Lightweight aluminium-silicon alloy is an attractive material for making engine cylinders in automobiles. It imparts good power to weight ratio to the engine. High silicon containing aluminium alloys are used in current engine block castings where the bore surface is etched or honed to partially expose the silicon particles to provide the primary contact between the piston ring and certain regions of the piston and the cylinder. Piston reversal near the top dead centre however causes starvation of lubrication which leads to wear. To explore the wear behaviour of etched aluminium-silicon alloys under nominally dry conditions and extreme lubricated conditions, a host of mechanical and spectroscopic techniques are used here to characterize mechanical and chemical changes caused by wear. In the absence of complex chemical transformations on the wear surface in dry condition, allows a close examination of surface and subsurface microstructures. Given this understanding of the wear under dry condition, we explore the effect of boundary lubrication, where chemical transformations leading to surface modifications are involved. In dry sliding tribology of aluminium-silicon alloy slid against a steel ball four stages of wear are identified; ultra-mild wear, mild wear, severe wear and post severe oxidative wear. In the ultra-mild wear regime silicon particles bears the load. Transition to mild wear occurs when the protruded silicon particles disappear(by sinking and fracture) under higher pressure and sliding. The sinking of silicon particles under normal loading is further investigated using a naoindenter. It is found that the resistance to sinking of such particles into the matrix increases with the unexposed surface area to the buried volume of the particles. In that sense, small particles are seen to provide the stiffest resistance to sinking. While in ultra-mild wear regime the basic energy dissipation mechanism is sinking/tilting, in mild wear regime the subsurface is either in an elastic or an incipiently plastic state. Subsurface plasticity in mild wear regime leads to a grain refinement, fracture of silicon and nucleation of cracks at silicon-matrix interfaces but does not promote large scale flow of the matrix. Transition to severe wear occurs when the contact pressure exceeds the plastic shakedown limit. Under this condition gross plasticity leads to a severe fragmentation of silicon particles and the fragmented silicon are transported by the matrix as it undergoes incremental straining with each cyclic contact at the asperity level. A large reduction in the inter-particle distance com-pared to that in a milder stage of wear, gives rise to high strain gradients in the severe wear regime which contribute to the enhancement of dislocation density. The resulting regions of very high strains at the boundaries of the recrystallised grains as well as within the subgrains lead to the formation of microvoids/ cracks. This is accompanied by the formation of brittle oxides at these subsurface inter-faces due to enhanced diffusion of oxygen. We believe that the abundance of such microcracks in the near surface region, primed by severe plastic deformation, is what distinguishes a severe wear regime from that in the mild wear. The transition from severe wear to post severe oxidative wear is thermally induced and it transfers the metal to metal contact interaction to metal to ceramic interaction. A thick oxide layer is abraded and spalls while the metal underneath continues to flow and delaminate. A study of lubricated tribology of ultra-mild and mild wear regime of aluminium-silicon alloy shows that the initial stages of sliding friction is controlled by the abrasion of the steel pin by the protruding silicon particles of the aluminium-silicon disc. Thegeneration of nascent steel chips helps to breakdown the additive in the oil by a cationic exchange that yields chemical products of benefits to the tribology. The friction is initially controlled by abrasion, but the chemical products gain increasing importance in controlling friction with sliding time. After long times, depending on the contact pressure, the chemical products determine sliding friction exclusively. In the mild wear chemically induced low friction is achieved in short periods of time whereas in ultra-mild wear regime it takes very long time to reach this low friction state. While the basic dissipation mechanisms are the same in the ultra-mild wear and mild wear regimes ,the matrix remains practically unworn in the low pressure ultra-mild wear regime. In the higher pressure mild wear regime at long sliding times a small but finite wear rate prevails. Incipient plasticity in the subsurface controls the mechanism of wear.

No description available.

