Preparation of titania microballoons by sol-gel process in reverse dispersion

Titania microballoons were prepared by sol-gel process of titanium tetra-2-propoxide in reverse dispersion. Hexane was used as continuous phase, in which sorbitan monooleate was dissolved as dispersion stabilizer. A buffer solution was used as dispersed phase, of which pH was adjusted from 5.0 to 7.0. These phases were mixed and stirred to prepare reverse dispersion. Titanium tetra-2-propoxide was added to the dispersion to start reaction, and stirring was kept for 24 h at 30 °C. The crystalline phase of specimens calcined at 500 °C was identified as anatase. Scanning electron microscopy showed that the products were hollow microspheres or microballoons. The effects of preparation duration, dispersion stabilizer concentration, and pH on the yield and the mean diameter were investigated.     

Machinable Al2O3/BN composite ceramics with strong mechanical properties

Al₂O₃/BN composite ceramics with nano-sized BN dispersions ranging from 0 to 30 vol.% were successfully fabricated by hot-pressing α-Al₂O₃ powders with turbostratic BN (t-BN) coating, which was prepared through chemical processes using boric acid and urea. SEM observations revealed that the nano-sized hexagonal BN (h-BN) particulates were homogeneously dispersed within Al₂O₃ grains as well as at grain boundaries. Vickers hardness of materials decreased with an increase in BN content. The fracture toughness was improved but the fracture strength had a small decrease, in comparison to Al₂O₃ monolithic ceramics. The nanocomposite ceramics with BN content more than 20 vol.% exhibited excellent machinability, which could be drilled using conventional hard metal alloy drills. Drilling rates and normal forces demonstrate the ease of machining of these materials. The preliminary information on the relationship between microstructures and properties are provided. The mechanism of material removal is also discussed.     

Synthesis, characterization, and dielectric properties of Ba(Ti1−xSnx)O3 nanopowders and ceramics

We prepared Ba(Ti_1−xSn_x)O₃ powders and ceramics by means of the sol-gel process, with dibutyltin dilaurate as the Sn precursor. The samples were characterized by means of Fourier-transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and scanning electron microscopy, and also determined the dielectric properties of the ceramics. The powders synthesized by means of the sol-gel process had a grain size on the nanometer scale, with the grains mainly composed of a cubic BaTiO₃ phase. Sn can disperse into BaTiO₃ more uniformly in the sol-gel technique using dibutyltin dilaurate as the Sn precursor. With increasing Sn concentration, the grain size of the Ba(Ti_1-xSn_x)O₃ ceramics increased and the maximum dielectric constant (?_max) first increased and then decreased. At a Sn concentration of 5 mol%, ?_max reached its maximum value (19,235).     

The microwave effect on the properties of silica-coated TiO2 fine particles prepared using sol-gel method

The silica coating of TiO₂ fine particle was conducted using microwave assisted sol-gel method and conventional sol-gel method to suppress its photo-catalytic activity. The amount and uniformity of silica coating on TiO₂ surface were characterized by X-ray photoelectron spectroscopy (XPS), X-ray fluorescence spectroscopy (XRF), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and zeta potential measurements. XPS and XRF results showed that the presence of catalyst and reaction time were important factors to reach high silica amounts. SEM, TEM, and zeta potential results indicated that dense film coating of SiO₂ layer formed on TiO₂ surface in conventional sol-gel method, whereas the nucleation coating was observed on sample prepared by microwave assisted sol-gel method. When photo-catalytic activities and ultraviolet (UV) shielding abilities of these samples were evaluated, the sample prepared by microwave processing showed higher inhibition of photo-catalytic activity and better UV shielding ability than the sample prepared by conventional method. These results suggested that the coating method significantly affected the photo-catalytic activity and UV shielding ability of coated TiO₂.     

Microstructures and mechanical properties of silicon nitride bonded silicon carbide ceramic foams

Silicon nitride bonded silicon carbide foams have been produced by nitridation of the foamed compacts containing silicon carbide and silicon powders. When no nitridation additive was used the ceramic foams nitrided at all temperatures studied contained a significant amount of whisker phase α-Si₃N₄ formed both inside and outside the cell walls leading to a loose microstructure and a low mechanical strength. When the Al₂O₃ and Y₂O₃ were used as nitridation additives, the ceramic foams nitrided at temperatures of 1360 and 1395 °C containing certain amount of Si₂N₂O and whisker α-Si₃N₄ phases that are bonded by a glassy phase and behave as reinforcements for the ceramic foams exhibited a much higher mechanical strength. At nitridation temperature of 1430 °C, the ceramic foam showed the locally formed β-Si₃N₄ as the main nitrided phase that caused no increase in bonding area between the nitrided phase and the silicon carbide particles. Thus, a relatively lower mechanical strength was observed for the ceramic foam.     

