α–Si3N4 whiskers were fabricated first through combustion synthesis (CS) technology. The as-synthesized crystals with [001] as the elongated axis contain a large amount of linear defects including (a + b)-type, (a + b + c)-type, and c-type of dislocations. The growth of α–Si3N4 whiskers is mainly controlled by vapor-condensation (VC) mechanism. Special additive plays an important role in promoting the growth of α–Si3N4 whiskers and suppressing the phase transformation of α–Si3N4 to β–Si3N4.

Compressive creep of dense BaTiO3 having linear-intercept grain sizes of 19.3–52.4 μm was investigated at 1200–1300 °C by varying the oxygen partial pressure from 102 to 105 Pa in both constant-stress and constant-crosshead-velocity modes. Microstructures of the deformed materials were examined by scanning and transmission electron microscopy. The stress exponent was ≈1, the grain-size dependence was ≈1/d2, and the activation energy was ≈720 kJ/mole. These parameters, combined with the microstructural observations (particularly grain displacement and absence of deformation-induced dislocations), indicated that the dominant deformation mechanism was grain-boundary sliding accommodated by lattice cation diffusion. Because of the absence of an oxygen partial pressure dependence, diffusion was probably controlled extrinsically.

The products obtained from MnO2–V2O5 mixtures at the ambient oxygen pressure and temperatures up to 900 °C were studied by means of thermal analysis and x-ray diffraction methods. The following phases were found to exist in equilibrium, depending on the composition: (I) Mn2O3–Mn2V2O7, (II) Mn2V2O7–MnV2O6, and (III) V2O5–solid solution of VO2 in MnV2O6. A phase diagram was obtained for the composition region III. The data are instructive for syntheses of manganese vanadates by thermal methods.

The in-plane thermal diffusivity of chemical-vapor-deposited diamond films was measured as a function of diamond-growth rate. The films, 0.1–0.4 mm thick, were prepared in microwave-plasma reactor at growth rates ranging from 1 to 10 μm/h. A modification of Ångstöm's method was used to perform the diffusivity measurements. The thermal conductivity calculated from the thermal diffusivity shows an inverse relationship with growth rate. Analyses of Raman spectra indicate that both the line shifts and the line widths of the diamond Raman peak are practically independent of the deposition rate, except for the specimen grown at the highest growth rate.

A study of the electrical resistivity and microstructure of thin copper films deposited by low-pressure chemical vapor deposition from copper (I) hexafluoroacetylacetonate vinyltrimethylsilane (Cupra Select) was undertaken. Evidence for the nucleation of solid copper in the gas phase at substrate temperatures of about 250 °C is presented. A process to predict the effects of gas-phase nucleation and growth on the electrical resistivity of the resulting film is discussed.

Nanosized Ce-doped silica particles (without and with Al addition) dispersed within pores of mesoporous silica host were synthesized by soaking and sol-gel technique. It was found that the dispersed phosphor particles are mainly located within the pores that are less than 4 nm in diameter. There exist two luminescence peaks at about 350 and 700 nm, respectively, for this phosphor in the dispersed or aggregated state. For the dispersed system, the luminescence intensities of both peaks are more than 14 times higher than those of the aggregated one, the shoulders on the lower sides of the luminescence peaks disappear, and no effect of Al addition on the luminescence occurs which is in contrast to the aggregated system. This is mainly attributed to the high dispersity of nanosized phosphor particles in the host and the effective avoidance of a clustering of Ce3+ ions.

Oxidic zirconium films prepared by chemical deposition from aqueous medium on sulfonic acid terminated self-assembled monolayers attached to an oxidized silicon surface were investigated with scanning electron microscopy and atomic force microscopy. Bulk precipitate forms in the 4 mM Zr(SO4)2 · 4H2O, 0.4 N HCl deposition medium at 343 K after approximately 30 min. Precipitate particles (200 nm and larger) were found embedded in the oxidic zirconium film and adsorbed on top of the film; they could be washed off, but patches of the film were removed. Working with unstable deposition solutions, in which homogeneous nucleation occurs, leads to preparation-inherent flaws in the film.

