We describe a vapor-phase route to the controllable synthesis of indium oxide micro-and nanopyramids on the silicon wafer via selective epitaxial vapor-solid growth by a methane-assist thermal reduction method. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy revealed that the pyramids were cubic single crystals with a tetragonal symmetry. The size, morphology, and density of pyramids could easily be controlled by tuning reaction parameters. The method has good compatibility with other procedures involved in the microfabrication processes. Laterally grown indium oxide nanorods on the silicon wafer were also prepared via a vapor-liquid-solid mechanism. Those crystalline In2O3 nanorods were about 100 nm in diameter and 1 μm in length. The as-synthesized indium oxide nanopyramids and nanorods could offer novel opportunities for both fundamental research and technological applications.

This article describes both electrochemical deposition and electrophoretic deposition of high-density tellurium (Te) nanowire arrays with wire diameters of 60 nm and lengths of 15–20 μm in the nanochannels of anodic aluminum oxide (AAO) templates. The Te nanowires synthesized via electrochemical deposition (ECD) are generally single crystalline in nature with the wire longitudinal axis along the [001] direction, whereas those synthesized via electrophoretic deposition (EPD) show polycrystalline structures with numerous tiny Te crystallites packed randomly in the wires. The single-crystalline Te nanowires produced by the ECD route are believed to form under a near chemical equilibrium condition; however, the imposed transport and the rapid packing of Te nanocrystallites in the nanochannels of AAO template in external fields lead to polycrystalline Te nanowires in the EPD process. This comparative study of the Te nanowire formation in the nanochannels of AAO template will facilitate the tailoring of the growth of other inorganic nanowires of high quality.

Ferroelectric domain configurations in silver- and lanthanum-doped lead zirconate titanate (PZT) ceramics were characterized by scanning force microscopy using contact as well as piezoelectric response force [i.e., piezoelectric force microscopy (PFM)] modes. Coarse crystallites of hard and soft PZT ceramics (12 μm in Ag-PZT and 30 μm in La-PZT average grain size, respectively) with surface oriented in the {001} planes were chosen to characterize the domain configuration. Results show the conventional right-angled domain structures, which correspond to the {110} twin-related 90° and 180° domains of homogeneous width from 50 to 150 nm. The ability of PFM to image the orientation of pure in-plane arrays of domains (containing 90°-aa- and 180°-aa-types of domain boundaries) is highlighted, and a more detailed notation for in-plane domains is proposed. In addition to such periodical domain arrays, other ordered domains were found, having a misfit of 26° with respect to the{110} domain walls and the {100} surface. This array of domain walls could not be predicted with a geometrical analysis of the intersection of domain walls at the surface according to the conventional spatial array of {110} crystallographic planes. It could be explained only with {210} planes being the domain walls. The reason for this unconventional domain configuration is explained with the clamped conditions of the investigated crystallites in the polycrystalline material.

Sol-gel materials of TiO2 and vanadium-modified TiO2 of nominal composition 4, 8, and 16 wt.% vanadium were prepared by evaporation of aqueous colloidal sols obtained by the hydrolysis of aqueous solutions of titanium(IV) chloride with the appropriate amount of vanadyl oxalate using aqueous ammonia followed by peptization of the resulting hydrated solids using nitric acid. The nature of the sol-gel materials and their behavior on calcinations at temperatures up to 1273 K were investigated using x-ray fluorescence, powder x-ray diffraction, transmission electron microscopy, and electron diffraction and FT-Raman spectroscopy. At 333 K, all the gels comprised small (about 5 ± 1 nm) particles of anatase together with traces of brookite. The particle size changed little on thermal treatment at 573 K, but increased significantly at higher temperatures and was accompanied by transformation to rutile. Incorporation of vanadium in the gels reduced the temperature at which rutile began to appear from 923 K in pure TiO2 to 773 K in the V/TiO2 gels. Only rutile was present at high temperatures, except for the 16 V/TiO2 gel, when small amounts of phase-separated vanadia were also observed. A 2–3% substitutional incorporation of V4+ ions in the tetragonal rutile lattice occurred at high temperatures, but the majority of the vanadium was present in an amorphous, highly dispersed fashion.

The thermal endurance of poly(butylene terephthalate) was evaluated by both consolidated long-term conventional life tests and a short-term analytical procedure. The latter is based on oxidative stability measurements by isothermal differential calorimetry in a pure oxygen flow. The capability of the analytical technique to provide an activation energy for the thermo-oxidation process was verified. The results obtained by the two methods were compared and discussed. It is shown that the temperature index derived by the analytical procedure can be close to that obtained by the conventional tests, provided that a suitable selection of the test temperatures and failure criteria is made; however, benefits in term of test time shortening are lower than those previously obtained for polyolefin-based materials.

