Friction stir processing (FSP) is applied to produce particulate-reinforced aluminum matrix composites with ultrafine grained structure from elemental powder mixtures of Al-Cu, Al-Ti and Al-Si. The microstructures of the composites were characterized by the use of XRD, SEM and TEM. Microhardness, tensile and compressive tests were performed to evaluate the mechanical properties of these composites. The mechanisms of microstructure evolution in FSP and the strengthening mechanisms in these composites are discussed. In the Al-Si system, the Si particles were broken and uniformly distributed in the stir zone by the application of multiples-pass FSP. The average size of Si particles and Al grains were refined to below ~2

Laser powder bed fusion (LPBF), one of the most promising additive manufacturing (AM) techniques, has enabled the production of previously impossible structures. This breakthrough in AM has not only facilitated the creation of new designs, but also the redesign of existing industrial and engineering components to produce lightweight and highly efficient dies and molds, biomaterial scaffolds, aircraft brackets, heat sink and heat exchangers. In many of the mentioned applications in industries such as automotive, aerospace, heat exchanger, and electronics, aluminum (Al), Al alloys, and Al matrix composites (AMCs) are considered potential candidates. In the first phase of this study, the optimum powder particle size and size distribution of an Al alloy powder (i.e., AlSi10Mg) was determined with the aim being to achieve highest densification levels and dimensional accuracies. In the second phase, three materials with high thermal conductivities were selected, namely, pure Al, AlSi12 and AlSi10Mg alloys. Since Al/Al alloys are prone to oxidation, the LPBF process parameters were optimized not only in terms of the densification level but also oxygen content of the fabricated parts. It was found out that the rate of oxide diminishment for Al/Al alloys during the LPBF process is more than in-situ oxidation. Despite the efforts, the optimized LPBF fabricated samples showed lower thermal conductivity than their conventionally manufactured counterparts. To tackle the issue, two different potential solutions were put into test. In the third phase, the influence of preheating on thermal properties of pure Al, AlSi12, and AlSi10Mg was investigated and a huge improvement in the thermal conductivity of the optimized as-built parts was obtained. In the fourth phase, the possibility of enhancing thermal conductivity of the LPBF fabricated Al/Al alloys in as-built condition through the incorporation of a second constituent with a higher thermal conductivity (i.e., graphene) was investigated. / Thesis / Doctor of Philosophy (PhD)

Orientadores: Maria Helena Robert, Elisa Maria Ruiz Navas / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-19T00:27:43Z (GMT). No. of bitstreams: 1 BravoSalazar_JaimeAlejandro_D.pdf: 9695376 bytes, checksum: d35ebfbcaf1dac8c6665392b7d784d23 (MD5) Previous issue date: 2007 / Resumo: Este trabalho estuda o processo de fabricação de compósitos de matriz de alumínio AA6061 reforçado com TiCN por metalurgia do pó, envolvendo as etapas de mistura de pós, compactação uniaxial e sinterização com fase líquida. Para efeitos de comparação foram produzidos e caracterizados compactados da liga AA6061 sem adição de reforços. Foram investigados os parâmetros de processo: teores de reforço (5% e 10% massa), teor de aditivos Pb e Sn (0,1, 0,15, 0,2 e 0,4% massa), pressão de compactação (400, 600 e 800 MPa), tempos (15, 30, 45 e 60 min) e temperatura de sinterização (590, 600, 610 e 620 ºC). Em cada etapa do processo foram caracterizados os produtos (mistura de pós e compactados); o produto final obtido, após sinterização, foi caracterizado com relação à sua microestrutura, propriedades físicas (densificação e variação dimensional) e mecânicas (resistência à flexão e dureza). Os resultados obtidos mostraram uma grande eficiência do processo na obtenção de compósitos; a adição do teor de reforço de 5%TiCN foi eficiente na promoção de rupturas das camadas de óxidos do pó da liga de alumínio compactado à pressão de 400 MPa, auxiliando a sinterização por difusão da fase líquida formada a partir da fusão de Al+Mg2Si, melhorando a densificação e diminuindo a variação dimensional dos produtos