We have studied grain-growth and texture development in polycrystalline lithium fluoride thin films using dark-field transmission electron microscopy. We demonstrate that we can isolate the size distribution of 〈111〉 surface normal grains from the overall size distribution, based on simple and plausible assumptions about the texture. The {111} texture formation and surface morphology were also observed by x-ray diffraction and atomic force microscopy, respectively. The grain-size distributions become clearly bimodal as the annealing time increases, and we deduce that the short-time size distributions are also a sum of two overlapping peaks. The smaller grain-size peak in the distribution corresponds to the {111}-oriented grains, which do not grow significantly, while all other grains increase in size with annealing time. A novel feature of the LiF films is that the {111} texture component strengthens with annealing, despite the absence of growth for these grains, through the continued nucleation of new grains.

We report the synthesis of Th1–xMnxO2 (x = 0, 0.001, 0.002, 0.004, and 0.01 wt%) nanoparticles by the urea combustion method using thorium nitrate gel followed by heat treatment at a higher temperature (T). The obtained Th1–xMnxO2 nanocrystals were characterized by x-ray diffraction (XRD), direct-current magnetization (M) measurements and electron paramagnetic resonance (EPR). XRD analysis revealed that Th1–xMnxO2 crystallizes in the cubic structure (Fm3m). M measurements showed ferromagnetic ordering at room temperature for Th0.99Mn0.01O2 samples annealed at 775 K. An intense and broad ferromagnetic resonance (FMR) having linewidth of ∼1200 G, was observed at relatively lower fields in the EPR spectra of Th0.99Mn0.01O2 samples annealed at 775 K, indicating the presence of a ferromagnetic phase at room temperature. EPR measurements were used to estimate the number of spins involved in the ferromagnetic ordering. Out of the total Mn present in Th0.99Mn0.01O2 samples, about 25% of the Mn2+ ions were found to be responsible for the ferromagnetic ordering. In addition to the FMR signal, a weak hyperfine sextet was observed at g = 2.0048 (55Mn, I = 5/2), which corresponds to the −1/2 ↔ +1/2 transition of Mn2+ ions, suggesting its presence at thorium sites (uncoupled spins). X-ray photoelectron spectra indicated that the manganese ions exist mainly as Mn2+, Mn3+, and Mn4+. The room-temperature ferromagnetism may be attributed to the coupling between these Mn2+ ions at thorium sites in ThO2 rather than due to the formation of any metastable secondary phases.

The electrical conductivities of Cu–3at.%Ti alloys aged at 773 K in a hydrogen atmosphere were investigated as a function of aging time. The electrical conductivity of the quenched alloy, 5.2% International Annealed Copper Standard (IACS), improved with aging time to 66% IACS after 48 h. This was mainly caused by the dilution of the Cu–Ti solid solution in the alloy, which is supported by the fact that the lattice parameter of the face-centered cubic (fcc) phase approaches that of pure Cu by aging in a hydrogen atmosphere.

The ultrastructure of nanoscale apatite biomimetically formed on an organic template from a supersaturated mineralizing solution was studied to examine the morphological and crystalline arrangement of mineral apatites. Needle-shaped apatite crystal plates with a size distribution of ∼100 to ∼1000 nm and the long axis parallel to the c axis ([002]) were randomly distributed in the mineral films. Between these randomly distributed needle-shaped apatite crystals, amorphous phases and apatite crystals (∼20–40 nm) with the normal of the grains quasi-perpendicular to the c axis were observed. These observations suggest that the apatite film is an interwoven structure of amorphous phases and apatite crystals with various orientations. The mechanisms underlying the shape of the crystalline apatite plate and aggregated apatite nodules are discussed from an energy-barrier point of view. The plate or needle-shaped apatite is favored in single-crystalline form, whereas the granular nodules are favored in the polycrystalline apatite aggregate. The similarity in shape in both single-crystalline needle-shaped apatite and polycrystalline granular apatite over a wide range of sizes is explained by the principle of similitude, in which the growth and shape are determined by the forces acting upon the surface area and the volume.