No presente trabalho quatro ligas Al-Si hipereutéticas, três das quais foram produzidas por conformação por \"spray\" e a outra por fundição, foram caracterizadas quanto a textura, dureza, microestrutura e resistência à corrosão em meio de condensado sintético automotivo (CSA). Duas das ligas conformadas por \"spray\" foram retiradas de camisas de cilindro e a outra de um pré-formado obtido em laboratório. A conformação por \"spray\" envolve a atomização de uma liga e a deposição de gotículas em um substrato, antes mesmo que todas se encontrem no estado sólido. Este processo permite a obtenção de materiais que se caracterizam por uma microestrutura livre de macrossegregações e bastante refinada, implicando melhor trabalhabilidade a quente. A caracterização da microestrutura das quatro ligas hipereutéticas revelou a presença de porosidades na liga obtida em laboratório, e microestrutura com distribuição homogênea de precipitados primários nas três ligas conformadas por \"spray\". A microestrutura de uma das ligas apresentou-se muito diferenciada, com a presença de eutético, sugerindo que esta foi fabricada por fundição. Nas camisas de cilindro foram feitas medidas de rugosidade, e em todas as ligas foram realizados ensaios de microdureza. A liga conformada por \"spray\" e obtida em laboratório foi laminada a quente e a frio. Foram realizados também estudos de textura, para tentar estabelecer uma correlação entre todas as ligas quanto ao processo de fabricação. A avaliação da textura indicou que a presença de fases de silício primário, finamente distribuídas impedem o aparecimento de texturas típicas de deformação de ligas de alumínio, mesmo após severas deformações, como as necessárias para a transformação de pré-formados em tubos que originam as camisas de cilindro. As medidas de rugosidade indicaram características próprias do acabamento superficial usado para a produção das camisas, por brunimento ou por ataque químico. Os ensaios de microdureza apresentaram variações de acordo com as rotas de fabricação sendo que a liga eutética apresentou os maiores valores de microdureza em comparação às ligas conformadas por \"spray\". Todas as ligas foram avaliadas quanto a resistência à corrosão por ensaios de espectroscopia de impedância eletroquímica em dois meios, CSA com pH 3,3 e CSA com pH 11. As quatro ligas hipereutéticas estudadas apresentaram mecanismo de corrosão similar em condensado sintético automotivo (CSA) pH 3,3. Em todas ocorreu o ataque intenso da matriz de alumínio e as partículas de silício primário atuaram como regiões catódicas. A liga 2 apresentou maior resistência à corrosão entre todas as ligas ensaiadas, tanto em CSA pH 3,3 como em pH 11. Neste último meio, uma camada de produtos de corrosão formou-se sobre todas as ligas, e os resultados indicaram mecanismos diferentes para o ataque da matriz de Al e para o crescimento da camada depositada na superfície das ligas estudadas. O ataque da matriz da liga 2 neste meio foi aparentemente mais lento do que sobre as demais ligas, com a formação de uma camada mais compacta de produtos de corrosão, estabelecendo um controle por difusão dos processos interfaciais para maiores períodos de ensaio. A camada formada sobre as demais ligas neste meio apresentou-se mais defeituosa, e nestas ocorreu também menor controle da velocidade das reações interfaciais por processos difusionais. / In the present study four hypereutectic Al-Si alloys, three produced by spray forming and one by casting, were characterized for microhardness, roughness, microstructure, texture and corrosion resistance in a synthetic automotive condensed solution (SACS). Two of the spray formed alloys tested were obtained from cylinder liners and the other was laboratory made. Spray forming involves alloy atomization and droplets deposition on a substrate, previous to the solidification of all of the droplets. This process favours the production of materials with a fine microstructure free of macrosegregation that is related to improved hot workability. The microstructure characterization of the four alloys revealed the presence of porosities in the laboratory made alloy. All the three alloys produced by spray forming showed a homogeneous distribution of primary precipitates. The microstructure of one of the alloys showed eutectic microstructure, indicating that this alloy was fabricated by casting. In the cylinder liners, the surface roughness was measured and the microhardness of all the alloys was also evaluated. Furthermore, the laboratory made alloy was hot and cold rolled. Texture determinations were carried out to investigate the correlation between the alloy type and their fabrication process. The texture investigation indicated that the fine distribution of primary silicon phase in the alloy hindered the development of texture typical of aluminium alloys deformation, even after severe mechanical work, such as those used in the conversion of pre-formed in cylinder liners. The surface roughness results indicated typical characteristics of the surface finishing used, honing or chemical etching. The microhardness results were dependent on the fabrication process used, with higher microhardness associated to the eutectic alloy comparatively to the spray formed ones. All hypereutectic alloys were tested for corrosion resistance using electrochemical impedance spectroscopy in two electrolytes, SACS with pH 3.3 and SACS with pH 11. The four tested alloys showed similar corrosion mechanisms in the acid electrolyte (SACS pH 3.3). The intense attack of the aluminium matrix occurred in ali tested alloys and the primary silicon phase was unattacked and appeared as emerging from the surface after corrosion immersion test. The primary silicon particles acted as cathodic sites. The alloy 2 showed the highest corrosion resistance among the tested alloys in both electrolytes, SACS pH 3.3 and SACS pH 11. In this last medium, a layer of corrosion products formed on all the alloys, and the results indicated different mechanisms for the aluminium matrix corrosive attack and growth of the deposited layer on the alloys surface. The kinetics of aluminium matrix attack was apparently slower in the alloy 2 than for the other alloys, resulting in the formation of a more compact layer of corrosion products, leading to diffusion controlled interfacial processes for longer test periods. The layer of corrosion products on the other three alloys (1, 3, and 4) had more defects and for these alloys diffusional controlled interfacial processes were not as significant as for alloy 2.

