The transformation behavior from glassy state was investigated in Zr- and Hf-based glassy alloys. The primary phases are metastable face-centered-cubic (fcc) Zr2Ni and fcc Hf2Ni phases in the Zr65Al7.5Ni10Cu17.5 and Hf65Al7.5Ni10Cu17.5 glassy alloys, respectively. By substitution of 5 at.% Pd for Cu, the primary phase changes to an icosahedral quasicrystalline phase in both alloys. It is found that the addition of elements, which have a positive or weak chemical affinity with one of the constitutional elements in the Zr–Al–Ni–Cu and Hf–Al–Ni–Cu glassy alloys, is effective for the precipitation of the icosahedral phase. It is suggested that Pd plays a dominant role in an increase in the number of nucleation sites. Since an icosahedron is contained as a structure unit in the icosahedral, fcc Zr2Ni and fcc Hf2Ni phases, it is implied that these phases are correlated with the local icosahedral order. The high-resolution transmission electron microscopy images of the as-spun Zr65Al7.5Ni10Cu7.5Pd10 and Hf65Al7.5Ni10Cu12.5Pd5 alloys reveal a possibility of the existence of the icosahedral ordered regions. It is therefore, concluded that the icosahedral short- or medium-range order exists and it stabilizes the glassy state in the Zr- and Hf-based multicomponent alloys.

The results of an in situ transmission electron microscopy study of the formation of Co-silicides on patterned (001) Si substrates are discussed. It is shown that the results of the in situ heating experiments agreed very well with the data based on standard rapid thermal annealing experiments. Fast heating rates resulted in better definition of the silicide lines. Also, better lines were obtained for samples that received already a low-temperature ex situ anneal. A Ti cap layer gave rise to a higher degree of epitaxy in the CoSi2 silicide.

The mechanochemical behavior of the Ti–Si system was investigated across the whole composition range at a constant milling intensity. At low Si content the mechanical alloying process leads progressively to an amorphous structure. In the central range of the equilibrium diagram, crystalline intermetallic compounds form with a combustion-like behavior. A nanostructured composite of TiSi2 gradually evolves above the Ti25Si75 stoichiometry. Transformation behaviors relate to the thermodynamic and thermochemical properties of the tested mixtures as well as with their mechanical features and structural refinement, which change drastically within the explored composition range.

The fracture behavior upon stable crack propagation in bending was investigated for a ceramic matrix composite comprising 15 vol% of calcium hexaluminate (CaAl12O19 or “CA6”) in an Al2.O3 matrix and compared to the crack bridging stresses as measured by microprobe fluorescence spectroscopy. In addition, piezospectroscopy coefficients of -4.57 and -3.79 cm-1 GPa-1 were determined for the peaks located at 14488 and 14528 cm-1, respectively, for monolithic CA6. It was concluded that the macroscopic R-curve behavior of the composite could be predicted from microscopic bridging stress data and indicated microprobe fluorescence spectroscopy to be a significant experimental tool for the investigation of fracture micromechanisms in ceramic materials.

The low-temperature phase, trigonal phase, of space group R32 was discovered in the compound LaSc3(BO3)4 (LSB) doped with arbitrary concentration of Nd3+ ions (NLSB). For LSB, the lattice constants are a = 9.820 ± 0.003 Å, c = 7.975 ± 0.003 Å. The decomposition of NLSB phase was observed in two regions of temperature below and above the congruent melting point by differential thermal analysis and x-ray powder diffraction methods. The single crystals of 2 × 2 × 3mm3 of dominant trigonal phase for x = 0.5 were grown by the flux method (LiBO2). Second harmonic generation effect was observed in NLSB for x = 0 to 1. The concentration dependence of fluorescence lifetime was measured and derived from Dexter's theory of resonant energy transfer.

The optical absorption spectra of AgInS2:Co2+ single crystals grown by chemical transport reaction using iodine as a transporting medium have been studied at 6 K. The peaks can be explained by the transitions of Co2+ in the Td symmetry with the spin-orbit coupling, which means that the deviations of the atomic sites from those of the ideal wurtzite structure can be considered negligibly small. The consideration of both the crystal field parameters and the electronegativity difference between atoms may indicate that Co atoms substitute In atoms.

For a few years, we had been concentrating on development of completely closed diamond synthesizing system aimed for microgravity experiments. Recently we started the new method with a graphite heater as carbon source. With this method, a completely closed system is successfully performed. In situ gaseous species analysis with gas chromatography and the possible reaction model is discussed.

