Structure Evolution of Highly Crystallized BaWO4 Film Prepared by an Electrochemical Method at Room Temperature

Highly crystallized BaWO₄ films have been prepared on a tungsten substrate in an alkaline solution containing barium ions by an electrochemical method with a constant direct current density of 1 mA/cm² at room temperature (25°C). The average grain size was about 13 μm, and the thickness about 9 μm after a treatment time of 35 min. The dependence of cell voltage on deposition time was divided into three steps: conduction, anodic oxidation, and breakdown steps. The BaWO₄ film formed during the first step. Electrochemical dissolution of metal tungsten occurred with an accompanying positive change of overpotential in the first step. The crystallization of BaWO4 was characterized by three-dimensional nucleation. In the second step, an amorphous tungsten oxide film formed, thereby increasing the potential. An electrical breakdown occurred in the third step, and the breakdown voltage (about 90 V) was practically the same as those of anodic tungsten oxide films.     

Room-Temperature Preparation of Crystallized Ba1-χSrχWO4 Solid-Solution Films by an Electrochemical Method

Films of a complete series of solid-solution oxides, Ba^1-χSr^χWO⁴ (O ≥ X ≥ 1), have been prepared on tungsten substrates in an electrolytic solution containing Ba²⁺ and Sr²⁺ ions by an electrochemical method at room temperature (25°C). The composition X could easily be controlled by the concentrations of Ba and Sr species in the starting solutions. X-ray diffraction and X-ray photoelectron spectroscopy analyses showed that a complete series of well-crystallized solid-solution oxides was formed even at room temperature.     

Preparation of Crystallized Sr1−XCaXMoO4 Solid-Solution Films by an Electrochemical Method at Room Temperature and Their Luminescence

A complete series of well-crystallized solid-solution Sr_{1– X} -Ca_XMoO₄ films has been prepared on molybdenum substrates in an electrolytic solution containing Sr²⁺ and Ca²⁺ ions by an electrochemical method at room temperature (25°C). The peak positions of excitation and emission of the Sr_1–XCa_XMoO₄ solid-solution films were independent of the Ca content: 285 ± 2 nm for excitation and 536 ± 2 nm for emission at liquid-nitrogen temperature (−196°C).     

Active Electrochemical Dissolution of Molybdenum and Application for Room-Temperature Synthesis of Crystallized Luminescent Calcium Molybdate Film

Crystallized luminescent calcium molybdate (CaMoO₄) film has been prepared on a molybdenum substrate in an alkaline solution containing calcium ions by active electrochemical dissolution of molybdenum at room temperature (25°C). The dissolution rate became faster with an increase of pH value. A high concentration of calcium (0.02M) and a high pH value (13) favored the reaction of film formation. The film showed only a single green emission at 536 nm with the excitation of 285 nm at liquid-nitrogen temperature (-196°C), strongly suggesting that it consisted of well-crystallized defect-free crystals.     

Room-Temperature KIc Values for Single-Crystal and Polycrystalline MgAl2O4

The K_lc values for (100), (110), and (111) single-crystal MgAl₂O₄ as well as those for polycrystalline MgAl₂O₄ with transgranular and intergranular fractures are presented and discussed on the basis of their elastic moduli. It is observed that the single-crystal toughnesses are directly related to the elastic modulus. Polycrystalline and single-crystal toughnesses are comparable; however, the intergranular fracture has the lowest toughness.     

