Process parameter dependency on the phase transition from anatase to rutile phase of laser-ablated TiO2 films was investigated. Lower ambient argon pressure, longer deposition time, higher laser fluence, and smaller target–substrate separation give rutile phase from anatase phase at comparatively lower temperature. The relationship between thickness and onset temperature of anatase–rutile transformation can be comprehensively explained in terms of film thickness. Thinner films have higher phase transition temperature. The presence of helium gas during deposition favors the anatase–rutile transition at a temperature lower than that expected from the above relationship.

The nucleation and growth of the c-axis-aligned Yba2Cu3Ox on SrTiO3 and CeO2, from precursor films, were studied by examining quenched and fully processed specimens using transmission electron microscopy techniques. The precursor films, a stoichiometric mixture of fine-grained Y, Cu, and BaF2, were deposited using physical vapor deposition methods. An Y-Ba oxy-fluoride formed from the precursor contributed to the nucleation of Yba2Cu3Ox, while a liquid layer between the unreacted precursor and the Yba2Cu3Ox layer played an important role in the growth of Yba2Cu3Ox. However, the process of nucleation of Yba2Cu3Ox on SrTiO3 and CeO2 were significantly different.

A spray pyrolysis deposition technique has been used to prepare thick films of half-metallic ferromagnet La0.7Ca0.3MnO3 on LaAlO3 (001) and yttria-stabilized zirconia Y–ZrO2 (100) single-crystal substrates. The films deposited on LaAlO3 (001) exhibited a high degree of crystallinity with both in-plane and out-of-plane texture and a very sharp insulator to metal transition at TIM = 270 K. The intrinsic magnetoresistance (MR) reaches 70% at TIM in 3 T, a similar value as in the bulk material of the same composition. The extrinsic intergrain MR, however, is only 0.5% at 40 K in 3 T, 50 times smaller than for the bulk. By contrast, films grown on YSZ single crystals have a broad insulator to metal transition at a lower TIM of approximately 220 K and poor intrinsic MR. They show however an extrinsic MR as large as in the bulk. The extrinsic MR is interpreted as arising from crystalline and magnetic disorder at the grain boundaries.

A phase transformation in an alumina gel provided an elegant means of isolating the effect of filler properties on the wear resistance of particle-reinforced thermosetting polymer–matrix composites. This transformation was useful because it takes place without significantly altering filler porosity. This produced a wear surface apparently reflecting the vermicular growth patterns in the γ-alumina in the δ-aluminum monohydrate matrix. Nucleation of γ-alumina in the gel matrix produced wear rates comparable to commercial composites.

A systematic behavior in the crystal structure parameters of natural, synthetic, carbonate, and non-carbonate apatite is revealed from Rietveld refinements of neutron powder diffraction experiments. The results of this work on synthetic carbonate hydroxyapatites (CHAps) are consistent with the mechanism of carbonate substitution on the mirror plane of the phosphate tetrahedron, as it was introduced for the natural carbonate fluorapatite (CFAp). The present comparison shows that the tetrahedral bond lengths P–O1 and P–O2 decrease by 3–4% in all carbonate apatites. The atomic displacement parameters (ADPs) of the tetrahedral (T) and the O3 sites are greater in the carbonate than in the non-carbonate apatites. The atomic positional disorder of the T site (P/C site) is greater in the CFAp than in the CHAps, while the opposite happens at the O3 sites. Finally, the room-temperature ADPs of all of the atoms in the CFAp and CHAps show the same behavior as in the corresponding non-carbonate materials.

The effect of the mechanical activation of the reactants on the self-propagating high-temperature synthesis (SHS) of titanium silicides was investigated. SHS experiments were performed on reactant powders that were milled for different times. Mechanical activation was shown to have a large influence on the combustion characteristics, particularly on wave speed. A much weaker effect was observed on the products phase composition. Single-phase products were obtained only from Ti:Si = 1:2 and Ti:Si = 5:3 starting compositions. Observation of microstructural evolution in quenched reactions of Ti:Si = 1:2 mixtures milled for relatively long times revealed that the combustion reaction was primarily a solid-state process restricted to a surface layer of the large Ti grains. A secondary process involving a solid–liquid interaction between solid Ti and melted Si was dominant in the post front region. The mechanical activation in this case took the role of increasing the contact surface between the reactants. A single reaction coalescence mechanism involving only liquid phases was proposed for the Ti:Si = 5:3 composition. For this composition the apparent activation energy for the overall combustion process was determined (155 kJ mol−1) and was shown to be independent on the degree of mechanical activation of the reactants.

Nanocrystalline Zn was prepared by cryomilling (mechanical attrition at liquid nitrogen temperature). Differential scanning calorimetry (DSC), x-ray diffraction, and transmission electron microscopy were used to study the structural changes and grain size distribution with milling time and subsequent annealing. Maxima in both stored enthalpy (for the low-temperature DSC peak) and lattice strain on the Zn basal planes were observed at the same milling time. Dislocation density on the basal planes is proposed as a major source for lattice strain and the measured stored enthalpy. The released enthalpy that might be due to grain growth is very small.

