A Dy2O3 single crystal has been used as a seed for the growth of isothermally melt-textured Dy-123 material. The nucleation-controlled step has been observed to be related to the heterogeneous nucleation of 211 particles at the surface of the dysprosium oxide single crystal. The subsequent growth mode seems to be controlled by a high concentration gradient of dysprosium in the liquid phase. This leads to a directional solidification process of the 123 phase. The size of the 211 particles seems to decrease as the distance from the dysprosium oxide single crystal increases.

The standard molar enthalpies of formation ΔfH°m of α−Si3N4 and β−Si3N4 have been determined by fluorine combustion calorimetry: ΔfH°m (Si3N4, cr, α, 298.15 K) = − (828.9 ± 3.4) kJ · mol−1 and ΔfH°m (Si3N4, cr, β, 298.15 K) = – (827.8 ± 2.5) kJ · mol−1. These results indicate that the enthalpy of the α-to-β transition, approximately (1 ± 4) kJ · mol−1, is negligible within experimental uncertainty.

Al2O3−34 wt.% TiC ceramics have been machined with a KrF (248 nm) excimer laser under normal atmosphere. In the initial steps of the irradiation process both the roughness and the removal rate present a strong variation with the number of pulses. After approximately 200 pulses the process reaches a stationary regime where the roughness and the removal rate become constant. Characterization of the machined areas by scanning electron microscopy showed that the variations in roughness and removal rate are related to the evolution of the surface topography of the samples. Also, as a consequence of laser irradiation, TiC and Al2O3 are partially transformed into TiO2, TiC0.7N0.3, and an Al–Ti solid solution.

Pure, Pr3+, and Yb3+ doped Ca-fluoroapatite (Ca-FAP) crystals were grown by the Czochralski method. The effective distribution coefficient keff for Yb3+ was 0.5. For Pr3+ a very high keff of 1.4 was obtained. Values for keff are discussed in terms of an elastic model accounting for the strain energy originating from the difference in the size of Ln3+ ions. The Ln3+ concentrations were measured by absorbance spectroscopy, by inductively coupled plasma optical emission spectroscopy, and by electron microprobe analyses.

Superconducting Bi2Sr2CaCu2O8+δ (Bi-2212) compound was electrochemically reduced in a protogenic electrolyte of benzoic acid dissolved in acetone. The critical temperatures (Tc) of the reduced Bi-2212 were enhanced from 75 K up to ∼90 K, which were reportedly the highest value of Bi-2212 superconductor. In spite of the enhancement of Tc, a diamagnetism of Bi-2212 was weakened after the reduction. This phenomenon was discussed in terms of the flux penetration depth. The electrochemically reduced Bi-2212 had a different structural stability from a partly oxygen-removed Bi-2212 which was prepared by annealing in reducing atmospheres. These results are attributable to injection of protons from the benzoic acid into the Bi-2212 structure.

Atomic force microscopy (AFM) is commonly used for microwear/machining studies of materials at very light loads. To understand material removal mechanism on the microscale, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) studies were conducted on the microworn/machined single-crystal silicon. SEM studies of micromachined single-crystal silicon indicate that at light loads material is removed by ploughing. Fine particulate debris is observed at light loads. At higher loads, cutting type and ribbon-like debris were observed. This debris is loose and can be easily removed by scanning with an AFM tip. TEM images of a wear mark generated at 40 μN show bend contours in and around the wear mark, suggesting that there are residual stresses. Dislocations, cracks, or any special features were not observed inside or outside wear marks using plan-view TEM. Therefore, material is mostly removed in a brittle manner or by chipping without major dislocation activity, crack formation, and phase transformation at the surface. However, presence of ribbon-like debris suggests some plastic deformation as well.

A novel, simple, clean, and fast microwave assisted method of preparing important transition metal silicides (MoSi2, WSi2, CoSi2, and TiSi2) has been described. Amorphous carbon is used both as a microwave susceptor and as a preventer of oxidation.

Time-resolved x-ray diffraction (TRXRD) was performed during Ti5Si3 synthesis by the self-propagating high-temperature synthesis mode for different Ti size fractions. It was determined that the time for product formation (ca. 15 s) was independent of Ti particle size. However, the formation of Ti5Si4 phase occurred when relatively large titanium particles were used. A simultaneous measurement of the temperature and TRXRD allowed us to attribute the shifting of XRD peaks at high temperature to thermal expansion of the Ti5Si3 product. The thermal expansion coefficients differ for different crystal planes, and their numerical values compare well with those reported previously in the literature.