电化学法制备纳米TiO2/聚邻甲苯胺复合膜

用3mol     

Preparation of ZnGa2O4 Spinel Fine Particles by the Hydrothermal Method

ZnGa₂O₄ fine particles with a single phase of spinel were synthesized from a mixed solution of gallium sulfate and zinc sulfate in the presence of aqueous ammonia under hydrothermal conditions above 180°C. The effects of treatment temperature and ZnO/Ga₂O₃ molar ratio in the starting solution on the crystallite size, morphology, lattice parameter, and chemical composition of the ZnGa₂O₄ spinel particles were examined. Spinel with different morphologies, cubic nanoparticles, and elongated rodlike particles were thought to be formed based on the structure of amorphous gallium hydroxide and needlelike GaO(OH) particles, respectively. By treatment at a higher temperature, these particles with nonstoichiometric composition grew large and thick, and their composition approached ZnO/Ga₂O₃= 1. With an increase in the starting ZnO/Ga₂O₃ molar ratio, the lattice parameter of the synthesized ZnGa₂O₄ spinel approached the reported value for the stoichiometric composition and reached a = 0.8335 nm at ZnO/Ga₂O₃= 1.95 by treatment at 240°C for 50 h.     

Synthesis of Li4SiO4 by a Modified Combustion Method

We report for the first time the synthesis of Li₄SiO₄ by the modified combustion method, a rapid chemical process that takes 5 min for completion. This method uses nonoxidizer compounds instead of nitrate mixtures, which are not always commercially available.
The effects of the following parameters on the production of Li₄SiO₄ were studied: (1) different lithium hydroxide:silicic acid:urea (LiOH:H₂SiO₃:CH₄N₂O) molar ratios; (2) the presence of air flow in the furnace chamber; and (3) the furnace heating temperature. It was found that LiOH:H₂SiO₃:CH₄N₂O molar ratios 6:1:3 heated at 1100°C in the presence of additional air in the muffle chamber formed the best precursors to produce Li₄SiO₄.     

Preparation of Li2B4O7 Films with Preferential Orientation by Sol–Gel Method

Li₂B₄O₇ films, a promising material for surface acoustic wave devices, were prepared by the sol—gel method using metal alkoxide precursors as starting materials. The Li₂B₄O₇ films on silicon (100) and (111) single crystals prepared from a coating solution to which acetic or hydrochloric acid was added were highly oriented along the (122) plane, whereas those without acid additive were randomly oriented. The results were interpreted based on the basic sol-gel chemistry and the lattice matching between the film and substrate.     

Mechanochemical Synthesis and Electrochemical Properties of LiMn2O4

Spinel LiMn₂O₄ as a cathode material for lithium secondary batteries has been synthesized by a mechanochemical process, and its electrochemical properties have been characterized. Highly disordered nanocrystalline LiMn₂O₄ powders have been prepared by the mechanochemical processing of Li₂O and MnO₂ powder mixtures for 24 h. Electrochemical characterization of mechanochemically processed powder has shown that the intercalation of Li⁺ takes place with an initial capacity of 167 mA·h/g in the 2.5–4.3 V range and has better capacity retention as compared to the well-ordered crystalline LiMn₂O₄ powders. The better capacity retention of the mechanochemically processed LiMn₂O₄ powder may be attributed to the highly disordered structure that could accommodate the Jahn–Teller distortion of the spinel structure during Li⁺ intercalation around the 3 V region.     

Preparation of BaTi4O9 from Oxalates

A barium titanate precursor with a barium:titanium ratio of 1:4 was prepared by controlled coprecipitation of mixed barium and titanium species with an ammonium oxalate aqueous solution at pH 7. The results of thermal analysis and IR measurement show that the obtained precursor is a mixture of BaC₂O₄·0.5H₂O and TiO(OH)₂·1.5H₂O in a molar ratio of 1:4. Crystallized BaTi₄O₉ was obtained by the thermal decomposition of a precipitate precursor at 1300°C for 2 h in air. The dimensions of the powder calcined at 1000°C are between 100 and 300 nm. The grain dimensions of the sintered sample for 2 h at 1300°C are of the order of 10 to 30 μm. Dielectric properties of disk-shaped sintered specimens in the microwave frequency region were measured using the TE₀₁₁ mode. Excellent microwave characteristics for BaTi₄O₉—ɛ= 38 ± 0.5, Q = 3800–4000 at 6–7 GHz and τ _f = 11 ± 0.7 ppm/°C—were found.     

