An apparatus for acquisition of highly resolved macroscopic photoluminescence topograms has been developed, using a laser scanner for PL excitation, and a linear diode array as imaging device. As a typical application, room temperature PL-topograms of various 2″ In P wafers are presented and discussed. Substrate inhomogeneities revealed in these topograms are growth striations, dendrites, and subsurface damage from wafer handling and processing.

Fine particles of BaTiO3 and SrTiO3 have been synthesized by the spray pyrolysis technique, and the chemical homogeneity of their particles was analyzed by x-ray diffraction (XRD) and analytical electron microscopy (AEM). The stock solutions were prepared by dissolving Ti(OC3H7)4 and Ba(NO3)2 or Sr(NO3)2 in diluted nitric acid solution. They were atomized into a reaction chamber held at 1000 °C through a two-fluids atomizer with N2 gas. Mostly hollow spherical particles 3 μm in diameter were obtained, composed of very fine grains of 40 nm. As-prepared powders were crystallized to BaTiO3 or SrTiO3 with a small amount of by-product such as Ba2TiO4, Sr2TiO4, and TiO2. The AEM study revealed that the bulk composition of each particle was chemically homogeneous, but a local chemical composition segregation was observed within each particle. This chemical inhomogeneity was considered to be caused by the difference in the precipitating speed of each component from the precursor salts; that is, the precipitation of Ti4+ ion as TiO2 · xH2O was faster than those of Ba2+ and Sr2+ ions. To control this segregation, (a) replacing a part of the solvent of stock solutions with methanol or ethanol, (b) adding H2O2 to the solutions, and (c) increasing the concentration of the solution, are found to be effective. The reasons for these effects are discussed.

The relationship between phase equilibria in the PbF2−AlF3 system and the solidification behavior of several ternary lead aluminum fluoride compounds was explored. A partial binary phase diagram for the PbF2−AlF3 system was determined from differential thermal analysis, annealing and directional solidification studies. The compounds AlF3, Pb3Al2F12, Pb9Al2F24, and a PbF2 solid solution were identified by x-ray diffraction, energy dispersive and microprobe analysis. The previously reported phases PbAlF5 and PbAl2F8 were not observed. Directional solidification studies showed that it is possible to grow crystals of AlF3, Pb3Al2F12, and the PbF2 solid solution from nonstoichiometric PbF2−AlF3 melts. The compound Pb9Al2F24 was found to decompose on heating by a peritectoid reaction (forming two other solids) and thus could not be solidified directly from a PbF2−AlF3 melt.

We report initial results on the synthesis of monolithic aluminum nitride by burning Al–AlN mixtures in high pressure nitrogen. The objective is to synthesize economically large, near-theoretical density AlN parts. In this work, we begin with compacted mixtures of 10 μm Al and 3 μm AlN powder formed into 7.62 cm diameter by 3.81 cm thick disks having densities up to 60% of theoretical. Then, at N2 pressures up to 180 MPa (26 000 psi), we ignite the disk on one face. The fraction of Al converted to AlN, density, and severity of macroscopic cracking vary with N2 pressure and heat transfer from the sample. Presently, products are inhomogeneous, showing regions of relatively high porosity, regions with no porosity but with AlN in a matrix of Al, and regions of nearly theoretical density AlN.

Reactive rf-magnetron sputtering has been employed for the growth of thin films of InN on the (001) face of mica at a variety of substrate temperatures from 50 to 550 °C. These films have been characterized by x-ray scattering, stylus profilometry, and electrical transport measurements, and their topography has been studied by SEM and STM. At low deposition temperatures, the InN films exhibit texture [(00.1)InN‖ (001)mica], while at higher deposition temperatures a large fraction of the grains are heteroepitaxial [(00.1)InN‖(001)mica, (2.0)InN · (060)mica]. The utility of the x-ray precession method in the determination of this heteroepitaxial relationship is highlighted. The films exhibit a local mobility maximum near a substrate temperature of 350 °C, beyond which a sharp increase in resistivity associated with voids and cracks owing to the onset of secondary grain growth leads to a dramatic decrease in electrical mobility. At the highest growth temperatures, however, the interconnection between grains improves and lower resistivity and higher mobility are re-established.

