Microwave assisted preparation and sintering of Al2O3, ZrO2 and their composites from metalorganics

Controlled pyrolysis of Al(OBus)(3), Zr(OPrn)(4) and their mixtures in ethyl acetate induced using microwaves of 2.45 GHz frequency has been carried out. Microwave irradiation yields second-stage precursors for the preparation of respective oxides and their composites. It is observed that the microwave irradiation has a directive influence on the morphology of the ultimate oxide products. Al2O3, ZrO2 and the two composites 90% Al2O3-10% ZrO2 and 90% ZrO2-10% Al2O3 are also found to be sintered to very high densities within 35 min of microwave irradiation by the use of beta-SiC as a secondary susceptor.

Nanocomposite microstructure in a melt spun Al-Cu-Zr alloy

Rapid solidification of a ternary Al-Cu-Zr alloy results in a nanocomposite microstructure. In this study, melt spinning a Al82Cu15Zr3 alloy has resulted in the combined occurrence of, (a) 0.5 mu m sized grains of Al solid solution and (b) fine grains (10-20 nm) of intermetallic Al2Cu (theta) and alpha-Al, along side each other. The larger alpha-Al grains contain nanometric GP zones, with the Zr addition resulting in a grain refinement. In the other type of microstructure Zr promotes simultaneous nucleation of nanosized grains of the two equilibrium phases, Al2Cu and alpha-Al. Both these lead to a very high hardness of similar to 540 VHN for this alloy and can be used as a candidate for a high strength alloy with good ductility at a low strain rate.

The effect of SiC particles on the size and morphology of eutectic silicon in cast A356/SiCp composites

Properties of cast aluminium matrix composites are greatly influenced by the nature of distribution of reinforcing phase in the matrix and matrix microstructural length scales, such as grain size, dendrite arm spacing, size and morphology of secondary matrix phases, etc. Earlier workers have shown that SIC reinforcements can act as heterogeneous nucleation sites for Si during solidification of Al-Si-SiC composites. The present study aims at a quantitative understanding of the effect of SiC reinforcements on secondary matrix phases, namely eutectic Si, during solidification of A356 Al-SiC composites. Effect of volume fraction of SiC particulate on size and shape of eutectic Si has been studied at different cooling rates. Results indicate that an increase in SiC volume fraction leads to a reduction in the size of eutectic Si and also changes its morphology from needle-like to equiaxed. This is attributed to the heterogeneous nucleation of eutectic Si on SiC particles. However, SiC particles are found to have negligible influence on DAS. Under all the solidification conditions studied in the present investigation, SiC particles are found to be rejected by the growing dendrites. (C) 1999 Elsevier Science Ltd. All rights reserved.

MOCVD of aluminium oxide films using aluminiurn beta-diketonates as precursors

Deposition of Al2O3 coatings by CVD is of importance because they are often used as abrading material in cemented carbide cutting tools. The conventionally used CVD process for Al2O3 involves the corrosive reactant AlCl3. In this paper, we report on the thermal characterisation of the metalorganic precursors namely aluminium tristetramethyl-heptanedionate [Al(thd)(3)] and aluminium tris-acetylacetonate [Al(acac)(3)] and their application to the CVD of Al2O3 films. Crystalline Al2O3 films were deposited by MOCVD at low temperatures by the pyrolysis of Al(thd)(3) and Al(acac)(3). The films were deposited on a TiN-coated tungsten carbide (TiN/WC) and Si(100) substrates in the temperature range 500-1100degreesC. The as-deposited films were characterised by x-ray diffraction, optical microscopy, scanning and transmission electron microscopy, Auger electron spectroscopy. The observed crystallinity of films grown at low temperatures, their microstructure, and composition may be interpreted in terms of a growth process that involves the melting of the metalorganic precursor on the hot growth surface.

