Le volcan Kilauea, Hawaï, est probablement le système magmatique basaltique actif le plus étudié sur Terre, et représente donc un site privilégié pour l'étude des processus de solidification basaltique en milieu naturel. Une meilleure compréhension de la solidification magmatique est d'importance majeure dans le raffinement de modèles expliquant le dynamisme des chambres magmatiques, et son étude détaillée est susceptible de grandement améliorer notre connaissance de l'évolution globale des systèmes magmatiques. Dans ce contexte volcanique, les lacs de lave offrent une rare opportunité d'étudier directement la solidification magmatique et peuvent être considérés, en première approximation, comme des analogues superficiels de petites chambres magmatiques. Le but premier de ce doctorat est de déterminer et quantifier les principaux processus de solidification magmatiques à l'œuvre dans la genèse des basaltes tholéiitiques. Ce travail s'articule autour du minéral olivine comme composant central. Dans les deux premiers chapitres, l'approche est double, texture et géochimie, mais l'emphase porte sur l'aspect textural dont l'analyse de la distribution de la taille des cristaux (CSD) est la composante phare. Ce travail a été réalisé sur les laves produites par les éruptions de 1969-1974 (Mauna Ulu) et 1959 (Kilauea Iki) du volcan Kilauea. L'étude des coulées de lave produites par l'éruption du Mauna Ulu permet de mieux comprendre les processus actifs de solidification dans tout le système magmatique superficiel (la "tuyauterie") de l'édifice. L'étude du lac de lave Kilauea Iki renseigne quant à elle sur la solidification en système semi-fermé en sub-surface. Dans un dernier temps, il est question d'évaluer plus en détail l'influence de la déformation magmatique sur la structure interne des olivines, et de la quantifier, en utilisant une technique in situ récente de micro-diffraction des rayons X. Chacun des trois chapitres de cette thèse est un article publié ou destiné à la publication dans une revue scientifique internationale. L'article 1 présente les résultats en éléments majeurs et traces (roche totale), les compositions de l'olivine, et les CSDs de 11 échantillons de laves du Mauna Ulu. Les variations chimiques en roche totale sont interprétées comme étant partiellement produites par addition d'olivine dans le système magmatique. Les profiles CSD suggèrent qu'au moins deux populations d'olivines interviennent : (1) une population d'âges 3-40 ans, caractérisée par une faible densité de "gros" cristaux et des pentes CSD relativement faibles ; et (2) une population d'âges 1,5-15 ans, marquée par une forte densité de petits cristaux et des pentes CSD plus fortes. La gamme de compositions de l'olivine suggère que ces cristaux se sont formés à partir de magmas différents, probablement reliés par crystallisation fractionnée. La présence d'olivines déformées de toutes tailles couvrant la totalité de la gamme de compositions, montre que la population 1 provient principalement de la désintégration et assimilation d'un cumulat déformé. Cette population d'olivines représente un composant magmatique cumulatif précoce qui a subi du mûrissement textural. A l'inverse, la population 2 représente un composant magmatique tardif formé dans la région sommitale de stockage de magma. Nos résultats sont en accord avec l'hypothèse que ces deux composants magmatiques ont suivi deux trajets différents avant d'alimenter l'éruption du Mauna Ulu. Le magma contenant les olivines déformées aurait transité le long du décollement basal sous le Kilauea, puis remonté verticalement par des conduits de type "pipe" sous le rift du Mauna Ulu. Le magma contenant la plupart des olivines non déformées aurait quant à lui transité vers le réservoir sommital à travers le conduit magmatique principal, puis le long de la rift zone où les magmas se seraient finalement mélangés dans de petites chambres magmatiques satellites. La présence de fines zonalités inverses à la bordure de certains cristaux suggère que le mélange s'est fait juste avant l'éruption. L'article 2 présente les compositions et CSDs d'olivine provenant de scories et d'échantillons de forage (0-90 m de profondeur) du lac de lave Kilauea Iki. Trois populations d'olivines sont distinguées sur la base de leur composition en forstérite (Fo) : (1) une population riche en