We have investigated the effect of oxygen vacancies on imprint and fatigue behavior of the PLZT thin films. It is found that the compensation of oxygen vacancies with various dopant concentrations and electrode structures is an important process parameter in determining the tendency to imprint and fatigue. In the case of PLZT thin films, the voltage shifts related to imprint are attributed to the trapping of electrons at ionic defect sites such as oxygen vacancies near the film/electrode interface, the magnitude of polarization, and concentration of defect-dipole complexes involving oxygen vacancies such as V′Pb–V••o. The strong dependence of fatigue rate on electrode material for PLZT thin films is due to the effect of the ferroelectric/electrode interaction on the pinning and/or unpinning rate involving the accumulation of oxygen vacancies near the film/electrode interface during fatigue cycling. By using RuO2 as the top and/or bottom electrode instead of Pt, improved fatigue properties are obtained compared to Pt/PLZT/Pt capacitors. This is because a reduced accumulation of oxygen vacancies near the interface by the oxide electrode such as RuO2 may reduce the electronic charge trapping and, consequently, lead to less domain wall pinning.

A composite microstructure, consisting of β-Sialon, O-Sialon, and X-Sialon phases was produced by coating β–Si3N4 particles with amorphous alumina followed by hot pressing and reactive sintering at 1923 K. The particle coating procedure was selected over conventional powder blending in order to promote heterogeneous nucleation of β-Sialon grains on β–Si3N4 particles uniformly. The microstructure, chemistry of the phases, and interphase interfaces of this ceramic were characterized by transmission electron microscopy (TEM) and high-resolution analytical electron microscopy (AEM). Both electron energy-loss spectroscopy (EELS) and energy-dispersive spectroscopy (EDS) x-ray microanalysis in AEM revealed that b-Sialon grains had varying aluminum and oxygen contents. High-resolution electron microscopy (HREM) examination of several interphase interfaces and triple junctions suggests that the amount of glassy phase in the produced ceramic is substantially lower compared to those reported in the literature. This is of importance of high temperature properties. The fracture toughness and wear properties were evaluated at room temperature. Available data indicate that the fracture toughness and wear of β-Sialon composite can be significantly improved by the powder coating technique compared to the conventional powder blending technique.

Patterned KTiOPO4 (KTP) films were successfully synthesized through metallo-organics using ultraviolet (uv) patterning. A homogeneous precursor solution was prepared by the reaction control of (nBuO)2P(O) (OH), Ti(OEt)4, and KOEt in ethanol. The solubility of the KTP precursor films in ethanol changed with uv irradiation because of the polymerization of KTP precursor. The patterned KTP precursor films crystallized to single-phase KTP after heat treatment at 600 °C for 2 h. The patterned films were found to be exactly stoichiometric KTP.

Thin AlN films were grown by molecular beam epitaxy on MgO(001) substrate with a thin TiN buffer layer. The as-prepared AlN/TiN/MgO(001) interfaces have been characterized by cross-sectional high-resolution electron microscopy (HREM). It is found that the thin TiN buffer layer is epitaxially grown on the MgO(001) substrate and hexagonal AlN epitaxially on the as-received TiN(001). Based on the growth orientation relationship and HREM images, atomistic structure models for the AlN/TiN interface are proposed, image simulated, and compared with experimental images.

CaSiO3 powders were prepared from an ethanol solution dissolving Ca(NO3)2 · 4H2O and Si(OC2H5)4 by the coprecipitation method using various concentrations of NaOH as precipitants. Some Na component remained in the precipitates without washing and strongly affected the characteristics of the resultant powders, but the Na residue was removed by a washing treatment. The precipitate prepared by using 0.33 mol/l of NaOH and twice-washing contained the lowest amount of Na residue. It was calcined at 500 and 900 °C, respectively, to crystallize CaSiO3 phase and ground by a planetary potmill. The ground CaSiO3 powder was sintered to about 89% theoretical density by firing at 1400 °C. By soaking the CaSiO3 sintered bodies in simulated body fluid (SBF) solution for various times, an hydroxylapatite (HAp) layer formed as aggregates of ball-like particles on the surface of the CaSiO3 sintered bodies after soaking for a short period; thereby, the CaSiO3 ceramics is suggested to have very good biocompatibility.

