Cette étude a pour but de développer de nouveaux matériaux composites à matrice métallique renforcés par des nanotubes de carbone (CNT) et présentant des propriétés mécaniques améliorées. La majeure partie de ce travail a été réalisée en utilisant des CNT multi-feuillets synthétisés par déposition chimique en phase vapeur en tant que renforts et un alliage d'aluminium AA5083 comme matrice. Des composites CNT/AA5083 denses et homogènes ont été élaborés par le procédé de métallurgie des poudres suivi par une étape de mise en forme, l'extrusion. L'homogénéité de la dispersion des CNT à l'échelle microscopique dans les composites s'avère être un paramètre clé pour l'amélioration des propriétés mécaniques. Ceci a été réalisé par broyage planétaire à haute énergie impliquant des mécanismes de déformation plastique et de soudure à froid et a été démontré à l'aide d'études cartographiques par spectroscopie Raman. La limite d'élasticité, la résistance à la traction et la micro-dureté des composites homogènes ont été augmentées jusqu'à respectivement 55%, 61% et 33% en comparaison avec l'alliage sans CNT et préparé dans les mêmes conditions. Le coefficient de dilatation thermique a été quant à lui réduit de 10%. Les propriétés optimales ont été obtenues pour des concentrations en CNT de 1,5 % en masse. Le renforcement du matériau a été principalement attribué au transfert de charge à l'interface CNT/matrice. / The overall goal of this thesis is to process new metal matrix composites reinforced by CNT with enhanced mechanical properties. The main part of this work was achieved using CVD-grown multi-walled CNT as reinforcement and a high-performance light aluminium alloy, AA5083, as the matrix. Dense and homogeneous CNT/AA5083 composites were processed by the powder metallurgy route, followed by an extrusion forming process. A homogeneous dispersion of the CNT in the composites at the micron scale appears to be a key parameter for improving the mechanical properties. This could be achieved using high energy ball milling through the mechanisms of plastic deformation and cold-welding, and was demonstrated from Raman spectroscopy cartography studies. Yield strength, ultimate tensile strength and micro-hardness of the homogeneous composites were increased by up to 55%, 61% and 33%, with respect to raw alloys processed in the same conditions, and the coefficient of thermal expansion was decreased by 10%. Optimal results were obtained with a CNT con-tent of 1.5 wt.-%. The material strengthening was principally attributed to load transfer at the CNT/matrix interface.

En raison de leur propriétés spécifiques élevées, par rapports aux alliages légers, les Composites à matrice métallique (CMM) représentent des matériaux d'intérêt pour des applications de haute technologie dans les domaines aéronautique et aérospatiale. Les CMM les plus couramment utilisés sont à renfort particulaire, ou PRMMC, et à matrice Al en raison de leur faible densité. Cette thèse porte sur la mise au point de PRMMC à renfort nanométrique par une voie de synthèse réactive globale. En raison des normes encadrant l’usage des nanomatériaux et visant à limiter l’exposition des usagers et de l’environnement, la manipulation de poudres de taille nanométrique est coûteuse et problématique dans le cadre d’un usage industriel. La nouvelle voie de synthèse qui a été développée dans le cadre de cette thèse a permis de démontrer la faisabilité de composites à matrice métallique et à renfort particulaire nanométrique, dimension moyenne de 30 nm, sans avoir recourt initialement à des poudres de taille nanométrique. Le procédé étudié consiste en une réaction chimique à haute température entre deux matériaux précurseurs qui conduit à la formation in-situ non seulement du renfort mais aussi de la matrice. Par rapport aux techniques de synthèse classiques, cette technique permet de synthétiser des nanoparticules in situ et d’en contrôler la taille. De plus, la matrice et le renfort étant co produits par la réaction à haute température, l’interface entre les deux phases est exempte de couches d’oxydes, ce qui lui assure une très bonne adhésion. Dans le cadre du projet ANR NanoTiCAl, la faisabilité de cette nouvelle méthode a été étudiée à travers le cas d'un composite à matrice aluminium renforcé par des particules de carbure de titane (TiC). Les synthèses ont été réalisées entre 900°C et 1000°C à partir d’un couple de précurseurs incluant le graphite et un aluminiure de titane (Al3Ti). Le composite obtenu, caractérisé par un taux de renfort élevé de 34wt.