A triphasic cordierite-type gel was prepared from silica sol, boehmite sol, and an aqueous solution of Mg(NO3)2 · 6H2O. The silica sol was obtained from water glass by the ion exchange method, while boehmite sol was obtained by peptization of freshly prepared Al(OH)3. Phase transformations occurring in the gel were studied by differential scanning calorimetry, x-ray diffractometry, and Fourier transform infrared spectrometry. Spinel was observed to crystallize from the gel prior to cristobalite; their reaction subsequently yielded α-cordierite. At higher temperatures, α-cordierite transformed into modulated β-cordierite. Kinetic parameters of α-cordierite formation and α-cordierite to modulated β-cordierite transformation were determined by differential scanning calorimetry under nonisothermal conditions. Formation of a-cordierite was found to be a diffusion-controlled process, with an overall activation energy of Ea = 1242 ± 66 kJ/mol. During the α → β-cordierite transformation, a modulated phase was formed by surface transformation of α-cordierite. The overall activation energy for the formation of the modulated structure is Ea = 583±77 kJ/mol.

The densification and grain growth of ZnO doped with Al from 0.08 to 1.2 mol% were investigated during isothermal sintering between 1100 and 1400 °C. The Al dopant significantly inhibited the grain growth of ZnO and increased the grain growth exponent from 3 for pure ZnO to 4–6 for Al-doped ZnO. The grain growth activation energy was also changed from approximately 200 kJ/mol for pure ZnO to approximately 480 kJ/mol for Al-doped ZnO. The results of x-ray diffraction, scanning electron microscopy, and transmission electron microscopy showed that a ZnAl2O4 spinel phase existed as a second phase at the ZnO grain boundaries in Al-doped ZnO specimens. The spinel particles exerted an effective drag (pinning) on the migration of ZnO grain boundaries. The analyses of the Al doping effect on the densification rate provided evidence that the driving force for densification was reduced by the second-phase particles. A mechanism of pore surface drag (pinning) on densification equivalent to the observed drag (pinning) of grain boundaries on grain growth was proposed.

An aluminum nitride–diamond composite has been produced by sequential deposition of AlN and diamond in a triple torch plasma reactor (TTPR). AlN was deposited from AlN powder by injection into the argon–nitrogen, converging plasma plume of a TTPR. Velocity and temperature profiles of the converging plasma plume, obtained by enthalpy probe measurements, were used to show that the powder decomposed prior to reaching the substrate. Diamond was deposited in an argon–hydrogen–methane system onto the existing AlN film. Characterization of an AlN–diamond–AlN composite indicated a Vickers hardness of 18.6 GPa and a modulus of elasticity of 245–282 GPa.

Nanostructured WC–18% Co powder was synthesized by using cryogenic mechanical milling, and the thermal stability of the nanostructured powder was investigated in detail. The results indicated that the as-synthesized WC–18% Co powder had an average WC particle size of 25 nm. Growth of WC particles occurred above 873 K; however, the average WC particle size remained smaller than 100 nm in the powder isothermally heated for 4 h at 1273 K. Thermal exposure in air at T < 623 K did not result in significant oxidation of the cryomilled powder. The thermal exposure did promote the formation of WO2 and WO3 oxides. The Co6W6C phase was detected by x-ray diffraction in the powder heated in nitrogen at 1273 K, and the phases associated with decarburization of WC, such as W2C, W3C phases, were not observed. With increasing temperature, the dissolution of W and C elements in the Co matrix led to a gradual increase in {111} crystallographic plane spacing, eventually leading to the formation of an amorphous phase.

Portions of the same epitaxial (103)-oriented SrBi2Nb2O9 film grown on (111) SrTiO3 for which we recently reported the highest remanent polarization (Pr) ever achieved in SrBi2Nb2O9 (or SrBi2Ta2O9) films, i.e., Pr = 15.7 μC/cm2, have been characterized microstructurally by plan-view and cross-sectional transmission electron microscopy (TEM) along three orthogonal viewing directions. SrBi2Nb2O9 grows with its c axis tilted 57° from the substrate surface normal in a three-fold twin structure about the substrate [111], with the growth twins' c axes nominally aligned with the three 〈100〉 SrTiO3 directions. (103) SrBi2Nb2O9 films with and without an underlying epitaxial SrRuO3 bottom electrode have been studied. Dark-field TEM imaging over a 12 μm2 area shows no evidence of second phases (crystalline or amorphous). A high density of out-of-phase boundaries exists in the films.