Using bandgap engineering, silicon-germanium (SiGe) BiCMOS technology effectively combines III-V transistor performance with the cost and integration advantages associated with CMOS manufacturing. The suitability of SiGe technology for cryogenic and radiation-intense environments is well known, yet SiGe has been generally overlooked for applications involving extreme high temperature operation. This work is an investigation into the potential capabilities of SiGe technology for operation up to 300°C, including the development of packaging and testing procedures to enable the necessary measurements. At the device level, SiGe heterojunction bipolar transistors (HBTs), field-effect transistors (FETs), and resistors are verified to maintain acceptable functionality across the temperature range, laying the foundation for high temperature circuit design. This work also includes the characterization of existing bandgap references circuits, redesign for high temperature operation, validation, and further optimization recommendations. In addition, the performance of temperature sensor, operational amplifier, and output buffer circuits under extreme high temperature conditions is presented. To the author's knowledge, this work represents the first demonstration of functional circuits from a SiGe technology platform in ambient temperatures up to 300°C; furthermore, the optimized bandgap reference presented in this work is believed to show the best performance recorded across a 500°C range in a bulk-silicon technology platform.

Made available in DSpace on 2016-12-08T17:19:17Z (GMT). No. of bitstreams: 1 introducao 1.pdf: 60637 bytes, checksum: 290595bc9c94456b344557782acd7d97 (MD5) Previous issue date: 2012-02-29 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The properties of aluminum-silicon alloys are strongly dependent on the casting process used, the chemical additions made to control eutectic structure, primary silicon and grain structure, and molten metal treatment to reduce hydrogen gas content and to remove inclusions. Modification treatments transform the flake eutectic silicon into a fibrous form producing a structure with increased ultimate tensile strength, ductility, hardness, and machinability. Elements in groups I and II and the rare earths europium, lanthanum, cerium, praseodymium, and neodymium modify, but only sodium and strontium produce a strong modifying action at the low concentration required for commercial application. In this investigation, the effect of strontium concentration on the modification of the eutectic silicon in the 356 alloy was studied. For this porpoise the 356 alloy in as-cast and modified conditions using different Sr concentrations were examined. The results were accessed by tensile tests and metallographic examinations. As evaluated the effect of strontium in the formation temperature and the supercoiling of eutectic Al-Si through DTA. The results indicate that the Sr content of from 0 012% by weight resulted in total of Si modification with substantial increases in the toughness of the alloy 356, and supercoiling of 7.1 ° C temperature of the eutectic Al-Si. The indication of from 0.031% by weight mechanical properties, and temperature of the eutectic microstructure way similar to the alloys of the semi - modified but still higher than the same properties of the alloy without modification. / A resistência mecânica e a qualidade de ligas fundidas alumínio-silício são determinadas pela microestrutura e pela sanidade interna das peças fundidas. Tratamentos de refino de grão e de modificação do silício causam alterações microestruturais que resultam em melhorias nas propriedades mecânicas das ligas Al-Si de fundição. O tratamento de modificação altera a forma do silício do eutético da forma acicular para forma fibrosa interferindo sobre o comportamento mecânico da liga. Diversos tipos de modificadores são descritos na literatura, os mais utilizados são estrôncio e o sódio, pois apresentam efeitos de modificação adequados para as baixas concentrações requeridas. O estrôncio é o mais empregado em fundições, em função da maior facilidade no manuseio e uma maior resistência ao desvanecimento. Entretanto, adições de Sr estão associadas com a formação da porosidade em ligas modificadas. O principal objetivo deste estudo é avaliar a influência de diferentes percentuais de estrôncio sobre a morfologia e a distribuição das partículas de Si na matriz e os efeitos destas alterações sobre as propriedades mecânicas. Também foi avaliado o efeito do estrôncio na temperatura de formação e no superesfriamento do eutético Al-Si através de DTA. Os resultados obtidos indicam que teores de Sr a partir de 0, 012% em peso resultaram na modificação total do Si, com incrementos consideráveis na ductilidade da liga 356 e superesfriamento de 7,1 °C na temperatura do eutético Al-Si. Com valores a partir de 0,031% em peso as propriedades mecânicas, microestrutura e temperatura do eutético apresentavam semelhança com as das ligas semi-modificadas, porém superiores à condição sem modificação.

