Textural and structural studies of sol–gel derived SiO2–CaO–P2O5–MgO glasses by substitution of MgO for CaO

The partial substitution of MgO for CaO in the ternary SiO₂–CaO–P₂O₅ glass system was conducted by the sol–gel method and a comparison of the textural and structural properties was reported. The textural properties (specific surface area and pore size distribution) were obtained by N₂-adsorption measurement and the glasses structure was elucidated by Fourier transform infrared spectroscopy. It is observed that, in general, all synthesized glasses show high specific surface area and present porous nature in mesopore region. The presence of MgO in glass composition has little influence on its textural properties, however, with increasing MgO concentration the frequency of Si–O(s,asym) group shifts towards lower energy and the absorbance intensity ratio of Si–O–NBO(Q³)/Si–O–Si(s,sym)(Q⁴) declines, indicating the structure modification of MgO in glass composition.     

Photonic band gap structures by sol–gel processing

Since the launching of the photonic bandgap concept in 1987, the development of corresponding structures has expanded very rapidly, in particular two-dimensional semiconductor-based structures. In the case of sol–gel derived materials, the main emphasis for the past year has been on one-dimensional multilayer stacks and, in particular, on three-dimensional structures of the opal and inverse opal type.     

Characteristics of glass ionomer cements composed of glass powders in CaO–SrO–ZnO–SiO2 system prepared by two different synthetic routes

Glass ionomer cements (GICs) are composed of an acid degradable glass, polyacrylic acid and water. Sol–gel processing to prepare the glass phase has certain advantages, such as the ability to employ lower synthesis temperatures than melt quenching and glasses that are reported to have higher purity. A previous study reported the effects of glass synthesis route on GIC fabrication. However, in that study, the sol–gel derived glass exhibited a reduced concentration of cations. This study investigates increasing the cation content of a sol–gel derived glass, 12CaO·4SrO·36ZnO·48SiO₂ (molar ratio) by heating before aging to reduce dissolution of cations. This glass was prepared by both sol–gel and melt-quenched routes. GICs were subsequently prepared using both glasses. The resultant cement based on the sol–gel derived glass had a shorter working time than the cement based on the melt-quenched one. Contrary to this, setting time was considerably longer for the cement based on the sol–gel derived glass than for the cement based on the melt-quenched one. The cements based on the sol–gel derived glass were stronger in both compression and biaxial flexure than the cements prepared from the melt-quenched glass. The differences in setting and mechanical properties were associated with both cation content in the glass phase and the different surface area of the resultant cements.     

Antibacterial and bioactive silver-containing Na2O·CaO·2SiO2 glass prepared by sol–gel method

The antibacterial effect of addition of silver oxide to Na2O x CaO x 2SiO2 glass have been studied. Silver containing and silver free Na2O x CaO x 2SiO2 glasses have been prepared by sol-gel synthesis using tetramethil orthosilicate, sodium ethoxide, calcium nitrate tetrahydrate and silver nitrate as starting materials and methyl ethyl ketone as solvent. The gel was examined by differential thermal analysis, thermo gravimetric analysis, FTIR spectroscopy and X-ray diffraction analysis. Antibacterial and bioactive tests on gel glass powders, obtained after a heat treatment of 2 h at 600 degrees C of the dried gel, were carried out. High antimicrobial effects of samples against Escherichia coli and Streptococcus mutans were found. FTIR measurements and SEM micrographs have ascertained the formation of a hydroxyapatite layer on the surface of samples soaked in a simulated body fluid for different times.     

Continuous fibre reinforced mullite matrix composites by sol–gel processing: Part I Fabrication and microstructures

The fabrication of ceramic composites based on a mullite matrix uniaxially reinforced with either high strength carbon or Nicalon-SiC continuous fibres is described. Sols of high solids contents of up to 40 vol% were prepared using colloidal silica sol with either -alumina powder or colloidal boehmite as reactants for the preparation of the mullite matrix, 3Al2O3·2SiO2. Single-stage infiltration was used for the preparation of prepregs for laminating into composites. The composites were consolidated by uniaxially hot-pressing at 1300 or 1550°C, depending on the matrix precursors and the final phases in the matrix. Highly densified composites with fibre volume fractions of 32–60% were obtained and the microstructures characterised by mercury porosimetry, X-ray diffraction, scanning electron microscopy and transmission electron microscopy.     