Gas effusion measurements on zinc phthalocyanine (ZnPc) layers showed the presence of a significant amount of oxygen and water inside the material during exposure to ambient conditions. Of both species the bulk concentration lay in the range of 1020 molecules per cm3. Temperature-dependent analysis indicated that at 296 K all O2 molecules, and roughly one half of the H2O molecules, were mobilized and diffused with diffusion coefficients DO2 of 3 ∗ 10−8 cm2/s and DH2O of 1.3 ∗ 10−10 cm2/s. Electrical analysis of ZnPc layers in controlled atmospheres revealed that the electrical properties of the bulk were determined by O2, whereas H2O influences the surface conductivity. A space-charge density of (1.6 ± 0.2) ∗ 1016 O2− ions per cm3 was measured in atmospheric conditions.

Ti, Fe, and Co ions were implanted in two ceramics, SiC and Si3N4, to reach concentrations on the order of 10% over a depth of about 50–60 nm. X-ray absorption spectroscopy was performed at the K edge of the implanted ions to identify their local environment at the end of the implantation process. Ti was found to form Ti–C and Ti–N bonds whereas Co and Fe precipitated and formed clusters in Si3N4. CoSi was detected in SiC whereas, in the same matrix, Fe clusters coexist with FeSi. A coherent interpretation of these results is given in terms of the heat of reaction for all possible systems. We also successfully interpret in the same way some results found in literature in the case of implanted oxides.

Carrier diffusivity has been experimentally determined in low-doped n-type epitaxial 4H–SiC over a wide injection range using a Fourier transient grating technique. The data showed that, with injection, the diffusion coefficient increased from a minority-hole diffusivity Dh = 2.3 cm2/s to an ambipolar diffusivity Da = 4.2 cm2/s at approximately 1016 cm−3 with a substantial decrease occurring at higher injections. The derived Dh value corresponded to a minority-hole drift mobility of μh = 90 cm2/Vs, about 30% lower than available majority-hole mobilities. Also, the temperature dependence of the ambipolar diffusivity in the 296–523 K range has been determined. It followed a power law Da ∼ T−1.3 which notably differed from the expected one using the majority-hole mobility temperature dependence.

With the addition of Sr into the NdO1.5–BaO–CuOz flux, series single crystals of Nd1+x (Ba1−ySry)2−x Cu3O7±δ solid solutions (Nd1113ss) were successfully grown by crystal pulling. The liquid composition control was of key importance for controlling the crystal composition, which led to a fundamental structure control. The tetragonal Nd1113ss structure was readily obtained, using a Ba-poor liquid, due to a higher Sr liquid solubility, or using a liquid with the Ba/Cu ratio around 0.33. On the other hand, a Ba-rich liquid could effectively suppress the Nd substitution at Ba sites. The higher Sr addition for achieving a stoichiometric Nd1113 compound was thermodynamically prohibited by (i) an inherently low Sr liquid solubility and (ii) the formation of BaSrCu2Oz phase in the flux at the temperature range for crystal growth. The liquid-solid-structure relation was studied.

The synthesis of silicides of tantalum (TaSi2, Ta5Si3, Ta2Si, and Ta3Si) by field-activated combustion synthesis was investigated. The phases TaSi2, Ta5Si3, and Ta2Si can be synthesized in relatively pure form through field activation. The first compound requires a threshold field of 6 V cm−1 to initiate a combustion wave. The second and third compounds can be synthesized with all field values (0 < E < 20 V cm−1), but require considerable ignition time when E = 0. The stoichiometry Ta3Si does not sustain a combusion front unless E ≥ 20 V cm−1. However, the product is not the desired single phase. Wave velocities in the synthesis of the Si-rich phase, TaSi2, are considerably lower than those of the other two and showed a much weaker dependence on the field. The mechanism of phase formation for TaSi2 and Ta5Si3 was investigated from frozen wave analysis. No intermediate phase forms in the TaSi2 case, while in the case of Ta5Si3, TaSi2 is present as an intermediate phase. Additional investigations on the mechanism of silicide formation included isothermal solid–solid diffusion-couple and solid–liquid experiments.

