This master's thesis deals with the challenges of undesirable thermal expansion in lightweight materials. Thermal expansion of parts or components can lead to malfunction or breakdowns of complete systems in demanding environment where a large temperature gradient often exists. This work investigates a class of lightweight materials of which the thermal expansion coefficient can be controlled. Moreover, an additive manufacturing approach to produce these thermal management materials with high fidelity and reliability are critical to reach this goal. To achieve these two major research objectives analytic predictions, simulations, and measurement of thermal expansion coefficient with respect to temperature changes are conducted. Design and optimization of a high precision multi-material manufacturing apparatus has been conducted, leading to significant increase in production quality including reliability, efficiency, and costs. / Master of Science

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The effect of thermal-cycling-induced microcracking in fiber-reinforced polymer matrix composites is studied. Specific attention is focused on microcrack density as a function of the number of thermal cycles, and the effect of microcracking on the dimensional stability of composite materials. Changes in laminate coefficient of thermal expansion (CTE) and laminate stiffness are of primary concern. Included in the study are materials containing four different Thornel fiber types: a PAN-based T50 fiber and three pitch-based fibers, P55, P75, and P120. The fiber stiffnesses range from 55 Msi to 120 Msi. The fiber CTE's range from -0.50x10⁻⁶/°F to -0.80x10⁻⁶/°F. Also included are three matrix types: Fiberite's 934 epoxy, Amoco's ERL1962 toughened epoxy, and YLA's RS3 cyanate ester. The lamination sequences of the materials considered include a cross-ply configuration, [0/90]2s, and two quasi-isotropic configurations, [0/+45/-45/90]s and [0/+45/90/-45]s. The layer thickness of the materials range from a nominal 0.001 in. to 0.005 in. In addition to the variety of materials considered, three different thermal cycling temperature ranges are considered. These temperature ranges are ±250°F, ±150°F, and ±50°F. The combination of these material and geometric parameters and temperature ranges, combined with thermal cycling to thousands of cycles, makes this one of the most comprehensive studies of thermal-cycling-induced microcracking to date. Experimental comparisons are presented by examining the effect of layer thickness, fiber type, matrix type, and thermal cycling temperature range on microcracking and its influence on the laminates. Results regarding layer thickness effects indicate that thin-layer laminates microcrack more severely than identical laminates with thick layers. For some specimens in this study, the number of microcracks in thin-layer specimens exceeds that in thick-layer specimens by more than a factor of two. Despite the higher number of microcracks in the thin-layer specimens, small changes in CTE after thousands of cycles indicate that the thin-layer specimens are relatively unaffected by the presence of these cracks compared to the thick-layer specimens. Results regarding fiber type indicate that the number of microcracks and the change in CTE after thousands of cycles in the specimens containing PAN-based fibers are less than in the specimens containing comparable stiffness pitch-based fibers. Results for specimens containing the different pitch-based fibers indicate that after thousands of cycles, the number of microcracks in the specimens does not depend on the modulus or CTE of the fiber. The change in laminate CTE does, however, depend highly on the stiffness and CTE of the fiber. Fibers with higher stiffness and more negative CTE exhibit the lowest change in laminate CTE as a result of thermal cycling. The overall CTE of these specimens is, however, more negative as a result of the more negative CTE of the fiber. Results regarding matrix type based on the ±250°F temperature range indicate that the RS3 cyanate ester resin system exhibits the greatest resistance to microcracking and the least change in CTE, particularly for cycles numbering 3000 and less. Extrapolations to higher numbers of cycles indicate, however, that the margin of increased performance is expected to decrease with additional thermal cycling. Results regarding thermal cycling temperature range depend on the matrix type considered and the layer thickness of the specimens. For the ERL1962 resin system, microcrack saturation is expected to occur in all specimens, regardless of the temperature range to which the specimens are exposed. By contrast, the RS3 resin system demonstrates a threshold effect such that cycled to less severe temperature ranges, microcracking does not occur. For the RS3 specimens with 0.005 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between between ±150°F or ±50°F. For the RS3 specimens with 0.002 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between ±50°F.. Results regarding laminate stiffness indicate negligible change in laminate stiffness due to thermal cycling for the materials and geometries considered in this investigation. The study includes X-ray examination of the specimens, showing that cracks observed at the edge of the specimens penetrate the entire width of the specimen. Glass transition temperatures of the specimens are measured, showing that resin chemistry is not altered as a result of thermal cycling. Results are also presented based on a one-dimensional shear lag analysis developed in the literature. The analysis requires material property information that is difficult to obtain experimentally. Using limited data from the present investigation, material properties associated with the analysis are modified to obtain reasonable agreement with measured microcrack densities. Based on these derived material properties, the analysis generally overpredicts the change in laminate CTE. Predicted changes in laminate stiffness show reasonable correlation with experimentally measured values. / Ph. D.

