Si(100) wafers were prepared by both diamond turning and standard lapping and polishing techniques. For single-point diamond machining, characterization of subsurface damage resulting from ductile-regime machining identified a plastic-yield zone consisting of slip planes and dislocation networks extending 1 to 3 μm deep despite surface root-mean-square roughness values as low as 5 nm. For conventional lapping and polishing using alumina grit, a transition from brittle to ductile yield was observed for grit sizes less than 300 nm. Subsurface damage depth correlated to surface roughness in a more straightforward manner than for the diamond point machining. Completely damage-free material removal was obtained only when a chemical component to the polishing was present.

A nanocrystalline α–Fe2O3 particle/oligomer hybrid can be synthesized by polymerization of iron (III) 3-allylacetylacetonate (IAA) followed by in situ hydrolysis. The polymerization of IAA was dependent upon the polymerization temperature and solvent. GPC measurement showed that the polymerization degree of the IAA oligomer ranged from ∼3 to ∼6. The magnetic particle/oligomer hybrid was synthesized by hydrolysis of the IAA oligomer under a neutral or alkaline condition. Crystalline particles from 10 to 40 nm were finely dispersed in the oligomeric matrix, depending upon the hydrolysis conditions. The nanocrystalline particles below 10 nm in diameter were identified to be α−Fe2O3 by electron diffraction. The nanosized α−Fe2O3/oligomer hybrid was found to show superparamagnetic behavior.

A comparative study of the deposition of diamond-like carbon films using methane or benzene in a microwave electron cyclotron resonance plasma-enhanced chemical vapor deposition system has been performed. Process variables studied were reactor pressure, applied radio frequency substrate bias, and microwave power. The plasma stream was characterized using optical emission spectroscopy and mass spectrometry. Film properties studied included optical energy gap, total hydrogen content, integrated C-H stretch absorption, index of refraction, and Raman spectra. The use of a high C/H ratio reactant such as benzene was found to be advantageous over methane in that higher deposition rates were possible and the resultant films exhibit diamond-like properties without the application of large substrate biases. Another result of this investigation was further confirmation that hard carbon films contain a significant quantity of nonbonded hydrogen [A. Grill and V. Patel, Appl. Phys. Lett. 60 (17), 2089 (1992)].

Planar microstructure, 90° domain configurations, and cross-sectional perovskite grain morphology were characterized for a series of Pb(Zr, Ti)O3//RuO2 thin film capacitors. Perovskite grain size increased substantially with increasing Zr concentration of the Pb(Zr, Ti)O3 (PZT) films, being on the order of 0.15 μm for PZT 20/80 films and 2.5 μm for PZT 50/50 films. While PZT 20/80 and PZT 30/70 films were single phase perovskite, the PZT 40/60 and 50/50 films contained a second phase with fluorite structure. The second phase matrix consisted of two nanophases, one having fluorite structure while the other was amorphous. Both the amorphous nanophase and the fluorite nanophase were Pb deficient compared to the perovskite phase. Differences in cross-sectional perovskite grain morphology were substantial for these materials, with the PZT 40/60 film being almost entirely columnar and the PZT 20/80 film exhibiting almost entirely granular morphology. Differences in 90° domain wall density were essentially negligible among the films, suggesting that if 90° domains were responsible for the differences in electrical properties, it is not due to 90° domain population.

Silica glass was implanted with chromium at the energy of 35 and 160 keV and at fluences varying from 1 × 1016 to 11 × 1016 ions cm−2. In a set of chromium-implanted samples significant amounts of carbon were detected. Samples were characterized by x-ray photoelectron spectroscopy, x-ray-excited Auger electron spectroscopy, secondary ion mass spectrometry, and Rutherford backscattering spectrometry. Chromium silicide and chromium oxide compounds were observed; the presence of carbon in the implanted layers induces the further formation of chromium carbide species. Thermodynamic considerations applied to the investigated systems supply indications in agreement with the experimental evidences.

