Glass-ceramic powders with a composition of Li2O · Al2O3 · 4SiO2 (LAS) have been synthesized by the sol-gel technique using LiOCH3, Al(OC2H5)3, Si(OC2H5)4, Ti(OC2H5)4, and Zr(OC2H5)4 as starting materials and the phase transformation behavior during calcination has been investigated. Differential thermal analysis (DTA), x-ray diffraction (XRD), and scanning electron microscopy (SEM) were utilized to determine the thermal behavior of the gels. Considering the LAS gels with 6.0 wt. % TiO2 and various wt. % ZrO2 content, and peak position of the β-spodumene phase formation in DTA curves was shifted to a higher temperature when the ZrO2 content was increased. The activation energy of β-spodumene crystallization was 283.8 kcal/mol for LAS gels with 6.0 wt. % TiO2 and 2.0 wt. % ZrO2. Unlike foregoing studies for LAS gels, during calcination of the dried LASTZ gels from 800 °C to 1200 °C neither β-eucryptite nor γ-spodumene was noted to be present. The crystallized phases comprised of β-spodumenes as the major phase and rutile (TiO2) together with zirconia (ZrO2) are precipitated as minor phases.

The formation process of Ba(Mg1/3Ta2/3)O3 was confirmed to be a direct reaction between constituent compounds without the presence of intermediate compounds. Isothermal analysis of reaction kinetics indicated the controlling reaction to be a three-dimensional diffusion process. Based on the Ginstling–Brounshtein model, the activation energy of the formation process was estimated to be 257 kJ/mol. A new definition of the ordering parameter for Ba(Mg1/3Ta2/3)O3 was deduced to quantitatively evaluate the ordering degree. Raising sintering temperatures resulted in an increase in the ordering degree and bulk density of Ba(Mg1/3Ta2/3)O3. Reducing the barium content in Ba(Mg1/3Ta2/3)O3 substantially resulted in improved densification and enhanced ordering structure. On the other hand, an excess barium content in specimens hindered the progress of sintering, and also induced the disordering structure.

The finite element method has been used to study the behavior of aluminum alloy 8009 during elastic-plastic indentation to establish how the indentation process is influenced by applied or residual stress. The study was motivated by the experiments of the preceding paper which show that nanoindentation data analysis procedures underestimate indentation contact areas and therefore overestimate hardness and elastic modulus in stressed specimens. The NIKE2D finite element code was used to simulate indentation contact by a rigid, conical indenter in a cylindrical specimen to which biaxial stresses were applied as boundary conditions. Indentation load-displacement curves were generated and analyzed according to standard methods for determining hardness and elastic modulus. The simulations show that the properties measured in this way are inaccurate because pileup is not accounted for in the contact area determination. When the proper contact area is used, the hardness and elastic modulus are not significantly affected by the applied stress.

Structural and microstructural properties of synthetic thin films of pyrite (FeS2−x), prepared by thermal sulfuration of iron layers, were investigated from Rietveld refinements of x-ray diffraction data, collected by step/scan mode. From this refinement lattice constant, a, and sulfur position parameter, u, nearest neighbor Fe–S and S–S bond distances and tetrahedral and octahedral bond angles have been determined. Moreover, sulfur deficit in the samples, surface and volume-weighted crystallite size and microstrains were also obtained. From these data, the influence of temperature and time of sulfuration and sulfur pressure on their structural and microstructural properties has been established. Stoichiometric pyrite thin films are obtained by sulfurating the iron films at low temperatures (Ts ∼ 600–700 K) during short times (ts ∼ 0.5–2 h). These experimental conditions yield films with the highest a, u, Fe–S bond distance, and microstrains, as well as S/Fe ratios about 2.00, i.e., null sulfur vacancies, the smallest S–S bond distances, and crystallite size. Finally, the possible influence of these structural and microstructural characteristics on some physical properties (optical absorption, electrical resistivity …) of the films is discussed.