Du fait leur conductivité thermique élevée, les matériaux composites à matrice métallique et renfort carbone possèdent un fort potentiel d’application pour la gestion thermique en électronique. Ces travaux présentent le développement d’un nouveau procédé pour la synthèse de matériaux composites Ag/rGO (argent / « reduced Graphene Oxide ») et Ag/GF (argent / « Graphite Flakes ») par métallurgie des poudres. Ce procédé, inspiré des méthodes de « molecular level mixing », permet d’obtenir des poudres composites Ag/rGO dans lesquelles les nano-renforts sont individualisés jusqu’à une concentration volumique de 1 %. Lorsqu’il est appliqué à la synthèse de matériaux composites Ag/GF, ce dernier permet l’élaboration de matériaux composites denses avec une concentration volumique en graphite jusqu’à 70 % et une conductivité thermique jusqu’à 675 W.m-1.K-1 (426 W.m-1.K-1 pour l’argent pur). En outre, il a été montré que le procédé d’élaboration des poudres composites Ag/GF a une forte influence sur l’anisotropie structurale des matériaux massifs ainsi que sur la résistance thermique d’interface extrinsèque Ag-graphite. Le procédé d’élaboration développé dans ces travaux permet ainsi d’obtenir des matériaux ayant une conductivité thermique jusqu’à 19 % supérieure à celle des matériaux obtenus par un procédé de mélange conventionnel. Néanmoins, comme la plupart des matériaux composites métal/GF (à matrice Cu, Al, Mg et Fe), la dilatation thermique des matériaux composites Ag/GF présente des « anomalies ». En effet, l’anisotropie de leur coefficient d’expansion thermique (CTE) est opposée à leur anisotropie structurale, leur CTE a une dépendance anormalement élevée vis-à-vis de la température et ces matériaux présentent une instabilité dimensionnelle en cyclage thermique. S’il est communément admis dans la littérature que ces anomalies sont la conséquence des contraintes internes générées lors de l’élaboration des matériaux (du fait de la différence de CTE entre matrice et renfort), ce phénomène reste mal compris et difficile à maitriser. Une part importante de ces travaux est consacrée à l’étude de ces « anomalies » et en particulier à l’étude de l’influence des propriétés mécaniques de la matrice d’argent sur la dilation thermique des matériaux composites. Grâce à la combinaison des caractérisations d’EBSD, de DRX, de microdureté instrumentée et de microscopie, des phénomènes clés responsables des propriétés thermomécaniques des matériaux composites Ag/GF ont pu être identifiés. En particulier, il a été montré qu’une part importante des contraintes internes est relaxée via la déformation plastique de la matrice d’argent et la déformation pseudo plastique du graphite lors du refroidissement post-densification des matériaux composites. Ainsi, le contrôle des propriétés mécaniques de la matrice métallique (en particulier de sa limite d’élasticité) permet d’atténuer les anomalies en CTE et confère une meilleure stabilité dimensionnelle aux matériaux composites Ag/GF lors d’un cycle thermique. L’addition de rGO dans la matrice d’argent des matériaux composites Ag/GF a également permis de réduire l’instabilité dimensionnel des matériaux jusqu’à 50 % grâce aux propriétés d’amortissement du rGO. / Due to their high thermal conductivity, metal matrix composite materials reinforced with carbon allotropes exhibit a high potential application for thermal management in electronics. This work deals with the elaboration of new synthesis process to produce Ag/rGO (silver/reduced Graphene Oxide) and Ag/GF (silver/Graphite Flakes) composite materials. This process, based on “molecular level mixing” methods, makes it possible to obtain Ag/rGO composite powders with individualized nano-reinforcements up to a concentration of 1 % in volume. Applied to the synthesis of Ag/GF composite materials, it allows to synthesize dense composite materials with a graphite concentration up to 70 % in volume and with a thermal conductivity up to 675 Wm-1.K-1 (426 Wm-1.K-1 for pure silver). Moreover, it has been shown that Ag/GF powders elaboration process has a strong influence on the structural anisotropy of bulk materials as