Fo (Fo85-88) ; (2) une population intermédiaire (Fo77-81) ; et (3) une population mineure appauvrie en Fo (Fo72-76). Les populations 1 et 2 sont composées à la fois de cristaux déformés et non déformés. La troisième population pourrait résulter d'une phase de recroissance tardive. Dans les 60 derniers mètres du lac, l'olivine est moins riche en Fo et la proportion de cristaux déformés augmente. Ces observations laissent penser à l'existence d'une stratification minéralogique et chimique verticale dans le lac de lave. L'analyse CSD a permis d'estimer les temps de résidence des olivines dans le magma, 1-60 ans, valeurs qui sont en accord avec les estimations préexistantes. Les CSDs sont globalement uniformes eu égard à la profondeur. Cependant, certaines caractéristiques spécifiques ressortent. Ainsi, les CSDs courbées sont considérées comme évidence de mélange de magmas ou de cristaux. L'inversion de pente aux petites tailles de la plupart des CSDs du lac de lave est interprétée comme résultant du mûrissement. Les résultats de la modélisation CSD suggèrent que la décantation / sédimentation des olivines et la convection à grande échelle ne sont pas significatives dans l'évolution du lac de lave. Enfin, la stratification verticale du lac peut être expliquée de différentes façons. Il peut s'agir d'une caractéristique originelle, résultat de la stratification de la chambre magmatique source. Cependant, plusieurs évidences montrent que le magma du lac a été fortement brassé pendant toute la durée de l'éruption ; cette première hypothèse n'est donc pas crédible. Le remplissage par la base du lac durant l'éruption serait une autre hypothèse à même d'expliquer cette stratification. Cependant, il nous manque encore de quoi définitivement valider cette théorie. L'article 3 présente l'analyse microstructurale in situ par micro-diffraction des rayons X (µXRD) d'olivines déformées et non déformées provenant d'une sélection d'échantillons préalablement étudiés dans les articles 1 et 2. Cette étude utilise une technique innovante, non destructive, peu coûteuse et rapide à mettre en œuvre permettant de recueillir des informations sur la structure interne des cristaux, ainsi que le mode et l'intensité de déformation. Les résultats ont permis de valider les observations pétrographiques de déformation faites à l'aide du microscope. Cette analyse µXRD a aussi permis de confirmer la présence de déformation pour toutes les tailles de grains d'olivine, sans corrélation simple avec leur chimie, et de quantifier cette déformation. Cette technique ne permet cependant pas une estimation simple des conditions pression-température de déformation ou de formation des cristaux, ni d'apporter d'informations sur l'histoire magmatique. Il a cependant été possible de fixer un seuil quantitatif au-delà duquel toute olivine est déformée de façon significative : full width at half maximum (FWHM) > 1°.

Ce travail présente deux approches pour la modélisation des structures de grains et de la ségrégation chimique associée à l'état de fonderie après solidification. La première approche est de développer un modèle basé sur une description semi-analytique des couches de diffusion chimique dans la phase solide et à l'extérieur des enveloppes des grains. L'originalité de ce modèle réside dans la prise en compte de la surfusion de germination des structures dendritique et eutectique. Nous avons appliqué le modèle développé aux gouttes solidifiées par lévitation électromagnétique (EML) et dont la germination de la structure primaire s'est produite spontanément. La technique EML est utilisée comme modèle expérimental pour produire des échantillons sphériques d'alliage aluminium–cuivre (Al-Cu) a différentes compositions nominales de cuivre. Pour chaque échantillon, nous avons étudié le cas d'une germination spontanée et le cas d'une germination déclenchée. Plusieurs degrés de surfusion ont été mesurés avant la germination des structures dendritique et eutectique. Des investigations expérimentales ont été menées pour caractériser une section centrale de chaque échantillon. Un microscope électronique à balayage (MEB), équipé d'un capteur rayon X, a été utilise pour l'analyse dispersive en énergie. Un ensemble complet de données a été généré pour chaque échantillon a travers des cartes de distribution du cuivre, de la structure eutectique