The microstructure and mechanical properties of hot-pressed zirconia-toughened alumina (ZTA), fabricated from the ZTA powders containing (Zr, Ti)O2 in Ar gas were investigated. In hot-pressed ZTA, the presence of Ti concentration in the grains of Al2O3 or (Zr, Ti)O2 was analyzed by the energy dispersive spectroscopy (EDS) attached to the analytical electron microscope (AEM) apparatus. Experimental results showed that some Ti ions diffused to the grain boundary and into the Al2O3 grains, thereby enhancing the densification of hot-pressed ZTA. It was possible to retain tetragonal ZrO2 at room temperature in the ZTA specimens containing ≥5.5 mol% TiO2 and hot pressed at 1350 °C for 1 h. The bending strength and toughness of hot-pressed ZTA were enhanced by the addition of TiO2.

C60/C70: Ni films with 1.5 wt. % Ni concentration obtained by vacuum deposition under different thermal conditions have been investigated. The structural changes of the layers were investigated by transmission electron microscopy, electron and x-ray diffraction, and Raman spectroscopy. The polycrystalline structure was detected for the layers grown at approximately 450 K on the substrate. At elevated temperature and maintained temperature gradient on the substrate during the process, the changes of the layer's structure and the formation of Ni microcrystals were observed. The Ni microcrystals (5–10 nm in the diameter) and the elongated shapes dimensioned 10 × 150 nm were perceived.

The role of precursor stoichiometry and local firing environment on the microstructural development of sol-gel derived lead zirconate titanate (PZT) thin films was investigated. Typically, excess Pb is added to films to compensate for PbO volatilization during heat treatment. Here, it is shown that the use of stoichiometric precursors with either a PbO atmosphere powder or a PbO overcoat during the crystallization heat treatment is an attractive and viable alternative method for control of film stoichiometry. Using these approaches, we have fabricated single phase perovskite thin films with microstructures and electrical properties (Pr ∼ 36 μC/cm2 and Ec ∼ 45 kV /cm) comparable to those of films using optimized solution chemistries and excess Pb additions. The potential advantage of increasing PbO partial pressure, or activity, during firing versus excess Pb additions is discussed from the standpoint of a proposed crystallization scenario based on the kinetic competition between Pb loss and the nucleation and growth rates of the perovskite phase.

Weakly agglomerated nanoparticles of yttria-stabilized zirconia (YSZ) were synthesized by a novel process which involved the decomposition of metal nitrates that had been coated on ultrafine carbon black powder, after which the carbon black was gasified. The use of ultrafine, high-surface-area carbon black powder apparently allowed the nanocrystalline oxide particles to form and remain separate from each other, after which the carbon black was gasified at a somewhat higher temperature. As a result, the degree of agglomeration was shown to be relatively low. The average crystallite size and the specific surface area of the as-synthesized YSZ nanoparticles were 5−6 nm and 130 m2/g, respectively, for powder synthesized at 650 °C. The as-synthesized YSZ nanoparticles had a light brown color and were translucent, which differs distinctly from conventional YSZ particles which are typically white and opaque. The mechanism of the synthesis process was investigated, and indicated that the gasification temperature had a direct effect on the crystallite size of the as-synthesized YSZ nanoparticles. High-density and ultrafine-grained YSZ ceramic articles were prepared by fast-firing, using a dwell temperature of 1250 °C and a dwell time of two minutes or less.

In this paper, a new set of experimental data, αVKTV, representing the partial temperature derivative of the work done by the thermal pressure of the solid, is fitted by n terms of a modified Einstein model. Experimental data show that αVKTV, not αVKT, approaches a constant value at high temperature. Based on the observed linear relationship of isothermal bulk modulus with temperature at high temperature, thermal expansion can be evaluated by fitting αVKTV data. Our previous results have shown that at low temperature or for materials with less variable bulk modulus and expansivity, thermal expansion data can be simply approximated by an n term Einstein model. More generally and for many materials, αVKTV data resemble an isochoric specific heat curve. With this method, thermal expansion can be predicted at high temperatures from low and intermediate temperature range data. With accurate thermal expansion data, high temperature bulk moduli can also be predicted.

Selsing's formula for radial tension at the particle-matrix interface is extended into a general formula which includes the effects of the amount of dispersed particles. A relationship is derived between individual volumes of strained unit cells in the crystal lattices of the particles and of the surrounding matrix. These relationships are used to predict the effect of the particles (2H−TiB2, 2H−ZrB2, and t−WB) on their unit cells and on the unit cell of the surrounding 6H–SiC matrix. The precision of these predictions was 7.1% or better. Hence, in principle, it is possible to investigate the distributions of residual bulk stress/strain. Estimates of characterizing values of the three composite systems are attempted on the rough basis of the elastic constants of the SiC matrix, confirming the physical validity of this approach as a first approximation. Further, the residual bulk strain energies of the particles and the matrix are discussed in connection with the elastic term involved in the fracture energy of such composites.

