Dielectric,piezo and ferroelectric properties of microwave sintered PbTiO3 synthesized by sol–gel method

Journal of Sol-Gel Science and Technology - Of all the piezoelectric ceramics, lead titanate (PbTiO3) has an important place as an electromechanical transducer. In the present article PbTiO3...     

Synthesis and characterization of sol–gel alumina nanofibers

Abstract Alumina nanofibers of high aspect ratio with surface area of >300 m² g⁻¹ has been prepared successfully in bulk quantities by the sol–gel method. The synthesis parameters including the binary water–alcohol solvent system to aluminium isopropoxide ratio, pH, type of solvent and aging temperature affect the uniformity and formation of nanofibers. It is proposed that alumina nanofibers were formed by the curling of the nanosheets upon condensation after the hydrolysis. The phase evolution of alumina nanofibers from pseudoboehmite to α phase has been shown by XRD and FTIR. ²⁷Al NMR investigations show that the Al atoms are six and four coordinated. The morphology of the alumina nanofibers does not change much as the calcination temperature was increased. In addition, the average pore size increases and the BET surface area decreases as a function of calcination temperature. The thermal behavior of alumina nanofibers was investigated by TGA. Graphical Abstract      

Thermally stable and transparent superhydrophobic sol–gel coatings by spray method

A facile method was developed for the fabrication of the methyltriethoxysilane based transparent and superhydrophobic coating on glass substrates. The transparent and hydrophobic coatings were deposited on the glass substrates, using spray deposition method followed by surface modification process. A spray deposition method generates hierarchical morphology and post surface modification with monofunctional trimethylchlorosilane decreases the surface free energy of coating. These combined effects of synthesis produces bio-inspired superhydrophobic surface. The deposited coating surface shows high optical transparency, micro-nano scale hierarchical structures, improved hydrophobic thermal stability, static water contact angle of about 167° ± 1°, low sliding angle about 2° ± 1° and stable superhydrophobic nature. This paper provides the very simple sol–gel approach to the fabrication of optically transparent, thermally stable superhydrophobic coating on glass substrates. This fabrication strategy may easily extend to the industrial scale up and high-technology fields.     

Sintering properties of sol–gel derived lithium disilicate glass ceramics

Lithium disilicate (Li₂Si₂O₅) glass-ceramics were fabricated through two sol–gel methods: the nitrate route and the alkoxide route. Thermal analysis revealed different crystallization processing of two gel-derived powders. Li₂Si₂O₅ powders were obtained after heat treatment at 800?°C. These powders were pressed and pressureless sintered under 900–1030?°C. Microstructure of sintered samples revealed the grain size and morphology of Li₂Si₂O₅ ceramics. Although grain size in both samples increased with increasing sintering temperature, samples from the alkoxide route derived powders had more uniform grain size and pore distribution. In addition, open porosity decreased in both samples with increasing sintering temperature. Unlike familiar nucleation that resulted in grain growth mechanism, the Li₂Si₂O₅ particles developed into irregular large size grains at first, and then grew into rod-shaped grains.

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Nanoporous morphology of alumina films prepared by sol–gel dip coating method on alumina substrate

Nanoporous crack free alumina thin films were fabricated in two phases gamma (??) and alpha (??) by sol?Cgel dip coating method. The thickness of the mesoporous films was increased with binder by varying its concentration, and with increasing the number of coating. The porosity, pore size, surface area and phase were controlled by sintering temperature. Interconnected pore structure of 8?C15?nm diameter were successfully prepared by repeating the deposition several times. FESEM, BET, AFM and XRD techniques were employed for the microstructural characterization.     

Thermal properties of pressure sintered alumina–graphene composites

Journal of Thermal Analysis and Calorimetry - The work concerns the alumina–graphene materials sintered by two different pressure methods. The different particle sizes of graphene were used....     

A novel low temperature synthesis technique of sol–gel derived nanocrystalline alumina abrasive

The effect of ball milling process, co-doped seed and two step sintering technique on the properties of sol–gel derived alumina abrasive sintered at low temperature was investigated. The results showed that ball milling time with 10 h can be effective in enhancing the activity of the precursor and the microstructural uniformity of sintered alumina abrasive. A small amount of Al₂O₃–(NH₄)₃AlF₆ co-doped seed addition had potential synergistic effects for reducing α-Al₂O₃ phase transformation temperature and improving the mechanical property of alumina abrasive. A remarkable suppression of grain growth was achieved by controlling sintering temperature with two-step sintering method. Therefore, by using ball milling process, co-doping α-Al₂O₃–(NH₄)₃AlF₆ seed and two-step sintering technique, the sol–gel derived uniform nanocrystalline alumina abrasive is easily achieved at low temperature. Nanocrystalline alumina abrasive prepared at these conditions exhibited excellent mechanical properties and wear resistance compared to fused corundum abrasive and those sol–gel derived corundum abrasive with conventional sintering methods.     