Bi4Ti3O12 thin films were grown epitaxially on SrTiO3(100) substrates by chemical solution deposition using metal naphthenates as starting materials. Homogeneous Bi–Ti solution with toluene was spin-coated onto the substrates and pyrolyzed at 500 °C for 10 min in air. Highly c-axis-oriented Bi4Ti3O12 thin films were crystallized by annealing pyrolyzed films at ≥650 °C. The x-ray pole-figure analysis indicated that the Bi4Ti3O12 thin films have an epitaxial relationship with the SrTiO3(100) substrates. The surface morphology of the films annealed at lower temperature, i.e., 650 °C, exhibited flat and smooth surfaces, while films annealed at higher temperatures, i.e., 750 and 800 °C, were characterized by three-dimensional outgrowth.

Twinned and detwinned Yba2Cu3O7−y (Y123) single crystals were observed by transmission electron microscopy to investigate the influences of the lattice defects on the peak effect for Y123 single crystals. Twin boundaries with the spacing of 0.2–0.5 μm were seen only in the twinned Y123 single crystals. Antiphase boundaries (APBs) along the (110)Y123 plane were observed in both twinned and 0.5h-detwinned samples, which showed the peak effect in high magnetic field over 3 T at 70 K. In contrast, APBs were not found in 100h-detwinned sample. Critical current densities of this sample were small all over the range of the applied magnetic field. In conclusion, we suggest that APBs have a significant influence on the peak effect of Y123 single crystals in the high magnetic field.

The fundamental absorption edge of Cu6P(S0.6Se0.4)5I and Cu6P(S0.4Se0.6)5I crystals was studied in the 77–320 K temperature range where no phase transitions were revealed by optical techniques. The temperature behavior of the exponential Urbach absorption edge in Cu6P(S0.6Se0.4)5I and Cu6P(S0.4Se0.6)5I crystals was analyzed. The effect of compositional disorder upon the Urbach edge parameters, parameters of exciton-phonon interaction, and lattice parameters in Cu6P(S1−xSex)5I, 0 ≤ x ≤ 1, crystals was studied. The effect of various types of disordering upon the optical absorption processes in Cu6P(S1−xSex)5I crystals is discussed.

The modified edge lift-off test (MELT) has gained enough acceptance in the community for evaluating interfacial adhesion that there is now commercial equipment for automating the test. However, there are several experimental and mechanics assumptions of the test that may provide unexpected outcomes. Experimental data suggested that for crack lengths greater than 5% of the film thickness the energy release rate was independent of crack length, contradicting the rule of thumb suggesting that the crack length should be greater than 10–20 times the film thickness to obtain a steady-state energy release rate in the edge crack problem. Finite element simulations not only corroborated the experimental observation but seemed to indicate that the crack length required for steady-state conditions was a function of the relative Young's moduli for the film and substrate. It was also shown via an analytical model that plate bending (commonly neglected) can significantly affect the energy release rate in the MELT and lead to incorrect conclusions regarding the reliability of an interface.

A new microtensile test device using a magnetic-solenoid force actuator was developed to evaluate the mechanical properties of microfabricated polysilicon thin films that were 100–660 mm long, 20–200 μm wide, and 2.4-μm thick. It was found that the measured average value of Young's modulus, 164 GPa ± 1.2 GPa, falls within the theoretical bounds. The average fracture strength is 1.36 GPa with a standard deviation of 0.14 GPa, and the Weibull modulus is 10.4–11.7. Statistical analysis of the specimen size effects on the tensile strength predicated the size effects on the length, the surface area, and the volume of the specimens. The fracture strength increases with an increase of the ratio of surface area to volume. In such cases, the size effect can be corrected to the ratio of the surface area to volume as the governing parameter. The test data accounts for the uncertainties in mechanical properties and may be used to enhance the reliability and design of polysilicon microelectromechanical systems devices.

The microstructure of La1–xAx(A = Ca or Sr)MnO3–δ thin films grown by liquid-delivery metalorganic chemical vapor deposition on (001) MgO and (110)pseudo-cubic LaAlO3 were studied by transmission electron microscopy. The La1–xCaxMnO3–δ thin film on large lattice mismatched MgO exhibited very defective microstructures and consisted of two typical regions. The first region was close to the film–substrate interface and had an epitaxial relationship to the substrate with many differently oriented domains nucleated on the substrate surface. The second region consisted of columnar grains with some degree of texture. In contrast, the smaller lattice-mismatched La1–xSrxMnO3–δ/(110)pseudo-cubic LaAlO3 film had good crystalline quality with highly oriented columnar grains but exhibited complicated dislocation structures. Apart from the misfit dislocations formed at the film–substrate interface, two types of anomalous dislocations with limited contribution to relieving misfit stresses were also observed. One type of dislocation had extra planes in the film and some climbed into the substrate. These dislocations were considered to form from dislocation loops during nucleation of the film. The other type of dislocations had extra planes parallel to the film–substrate interface and glided into the substrate side resulting in a 2° tilt of the film with respect to the substrate. The complicated dislocation configurations present in the sample were related to the complex strain field in the film. The relative strains along the interface measured in the film were heterogeneous. The variations of the strains in the film were related to the local Curie temperature changes and second-order phase transitions of the film.

