Investigations on post service material showed that Alloy 800H pigtails from methanol producer Methanex have service lives ranging from 3 to 18 years. Because of this variability in service life, Alloy 800H creep performance was assessed and a new criterion for its procurement developed. The current criterion recommends an ASTM grain size of 5 (72µm) or coarser with no consideration given to grain size distribution, grain boundary types, or grain boundary network topology. Results from the investigation showed that this current criterion may produce variations in steady state creep rates of an order of magnitude between ASTM grain size 1 and 5, and a 2.5 times variation in creep ductility. The ability to accurately reveal grain boundaries and assess grain boundary types is fundamental to the identification and quantification of coherent twin boundaries, and the measurement of average grain size and grain size distribution. EBSD mapping has the ability to distinguish grain boundary types using crystal orientation measurement. Grain size measurement from optical micrographs relies on morphological indicators to identify coherent twins. However, it is shown that many of the boundaries observed as straight line morphology on 2D sections did not possess {111} (coherent) interfaces. 3D reconstructions of Alloy 800H revealed the deficiencies in classifying geometry from two-dimensional (2D) sections. Σ3 Crystal volumes can be categorized as lamellar or edge structures. Lamellar structures are characterized by the appearance of parallel Σ3 boundary planes while an edge structure contains a single Σ3 interface. Sectioning plane location alters the perception of morphology. For simple twin structures, the tradition 2D classifications of morphology (complete parallel, incomplete parallel and corner Σ3) may all appear on a section plane from a single lamellar structure.

Cementitious materials such as concrete, cement and gypsum are widely used in construction, as the raw materials of which they are made are abundant on Earth. Such trend is unlikely to change in the coming decades. But these materials suffer from creep. The creep of cementitious materials is a complex issue. On one hand, in cementitious materials creep is often coupled with other phenomena such as drying, hydration and cracking, and can be influenced by various parameters such as temperature, level of stress, water content and mix design. On the other hand, measuring creep by traditional macroscopic creep testing is time-consuming (creep test on concrete is recommended to be carried out over several months in order to provide a reliable characterization of long-term creep) and tedious, since experimental parameters need to be well controlled over extensive periods of time. This thesis studied microindentation at the scale of cement paste or gypsum plaster for the assessment of long-term basic creep properties of cementitious materials, by comparing creep functions obtained by minutes-long microindentation testing with those obtained with macroscopic creep experiments which lasted up to years. For cement paste, the comparison was made at the scale of concrete with the aid of upscaling tools. The study validated that minutes-long microindentation testing can provide a measurement of the long-term creep properties of cementitious materials. With the validated indentation technique, we studied the effect of microstructure (i.e., the distribution and the spatial organization of phases) and of water on long-term basic creep of cementitious materials. The effect of microstructure was studied on materials such as C3S pastes and C2S pastes as well as on compacts of synthetic C-S-H, portlandite (CH) and their mixtures prepared by compaction of powders. For all samples considered, we identified the right micromechanical model that allows predicting the results. The choice of micromechanical model was consistent with microstructural observations. The effect of relative humidity was studied by conditioning and testing some of those materials (i.e., C3S paste, compact of C-S-H, and compact of CH) in various relative humidities ranging from 11% to 94%. Relative humidity had a significant effect on creep: for all materials tested, a greater humidity led to a greater creep. The compact of portlandite was the most sensitive to relative humidity, probably because creep occurs at interfaces between portlandite crystals. For C3S paste, a linear relation was identified between long-term creep properties and water content at relative humidities ranging from 11% to 75%.Finally, we proposed micromechanical models that allow predicting long-term basic creep properties of cementitious materials with a wide range of volume fraction of crystalline phase and over a wide range of relative humidities

For microelectronics used in the low-temperature applications, the understanding of their reliability and performance has become an important research subject characterised as electronics to serve under the severe or extreme service conditions. Along with the impact from the increased miniaturization of devices, the various properties and the relevant thermo-mechanical response of the interconnection materials to temperature excursion at micro-scale become a critical factor which can affect the reliable performance of microelectronics in various applications. Pure indium as an excellent interconnection material has been used in pixellated detector systems, which are required to be functional at cryogenic temperatures. This thesis presents an extensive investigation into the thermo-mechanical properties of indium joints as a function of microstructure, strain (loading histories-dependent) and temperature (service condition-sensitive), specifically in the areas as follows: (i) the interfacial reactions and evolution between indium and substrate during the reflow process (liquid-solid) and thermal aging (solid-solid) stages by taking low-temperature cycling into account; (ii) determination of the effects of joint thickness and the types of substrate (e.g. Cu or Ni) on the mechanical properties of indium joints, and the stress- and temperature-dependent creep behaviour of indium joints; (iii) the establishment of a constitutive relationship for indium interconnects under a wide range of homologous temperature changes that was subsequently implemented into an FE model to allow the analysis of the evolution of thermally-induced stresses and strains associated with a hybrid pixel detector.