et de l'espacement interdendritique secondaire. Le modèle permet une prédiction quantitative de la fraction de structure eutectique en accord avec les mesures effectuées et cela grâce à la prise en compte de la surfusion de germination eutectique. L'accord avec les mesures expérimentales est dû à la prise en compte de l'effet de la surfusion et de la recalescence eutectique. Dans la seconde approche, un modèle numérique 2D couplant Automate Cellulaire (CA) – Eléments Finis (FE) est développé pour la prédiction de la variation de la température et des cartes de ségrégation mesurées pour les échantillons Al-Cu. Un modèle de micro-ségrégation a été intégré dans chaque cellule de l'automate. Ce modèle permet de prendre en compte la surfusion de la germination de la phase primaire ainsi que la diffusion du soluté dans la phase solide. Les longueurs caractéristiques de diffusion ont été exprimé en fonction des espacements interdendritiques primaires et secondaires. Les équations de conservation d'énergie, de masse et de quantité de mouvement sont résolues par la méthode des éléments finis. Un nouveau schéma de couplage entre l'automate cellulaire et les éléments finis a été développé pour permettre l'adaptation du maillage. Un estimateur d'erreur géométrique a été intégré pour le contrôle de la taille et l'orientation des mailles afin d'optimiser la résolution par la méthode des éléments finis. L'application du modèle 2D CAFE a permis une compréhension avancée des résultats expérimentaux. Ce modèle a aussi été appliqué à la solidification d'une cavité rectangulaire d'un alliage étain-plomb. Les capacités du modèle pour l étude des transferts d'énergie et de masse aux échelles micro et macro ont été mise en évidence par le bon accord entre ces perditions et les mesures expérimentales (des cartes de température, de la macro–ségrégation et des structures de grains).

Experiments on the production of porous metallic materials were performed on Fe-base and Al-base alloys. The method involves dissolution of gases in the liquid state and solidification at various cooling rates. The alloy compositions were selected to induce solidification of primary particles intended to control the pore distribution. For the Fe-base alloys, nitrogen was introduced into the melt by dissolution of chromium nitride powder. Fe-Cr-Mn-Si-C alloys featuring M7C3 carbide particles were selected. For the Al-base alloys, hydrogen gas was dissolved into the melt by decomposition of water vapor. Al-Ti and Al-Fe alloys featuring primary Al3Ti and Al3Fe intermetallic particles, respectively, were considered. In the Fe-base alloys, a homogeneous distribution of gas pores through the specimens’ volume was obtained at high cooling rate (water quenching) and after introduction of external nucleating agents. In the case of the Al-base alloys, a good pore distribution was observed at all cooling rates and without addition of nucleating agents. Calculations of the variation of nitrogen (respectively hydrogen) solubility based on Wagner interaction parameters suggest that pore nucleation and growth occur during precipitation of the primary particles (M7C3 carbides, Al3Ti or Al3Fe intermetallics), due to composition changes in the melt and resultant supersaturation with gas atoms. Microscopic analyses revealed that the primary particles control the pore growth in the melt and act as barriers between adjacent pores, thereby preventing pore coalescence and promoting a fine pore distribution. Uniaxial compression testing of the porous Al-Ti and Al-Fe materials showed the typical compressive behavior of cellular metals. Further work is needed to improve the quality and reproducibility of the porous structures which can possibly be used in energy absorption or load-bearing applications. As a corollary result of the quenching of hypereutectic Fe-Cr-Mn-Si-C alloys in the experiments of synthesis of porous metals, a homogeneous featureless structure was observed in some parts of the samples, instead of the equilibrium structure of M7C3 and eutectic phases. Subsequent investigations on rapid solidification of Fe-base alloys at various alloy compositions and cooling rates led to the formation of a single-phase structure for the composition Fe-8Cr-6Mn-5Mo-5Si-3.2C (wt.%), at relatively low cooling rates (≈103 K/s) and for large sample dimensions (2.85 mm). The single phase, which is likely to be the hcp ɛ-phase, was found to decompose into a finely distributed structure of bainite and carbides at ≈600 °C. The annealed structure showed very high hardness values (850 to 1200 HV), which could be exploited in the development of high-strength Fe-base materials. / QC 20100809

