Preparation of alumina–silica–nickel nanocomposite by in situ reduction through sol–gel route

Ceramic based composites with dispersion of nano sized metal/metal carbide particles have generated wide technological interest for their improved mechanical properties — hardness, fracture strength as well as fracture toughness, superior electrical properties and magnetic properties. In the present investigation alumina–silica gels have been prepared along with nickel chloride and dextrose distributed in the nanometric pores of the gel. The gels are prepared with different molar proportions of alumina and silica containing 5 wt% of nickel chloride and 50 wt% excess dextrose. During heat treatment at a temperature of 900°C for half an hour in nitrogen atmosphere, nickel chloride is reduced to metallic nickel by in situ generated hydrogen in the silica–alumina matrix. X-ray analyses indicate that no nickel chloride reduction is possible upto 50 mol% silica in alumina–silica matrix. Beyond this range, higher the silica content, higher is the reduction of nickel chloride. The presence of metallic nickel has been substantiated further by SAD analysis. Particle size analysis based on X-ray diffraction as well as transmission electron micrograph shows the presence of nickel particles of size ∼20 nm distributed in the alumina–silica nanocomposite.     

Preparation of nanoporous silica–zirconia layers by in situ sol–gel method

Abstract

Silica–zirconia membranes were prepared using a sol–gel process, never before used on this system. Thin layers of gel were grown on the outside of porous alumina support tubes using the permeation of water through pores of the tube to control the rate of hydrolysis with a reactive silica–zirconia alkoxide solution. A recipe was developed and optimum coating conditions were found to be the ratios of tetraethylorthosilicate (TEOS) to Zr propoxide to 1-propanol molar ratios (1:0·5:17), with a coating time of 300 s. The method allowed the formation of a membrane in a single step compared with repeated coating and firing. The coatings could be prepared adherent and without cracks when properly prepared.     

Preparation of continuous alumina gel fibres by aqueous sol–gel process

Continuous alumina gel fibres were prepared by sol–gel method. The spinning sol was prepared by mixing aluminum nitrate, lactic acid and polyvinylpyrrolidone with a mass ratio of 10:3:1· 5. Thermogravimetry–differential scanning calorimetry (TG–DSC), Fourier transform infrared (FTIR) spectra, X-ray diffraction (XRD), and scanning electron microscopy (SEM) were used to characterize the properties of the gel and ceramic fibres. The Al₂O₃ fibres with a uniform diameter can be obtained by sintering gel fibres at 1200 °C.     

Preparation and complex characterization of silica holmium sol–gel monoliths

Amorphous, sol–gel derived SiO₂ are known to biocompatible and bioresorbable materials. Biodegradable and inert materials containing radioactive isotopes have potential application as delivery vehicles of the beta radiation to the cancer tumors inside the body. Incorporation of holmium in the sol–gel derived SiO₂ could lead to the formation of a biodegradable material which could be used as carrier biomaterial for the radiation of radioactive holmium to the various cancer sites. The homogeneity of the prepared sol–gel silica holmium monoliths was investigated by Back Scattered Electron Imaging of Scanning Electron Microscope equipped with Energy Dispersive X-ray Analysis, X-ray Induced Photoelectron Spectroscopy and Nuclear Magnetic Resonance Spectroscopy. The biodegradation of the monoliths was investigated in Simulated Body Fluid and TRIS (Trizma pre-set Crystals) solution. The results show that by suitable tailoring of the sol–gel processing parameters holmium can be homogeneously incorporated in the silica matrix with a controlled biodegradation rate.     

Study of silicon nanoparticles in dielectric oxides obtained by sol–gel route

Silicon nanoparticles (Si-NPs) obtained by electrochemical etching of silicon wafer were incorporated into various dielectric matrices using sol–gel method. To attain a wide range of dielectric constant and band gap energy, three matrices are selected (SiO₂, ZrO₂ and TiO₂) and the Si-NPs were incorporated in these matrices at different concentrations. Structural studies by transmission electron microscopy and Raman spectroscopy confirm the presence of Si-NPs in the matrices. Moreover, the significant compressive stress induced by the matrix is observed. Photoluminescence (PL) studies show that Si-NPs preserve their luminescent properties in SiO₂ matrix and ZrO₂ matrix but not in TiO₂ matrix. The PL peak position depends not only on the dimension of Si-NPs but also depends on their concentrations. This is due to the coupling effect between the nanoparticles which increases with concentration.     