The relationship between the preparation conditions of MgB2 powder and the performance of the critical current density (Jc) of an applied magnetic field (B) of the final ex situ tape produced from it was investigated. The pelletizing pressure of the precursor is crucially important for improving the Jc-B performance of ex situ tape. The higher the pressure, the greater the resulting Jc of the ex situ MgB2 tape. We have shown that the pelletizing pressure used for the precursor mixture during the powder preparation process affects the phases formed in the MgB2. On the other hand, the heating time used is effective in changing the slope of the Jc-B curve of the final tape. This is thought to be due to a change in the crystallinity of the prepared MgB2 powder. The experimental data gathered here will become the basis for investigating the establishment of a guideline for preparing the starting powder used for the manufacture of ex situ MgB2 tape.

The relations among the process, microstructure, and nanomechanical properties of cosputtered Ta–Si–N thin films have been investigated. The microstructure evolution and varied hardness and elastic modulus property of Ta–Si–N were influenced by nitrogen flow ratios [FN2% = FN2/(Far + FN2) × 100%] during cosputtering together with phase formation and the composition of films. The microstructure of Ta–Si–N formed at a low 2–10 FN2% was an amorphous-like phase with nanocrystalline grains embedded in an amorphous matrix, while polycrystalline Ta–Si–N was obtained at a high 20–30 FN2%. The cubic TaN phase or (Ta1–x,Six)N solid solution is much easier to form polycrystallites than noncubic Ta5Si3, Ta2Si, and Ta2N phases from grazing incidence x-ray diffractometry results. Amorphous-like Ta–Si–N films had much higher nanohardness, stiffness, elastic recovery percentage, and a closer boundary compared to polycrystalline films. A maximum nanohardness of 15.2 GPa was obtained at 3 FN2%. An increased hardness of polycrystalline films at 20–30 FN2% is attributed to the higher amount of the hard TaN phase.

In situ scanning electron microscopy was performed during elevated-temperature (⩽760 °C) tensile-creep deformation of a face-centered-cubic cobalt-based Udimet 188 alloy to characterize the deformation evolution and, in particular, the grain boundary-cracking evolution. In situ electron backscatter diffraction observations combined with in situ secondary electron imaging indicated that general high-angle grain boundaries were more susceptible to cracking than low-angle grain boundaries and coincident site-lattice boundaries. The extent of general high-angle grain-boundary cracking increased with increasing creep time. Grain-boundary cracking was also observed throughout subsurface locations as observed for postdeformed samples. The electron backscattered diffraction orientation mapping performed during in situ tensile-creep deformation proved to be a powerful means for characterizing the surface deformation evolution and in particular for quantifying the types of grain boundaries that preferentially cracked.

We have studied grain coupling and critical current density (Jc) in ex situ processed Fe-sheathed MgB2 tapes fabricated by a powder-in-tube (PIT) technique, using MgB2 powder soaked in various chemical solutions. The grain coupling and the Jc are strongly influenced by the chemical solutions. Compared with the chemical treatment in a benzene solution of benzoic acid, the use of a cyclohexane solution of benzoic acid doubles the Jc value. Cyclohexane is less stable and hence effectively removed from the surface of MgB2 grains, bringing about the improved coupling of grains and the Jc enhancement.

The influence of the cooling rate on the structure, microhardness, relaxation, and devitrification behavior of Cu44Ag15Zr36Ti5 glassy alloy on heating is studied in the present work. According to transmission electron microscopy investigations, the structures of Cu44Ag15Zr36Ti5 glassy ribbon and bulk samples are somewhat different. The structure of the ribbon samples is amorphous while, the nanoscale clusters of the crystalline phase (highly ordered regions) are formed in the bulk samples. It is reflected in the shift of the x-ray diffraction peak, in the magnitude of the heat of structure relaxation and crystallization, as well as in the change in the Vickers microhardness. An analysis of the cooling curve is also performed.