We report the microwave dielectric properties of composites made of nickel-coated graphite fibers in two different types of silicone polymers. The influence of matrix viscosity on the fiber alignment, fiber filamentation in the composites, and how those affect the permittivity and loss tangent of the composite are discussed. The dependence of the permittivity and loss of the composites on the permittivity and loss of the matrix will also be compared.

Using a cylindrical indenter (or punch), the impression creep behavior of MoSi2-SiC composites containing 0–40% SiC by volume, was characterized at 1000–1200 °C, 258–362 MPa punch pressure. Through finite element modeling, an equation that depends on the material stress exponent was derived that converts the stress distribution beneath the punch to an effective compressive stress. Using this relationship, direct comparisons were made between impression and compressive creep studies. Under certain conditions, compressive creep and impression creep measurements yield comparable results after correcting for effective stresses and strain rates beneath the punch. However, rate-controlling mechanisms may be quite different under the two stressing conditions, in which case impression creep data should not be used to predict compressive creep behavior. The addition of SiC affects the impression creep behavior of MoSi2 in a complex manner by pinning grain boundaries during pressing, thus leading to smaller MoSi2 grains and by obstructing or altering both dislocation motion and grain boundary sliding.

The effects of secondary pretreatments on diamond nucleation were investigated for the Si substrates pretreated by the diamond abrasion. When the substrate was just abraded with diamond powder, the nucleation density of diamond was 7 × 108/cm2. However, the nucleation density was found to be greatly decreased by various secondary pretreatments except by one wet chemical etching method. The nucleation density was reduced to 3 × 107/cm2 by the chemical etching (I), to 7 × 106/cm2 by the H2 plasma etching, and to ∼104/cm2 by the Ar sputtering, or O2 plasma etching. It was very slightly reduced to 3 × 108/cm2 by the chemical etching (II). The effects of secondary pretreatments in reducing the nucleation density were found to be very closely related to the removal of diamond seeds rather than topographic sites or structural defects. Therefore, diamond seeds generated by the diamond abrasion are considered as the main nucleation sites of diamond.

Copper oxide powders were prepared by the spray pyrolysis of copper nitrate solutions over a range of temperatures (400–1300 °C) and residence times (3–7 s). Phase-pure [by x-ray diffraction (XRD)] copper (I) oxide was obtained at 800–1300 °C in an inert (nitrogen) atmosphere. The particles varied from smooth, solid spheres at 1300 °C to irregularly shaped and hollow particles at 800 °C with dense particles of Cu2O being made only at 1000 °C or higher. The particles were polycrystalline with an average crystallite size of 42 nm at 800 °C, while at 1000–1200 °C, the particles were single crystals. Spray pyrolysis in forming gas (7% H2–N2) atmosphere at 500–700 °C gave Cu while spray pyrolysis in air yielded CuO over 800–1000 °C and a mixture of Cu2O/CuO at 1200 °C. These results show that solid, phase-pure Cu2O particles can be produced by aerosol-phase densification at temperatures below its melting point (1235 °C).

The effect of A-site vacancy order-disorder states on diffuse phase transition (DPT) of tungsten bronze Pb1−xBaxNb2O6 (PBN) ferroelectrics has been investigated. The A-site vacancy disordered PBN ceramics exhibit notable variations of the Curie temperatures (i.e., the temperatures at the dielectric maximum permittivities) up to 12 °C in response to frequency changed from 0.1 KHz to 100 KHz. The largest frequency dispersion occurred at the morphotropic phase boundary of 1 − X = 0.63, along with the lowest Curie point. In contrast, the A-site vacancy ordered PBN ceramics present little frequency dispersion in the range of 2 °C from 0.1 KHz to 100 KHz. Dielectric constants of the disordered PBN ceramics were generally higher than those of the ordered ones. In comparison with the ordered PBN ceramics, the Curie points of the disordered ceramics were shifted from lower to higher temperature as the Pb2+ cation percentage was decreased; i.e., the Curie temperatures of the disordered PBN ceramics were lower than those of the ordered ones when 1 − X ≥ 0.70, but higher when 1 − X ≤ 0.65. These differences are suggested to inherently result from the A-site vacancy order-disorder states. The relationship between the A-site vacancy order-disorder states and the dielectric properties has also been confirmed with studies of thermal hysteresis.