In this work, we report on the observation of Nd1Ba6Cu3O10,5 (Nd163) phase of the NdBaCuO system in melt-textured Nd123 bulk samples grown from a mixture of Nd123 and Nd210 phase powders. The observation was performed with polarized light optical microscopy and scanning electron microscopy–energy dispersive x-ray analyses. Images of the identified phase crystals show an aspect quite different from Nd422 crystals. Unexpectedly, Nd163 was individuated, even in “pure” Nd123 samples. Moreover, after long exposure to air, Nd163 disappeared completely in samples synthesized from powders containing Nd210. Thermogravimetry analyses of powders show that the stability of this phase in air is limited to temperatures higher than 900 °C, so Nd163 is unstable and highly reactive at room temperature. Moreover, an explanation of the observation of Nd163 in Nd210 free samples, based on the spontaneous formation of Nd163 phase in a Nd123 melt, is proposed.

NiO-yttria-stabilized zirconia powder mixtures were prepared from reactive citrate-nitrate gels using the combustion technique. The influence of the fuel/oxidant molar ratio in the precursor on the combustion rate and its thermal characteristics was studied by thermal analysis and evolved gas analysis. It was found that the precursor thermal decomposition properties depended strongly on the citrate/nitrate ratio prior to the combustion. Intermediate precursors and final powder ashes were also analyzed by x-ray diffraction.

In this paper, we present results obtained from a comparison study relating to the deposition of diamond films using two processes, namely, time-modulated chemical vapor deposition (TMCVD) and conventional CVD. Polycrystalline diamond films were deposited onto silicon substrates using both hot-filament CVD and microwave plasma CVD systems. The key feature of TMCVD is that it modulates methane (CH4) flow during diamond CVD, whereas in conventional CVD the CH4 flow is kept constant throughout the deposition process. Films grown using TMCVD were smoother, harder, and displayed better quality than similar films grown using constant CH4 flow during CVD. The advantage of using TMCVD is that it promotes secondary nucleation to occur on existing diamond crystals. Pulsing CH4, consecutively, at high and low concentrations allows the depositing film to maintain its quality in terms of diamond-carbon phase. Films grown under constant CH4 flow during diamond CVD displayed a columnar growth mode, whereas with the time modulated films the growth mode was different. The mechanism of film growth during TMCVD is presented in this paper. The growth rate of films obtained using the hot filament CVD system with constant CH4 flow was higher than the growth rate of time modulated films. However, using the microwave-plasma CVD system, the effect was the contrary and the time-modulated films were grown at a higher rate. The growth rate results are discussed in terms of substrate temperature changes during TMCVD.

An organic–inorganic, hybrid, low-melting glass free of pollution elements such as Pb and F was prepared through nonaqueous acid-base reactions of Si—Cl + P—OH ⇉ Si—O—P + HCl⇈ and Sn—Cl + P—OH ⇉ Sn—O—P + HCl⇈ using phosphonic acid (H3PO3), dimethyldichlorosilane (Me2SiCl2), and tin(II)chloride (SnCl2) as starting materials. Transparent, colorless, and homogeneous phosphite glass was successfully obtained. The formation of P—O—Si linkage and the disappearance of P—OH were confirmed by 31P nuclear magnetic resonance spectra. With increasing Si content, the glass-transition temperature decreased, reflecting the decrease of the average linkage number per one cation.

Ribbon and bulk nanocrystalline body-centered-cubic (bcc) (Fe,Co) alloys exhibiting good soft magnetic properties were synthesized in Fe71.5-xCoxB13.5Si10Nb4Cu1 system by the simple production processes of melt-spinning or casting and annealing. The glass-type alloys were formed in the Co content range below 30 at.%. These glassy alloys crystallized through two exothermic reactions. The first stage was due to the precipitation of nanoscale bcc-(Fe,Co) phase with a grain size of about 10 nm, and the second stage resulted from the decomposition of the remaining amorphous phase to α–(Fe,Co), (Fe,Co)2B, (Fe,Co)23B6, (Fe,Co)3Si, and (Fe,Co)2Nb phases. The glass transition temperature increased from 820 to 827 K with increasing Co content from 5 to 20 at.%, while the supercooled liquid region decreased slightly from 37 to 30 K because of the nearly constant crystallization temperature. By choosing the 10 at.% Co-containing alloy, we produced cylindrical glassy alloy rods 1.0 and 1.5 mm in diameter by copper mold casting. The subsequent annealing for 300 s at 883 K corresponding to the temperature just above the first exothermic peak caused the formation of nanoscale bcc-(Fe,Co) structure. The bcc-(Fe,Co) alloy rods exhibited good soft magnetic properties of 1.26 T for saturation magnetization and 5.0 A/m for coercive force, which were comparable to those for the corresponding bcc-(Fe,Co) alloy ribbon. The nanocrystalline alloy in a bulk form is encouraging for future use as a new type of soft magnetic material that requires three-dimensional shapes.