Sol–gel derived mesoporous and microporous alumina membranes

Stable polymeric and colloidal boehmite sols were prepared by sol–gel process through controlled hydrolysis/condensation reactions. The particle sizes of the colloidal sols were in the 12–25 nm range depending on the process parameters and about 2 nm for polymeric sols. The presence of a significant increase in the microporosity content of the heat treated polymeric membranes relative to the mesoporous colloidal membranes might make the design of thermally stable microporous alumina membranes with controlled pore structures possible. The phase structure evolution in the 600–800 °C range had shown that the crystallization of the gamma alumina in the amorphous matrix starts at about 800 °C. This indicated that the pore structure stability may be enhanced through processing up to this relatively high temperature in polymeric alumina derived unsupported membranes. The permeance values of the two and three layered colloidal alumina membranes were observed to be independent of pressure which implies that the dominant gas transport mechanism is Knudsen diffusion in these structures. This was also supported by the 2.8 nm BJH pore sizes of the colloidal membranes. The Knudsen diffusion equation derived permeances of the polymeric alumina membranes with thicknesses of about 300 nm were determined to be very close to the experimentally determined permeance values.     

Preparation and properties of sol–gel waterborne polyurethane adhesive

Waterborne polyurethane (WBPU) sol–gel adhesives were prepared through a prepolymer process followed by a sol–gel reaction of (3-aminopropyl)triethoxysilane (APTES). The terminal amine group of APTES reacted with the NCO group of the prepolymer, and the ethoxy group created Si–O–Si branching by hydrolysis and condensation reactions in water at the dispersion step. Water swelling (%), tensile strength and Young’s modulus of the synthesized WBPU sol–gel adhesives were improved by increasing APTES content. Synthesized WBPU sol–gel adhesives were used for bonding nylon fabrics. A significant improvement in adhesive strength was recorded, and the potential for good adhesive strength under water at moderately high temperature (up to 75 °C) was observed with 6.84 mol% APTES in WBPU sol–gel adhesives.     

Electrochromic and photoelectrochromic properties of sol–gel derived tungsten trioxide/titania composite thin films

Tungsten trixoide/titania (WO₃-titania) composite thin films with W/Ti molar ratios of 100/0, 98/2, 96/4, 94/6 92/8 and 90/10 were prepared on fluorine-doped tin oxide conducting glass, and their electrochromic (EC) and photoelectrochromic (PEC) performances were investigated in this study. The composite thin films were synthesized by sol–gel process using peroxotungstic acid and titanium (IV) n-butoxide as the precursors. The surface morphology and composition of the composite thin films were characterized using scanning electron microscope with energy dispersive spectrometer. Electrochemical experiments with in situ spectroscopic measurement were employed to study the EC properties of the composite thin films. It was found that the presence of titania in the WO₃ matrix might slightly decreases its EC performance. PEC cells using the composite thin films as the working electrode and a sputtered semitransparent platinum thin film on ITO as the counter electrode were fabricated and their PEC performances were investigated. The device using composite thin film prepared from sol solution with a W/Ti molar ratio of 96/4 exhibited the best PEC performance.     

Role of reaction atmosphere in preparation of potassium tantalate through sol–gel method

Potassium tantalate (KT) thin films and powders of both K₂Ta₂O₆ (KT pyrochlore) and KTaO₃ (KT perovskite) structures were prepared by means of chemical solution deposition method using Si(111) with ZnO and MgO buffer layers as a substrate. The influence of reaction atmosphere on reaction pathway and phase composition for both KT powders, and KT thin films has been studied mainly by means of powder diffraction and infrared spectroscopy. When an oxygen flow instead of static air atmosphere has been used the process of pyrolysis in oxygen runs over much narrower temperature interval (200–300 °C), relatively to air atmosphere (200–600 °C) and almost no (in case of powders), or no (in case of thin films) pyrochlore intermediate phase has been detected in comparison with treatment in air, where the pyrochlore phase is stable at temperatures 500–600 °C (powders). KT perovskite phase starts to crystallize at temperatures 50° and 150 °C lower compared to air atmosphere in case of powders and thin films, respectively. Microstructure formed by near-columnar grains and small grains of equiaxed shape was observed in films treated in oxygen and air atmosphere, respectively.     

Small-angle scattering of synchrotron radiation investigations of nanostructured alumina membranes synthesized by sol–gel method

Alumina asymmetric ceramic membranes were prepared by sol–gel method. Research on structure of alumina membrane active layer is conducted by methods of physical nitrogen adsorption and small-angle scattering of synchrotron radiation, the obtained data confirms and supplements each other. Surface area for the studied material varies from 255 to 264 m²/g, average pore diameter varies from 5.3 nm to 5.4 nm.     