Influence of matrix characteristics on fracture toughness of high volume fraction Al2O3/Al–AlN composites

The role of matrix microstructure on the fracture of Al-alloy composites with 60 vol% alumina particulates was studied. The matrix composition and microstructure were systematically varied by changing the infiltration temperature and heat treatment. Characterization was carried out by a combination of metallography, hardness measurements, and fracture studies conducted on compact tension specimens to study the fracture toughness and crack growth in the composites. The composites showed a rise in crack resistance with crack extension (R curves) due to bridges of intact matrix ligaments formed in the crack wake. The steady-state or plateau toughness reached upon stable crack growth was observed to be more sensitive to the process temperature rather than to the heat treatment. Fracture in the composites was predominantly by particle fracture, extensive deformation, and void nucleation in the matrix. Void nucleation occurred in the matrix in the as-solutionized and peak-aged conditions and preferentially near the interface in the underaged and overaged conditions. Micromechanical models based on crack bridging by intact ductile ligaments were modified by a plastic constraint factor from estimates of the plastic zone formed under indentations, and are shown to be adequate in predicting the steady-state toughness of the composite.

Transient analysis in Al-doped barium strontium titanate thin films grown by pulsed laser deposition

Thin films of (Ba0.5Sr0.5)TiO3 (BST) with different concentrations of Al doping were grown using a pulsed laser deposition technique. dc leakage properties were studied as a function of Al doping level and compared to that of undoped BST films. With an initial Al doping level of 0.1 at. % which substitutes Ti in the lattice site, the films showed a decrease in the leakage current, however, for 1 at. % Al doping level the leakage current was found to be relatively higher. Current time measurements at elevated temperatures on 1 at. % Al doped BST films revealed space-charge transient type characteristics. A complete analysis of the transient characteristics was carried out to identify the charge transport process through variation of applied electric field and ambient temperature. The result revealed a very low mobility process comparable to ionic motion, and was found responsible for the observed feature. Calculation from ionic diffusivity and charge transport revealed a conduction process associated with an activation energy of around 1 eV. The low mobility charge carriers were identified as oxygen vacancies in motion under the application of electric field. Thus a comprehensive understanding of the charge transport process in highly acceptor doped BST was developed and it was conclusive that the excess of oxygen vacancies created by intentional Al doping give rise to space-charge transient type characteristics. © 2001 American Institute of Physics.

Response of Materials during sliding on various surface textures

In the present investigation, basic studies were conducted using Inclined pin-on-plate sliding Tester to understand the role of surface texture of hard material against soft materials during sliding. Soft materials such as Al-Mg alloy, pure Al and pure Mg were used as pins and 080 M40 steel was used as plate in the tests. Two surface parameters of steel plates — roughness and texture — were varied in tests. It was observed that the transfer layer formation and the coefficient of friction which has two components, namely adhesion and plowing component, are controlled by the surface texture of harder material. For the case of Al-Mg alloy, stick-slip phenomenon was absent under both dry and lubricated conditions. However, for the case of Al, it was observed only under lubricated conditions while for the case of Mg, it was observed under both dry and lubricated conditions. Further, it was observed that the amplitude of stick-slip motion primarily depends on plowing component of friction. The plowing component of friction was highest for the surface that promotes plane strain conditions near the surface and was lowest for the surface that promotes plane stress conditions near the surface.

Response of Materials During Sliding on Various Surface Textures

In the present investigation, soft materials, such as Al-4Mg alloy, high-purity Al and pure Mg pins were slid against hard steel plates of various surface textures to study the response of materials during sliding. The experiments were conducted using an inclined pin-on-plate sliding apparatus under both dry and lubricated conditions in an ambient environment. Two kinds of frictional response, namely steady-state and stick-slip, were observed during sliding. In general, the response was dependent on material pair, normal load, lubrication, and surface texture of the harder material. More specifically, for the case of Al-4Mg alloy, the stick-slip response was absent under both dry and lubricated conditions. For Al, stick-slip was observed only under lubricated conditions. For the case of Mg, the stick-slip response was seen under both dry and lubricated conditions. Further, it was observed that the amplitude of stick-slip motion primarily depends on the plowing component of friction. The plowing component of friction was the highest for the surfaces that promoted plane strain conditions and was the lowest for the surfaces that promoted plane stress conditions near the surface.