Ba(Ti1−xSnx)O3 (0 ≤ x ≤ 0.3) thin films were deposited on a platinized silicon substrate by a solution deposition process with methoxyethanol, water, and propylene glycol as solvents. Dielectric properties and current–voltage characteristics of the thin films were investigated in conjunction with phase evolution and microstructures by varying heating temperatures and Sn contents (x). Thin films annealed above 700 °C showed a pure perovskite phase with nanoscaled grains (20–30 nm). The dielectric constant of the thin films depended on the Sn content and showed a maximum value of 330 at x = 0.15. The leakage current behavior of an optimum composition corresponding to x = 0.15 was examined by correlating with charge transport mechanisms. Schottky emission was found to be predominant at voltages less than 6.8 V, and Fowler–Nordheim tunneling appeared to be responsible above 6.8 V. The Schottky barrier of the Ba(Ti0.85Sn0.15)O3–Pt interface was determined to be 1.49 eV.

Failures in aluminum interconnects in display control devices are often caused by the formation of hillocks during postdeposition annealing. Ion-beam-assisted deposition was used to create a (110) out-of-plane texture in aluminum films to suppress hillocking. X-ray diffraction was used to quantify the (110)/(111) out-of-plane texture ratio, and scanning electron microscopy and atomic force microscopy were used to characterize the surface topology. Results show that no hillocks were observed on (110)-textured aluminum films following annealing for 30 min at 450 °C. Following annealing, the resistivity of the films made by ion-beam-assisted deposition recovered to within a factor of 2 of the physical-vapor-deposition films. Results show that ion-beam-assisted deposition can effectiv09ely modify the aluminum out-of-plane texture in such a way that hillock suppression can be achieved without significant change in resistivity.

Gravimetry and x-ray diffraction were used to study the kinetics and mechanism of internal oxidation in air at 300–600 °C of Ag–2 and 4 at.% Mg alloys. All the features typical of the non-Wagnerian behavior in more dilute alloys (the slower initial and faster intermediate kinetics, oxygen release from the samples at the late stages, and stabilization of highly hyperstoichiometric oxides with O/Mg up to 1.74 ± 0.02) are also observed in these more concentrated alloys. A linear correlation between the lattice parameter of oxidized alloys, magnesium content, and amount of excess oxygen is found and used for analyzing the published data on the lattice parameters in other oxidized Ag–Mg alloys. Such analysis suggests that, at early stages of low-temperature oxidation, O/Mg ratios could be higher than 4 ± 0.8, which is interpreted as evidence that O–Mg interaction at these stages is the trapping of mobile O atoms by immobile Mg atoms, so that oxidation of Ag–Mg alloys can be considered as formation and subsequent decomposition of Ag–Mg–O solid solutions, and it is the decomposition stage that significantly affects the oxidation kinetics. Possible impact of these findings on optimization of alloy-sheath composition and microstructure in Bi2223/AgMg superconducting tapes is discussed.

High molecular weight anionic polymers have been incorporated into the calcium silicate hydrate (C–S–H) structure during precipitation of quasicrystalline C–S–H from aqueous solution. The anionic polymers studied were poly(methacrylic acid), poly(acrylic acid), and the sodium salt of poly(vinyl sulfonic acid). Expansion of the interlayer spacing coupled with high-carbon contents confirmed that the polymers intercalated between the layers. D-gluconic acid behaves similarly. Intercalation characteristics strongly depended on both the type of polymer and Ca/Si molar ratio of C–S–H; intercalation reached a maximum at an initial Ca/Si = 1.3 in all cases. Poly(vinyl alcohol) was the only nonionic polymer among those studied that was incorporated into C–S–H. Evidence for interlayer intercalation is less definite. The C–S–H/polymer complexes were examined by Fourier transform infrared spectroscopy, 29Si nuclear magnetic resonance magic angle spinning, and 13C cross-polarization, magic angle spinning nuclear magnetic resonance spectroscopy.