In a metastable solution the particle growth rate of silicon dioxide increased with an increase in the initial supersaturation of the metastable solution and agitation speed in the ranges of 2.5 × 10−4 to 2.0 × 10−3 M and 300–1500 rpm, respectively. Based on a power law expression, the particle growth rate order was estimated as 2.0 independent of the initial supersaturation and agitation speed. Meanwhile, the particle growth rate coefficient was enhanced from 2.0 × 10−3 to 1.4 × 10−2 with increase in the agitation speed from 300 to 1500 rpm. From the experimental data, it would appear that the enhanced particle growth rate resulted from the promotion of molecular transport due to the agitation and driving force of the supersaturation in the particle growth process. A slight addition of sodium chloride into the metastable solution caused a marked reduction of the particle growth rate due to the inhibition of growth process by sodium chloride adsorbed on the particle. This effect of sodium chloride on the particle growth appeared in a significant drop of the particle growth rate coefficient from 4.5 × 10−3 to 8.0×10−4 with increase in the sodium chloride concentration from zero to 5.0×10−3 M, but not in the particle growth rate order. The influence of sodium chloride on the particle growth process of silicon dioxide predicted with a Langmuir isotherm matched with the experimental data.

We developed a diamond surface that does not mist near the room temperature under a saturated humidity atmosphere, by sheet electron beam irradiation (SEBI) treatment. SEBI treatment decreased the time to clear vision of the diamond surface. Following SEBI treatment for 1.91 s (= 0.72 MGy) to a diamond surface, the time to clear vision was less than 2 s. The effective duration time was a few hours. Based on the results of the size distribution of the drops on the misting-free diamond surface following blowing for 3 s, we proposed an explanation for the short time to clear vision of the diamond surface treated by SEBI.

Microscale sensing and actuating components are prevalent in microelectromechanical systems. Deformations of microscale components are dependent not only on the strains in the body, but also on the strain gradients. The contribution of strain gradients to plastic hardening is characterized by the specific strain gradient modulus of the material. The specific strain gradient modulus has been predicted to vary with the plastic strain. The moduli of plastically prestrained epoxy specimens were experimentally characterized in this investigation using nanoindentation. Prestraining induced softening and an energy model are developed to separate the effect of prestrain softening from the effect of strain gradient. The results indicated that the contribution of strain gradient to hardening was initially large but diminished with increased plastic deformation. A model was developed for power law material and was shown to compare well with the experimental results.

Crystalline and pore-free films of α–Fe2O3 were prepared on hydrophilic self-assembled organic monolayers (DTT-SAMs) at 80 °C. Subsequently, Fe3O4 and γ–Fe2O3 films were synthesized via post annealing of as-deposited α–Fe2O3. In situ patterning of crystalline iron oxide thin layers was achieved via microcontact printing (μCP) and selective deposition. μCP was used to pattern two different surface moieties of self-assembled organic monolayers (SAMs) on Au–Cr–Si substrates. An elastomeric stamp was used to transfer either hexadecanethiol (HDT) SAMs, which are to sustain deposition of iron oxide precipitates, or hydrophilic SAMs [e.g., dithiothreitol (DTT)]. Selective deposition was realized through precipitation of iron oxide phases. Iron oxide films were deposited onto hydrophilic SAMs, but not onto HDT surfaces. Line (width of <1 μm) patterns in crystalline α–Fe2O3 thin films were obtained.