%, possède un module de Young de 106 GPa, un allongement maximal à la rupture de 6% ainsi qu’une énergie à rupture de l’ordre de 28 J.cm-3. Ces valeurs démontrent un compromis entre résistance et capacité d’endommagement original et particulièrement intéressant, jamais observé dans la littérature pour des composites d’une teneur en renfort aussi importante. La caractérisation fine de la microstructure du composite ainsi que du renfort TiC après extraction du composite massif, ont permis de mieux comprendre les mécanismes à l’oeuvre dans cette voie de synthèse réactive. Enfin, sur la base de la compréhension obtenue dans le cas du composite Al/TiC, des critères ont été identifiés permettant d’aller vers une généralisation de ce procédé de synthèse. La pertinence de cette généralisation a finalement pu être démontrée par quelques mises en application à d’autres systèmes / Metal Matrix Composites (MMCs) have attracted research and industrial attentions as materials for high technological applications in the aeronautic and aerospace industry. The MMCs differ by their high specific mechanical properties compared to light weight alloys. The most commonly used are the Particulate Reinforcement Metal Matrix Composites (PRMMCs), especially the Al based matrices because of their low density.This thesis deals with the reactive synthesis of PRMMCs reinforced by nanoparticles. Because of the standards governing the use of nanomaterials to limit the exposure of users and environment, handling nanoscaled powders is very problematic and expensive in industry. Furthermore, the cost of this kind of processes is very high. This new synthesis route, developed during this thesis, shows the feasibility of PRMMCs reinforced by nanosized particles, with a mean size of 30 nm, without using any starting nanoparticles.The process consists in a chemical reaction at high temperature between precursor materials which leads to form both of the matrix and the reinforcement phase. Compared to conventional synthesis techniques as stir casting, this route allows to synthesis nanoparticles in-situ and to control their size. In addition, the matrix and the reinforcement, which are formed by a reaction at high temperature, have an interface free of oxide layers which assures a good adhesion.In the NanoTiCAl project, the feasibility of this new method is illustrated in the case of an aluminium based composite reinforced by titanium carbide (TiC). The synthesis were realized between 900°C and 1000°C from a couple of precursors including graphite and titanium aluminide (Al3Ti). The resulting composite, characterized by a high reinforcement ratio (34 wt.%), presents a Young’s modulus of 106 GPa, a maximum elongation of 6 % and a high toughness, about 28 J.cm-3. These values represent an uncommon compromise between strength and toughness never seen in the literature regarding to the high content of reinforcement.The characterization of the composite microstructure and of the reinforcement phase, after extraction of the solid composite, allowed a better understanding of the reaction mechanism during the reactive synthesis. Finally, based on our understanding of the Al-TiC composite, criteria have been identified to generalize this synthesis process. This generalization was demonstrated with success in other systems

Este trabalho versa sobre a caracterização de uma junta soldada em cheio (bead-onplate) de liga AA356 reforçada com partículas de SiC, soldada por um Laser de fibra de alta potência. A soldagem foi realizada em duas amostras com diferentes condições térmicas, tratadas termicamente T6 (solubilização e envelhecimento) antes da soldagem (amostra A) e após a soldagem (amostra B). Nas amostras A e B foram realizadas as análises de materialográfia via Microscopia Óptica de luz reflexiva (M.O) e Microscopia Eletrônica de Varredura (MEV), também foram realizadas análises microquímica por Energia Dispersiva de Raios-X (EDX), ensaio mecânico de microdureza e difração de Raios-X. Os corpos de prova submetidos ao ensaio de tenacidade em Flexão três pontos tinham condições térmicas iguais a da amostra A, pois essa condição térmica é a condição que