The reduction of CuO with different amounts of C (CuO:C = 2:1, 2:1.5, and 2:2 molar ratios) driven by mechanical alloying was examined by x-ray diffraction and transmission electron microscopy. It was found that reduction behaviors are closely related to the carbon content. The reduction of CuO for the mixture with 1 mol of carbon follows a two-step process; i.e., CuO → Cu → Cu2O. However, the CuO can be completely converted to Cu for the mixtures with higher carbon content. A tentative model in terms of solid-state reactions at the interfaces is proposed to explain the effect of carbon content. Additionally, the thermal responses of the premilled mixtures were investigated by thermogravity and differential thermal analysis followed by x-ray identification. Contrary to mechanical alloying, reduction of CuO during thermal treatment follows a transition sequence of CuO → Cu2O → Cu. The preferential formation of Cu2O at the early annealing stage is probably due to the involvement of gaseous reduction.

Some high molecular weight cationic polymers, poly(diallyldimethylammonium chloride) (PDC) and poly(4-vinylbenzyltrimethylammonium chloride) (PVC), have been incorporated into the calcium silicate hydrate (C–S–H) structure during precipitation of quasicrystalline C–S–H from aqueous solution. Expansion of the interlayer spacing [0.9 nm (PDC), 1.5 nm (PVC)] and a high-carbon content provided evidence that these polymers were intercalated between layers of C–S–H when Ca/Si <1.0. Intercalation characteristic properties strongly depended on both of the type of polymer and Ca/Si ratio in C–S–H. Poly(4-vinyl-1-methylpyridinium bromide) and methyl glycol chitosan (iodide) also interacted with C–S–H, probably by surface adsorption. The C–S–H/polymer complexes were examined by Fourier transform infrared spectroscopy, 29Si nuclear magnetic resonance magic angle spinning, and 13C cross-polarization, magic angle spinning nuclear magnetic resonance spectroscopy. Mechanisms of intercalation of different kinds of polymers between the C–S–H layers are discussed.

The influence of the presence of free PbO on densification, the perovskite/pyrochlore phase ratio, and corresponding dielectric properties has been studied for 0.9 PMN–0.1 PT-based ceramics with different added PbO excess. The sintering behavior of PMN-PT-based ceramics was basically controlled by PbO losses. However, the presence of a rich-PbO liquid phase during sintering produced pyrochlore grains, mainly located at the surface of the specimens. The dielectric properties of the PMN-PT-based materials, fabricated with different values of PbO excess, were similar when the secondary phase preferentially located at the surface was removed by polishing prior to electrode deposition. The thickness of the PbO-rich intergranular layers of the four samples with different initial PbO content was mainly independent of the amount of PbO excess because most of the free PbO was eliminated during sintering. Dielectric constant values of approximately 17,000 at 1 kHz and 40 °C were measured.

The mechanisms are studied for enhanced formation of C54–TiSi2 at about 700 °C when rapid thermal annealing at 3 °C/s in N2 is performed on 32-nm-thick codeposited Ti–5.9 at.% Ta on Si(100) single-crystal substrates. The enhancement is related to an increased C54–TiSi2 nucleation rate due to the development of a multilayered microstructure. The multilayer microstructure forms at temperatures below 600 °C with the formation of an amorphous disilicide adjacent to the Si substrate and a M5Si3 (M = Ti, Ta) capping layer. This amorphous disilicide crystallizes at higher temperatures to C49–TiSi2. The multilayer microstructure introduces an additional interface that increases the area available for the heterogeneous nucleation of C54. The capping layer is identified as hexagonal Ti 5Si3 or its isomorphous compound (Ti1–xTax)5Si3. Crystal simulations demonstrate that C54(040) has a lattice mismatch of 6–7% relative to Ti5Si3(300) suggesting that a pseudomorphic epitaxial relationship may lower the interfacial energy between these two phases and reduce the energy barrier for C54 nucleation. A C40 disilicide phase was also observed at temperatures above that required to form C54–TiSi2 suggesting that, in the present experiments, the C40 phase does not play a major role in catalyzing C54 formation.