Thermal oxide covered silicon wafers were polished with slurries containing (i) only nano-sized particles of ceria, monodispersed colloidal spherical silica, or hematite of different shapes, (ii) a binary mixture of the same nano-sized and uniform colloidal particles, and (iii) the same colloids coated with nano-sized ceria. The procedures for the preparation of the coated particles are described in this article. The polish rates and surface qualities were in all cases higher with mixed slurries, and even more so with coated particles. The performance of composite systems also depended on the shape of the particles, cubic ones being the most and spheres least efficient. Experimental results indicated that ceria in mixtures was responsible for the enhanced polish process, while core materials enhanced a closer contact of nano-sized particles with the wafer. In general, the polish rates were higher with the larger contact area between the abrasives and the wafer. This mechanism was further verified by polishing oxide wafers on 3-M fixed abrasive pads, which have cylindrical structures with flat surfaces.

Ti-peroxy compound was synthesized from Ti(O-iPr)4 and H2O2. Anatase and rutile TiO2 nanoparticles were prepared by heating the Ti-peroxy compound diluted with a polyol aqueous solution at 368 K for 24 h. In this research, ethylene glycol, glycerin, erythritol, and D-mannitol were used as polyols in the diluting solution. The ratio of anatase/rutile of the TiO2 obtained depended on the polyol concentration in the diluting solution. Furthermore, the polyol concentration at which single-phase anatase could be obtained was lowest when the number of OH groups in the polyol molecule was the highest. With increasing polyol concentration, the obtained TiO2 nanoparticles showed increasing specific surface area and decreasing particle size.

H2 reduction and densification of extruded Fe2O3–Cr2O3 mixtures with honeycomb geometry (0.3-mm wall thickness) were studied using dilatometry, x-ray diffraction, and scanning electron microscopy. Reduction of pure Fe2O3 heated at 5 °C/min was completed by approximately 525 °C. Two separate sintering steps ensued, well separated in temperature from reduction, one associated with elimination of pores between Fe agglomerates (750–900 °C), and the other associated with sintering of these agglomerates (995–1275 °C). With increasing Cr2O3 content, sintering was increasingly delayed until initiation of Cr2O3 reduction above 1000 °C. The α → γ iron phase transformations were consistent with the Fe–Cr phase diagram, but the γ → α transformations at higher temperatures deviated from the phase diagram because of the influence of impurities (Si, Ca) in the solid solution. Pure Cr2O3 honeycomb formed an approximately 35-μm-thick porous Cr coating that imposed a diffusion barrier to further reduction. The high vapor pressure of chromium prohibited compositions in excess of 25 wt.% Cr2O3 from full reduction and densification.

A single LaMnO3 buffer layer was developed for the growth of superconducting thick YBa2Cu3O7−δ (YBCO) films on polycrystalline Ni-alloy substrates where a biaxially textured MgO layer, produced by ion-beam assisted deposition (IBAD), was used as a template. Using pulsed laser deposition, a 1.65-μm-thick YBCO film with a critical current density of 1.4 × 106 A/cm2 in self field at 75 K was achieved on sputtered LaMnO3-buffered IBAD MgO substrates. This corresponds to a critical current (Ic) of 231 A/cm-width. This result demonstrates the possibility of using both LaMnO3 buffer and IBAD MgO template for producing high current density YBCO-coated conductors.

Uniformly distributed nanoparticles created by heating carbon nanotubes synthesized by arc-discharge were studied by electron diffraction, high-resolution transmission electron microscopy (HRTEM), electron energy loss spectroscopy (EELS), and x-ray energy dispersive spectrometer (EDS). The nanoparticles have diameters in the range of 3–15 nm. Electron diffraction pattern and HRTEM images analysis both show that the nanoparticles can be nickel or diamond. EELS and EDS analysis in a dedicated scanning transmission electron microscope showed that the nanoparticles are face-centered-cubic nickel particles rather than diamond nanocrystals. The mechanism of formation of nickel nanoparticles below its melting point is discussed.