Direct β–FeSi2 film preparation from gaseous phase was examined using a radio-frequency (rf) sputtering deposition apparatus equipped with a composite target of iron and silicon. Films composed of only β–FeSi2 phase were formed at substrate temperatures above 573 K when the chemical composition of the film was very close to stoichiometric FeSi2. The β–FeSi2 films thus formed showed rather large positive Seebeck coefficient. When the chemical composition of the films were deviated to the Fe-rich side, ∈–FeSi phase was formed along with β–FeSi2. On the other hand, α–FeSi2 phase, which is stable above 1210 K in the equilibrium phase diagram, was formed at the substrate temperature as low as 723 K when the chemical composition was deviated to the Si-rich side. The formation of α–FeSi2 phase induced drastic changes in the morphology and thermoelectric properties of the films. The α–FeSi2 phase formed in the films was easily transformed to β–FeSi2 phase by a thermal treatment.

Diamond films were selectively nucleated and grown on single crystal (100) silicon by microwave plasma assisted chemical vapor deposition with submicron spatial resolution. A thermal silicon dioxide layer on the wafers was patterned by standard photolithography. Nucleation was performed by applying a dc bias of −250 to −350 V in a hydrogen-methane plasma. Lifting off the oxide layer by HF etching prior to growth delineated the nucleation pattern which was replicated by the diamond film after growth. The growth of polycrystalline diamond was performed in a hydrogen-carbon monoxide-methane mixture selected to facilitate (100) texturing. Individual faceted crystallites were grown on a square matrix of sites, with a pitch of 3 μm, by controlling the nucleation densities within the windows exposing the prenucleated silicon. However, the orientation of the crystallites was randomly aligned with respect to the (100) silicon lattice within the micron scale windows employed in this study.

TiB2 and TiB2/FeB composites have been formed at temperatures below 1000 °C, directly from ilmenite sand by reaction with amorphous boron. The structural transformations occurring during high-energy mechanical milling pretreatment and subsequent annealing of different mixtures of the constituents have been studied. On heating at temperature below 800 °C, complete borothermic reduction of the ilmenite structure is accomplished. The mixture so obtained with an ilmenite-boron ratio equal to 1/6 undergoes a sequence of reactions on further heating to form TiB2, FeB, and the amorphous phase B2O2.

The relationship between microtexture and crystallinity of highly crystallized graphites with the residual resistivity ratio ρ300K/ρ4.2K of 3.45–5.50 was investigated. The graphite crystals studied were kish graphite (KG), highly oriented pyrolytic graphite (HOPG), and highly crystallized graphite films prepared from carbonized aromatic polyimide films. The study was made by the observations of an electron channeling pattern and electron channeling contrast image (ECI) under scanning electron microscope and the measurements of x-ray diffraction, magnetoresistance, and Hall coefficient. The values of the mean free path of the carriers λ, which approximates the mean crystal grain size, were estimated to be 2.6–6.1 μm from the magnetoresistance at 4.2 K for the highly crystallized graphites. The values of the average crystal grain diameter D in the basal plane evaluated from ECI were several hundred microns or more for KG, 60 μm for HOPG, and 6 and 12 μm for the graphite films. The difference between the values of λ and D for each crystallized graphite was discussed in relation to other results obtained.

Porous resorbable Ca–P–O glassceramic tooth roots based on calcium biphosphate were prepared by loose-powder-sintering then crystallization-annealing. The glass composition is, by weight, CaO/(CaO + P2O5) = 0.33. The sintering behavior of the glass can be described by a conventional viscous flow model. The resultant glassceramic has a pore size of 6 to 36 μm, depending on starting particle size and sintering temperature, while the pore size distribution is independent of sintering time. The flexural strength is 33 to 150 MPa depending mostly on crystallization-annealing treatment. The crystalline phases are β−Ca2P2O7 and CaP2O6. After being implanted into rabbits, these porous implants show remarkable biocompatibility and induce the ingrowth of new bone within 30 days. They are partly resorbed after 90 days and replaced by new bone. In spite of the original small porosity, the ingrowth of blood vessels and bone cells is abundantly seen after 90 days, due to enlarged pores produced by progressive resorption. This glassceramic is a good candidate for resorbable tooth and bone implants. The loose-powder-sintering technique resulting in intricate bulk shapes with controllable pore size distribution and good machinability as well as adjustable mechanical strength hence is a powerful technique for the preparation of porous glassceramics.