Submitted by Mery Piedad Zamudio Igami (mery@ipen.br) on 2017-03-10T16:45:35Z No. of bitstreams: 0 / Made available in DSpace on 2017-03-10T16:45:35Z (GMT). No. of bitstreams: 0 / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / O presente estudo foi realizado para verificar a possibilidade de redução do núcleo do reator IEA-R1 do IPEN/CNEN-SP. Cálculos neutrônicos foram desenvolvidos para um conjunto de novas configurações para que, a posteriori, a análise termo-hidráulica e de segurança pudessem ser realizadas. As novas configurações analisadas são menores por diversos motivos, como obter uma melhor utilização do combustível, melhor distribuição dos fluxos de nêutrons, dentre outros. Para que se possa atingir tais configurações, a densidade de Urânio no combustível deve ser aumentada. Neste estudo, combustíveis de U3Si2-Al com 4,8gU/cm3 foram testados e novos núcleos para o reator IEA-R1 foram propostos e discutidos. A análise neutrônica não impõe restrições aos núcleos estudados. A análise termohidráulica mostrou que as margens de segurança e os perfis de temperatura ao longo das placas combustíveis não excedem os limites de projeto. Os coeficientes de temperatura obtidos para os novos núcleos, no caso isotérmico, são todos negativos, conforme desejado. A queima mostrou que núcleos supercompactos não apresentam excesso de reatividade suficiente para o funcionamento dos mesmo, ao se utilizar combustíveis com 4,8gU/cm3. Um APR (Acidente de Perda de Refrigerante) foi simulado para os núcleos remanescentes. A ruptura da fronteira do primário se mostrou o acidente mais crítico, devido ao curto tempo para o esvaziamento completo da piscina do reator. As temperaturas atingidas após o descobrimento foram calculadas e não excedem aquelas cujos valores propiciam empolamento nas placas combustíveis (475 °! a 550 °!), uma vez que se obedeça os tempos de esvaziamento seguro da piscina para as novas configurações. / Tese (Doutorado em Tecnologia Nuclear ) / IPEN/D / Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP / FAPESP: 11/17090-7

No presente trabalho quatro ligas Al-Si hipereutéticas, três das quais foram produzidas por conformação por \"spray\" e a outra por fundição, foram caracterizadas quanto a textura, dureza, microestrutura e resistência à corrosão em meio de condensado sintético automotivo (CSA). Duas das ligas conformadas por \"spray\" foram retiradas de camisas de cilindro e a outra de um pré-formado obtido em laboratório. A conformação por \"spray\" envolve a atomização de uma liga e a deposição de gotículas em um substrato, antes mesmo que todas se encontrem no estado sólido. Este processo permite a obtenção de materiais que se caracterizam por uma microestrutura livre de macrossegregações e bastante refinada, implicando melhor trabalhabilidade a quente. A caracterização da microestrutura das quatro ligas hipereutéticas revelou a presença de porosidades na liga obtida em laboratório, e microestrutura com distribuição homogênea de precipitados primários nas três ligas conformadas por \"spray\". A microestrutura de uma das ligas apresentou-se muito diferenciada, com a presença de eutético, sugerindo que esta foi fabricada por fundição. Nas camisas de cilindro foram feitas medidas de rugosidade, e em todas as ligas foram realizados ensaios de microdureza. A liga conformada por \"spray\" e obtida em laboratório foi laminada a quente e a frio. Foram realizados também estudos de textura, para tentar estabelecer uma correlação entre todas as ligas quanto ao processo de fabricação. A avaliação da textura indicou que a presença de fases de silício primário, finamente distribuídas impedem o aparecimento de texturas típicas de deformação de ligas de alumínio, mesmo após severas deformações, como as necessárias para a transformação de pré-formados em tubos que originam as camisas de cilindro. As medidas de rugosidade indicaram características próprias do acabamento superficial usado para a produção das camisas, por brunimento ou por ataque químico. Os ensaios de microdureza apresentaram variações de acordo com as rotas de fabricação sendo que a liga eutética apresentou os maiores valores de microdureza em comparação às ligas conformadas por \"spray\". Todas as ligas foram avaliadas quanto a resistência à corrosão por ensaios de espectroscopia de