normalmente o Compósito de Matriz Metálica (CMM) exibe em serviço. A inspeção materialográfica por M.O identificou a interferência do tratamento térmico T6 realizado na amostra A, fazendo que fosse possível identificar a baixa proporção das partículas de Si na matriz, conforme análise se aproximava da zona fundida (ZF), e a presença de uma estrutura metaestável com a presença dendritas na ZF, aos quais foram diretamente correlacionados com os resultados da microdureza. A amostra B exibiu uma microestrutura bem homogênea em relação à amostra A, em termos de dispersão das partículas de Si e presença de dendritas na ZF. A fratográfia por MEV em modo de imageamento por elétrons secundários, permitiu analisar as superfícies de fratura do compósito em estudo (AA356+SiC), fraturado após o ensaio de tenacidade em Flexão três pontos, identificando a presença de muitos dimples que formavam uma estrutura alveolar, conhecida como uma estrutura típica de um regime dúctil. Por meio desta técnica, também foi possível detectar os principais mecanismos de tenacificação nos CMM, tais como: trincamento, descolamento ou destacamento das partículas de SiC, e o crescimento e coalescência de dimples na estrutura da matriz, os quais foram identificados e correlacionados com o desempenho mecânico dos corpos de prova analisados. A microanálise química por EDS permitiu o mapeamento dos elementos químicos presentes nas regiões do Metal Base (MB) e na Zona Termicamente Afetada (ZTA) do CMM. Por meio desta técnica, foi possível identificar a presença das partículas de Si e SiC, os elementos químicos presentes nas regiões dendriticas, os elementos fragilizantes presentes na microestrutura do CMM, tais: como Fe, Cr e Mn, e a presença de carbeto de Aluminio-Silício (Al4SiC4) presentes nas ZF, em forma de agulhas. A microanálise química foi realizada tanto nas regiões das juntas soldadas quanto nas superfícies de fraturas provenientes do ensaio de tenacidade em Flexão três pontos. / This work focuses on the characterization of a joint welded bead-on-plate of SiC particulate-reinforced A356-alloy welded by high power fiber laser. The welding was achieved in two samples with different conditions, both with T6 applied, before (sample A) and after (sample B) the welding process respectively. Samples A and B were performed materialographic analysis by Optic Microscopy of light reflected (O.M) and scanning electron microscopy (SEM), were also performed chemical microanalysis by energy dispersive X-ray , mechanical testing microhardness and X-ray diffraction. Specimens submitted to the three point bending toughness test present a thermal condition similar to sample A, because this thermal condition is the condition that normally the Metal Matrix Composite (MMC) exhibits in service. The inspection metallographic by (O.M) identified heat treatment T6 interference in the sample A, and though this is it was possible to identify low proportion of Si particles in the matrix, while the analysis was approaching fused zone, and the presence of a metastable structure with formation of dendrites in the fused zone, were which promptly correlated with results of microhardness. The sample B exhibited more homogenous a microstructure in terms of dispersion of Si particles. SEM fractography in secondary electron imaging mode allowed to analyze fracture surface of MMC, identifying the presence of more microvoids creating an alveolar structure typical of an ductile regime. Through this technique, it also was possible to detect main toughening mechanisms for MMC, such as, cracking, debonding and growth and coalescence dimples in the structure the of matrix which were identified and correlated with performance of specimens analyzed. EDS micro-chemical analysis allowed to map chemistry elements present in various regions of CMM, such as, Base Metal (BM), heat affected zone (HAZ) and Fused Zone (FZ). Through this technique, it was possible to identify and quantify the presence of Si and SiC particles, the elements present in the dendrites and presence of embrittlement elements in the microsctructure of MMC, such as, Fe,Cr and Mn and presence of needle-shapped Aluminium-Silicon carbides (Al4SiC4) in the FZ of sample A. Chemical microanalyses were performed both in regions of welded joints and in surface of fracture from the three points bending toughness test.