CO oxidation by CeO(2)-Al(2)O(3)-CeAlO(3) hybrid oxides

A modified solution combustion technique was successfully used to synthesize sub-10 nm crystallites of hybrid CeO(2)-Al(2)O(3)-CeAlO(3). The fuel in the solution combustion was tuned to obtain mixed oxides and solid solutions of the compound. The compounds were characterized by X-ray diffraction, transmission electron microscopy and X-ray photoelectron spectroscopy. XRD and TEM analysis showed the substitution of Al(3+) ions in the CeO(2) matrix when a combination of glycine, urea, hexamine and oxalyl dihydrazide was used as fuel for the synthesis. The compounds showed high activity for CO oxidation and the activity of the compounds was dependent upon the composition of the oxide.

Effect of substrate bias voltage on the structure, electric and dielectric properties of TiO(2) thin films by DC magnetron sputtering

Titanium dioxide (TiO(2)) films have been deposited on glass and p-silicon (1 0 0) substrates by DC magnetron sputtering technique to investigate their structural, electrical and optical properties. The surface composition of the TiO(2) films has been analyzed by X-ray photoelectron spectroscopy. The TiO(2) films formed on unbiased substrates were amorphous. Application of negative bias voltage to the substrate transformed the amorphous TiO(2) into polycrystalline as confirmed by Raman spectroscopic studies. Thin film capacitors with configuration of Al/TiO(2)/p-Si have been fabricated. The leakage current density of unbiased films was 1 x10(-6) A/cm(2) at a gate bias voltage of 1.5 V and it was decreased to 1.41 x 10(-7) A/cm(2) with the increase of substrate bias voltage to -150 V owing to the increase in thickness of interfacial layer of SiO(2). Dielectric properties and AC electrical conductivity of the films were studied at various frequencies for unbiased and biased at -150 V. The capacitance at 1 MHz for unbiased films was 2.42 x 10(-10) F and it increased to 5.8 x 10(-10) F in the films formed at substrate bias voltage of -150 V. Dielectric constant of TiO(2) films were calculated from capacitance-voltage measurements at 1 MHz frequency. The dielectric constant of unbiased films was 6.2 while those formed at -150 V it increased to 19. The optical band gap of the films decreased from 3.50 to 3.42 eV with the increase of substrate bias voltage from 0 to -150 V. (C) 2011 Elsevier B. V. All rights reserved.

Nanostructured titanium-nickel alloys: a comparison of processing routes

Rapid solidification, mechanical alloying and devitrificaiton of precursor metallic glasses are all possible routes for the synthesis of nanocrystals and nanocomposites, though their efficacy is system dependent. In a comprehensive study of alloys across the Ti-Ni phase diagram, nanocrystals of Ti and Ni and nanocomposites of alpha -Ti and Ti sub 2 Ni, Ti sub 2 Ni and TiNi and beta -Ti and glass have been produced. By the addition of Al, devitrification of metallic glasses created by mechanical alloying led to nanocrystalline intermetallic compounds. The evolution of these nanocrystalline microstructures has been rationalized on the basis of thermodynamic and kinetic considerations involving the metastable phase diagram for this system.

Effect of liquid precursor pyrolysis on phase selection in the MgO-MgAl2O4 system

Aqueous solutions of Al and Mg nitrates have been spray pyrolysed at 673 K to synthesize powders with compositions varying between MgO and MgAl2O4. This has been carried out with the aim of studying phase selection and phase evolution in this system. The powders have been subsequently heat treated and the sequence of phases characterised by X-ray diffraction and transmission electron microscopy. Metastable extensions of the different phase fields have been calculated based on functions which predict the equilibrium phase diagram accurately. The appearance of phases is closely related to the temperature and to the non-stoichiometry in different compositional ranges of the system. The sequence of phase evolution has been correlated to the thermodynamics of nucleation in the system.