Additive manufacturing methods have been developed from rapid prototyping techniques and are now being considered as alternatives to conventional techniques of manufacturing. Stereolithography is one of the main additive methods and is considered highly accurate and consistent. Polymers are used as stereolithography materials and exhibit features such as high strength-to-weight ratio, corrosion resistance, ease of manufacturing and good thermal and electrical resistance properties. However, they are sensitive to environmental factors such as temperature, moisture and UV light, with moisture being identified as one of the most important factors that affect their properties. Moisture generally has an adverse effect on the mechanical properties of polymers. Investigation of the effects of moisture on polymers can be carried out using a number of experimental techniques; however, the benefits of the depth sensing indentation method over bulk tests include its ability to characterise various mechanical properties in a single test from only a small volume of material and the investigation of spatial variation in mechanical properties near the surface. The aim of this research was to investigate the effects of varying relative humidity on the indentation behaviour of stereolithography polymers and to develop a modelling methodology that can predict this behaviour under various humidities. It was achieved by a combination of experimental and numerical methods. Depth sensing indentation experiments were carried out at 33.5 %, 53.8 %, 75.3 % and 84.5 % RH (relative humidity) and 22.5 °C temperature to investigate the effects of varying humidity on the micron scale properties of the stereolithography resin, Accura 60. In order to minimise the effects of creep on the calculated properties, appropriate loading and unloading rates with suitable dwell period were selected and indentation data was analysed using the Oliver and Pharr method (1992). A humidity control unit fitted to the machine was used to condition the samples and regulate humidity during testing. Samples were also preconditioned at 33.5 %, 53.8 %, 75.3 % and 84.5 % RH using saturated salt solutions and were tested at 33.5 % RH using humidity control unit. It was seen that properties such as indentation depth increased and contact iv hardness and contact modulus decreased with increasing RH. The samples conditioned and tested using the humidity control unit at high RH showed a greater effect of moisture than the preconditioned samples tested at 33.5 % RH. This was because the samples preconditioned at high RH exhibited surface desorption of moisture when tested at ambient RH, resulting in some recovery of the mechanical properties. In order to investigate these further, tests were performed periodically on saturated samples after drying. Ten days drying of samples conditioned for five days at 84.5 % RH provided significant, though not complete, recovery in the mechanical properties. These tests confirmed that Accura 60 is highly hygroscopic and its mechanical properties are a function of RH and removal of moisture leads to a significant recovery of the original mechanical properties.

