Stability of the binary phases in the quaternary system Mo–Ti–Si–C was examined for the combustion synthesis or Self-propagating High-temperature Synthesis (SHS) of MoSi2−TiC composites. Thermochemical calculations were carried out to obtain the adiabatic temperatures and the amounts of molten phases at the adiabatic temperature for the SHS of these composites. MoSi2−20 wt. % TiC and MoSi2−40 wt. % TiC composites were prepared by thermal explosion and SHS modes of combustion from elemental powders. The phase formation was confirmed by x-ray diffraction, and the morphologies were observed under SEM. No general correlation was obtained between the phase formation or product morphology on the one hand, and the adiabatic temperature or the amount of molten phase formed at the adiabatic temperature, on the other. MoSi2−40 wt. % TiC composites obtained by SHS mode of combustion show a highly homogeneous distribution of the two phases with negligible amounts of ternary phases.

A mathematical model of micropyretic synthesis, including the consideration of pressure rise (due to gas evolution) in a porous compact, is developed for a multistep reaction. D'Arcy's law of gas flow, continuity equation, and gas law are combined to obtain a relationship between the pressure and temperature of gas. This equation for the gas pressure is solved along with the energy equations of gas and solid phase. The numerical analysis shows that the magnitude of pressure increase depends on the initial gas pressure, temperature, and permeability. When gas evolution is considered, the pressure increase depends on the variables that determine the kinetics of the gas evolution reaction, such as the activation energy and the pre-exponential factor. The pressure increase is maximum when the gas evolution takes place in the combustion reaction zone. The gas evolution is noted not to influence the combustion wave propagation.

Formation of nanocrystalline composites γ-TiAl + Ti2AlN by mechanically alloying (MA) Ti50Al50 in a N2 atmosphere and subsequent annealing treatment are investigated. The development of the microstructure was monitored by x-ray diffraction, and differential thermal analysis and transmission electron microscopy. The amorphous phase could be obtained after milling for 30 h in a nitrogen atmosphere. The TEM results show that some nanocrystalline solid solution of Al in Ti also existed in the amorphous matrix. The results of annealing treatments at different temperatures for 0.5 h on the amorphous phase obtained by MA in N2 gas for 30 h show the formation of γ-phase (TiAl) and a nitride of titanium and aluminum (Ti2AlN). Available annealing treatments could produced nanocrystalline composites of γ-TiAl and Ti2AlN with a grain size less than 20 nm. With increasing annealing temperature, the crystalline sizes of γ-TiAl and Ti2AlN increase, but the values of microhardness increase slightly.

The amount of Si3N4 in a Si3N4-BaO · Al2O3 · 2SiO2 (BAS) composite and the time of sintering was examined in the context of the low temperature hexagonal to orthorhombic transformation in BAS. It was found that with increasing amounts of Si3N4 in the composite, the temperature of the hexagonal to orthorhombic transformation was decreased. As the sintering time was increased for a given composite composition, a drop in the temperature of the hexagonal to orthorhombic transformation was observed. which was linked to an increase in the β-Si3N4 content in the composite. In addition, as the Si3N4 content in the composite was increased, a resultant drop in the coefficient of thermal expansion of the composite occurred. The extent of the linear dimensional change of the composite during the BAS hexagonal to orthorhombic transformation is reported.

Nanosized TiO2 is synthesized in a nanosized alumina matrix by a sol-gel procedure. The results of the study of the blueshift of the TiO2 UV band edge are compared to the information obtained from transmission electron microscopy (TEM). As long as the atomic ratio Ti/Al remains smaller than 17.5%, no individualized TiO2 particles are detected by TEM, in spite of the fact that no modification of the alumina structure occurs, as revealed by 27Al MAS NMR. The shift of the UV band edge suggests the growth of homogeneous TiO2 domains in the alumina matrix. Above a critical radius, on the order of 1.2 nm, individual and crystalline TiO2 particles become visible in the TEM picture, and the porosity of the material decreases markedly.

The model proposed by Harris et al. [J. Mater. Res. 5, 1763–1773 (1990)], describing planar inversion domain boundaries in aluminum nitride, consists of a basal plane of aluminum atoms octahedrally coordinated with respect to oxygen, and with a translation of R = 1/3〈1011〉. This thin sandwich is inserted onto the basal plane of the wurtzite structure of aluminum nitride. This model does not take into consideration any interfacial relaxation phenomena, and is arguably electrically unstable. Therefore, this paper presents a refinement of the model of Harris et al., by incorporating the structural relaxations arising from modifications in local chemistry. The interfacial structure was investigated through the use of conventional transmission electron microscopy, convergent electron diffraction, high resolution transmission electron microscopy, analytical electron microscopy, and atomistic computer simulations. The refined planar inversion domain boundary model is closely based on the original model of Harris et al.; however, the local chemistry is changed, with every fourth oxygen being replaced by a nitrogen. Atomistic computer simulation of these defects, using a classical Born model of ionic solids, verified the stability of these defects as arising from the adjustment in the local chemistry. The resulting structural relaxations take the form of a 0.3 mrad twist parallel to the interface, a contraction of the basal planes adjacent to the planar inversion domain boundary, and an expansion of the c-axis component of the displacement vector; the new displacement vector across the interface is R = 1.3〈1010〉 + ∊〈0001〉, where ∊meas = 0.387 and ∊calc = 0.394.