The objective of this research is to increase the understanding of the solidification behaviour of some industrially important wrought aluminium alloys. The investigation methods range from direct investigations of as-cast ingots to laboratory-scale techniques in which ingot casting is simulated. The methods span from directional solidification at different cooling rates to more fundamental and controlled techniques such as DTA and DSC. The microstructure characteristics of the castings have been investigated by optical and Scanning Electron microscopy. Hardness tests were used to evaluate the mechanical properties. The effects of adding alloying elements to 3XXX and 6XXX aluminium alloys have been studied with special focus on the effects of Zn, Cu, Si and Ti. These elements influence the strength and corrosion properties, which are important for the performance of final components of these alloys. Solidification studies of 0-5wt% Zn additions to 3003 alloys showed that the most important effect on the microstructure was noticed at 2.5 wt% Zn, where the structure was fine, and the hardness had a maximum. Si addition to a level of about 2% gave a finer structure, having a relatively large fraction of eutectic structure, however, it also gave a long solidification interval. The addition of small amounts of Cu, 0.35 and 1.0 wt%, showed a beneficial effect on the hardness. Differences have been observed in the ingot surface microstructures of 6xxx billets with different Mg and Si ratios. Excess Si compositions showed a coarser grain structure and more precipitations with possible negative implications for surface defect formation during DC casting. The comparison of alloys of different Ti content showed that the addition of titanium to a level of about 0.15 wt% gave a coarser grain structure than alloys with a normal Ti content for grain refinement, i.e. < 0.02 wt%, although a better corrosion resistance can be obtained at higher Ti contents. The larger grain size results in crack sensitivity during DC casting. A macroscopic etching technique was developed, based on a NaOH solution, and used in inclusion assessment along DC cast billets. Good quantitative data with respect to the size and spatial distribution of inclusions were obtained. The results from studied billets reveal a decreasing number of inclusions going from bottom to top, and the presence of a ring-shaped distribution of a large number of small defects in the beginning of the casting. The present study shows how composition modifications, i.e. additions of certain amounts of alloying elements to the 3xxx and 6xxx Al alloys, significantly change the microstructures of the materials, its castability, and consequently its mechanical properties / QC 20100901

Melt flow plays an important role in directional solidification of multicrystalline silicon influencing the temperature field and the crystallization interface as well as the transport of impurities. This work investigates the potential of a traveling magnetic field (TMF) for an active control of the melt flow. A system of 3D numerical models was developed and adapted based on open-source software for calculations of Lorentz force, melt flow, and related phenomena. Isothermal and non-isothermal model experiments with a square GaInSn melt were used to validate the numerical models by direct velocity measurements. Several new 3D flow structures of turbulent TMF flows were observed for different melt heights. Further numerical parameter studies carried out for silicon melts showed that already a weak TMF-induced Lorentz force can stir impurities near to the complete mixing limit. Simultaneously, the deformed temperature field leads to an increase of the deflection of crystallization interface, which may exhibit a distinct asymmetry. The numerical results of this work were implemented in a research-scale silicon crystallization furnace. Scaling laws for various phenomena were derived allowing a limited transfer of the results to the industrial scale.