Fabrication of CaO–NaO–SiO2/TiO2 scaffolds for surgical applications

A series of titanium (Ti) based glasses were formulated (0.62 SiO₂?C0.14 Na₂O?C0.24 CaO, with 0.05?mol% TiO₂ substitutions for SiO₂) to develop glass/ceramic scaffolds for bone augmentation. Glasses were initially characterised using X-ray diffraction (XRD) and particle size analysis, where the starting materials were amorphous with 4.5???m particles. Hot stage microscopy and high temperature XRD were used to determine the sintering temperature (~700?°C) and any crystalline phases present in this region (Na₂Ca₃Si₆O₁₆, combeite and quartz). Hardness testing revealed that the Ti-free control (ScC??2.4?GPa) had a significantly lower hardness than the Ti-containing materials (Sc1 and Sc2 ~6.6?GPa). Optical microscopy determined pore sizes ranging from 544 to 955???m. X-ray microtomography calculated porosity from 87 to 93?% and surface area measurements ranging from 2.5 to 3.3?SA/mm³. Cytotoxicity testing (using mesenchymal stem cells) revealed that all materials encouraged cell proliferation, particularly the higher Ti-containing scaffolds over 24?C72?h.     

Microstructural characterization of donor-doped lead zirconate titanate films prepared by sol–gel processing

Lanthanum and niobium-doped lead zirconate titanate, Pb(Zr,Ti)O₃, (PZT) thin films were prepared on Pt/Ti/SiO₂/Si substrates by sol–gel processing. Films have a Zr/Ti ratio of 52:48 and tetragonal perovskite phase structure. The influence of donor dopants on the morphology, texture and defects of PZT films was studied using X-ray diffraction, X-ray photoelectron spectroscopy, atomic force microscopy, scanning electron microscopy, breakdown field strength and fatigue. Donor doping of PZT films results in increased breakdown field strength and improved fatigue properties. These originate from (i) the reduction of texture in the [111] and increase in the texture in [100]; (ii) lower porosity, smaller grain size and smoother surfaces; (iii) granular grain structure; and (iv) reduction in the oxygen vacancy concentration in the films.     

Characterization and catalytic activity studies of sol–gel Co–SiO2 nanocomposites

Silica embedded with transition metals exhibits adequate properties for applications in catalysis, sensors and optics. Cobalt–silica (Co–SiO₂) nanocomposites were prepared by the sol–gel method and thermally treated at 700, 900, 1100 and 1250 °C. Characterization of the samples was performed by XRD and BET nitrogen adsorption. The performance of the nanocomposites was investigated by catalysis reactions of oxidation. These catalysts were found to be recyclable showing a catalytic activity even after a third recovering. The results indicate that thermal treatment of sol–gel nanocomposites at temperatures higher than 900 °C is essential for the preparation of active heterogeneous catalysts.     

Microwave-assisted sol–gel process for production of spherical mesoporous silica materials

Spherical mesoporous SiO₂ and SiO₂–TiO₂ particles were synthesized by sol–gel method using W/O emulsion under microwave irradiation. In SiO₂ system, W/O emulsion was prepared by mixing partially hydrolyzed Si(OC₂H₅)₄ aqueous solution including C₁₈TAC as template with n-hexane solution including polyglycerol polyricinalate as emulsifier. In SiO₂–TiO₂ system, Ti(OC₂H₅)₄ capped by acetylacetone was added to the aqueous phase. In both cases, spherical products were synthesized by heating of W/O emulsion for 30 min under microwave irradiation. The specific surface area and pore size of spherical products were 800 m²/g and 1.6 nm, respectively, which indicates that the spherical products are mesoporous. These results suggest that sol–gel reaction in water phase proceeds rapidly because microwave quickly and selectively heats up the aqueous solution.     

Adsorption and photocatalysis of nanocrystalline TiO2 particles prepared by sol–gel method for methylene blue degradation

Titanium dioxide (TiO₂) powders were synthesized by using TiO₂ colloidal sol prepared from titanium-tetraisopropoxide (TTIP) and used as a starting material by applying the sol–gel method. The effect of aging times and temperatures on physical and chemical properties of TiO₂ sol particles was systematically investigated. The results showed that the crystallinity and average particle size of TiO₂ can be successfully controlled by adjusting the aging time and temperature. The samples after calcination of TiO₂ powders were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and nitrogen adsorption measurements. In addition, the photocatalytic activity of synthesized TiO₂ powders was evaluated by studying the degradation of 10 ppm aqueous methylene blue dye under 32 W high pressure mercury vapor lamp with 100 mg of TiO₂ powders. The highest photocatalytic activity was observed in TiO₂ powder synthesized at 90 °C for 0 h attributed to the presence of anatase and rutile phases in an 80:20 ratio.     