The nucleation and growth mechanisms during high temperature oxidation of liquid Al−3% Mg and Al−3% Mg−3% Si alloys were studied with the aim of enhancing our understanding of a new composite fabrication process. The typical oxidation sequence consists of an initial event of rapid but brief oxidation, followed by an incubation period of limited oxide growth after which bulk Al2O3/Al composite forms. A duplex oxide layer, MgO (upper) and MgAl2O4 (lower), forms on the alloy surface during initial oxidation and incubation. The spinel layer remains next to the liquid alloy during bulk oxide growth and is the eventual repository for most of the magnesium in the original alloy. Metal microchannels developed during incubation continuously supply alloy through the composite to the reaction interface. During the growth process, a layered structure exists at the upper extremity of the composite, consisting of MgO at the top surface, MgAl2O4 (probably discontinuous), Al alloy, and finally the bulk Al2O3 composite containing microchannels of the alloy. The bulk oxide growth mechanism appears to involve continuous formation and dissolution of the Mg-rich oxides at the surface, diffusion of oxygen through the underlying liquid metal, and epitaxial growth of Al2O3 on the existing composite body. The roles of Mg and Si in the composite growth process are discussed.

A mathematical model has been used to compute temperature profiles in ceramic preforms that are heated by microwaves. The temperature profiles were then input to a second part of the model describing chemical vapor infiltration of the preform, that is the diffusion of gaseous reactants, heterogeneous reaction, and evolution of the pore structure. Equations were solved numerically for parameters corresponding to the infiltration of SiC preforms by pyrolysis of trichloromethylsilane. While based on some simplifications, the model leads to the conclusion that infiltration proceeds more rapidly, and to a greater extent, with microwave heating/external cooling than in isothermal infiltration. The model suggests that infiltration might be optimized by manipulation of microwave power and external cooling. The computed extent of infiltration is seen to be very sensitive to the initial pore size.

We have examined the wear and friction and surface hardness of the mixed phase Ti–Si–C alloy formed by excimer laser surface processing of Ti layers on SiC substrates. The friction between a ruby pin and the mixed surface shows a complex behavior depending on relative humidity, a behavior clearly moderated by the chemistry of the interface between the sliding pin and the surface. The friction is sometimes much lower and sometimes comparable to that between the ruby pin and the unalloyed substrate. Wear in the unalloyed case is characterized by fatigue fracture and flaking of the SiC surface which leads to abrasive wear of the ruby pin. In the alloyed case, a transfer film forms and even in the worst case, a smooth wear track results in the alloy and the pin is undamaged. The surface hardness is intermediate between that of the SiC and the unalloyed Ti surface layer. The wear results are understood in terms of changes in the grain boundary structure of the surface induced by the laser alloying process.

Gels of various composition containing SiO2, Al2O3, and P2O5 have been investigated by employing high resolution magic-angle-spinning (MAS) 27Al, 29Si, and 31P NMR spectroscopy. Changes occurring in the NMR spectra as the gels are progressively heated have been examined to understand the nature of structural changes occurring during the crystallization of the gels. 27Al resonance is sensitive to changes in the coordination number even when the Al concentration is as low as 1 mol%. As the percentage of Al increases, the hydroxyl groups tend to be located on the Al sites while Si remains as SiO4/2 (Q4). Mullite is the major phase formed at higher temperature in the aluminosilicate gels. In the case of the silicophosphate gels, Si is present in the form of Q4 and Q3 species. There is a change in the coordination of Si from four to six as the gel is heated. The formation of six-coordinated Si is facilitated even at lower temperatures (∼673 K) when the P2O5 content is high. The phosphorus atoms present as orthophosphoric acid units in the xerogels change over to metaphosphate-like units as the gel is heated to higher temperatures. In aluminosilicophosphates, Si is present as Q4 and Q3 species while P is present as metaphosphate units; Al in these gels seems to be inducted into the tetrahedral network positions.