sinterizados. Do ponto de vista metalúrgico, os materiais compósitos obtidos apresentaram microestruturas homogêneas, com uma boa distribuição dos reforços na matriz e relativa diminuição de poros. A adição de Pb e Sn promovem maior eficiência de ativação de mecanismos de sinterização; para compactados produzidos à pressão de 800 MPa, a adição de 0,1% desses elementos já apresentou significativa influência na sinterização. Com relação às propriedades mecânicas e físicas observou-se que a adição de TiCN aumentou quase no dobro de seus valores obtidos quando são comparados com a liga AA6061 / Abstract: This work investigates the process of production of composites of the alloy AA6061 reinforced with TiCN particles, by powder metallurgy involving the steps: conventional mixture of powders, compaction by uniaxial cold pressing and sintering with formation of a liquid phase. For comparative analysis it was also produced sintered AA6061 without addition of reinforcements. The following processing parameters were studied: reinforcing particles content (5 and 10 wt%); content of trace elements Pb and Sn (0.1, 0.15, 0.2 0.4 wt%); compaction pressure (from 400, 600 and 800 MPa); time and temperature of sintering (15, 30, 45, 60 min and 590, 600, 610, 620 oC). In each step products were characterized (powder mixture and green compacts); the final sintered product was characterized related to microstructure, physical (densification and dimensional changes) and mechanical (hardness and bending strength) properties. Obtained results showed high efficiency of the applied process to produce reliable composite products; the addition of 5 wt% TiCN was efficient to promote fracture of the oxide layer in the aluminum particles surface during pressing. At sintering temperatures liquid phase is formed by Al+Mg2Si melting and is distributed among particles through the fractures of the oxide layer, improving the material densification and its mechanical properties. Microstructures obtained showed homogeneous distribution of TiCN and reduced porosity, whereas AA6061 alloy microstructure showed higher porosity. Addition of Pb and Sn promoted higher efficiency of sintering mechanisms in compacts submitted to high pressures, leading to enhanced physical and mechanical properties in those materials. / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

In this thesis, the effect of mechanical deformation on structure, thermal stability and hardness of a single-phase spray-deposited quasicrystalline alloy with composition Al62.5Cu25Fe12.5 has been investigated in detail. The purpose of the investigation was to study the effect of mechanical milling at different milling speeds (which approximately scale with the milling intensity) on mechanically-induced phase transformations during milling and on the phase evolution during subsequent heating. The results of the milling experiments indicate that, irrespective of the milling speeds used, mechanical milling of Al62.5Cu25Fe12.5 quasicrystals leads to the formation of a disordered CsCl-type ß phase with grain size of about 10 – 20 nm. The analysis of the kinetics of the QC–to–ß phase transformation reveals that the milling intensity has a considerable effect on the characteristics of the transformation. The increase of the milling speed considerably shortens the incubation time needed to start the QC–to–ß phase transformation. Also, the overall transformation is much faster for milling at high speeds. The QC–to–ß phase transformation starts when the grain size of the quasicrystals is reduced to about 10 nm irrespective of the milling speed used and clearly indicates that a critical grain size of the quasicrystals for initiating the transformation exists. On the other hand, no critical value of lattice strain was found for the QC–to–ß transformation. This indicates that the phase transformation is controlled by the local length scale (i.e. the grain size) and by the corresponding grain boundaries rather than by the energy stored in the lattice. Energetic considerations obtained through a simple model based on the mass and velocity of the milling balls reveal that the energy needed for the QC–to–ß transformation increases with increasing the milling speed, that is, the energetic efficiency of the process decreases with increasing the milling intensity. This indicates that part the