A set of simple and accurate formulae for the first four moments of nuclear and electronic energy losses is proposed. A new variable is introduced to include the finite maximum-impact-parameter effect in the nuclear stopping process, which is assumed to be infinite in most studies. A critical energy at which the electronic energy loss is equal to the nuclear energy loss is also defined. It determines whether the nuclear or the electronic stopping process is the dominant mechanism in terms of incident-ion energy. The critical energy increases for heavy ions implanted in heavy target materials during the first moment of energy loss. The second moment of electronic energy loss is important only for light ions implanted at high ion energies. The third and fourth moments of nuclear energy loss are much larger than those of the electronic energy loss for all ion-target combinations. Theoretical predications of the projected ranges and range stragglings for gold ions implanted in carbon films are close to the experimental data when these proposed four moments of nuclear and electronic energy losses are considered.

Thin, oriented films of poly-1,4-phenylene (PPP) were prepared with a specially designed reaction vessel. Various kinds of metals were deposited by vacuum evaporation on the PPP substrate, the temperature of which was able to be changed up to 400 °C. Of the studied metals, tellurium and bismuth exhibited the oriented crystallization on it. The oriented overgrowth of tellurium crystallites occurred in the temperature range of 150 °C–200 °C. There were two modes of oriented overgrowths of crystallites in the case of bismuth; one was performed by deposition around room temperature and the other at about 100 °C. The oriented overgrowths of bismuth and tellurium on PPP were examined in terms of the mismatch parameter of the crystal lattice, and it was found that the overgrowths were caused by the lattice matching at the interface between the crystallites of the metals and the PPP substrate.

Multivariable screening and response surface experiments have been performed to model ohmic contact resistance (Rc) of a Ni–Ge–Au ohmic metal process for n+ GaAs-based high electron mobility transistors (HEMTs). Seven variables were examined via a fractional factorial screening experiment to rank the effects of each process variable. The results of the screening experiment indicated that the most significant variables were total Ge and Au evaporated thickness, Ge-to-Au ratio, and the post-alloy cooling time. Response surface experiments were designed around these three variables to examine the first- and second-order effects. The results enabled the development of an empirical model of ohmic contact resistance from which a new low value of 0.03 ± 0.03 Ω · mm (one-sigma) was predicted. Twenty confirmation runs on the new process indicated an average Rc of 0.06 ± 0.02 Ω · mm (one-sigma), with a range of 0.02 Ω · mm to 0.11 Ω · mm, a reduction from the previous average process value of 0.14 ± 0.07 Ω · mm (one-sigma).

Cubic diamond was synthesized with two systems, (1) graphite with pure magnesium carbonate (magnesite) and (2) graphite with mixed potassium and magnesium carbonate at pressures and temperatures above 9.5 GPa, 1600 °C and 9 GPa, 1650 °C, respectively. At these conditions (1) the pure magnesite is solid, whereas (2) the mixed carbonate exists as a melt. In this pressure range, graphite seems to be partially transformed into hexagonal diamond. Measured carbon isotope δ13C values for all the materials suggest that the origin of the carbon source to form cubic diamond was the initial graphite powder, and not the carbonates.

Planar laser-based imaging measurements of fluorescence and particle scattering have been obtained during flame synthesis of iron-oxide/silica superparamagnetic nanocomposites. The theory and application of laser-induced fluorescence, the spectroscopy of FeO(g), and the experimental approach for measurement of gas phase precursors to particle formation are discussed. The results show that the vapor phase FeO concentration rapidly rises at the primary reaction front of the flame and is very sensitive to the amount of precursor added, suggesting nucleation-controlled particle growth. The FeO vapor concentration in the main nucleation zone was found to be insensitive to the amount of silicon precursor injected, indicating that nucleation occurred independently for the iron and silicon components. Light scattering measurements indicate that nanocomposite particles sinter faster than single component silica, in agreement with TEM measurements.