Three distinct morphologies of curved (curved, facetted, and corrugated) inversion domain boundaries (IDB's), observed in aluminum nitride, have been investigated using conventional transmission electron microscopy, convergent beam electron diffraction, high-resolution transmission electron microscopy, analytical electron microscopy, and atomistic computer simulations. The interfacial structure and chemistry of the curved and facetted defects have been studied, and based upon the experimental evidence, a single model has been proposed for the curved IDB which is consistent with all three observed morphologies. The interface model comprises a continuous nitrogen sublattice, with the aluminum sublattice being displaced across a {1011} plane, and having a displacement vector R = 0.23〈0001〉. This displacement translates the aluminum sublattice from upwardly pointing to downwardly pointing tetrahedral sites, or vice versa, in the wurtzite structure. The measured value of the displacement vector is between 0.05〈0001〉 and 0.43〈0001〉; the variation is believed to be due to local changes in chemistry. This is supported by atomistic calculations which indicate that the interface is most stable when both aluminum vacancies and oxygen ions are present at the interface, and that the interface energy is independent of displacement vector in the range of 0.05〈0001〉 to 0.35〈0001〉. The curved IDB's form as a result of nonstoichiometry within the crystal. The choice of curved IDB morphology is believed to be controlled by local changes in chemistry, nonstoichiometry at the interface, and proximity to other planar IDB's (the last reason is explained in Part III). A number of possible formation mechanisms are discussed for both planar and curved IDB's. The Burgers vector for the dislocation present at the intersection of the planar and curved IDB's was determined to be b = 1/3〈1010〉 + t〈0001〉, where tmeas = 0.157 and tcalc = 0.164.

Compositions in the (Pb1−xBix (Ti1−xFex)O3 solid solution system for x ⋚ 0.7 show unusually large tetragonal distortion. High-temperature x-ray diffraction was used to study the tetragonal distortion as a function of temperature (25–700 °C) for compositions (x = 0–0.7) using powders prepared by solid-state reaction in the above system. Large changes in the lattice parameters were observed over a narrow temperature range near Curie temperature (TC) for compositions near the morphotropic phase boundary (MPB) (x ≃ 0.7). Compositions near MPB showed a c/a ratio of 1.18 at room temperature. Polar plots of lattice constants at different temperatures indicated strong anisotropic thermal expansion with zero thermal expansion along the [201] direction.

α-Fe2O3 thin films have been deposited on Si(111) substrates at high temperatures (600–800 °C) by the spray pyrolysis method. Four different iron(III) β-diketonates have been used as precursors in order to obtain polycrystalline films of good adherence, which have been characterized by x-ray diffraction, scanning electron microscopy, and magnetic measurements.

Cristobalite is known to precipitate out of borosilicate glass (Corning 7740) and a binary glass mixture of borosilicate glass and high silica glass when these glasses are heated to elevated temperatures. To prevent cristobalite from forming in these glass systems, a devitrification inhibitor needs to be found. Among oxides selected for testing, both Al2O3 and Ga2O3 are found to prevent cristobalite from forming in these glass systems.

The kinetics of constrained-film sintering were studied in a borosilicate glass (BSG) + silica system because of their applications in microelectronic packaging technologies. Samples with a silica content by 20% by volume were prepared from slurries of powder mixtures in a commercial polyvinyl butyral (PVB) binder solution. Constrained films about 0.2 mm thick were formed by doctor-blade casting the slurries on silicon wafers. Free-standing films about 0.6 mm thick were also produced by casting the slurries on a treated mylar sheet for easy lift-off. Sintering experiments were carried out in a hot stage at temperatures between 715 °C and 775 °C. Shrinkage profiles of the free and constrained (shrinkage in thickness only) films were determined in situ using a custom-designed optical system. The densification rates measured in the constrained films were slower than those in the free films. However, the substrate constraint had no effect on the activation energy of densification which was found equal to 385 ± 10 kJ/mol, the same for both free and constrained films. A relation between the constrained-film and free-film densification profiles was derived using the viscous analogy for the constitutive equations of a porous sintering body.

Five kinds of uniform metal oxide particles (α-Fe2O3, CeO2, CuO, NiO, and SiO2) were coated with polypyrrole by reacting the dispersed solids with pyrrole in a water/ethanol medium without the use of a soluble oxidant. When the process was carried out in air, all particles were coated with the polymer, although the thickness of the layer varied on different cores. In CuO dispersions, independent polypyrrole particles were produced in addition to coated spheres. While oxygen is the major oxidant that initiates the polymerization of pyrrole, some metal oxides may also affect the reaction both in terms of the amount and the composition of the shell. Thus, α-Fe2O3 and SiO2 were found to be inactive in the polymerization, while CeCh and CuO react with the adsorbed pyrrole molecules through a reductive-dissolution process, in which the monomers are oxidized, causing a release of reduced metal ions.