Activated milled mesophase carbon fibers (AC-mMPCF, MP-series) show a higher specific capacitance in spite of a smaller specific surface area than those of powder-type activated carbons (AC-series). This phenomenon can be interpreted to mean that it is difficult to predict the capacitance of an electric double-layer capacitor (EDLC) knowing just the surface area and the pore size. More information is needed about other inherent characteristics of the samples, for example, the equivalent series resistance (ESR), shape of the pores, etc. We investigate here other characteristics of the samples. Consequently, it was deduced that the MP-series of EDLCs have a slit pore shape, which affects the accessibility of the electrolyte ion onto the electrode surface. Moreover, the MP-series of materials have suitable ESR values, and these material properties themselves should be considered as factors that affects the deterioration of the specific capacitance of EDLCs.

Cu(In,Ga)Se2(CIGS) thin films were prepared at substrate temperatures of 350 to 500 °C. The (In,Ga)2Se2 precursor layers were deposited on Mo coated soda-lime glass and then exposed to Cu and Se fluxes to form CIGS films. The surface composition was probed by a real-time composition monitoring method. The CIGS films were characterized by x-ray diffraction, energy dispersive x-ray spectroscopy, secondary ion mass spectroscopy, and atomic force microscopy. The transient formation of a Cu–Se phase with a high thermal emissivity was observed during the deposition of Cu and Se at a substrate temperature of 350 °C. Faster diffusion of In than Ga from the (In,Ga)2Se3 precursor to the newly formed CIGS layer was observed. A growth model for CIGS films during the deposition of Cu and Se onto (In,Ga)2Se3 precursor is proposed. A solar cell using a CIGS film prepared at about 350 °C showed an efficiency of 12.4%.

The hydrogen loading characteristics of nanocrystalline Mg, Mg–Ni (Ni from 0.1 to 10 at.%), and Mg–Fe (Fe from 1 to 10 at.%) alloys in 3 MPa H2 were examined using high pressure differential scanning calorimetry and thermogravimetric analysis. All samples showed rapid uptake of hydrogen. A decrease in the onset temperature for hydrogen absorption was observed with increasing Ni and Fe alloy content, but the thermal signatures obtained suggested that only Mg was involved in the hydriding reaction; i.e., no clear evidence was found for the intermetallic hydrides Mg2NiH4 and Mg2FeH6. Hydrogen loading capacity decreased with temperature cycling, and this was attributed to a sintering process in the alloy, leading to a reduction in the specific surface available for hydrogen absorption.

A simple procedure for the purification of the single-walled carbon nanotube (SWNT) product synthesized by the hydrogen arc-discharge method was proposed and discussed. The procedure involves ultrasonication in alcohol, oxidation in fixed air, and soaking in hydrochloric acid. Most of the amorphous carbon and carbon nanoparticles as well as metal particles in the product was successfully removed, according to the results obtained from transmission electron microscopy, thermogravimetric analysis, and resonant laser Raman measurements. With this procedure, a 41 wt% yield of the SWNTs with a purity of about 96% was achieved after purification.

Electrodeposited thin films of CdTe and CdxHg1−xTe with 1 − x = 0 and approximately 0.1 were characterized by x-ray photoelectron spectroscopy. The composition of the bulk and the thickness and composition of the native surface oxide before and after Ar+ ion sputtering were determined. A surface oxide layer 20-Å thick constituted mainly of alloyed TeO2 and CdO was found over a nearly stochiometric bulk. Chemical diffusion of Hg, Cd, and Te to the surface was observed. Hg appears to inhibit oxidation of the telluride, mainly of Te. Ar sputtering removed undesirable oxides and impurities off the films.

The structure and magnetic properties of Nd8.4Fe86Mo1.1B4.5 nanostructured magnets prepared by mechanical alloying (MA), compared with those by mechanical milling (MM), were studied. The intrinsic coercivity μ0Hc, the reduced remanence Jr/Js, and the maximum magnetic energy product (BH)max for Nd8.4Fe86Mo1.1B4.5 magnets were prepared by MM were notably higher than the values of the corresponding MA-prepared samples. The average grain sizes of both α–Fe and Nd2Fe14B in the MM-prepared samples were measurably smaller than corresponding values of the MA-prepared samples. A more homogeneous distribution of α–Fe grains in the MM-prepared samples than in the MA-prepared samples was obtained.

A simple and convenient solvothermal reaction has been developed to produce CuInS2 nanorods and nanotubes from the elements in ethylenediamine at 280 °C. The products were characterized by x-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, scanning electron microscopy, and x-ray photoelectron spectroscopy. Analysis shows that the coordinating ability of ethylenediamine and the existence of liquid In may play important roles in the growth of one-dimension nanocrystallites and the electron-transfer reaction. In addition, spherical CuInS2 micrometer particles were obtained at 350 °C.