well as on the extrinsic thermal boundary resistance Ag-graphite. The process developed in this work allows Ag/GF composite materials to reach thermal conductivity up to 19 % higher than the same materials synthesized by conventional mixing powder process. However, like most metal/GF composite materials (with Cu, Al, Mg and Fe matrix), thermal expansion of Ag/GF composite materials shows “anomalies”. Indeed, the anisotropy of their coefficient of thermal expansion (CTE) is opposed to their structural anisotropy, their CTE has an abnormally high dependence on temperature and these materials exhibit dimensional instability during thermal cycling. While it is commonly admit in literature that these “anomalies” are the consequence of internal stresses generated during materials densification (because of CTE mismatch between matrix and reinforcement), this phenomenon remains poorly understood and difficult to control. A significant part of this work is devoted to the study of these anomalies and especially to the study of the influence of matrix mechanical properties on composite materials thermal expansion. Thanks to EBSD, XRD, instrumented microhardness and microscopy analysis, key phenomena responsible of thermomechanical behavior of Ag/GF composite materials have been identified. Especially, it has been shown that a large part of the internal stresses is relaxed by plastic deformation of silver matrix and pseudo-plastic deformation of graphite during the post-densification cooling step of the materials. Thus, the control of mechanical properties of metallic matrix (especially of its elastic limit) makes it possible to attenuate the anomalies in CTE and confers a better dimensional stability to Ag / GF composite materials during thermal cycling. Finally, the addition of rGO in silver matrix of Ag/GF composites materials has also reduced material dimensional instability by up to 50 % thanks to the damping properties of rGO.

Les matériaux composites à matrice métallique (CMM) sont actuellement étudiés pour être utilisés dans de nombreux domaines d’application. L’une des applications potentielles concerne leur utilisation en tant que drain thermique pour les modules de puissance. Pour cette application, deux conditions sont requises : une conductivité thermique (CT) élevée pour évacuer la chaleur générée par la puce électronique et un coefficient d’expansion thermique (CTE) proche du substrat céramique (2-8×10-6 /K) utilisé dans le module de puissance.Ainsi des matériaux composites à matrice aluminium (Al : CT de 217 W/m.K et CTE de 24×10-6 /K) et à renfort plaquette de graphite (GF : CT de 1000 W/m.K et CTE de -1×10-6 /K dans le plan de la plaquette) ont été élaborés. Ces matériaux composites ont été fabriqués par Métallurgie des Poudres (MP) conventionnelle mais aussi par un procédé original nommé Flake Powder Metallurgy (FPM). Ce procédé, qui consiste à utiliser une poudre métallique à morphologie plaquette, a permis d’optimiser l’orientation des renforts plaquette dans un plan perpendiculaire à la direction de densification sous l’action d’une pression uniaxiale. De plus, ce procédé a permis d’obtenir une meilleure adhésion entre la matrice et le renfort comparé aux matériaux composites élaborés par MP conventionnelle. Cela a abouti à une amélioration de la CT qui est passée de 400 W/m.K à 450 W/m.K pour un taux de renfort de 50%vol. Néanmoins, concernant la dilatation thermique, des CTE de 21,8×10-6 /K et 21,7×10-6 /K ont été obtenus par MP et FPM respectivement, ce qui est incompatible avec l’application visée.Pour surmonter cette problématique, des matériaux composites à renfort multiple ont été élaborés par frittage en phase liquide. Ainsi des fibres de carbone (FC) ont été rajoutées à l’aluminium et aux plaquettes de graphite. L’ajout de ce second renfort au graphite a permis de diminuer de manière importante le CTE des composites Al/(GF+FC) avec une faible proportion en FC tout en maintenant une haute CT. De plus les matériaux composites Al/(GF+FC) présentent des CTE nettement inférieurs aux composites Al/FC avec un %vol. de FC équivalent. Ainsi des matériaux composites