Single phase CoO, NiO, and Ni0.5Co0.5O epitaxial films have been prepared by reactive sputtering onto 〈0001〉 α−Al2O3 substrates maintained at 373 K. Epitaxy was confirmed by x-ray diffraction (XRD) and high resolution electron microscopy (HREM) techniques. XRD experiments indicate that these monoxide films are cubic and contain rotation twins with the twin axis parallel to 〈111〉. Lattice parameters for the CoO and NiO films are 0.4254 ± 0.0001 nm and 0.4173 ± 0.0006 nm, respectively, and agree with published values for the corresponding bulk oxides. The lattice parameter 0.4220 ± 0.0001 nm for the Ni0.5Co0.5O film lies between those of CoO and NiO and suggests that the mixed oxide film is compositionally homogeneous. Cross-sectional HREM images of the Ni0.5Co0.5O specimen show Σ3(12) twin boundaries perpendicular to the oxide-substrate interface. The twin regions are approximately 30 nm in size and are uniformly distributed throughout the film. The epitaxial orientation of the monoxide films with respect to the substrate can be summarized by the relationships [111] monoxide // [0001] α−Al2O3, [10] monoxide // [100] α−Al2O3, and [11] monoxide // [110] α−Al2O3.

Using the lattice Green's function approach and LCAO (linear combination of atomic orbitals) electron theory, we investigate the atomistic configuration and lattice trapping of cracks in Si. The LCAO electron theory coupled to second order perturbation theory (SOP) has been used to derive explicit expressions for the bond breaking nonlinear forces between Si atoms. We calculate the cracked lattice Green's functions for a crack on the (111) plane and lying in the (110) direction. With the nonlinear forces acting in a cohesive region near the crack tips, the crack structure is then calculated. The calculated structure possesses a crack opening at the Griffith load which should allow penetration of typical external molecules to the crack tip at the Griffith loading. Other consequences for chemical reactions at the crack tip are discussed in the light of these results. The lattice trapping is low, only a few percent of the Griffith load.

Magnetic domains in the vicinity of shear bands produced by bending were investigated to study the effect of furnace annealing on the domain structures. Domain wall spacings were measured as a function of annealing time at several temperatures. The same specimens were also used to evaluate the degree of embrittlement by measuring the bending fracture strains.

Small angle neutron scattering (SANS) was employed to characterize the pore structure of nanophase TiO2 ceramic materials compacted at different temperatures. Nanophase samples, produced by inert gas condensation, were compacted at 25, 290, 413, and 550 °C using a pressure of ≍1 GPa. The pore size distribution of the sample compacted at room temperature was very broad, with sizes ranging from ≍3–30 nm and pores comprising 38% of the sample volume. Compaction at 290 and 413 °C reduced the pore volume to 25% and 20%, respectively, by eliminating pores at both the small and large ends of the distribution. Compaction at 550 °C resulted in a pore volume that was less than 8%. Complications in the SANS analysis arising from the scattering from grain boundaries are discussed. The results from SANS are compared with those derived from nitrogen absorption, BET, measurements.

Controlled chemical polymerization of tantalum ethoxide in the presence of glacial acetic acid (HOAc/Alk. = 16) and solubilized lithium acetate (Li/Ta = 1.00, H2O/Alk. = 55.55) was used for the preparation of an amorphous gel precursor to LiTaO3. Although additional investigations are required, the results suggest that successful formation of amorphous gel network, as opposed to that of colloidal tantalum (hydrous) oxide, may be due to the generation of a new organotantalum precursor via a structural modification reaction between the tantalum ethoxide and glacial acetic acid. The evolution of LiTaO3 ceramics from pre-ceramic gels was investigated using thermal analysis, electron microscopy, and x-ray diffraction. The results indicate that after the completion of gel pyrolysis (200–400 °C) and crystallization (Tc = 590 °C), ultrafine (average particle size 100–300 nm), single phase, crystalline (a = 5.243, c = 13.812 Å) LiTaO3 powders can be prepared at low processing temperatures.