Compósitos de matriz metálica (CMM) reforçados com dois tipos de particulado cerâmico foram produzidos por meio do processo ARB (Accumulative Roll Bonding) a fim de estudar os efeitos destes no que diz respeito às propriedades mecânicas e microestruturais. ARB é um processo de deformação plástica severa aplicada originalmente a uma pilha de lâminas metálicas, a qual é laminada, seccionada em duas metades, as quais são empilhadas e novamente laminadas, e assim por diante, desenvolvido com o propósito de reduzir o tamanho de grão e aumentar a resistência mecânica do produto final. O processo é econômico e capaz de produzir de folhas ultrafinas a placas espessas, sem que haja restrição de quantidade. Confeccionou-se CMM de alumínio reforçados com partículas de carbeto de silício (Al+SiCp) e alumina (e Al+Al2O3p) com granulometria média de 40µm, as quais foram caracterizadas microestruturalmente e ensaiadas em tração até a falha, cuja análise foi conduzida via microscopia eletrônica de varredura. Ambas as amostras obtiveram ganho em sua resistência mecânica, comparadas ao alumínio monolítico (sem adição de partículas de reforço) e alumínio recozido. Foram ensaiados em tração corpos de prova com e sem presença de entalhe, sendo que as peças entalhadas apresentaram comportamento esperado de aumento de resistência mecânica e baixo alongamento e fratura de aspecto frágil. De acordo com análise feita por fratografia houve boa ancoragem e dispersão das partículas de reforço na matriz. / Metal matrix composite (CMM) reinforced with two types of ceramic particles have been produced through the process ARB (Accumulative Roll Bonding) in order to study their effect as regards the mechanical and microstructural properties. ARB is a severe plastic deformation process originally applied to a stack of metal sheets, which is laminated, sectioned into two halves, which are stacked and rolled again, and so on, developed with the purpose of reducing the grain size and increase the mechanical strength of the final product. The process is economical and capable of producing ultrafine sheets to thicker plates without much restriction. Were fabricated CMM of the aluminum reinforced with particles of silicon carbide (Al + SiCp) and alumina (and Al + Al2O3p) with an average particle size of 40μm, which are characterized microstructurally and tested in tension until failure, whose analysis was conducted via scanning electron microscopy. Both samples were successful in its mechanical strength compared to the monolithic aluminum (without addition of reinforcing particles) and annealed aluminum. They were tested for tensile specimens with and without the presence of notch, and the carved pieces showed strength-enhancing behavior and low elongation and frail fracture. According to analysis by fractography was good anchoring and reinforcement particles dispersed in the matrix.

There is a great need in the transportation industry for high strength, high stiffness and lightweight materials with excellent dimensional stability. The use of these materials reduces fuel consumption and greenhouse gas emission as well as malfunctioning of components when subjected to fluctuating temperatures. Metal matrix composites (MMCs) are designed to meet these needs of transportation and other industries. However, their use is limited by lack of information on their thermal behaviour. In addition, reactions that occur in MMCs alter their microstructure and properties. These reactions have been widely investigated using X-ray Diffractometry (XRD) and electron microscopy (EM). However, these techniques cannot provide information such as charge transfer and local elemental structures in materials. Synchrotron X-ray Absorption Spectroscopy (XAS) could be used to identify reaction products in MMCs as well as provide information which XRD and EM cannot provide.<p> The thermal behaviour of Al-Mg alloy A535 containing fly ash particles as well as charge transfer and reactivity in particulate aluminium alloy metal matrix composites (MMCs) were investigated in this work. The materials studied were (i) Al-Cu-Mg alloy AA2618 and its composites reinforced with 10 and 15 vol.% alumina (Al2O3) particles and (ii) Al-Mg alloy A535 and its composites reinforced with a mixture of 5 wt.% fly ash and 5 wt.% silicon carbide, 10 wt.% and 15 wt.% fly ash. The investigative techniques used included Differential Scanning Calorimetry (DSC), Thermomechanical Analysis (TMA), Optical Microscopy (OM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), and synchrotron X-ray Absorption Spectroscopy (XAS).<p> The results obtained showed that the coefficient of thermal expansion (CTE) of A535 decreased with the addition of fly ash and silicon carbide. Also, the addition of these particles improved the dimensional stability of the alloy in that the residual strain, åp, cycling strain, åc, and CTE decreased. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The addition of alumina particles into AA2618 increased the p-orbital population and also changed the surface chemistry of the matrix. It was also demonstrated that the XAS technique can be used to determine the presence of various oxides in industrial fly ash and spinel (MgAl2O4) in alumina and fly ash particles extracted from the MMCs.