Structural characterisation of reaction zone for friction stir welded aluminium-stainless steel joint

In the present investigation, commercially pure Al has been joined with 304 stainless steel (SS) by friction stir welding. The assembly finds widespread application in the field of cryogenics, nuclear, structural industries and domestic appliances. Microstructural characterisation was carried out using scanning and transmission electron microscopes. It has been found that diffusion of Fe, Cr and Ni is substantial within Al; however, diffusion of Al within 304SS is limited. Owing to interdiffusion of chemical species across the bondline, discrete islands of Fe3Al intermetallic form within the reaction zone. The rubbing action of tool over the butting edge of 304SS removed fine particles from 304SS, which were embedded in the stirring zone of Al matrix. Subsequently, austenite underwent phase transformation to ferrite due to large strain within this grain. Fracture path mainly moves through stirring zone of Al alloy under tensile loading; however, in some places, presence of Fe3Al compound has been also found.

Synthesis and characterization of carbon-covered alumina (CCA) supported TiO2 nanocatalysts with enhanced visible light photodegradation of Rhodamine B

The anatase phase of titania (TiO2) nano-photocatalysts was prepared using a modified sol gel process and thereafter embedded on carbon-covered alumina supports. The carbon-covered alumina (CCA) supports were prepared via the adsorption of toluene 2,4-diisocyanate (TDI) on the surface of the alumina. TDI was used as the carbon source for the first time for the carbon-covered alumina support system. The adsorption of TDI on alumina is irreversible; hence, the resulting organic moiety can undergo pyrolysis at high temperatures resulting in the formation of a carbon coating on the surface of the alumina. The TiO2 catalysts were impregnated on the CCA supports. X-ray diffraction analysis indicated that the carbon deposited on the alumina was not crystalline and also showed the successful impregnation of TiO2 on the CCA supports. In the Raman spectra, it could be deduced that the carbon was rather a conjugated olefinic or polycyclic hydrocarbons which can be considered as molecular units of a graphitic plane. The Raman analysis of the catalysed CCAs showed the presence of both the anatase titania and D and G band associated with the carbon of the CCAs. The scanning electron microscope micrographs indicated that the alumina was coated by a carbon layer and the energy dispersive X-ray spectra showed the presence of Al, O and C in the CCA samples, with the addition of Ti for the catalyst impregnated supports. The Brunauer Emmet and Teller surface area analysis showed that the incorporating of carbon on the alumina surface resulted in an increase in surface area, while the impregnation with TiO2 resulted in a further increase in surface area. However, a decrease in the pore volume and diameter was observed. The photocatalytic activity of the nanocatalysts was studied for the degradation of Rhodamine B dye. The CCA-TiO2 nanocatalysts were found to be more photocatalytically active under both visible and UV light irradiation compared to the free TIO2 nanocatalysts.

Hardness and Nitrogen Bonding Structure of A(x)Ti(1-x)N/CrN Multilayer Hard Coating

AlxTi1-xN/CrN multilayer coatings were fabricated by magnetron sputtering and those hardness variations were studied by observing the crack propagation and measuring the chemical bonding state of nitrides by Ti addition. While AlN/CrN multilayer shown stair-like crack propagation, AlxTi1-xN/CrN multilayer illustrated straight crack propagation. Most interestingly, Ti addition induced more broken nitrogen bonds in the nitride multilayers, leading to the reduction of hardness. However, the hardness of Al0.25Ti0.75N/CrN multilayer, having high Ti contents, increased by the formation of many Ti-N bond again instead of Al-N bond. From these results, we found that linear crack propagation behavior was dominated by broken nitrogen bonds in the AlxT1-xN/CrN multilayer coatings.