A relaxor ferroelectric of composition 0.93Pb(Mg1/3Nb2/3)O3-0.07PbTiO3 was sintered with 3 wt.% commercial sealing glass at 750 °C for 30 min to achieve ≥95% of theoretical density and a nearly pure perovskite phase. At higher glass additions (up to 20 wt.%), higher sintering temperatures (up to 800 °C), and longer sintering times (up to 4 h), the amount of perovskite (PMN type) decreases and that of pyrochlore (6PbO · MgO · 3Nb2O5 or 3PbO · 2Nb2O5) increases. On sintering at 800 °C for 4 h no perovskite phase is present in compositions with even 1% glass addition. The reaction of glass with the PMN phase was found to lead to the disappearance of the perovskite. Addition of 0.1 to 0.6 wt.% MgO to compositions containing 1 and 3 wt.% glass (and balance PMN-PT) results in essentially pure PMN perovskite phase on sintering at 700–800 °C for 30–240 min, confirming that the reaction of glass with PMN and depletion of MgO from PMN can be arrested. The sintered ceramics exhibit relaxor behavior and possess dielectric properties essentially commensurate with the phase composition.

The reduction of dislocation density in heteroepitaxial III-V compound films on Si substrates has been studied using MOCVD (Metal-Organic Chemical Vapor Deposition). High-quality GaAs films on Si, with a dislocation density of about 106 cm−2, have been obtained by combining strained-layer superlattice insertion and thermal cycle annealing. Reduction of dislocation density in the III-V compounds on Si is discussed based on a simple model, where dislocation annihilation is assumed to be caused by dislocation movement under thermal and misfit stress. As a result of dislocation density reduction, high-efficiency GaAs-on-Si solar cells with total-area efficiencies of 18.3% (AM0) and 20% (AM1.5), and red and yellow emissions from InGaP-on-Si light-emitting diodes have been realized. Moreover, future prospects of heteroepitaxy of III-V compounds on Si are also discussed.

Transformation characteristics of CeO2 stabilized ZrO2 gels have been studied during heating in the temperature region 1273–1473 K. The nature of the major phase present changes drastically in this temperature region. The crystallite sizes of tetragonal and monoclinic ZrO2 crystallites have been calculated by x-ray line broadening. The change in the nature of the major phase observed during heat treatment seems to be related to the presence of a barrier for transformation from a metastable to a stable regime, which in turn appears to be related to the diffusion barriers of Ce4+ in ZrO2.

Oxynitride glasses in the Si–Zr–Na–Li–K–B–O–N system have been produced via incorporation of Si3N4 into the glass structure. This system is the oxynitride analogue of commercially available alkali resistant (AR) glasses used for concrete reinforcement. Glasses with nitrogen contents up to approximately 4 at.% have been obtained. Hardness, fracture toughness, and chemical durability were found to increase with increasing nitrogen content. Fibers were drawn from the glasses containing approximately 4 at.% nitrogen and used to produce reinforced cement composites. The microstructure of the fiber-matrix interface was examined in these samples after aging and compared to that of oxide AR glass fiber-matrix interface. Measurement of the wetting behavior of aqueous solution as a function of the nitrogen content of the glass suggests that this difference in microstructure is the result of changes in physiochemical properties of the glass surface due to the incorporation of nitrogen into the glass structure.

The presence of silicon dioxide (SiO2) in the renal calculi is detected, for the first time, by using an x-ray fluorescence technique.

In this paper a model is presented for predicting the structural changes that occur in a metaphosphate glass during nitriding in anhydrous ammonia. Predicted values for the nitrogen content, the mole fraction of phosphate groups, the bridging to nonbridging oxygen ratio, and the ratio of the structural types for nitrogen are compared to the values obtained in earlier experimental work. A plausible correlation is found between the values predicted from this structural model and those observed experimentally. In addition, a maximum nitrogen content (N/P = 0.9) is predicted and the lower nitrogen content normally observed is explained.