The effective symmetry and material properties of twinned ferroelectric crystals with perovskite structure were analyzed. The twins or twinbands studied here were formed during ferroelectric phase transitions, which resulted in one of the following symmetry changes: m3m → 3m, m3m → 4mm, and m3m → mm2. It was found that the volume ratios of the two domains in a twin structure were not always equal due to the existence of defect pinning to the domain walls. This unequal partition changed the effective symmetry; hence, the effective macroscopic physical properties of the twin system. Using the data of LiNbO3, BaTiO3, and KNbO3, a detailed analysis has been carried out on macroscopic material property changes caused by the deviation from equal domain volume partition for crystals having 3m, 4mm, and mm2 symmetries.

Ca-α-sialon compacts pressureless-sintered to intermediate temperatures, which consisted of both α-sialon and unreacted α–Si3N4 grains, were investigated with transmission electron microscopy for an overall composition Ca1.8Si6.6Al5.4O1.8N14.2. Special attention was paid to identification of the possible crystallographic orientation between a-sialon and the α–Si3N4 particles. In contrast to the frequently occurring heteroepitaxial nucleation of α-sialon in rare-earth-doped samples with low x values, this study showed that most of the newly formed α-sialon grains had no epitaxial orientation relationship with the α–Si3N4 particles, suggesting nonepitaxial heterogeneous nucleation to be a more probable mechanism for the Ca–α-sialon phase with high Ca concentrations.

Samples of an Al–3% Mg alloy and an Al–3% Mg–0.2% Sc alloy were subjected to equal-channel angular pressing (ECAP) to reduce the grain size to approximately 0.2–0.3 μm. Some samples of each alloy were also annealed for 1 h at temperatures of either 423 or 673 K, respectively. High-resolution electron microscopy was used to examine the microstructure both before and after annealing. The grain boundaries after ECAP were wavy and faceted and in high-energy nonequilibrium configurations. These results were consistent with earlier observations of materials subjected to severe plastic deformation using high-pressure torsion. In addition, some grain boundaries in the Al–Mg–Sc alloy had a zigzag appearance after annealing at 673 K, where the straight portions of the boundary were identified as low-energy {111} planes. It is suggested these are mobile boundaries lying in a lowest energy configuration where mobility may be restricted by the presence of incoherent Al3Sc particles.

A quantitative texture analysis, including calculations of the orientation distribution function, is applied to investigate the preferred orientation of β–Si3N4 in a fine-grained material containing almost equiaxed grains that has been hot-pressed, annealed, and plane-strain compressed. The results show that (i) plane strain compression can produce relatively strong textures that were dependent on the compressive strain; (ii) the basal plane of hexagonal β–Si3N4 was normal to the hot-pressing direction for the hot-pressed and annealed samples, whereas it was parallel to the stress axis for deformed samples; and (iii) the mechanisms for texture development were preferred grain growth for the annealed sample and grain rotation for the hot-pressed and deformed samples, respectively.

Microscale sandwich beams with cell diameters and wall widths down to 150 and 15 μm, respectively, and having both metallic and polymer/metal cores were produced through fabrication methods that combined photolithography and electrodeposition. Various core structures were used, including some with negative Poisson's ratio. The bending response was investigated and compared with beam-theory predictions. Most of the cores evaluated had sufficient shear stiffness that the bending compliance was relatively high and dominated by the face sheets. Two of the core configurations were “soft” and exhibited behavior governed by core shear. The relative dimensions of the cores evaluated in this study were far from those that minimize the weight, because of fabrication constraints. The development of an ability to make high-aspect ratio cores is an essential next step toward producing structurally efficient, lightweight microscale beams and panels.

The elastic properties of cubic samples of compressed expanded graphite determined by means of ultrasonic velocity measurements are presented. These materials are highly porous and exhibit porosity-dependent anisotropic moduli. The results are analyzed according to two approaches. The first involves semi-empirical equations fitted to the experimental data, resulting in information about the shape and the connectivity of pores. It is found that pores are oblate ellipsoids, connected parallel to their direction of flatness. The second approach is based on application of the percolation theory near the rigidity threshold. The value of the critical exponent indicates that compressed expanded graphites behave like elastic networks in which central forces are predominant. Results of this study give evidence that ultrasound is a convenient and accurate method for investigation of the critical behavior of the elastic properties in highly tenuous structures.