This thesis provides a research into properties of nickel-based single crystal superalloys. The underlying quantitative relationship between alloy chemistry and the important properties have been studied. To design new grade of single crystal superalloys, computational modelling methods have been proposed which build on the findings of composition-microstructure-property relationships. A physical model for the creep deformation of single crystal superalloys is presented, in which the dependence of the kinetics of creep deformation on alloy chemistry is rationalised. The rate-controlling step is considered to be climb of dislocations at the matrix/particle interfaces and their rate of escape from trapped configurations. The effects of microstructural scale precipitate size, geometry and spacing are also studied. A first order estimate for the rate of creep deformation emerges from the model, which is useful for the purposes of alloy design. Three new single crystal superalloys have been isolated using theory-based computational modelling approaches, termed Alloys-By-Design methods. They are (i) an oxidation-resistant low Re-containing alloy with balanced properties, intended for general-purpose gas turbine applications; (ii) an alloy containing 5.6 wt.% Re and 2.6 wt.% Ru suitable for high performance jet engine applications, and (iii) a cheap, corrosion-resistant alloy for power generation applications. The new alloys have been manufactured using investment casting techniques, and their creep and oxidation behaviour evaluated. The multicomponent composition space pertinent to the single crystal nickel-based superalloys has been mapped and searched, by using newly developed numerical algorithms. This allowed compositions of alloys conferring the microstructures needed for optimal properties to be identified, at a resolution of 0.1 wt.%. Databases have been constructed which contain all appropriate compositions available in these systems. When coupled with composition- and microstructure-dependent property models, the databases can be searched to identify new alloys predicted to exhibit the very best properties or combinations of them.

Le béton est un matériau hétérogène complexe dont les déformations comportent une partie différée qui est affectée par un grand nombre de facteurs tels que la température, l'humidité relative et l'évolution de la microstructure. La prise en compte des déformations différées et en particulier du fluage est indispensable dans le calcul des ouvrages en béton tels que ceux destinés à stocker des déchets radioactifs. Ce travail de thèse a pour objectifs : (1) de développer un modèle de fluage simple et robuste pour le béton en faisant appel à la micromécanique et en tenant compte de l'endommagement et des effets thermiques et hydriques ; (2) d'implanter numériquement le modèle développé dans un code de calcul par éléments finis de façon à pouvoir simuler le comportement d'éléments de structure simples en béton. Pour atteindre ce double objectif, le travail est scindé en trois parties. Dans la première partie, le matériau cimentaire est à l'échelle microscopique supposé être constitué d'une matrice viscoélastique linéaire caractérisée par un modèle de Maxwell généralisé et de phases particulaires représentant les granulats élastiques et les pores. Le schéma micromécanique de Mori-Tanaka, la transformée de Laplace-Carson et son inversion sont alors utilisés pour obtenir dans l'espace temporel des estimations analytiques ou numériques de ses paramètres mécaniques et hydromécaniques. Ensuite, le modèle micromécanique de fluage obtenu est couplé au modèle d'endommagement de Mazars via le concept de pseudo-déformations introduit par Schapery. Les paramètres intervenant dans le modèle viscoélastique endommageable ainsi établi sont systématiquement identifiés à l'aide de données expérimentales. Enfin, la prise en compte des effets de la température et de l'humidité relative dans le modèle viscoélastique endommageable est basée sur la méthode du temps équivalent ; l'efficacité de cette approche est démontrée et discutée dans le cas de chargements simples de fluage / Concrete is a complex heterogeneous material whose deformations include a delayed part that is affected by a number of factors such as temperature, relative humidity and microstructure evolution. Taking into account differed deformations and in particular creep is essential in the computation of concrete structures such as those dedicated to radioactive waste storage. The present work aims: (1) at elaborating a simple and robust model of creep for concrete by using micromechanics and accounting for the effects of damage, temperature and relative humidity; (2) at numerically implementing the creep model developed in a finite element code so as to simulate the behavior of simple structural elements in concrete. To achieve this twofold objective, the present work is partitioned into three parts. In the first part the cement-based material at the microscopic scale is taken to consist of a linear viscoelastic matrix