extra energy supplied during milling at high intensities is not used to induce the phase transformation but it is dissipated by heat. During heating, the milled powder displays a multi-step thermal behavior characterized by the grain growth of the disordered ß phase at low temperatures, followed, at higher temperatures, by its transformation into the original icosahedral quasicrystalline phase. The transformation is gradual and the quasicrystals and the disordered ß phase coexist over a temperature interval of more than 250 K. The phase transformations occurring during milling and subsequent annealing have a remarkable effect on the hardness, which can be tuned within a wide range of values (7–9.6 GPa) as a function of the volume fraction of the different phases. This suggests that a composite material with optimized mechanical properties can be produced by an appropriate thermo-mechanical treatment. The quasicrystals milled at a very low speed show a transition between Hall-Petch to inverse Hall-Petch behavior at a grain size of about 40 nm, which represents the critical value for grain size softening of the present Al62.5Cu25Fe12.5 quasicrystals. This behavior may be attributed to the complexity of the quasicrystalline structure and to its peculiar deformation mechanism at room temperature (i.e. shear banding), where meta-dislocation-assisted deformation is almost absent. In order to analyze the effectiveness of the Al62.5Cu25Fe12.5 quasicrystals as reinforcing agent in metal matrix composites, Al-based composites were synthesized by hot extrusion of elemental Al blended with different amounts of Al62.5Cu25Fe12.5 quasicrystalline particles. The work was focused on two specific aspects: evaluation of the mechanical properties through room temperature compression tests and modeling of the resulting properties. The addition of the quasicrystalline reinforcement is very effective for improving the room temperature mechanical properties of pure Al. The compressive strength increases from 155 MPa for pure Al to 330 and 407 MPa for the composites with 20 and 40 vol.% of reinforcement, respectively, reaching an ultimate strain of 55 % and 20 % before fracture occurs. These results indicate that the addition of the QC reinforcement leads to composite materials with compressive strengths exceeding that of pure Al by a factor of 2 – 2.5, while retaining appreciable plastic deformation. The mechanical properties of the composites have been modeled by taking into account the combined effect of load bearing, dislocation strengthening and matrix ligament size effects. The calculations are in very good agreement with the experimental results and reveal that the reduction of the matrix ligament size, which results in a similar strengthening effect as that observed for grain refinement, is the main strengthening mechanism in the current composites. Finally, the interfacial reaction between the Al matrix and the QC reinforcement has been used to further enhance the strength of the composites through the formation of a new microstructure consisting of the Al matrix reinforced with Al7Cu2Fe w-phase particles. The optimization of the structure-property relationship was done through the systematic variation of the processing temperature during consolidation. The mechanical behavior of these transformation-strengthened composites is remarkably improved compared to the parent material. The yield strength of the composites significantly increases as the Al + QC -> ω transformation progresses from 195 MPa for the sample reinforced only with QC particles to 400 MPa for the material where the Al + QC -> ω reaction is complete. These results clearly demonstrate that powder metallurgy, i.e. powder synthesis by ball milling followed by consolidation into bulk specimens, is an attractive processing route for the production of novel and innovative lightweight composites characterized by high strength combined with considerable plastic deformation. In addition, these findings indicate that the mechanical behavior of Al-based composites reinforced with Al62.5Cu25Fe12.5 quasicrystalline particles can be tuned within a wide range of strength and plasticity depending on the volume fraction of the reinforcement as well as on the extent of the interfacial reaction between Al matrix and QC reinforcing particles.

No description available.