AFM substantiation of the fracture behavior and mechanical properties of sol–gel derived silica packed epoxy networks

Silica packed epoxy networks are prepared in two steps via in situ, solvent free sol–gel processing of tetraethoxysilane in liquid epoxy monomer and curing the mixture with a flexible diamine afterwards. The influence of filler content and processing conditions on the mechanical properties and the fracture behavior is studied by means of the static mechanical analysis and AFM characterization of the pristine and the fractured polymer surfaces, and a mechanism to enhance polymer strength and toughness is proposed. The in–situ evolution and packing of silica nanostructures into epoxy networks influences the overall morphology and performance of polymers under high stress. It is found that smaller silica domains distributed at the molecular level cause efficient crack distribution by absorbing energy and thus improve the strength and toughness of silica packed epoxy polymers.     

Synthesis of sub-micro-sized solid alpha alumina fibers with smooth surfaces by sol–gel method

Alumina sol containing nano-meter sized Al₂O₃ particles were synthesized using aluminum sec-butoxide and nitric acid as precursor and peptizing agent, respectively. Polyvinylpyrrolidone (PVP) was added to prevent particle growth and adjust sol viscosity. PVP/alumina hybrid fibers were drawn from the sol with a viscosity value in the range of 2,500–3,000 mPa.s. By guided through a temperature gradient tube furnace at a rate of 4 m/min, the wet PVP/alumina hybrid fibers were sufficiently dried. Sub-micro-sized pure alpha alumina fibers were obtained by sintering the dry hybrid fibers at 1,000 °C for 3 h. The organic matters were decomposed within a wide temperature range from 150 to 800 °C allowing the nano Al₂O₃ particles to gradually get together and form solid alumina fibers with smooth surfaces.     

Effects of growth behaviors on chemical and physical properties of sol–gel derived ZnO:Ga films

In this study, we investigated the effects of different heating processes on the structural, electrical and chemical properties of ZnO:Ga (GZO) films from the viewpoint of nucleation and growth behaviors. An infrared heating furnace and a traditional tube furnace were employed for the homogeneous and heterogeneous nucleation of GZO films. XRD patterns demonstrated that the preferential growth orientation of both kinds of GZO films is still the (002) direction. XPS data implied that the infrared heating process enables more uniform distribution of the dopant material and retards the oxidization of gallium in grain boundary areas. At the same time, the textured crystallite might provide a free tunnel for oxygen diffusion. Thus, the activation of free charge carriers could be more efficient when the GZO films were annealed under vacuum. As a result, the samples annealed by the infrared heating furnace had a noticeably high carrier concentration. Although the mobility was slightly smaller than that of the samples annealed by the tube furnace, film resistivity dropped obviously in general.     

Cathodoluminescence properties of Pr3+-doped perovskite-type transparent red luminescent thin films processed by a sol–gel method

Transparent, luminescent films of Pr³⁺-doped (Ca_0.6Sr_0.4)TiO₃ (CSTO) have been prepared for cathodo-excitation of pure red luminescence by a sol–gel method from a stabilized sol with Ca²⁺, Sr²⁺, Pr³⁺ ions and titanium-isopropoxide in acetic acid. The structure and surface morphology of the obtained films are characterized by X-ray diffraction and Atomic Force Microscopy, respectively. The photoluminescence and cathodoluminescence (CL) properties of the films are evaluated. The films exhibit a strong single line of ¹D₂ → ³H₄ red photoluminescence of Pr³⁺ ions doped, which increases almost linearly with the number of the dip-coated layers. It is also found that strong single red photoemission is observed and the CL intensity increases with increasing acceleration voltage. The results demonstrate that it is potential for application in field-emission display devices.     

Growth, structure and optical properties of tartaric acid-templated silica nanotubes by sol–gel method

Photoluminescent nano material has been reported as an intriguing field during the past few decades. In this article, tartaric-templated silica nanotubes were conveniently synthesized by sol–gel method. X-ray diffraction analysis, scanning electron microscopy, transmission electron microscopy, fourier transform infrared spectra and photoluminescence spectra analysis were employed to characterize the growth, structure, morphology and optical property of the products. It is found that tartaric templates can form spindle/spherical-like aggregates composed of many sheets under static/stirring condition, which lead to the different shapes of silica nanotubes. Then the probable strategies for silica nanotubes templating with tartaric acid were described particularly. Hydrogen-bond interaction, supramolecular interaction and a competition of various effects may be the reasons of the nanotubes formation. Moreover, under ultraviolet light excitation, the silica nanotubes exhibited blue emission and luminescent intensity of the tubes prepared under the static condition is much stronger than the stirring ones, mostly because of more defect centers in the structures obtained under stirring condition.