L'estudi de la formació de microstructures en processos de solidificació té importants aplicacions científiques i tecnològiques. L'aparició d'aquestes estructures determina les propietats elèctriques i mecàniques del material solidificat, i té per tant un important interès tecnològic. La majoria d'aquestes estructures tenen el seu origen en una desestabilització morfològica de la interfase sòlid-líquid que es produeix a mesura que el front avança. Per aquest motiu, l'estudi del comportament dinàmic de la interfase resulta essencial per entendre els mecanismes que intervenen en la creació d'aquests patrons. Els processos de solidificació solen descriure's mitjançant problemes de contorn mòbil. Aquestes formulacions consten d'equacions per a la difusió del calor i de massa en les fases sòlida i líquida, que s'han de resoldre imposant l'acompliment de diverses condicions de contorn mòbils a la interfase. Els problemes de contorn mòbil, malgrat contenir tots els elements que intervenen en la dinàmica i ser de molta utilitat en l'àmbit de l'enginyeria, requereixen un cost computacional que no permet simular sistemes reals en règims interfacials complexos. Els mètodes de camp de fase (phase-field methods), van aparèixer a principis dels anys vuitanta com una eina computacional que permetia l'estudi de fenòmens interfacials de caire general. Aquests mètodes descriuen la forma de la interfase mitjançant un camp continu que pren valors diferents i constants en les dues fases. La dinàmica d'aquest camp és llavors acoblada al camp de difusió de calor o massa que determina l'avanç del front de solidificació. Un dels avantatges d'aquests mètodes és que la seva simulació no requereix d'algorismes de seguiment de la interfase (front tracking algorithsms). És ben conegut que les característiques principals de les microestructures en solidificació, es determinen durant els transitoris inicials en els que els corrents de massa i calor s'adapten a la evolució dinàmica del front. Un dels objectius en aquesta tesi és el de fer servir mètodes de camp de fase per descriure de forma quantitativa aquests transitoris. Per comprovar la validesa del nostre procediment, es realitza una comparació quantitativa entre els resultats numèrics obtinguts i diferents prediccions analítiques derivades del problema de contorn mòbil. Per un altra banda, la desestabilització del front es veu afectada per la presència de fluctuacions al sistema. Aquestes pertorbacions microscòpiques poden tenir el seu origen a les fluctuacions termodinàmiques internes, o bé ser conseqüència de imperfeccions experimentals que actuen com a font externa de soroll. El segon objectiu d'aquesta tesi és la introducció de fluctuacions en mètodes de camp de fase, de forma que es pugui estudiar l'amplificació dinàmica de les pertorbacions microscòpiques que acaben donant lloc a estructures macroscòpiques. Per finalitzar, analitzem el problema de la selecció en solidificació direccional. Estudiem els règims lineal i no-lineal, tot determinant les condicions, el moment i la forma en que apareixen les estructures dendrítiques i cel·lulars. / Crystal growth is a non-equilibrium process which involves physical mechanisms at very different scales. When a solidification front advances, mass and heat diffusion processes are combined with interfacial phenomena like capillarity or kinetic attachment. A complex interplay between these mechanisms gives rise to complex interfacial structures like snowflakes or cellular patterns. The formation of microstructures in solidification has both a scientific and a technological interest. On one hand, the study of the different interfacial structures constitutes a fundamental problem in the field of non-equilibrium pattern-forming systems. On the other side, from a technological point of view, the presence of microstructures determines the final mechanical and electrical properties of the processed material. Directional solidification is a controlled solidification technique which reproduces the conditions occurring in some important metallurgical processes like material casting or zone melting refining procedures. In a directional solidification experiment, the alloy sample is pulled at a constant velocity towards the cold region of an externally-imposed temperature gradient. Depending on the growth conditions, a morphological destabilization of the solid-liquid interface occurs during early transient stages. These initial transients are associated to a solute redistribution process due to the adaptation of the concentration field to the forced motion of the sample. The main objective of this thesis is to study the dynamical evolution of the morphological deformations of the front from these initial transients to the final stages where the properties of the interfacial pattern are determined. An important point in this process is that the internal fluctuations of the system play the role of an initiation mechanism for the morphological deformations of the front. During the initial transients, some of these microscopic perturbations are amplified by several orders of magnitude, and a range of wavelengths becomes morphologically unstable. The interfacial deformations of the front can be then characterized by means of power spectrum techniques. In order to study the dynamical evolution of the solidification front in directional solidification, we have used both theoretical and computational approaches: The main computational technique used in this thesis is the phase-field approach, which is a powerful method to simulate complex interfacial phenomena. The model equations describe the evolution of a continuous field , which takes different constant values at the solid and liquid bulks of the system. This field is then coupled with equations for the mass diffusion, and allows performing numerical studies without simulating the standard Stefan-like moving boundary problem. The phase-field method provides a diffuse interface description in which the transition from solid to liquid happens in a region of a certain thickness. The interface thickness introduces a new length in the simulations which must be taken into account to recover quantitative results. One major point in this thesis concerns with the introduction of fluctuations in phase-field methods. In the particular case of variational phase-field formulations -in which the model equations can be derived from a single free energy functional for the whole system-, the introduction of fluctuations can be done by applying the Fluctuation-Dissipation theorem. Variational formulations, however, although their appealing structure, present a poor computational efficiency and cannot be used to obtain quantitative results. To this extent, we have derived a general approach which does not relay in the Fluctuation-Dissipation assumption and permits to introduce fluctuations in both variational and non-variational phase-field formulations. Well-established analytical techniques like boundary integral methods for the transient front position and linear stability analysis of the interface during the transient have been used as theoretical predictions for the computational results. The dynamical evolution of the solidification front can be divided in two stages: A linear regime where the initial noise is amplified, and a non-linear coarsening process where the final properties of the interfacial pattern are selected. We have studied these different stages of the solidification process by using the phase-field approach, and good agreement is obtained when comparing with well-established theoretical and experimental predictions.