Diamondlike carbon (DLC) films were electrodeposited on nickel substrates from a solution of acetylene in liquid ammonia at low temperature and low potential using a three-electrode cell. Raman spectra showed a shoulder D peak at 1365 cm−1 and a broad G peak at 1558 cm−1 for the films, indicating an sp3 and sp2 carbon mixture. The presence of a 1230 cm−1 peak also indicated some four-fold-coordinated bonds of microcrystalline diamond. Fitting of the peaks in the Raman spectra specified the electrodeposited films were hydrogenated amorphous alloys, a-C:H. X-ray photoelectron spectra also pointed to the films containing a mixture of sp3 and sp2 carbon. Fourier transform infrared spectra of the electrodeposited films had C-H stretching vibrations, which is consistent with hydrogenated DLC films.

We report an effective procedure for fabricating carbon microcoils and nanocoils with three-dimensional spiral structures in high yield by nickel (Ni)-catalyzed thermal decomposition of acetylene. The Ni catalyst particles used in this preparation were electrochemically deposited onto tungsten substrates. Springlike coils having low pitch and micrometer-scale diameters and ropelike coils having higher pitch and nanometer-scale diameters were observed. Electrical and optical properties were investigated by employing a field-emission probe system equipped with an optical spectrometer. In an applied field above 1.5 V/μm, significant electron emission was observed from individual ropelike nanocoils. The approximately linear slope of the corresponding Fowler-Nordheim plot denotes predominately field-emission behavior. During measurement, individual carbon coils aligned themselves along the electric field, exhibiting a natural resonance on some occasions. As the field strength increased above 2.5 V/μm, the emission-current density for a single nanocoil was measured to be on the order of 104 A/cm2. This high-current density caused Joule heating, resulting in strong photon emission by incandescence.

Polycrystalline diamond films, single crystal bulk diamonds, and diamond powder were treated in microwave plasma of hydrogen at 1.6 torr under a negative direct-current bias of −150 to −300 V without metal catalyst. It was found that fibrous structures, uniformly elongated along the direction normal to the specimen surface, were formed on the diamond surfaces. Similar experiments for glasslike carbon resulted in conical structures with frizzy fibers at the tops. Transmission electron microscopy measurements indicated that the fibers formed on diamond consisted of randomly oriented diamond nanocrystals with diameters of less than 10 nm, while the conical structures formed on glasslike carbon consisted of graphite nanocrystals. Field emission measurements of the fibrous specimens exhibited better emission efficiency than untreated ones. The field emission electron microscopy of the fibrous glasslike carbon showed a presence of discrete electron emission sites at a density of approximately 10,000 sites/cm2.

The effect of TiB2 on the densification behavior and properties of microwave-sintered AlN/TiB2 ceramic was investigated. The densification of the composite was significantly retarded in nitrogen atmosphere due to strong nitridation of TiB2 compared to sintering in argon atmosphere. The densities of the AlN/TiB2 composites containing different amounts of TiB2 all reached 99% of the theoretical density during 2 h of sintering at 1850 and 1900 °C. Microstructure analysis revealed that the TiB2 particles were dispersed in the AlN matrix while AlN grains retained its contiguity. This microstructure led to a composite with superior properties; thermal conductivity as high as 149 W/(m K) was achieved. The microwave sintered composites are harder and tougher than pure AlN. Microwave-sintered AlN/TiB2 composite is a promising material for structural applications in which high thermal conductivity and controlled dielectric loss are important.

We used the Clusters model to study the densification kinetics and resulting porosity of a compact of polydispersed soda-;lime-;silica glass spheres. In addition to the physical data (viscosity, surface tension, particle size distribution) required by the Clusters model, for the first time in glass-;sintering studies, we took extra variables into account: the average number of necks per sphere, the effects of pre-;existing crystals on the particle surfaces, and sample size. The model predicted both the densification kinetics and the resulting pore-;size distribution of sintered compacts. A cross section of a porous sample displayed a porosity pattern that agreed with computer-;simulated cross sections, whose pore-;size distributions was calculated via the Clusters model using a Monte Carlo technique. Its capacity to predict both density and pore-;size distribution makes the Clusters model a valuable tool for designing sintered glasses with any desired microstructure.