This paper reports a study of microscopic on-chip corrosion on a 17 μm × 17 μm microelectromechanical device. The active atmospheric corrosion occurred only on the Al−Si−Ti components which were connected directly to the TiW components. Adsorbed fluoride ionic species on the microelectromechanical device were found to activate the observed bimetallic corrosion on the Al−Si−Ti/TiW contacts. Water rinse or replacement of TiW by TiAlx completely eliminates the active corrosion. Electrochemical potential data confirm the dissimilar metal corrosion mechanism. Effective prevention of on-chip corrosion was achieved by the judicious design of the device components to avoid dissimilar metal contacts with large galvanic potential differences.

The mechanical properties of ion-implanted Al–Si alloy were studied using disk samples of alloy irradiated with Ar+, B+, and N2+ ions. Knoop hardness of ASTM 336.0 disks increased from 117 to 165 kgf/mm2 upon N2+ ion implantation. To measure tribological properties, lubricated ball-on-disk tests were performed using steel balls. The coefficients of friction of ion-implanted disks were higher than those of unimplanted ones. Ion implantation improved the wear resistance of the disks, and in the case of N2+ ion-implanted disks, the worn volume was smaller than 10−4 mm3. XPS analysis for the N2+ ion-implanted samples revealed the formation of aluminum and silicon nitride on the sample surface. On the other hand, the cross-sectional image of the ion-implanted surface showed precipitated Si which is held under the implanted N2+ ions.

Three-dimensional temperature (T)–pressure (P)–composition (X) phase diagrams of binary carbon-hydrogen (C–H) and carbon-oxygen (C–O) systems for activated low pressure diamond growth have been calculated. Based on an approximation of linear combination between C–H and C–O systems, a projective ternary carbonhydrogen-oxygen (C–H–O) phase diagram has also been obtained. There is always a diamond growth region in each of these phase diagrams. Once a supply of external activating energy stops, the diamond growth region will not exist. Nearly all of the reliable experimental data reported in the literature drop into the possible diamond growth region of the calculated projective ternary C–H–O phase diagram under the conditions of 0.01–100 kPa and above 700 K.

Ball milling has been used as a solid-state mechanical alloying technique in two binary systems of plastic crystals: neopentylglycol/pentaglycerin (NPG/PG), showing a partial solubility in the ordered phase, and 2-amino-2-methyl-1,3-propanediol/tris(hydroxymethyl) (AMP/TRIS) whose immiscibility in this ordered solid phase is almost total. For the AMP/TRIS system the stable state at room temperature was reached by milling. Contrarily, for NPG/PG, DSC measurements reveal that an annealing period is required after milling. These results have been compared with those of the pentaglycerin/pentaerythritol (PG/PE) binary system, previously studied, whose miscibility is total at room temperature.

Thin films of ZrO2 doped with MgO and Gd2O3, 1–1.5 μm in thickness are formed onto nickel substrates by reactive thermal evaporation using a dual-hearth electron gun. X-ray diffraction patterns of the deposits show changes in the crystallographic structure and average particle size as a function of the dopant content. A mixture of monoclinic and tetragonal phases gradually disappears to become a single cubic phase with increasing dopant molar fraction. The average crystallite size deduced from diffraction line broadening decreases as the dopant content increases. This observation is strongly confirmed by scanning electron micrographs which reveal a smooth surface topography. Fine-grained materials obtained here are interpreted in terms of high nucleation rate and kinetically limited grain growth. It appears that composition, crystallographic structure, and microstructure relations are of paramount importance in ZrO2-based films prepared by electron-beam evaporation.

Superplastic silicon carbide ceramics were fabricated at low temperatures by a liquid phase sintering very fine β–SiC powder. The microstructural features of this material, of both before and after the superplastic deformation, have been investigated by transmission electron microscopy. Evaluated from the point of view of phase transformation, dislocation motion, and dynamic grain growth, the materials show very stable microstructures, indicating that the superplastic deformation process was dominated by the liquid phase assisted grain boundary sliding. In addition, the material is also characterized by the formation of clusters of fine SiC particles (5–20 nm) encapsulated in layered graphitized carbon.

Post formed, silica submicrospheres synthesized by Stober's method have been subjected to a high intensity ultrasound radiation (20 kHz, 100 W/cm2) and their size, morphology, and surface silanol structure modified in situ. The processed silica powders have been characterized by a variety of techniques, such as powder x-ray diffraction (XRD), transmission electron microscopy (TEM), dynamic light scattering (DLS), BET nitrogen adsorption, and FT-IR spectroscopy. The silica microspheres formed through an irreversible sol-gel transition have been shown to aggregate by the condensation of interparticle silanols to larger particles under the influence of the shock waves emanating from an imploding cavity. The particle size as a function of sonication time passes through a maximum, suggesting the disintegration of the aggregates on longer exposure to ultrasound radiation. The sonication of dried silica microspheres in an inert dispersant decalin also led to the aggregation of microspheres to a lesser degree, suggesting the deactivation of surface silanols. Infrared spectroscopic investigations suggest a disruption of the hydrogen bonded network of surface silanols. The observed morphological changes have been discussed in terms of direct effect of cavitation on well-formed spheres rather than changes in growth mechanism and capture of primary particles.