impedância eletroquímica em dois meios, CSA com pH 3,3 e CSA com pH 11. As quatro ligas hipereutéticas estudadas apresentaram mecanismo de corrosão similar em condensado sintético automotivo (CSA) pH 3,3. Em todas ocorreu o ataque intenso da matriz de alumínio e as partículas de silício primário atuaram como regiões catódicas. A liga 2 apresentou maior resistência à corrosão entre todas as ligas ensaiadas, tanto em CSA pH 3,3 como em pH 11. Neste último meio, uma camada de produtos de corrosão formou-se sobre todas as ligas, e os resultados indicaram mecanismos diferentes para o ataque da matriz de Al e para o crescimento da camada depositada na superfície das ligas estudadas. O ataque da matriz da liga 2 neste meio foi aparentemente mais lento do que sobre as demais ligas, com a formação de uma camada mais compacta de produtos de corrosão, estabelecendo um controle por difusão dos processos interfaciais para maiores períodos de ensaio. A camada formada sobre as demais ligas neste meio apresentou-se mais defeituosa, e nestas ocorreu também menor controle da velocidade das reações interfaciais por processos difusionais. / In the present study four hypereutectic Al-Si alloys, three produced by spray forming and one by casting, were characterized for microhardness, roughness, microstructure, texture and corrosion resistance in a synthetic automotive condensed solution (SACS). Two of the spray formed alloys tested were obtained from cylinder liners and the other was laboratory made. Spray forming involves alloy atomization and droplets deposition on a substrate, previous to the solidification of all of the droplets. This process favours the production of materials with a fine microstructure free of macrosegregation that is related to improved hot workability. The microstructure characterization of the four alloys revealed the presence of porosities in the laboratory made alloy. All the three alloys produced by spray forming showed a homogeneous distribution of primary precipitates. The microstructure of one of the alloys showed eutectic microstructure, indicating that this alloy was fabricated by casting. In the cylinder liners, the surface roughness was measured and the microhardness of all the alloys was also evaluated. Furthermore, the laboratory made alloy was hot and cold rolled. Texture determinations were carried out to investigate the correlation between the alloy type and their fabrication process. The texture investigation indicated that the fine distribution of primary silicon phase in the alloy hindered the development of texture typical of aluminium alloys deformation, even after severe mechanical work, such as those used in the conversion of pre-formed in cylinder liners. The surface roughness results indicated typical characteristics of the surface finishing used, honing or chemical etching. The microhardness results were dependent on the fabrication process used, with higher microhardness associated to the eutectic alloy comparatively to the spray formed ones. All hypereutectic alloys were tested for corrosion resistance using electrochemical impedance spectroscopy in two electrolytes, SACS with pH 3.3 and SACS with pH 11. The four tested alloys showed similar corrosion mechanisms in the acid electrolyte (SACS pH 3.3). The intense attack of the aluminium matrix occurred in ali tested alloys and the primary silicon phase was unattacked and appeared as emerging from the surface after corrosion immersion test. The primary silicon particles acted as cathodic sites. The alloy 2 showed the highest corrosion resistance among the tested alloys in both electrolytes, SACS pH 3.3 and SACS pH 11. In this last medium, a layer of corrosion products formed on all the alloys, and the results indicated different mechanisms for the aluminium matrix corrosive attack and growth of the deposited layer on the alloys surface. The kinetics of aluminium matrix attack was apparently slower in the alloy 2 than for the other alloys, resulting in the formation of a more compact layer of corrosion products, leading to diffusion controlled interfacial processes for longer test periods. The layer of corrosion products on the other three alloys (1, 3, and 4) had more defects and for these alloys diffusional controlled interfacial processes were not as significant as for alloy 2.

