proposed to explain the creep behaviour of alumina in the literature, but until now there is no any unanimous decision as to what the rate controlling mechanism is. Magnesia doped at ppm levels can produce significant changes in the microstructure of alumina, the most important consequence of that being the grain growth inhibition, which renders alumina superplastic. However, in a stoichiometric oxide like alumina, small impurities can create extrinsic defects which would change the diffusivities and creep rates. Therefore the background impurities in alumina should be kept to a minimum, if small dopant effects have to be studied. The present study was undertaken making use of high purity alumina powder and comparing the grain growth and creep properties of pure and magnesia doped alumina, especially since no such investigation was carried out in the recent past with high purity alumina. Pure alumina was processed by cold compaction followed by cold isostatic pressing (CIP) and pressureless sintering in air at 1773 K for 1 hour. Magnesia doped alumina was prepared by calcining a mixture of alumina and magnesium nitrate at 973 K for 2 hours followed by cold compaction, CIPing and pressureless sintering in air at 1773 K. Both pure and magnesia doped alumina were further annealed at 1873 K for various times to get grain sizes in the ranges of 1-5 μm. Grain growth kinetics of pure and magnesia doped alumina were studied at 1823 and 1873 K. The parameter Kg which quantifies the mobility of the grain boundary was got. It was found that Kg had decreased in the magnesia doped alumina (in comparison with pure alumina) by a factor of about 3 to 4 which was marginal and insignificant. The grain sizes followed a log normal distribution in both the cases, indicative of normal grain growth. Creep studies were conducted on pure and magnesia doped alumina in three modes, namely, constant stress, temperature jump and stress jump test. The temperature range used was 1673 to 1773 K and the stress range used was 10 to 100 MPa. The creep parameters were found to be n~1.6, p~3.7 and Q-545 kJ mol"1 for pure alumina and n~l .3, p~3.0 and Q~460 kJ mol-1 for magnesia doped alumina. The creep rates in the case of magnesia doped alumina were found to have increased by a factor of 2 to 3, in comparison with pure alumina. The increase in creep rates were found to be insignificant. The creep data were analyzed and the possibility of the dislocation and interface reaction controlled creep mechanisms were ruled out since they were inconsistent with the data. It was found, from creep parameters and the comparison of theoretical Coble and Nabarro-Herring creep rates with the experimental rates, that Coble creep might be rate controlling. The activation energy values suggested that aluminium ion diffusing along grain boundary might be the rate controlling species. However, when the theoretical creep rates considering various species were compared, the rate controlling species turned out to be oxygen ion diffusing along the grain boundary.

Grade 91 (Gr.91) is a common structural material used in boiler applications and is favored due to its high temperature creep strength and oxidation resistance. Under cyclic stresses, the material will experience creep deformation eventually causing the propagation of type IV cracks within its heat-affected-zone (HAZ) which can be a major problem under short-term and long-term applications. In this study, we aim to improve this premature failure by performing a computational thermodynamic study through the Calculation of Phase Diagram (CALPHAD) approach. Under this approach, we have provided a baseline study as well as simulations based on additional alloying elements such as manganese (Mn), nickel (Ni), and titanium (Ti). Our simulation results have concluded that high concentrations of Mn and Ni had destabilized M23C6 for short-term creep failure, while Ti had increased the beneficial MX phase, and low concentrations of nitrogen (N) had successfully destabilized Z-phase formation for long-term creep failure.