X-ray diffraction analysis on C60 films shows that besides fcc phase, there also exists hcp phase, as well as a new crystalline phase with interplanar spacing (d-spacing) of planes parallel to the substrate 0.95 nm. The new phase may relate to the intercrystalline packed C60 molecules between fcc crystallites. The room temperature electrical conductivity of C60 films is found to be in the range of 10−5–10−8 (Ω · cm)−1. The room temperature conductivities of C60 films annealed at temperatures above 473 K are lower by one order of magnitude than those at temperatures below 463 K. This is because the interconnection between the fcc crystallites is weakened due to the disappearance of the new intercrystalline phase and the subsequent heightening of the intercrystalline potential barrier. From the measurement on the conductivity versus time when the film is maintained at a constant temperature, we identified the increase of conductivity is the result of the decrease of hcp phase, while the decrease of conductivity is due to the decrease of the new intercrystalline phase. Because the structures of the films become highly ordered, and defect states in the energy band gap decrease on annealing at high temperature, the conductivity activation energy increases.

Prior to considering crack-face bridging, the stress/strain-field ahead of the crack tip in the compact tension (CT) geometry is numerically assessed by means of finite element method (FEM). The stress field along the crack line which has a decreasing profile of tensile stresses from the crack tip converts to monotonically increasing compressive stresses toward the back face of the CT specimen via a rotational center. Based on these stress-field analyses, a novel crack-face bridging model for fiber-reinforced brittle matrix composites is presented. The application of the model to the experimental result of a 2D-C/C composite enables one to estimate the crack-face fiber bridging stresses and their distribution profile.

Growth of Li2B4O7 crystals has been carried out under hydrothermal conditions at relatively low temperature and pressure conditions (T = 250 °C, P = 100 bars). A systematic study of electrical measurements has been carried out within a wide range of internal frequency and temperature. The corresponding impedance, Arrhenius, and Bode plots are given.

PbMg1/3Nb2/3O3 (PMN) prepared by organic solution of citrates was analyzed by the Rietveld method to determine the influence of seeds and dopants on the perovskite and pyrochlore phase formation. It was observed that pyrochlore phase formation increases with an increase in calcination time when no additives are included during the preparation. It was also observed that a greater amount of perovskite phase appeared in doped or seeded samples. The fraction of perovskite phase increased from 88 mol% in pure sample to ∼95 mol% in doped and seeded samples calcined at 800 °C for 1 h. It is clear that the addition of dopants or seeds during PMN preparation can enhance the formation of perovskite phase.

The growth of NaLa(WO4)2 crystals has been carried out by the hydrothermal method at fairly low P-T conditions. The crystal morphology has been studied with respect to the growth parameters. The crystals obtained were characterized by various techniques such as x-ray diffraction (XRD), differential thermal analysis (DTA), and infrared (IR) spectroscopy.

Using a continuous microscratch technique, the adhesion strengths of Pt, Cr, Ti, and Ta2N metallizations to NiO and Al2O3 substrates have been characterized. The practical work of adhesion was determined as a function of both thickness and annealing conditions. For all except the Ta2N films, the practical work of adhesion increases nonlinearly from a few tenths of a J/m2 to several J/m2 as the thickness of the thin film is increased, indicating that a greater amount of plastic work is expended in delaminating thicker films. Further, the practical work of adhesion also increases with increasing annealing temperature, indicating stronger bonding at the interface. In the limit that the film thickness tends to zero, the plastic energy dissipation in the film tends to zero. As a result, the extrapolation to zero thickness yields the true work of adhesion for that system.