The problem of inaccurate measurement techniques for quantifying isothermal solidification kinetics during transient liquid phase (TLP) bonding in binary and ternary systems; and resulting uncertainty in the accuracy of analytical and numerical models has been addressed by the development of a new technique using differential scanning calorimetry (DSC). This has enabled characterization of the process kinetics in binary and ternary solid/liquid diffusion couples resulting in advancement of the fundamental theoretical understanding of the mechanics of isothermal solidification. The progress of isothermal solidification was determined by measuring the fraction of liquid remaining after an isothermal hold period of varying length. A 'TLP half sample', or a solid/liquid diffusion couple was setup in the sample crucible of a DSC enabling measurement of the heat flow relative to a reference crucible containing a mass of base metal. A comparison of the endotherm from melting of an interlayer with the exotherm from solidification of the residual liquid gives the fraction of liquid remaining. The Ag-Cu and Ag-Au-Cu systems were employed in this study. Metallurgical techniques were used to compliment the DSC results. The effects of sample geometry on the DSC trace have been characterized. The initial interlayer composition, the heating rate, the reference crucible contents, and the base metal coating must be considered in development of the experimental parameters. Furthermore, the effects of heat conduction into the base metal, baseline shift across the initial melting endotherm, and the exclusion of primary solidification upon cooling combine to systematically reduce the measured fraction of liquid remaining. These effects have been quantified using a modified temperature program, and corrected using a universal factor. A comparison of the experimental results with the predictions of various analytical solutions for isothermal solidification reveals that the moving interface solution can accurately predict the interface kinetics given accurate diffusion data. The DSC method has been used to quantify the process kinetics of isothermal solidification in a ternary alloy system, with results compared to a finite difference model for interface motion. The DSC results show a linear relationship between the interface position and the square root of the isothermal hold time. While the numerical simulations do not agree well with the experimental interface kinetics due to a lack of accurate thermodynamic data, the model does help develop an understanding of the isothermal solidification mechanics. Compositional shift at the solid/liquid interface has been measured experimentally and compared with predictions. The results show that the direction of tie-line shift can be predicted using numerical techniques. Furthermore, tie-line shift has been observed in the DSC results. This study has shown that DSC is an accurate and valuable tool in the development of parameters for processes employing isothermal solidification, such as TLP bonding.

This work presents a study and implementation of the simulation of residual stresses in castings. The objects of study are a cast iron truck Hub part (provided by the company Volvo 3P) and an optimized version of the Hub resulting from the application of a topology optimization process. The models are solved through an uncoupled thermo-mechanical solidification analysis, performed both in the FE commercial software Abaqus and the FD commercial software Magmasoft and the results are compared. First, a thermal analysis is carried out where the casting is cooled down from a super-heated temperature to room temperature. The thermal history obtained, is then used as an external force to calculate the residual stresses by means of a quasi-static mechanical analysis, using a J2-plasticity model. The simulation procedures are explained through a simplified model of the Hub and then applied to the geometries of interest. A results comparison between the original Hub and its optimized version is also presented. The theoretical base is given in this work as well as detailed implementation procedures. The results shows that the part subjected to the topology optimization process develop less residual stresses than its original version.