Organic acids on the fabrication of sol-gel lead zirconate titanate fibers

Lead zirconate titanate (PZT, 53/47) fibers are prepared by sol-gel method using organic acids - acrylic and methacrylic acid - to modify the precursors. The macroscopic properties, molecular structure, crystallization behaviour and microstructure of the fibers are investigated as a function of the content and type of acid. Organic acids produce long gel and ceramic fibers, due to the beneficial effect of the long polymeric chains that are generated in the precursor gel. However the longest, strongest, densest and with the highest homogeneity fibers are obtained when acrylic acid is used. The linear shape of the molecular structure of acrylic acid, together with a lower content of organic species to be released, is favourable to the preparation of round and crack free PZT fibers, when acrylic acid is used.     

Synthesis and microwave dielectric properties of CaO-MgO-SiO2 submicron powders doped with Li2O-Bi2O3 by sol-gel method

Using Ca(NO₃)₂·4H₂O, Mg(NO₃)₂·6H₂O, Si(OC₂H₅)₄, LiNO₃ and Bi(NO₃)₃·5H₂O as raw materials, CaO-MgO-SiO₂ submicron powders were prepared at low temperature by sol-gel method. The crystallization temperature was decreased enormously by the introduction of Li-Bi liquid phase sintering aids into Ca-Mg-Si sol, and the powders with average particle sizes of 80-100 nm and 200-400 nm were obtained at the calcining temperature of 750 °C and 800 °C, respectively. The sintering characteristic and dielectric properties of powders calcined at 750 °C with different content of powders calcined at 800 °C were studied. When the content of powders calcined at 800 °C was 10 wt%, the dielectric ceramic sintered at 890 °C had compact structure, and possessed excellent microwave dielectric properties: ?_r = 7.16, Q × f = 25630 GHz, τ_f = −69.26 ppm/°C.     

Improved properties of GRC composites using commercial E-glass fibers with new coatings

A study was carried out to evaluate the action of a new 15CaO-15BaO-20SiO₂-50TiO₂ coat on long-term durability of glass fiber reinforced cement. Compressive strength, flexural strength and drying shrinkage were measured. Significant improvement was observed and four reasons were given to explain it. The results testify further the effectiveness of the alkali resistance of the new coat.     

Third-order nonlinear optical properties of Bi2S3 nanocrystals doped in sodium borosilicate glass studied with Z-scan technique

The third-order nonlinear optical properties of Bi₂S₃ nanocrystals doped in sodium borosilicate glass are measured by Z-scan technique. The microstructures of the glass are characterized by means of X-ray diffraction, transmission electron microscopy, scanning transmission electron microscopy, energy dispersion X-ray spectra, and high-resolution transmission electron microscopy. The results show that the Bi₂S₃ nanocrystals ranging from 10 to 30 nm are determined to be of the orthorhombic crystalline phase, and the third-order optical nonlinear refractive index γ, absorption coefficient β, and susceptibility χ⁽³⁾ of the glass are determined to be 2.56 × 10⁻¹⁶ m² W⁻¹, 4.13 × 10⁻¹⁰ mW⁻¹, and 1.43 × 10⁻¹⁰ esu, respectively.     

Structural properties of Al2O3-La2O3 binary oxides prepared by sol-gel

The structural properties of La₂O₃ and Al₂O₃-La₂O₃ binary oxides prepared by sol-gel were studied by XRD, HRTEM and UV-vis. The binary oxides with high lanthana contents show an amorphous structure after calcination at 650 °C. At calcination temperatures higher than 1000 °C there is a phase transformation from the amorphous state to the crystalline LaAlO₃ with a perovskite structure. The structure of La₂O₃ is consistent with the hexagonal system; however, some crystalline microdomains with a monoclinic structure were detected by HRTEM. Islands of La₂O₃ and LaAl₁₁O₁₈ phases were detected at high lanthana concentration in the binary oxide. The modification in the coordination shell of the Al³⁺ cations due to the interaction with La³⁺ cations confirms the formation of phases with a perovskite structure and the presence of islands of the LaAl₁₁O₁₈ phase.     