Preparation of polycrystalline YAG/alumina composite fibers and YAG fiber by sol–gel method

Polycrystalline yttrium–aluminum garnet, Y₃Al₅O₁₂ (YAG) fiber and α-alumina and YAG matrix composite fiber were prepared by the sol–gel method. α-Alumina and YAG matrix composite fiber with fine and homogeneous microstructure could be successfully fabricated by interpenetrating YAG in alumina matrix and adding α-alumina of seed particles to fibers. Effect of α-alumina seed particles and YAG on crystallization and microstructure of composite fiber were discussed. The size of alumina matrix of the composite fibers heated at 1600°C for 4 h was below 2 μm. The tensile of strength alumina fiber heat-treated at 1500°C was 0.2 GPa, while that of the composite fiber was 1.1 GPa.     

Preparation of nanocrystalline nickel oxide thin films by sol–gel process for hydrogen sensor applications

Preparation of nanocrystalline NiO thin films by sol–gel method and their hydrogen (H₂) sensing properties were investigated. The thin films of NiO were successfully deposited on the glass and SiO₂/Si substrate by a sol–gel coating method. The films were characterized for crystallinity, electrical properties, surface topography and optical properties as a function of calcination temperature and substrate material. It was found that the films produced by this method were polycrystalline and phase pure NiO. The H₂ gas sensitivity of these films was studied as a function of H₂ concentration and calcination temperature. The results indicated that the sol–gel derived NiO films could be used for the fabrication of H₂ gas sensors to monitor low concentration of H₂ in air quantitatively at low temperature range (< 200 °C).     

Densification of mullite–SiC nanocomposite sol–gel precursors by pressureless sintering

Mullite–SiC nanocomposite has been synthesised based on a nanoprecursor route and sintered to high density through pressureless sintering technique. The approach has been first to evolve a method to obtain high density, fine-grained mullite matrix phase through a sol–gel seeded route. Nanosize SiC particles (∼200 nm) were dispersed in a seeded mullite precursor sol to obtain mullite-coated SiC particles, which were further compacted and sintered to hybrid composites, resulting in distribution of SiC particles at the inter- and intra-mullite grain positions.     

Synthesis of nanocomposite powders of γ-alumina-carbon nanotube by sol–gel method

The nanocomposite powders of γ-alumina-carbon nanotube were successfully synthesized by a sol–gel process. The homogeneous mixture of carbon nanotubes and alumina particles was obtained by mixing the carbon nanotubes within alumina solution and followed by heating into gel. The resultant gel was dried and calcined at 200 °C into boehmite-carbon nanotubes composite powders. The mean particle size of synthesized boehmite was of the order of 4 nm. The boehmite-carbon nanotubes composite powders were calcined at different temperatures and XRD investigations revealed that as the amount of carbon nanotube increases, γ- to α-alumina phase transformation is completed at higher temperatures. The specific surface area and mean particle size of resultant nanocomposite powders increased and decreased, respectively by increasing the content of carbon nanotubes.     

Superhydrophilic titania wall coating in microchannels by in situ sol–gel modification

An in situ reaction sol–gel method to synthesize superhydrophilic titania films in silicon microchannels at room temperature is reported. Superhydrophilic surface can be realized on TiO₂ films with thickness less than 10 nm. The water flow velocity in the TiO₂-coated silicon channels reached almost 4 times of the velocity in SiO₂-coated channels. The ultra-thin superhydrophilic TiO₂ films fabricated by this method show the ability to strongly improve the capillary of microchannels without affecting the morphology of the channel walls, indicating potential applications to biomolecule analysis and surface tension driven microfluidic systems. Due to its low operating temperature, this method is also suitable for polymer microstructures such as PDMS and PMMA microfluidic chips.     

Preparation of DNA–cyclodextrin–silica composite by sol–gel method and its utilization as an environmental material

A DNA–cyclodextrin–silica composite was prepared by the sol–gel method. This composite possessed the bi-functions of double-stranded DNA, such as intercalation into DNA, and cyclodextrin, such as inclusion into its intramolecular cavity. Therefore, we demonstrated the accumulation of harmful compounds from an aqueous multi-component solution using a DNA–cyclodextrin–silica composite column. As a result, the DNA–cyclodextrin–silica composite column can effectively accumulate not only planar structure-containing harmful compounds, such as dioxin and polychlorobiphenyl (PCB) derivatives, but also non-planar structure containing compounds, such as bisphenol A and diethylstilbestrol, from an aqueous multi-component solution. The accumulated amount of these harmful compounds was more than 90%. Additionally, the DNA–cyclodextrin–silica composite column was recycled by the application of methanol. Therefore, the DNA–cyclodextrin–silica composite may have the potential to be used as an environmental material for the accumulation of harmful compounds from industrial or experimental waste.     