An aluminum nitride–diamond composite has been produced by sequential deposition of AlN and diamond in a triple torch plasma reactor (TTPR). AlN was deposited from AlN powder by injection into the argon–nitrogen, converging plasma plume of a TTPR. Velocity and temperature profiles of the converging plasma plume, obtained by enthalpy probe measurements, were used to show that the powder decomposed prior to reaching the substrate. Diamond was deposited in an argon–hydrogen–methane system onto the existing AlN film. Characterization of an AlN–diamond–AlN composite indicated a Vickers hardness of 18.6 GPa and a modulus of elasticity of 245–282 GPa.

Preferred domain orientation of a piezoelectric ceramic develops through domain switching under electric poling. In previous investigations the critical free energy required for domain switching has been assumed as a constant. This assumption leads to overestimation of the poling-induced texture and provides no explanation for the switching reversal in ferroelectric ceramics after the poling field is removed. In this paper, the contribution of intergranular stress to critical energy for 90° domain switching is investigated. A criterion including intrinsic threshold energy and an interaction energy, which is related to the intergranular stress and the intergranular depolarization field, is proposed. The texture evolution during poling process is simulated using a computational model starting from an initial random domain orientation distribution. The resulted domain orientation distributions under and after poling are predicted. The remanent domain switching after poling is the result of the balance between the interaction energy and intrinsic threshold energy. The final texture is much weaker than that under the electric field. Pole figures of poled Navy VI lead zirconate titanate measured by x-ray diffraction are consistent with the predicted textures.

To improve the oxidation resistance of TiB2 material, dense silica (SiO2) layer was caused to form on the surface. The coating layer was formed on the surface by exposing the specimens next to a bed of SiC powder in a flowing H2 containing 0.1% H2O at 1450 °C. Part of SiO2 “smoke”, generated by a reaction between the SiC powder and H2O in the H2 gas stream, was deposited on the sample surface to form a dense and uniform SiO2 layer. Beneath the SiO2 layer, an interfacial layer composed of Ti2O3 and B2O3was formed. Oxidation resistance of the specimen was improved markedly by the coating layers. The coating layers enhanced the oxidation resistance through the retardation of oxygen transport and also through the consumption of oxygen by a reaction with Ti2O3 to form TiO2.

The manganate with nominal composition La1.5Ca1.5Mn2O7, which is regarded as a single-phase compound with layered perovskite structure in the literature, was prepared using a standard ceramic process. The structures and morphology of the manganate were investigated by x-ray diffraction, transmission electron microscopy (TEM), scanning electron microscopy, and energy-dispersive x-ray microanalysis. However, no direct evidence of layered Sr3Ti2O7-type structure was observed in TEM experiments; instead, we observed multiphase mixtures of an orthorhombically distorted perovskite phase as majority and cubic perovskite phase as minority, as well as a small amount of calcium oxide. The measured magnetic and transport properties of this manganate arise mainly from the presence of hole-doped multiphase perovskite manganates. These physical properties demonstrated again the correctness of our phase component analysis.

A magnetically-driven method for controlling nanodimensional porosity in sol-gel-derived metal–oxide films, including TiO2, Al2O3, and SnO2, coated onto ferromagnetic amorphous substrates, such as the magnetically-soft Metglas1 alloys, is described. On the basis of the porous structures observed dependence on external magnetic field, a model is suggested to explain the phenomena. Under well-defined conditions it appears that the sol particles coming out of solution, and undergoing Brownian motion, follow the magnetic field lines oriented perpendicularly to the substrate surface associated with the magnetic domain walls of the substrate; hence the porosity developed during solvent evaporation correlates with the magnetic domain size.

A new experimental technique for determining mechanical properties of polymer–metal interfaces was developed by replacing the conventional mechanical testing machine with a piezoelectric actuator. The actuator was made from a thin ferroelectric ceramic beam attached to a bilayer polymer-metal composite specimen. The trilayer specimen was loaded by applying ac electric fields on the piezoelectric actuator to drive crack growth along the polymer-metal interface. Subcritical crack growth was observed along the epoxy/aluminum interface, and the growth rate was found to depend on the magnitude of the applied electric field. The fracture mechanics driving force for the crack growth was computed from the finite element analysis as a function of crack length, applied field, material properties, and specimen geometry. Kinetics of the crack growth was correlated with the piezoelectric driving force.

Aligned fibers of barium and strontium M hexaferrite (BaFe12O19 and SrFe12O19) were manufactured from an aqueous inorganic sol-gel-based spinning process, but halides have been found to be retained up to 1000 °C, inhibiting the formation of the hexagonal ferrite phases. Therefore an investigation was carried out into the removal of the halides at lower temperatures through steaming between 500 and 900 °C/3 h, and the subsequent effects upon microstructure and magnetic properties. The fibers were prefired to 400 °C to remove all organic components, and in all cases the steaming process resulted in loss of alignment of the fibers. It was found that the M phase began to form at only 600 °C, becoming single-phase SrM or virtually pure phase BaM at 700 °C, confirming that halides had indeed delayed M phase formation. Both materials had a grain size below 100 nm, but other unusual surface features not seen before on ferrite fibers were observed. The fibers steamed at 700 °C had Ms and Hc values comparable to random M ferrite fibers fired to 1000 °C in air, while steaming over a temperature range from 400 to 800 °C/3 h gave products with improved magnetic properties, with SrM fibers having an Ms of 81.4 emu g–1 and Hc of 457 kA m−1.