Luminescent properties of Gd2Ti2O7: Eu phosphor films prepared by sol-gel process

Gd₂Ti₂O₇: Eu³⁺ thin film phosphors were fabricated by a sol-gel process. X-ray diffraction (XRD), atomic force microscopy (AFM) and photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 800 °C and the crystallinity increased with the elevation of annealing temperatures. Uniform and crack free phosphor films were obtained, which mainly consisted of grains with an average size of 70 nm. The doped Eu³⁺ showed orange-red emission in crystalline Gd₂Ti₂O₇ phosphor films due to an energy transfer from Gd₂Ti₂O₇ host to them. Both the lifetimes and PL intensity of the Eu³⁺ increased with increasing the annealing temperature from 800 to 1000 °C, and the optimum concentrations for Eu³⁺ were determined to be 9 at.%. of Gd³⁺ in Gd₂Ti₂O₇ film host.     

Preparation of silica-sustained electrospun polyvinylpyrrolidone fibers with uniform mesopores via oxidative removal of template molecules by H2O2 treatment

Silica-sustained electrospun PVP fibers with uniform mesopores were synthesized via facile oxidative removal of template molecules by H₂O₂ extraction. Tetraethyl orthosilicate, polyvinylpyrrolidone (PVP), and triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) copolymer pluronic P₁₂₃ compose the electrospinning sol to fabricate the silica-sustained PVP hybrid fibers. The effect of different post-treatment methods on the pore size distribution was investigated by calcination and extraction, respectively. Experimental results showed that oxidative removal of structure-directing agent P₁₂₃ in the hybrid fibers by H₂O₂ treatment can easily form narrow pore size distribution, and the incorporation of 3D silica skeleton built by hot steam aging facilitated preserving the original cylindrical morphology of fibers. Scanning electron microscopy (SEM), N₂ adsorption-desorption isotherm, transmission electron microscopy (TEM), X-ray diffraction (XRD), FT-IR spectra and thermogravimetric analysis (TGA) were used to characterize the hybrid fibers. The hybrid fibers can be expected to have potential applications in drug release or tissue engineering because of their suitable pore size, large surface area and good biocompatibility.     

Rapid synthesis, characterization and optical properties of TiO2 coated ZnO nanocomposite particles by a novel microwave irradiation method

A novel and rapid microwave method was used to prepare TiO₂ coated ZnO nanocomposite particles. The resulted particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Results show that ZnO nanoparticles were coated with 6-10 nm amorphous TiO₂ layers. In addition, zeta potential analysis demonstrated the presence of TiO₂ layer on the surface of ZnO nanoparticles. Photoluminescence (PL) spectroscopy and UV-visible spectroscopy were used to investigate the optical properties of the nanoparticles. Compared to uncoated ZnO nanoparticles, the TiO₂ coated ZnO nanoparticles showed enhanced UV emission. The UV-visible diffuse reflectance study revealed the significant UV shielding characteristics of the nanocomposite particles. Moreover, amorphous TiO₂ coating effectively reduced the photocatalytic activity of ZnO nanoparticles as evidenced by the photodegradation of Orange G with uncoated and TiO₂ coated ZnO nanoparticles under UV radiation.     

Structural and chemical characterization of BaTiO3 nanorods

An electron-microscopy investigation was performed on BaTiO₃ nanorods that were processed by sol-gel electrophoretic deposition (EPD) into anodic aluminium oxide (AAO) membranes. The BaTiO₃ nanorods grown within the template membranes had diameters ranging from 150 to 200 nm, with an average length of 10-50 μm. By using various electron-microscopy techniques we showed that the processed BaTiO₃ nanorods were homogeneous in their chemical composition. The BaTiO₃ nanorods were always polycrystalline and were composed of well-crystallized, defect-free, pseudo-cubic BaTiO₃ grains, ranging from 10 to 30 nm. No intergranular phases were observed between the BaTiO₃ grains. A low-temperature hexagonal polymorph that is coherently intergrown with the BaTiO₃ perovskite matrix was also observed as a minor phase. When annealing the AAO templates containing the BaTiO₃ sol in an oxygen atmosphere the presence of the hexagonal polymorph was diminished.     

Influence of calcination ambient and film thickness on the optical and structural properties of sol-gel TiO2 thin films

Influence of both calcination ambient and film thickness on the optical and structural properties of sol-gel derived TiO₂ thin films have been studied. X-ray diffraction results show that prepared films are in an anatase form of TiO₂. Films calcined in argon or in low vacuum (∼2 × 10⁻¹ mbar) are found to be smaller in crystallite size, more transparent at low wavelength region of ∼300-450 nm, denser, have higher refractive index and band gap energy compared to air-calcined films. Scanning electron microscopic study reveals that surfaces of TiO₂ films calcined in argon or in low vacuum are formed by densely packed nano-sized particulates. Presence of voids and signs of agglomeration can be seen clearly in the surface microstructure of air-calcined films. In the thickness range ∼200-300 nm, band gap energy and crystallite size of TiO₂ films remain practically unaffected with film thickness but refractive index of thinner film is found to be marginally higher than that of thicker film. In this work, it has been shown that apart from temperature and soaking time, partial pressure of oxygen of the ambient is also an important parameter by which crystallite size, microstructure and optical properties of the TiO₂ films may be tailored during calcination period.     