The problem of inaccurate measurement techniques for quantifying isothermal solidification kinetics during transient liquid phase (TLP) bonding in binary and ternary systems; and resulting uncertainty in the accuracy of analytical and numerical models has been addressed by the development of a new technique using differential scanning calorimetry (DSC). This has enabled characterization of the process kinetics in binary and ternary solid/liquid diffusion couples resulting in advancement of the fundamental theoretical understanding of the mechanics of isothermal solidification. The progress of isothermal solidification was determined by measuring the fraction of liquid remaining after an isothermal hold period of varying length. A 'TLP half sample', or a solid/liquid diffusion couple was setup in the sample crucible of a DSC enabling measurement of the heat flow relative to a reference crucible containing a mass of base metal. A comparison of the endotherm from melting of an interlayer with the exotherm from solidification of the residual liquid gives the fraction of liquid remaining. The Ag-Cu and Ag-Au-Cu systems were employed in this study. Metallurgical techniques were used to compliment the DSC results. The effects of sample geometry on the DSC trace have been characterized. The initial interlayer composition, the heating rate, the reference crucible contents, and the base metal coating must be considered in development of the experimental parameters. Furthermore, the effects of heat conduction into the base metal, baseline shift across the initial melting endotherm, and the exclusion of primary solidification upon cooling combine to systematically reduce the measured fraction of liquid remaining. These effects have been quantified using a modified temperature program, and corrected using a universal factor. A comparison of the experimental results with the predictions of various analytical solutions for isothermal solidification reveals that the moving interface solution can accurately predict the interface kinetics given accurate diffusion data. The DSC method has been used to quantify the process kinetics of isothermal solidification in a ternary alloy system, with results compared to a finite difference model for interface motion. The DSC results show a linear relationship between the interface position and the square root of the isothermal hold time. While the numerical simulations do not agree well with the experimental interface kinetics due to a lack of accurate thermodynamic data, the model does help develop an understanding of the isothermal solidification mechanics. Compositional shift at the solid/liquid interface has been measured experimentally and compared with predictions. The results show that the direction of tie-line shift can be predicted using numerical techniques. Furthermore, tie-line shift has been observed in the DSC results. This study has shown that DSC is an accurate and valuable tool in the development of parameters for processes employing isothermal solidification, such as TLP bonding.

In the present study, the powder metallurgy was evaluated as a technique to produce high performance Al &amp / #8211 / 8Fe &amp / #8211 / 1.7V &amp / #8211 / 7.9Si (wt%) alloys for elevated temperature applications and the role of powder particle size range and extrusion ratio in the microstructural and mechanical properties of the extruded alloys was investigated. For this purpose, an air atomization method was employed to produce powders of the high temperature alloy and after that the produced powders were sieved and cold compacted. The compacted billets were subsequently hot extruded at 450 &amp / #8211 / 480 &deg / C. Five selected ranges of powders which were different in particle size (&amp / #8722 / 2000+212 &amp / #956 / m, &amp / #8722 / 212+150 &amp / #956 / m, &amp / #8722 / 150+106 &amp / #956 / m, &amp / #8722 / 106+90 &amp / #956 / m, and &amp / #8722 / 90 &amp / #956 / m) and three different extrusion ratios (144:1, 81:1, and 26:1) were used in this study. In the first part of the thesis, microstructure and thermal stability of as &amp / #8211 / air atomized powders were described. &amp / #945 / &amp / #8211 / Al matrix and &amp / #945 / &amp / #8211 / Al13(Fe, V)3Si phases were characterized in all rapidly solidified powders by XRD. The fraction of the intermetallic phases was reduced as the powder particle size increased. DTA analysis revealed an exothermic reaction at 581 &deg / C in all alloy powders of different size fractions. In the second part of the study, the effect of powder particle size and extrusion ratio on microstructural and mechanical properties (at different temperatures) of the extruded alloys was investigated. The results showed that decrease in powder particle size and increase in extrusion ratio refined the microstructure and improved the mechanical properties. It was revealed that the effect of powder size was more evident than that of extrusion ratio. Remarkable increases in mechanical properties (e.g. 60.7% increase in ultimate tensile strength at 250 &deg / C) were observed as a result of rapid solidification process (atomization) and hot extrusion.