In this thesis, the effect of mechanical deformation on structure, thermal stability and hardness of a single-phase spray-deposited quasicrystalline alloy with composition Al62.5Cu25Fe12.5 has been investigated in detail. The purpose of the investigation was to study the effect of mechanical milling at different milling speeds (which approximately scale with the milling intensity) on mechanically-induced phase transformations during milling and on the phase evolution during subsequent heating. The results of the milling experiments indicate that, irrespective of the milling speeds used, mechanical milling of Al62.5Cu25Fe12.5 quasicrystals leads to the formation of a disordered CsCl-type ß phase with grain size of about 10 – 20 nm. The analysis of the kinetics of the QC–to–ß phase transformation reveals that the milling intensity has a considerable effect on the characteristics of the transformation. The increase of the milling speed considerably shortens the incubation time needed to start the QC–to–ß phase transformation. Also, the overall transformation is much faster for milling at high speeds. The QC–to–ß phase transformation starts when the grain size of the quasicrystals is reduced to about 10 nm irrespective of the milling speed used and clearly indicates that a critical grain size of the quasicrystals for initiating the transformation exists. On the other hand, no critical value of lattice strain was found for the QC–to–ß transformation. This indicates that the phase transformation is controlled by the local length scale (i.e. the grain size) and by the corresponding grain boundaries rather than by the energy stored in the lattice. Energetic considerations obtained through a simple model based on the mass and velocity of the milling balls reveal that the energy needed for the QC–to–ß transformation increases with increasing the milling speed, that is, the energetic efficiency of the process decreases with increasing the milling intensity. This indicates that part the extra energy supplied during milling at high intensities is not used to induce the phase transformation but it is dissipated by heat. During heating, the milled powder displays a multi-step thermal behavior characterized by the grain growth of the disordered ß phase at low temperatures, followed, at higher temperatures, by its transformation into the original icosahedral quasicrystalline phase. The transformation is gradual and the quasicrystals and the disordered ß phase coexist over a temperature interval of more than 250 K. The phase transformations occurring during milling and subsequent annealing have a remarkable effect on the hardness, which can be tuned within a wide range of values (7–9.6 GPa) as a function of the volume fraction of the different phases. This suggests that a composite material with optimized mechanical properties can be produced by an appropriate thermo-mechanical treatment. The quasicrystals milled at a very low speed show a transition between Hall-Petch to inverse Hall-Petch behavior at a grain size of about 40 nm, which represents the critical value for grain size softening of the present Al62.5Cu25Fe12.5 quasicrystals. This behavior may be attributed to the complexity of the quasicrystalline structure and to its peculiar deformation mechanism at room temperature (i.e. shear banding), where meta-dislocation-assisted deformation is almost absent. In order to analyze the effectiveness of the Al62.5Cu25Fe12.5 quasicrystals as reinforcing agent in metal matrix composites, Al-based composites were synthesized by hot extrusion of elemental Al blended with different amounts of Al62.5Cu25Fe12.5 quasicrystalline particles. The work was focused on two specific aspects: evaluation of the mechanical properties through room temperature compression tests and modeling of the resulting properties. The addition of the quasicrystalline reinforcement is very effective for improving the room temperature mechanical properties of pure Al. The compressive strength increases from 155 MPa for pure Al to 330 and 407 MPa for the composites with 20 and 40 vol.% of reinforcement, respectively, reaching an ultimate strain of 55 % and 20 % before fracture occurs. These results indicate that the addition of the QC reinforcement leads to composite materials with compressive strengths exceeding that of pure Al by a factor of 2 – 2.5, while retaining appreciable plastic deformation. The mechanical properties of the composites have been modeled by taking into account the combined effect of load bearing, dislocation strengthening and matrix ligament size effects. The calculations are in very good agreement with the experimental results and reveal that the reduction of the matrix ligament size, which results in a similar strengthening effect as that observed for grain refinement, is the main strengthening mechanism in the current composites. Finally, the interfacial reaction between the Al matrix and the QC reinforcement has been used to further enhance the strength of the composites through the formation of a new microstructure consisting of the Al matrix reinforced with Al7Cu2Fe w-phase particles. The optimization of the structure-property relationship was done through the systematic variation of the processing temperature during consolidation. The mechanical behavior of these transformation-strengthened composites is remarkably improved compared to the parent material. The yield strength of the composites significantly increases as the Al + QC -> ω transformation progresses from 195 MPa for the sample reinforced only with QC particles to 400 MPa for the material where the Al + QC -> ω reaction is complete. These results clearly demonstrate that powder metallurgy, i.e. powder synthesis by ball milling followed by consolidation into bulk specimens, is an attractive processing route for the production of novel and innovative lightweight composites characterized by high strength combined with considerable plastic deformation. In addition, these findings indicate that the mechanical behavior of Al-based composites reinforced with Al62.5Cu25Fe12.5 quasicrystalline particles can be tuned within a wide range of strength and plasticity depending on the volume fraction of the reinforcement as well as on the extent of the interfacial reaction between Al matrix and QC reinforcing particles.