Al/(GF+FC) ont été élaborés par frittage en phase liquide permettant d’obtenir une CT de 400 W/m.K (comparable à la CT du cuivre) et un CTE de 8×10-6 /K (comparable au CTE de l’alumine). De plus la légèreté de l’aluminium confère aux matériaux composites Al/C une faible densité (d=2,4). Par conséquent, les matériaux développés dans cette étude sont prometteur en tant que drain thermique léger, notamment dans le domaine de l’électronique embarquée. / Many carbon/metal composites are currently used in several applications. One of them concerns their use as heat sinks in microelectronics. Concerning this application, two conditions are required: a high thermal conductivity (TC) in order to evacuate the heat generated by the electronic chip and a coefficient of thermal expansion (CTE) similar to the used material type of the electronic device (2-8×10-6 /K).Therefore, graphite flakes (GF; TC: 1000 W/m.K and CTE: -1×10-6 /K in the graphite plane) reinforced aluminum matrix (Al; TC: 217 W/m.K and CTE: 25×10-6 /K) composites were fabricated. These composite materials were fabricated by Powder Metallurgy (PM) and Flake Powder Metallurgy (FPM). This process, which consist to use a flattened metallic powder, helped to improve the in-plane orientation (perpendicular to the pressure direction) of GF under uniaxial pressure. Moreover, this process provided a better Al-C interface thanks to a planar contact between the matrix and the reinforcements. This resulted in an improvement of the CT from 400 W/m.K to 450 W/m.K for a reinforcement content of 50 vol.%. Nevertheless, regarding thermal dilation, CTEs of 21.8×10-6 /K and 21.7×10-6 /K were obtained by MP and FPM respectively, which is incompatible with the intended application.To overcome this problem, composite materials with multiple reinforcement were developed by solid-liquid phase sintering. Then, carbon fibers (CF) have been added to aluminum and graphite flakes. The addition of CF to GF reinforcement reduced significantly the CTE of the Al/(GF+CF) composites with a small proportion of CF, while preserving a high TC. In addition, the Al/(GF+FC) composite materials have significantly lower CTEs than the Al/CF composites with a equivalent vol.% of CF. Therefore, Al/(GF+CF) composite materials were developed by solid-liquid phase sintering to obtain a TC of 400 W/m.K (comparable to the TC of copper) and a CTE of 8×10-6 /K (comparable to the CTE of alumina). In addition, the lightweight of aluminum gives composite materials Al/C a low density (d = 2.4 g/cm3). Therefore, the composite materials developed in this study are promising as a lightweight heat sink in microelectronic industries.

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Solid oxide fuel cells (SOFC) in a flat-plate configuration require a hermetic seal between the fuel and air sides of the electrodes, and this seal must withstand a variety of thermally-induced stresses over the lifetime of the cell. In this study, quantitative microstructure-property relationships are developed to predict optimum seal structures for mechanical properties and thermal expansion coefficient criteria. These relationships are used to create an inverse approach to characterizing the processing method from the desired microstructure. The main focus of the work concentrates on providing tools to enable macroscopic property predictions from the constituent properties using homogenization techniques based on the individual phase properties and microstructure morphology. The microstructure is represented by two-point correlation functions. Statistical continuum mechanics models were then employed and developed to predict the mechanical and thermal properties of the material. The models enable the prediction of elastic modulus and coefficient of thermal expansion of the multi-phase material. The inelastic mechanical behavior was also studied, indicating microstructure dependence. These models will aid in predicting the a proper seal microstructure (with desired elastic stiffness, coefficient of thermal expansion, and viscoelastic behaviors) based on a desired level of crystallization glass-ceramic materials.