characterized by a generalized Maxwell model and of particulate phases representing elastic aggregates and pores. The Mori-Tanaka micromechanical scheme, the Laplace-Carson transform and its inversion are then used to obtain analytical or numerical estimates for the mechanical and hydromechanical parameters of the material. Next, the original micromechanical model of creep is coupled to the damage model of Mazars through the concept of pseudo-deformations introduced by Schapery. The parameters involved in the creep-damage model thus established are systematically identified using available experimental data. Finally, the effects of temperature and relative humidity are accounted for in the creep-damage model by using the equivalent time method; the efficiency of this approach is demonstrated and discussed in the case of simple creep tests

Les modèles basés sur la mécanique des milieux continus prévoient généralement une déformation à la rupture plus élevée, ainsi qu'une durée de vie en fluage beaucoup plus longue que les valeurs observées expérimentalement. Cette thèse met en évidence deux aspects de cette problématique en analysant l’endommagement à l'aide de tomographie in situ à rayons X de synchrotron et reconstruction 3D de la structure polycristalline par polissages successifs.L’endommagement en termes de fraction surfacique des cavités a été identifié dans les couches de reconstructions tomographiques perpendiculairement à l’axe de déformation. L'évolution de la fraction surfacique des cavités a été comparée avec le modèle de prédiction de Cocks et Ashby. Ce dernier surestime la durée de vie en fluage et sous-estime l’état de l’endommagement. L'importance de l'hétérogénéité initiale de l’endommagement et l’effet de localisation de l’endommagement est également souligné. L'amplitude de la plus grande fluctuation surfacique augmente de façon parabolique en fonction de la fraction surfacique moyenne.Une méthode de sectionnement sériel améliorée basée sur la profilométrie de surface a été développée. Elle permet la mesure précise de l'épaisseur du matériau enlevée localement. Les analyses ont montré que l'emplacement des cavités par rapport aux joints de grains et l’orientation cristallographique des grains au voisinage est similaire pour les échantillons déformé par différents mécanismes de fluage. La population relative des cavités de fluage présente aux joints de grains simples est supérieure à celle présente aux joints triples. Les cavités trouvées aux joints triples, cependant, sont plus grandes. / Power law creep damage is one of the most intriguing unsolved phenomena of materials science. Models based on continuum mechanics generally predict a much higher strain to failure, as well as a much longer creep lifetime than experimentally observed values. This thesis highlights two aspects of this problematic by analyzing creep damage in copper using in situ synchrotron tomography and 3D reconstruction of the damaged polycrystal structure by serial sectioning.Damage in terms of the area fraction of voids was first identified in slices of tomographic reconstructions of creep deformed copper. The local and global evolution of cavities area fraction was checked against the Cocks and Ashby model and it was found that the model overestimates creep lifetime and underestimates damage development. The importance of the initial damage heterogeneity and the role of damage localization are also emphasized. It was found that the amplitude of the largest damage fluctuation increases parabolically as a function of cavity’s mean area fraction.An improved serial sectioning method based on surface profilometry was developed, which allows the accurate measurement of the removed local material thickness. The 3D reconstructions enabled identifying the creep voids and the grains of the polycrystal. It was shown that with the exception of the void shape, the relationship between void location at a given grain boundary and crystallographic orientation of the neighbor grains is similar in samples deformed by different creep mechanisms. The relative population of creep voids is higher at simple grain boundaries than at triple junctions. Voids found at a triple boundary, however, are larger.

Les superalliages monocristallins à base de nickel sont couramment utilisés dans la fabrication des aubes de turbines à gaz aéronautiques. En service, ces pièces mécaniques sont soumises à des sollicitations mécaniques et thermiques sévères. La composition chimique et la microstructure de ces superalliages monocristallins ont été optimisées à travers différentes générations d'alliages dans le but de résister au fluage à des températures supérieures à 1100°C. Pour protéger ces matériaux des agressions environnementales (oxydation isotherme et cyclique à très haute température, corrosion à moyenne et haute température), les aubes de turbine sont généralement revêtues d'une couche de NiAlPt ou de MCrAlY (M=Ni, Co). Le procédé de dépôt et les traitements thermomécaniques entrainent la formation d'une zone d'interdiffusion entre