Reaction-Bonding Preparation of Si3N4/MoSi2 and Si3N4/WSi2 Composites from Elemental Powders

Si₃N₄/MoSi₂ and Si₃N₄/WSi₂ composites were prepared by reaction-bonding processes using as starting materials powder mixtures of Si-Mo and Si-W, respectively. A presintering step in an At-base atmosphere was used before nitriding for the formation of MoSi₂ and WSi₂; the nitridation in a N₂-base atmosphere was followed after presintering with the total stepwise cycle of 1350°C × 20 h +1400°C × 20 h +1450°C × 2 h. The final phases obtained in the two different composites were Si₃N₄ and MoSi₂ or WSi₂; no free elemental Si and Mo or W were detected by X-ray diffraction.     

Preferred Orientation of Bi4Ti3O12 Thick Film

The preferred orientation of thick films prepared by paste printing is rarely observed because of their bulky polycrystalline nature. We found that a Bi₄Ti₃O₁₂ thick film with a thickness of ca. 20 μm showed c -axis-preferred orientation. Initially, the texture of the screen-printed film was found to have a random orientation, which was attributed to the equiaxed particle shape of the raw powder synthesized by the co-precipitation method. During subsequent heating, c -axis orientation emerged in which the degree of orientation was proportional to the film density. Analysis of the orientation distribution revealed that the progress of texturing was attributed to the film deformation, indicating that anisotropic shrinkage and morphological changes in particles during heating influenced the preferred orientation.     

Preparation and Electrical Properties of an Anodized Al2O3–BaTiO3 Composite Film

A highly stable, water-based barium titanate BaTiO₃, BT, sol was synthesized using a sol–gel route through a chelate lactate technique. Dried BT precursor powders were measured by thermal gravimetry–differential thermal analysis and X-ray diffraction. It was found that BT powders first converted into barium carbonate BaCO₃, Ti complex, and intermediate phase Ba₂Ti₂O₅CO₃, and then transformed into perovskite phase BaTiO₃. The crystallization temperature was about 550°C. The low-voltage etched aluminum foils were covered with BT sol by dip coating, and then annealed at 600°C for 30 min in air. After that, the samples were anodized in a 15 wt% aqueous solution of ammonium adipate. The voltage–time variations during anodizing were monitored, and the electrical properties of the anodic oxide film were examined. It was shown that the specific capacitance, the product of specific capacitance and withstanding voltage, and leakage current of samples with a BT coating were about 48.93%, 38.50%, and 167% larger than that without a BT coating, respectively.     

Preparation and Process Chemistry of SnO2 Films Derived from SnC2O4 by the Aqueous Sol–Gel Method

Nanocrystalline SnO₂ films were prepared from SnC₂O₄ by a sol–gel route. A clarified and stable Sn-containing sol was obtained by dissolving and chelating SnC₂O₄ with C₆H₈O₇ and H₂C₂O₄ in a C₆H₈O₇/triethanolamine (TEA) mixing aqueous solution with a pH of 6.5–7.0. The chelation and condensation reactions were deducted based upon infrared, Raman, and X-ray photoelectron spectra analysis. Results illuminated that a number of ionized-state carboxyl groups and active tin hydrate were produced in the mixing solution by amido association of TEA with H on –COOH of H₃L and H₂C₂O₄, supplying a precondition for tin sol formation. X-ray diffraction and field emission scanning electron microscope analysis indicated that SnO₂ film had a rutile structure and consisted of nanocrystals with a mean size of about 7 nm. Film thickness could be controlled by the number of dip coating—annealing cycles according to 30–45 nm/cycle for a Sn concentration of 0.25 mol/L.     