Characterization and photocatalytic activity of Bi3TiNbO9 nanocrystallines synthesized by sol-gel process

Nanocrystalline Bi₃TiNbO₉ powders were synthesized by a sol-gel process, based on a colloid solution of bismuth acetate, titanium butoxide and niobium ethoxide. X-ray diffraction analysis revealed that pure Aurivillius phase of Bi₃TiNbO₉ could be prepared at a calcination temperature of 500 °C. By using scanning electron microscopy and gas adsorption method, the morphology and the specific surface area of the powders were examined. The photophysical properties of Bi₃TiNbO₉ were investigated by means of the UV-visible diffuse reflectance spectrum, from which a band gap ∼3.2 eV was empirically calculated. The as-prepared Bi₃TiNbO₉ powders were applied in the photodegradation of organic contaminant for the first time, and they showed effective photocatalytic activity for the complete decomposition of methyl orange under UV light irradiation.     

PLA/algae composites: Morphology and mechanical properties

Bio-composites with poly(lactic) acid as matrix and various algae (red, brown and green) as filler were prepared via melt mixing. Algae initial size (below 50 μm and between 200 and 400 μm) and concentration (from 2 to 40 wt%) were varied. First, algae morphology, composition and surface properties are analysed for each algae type. Second, an example of algae particle size decrease during processing is given. Finally, tensile properties of composites are analysed. The surface of algae flakes was covered with inorganic salts affecting filler–matrix interactions. The Young’s modulus of composites increased at 40 wt% load of algae as compared with neat PLA although the strain at break and tensile strength decreased. In most cases the influence of algae type was minor. Larger flakes led to better mechanical properties compared to the smaller ones.     

Dielectric and ferroelectric properties of Ba(Sn0.15Ti0.85)O3 thin films grown by a sol-gel process

Ferroelectric Ba(Sn_0.15Ti_0.85)O₃ (BTS) thin films were deposited on LaNiO₃-coated silicon substrates via a sol-gel process. Films showed a strong (1 0 0) preferred orientation depending upon annealing temperature and concentration of the precursor solution. The dependence of dielectric and ferroelectric properties on film orientation has been studied. The leakage current density of thin films at 100 kV/cm was 7 × 10⁻⁷ A/cm² and 5 × 10⁻⁵ A/cm² and their capacitor tunability was 54 and 25% at an applied field of 200 kV/cm (measurement frequency of 1 MHz) for the thin films deposited with 0.1 and 0.4 M spin-on solution, respectively. This work clearly reveals the highly promising potential of BTS compared with BST films for application in tunable microwave devices.     

On structure and mechanical properties of ultrasonically cast Al-2% Al2O3 nanocomposite

An investigation on the structure of an ultrasonically cast nanocomposite of Al with 2 wt.% nano-sized Al₂O₃ (average size ∼10 nm) dispersoids showed that the nanocomposite was consisting of nearly continuous nano-alumina dispersed zones (NDZs) in the vicinity of the grain boundaries encapsulating Al₂O₃ depleted zones (ADZs). The mechanical properties were investigated by nanoindentation and tensile tests. The nano-sized dispersoids caused a marginal increase in the elastic modulus, and a significant increase in the hardness (∼92%), and tensile strength (∼48%). Subsequent cold rolling to achieve a reduction ratio of 2 resulted in an appreciable increase in the hardness due to change in morphology of the microstructure. Estimation of the strength on the basis of inter-particle spacing, which was measured by transmission electron microscopy, could not be accounted for on the basis of Orowan mechanism, and therefore, strengthening mechanisms like local climb and/or cross slip might have a role in this room temperature (0.32T_M) deformation process.     

TiN/VN composites with core/shell structure for supercapacitors

TiN/VN core-shell composites are prepared by a two-step strategy involving coating of commercial TiN nanoparticles with V₂O₅·nH₂O sols followed by ammonia reduction. The highest specific capacitance of 170 F g⁻¹ is obtained when scanned at 2 mV s⁻¹ and a promising rate capacity performance is maintained at higher voltage sweep rates. These results indicate that these composites with good electronic conductivity can deliver a favorable capacity performance.