le revêtement et le substrat. De plus, la microstructure des différentes zones (le superalliage, le revêtement et la zone d'interdiffusion) évolue en service du fait de l'effet combiné des sollicitations mécaniques et thermiques. De telles évolutions sont susceptibles d'affecter localement les propriétés mécaniques des aubes de turbine. Les revêtements MCrAlY ont fait l'objet de nombreuses études portant sur l'oxydation et la corrosion à haute température. L'abattement des propriétés mécaniques du superalliage du fait de la présence du revêtement a été largement étudié sur le système complet, c'est à dire le superalliage revêtu. Ces études ont eu pour but d'estimer une épaisseur de superalliage qui soit considérée comme non porteuse de la charge, et ce indépendamment de la taille de la zone d'interdiffusion. L'affinement des modèles prédictifs de comportement mécanique et de durée de vie des matériaux requiert une base de données relative aux propriétés locales et à leur évolution au cours du vieillissement. Ces données n'étaient pas disponibles jusqu'à ce jour. Ce travail a donc porté sur la caractérisation microstructurale et mécanique de la zone d'interdiffusion du système MC2 revêtu de NiCoCrAlYTa par co-déposition électrolytique. Des éprouvettes de traction ont été extraites des différentes zones de ce système à gradient de propriétés à l'état de réception et aussi dans des états vieillis avec ou sans contrainte appliquée. Elles ont été ensuite testées mécaniquement à haute température dans des conditions environnementales optimisées de façon à limiter les effets induits par l'oxydation sur le comportement mécanique d'éprouvettes aussi minces. Ces échantillons de 20 à 400 μm d'épaisseur ont été obtenus en utilisant une machine de rodage afin de limiter l'impact de la méthode d'usinage sur l'état de contrainte résiduel. Deux bancs d'essais mécaniques ont spécialement été développés dans le cadre de cette étude pour réaliser des essais de fluage et de traction sur ces échantillons ultra-minces sous atmosphère contrôlée jusqu'à 1200°C. Les résultats obtenus sur ces échantillons minces ont été comparés aux résultats d'essais conduits sur des éprouvettes massives. L'effet « paroi mince » a été exploré parallèlement afin de statuer sur la possibilité d'utiliser ces données pour décrire le gradient de comportement du système. / Monocrystalline nickel based superalloys are the most suitable materials for the design of high performance turbine blades. In service, these mechanical parts undergo both harsh mechanical and thermal solicitations. The chemical composition and also microstructure of these superalloys have been optimized through different generations to resist creep deformation at temperature higher than 1373K. To protect these materials from environment stresses (isothermal and cyclic oxidation at high temperature, intermediate temperature corrosion) blades are generally coated with a NiAlPt or MCrAlY layer (M=Ni, Co). Both deposition process and thermomechanical treatment generate an interdiffusion zone (IDZ) between the coating and the substrate. Moreover, the microstructure of the different strata (superalloy, coating and interdiffusion zone) evolve in service due to the combine effect of high temperature and stress. Such evolutions may locally affect the mechanical properties of turbine blades. MCrAlY coatings have been studied extensively from an oxidation and hot corrosion point of view. The drop of mechanical properties of superalloys because of the presence of coating has been investigated on full system, so that to say the coated superalloy. These study aims to estimate a none bearing thickness of the superalloy independently from the size of the interdiffusion zone. Refinement of predictive models on mechanical behaviour and lifetime of materials require data relative to local properties and their evolution when ageing. These data were not available until now. Hence, this work deals with microstructural and mechanical characterisation of the interdiffusion zone of the system MC2 coated with NiCoCrAlYTa by electrochemical codeposition. Tensile specimens were extracted from the different zones of this functionally graded material on “as received” state and after ageing with and without applied stress. Then, these specimens were mechanically tested at high temperature in optimised controlled atmosphere in order to prevent ultrathin specimens from oxidation effects on the mechanical behaviour. These specimens in a range of 20 to 400μm thick were obtained by use of a lapping machine in order to limit the impact of gritting on residual stress. Two mechanical test rigs were especially designed for this study to perform creep and tensile testing on these ultrathin specimens under controlled atmosphere at temperature up to 1473K. Results obtained from these ultrathin specimens were compared with testing conducted on bulk materials. The “size effect” was explored in parallel so that to conclude on the feasibility of using these data to quantify the behaviour gradient of this system.