There is a great need in the transportation industry for high strength, high stiffness and lightweight materials with excellent dimensional stability. The use of these materials reduces fuel consumption and greenhouse gas emission as well as malfunctioning of components when subjected to fluctuating temperatures. Metal matrix composites (MMCs) are designed to meet these needs of transportation and other industries. However, their use is limited by lack of information on their thermal behaviour. In addition, reactions that occur in MMCs alter their microstructure and properties. These reactions have been widely investigated using X-ray Diffractometry (XRD) and electron microscopy (EM). However, these techniques cannot provide information such as charge transfer and local elemental structures in materials. Synchrotron X-ray Absorption Spectroscopy (XAS) could be used to identify reaction products in MMCs as well as provide information which XRD and EM cannot provide.<p> The thermal behaviour of Al-Mg alloy A535 containing fly ash particles as well as charge transfer and reactivity in particulate aluminium alloy metal matrix composites (MMCs) were investigated in this work. The materials studied were (i) Al-Cu-Mg alloy AA2618 and its composites reinforced with 10 and 15 vol.% alumina (Al2O3) particles and (ii) Al-Mg alloy A535 and its composites reinforced with a mixture of 5 wt.% fly ash and 5 wt.% silicon carbide, 10 wt.% and 15 wt.% fly ash. The investigative techniques used included Differential Scanning Calorimetry (DSC), Thermomechanical Analysis (TMA), Optical Microscopy (OM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), and synchrotron X-ray Absorption Spectroscopy (XAS).<p> The results obtained showed that the coefficient of thermal expansion (CTE) of A535 decreased with the addition of fly ash and silicon carbide. Also, the addition of these particles improved the dimensional stability of the alloy in that the residual strain, åp, cycling strain, åc, and CTE decreased. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The addition of alumina particles into AA2618 increased the p-orbital population and also changed the surface chemistry of the matrix. It was also demonstrated that the XAS technique can be used to determine the presence of various oxides in industrial fly ash and spinel (MgAl2O4) in alumina and fly ash particles extracted from the MMCs.

The aim of the present study was to investigate the effects of different levels of Saffil alumina fiber addition, magnesium content in aluminum alloy matrix and casting temperature on the mechanical behavior, microstructure and physical properties of short fiber reinforced aluminum matrix composites. The main alloying element silicon was kept constant at 10 wt%. Magnesium contents were selected as 0.3 wt% and 1 wt%. Saffil alumina fiber preforms varied from 10 to 30 vol%. The casting temperatures were fixed at 750 &deg / C and 800 &deg / C. Micro porosity was present at the fiber-fiber interactions. Closed porosity of the composites increased when fiber vol% increased, however, variation in casting temperature and magnesium content in matrix did not have influence on porosity. Hardness of the composites was enhanced with increasing fiber vol%, magnesium content in matrix and decreasing casting temperature. Alignment of fibers within the composite had an influence on hardness / when fibers were aligned perpendicular to the surface, composites exhibited higher hardness. The highest hardness values obtained from surfaces parallel and vertical to fiber orientation were 155.6 Brinell hardness and 180.2 Brinell hardness for AlSi10Mg1 matrix 30 vol% alumina fiber reinforced composite cast at 800 &deg / C and at 750 &deg / C, respectively. 30 vol% Saffil alumina fiber reinforced AlSi10Mg0.3 matrix composite cast at 750 &deg / C showed the highest flexural strength which is 548 MPa. Critical fiber content was found as 20 vol% for all composites.