The present thesis deals with Nb-Si alloy composites in both bulk and multilayer forms. The work has been divided into two parts. First part (chapter 4-6) deals with Nb based silicides binary and ternary alloys with alloying additions like Ga and Al. These alloys are synthesized by vacuum arc melting and suction casting (non-equilibrium processing techniques). The studies on intermetallic coatings of Nb-Si alloys and Nb/Si multilayer synthesized by pulsed laser deposition technique have been presented in the second part (chapter7-8). Nb-Si alloys are one of the candidate materials for the advanced structural and microelectronic applications. There are few issues with these materials like poor oxidation resistance, low fracture toughness and brittleness which need to be solved. Microstructure plays a crucial role to control these properties. The main focus of this work is to understand the process of phase transformation and thereby control the microstructure in both bulk alloys and thin films. We have also investigated in a limited manner mechanical and environmental properties of bulk alloys. This thesis is subdivided into nine chapters. After a brief introduction in the first chapter, a brief overview on Nb-Si phase diagram and literature reviews on Nb-Si based alloys are presented with emphasis on the current work in the second chapter. Literature reviews on the phase formations sequence and stability in Nb-Si alloys thin films and Nb/Si multilayers are also discussed in the same chapter. In the third chapter different experimental techniques, processing parameters and characterization tools like XRD, SEM, TEM etc. are briefly discussed. Special emphasis is given on two non-equilibrium techniques: laser deposition technique to deposit the thin film/multilayer and vacuum suction casting to produce the 3 mm diameter rods of different Nb-Si alloys. The fourth chapter discusses the microstructural aspects of Nb-Si alloys prepared by suction casting and its mechanical behavior. The samples have the compositions hypoeutectic (Nb-10at.%Si and Nb-14at.%Si), eutectic (Nb-18.7at.%Si) and hypereutectic (Nb-22at.% Si and Nb-25at.% Si). SEM microstructural analyses of all the samples clearly show the enhancement in the volume fraction of eutectic and decease in the eutectic spacings in microstructure due to large undercooling. Rod eutectic is observed in most of places with irregular eutectic a few places in all samples. First check of phases has been done by XRD in all samples. Phase confirmation using TEM showed the eutectic between Nbss and Nb3Si phases in all samples. The primary phase for hypoeutectic alloys is Nbss (dendritic structure), Nb3Si phase for eutectic composition and β-Nb5Si3 phase for hypereutectic alloys. Compositional analysis using EDS and EPMA also supported the above results. No signature of eutectoid reaction (Nb3Si→Nb+α-Nb5Si3) is observed. Mechanical properties like hardness, strength, ductility and indentation fracture toughness have been determined for above mention alloy compositions. SEM micrographs showed that silicides fractured by cleavage and Nb phase in a ductile manner during the compression tests carried out at room temperature. We attempt to explain how the above mention mechanical properties change with alloy compositions and processing. Chapter five deals with the effect of Ga addition on the microstructure and mechanical properties of the Nb-Si alloy. The composition selected for this study is Nb-20.2at.%Si-2.7at.%Ga. The results of ternary alloy have been compared with the binary alloy composition Nb-18.7at.%Si. Phase analysis has been carried out using TEM and XRD. Ga addition has suppressed the formation of Nb3Si phase and promoted the formation of β-Nb5Si3 phase. Ga addition also established the eutectic between Nbss and β-Nb5Si3, which is a metastable eutectic. Ga added ternary alloy, on suction casting, yields ultrafine eutectic with nanometer length scale (50-100nm). From the compression tests, it is concluded that the combination of ultrafine eutectic (Nbss-β-Nb5Si3) and primary β-Nb5Si3 in ternary alloy results in a high compressive strength ~2.8±0.1 GPa with 4.3% plasticity. In contrast binary alloy under identical conditions shows the compressive strength ~1.35±0.1 GPa and 0.2% plasticity. Ga addition also enhances the indentation fracture toughness from 9.2±0.05 MPa√m (binary) to 24.11±0.5 MPa√m (ternary). Composite hardness values of the ternary and binary alloys are 1064±20 Hv and 1031±20 Hv respectively. Chapter six deals with Al added Nb-Si ternary alloy. Here we have discussed microstructural and mechanical properties like in chapter 5 along with oxidation behavior for the alloy composition Nb-12.7at.%Si-9at.