The correlation among apparent global plasticity, Poisson’s ratio, and fragility in monolithic bulk metallic glass (BMG) alloys has been investigated in the present study. The shear and bulk moduli in monolithic Cu-based BMG alloys have been measured by resonant ultrasound spectroscopy (RUS) and ultrasonic technique. The Cu43Zr43Al7Ag7 BMG alloy showing a large apparent global plasticity (∼8%) exhibits a high Poisson’s ratio when compared with that of Cu43Zr43Al7Be7 BMG alloy. In addition, the fragility of Cu-based BMG alloys can be obtained by differential scanning calorimetry (DSC). The fragility index m of Cu43Zr43Al7Ag7 BMG alloy is slightly larger than that of Cu43Zr43Al7Be7 BMG alloy. The correlation between Poisson’s ratio and fragility in BMG alloys can be presented by a simple relation of m − 17 = 14 (B∞/G∞ − 1). Poisson’s ratio and fragility might be regarded as an important parameter that controls global plasticity of glass-forming alloys.

The formation of 10-nm ZnO nanopyramids using a simple synthetic route has been isolated from the reaction of Zn(OAc)2·2H2O in 1,4-butanediol followed by ripening at 90 °C. This was accomplished by establishing control over the Ostwald ripening process through the use of a carboxylic acid specific adsorbate. Using a variety of analytical methods, it is proposed that the carboxylate groups in the acetate precursor stabilize the {101} habit planes, creating septahedral shapes or nanopyramids. Particle assembly into crystallographically oriented dimers was observed with high specificity, and the association mechanism is suggested to relate to the crystal polarity and the variation in specific adsorption of the carboxylic acid to the surface facets. These materials are a candidate for biological labeling applications in living cells.

Ferroelectric thin films of the 0.1Pb(Ni1/3Nb2/3)O3–0.35Pb(Zn1/3Nb2/3)O3–0.15Pb (Mg1/3Nb2/3)O3–0.1PbZrO3–0.3PbTiO3 (PNN–PZN–PMN–PZ–PT) complex oxide system were prepared on Pt/Ti/SiO2/Si substrates using a polymer-modified sol-gel method followed by a rapid thermal annealing (RTA) process. It was found that the addition of excess NiO is effective in stabilizing the perovskite phase while suppressing the pyrochlore phase. The crystalline structure and morphology of the films with different amounts of access NiO were studied with x-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM), respectively. The electrical properties, including dielectric, ferroelectric, and piezoelectric, showed a significant improvement with excess NiO. The film sample with 3 mol% of excess NiO exhibited optimized electrical properties. Different parameters, including tolerance factors on the basis of ionic radii, electronegativity differences between cations and anions, and oxygen bond valences, were applied to analyze the stability of the perovskite phase with different amount of excess NiO. Analysis results indicated that only the bond-valence theory could explain the effect of excess NiO on the stability of the perovskite phase under the assumption that the excess Ni2+ entered the A sites of the perovskite structure.

High-energy synchrotron x-ray diffraction (XRD) has been used to quantify load transfer in bovine plexiform bone. By using both wide-angle and small-angle XRD, strains in the mineral as well as the collagen phase of bone were measured as a function of applied compressive stress. We suggest that a greater proportion of the load is borne by the more mineralized woven bone than the lamellar bone as the applied stress increases. With a further increase in stress, load is shed back to the lamellar regions until macroscopic failure occurs. The reported data fit well with reported mechanisms of microdamage accumulation in bovine plexiform bone.