Characterisation of the bioactive behaviour of sol–gel hydroxyapatite–CaO and hydroxyapatite–CaO–bioactive glass composites

The fabrication and characterization of sol–gel derived hydroxyapatite–calcium oxide (HAp–CaO) material is investigated focusing on the effect of the addition of a bioactive glass on the material bioactive behaviour through the fabrication of a novel HAp–CaO (70 wt.%)–bioactive glass (30 wt.%) composite material. The bioactive behaviour of the materials was assessed by immersion studies in Simulated Body Fluid (SBF) and the alterations of the materials surfaces after soaking periods in SBF were characterized by Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR). A brittle and weakly crystalline carbonate hydroxyapatite (HCAp) layer was found to develop on the surface of all samples, few hours after immersion in SBF, confirming the high bioactivity of the material. Alterations of the morphology of the developed HCAp layer, which led to a more compact structure, were observed on the surface of composite samples after 7 days of immersion in SBF. The presence of the CaO phase seems to accelerate the formation of HCAp, while the bioactive glass affects both the morphology and cohesion of the developed layer.     

Synthesis of ZnO nanowires by the hydrothermal method,using sol–gel prepared ZnO seed films

Zinc oxide (ZnO) nanowires with various morphologies are synthesized by the hydrothermal method on silicon substrates coated with ZnO thin films. The ZnO films are used as the seed layer and are prepared using the sol–gel technique. Experimental results demonstrate that the synthesis of ZnO nanowires is dependent on the crystalline properties of the ZnO seed-layer films. Sol concentration is the controlled parameter for the preparation of ZnO seed-layer films in this study. The ZnO films are found to have the hexagonal wurtzite structure with highly preferred growth along the c-axis at suitable sol concentrations. The vertically aligned ZnO nanowire arrays on the substrates are believed to be the result of the epitaxial growth of the ZnO seed layer. Scanning electron microscopy shows that nanowires with uniform distribution in length, diameter, and density are obtained. X-ray diffraction patterns clearly reveal that the ZnO nanowires are primarily grown along the c-axis direction. Transmission electron microscopy and selected-area electron diffraction measurements show that the nanowires have good crystalline properties. The well-aligned and high surface areas of the ZnO nanowires make them a potential candidate for applications in solar cells, field emission devices, and ultra-sensitive gas sensors.     

Photocatalytic degradation of gaseous toluene over TiO2–SiO2 composite nanotubes synthesized by sol–gel with template technique

TiO₂–SiO₂ composite nanotubes were successfully synthesized by a facile sol–gel technique utilizing ZnO nanowires as template. The nanotubes were well characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction, Fourier transform infrared spectroscopy, N₂ adsorption–desorption analysis and UV–vis diffuse reflectance spectroscopy. The nanotubular TiO₂–SiO₂ composite photocatalysts showed diameter of 300–325 nm, fine mesoporous structure and high specific surface area. The results indicated that the degradation efficiency of gaseous toluene could get 65% after 4 h reaction using the TiO₂–SiO₂ composite as the photocatalyst under UV light illumination, which was higher than that of P25.     

Optical and morphological characterization of Si nanocrystals/silica composites prepared by sol–gel processing

Linear (visible photoluminescence) and non-linear (third-order susceptibility) optical properties have been measured for laser-synthesized crystalline Si nanoparticles. The observed luminescence is compared to similar measurements on nanocomposite aerogels prepared integrating the Si-nanoparticles into a continuous silica phase by sol–gel processing. The results show that incorporation of the Si-nanoparticles into a silica matrix by sol–gel technology is not detrimental to the PL (photoluminescence) emission intensity. The effect on the nanocomposites of annealing in air (at temperatures in the range of 300–500°C) has been investigated by means of PL and Raman spectroscopy. The obtained results indicate that the oxidation treatment induces the bleaching of the smaller luminescent particles and is not effective in reducing the average size. Micro-Raman mapping and TEM analysis of the nanocomposites have shown the presence of agglomerated nanoparticles (in the sub-micrometer range), as confirmed by dynamic light scattering (DLS) measurements on colloidal suspensions of the as-synthesized powders.     