Pure and neodymium-doped gadolinium calcium oxoborate crystals of high quality were grown by the Czochralski method. The orientation of crystal was precisely determined, and the samples for measurements were prepared. Through synchrotron x-ray topography and high-resolution x-ray diffractometry, the twin structure was discovered. Some properties such as the figure of merit value, and dielectric, piezoelectric, and elastic constants were measured along with a discussion of the anisotropy of the laser properties.

High-quality ZnO thin films were grown epitaxially at 250–550 °C Al2O3(00·1) substrates using low-pressure metalorganic vapor phase epitaxy. The reactants for the growth were diethylzinc and oxygen. Growth temperature, one of the important experimental parameters for epitaxial layers, was optimized. The films grown at 500 °C exhibited good crystallinity and strong ultraviolet absorption and emission. Photoluminescence spectra of the films showed a dominant excitonic emission with a weak deep level emission. More importantly, a strong stimulated emission peak was observed even at room temperature.

Small spherical samples (diameter approximately 2 mm) of NdBa2Cu3O7−δ (Nd123) were fully melted in Ar gas flow in an aero-acoustic levitation device and subsequently rapidly cooled by splat quenching. For samples quenched above the liquidus, the microstructual and x-ray-diffraction (XRD) observations suggested the existence of the amorphous phase with small quantities of the BaCuO2 and BaCu2Ox. The high-temperature XRD results indicated that the decomposition of the amorphous phase, probably assisted by atmospheric CO2 and H2O, led to formation of the BaCO3 phase at 400 °C and, subsequently, the Nd123 phase was formed by the solid diffusion above 800 °C. Another set of Nd123 samples was fully melted in O2 gas flow, undercooled while levitated, and then splat quenched at a temperature below the peritectic temperature (TP). These samples possessed a microcrystalline microstructure of the Nd123 phase that was confirmed by XRD. This indicated that the Nd123 phase was solidified directly from the undercooled melt quenched below TP.

A method for the determination of site preference of substitutional elements in intermetallic compounds is proposed. It is demonstrated in Ni3Al–X alloys that the ridge direction in thermal conductivity contours in the ternary γ′ phase agrees with that of the solubility lobe of the γ′ phase in ternary phase diagrams. The ridge direction is a reliable indication of site preference of substitutional elements in intermetallic compounds. The present method is conveniently applied to a normal polycrystalline specimen with small size, and therefore, a versatile class of brittle compounds can be studied.

At very small layer spacings (< ∼2 nm) in Cu–Nb and Cu–Cr multilayers the Cu forms a metastable body-centered-cubic (bcc) structure and the films exhibit interesting mechanical properties. No information about the miscibility of bcc Cu in Nb or Cr is available and it is not known whether the films remain compositionally discrete. X-ray mapping in the analytical electron microscope has been used to study the compositional distributions in these films and show that they do remain discrete down to a layer spacing of 1.8 nm. A simple model for the experimentally measured distribution has been used to show that the expected analytical resolution has been achieved and that it should be possible to map layers with a spacing of 0.8 nm.

A nanocomposite (Mg–V)nano made of 90 wt% Mg and 10 wt% V was prepared by high-energy ball-milling during 40 h. The activation characteristics of (Mg–V)nano are rather poor, the hydrogen content [H] reaching 4 wt% after more than 100 h (t4wt%) following the initial exposure of the material to H2. Adding 9 wt% graphite to (Mg–V)nano and resuming the milling operation for 30 min leads to the formation of (Mg–V)nano /G, which exhibits a t4wt% value of only 10 min. The addition of more than 9 wt% graphite to (Mg–V)nano does not lead to any significant reduction of the t4wt% value. However, extending the milling period with graphite over 30 min leads to a steady increase in t4wt% and, thus, to a deterioration of the activation characteristics. Comparison of the behavior of graphite with other C-based compounds revealed that perylene (C20H12) and pentacene (C22H14), which are made of linked benzene rings, and thus have a 2D structure similar to that of the graphene sheet, are as effective as graphite in improving the activation characteristics of (Mg–V)nano. A structural investigation of (Mg–V)nano /G as a function of the milling time through both C 1s core-level x-ray photoelectron spectroscopy and C K edge x-ray absorption near-edge spectroscopy has shown that the integrity of graphite is progressively lost as the milling period is extended over 30 min. On the basis of these results, it is hypothesized that the adsorption of graphene layer on freshly created Mg surfaces and the formation of highly reactive C species during milling prevents the re-formation of the surface oxide layer responsible for the poor activation characteristics of untreated (Mg–V)nano