Den finkorniga sulfidjorden som finns längs Norrlandskusten är känd för sin stora sättningsbenägenhet och utgör en potentiell miljörisk genom försurning och urlakning av metaller om den inte hanteras rätt. För att förebygga miljörisker och utveckla jordförstärknings- och grundläggningsmetoder måste en ökad kunskap om sulfidjordar tas fram. I ett pågående forskningsprojekt vid Statens Geotekniska Institut studeras sulfidjords kompressionsegenskaper och rekommendationer ska tas fram avseende underlag för sättningsberäkningar. I projektet omfattas ett antal provbankar där ett av dessa områden, Lampen ligger i Kalix i norra Sverige. I detta examensarbete har det utförts numeriska analyser i finita elementprogrammet PLAXIS 2D av sättningar och portryck under en av provbankarna i Lampen och jämförelser görs med tidigare rapporterade fältmätningar. Tre olika delar analyseras i FE-programmet PLAXIS 2D. I den första delen, som är huvuddelen, utvärderas materialmodellernas, Soft Soil (SS) respektive Soft Soil Creep (SSC), förmåga att simulera de uppmätta sättningarna och porövertrycken för en period av cirka ett års belastning av provbank. Den andra delen består av en analys av de två deformationstillstånden, axialsymmetriskt och plant. De två deformationstillståden jämförs med hänsyn till sättningar och portryck. I den tredje delen utvärderas påverkan på simulerade resultat av olika nivåer på grundvattenytan, en variation som har observerats i provområdet i Lampen. Vid en jämförelse av de konstitutiva modellerna noteras som förväntat större sättningar vid användning av SSC-modellen i jämförelse med SS-modellen. SSC-modellen visar även ett högre porövertryck. Vid jämförelse med i fält uppmätta värden noteras att de mest överensstämmande sättningarna erhålls från SS-modellen medan portrycksutvecklingen simuleras bättre, men ändå långt från bra, med SSC-modellen (för simulering med dubbelsidig dränering). Vid analys av deformationstillstånd (axialsymmetriskt kontra plant) noteras en jämnare fördelning av deformationer längs banken vid användandet av axialsymmetriskt tillstånd. Den potentiella brottrörelsen som uppvisas vid släntkrön vid tillämpning av plant deformationstillstånd är inte lika tydlig vid axialsymmetriskt tillstånd. Det axialsymmetriska tillståndet visar även ett lägre porövertryck. Numeriska simuleringar av den varierande nivån på grundvattenytan som observerats i fältmätningar visar vid fallet en lägre antagen grundvattennivå en marginellt mindre sättning.  Potentiella brottrörelser blir inte lika tydliga då den lägre nivån på grundvattenytan simuleras.

The constitutive mechanical behaviour with a focus on creep of Sn-Pb and various Sn-Ag-Cu based Pb-free solders in the 25-150°C temperature range has been studied using nanoindentation and various new meso-scale tests. All alloys have been studied as bulk wave soldering bars, as-received solder balls and solder joints. Ball Grid Array (BGA) solder joints in a typical electronic configuration were manufactured in-house using both Cu and Pd-Ag metallizations. Microstructural characterisation of all configurations used various types of optical and electron microscopy and showed that the solder pad metallization type played a major role in intermetallic compound (IMC) formation. There were comparatively fine and coarse-grained microstructures in both as-received solder balls and BGA solder joints depending on ball diameter. Nanoindentation creep measurements in the stress range 20-500MPa showed that grain boundary sliding occurred together with dislocation glide and dislocation climb in the low temperature (25-50°C) and high temperature (100-150°C) regimes respectively. Smaller grain sizes (<20µm) encouraged grain boundary sliding that enhanced creep. New elevated temperature mechanical tests were developed using the nanoindentation platform to enable testing of entire solder joints in shear and compression, with stresses in the 1E-2 - 3MPa range, more relevant to in-service conditions than those in nanoindentation. Meso-scale spherical indentation creep behaviour in compression on as-reflowed solder balls showed good agreement with that obtained by conventional nanoindentation. However, when BGAs were tested in shear, the solder microstructure had relatively little influence on the creep response, which was significantly less creep resistant than individual phases in the ball obtained by nanoindentation or the ball itself obtained by meso-scale spherical indentation. In shear, the creep conformed to diffusion controlled behaviour and interfacial microstructure was suggested to now control creep response, with the microstructure of the majority of the solder joint playing only a minor role.