%Al. SEM micrograph shows the presence of primary dendrites structure with ultra fine lamellar eutectic (50-100nm). Detailed TEM studies confirm the Nbss as primary phase present in form of dendrites. These dendrites contain the plate shape precipitates of δ-Nb11Si4 (body centered orthorhombic structure) phase in Nb matrix (primary dendrites). Eutectic phases are Nbss and β-Nb5Si3. The analysis of the results indicates that Al addition promote the formation of β-Nb5Si3 phase in the eutectic. The results of this ternary composition were also compared with the binary alloy composition Nb-18.7at.%Si. Compression tests have been carried out at room and elevated temperatures to measure the strength of the material. Al added ternary alloy yields the compressive strength value 1.6±0.01 GPa whereas binary alloy yields the compressive strength value 1.1±0.01 GPa. Enhancement in indentation fractured toughness is observed in Al added ternary alloy (20.4±0.5MPa√m) compare to binary alloy (9.2±0.05 MPa√m). Thermal analysis by TGA and DTA were used to see the oxidation behavior of Al added ternary alloy. Chapter seven deals with the deposition characteristics and the TEM studies on the laser deposited Nb-Si thin films. Films were deposited on the NaCl crystals and Si single crystal substrates. The compositions chosen in this case are Nb-25at.%Si, Nb-37.5at.%Si and Nb-66.7at.%Si. These compositions correspond to the equilibrium intermetallic compounds Nb3Si, Nb5Si3 and NbSi2 respectively. In this chapter we have briefly discussed the microstructural and phase evolutions in the intermetallic coatings. The smooth films quenched from the vapor and/or plasma state show amorphous structure. The sequence of crystallization was studied by hot stage TEM experiments as well as by cross sectional TEM in the films deposited at the elevated temperatures (600oC and 700oC) on Si substrates. During the hot stage experiment, crystallization is observed in Nb-25at.%Si film around 850oC with nucleation of metastable cubic Nb3Si phase. Occasionally metastable hexagonal Nb3Si3 phase has also been observed (close to Si substrate) along with cubic Nb3Si phase in the films at elevated temperatures. For Nb-37.5at.%Si film, crystallization is observed at 800oC with the nucleation of grains of metastable hexagonal Nb5Si3 phase. Cross-sectional TEM shows the presence of hexagonal Nb5Si3 phase along with few grains of NbSi3 (equilibrium) phase in the films deposited at elevated temperatures. Hot stage experiment of Nb-66.3at.%Si film showed the onset of crystallization much earlier at 400oC and complete crystallization at 600oC. This crystallization leads to the nucleation of grains of NbSi2 phase. Films of this composition deposited at elevated temperatures showed the presence of NbSi2 and metastable hexagonal Nb5Si3 phases (occasionally). The laser ablated films, besides the film matrix also contain the micron and submicron sized spherical droplets of different sizes. These droplets travel at very high velocities and impinge on the substrate resulting in a very high rate of heat transfer during solidification from liquid state. Therefore in this work we have also studied the microstructural evolution in the droplets for each composition. The phases observed in the droplets embedded in the matrix of Nb-25 at% Si alloy film are the bcc Nb and the cubic Nb3Si (metastable phase). The droplets in the matrix of Nb-37.5 at% Si alloy showed the bcc Nb and tetragonal β-Nb5Si3 phases. The phases observed in the droplets of in the Nb-66.3at.%Si alloy are the bcc Nb, tetragonal β-Nb5Si3 and the hexagonal NbSi2 (metastable phase). Chapter eight describes the synthesis and microstructural characterization using TEM of Nb/Si multilayers. The aim of this work is to check the stability and phase formation sequence in Nb/Si multilayer. Nb/Si multilayers were first annealed at different time intervals at 600oC and at different temperatures (for 2 hours) and then characterized by the cross-sectional transmission electron microscopy. As-deposited Nb layer is crystalline while Si layer is amorphous. Microstructural and compositional evidences suggest the intermixing between the Nb and Si layers at the interfaces. Nb/Si multilayer annealed at 600oC for 1 hour, NbSi2 was identified as the first crystalline nucleating phase. However amorphous silicide layers were also observed between Nb and NbSi2 layers. Metastable hexagonal Nb5Si3 was identified as the next crystalline phase that nucleated from the amorphous silicide layers at the interfaces of Nb and NbSi2 layers. Occasionally few grains of cubic Nb3Si phase were also observed after 8 hours of annealing at 600oC. In the chapter we have compared the results to the other reported works in Nb-Si bulk diffusion couples and also thin film couples. The final chapter summarizes the major conclusions of the present work and scope of future work.