L'objectif de notre travail de développer des multi-matériaux de type sandwich acier/polymère/acier destinés au secteur automobile en vue de l'allègement des structures. Ce nouveau matériau doit satisfaire plusieurs critères, à savoir: i) grande déformabilité à froid en vue de l'emboutissage, ii) tenue au fluage à haute température (T=200°C, étape de cataphorèse), iii) tenue en milieu agressif (chaud, humide, brouillard salin). De plus, l'adhésion polymère-métal doit être maîtrisée en vue d'éliminer les phénomènes de délamination lors de l'emboutissage des tôles. Ce sandwich doit être réalisable sur une ligne industrielle dont la température maximale de complexage est limitée à 200°C. Si une solution à chacun de ces points particuliers peut être facilement apportée, la réponse à l'ensemble de ces critères par une formulation unique est beaucoup plus complexe. Nous nous sommes focalisés sur une formulation permettant de répondre au critère de tenue au fluage pour des températures supérieures à 200°C mais dont l'adhésion à chaud sur le métal (étape de complexage sur la ligne industrielle) doit être à inférieure à cette même température de 200°C. Pour cela nous avons développé une formulation à base de polymères immiscibles polyamide 11/polyoléfine fonctionnalisée anhydride maléique compatibilisés in-situ. Nos travaux ont donc porté sur l'optimisation de cette formulation, via le contrôle de la morphologie en vue de l'élaboration d'un film ayant les caractéristiques d'un fluide polymère à contrainte seuil d'écoulement tout en ayant les propriétés d'adhésion adéquate / The aim of this work is to develop multimaterials such as steel/polymer/steel composites for weight savings in automotive industry. To fully take advantage of properties of both steel and polymer materials, adhesion steel-polymer must be well controlled. Moreover, the composite must be compatible with processing on the industrial line and last not least, the structure must be flow resistant during the cataphoresis step (Painting process at 200°C for 30 minutes). This last condition is essential and our work will focuse on the development of compatibilized polymers blend made of polyamide 11 and polyolefin grafted maleic anhydride with yield stress properties. We successfully optimize the formulation via morphological control in order to develop a yield stress fluid with good adhesive properties

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L’objectif de ce travail est d’améliorer la durée de vie en fluage d’un alliage résistant à haute température. L’alliage étudié, nommé « C », appartient à la classe des aciers austénitiques de type HP utilisés pour la fabrication des tubes de reformage. L’évolution microstructurale de l’alliage « C » a été étudiée dans une vaste gamme de températures, s’étendant de 700 à 1040°C pour des temps de vieillissement allant jusqu’à 1000 h. La caractérisation de ces états vieillis a été réalisée au moyen de la microscopie électronique (MEB-FEG, MET) et de la diffraction des rayons X. L’accent a été mis sur une caractérisation fine de la précipitation secondaire présente Ces résultats ont ensuite été utilisés afin d’identifier les conditions thermiques optimales pour l’affinement de la précipitation en vue d’amélioration du comportement macroscopique de l’alliage. La cinétique de précipitation a été modélisée à l’aide du logiciel PRISMA ThermoCalc. Un bon accord entre la simulation et les mesures expérimentales a pu être obtenu.Dans la gamme de températures étudiée, la précipitation secondaire est majoritairement constituée de deux carbures : M23C6 (M=Cr, Fe) et NbC. En condition de service (980°C), la croissance du M23C6 est rapide. La coalescence des précipités survient dès 200 h de vieillissement. Nous avons prouvé qu’un vieillissement à des températures plus basses (700-750°C) permet d’affiner cette précipitation. De plus, notre étude a montré l’efficacité d’un prétraitement à des températures basses, effectué avant la mise en service du matériau à 980°C. Une nette amélioration de la résistance en fluage dans des essais accélérés a été obtenue pour l’alliage « C » ayant subi le prétraitement cité ci-dessus. Outre l’affinement et le retardement de la coalescence du M23C6, la présence d’une précipitation nanométrique du NbC sur des lignes de dislocations est probablement à l’origine de cet effet. / The purpose of this work is to optimise the microstructure of a creep-resistant alloy of the type HP, called “C” (industrial denomination). These austenitic steels are used for the manufacture of reformer tubes. The microstructural evolution of the alloy "C" has been studied in a wide range of temperatures, ranging from 700 to 1040 °C for aging times up to 1000 h. The characterization of these aged states was performed using electron microscopy (FEG-SEM, TEM) and X-ray diffraction, with emphasis on a detailed characterization of this secondary precipitation. This knowledge was then used to identify the optimal thermal conditions for the refinement of precipitation to improve the macroscopic behaviour of the alloy. The precipitation kinetics was modelled using the PRISMA ThermoCalc. A good agreement between simulation and experimental measurements has been obtained.In the studied range of temperature, the secondary precipitation consists mainly of two carbides M23C6 (M = Cr, Fe) and NbC. In the service conditions (980°C), the growth of M23C6 is fast. The coalescence of the precipitates starts after only 200h of aging. Aging at lower temperatures (700-750°C) refines this precipitation. Our study showed the efficacy of pre-treatment of the alloy at low temperatures, before the service of the material at 980°C. In the alloy "C", treated in such conditions, a significant increase in creep resistance was obtained in accelerated testing. In addition to refinement of the secondary precipitation and delaying the effects of coalescence of M23C6, the presence of a nanoscale precipitation of NbC on dislocation lines is probably the origin of this effect.