Preparation of NiAl2O4/SiO2 and Co2+-Doped NiAl2O4/SiO2 Nanocomposites by the Sol–Gel Route

NiAl₂O₄/SiO₂ and Co²⁺-doped NiAl₂O₄/SiO₂ nanocomposite materials of compositions 5% NiO – 6% Al₂O₃– 89% SiO₂ and 0.2% CoO – 4.8% NiO – 6% Al₂O₃– 89% SiO₂, respectively, were prepared by a sol–gel process. NiAl₂O₄ and cobalt-doped NiAl₂O₄ nanocrystals were grown in a SiO₂ amorphous matrix at around 1073 K by heating the dried gels from 333 to 1173 K at the rate of 1 K/min. The formations of NiAl₂O₄ and cobalt-doped NiAl₂O₄ nanocrystals in SiO₂ amorphous matrix were confirmed through X-ray powder diffraction, Fourier transform infrared spectroscopy, differential scanning calorimeter, transmission electron microscopy (TEM), and optical absorption spectroscopy techniques. The TEM images revealed the uniform distribution of NiAl₂O₄ and cobalt-doped NiAl₂O₄ nanocrystals in the amorphous SiO₂ matrix and the size was found to be ∼5–8 nm.     

Low-Temperature Synthesis of NiFe2O4 by a Hydrothermal Method

Nickel ferrite (NiFe₂O₄) nanoparticles were successfully synthesized via a hydrothermal process and characterized by X-ray diffraction and transmission electron microscope techniques. The effects of reaction temperature, holding time, and RH ratio (isopropyl alcohol/water) were discussed. The NiFe₂O₄ nanoparticles could be obtained at 60°C within 3 h. The crystallization of the spinel ferrites was promoted by the increase in reaction temperature, holding time, and RH ratio.     

Low-Temperature Synthesis of Fully Crystallized Spherical BaTiO3 Particles by the Gel–Sol Method

The synthesis of spherical BaTiO₃ particles was attempted by a new technique, the "gel–sol method," at 45°C. The (Ba–Ti) gel used as a starting material was prepared by aging mixtures of titanyl acylate with a barium acetate aqueous solution ([glacial acetic acid (AcOH)]/[titanium isopropoxide (TIP)] = 4, [barium acetate]/[TIP] = 1) at 45°C for 48 h. Potassium hydroxide (KOH) was used as a catalyst for the formation of BaTiO₃. Powder X-ray diffractometry (XRD) results and Fourier-transform infrared (FT-IR) measurements for the (Ba–Ti) gel showed that the gel was amorphous, but the spatial arrangement of barium and titanium in the (Ba–Ti) gel is similar to that in crystalline BaTiO₃ particles. Fully crystallized spherical BaTiO₃ powder with a particle size of 40–250 nm formed at the very low reaction temperature of 45°C. Scanning electron microscopy images showed that the final particles formed via aggregation of the fine particles that seem to be the primary particles of bulk (Ba–Ti) gel. From the XRD, FT-IR, and Raman spectroscopy analysis, it was found that the crystal structure of the as-prepared particles continuously transformed from cubic to tetragonal as the calcination temperature increased, and high crystalline tetragonal BaTiO₃ phase was obtained at 1000°C after 1 h of heat treatment.     

Room-Temperature Conducting LaNiO3 Thick-Film Coatings Prepared by Aerosol Deposition

Metallic conductive LaNiO₃ thick films with a thickness of 0.5–10 μm were fabricated by a room-temperature-operating powder deposition process—aerosol deposition method. The coated LaNiO₃ layers were fairly dense without pores or cracks, and maintained their phase stability due to low-temperature consolidation. The as-deposited LaNiO₃ film consisted of ∼10-nm-diameter grains, with a sheet resistance of 10–100 Ω/□, while the post-annealed LaNiO₃ film had a sheet resistance of 4.45 Ω/□, which is the lowest value ever reported for an LaNiO₃ film. This excellent conductivity result was attributed to the high crystal stability and dense microstructure.