Al-Mg alloys were infiltrated into porous alumina preforms at temperatures greater than 950°C where significant amount of nitride forms in the matrix. The present work aims to obtain a process window for growing A1N rich composites over uniform thicknesses so that bulk fabrication of these composites could be carried out. Initial experiments were carried out in a thermo-gravimetric analyser (TGA) to establish suitable conditions for growing useful thicknesses. Al- 2wt% Mg alloy, alumina preforms of particle size 53-63μm and N2 - 2% H2 (5ppm O2) were used for the present study based on previous work carried out in the fabrication of MMCs at low temperatures. Experiments carried out in the TGA indicate that oxygen in the system has to be gettered for the growth of nitride rich composites. Infiltration heights of about 8mm were obtained using an external getter (Al - 5wt%Mg) alloy in addition to the base alloy used for infiltration. The above process conditions were subsequently employed in a tube furnace to fabricate bulk composites and to study the effect of temperature on the volume fraction of aluminium nitride in the matrix. The volume fraction of nitride in the composite varied between 30 and 95 vol % with increase in process temperature from 950°C to 1075°C. Microstructures of these composites indicate that A1N starts to form on the particle surface and tends to grow outwards. The metal supplied through channels adjacent to the particle surface nitride until a point is reached when the composite growing from the adjacent particles meet each other and isolate the melt underneath from nitrogen thereby leading to a metal rich region underneath. Increase in temperature results in an increased nitridation rate resulting in reduced metal pocket size. Composites fabricated at 975°C had a minor leak at the O-rings, which seal the tube. This led to infiltration under conditions of varying oxygen partial pressure leading to different nitride fractions in the composite. The above fact was confirmed by conducting an experiment with commercial purity nitrogen, which has an oxygen content of about 5000ppm. The composite had an A1N content of about 30% whereas the composite fabricated with N2 -2%H2 (5ppm oxygen) showed a nitride content of 64%. This suggests that one can vary the nitride content in the composite by varying the oxygen content in the system at a particular process temperature. The hardness of the matrix increases with increase in process temperature from 3.5 ± 0.7 GPa at 975°C to about 9.8 ± 0.9 GPa at 1075°C. Porosity was observed in the composite processed at 1075°C. This increased porosity leads to decreased hardness though the nitride content in the composite has increased by 11%. The scatter in the data is attributed to variations in the microstructure as well as due to interference from underlying metal pockets or particles as well as due to porosity introduced in the composite at high processing temperatures.

D. Tech. Mechanical Engineering. / Discusses the main objective of this study was to extend the hybrid method developed by Paskaramoorthy, et al (1988). This objective was to study the effect of elastic wave on any particulate reinforced metal matrix composite (PRMMC). The specific objectives were: to compare the effect of plane wave and shear vertical wave on a particular particulate reinforced metal matrix composite (PRMMC)-Mg/TiC, using analytical method ; to use the extended hybrid method to determine the effect of particle size and single interface layer on Mg/TiC.

The preliminary goal of this study is to determine the effects of processing conditions, compositions and microstructural morphologies of the constituents on the physical and thermo-mechanical properties of alumina (Al_2O_3) reinforced aluminum (Al) composites. Composites with 0, 5, 10, 20 and 25 vol% Al_2O_3 were manufactured using powder metallurgy method. The elastic properties (Young's and shear modulus) and the coefficient of thermal expansion (CTE) of the composites were determined using Resonant Ultrasound Spectroscopy (RUS) and Thermo Mechanical Analyzer (TMA) respectively at various temperatures. Increasing compacting pressure improved relative density (or lowered porosity) of the composites. Furthermore, increasing the Al_2O_3 vol% in the composite increased the elastic moduli and reduced the CTE of the composites. Increasing the testing temperature from 25 to 450 oC, significantly reduced the elastic moduli of the composites, while the CTE of the composites changed only slightly with temperatures. Secondly, the goal of this study is to determine the effect of microstructures on the effective thermo-mechanical properties of the manufactured Al-Al_2O_3 composites using finite element (FE) method. Software OOF was used to convert the SEM micrographs of the manufactured composites to FE meshed models, which were then used to determine the effective elastic modulus and CTE. It was observed that, effective modulus dropped by 19.7% when porosity increased by 2.3%; while the effective CTE was mildly affected by the porosity. Additionally, the effect of residual stress on the effective thermo-mechanical properties was studied, and the stress free temperature of the composites was determined. Another objective of this study is to examine the stress-strain response of Al-Al_2O_3 composites due to compressive loads at various temperatures. Elastic modulus, yield stress and strain hardening parameters were determined from the stress-strain curves and their dependency on temperature, porosity and volume fraction were studied. The experimental results were compared with the numerical results. It was observed that high-localized stresses were present near the pores and at the interfaces between Al and Al_2O_3 constituents. Finally, functionally graded materials (FGMs) with varying Al_2O_3 concentration (0, 5and 10 vol%) in Al were manufactured; and their stress-strain response and CTE were determined at various temperatures.