We studied the effect of extended defects on electrical characteristics of Si doped n-type nonpolar a-plane GaN films. The n-type GaN layers were grown on co-loaded reduced defect density sidewall lateral epitaxial overgrowth (SLEO) a-plane GaN templates and high defect density planar a-plane GaN templates by metalorganic chemical vapor deposition (MOCVD). The highest conductivity value was observed at the carrier concentration of 1.05 × 1019 cm−3 as 261.12 cm2/Vs for SLEO a-GaN and 106.77 cm2/Vs for the planar a-plane GaN samples. At the same doping level, the carrier compensation for SLEO samples was ∼12% less than planar samples.

Fine grained, three-phase ceramic composites that exhibit favorable toughness, hardness, and high room-temperature strength were evaluated for high-temperature mechanical stability. A 50vol%Al2O3–25vol%NiAl2O4–25vol%3 mol%yttria-stabilized tetragonal zirconia polycrystal (3Y–TZP) and a 33vol%Al2O3–33vol%NiAl2O4–33vol%3Y-TZP composite were compression creep tested at temperatures between 1350 and 1450 °C under constant stresses of 20–45 MPa. The three-phase microstructure effectively limited grain growth (average d0 = 1.3 μm, average df = 1.6 μm after 65% true strain). True strain rates were 10−4 to 10−6 s−1 with stress exponents n = 1.7 to 1.8 and a grain-size exponent p = 1.3. A method for compensating for grain growth is presented using stress jump tests. The apparent activation energy for high-temperature deformation for 50vol%Al2O3–25vol%NiAl2O4–25vol%3Y–TZP was found to be 373 kJ/mol-K.

Compositions of xBiLaO3–(1 − x) PbTiO3 over the range 0 ≤ x ≤ 0.225 were calcined and sintered. The dielectric constant with temperature and differential scanning calorimetry measurements were in excellent agreement with respect to Curie-like tetragonal to cubic transformations starting at 495 °C for pure PbTiO3, shifting to lower temperatures with increasing x. For compositions of x ≥ 0.05, a second higher-temperature (∼600 °C) endotherm, and matching dielectric anomaly, were consistently observed, for which there were no structural changes indicated by hot-stage x-ray diffraction. This transformation was speculated to be based on a thermally induced desegregation of B-site cations.

In the present work, the damage tolerance and R-curve behavior of alumina–zirconia–niobium multiphase composites were studied by the indentation strength method. A matrix of yttria-stabilized zirconia (3Y–TZP) strengthened with particles of Al2O3 (ATZ) and an alumina matrix strengthened with particles of 3Y-TZP (ZTA) were prepared by hot press of commercial powders, containing Nb metal particles as reinforcing phase. The crack growth behavior was analyzed, and it was found that stress-induced transformation toughening of ZrO2 and bridging of the Nb inclusions were the two main factors that can shield an advancing crack and exert crack closure stresses on the crack wake. Moreover, on the basis of quantitative toughening analysis, it is argued that a synergistic effect originated from the interaction between the toughening mechanisms of Nb grains and zirconia, takes place in the alumina–zirconia–Nb multiphase composites. This showed that the combined toughening effect was bigger than the sum of the individual toughening effects when either reinforcement acted alone.

Highly porous Ti and TiZrV getter film coatings have been successfully grown on (100) silicon substrates using the glancing-angle direct-current magnetron sputtering method. The evolution of the microstructures of the Ti and the TiZrV films strongly depends on the sputtering flux rate, surface diffusion rate, nucleation rate, compositions, and self-shadowing geometry of the nuclei on the sputtering flux. The larger the glancing angle, the higher the porosity and specific surface area of the Ti and TiZrV films. The weight-gain results strongly depend on several factors, such as specific surface area, the surface structure of the getter film, the diffusion rate of O in the getter film, the reactivity of Ti, Zr, and V on O, and the order of the stabilities of Ti, Zr, and V oxides on the film’s surface. Porous Ti film absorbs oxygen better than porous TiZrV film does due to its higher surface area and the high diffusion rate of O in Ti films.