An electrochemical biosensor constructed by nanosized silver particles doped sol–gel film

The nanosized silver particles are used to dope into the sol–gel film to prepare a biosensor. The horseradish peroxidase (HRP), mediator methylene blue (MB), nanosized silver particles and sol–gel solution are mixed and coated on the surface of glass carbon (GC) electrode to get the biosensor. The silver nanoparticles in the sol–gel film can adsorb the enzyme molecules and improve the sol–gel film conductivity. The biosensor has a high sensitivity, quickly response to H₂O₂ and good stability. The biosensor responds to H₂O₂ in the linear range from 1 μM to 1 mM. The detection limit was down to 0.4 μM when the signal to noise ratio is 3. The apparent Michaelis-Menten constant of the biosensor to H₂O₂ was estimated to be 1.2 mM, showing a high affinity.     

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.     

Fabrication and characterization of bioactive composite coatings on Mg–Zn–Ca alloy by MAO/sol–gel

High corrosion rate and accumulation of hydrogen gas upon degradation impede magnesium alloys’ clinical application as implants. In this work, micro-arc oxidation (MAO) was used to fabricate a porous coating on magnesium alloys as an intermediate layer to enhance the bonding strength of propolis layer. Then the composite coatings were fabricated using sol–gel method by dipping sample into the solution containing propolis and polylactic acid at 40°C. The corrosion resistance of the samples was determined based on potentiodynamic polarization experiments and immersion tests. Biocompatibility was designed by observing the attachment and growth of wharton’s jelly-derived mesenchymal stem cells (WJCs) on substrates with MAO coating and substrates with composite coatings. The results showed that, compared with that of Mg–Zn–Ca alloy, the corrosion current density of the samples with composite coatings decreased from 5.37 × 10⁻⁵ to 1.10 × 10⁻⁶ A/cm² and the corrosion potential increased by 240 mV. Composite coatings exhibit homogeneous corrosion behavior and can promote WJCs cell adhesion and proliferation. In the meantime, pH value was relatively stable during the immersion tests, which may be significant for cellular survival. In conclusion, our results indicate that composite coatings on Mg–Zn–Ca alloy fabricated by MAO/sol–gel method provide a new type bioactive material.     

Comparison of a SiO2–CaO–ZnO–SrO glass polyalkenoate cement to commercial dental materials: glass structure and physical properties

Glass polyalkenoate cements (GPCs) have previously been considered for orthopedic applications. A Zn–GPC (BT 101) was compared to commercial GPCs (Fuji IX and Ketac Molar) which have a setting chemistry analogous to BT 101. Handling properties (working, T _w and setting, T _s times) for BT 101 were shorter than the commercial GPCs. BT 101 also had a higher setting exotherm (S _x —34 °C) than the commercial GPCs (29 °C). The maximum strengths for BT 101, Fuji IX, and Ketac Molar were 75, 238, and 216 MPa (compressive, σ _c), and 34, 54, and 62 MPa (biaxial flexural strengths, σ _f), respectively. The strengths of BT 101 are more suitable for spinal applications than commercial GPCs.     

Characterisation of Ga2O3–Na2O–CaO–ZnO–SiO2 bioactive glasses

The structural role of Gallium (Ga) is investigated when substituted for Zinc (Zn) in a 0.42SiO₂–0.40–xZnO–0.10Na₂O–0.08CaO glass series, (where x = 0.08). Each starting material was amorphous, and the network connectivity (NC) was calculated assuming Ga acts as both a network modifier (1.23), and also as a network former. Assuming a network forming role for Ga the NC increased with increasing Ga concentration throughout the glass series (Control 1.23, TGa-1 2.32 and TGa-2 3.00). X-ray photoelectron spectroscopy confirmed both composition and correlated NC predictions. Raman spectroscopy was employed to investigate Q-structure and found that a shift in wavenumbers occurred as the Ga concentration increased through the glass series, from 933, 951 to 960 cm^?1. Magic angle spinning nuclear magnetic resonance determined a chemical shift from ?73, ?75 to ?77 ppm as the Ga concentration increased, supporting Raman data. These results suggest that Ga acts predominantly as a network former in this particular Zn-silicate system.