Aim of the present work was to explore the possibility of improving strength of cast Mg by alloying additions, viz., Si and Zn+Al. All the alloys were produced by squeeze casting technique using squeeze pressure of 12MPa and their microstructure, tensile and corrosion properties were studied. Mg-Si system was chosen because the intermetallic compound Mg2Si possesses many desirable properties, such as, low density, high hardness, high melting point. Hence, there is scope for improving the strength of Mg by dispersion of primary Mg2Si particles. Addition of Si to Mg resulted in the formation of �-Mg, particles of primary Mg2Si and eutectic as microstructural constituents. The morphology of primary Mg2Si changed from polyhedral shaped particles to dendrites as Si content was increased from 3.57 to 5.5 wt%. Volume fraction of primary Mg2Si increased with increase in Si content. Particle size of primary Mg2Si also increased with increase in silicon content but at the same time it was found to be dependent on melt temperature, i.e., a lower particle size was obtained at higher melt temperatures. Addition of Al and Sr was made to Mg-2Si alloy in order to further increase the strength by solid solution strengthening and refinement/modification of primary Mg2Si particles/eutectic. Addition of 1.2 wt% Al to Mg-2Si alloy resulted in irregular type of morphology of Mg2Si particles and increased particle size. Addition of 0.2 wt% SrtoMg-2Si-1.2Al alloy resulted in slight refinement of primary Mg2Si particles and modification of eutectic. Addition of 0.4 wt% Sr resulted in both refinement and restoration of morphology of Mg2Si particles from irregular to polyhedral shape. This was accompanied by destruction of eutectic, and rods containing Mg, Si, Al and Sr were observed. The addition of 1.33 wt%Si to Mg resulted in improvement in 0.2%PS by about 80 MPa,UTS by about 40MPa and these values did not change much till the addition of 3.57 wt% Si. A drop in the strength values was observed at Si content of 5.5 wt%,where transition in morphology of primary Mg2Si occurred from polyhedral to dendrite. Addition of Si resulted in reduction in % elongation by about 2%. The addition of Al and Sr did not change the tensile properties of binary Mg-2Si alloy much. It was concluded that the volume fraction and size of primary Mg2Siparticles obtained with Si addition up to 3.57 wt% did not contribute much to strength and the strengthening mainly came from the eutectic present in the matrix. As Si content was increased to 5.5 wt% in order to increase the volume fraction of primary Mg2Si particles, the morphology of Mg2Si changed to dendritic type resulting in reduction in strength. Thus, the maximum increase in strength is achieved at near eutectic composition,i.e.,intheMg-1.33Sialloy,andfurtherincreaseinstrengthdoesnotseem to be feasible with this alloy system. The ductility of all the Mg-Si based alloys was also low, i.e, 0.5% elongation to fracture or less. Regarding the corrosion behaviour, the addition of Si to Mg deteriorated the corrosion resistance and the addition of Al and Sr further worsened it. Since further improvement in tensile properties did not seem feasible with Mg-Si alloy system, the focus was shifted to Mg-Zn-Al alloy system. There is scope for improvement in strength in Mg-Zn-Al alloy system by solid solution strengthening, grain refinement and precipitation hardening. It was observed that the addition of Zn and Al resulted in microstructure containing α-Mg grains and secondary phase at the grain boundary. XRD analysis showed the secondary phase to be Al5Mg11Zn4 but EDS analysis did not match with this composition. Therefore, the nature of this phase remains uncertain. Addition of 6 wt% Zn and 1 wt% Al resulted in improvement in strength as well as ductility: 0.2%PS improved by about 70 MPa, UTS by about 100 MPa and % elongation by about 7%. Addition of small amounts of Caresultedinrefinementofmicrostructurecausingimprovementinstrengthwithout much decrease in % elongation. Increase in Al content from 1 to 4 wt% resulted in increase in 0.2%PS but UTS slightly decreased, as % elongation reduced. Alloys subjected to T6 heat treatment showed improvement in strength but slight reduction in % elongation. ZA64 alloy in T6 condition gave 130 MPa 0.2%PS, 225 MPa UTS and 4.9% elongation, which are much higher tensile properties as compared Mg-Si alloys. All the three mechanisms mentioned above contribute to the strengthening. There is scope for further improvement in strength by employing a more suitable heat treatment. Regarding corrosion behaviour, addition of 6 wt% Zn and 1 wt% of Al to Mg did not deteriorate its corrosion resistance much. Addition of small amounts of Ca was found to be beneficial for corrosion resistance, whereas an increase in Al content lowered the corrosion resistance. Heat treatment also reduced the corrosion resistance.

This thesis investigates the effects of low temperatures on Silicon Germanium (SiGe) Hterojunction Bipolar Transistors (HBT) BiCMOS technology. A comprehensive set of dc measurements were taken on first, second, third and fourth generation IBM SiGe technology over a range of temperatures (room temperature to 43K for first generation, and room temperature to 15K for the rest). This work is unique in the sense that this sort of comprehensive study of dc characteristics on four SiGe HBT technology generations over a wide range of temperatures has never been done before to the best of the authors knowledge.