The influence of the starting materials on the crystalline phases observed after hydrothermal synthesis of nickel and manganese-zinc ferrites was investigated. The combination of sulfates and sodium hydroxide showed the best results for the conditions studied. The morphological parameters of MnZn ferrites produced at different hydrothermal conditions (110–190 °C, 4–30 h) were analyzed. Changes in lattice parameter, particle size, density, size and total volume of pores, and in the surface area of the particles were analyzed as a function of temperature and processing time. The sintering process was employed in order to verify the reactivity of the hydrothermal powders at controlled atmosphere. High density and surface homogeneous ceramic bodies were obtained, without zinc volatilization. Lattice parameter variations were associated with changes in the cations distribution of the spinel during sintering.

A method for the preparation of nanosized zirconium (hydrous) oxide particles of narrow size distribution is described. The procedure yields stable dispersions at low temperatures and short reaction times in the absence of surfactants, using inorganic zirconium salts. Crystal structure, particle size distribution, electrokinetic properties, stability, and thermal behavior of the prepared particles were investigated. Colloidal dispersions were treated with ultrasound to study their effect on the crystal structure of the calcined samples.

Magnesium titanate and MgTiO3–CaTiO3 ceramics were prepared by a chemical (Pechini) route and classical mixed oxide route. Selected specimens were doped with Cr or La. Specimens were sintered at 1350 °C and 1400 °C. Microstructures were examined by optical microscopy, scanning electron microscopy, and transmission electron microscopy. Dielectric properties were determined at 8 GHz by the Hakki and Coleman method. The highest Q values were obtained for undoped, chemically prepared MgTiO3 (20800); any dopants caused the Q value to be degraded. Additions of small amounts of Cr (≤1 mol %) to mixed oxide magnesium titanate increased the density to 97.1% theoretical, and increased the Q value (from 7000) to 13,000. Additions of La led to the formation of La2Ti2O7 second phase and reduction in the Q value for both materials. Both Cr and La acted as effective sintering aids, increasing density (to a maximum of 99% theoretical for 1% mol La in chemically prepared samples) and relative permittivity (to 18.1 for the same specimens). The relative permittivity of MgTiO3–CaTiO3 ceramics increased with calcium content, but the corresponding Q values decreased (∈r = 19.9, Q = 8500 for Mg:Ca = 94: 6). Small additions of La to Mg–Ca titanates enhanced the dielectric Q values but decreased the relative permittivities.

The RBAO (Reaction Bonded Aluminum Oxide) process and water-based gel casting were combined to produce alumina platelet reinforced RBAO composites. In the RBAO process, a precursor powder mixture of Al metal and Al2O3 is reacted to form 100% ceramic. To obtain composites in which the platelets are highly aligned, tapes consisting of 10 vol.% homogeneously distributed alumina platelets and 90 vol.% RBAO precursor powder were made by water-based gel casting using an extended doctor blade arrangement. Pellets of textured composites were subsequently prepared by stacking sheets cut from the green tapes, and filter pressing. Randomly oriented platelet composites were made using the same starting powders and gelling procedure, but without the tape-casting step. Reaction bonding was carried out in a box furnace in air. Microstructures of the composites were characterized using x-ray diffraction (XRD) and scanning electron microscopy (SEM). The effect of platelet orientation on contact damage behavior was studied using a Hertzian indentation method. It was found that the textured composite exhibited improved damage resistance compared to the random composite.

Alumina/silicon carbide nanocomposites with 5 vol.% SiC nanoparticles were produced by slip casting, pressureless sintering, and hot isostatic pressing. The grain size dependence of both the bend strength and fracture toughness have been investigated. The strength exceeds 1 GPa at a grain size of 1.7 μm. Crack opening displacements (COD) were measured, revealing that crack tip toughness is considerably lower than in pure alumina and an R-curve behavior is unlikely to occur. By introducing artificial pores with a size of 60 μm, the micromechanical fracture process has been studied in both pure alumina and nanocomposites. In contrast to alumina, where an annular precrack forms prior to fracture, it is suggested that precrack formation is strongly impeded in the nanocomposites and failure is controlled by microcrack initiation. The high strength of Al2O3/SiC nanocomposites seems to be the result of an unusually high crack initiation stress.