Temperature dependence of the dielectric properties of mesoporous silica films prepared by a sol–gel route in the presence of polyether modified polydimethylsiloxane

Mesoporous silica films were prepared from tetraethylorthosilicate by an acid-catalyzed sol–gel process in the presence of side-chain polyether modified polydimethylsiloxane. The samples were characterized using Fourier transform infrared spectroscopy, differential thermal analysis and thermogravimetric analysis, field emission scanning electron microscopy, and atomic force microscopy. Furthermore, the dielectric properties of the silica films annealed at different temperatures were investigated at frequencies ranging from 1 to 200 kHz. In addition, the temperature dependence of the dielectric properties of as-prepared porous silica films is discussed in detail.     

Dielectric properties of Fe-doped TiO2 nanoparticles synthesised by sol–gel route

Fe-doped nanocrystalline samples of titanium oxide have been synthesised by sol–gel route and conventional sintering process at 450°C under atmospheric conditions. These samples are characterised by X-ray diffraction (XRD), X-ray photoelectron spectroscopy, transmission electron microscopy (TEM) and dielectric property measurement. Samples with Fe content more than 4?mole% crystallises in rutile phase and those with less than 4?mole% crystallises in anatase phase. Nanocrystallite size has been controlled by Fe doping. Crystallite size was found to decrease with Fe concentration in the anatase phase samples whereas reverse happens in rutile phase samples of titanium oxide. There is a slight variation in numerical values of crystallite sizes measured by the two techniques: TEM and XRD peak broadening. The highest crystallite size was 86?nm in 10?mole% Fe-doped samples and the lowest 20?nm in 4?mole% Fe-doped sample. Large dispersions and anomalous values of the dielectric constant, εr were observed at low frequency in anatase phase samples. Rutile phase samples exhibit little dispersion over the measurement frequency range of 20?Hz to 10?MHz. The dielectric constant value of all the samples stabilises to a constant value at higher frequencies. This value is dependent on the final crystalline phase but independent of the crystallite size. The anomalous dielectric behaviour of anatase samples at low frequencies is assigned to the adsorbed –OH ions on the sample surface.     

Preparation and characterization of monodisperse silica nanoparticles via miniemulsion sol–gel reaction of tetraethyl orthosilicate

Monodisperse silica nanoparticles were prepared via miniemulsion sol–gel reaction of tetraethyl orthosilicate (TEOS). Hexadecane (HD) or hexadecyltrimethoxysilane was used as costabilizer to effectively retard the Ostwald ripening process involved in TEOS miniemulsion. The Ostwald ripening behavior was characterized by dynamic light scattering (DLS), and it was adequately described by the modified Kabal’nov equation. The miniemulsion sol–gel reaction of TEOS/HD with a volume fraction (φ _c) of 0.024 at 80 °C is stable in the pH range 6–10. By contrast, gelation of reacting miniemulsions occurs at 70 and 100 min at pH 4 and 5, respectively. The weight-average silica particle size (d _w) of colloidal products prepared at 80 °C and pH 7 decreases from 59 to 36 nm with low polydispersity index (PDI, in the range 1.02–1.03), determined by transmission electron microscopy, when the φ _c of HD increases from 0.024 to 0.23. At constant φ _c (0.024), the resultant silica nanoparticles show larger d _w (83 nm) and PDI (1.35) for the TEOS/HD system at pH 10 as compared to the counterpart of pH 7. Furthermore, for the TEOS/HD system at pH 7 and low φ _c (0.024), d _w increases significantly with temperature being increased from 25 to 80 °C. By contrast, the effect of temperature on silica nanoparticle size becomes insignificant when a high level of HD (φ _c = 0.23) is used. Zeta potential measurements and field emission scanning electron microscopy were used to characterize the surface charge density and morphology of resultant silica nanoparticles.     

Preparation of nickel–silver core–shell nanoparticles by liquid-phase reduction for use in conductive paste

Nickel–silver (Ni–Ag) core–shell nanoparticles (NPs) were prepared by depositing Ag on Ni nanocores using the liquid-phase reduction technique in aqueous solution, and their properties were characterised using various experimental techniques. The core–shell NPs had good crystallinity, and the thicknesses of the Ag nanoshells could be tuned effectively. The oxidation resistance of the Ag surface and the electroconductive properties of the Ni core allowed these Ni–Ag core–shell NPs to be used in a conductive paste. Thick films composed of Ni–Ag core–shell NPs were screen-printed on a polycrystalline silicon substrate then sintered at temperatures ranging from 500 °C to 800 °C. Stable resistivity was obtained when the sintering temperature was higher than 650 °C, and the electrical properties of the Ni–Ag core–shell paste were close to those of pure Ag paste. Thus, the Ni–Ag NPs can partly replace pure Ag NPs in conductive pastes.     