Stoichiometric Ca2CuO3, having square-planar Cu-chains [C. L. Teske and H. Müller-Buschbaum, Z. Anorg. Allg. Chem. 379, 234 (1970); M. Hjorth and J. Hyldtoft, Acta Chem. Scand. 44, 516 (1990)], is expectedly antiferromagnetic due to 1D intrachain superexchange [K. Okuda, S. Noguchi, K. Konishi, H. Deguchi, and K. Takeda, J. Magn. Magn. Mater. 104–107, 817 (1992)]. Nonetheless, we report remarkable spontaneous ferromagnetism at 293 K after sintering, prominently in oxygen. This apparently introduced excess oxygen at vacant quasioctahedral sites, promoting spin-flip and ferromagnetic interchain coupling. Thermogravimetry (TGA) revealed excess oxygen, ≈0.17 O/Cu. X-ray diffraction (XRD) yielded a comparatively smaller unit cell. Ferromagnetism disappeared by oxygen depletion, mimicking reported nonmagnetism of Ca2CuO3−δ [Okuda et al. (1992)]. Elemental analysis showed insignificant magnetic impurity traces. Tc ranged between 680 K and 723 K, depending on freshness and purity. Saturation magnetization varied with processing, optimally 0.30 A · m2/kg at 1.0 T applied field. Coercivity and remanence varied with purity.

A process for the formation of low-resistance Ni–Ge–Au ohmic contacts to n+ GaAs has been refined using multivariable screening and response surface experiments. Samples from the refined, low-resistance process (which measure 0.05 ± 0.02 Ω · mm) and the unrefined, higher resistance process (0.17 ± 0.02 Ω · mm) were characterized using analytical electron microscopy (AEM), transmission electron microscopy (TEM), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), and x-ray photoemission spectroscopy (XPS) depth profiling methods. This approach was used to identify microstructural differences and compare them with electrical resistance measurements. Analytical results of the unrefined ohmic process sample reveal a heterogeneous, multiphase microstructure with a rough alloy-GaAs interface. The sample from the refined ohmic process exhibits an alloy which is homogeneous, smooth, and has a fine-grained microstructure with two uniformly distributed phases. XPS analysis for the refined ohmic process sample indicates that the Ge content is relatively depleted in the alloy (relative to the deposited Ge amount) and enriched in the GaAs. This is not evidenced in the unrefined ohmic process sample. Our data lead us to conclude that a smooth, uniform, two-phase microstructure, coupled with a shift in Ge content from the post-alloy metal to the GaAs, is important in forming low-resistance ohmic contacts.

The thermal properties and the crystallization behavior of fluorogallate-based glasses were analyzed. The kinetic nature of the glass transition was used to determine the temperature dependence of the viscosity and from it an estimation of the appropriate drawing temperature for an optical fiber was established. The crystallization kinetics were studied by using both isothermal and continuous heating regimes. The temperature range for nucleation was evaluated and for samples previously nucleated the activation energy of the growth process was found. The results were used to estimate the empirical nucleation and crystal growth rates from which the time-temperature-transformation curves and the temperature-heating rate-transformation diagrams were constructed. The results obtained agree with experimental data and are discussed in the light of minimizing the volume of crystals formed during fiber drawing.

For the first time, the refractive index of polyparaxylylene films, the only polymers grown commercially by chemical vapor deposition (CVD), is reported throughout the visible spectrum. This information is required if optical components such as antireflective coatings or waveguides are to be fabricated with CVD polymers. These properties are compared to a low-index CVD copolymer, poly(parachloroxylylene-co-perfluorooctyl methacrylate), invented in our laboratory. The ellipsometric constants psi and delta were measured for wavelengths between 400 nm and 1000 nm using variable angle spectroscopic ellipsometry; many samples of each film were grown to improve statistics. The data were modeled assuming a birefringent Cauchy dispersion; excellent agreement between models and experimental data was obtained. The refractive index (λ = 632.8 nm) of the copolymer in the film plane was 1.389, compared to 1.645–1.665 for the homopolymers. PPX, PPX-C, and the copolymer showed negative birefringence, while PPX-D showed positive bifringence. The optical properties of PPX showed little thickness dependence for films ranging from 36 nm to 2100 nm thick.