In vitro study of hydroxyapatite/polycaprolactone (HA/PCL) nanocomposite synthesized by an in situ sol–gel process

Hydroxyapatite (HA) is the most substantial mineral constituent of a bone which has been extensively used in medicine as implantable materials, owing to its good biocompatibility, bioactivity high osteoconductive, and/or osteoinductive properties. Nevertheless, its mechanical property is not utmost appropriate for a bone substitution. Therefore, a composite consist of HA and a biodegradable polymer is usually prepared to generate an apt bone scaffold. In the present work polycaprolactone (PCL), a newly remarkable biocompatible and biodegradable polymer, was employed as a matrix and hydroxyapatite nanoparticles were used as a reinforcement element of the composite. HA/PCL nanocomposites were synthesized by a new in situ sol–gel process using calcium hydroxide and phosphoric acid precursors in the presence of Tetrahydrofuran (THF) as a solvent. Chemical and physical characteristics of the nanocomposite were studied by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FTIR) analyses. The results indicated that pure HA nanoparticles were well-incorporated and homogenously dispersed in the PCL matrix. It was found that the mechanical property of PCL was improved by addition of 20 wt.% HA nanoparticles. Furthermore, the biological property of nanocomposites was investigated under in vitro condition. For this purpose, HA/PCL scaffolds were prepared through a salt leaching process and immersed in a saturated simulated body fluid (SBF) after 3 and 7 days. It was found that a uniform layer of biomimetic HA could be deposited on the surface of HA/PCL scaffolds. Therefore, the prepared HA/PCL scaffolds showed good potential for bone tissue engineering and could be used for many clinical applications in orthopedic and maxillofacial surgery.     

Polyimide/silica/titania nanohybrids via a novel non-hydrolytic sol–gel route

Polyimide/silica/titania hybrid films were prepared via a non-hydrolytic sol–gel route. Silicic acid and titanium tetrachloride were used as the precursors of silica and titania, respectively. The absorption band of Si–O–Ti bonds in FTIR spectra of the hybrid films revealed the formation of the hybrid inorganic network between SiO₂ and TiO₂. Scanning electron microscopy results indicated that the nanometer-scaled inorganic domains were homogeneously dispersed in polyimide matrix due to the introduction of silica-stabilized TiO₂ and the interactions between organic and inorganic phases. The studies on the optical properties of the hybrid films indicated the red-shift of the absorption band increased with increasing TiO₂ content, while all the hybrid films maintained their transparencies. The surface resistances of the hybrid samples decreased with increasing TiO₂ content. The thermal decomposition temperature of the ternary hybrid films decreased slightly with increasing TiO₂ content. This kind of hybrid materials may have potential application in the preparation of opto-electronic devices.     

Protein encapsulation in functionalized sol–gel silica: influence of organosilanes and main silica precursors

Journal of Materials Science - Over the last few years, bone repair has increasingly gained in importance. In recent years, considerable attention has been given to the administration of...     

Fabrication of silica glass containing yellow oxynitride phosphor by the sol–gel process

We have prepared silica glass by the sol–gel method and studied its ability to disperse the Ca-α-SiAlON:Eu²⁺ phosphor for application in white light emitting diodes (LEDs). The emission color generated by irradiating doped glass with a blue LED at 450 nm depended on the concentration of SiAlON and the glass thickness, resulting in nearly white light. The luminescence efficiency of 1-mm-thick glass depended on the SiAlON concentration, and was highest at 4 wt% SiAlON.     

Structural characterization of nickel tantalum oxide synthesized by sol–gel spin coating technique

For the first time, crack-free, dense and transparent tetragonal NiTa₂O₆ single-phase structure thin films have been prepared by a sol–gel method using tantalum isopropoxide and nickel acetate. The formation of the NiTa₂O₆ phase starts from 750°C onwards. The complete tetragonal structure of NiTa₂O₆ forms on silicon(100) substrates at an annealing temperature of 850°C for 5 h. As the annealing temperature increased from 750°C to 950°C, we have not observed any kind of silicate phases due to silicon diffusion at the interface of Si and NiTa₂O₆ phase. Structural, morphological and elemental evolution of these NiTa₂O₆ thin films produced by the sol–gel synthesis were characterized by grazing incidence X-ray diffraction (GIXRD), tapping mode atomic force microscopy (TMAFM) and X-ray photoelectron spectroscopy (XPS), respectively.