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.     

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 of monolithic aluminium titanate with well-defined macropores via a sol–gel process accompanied by phase separation

Monolithic aluminium titanate with well-defined macropores has been prepared through a sol–gel process accompanied by phase separation, using poly(ethylene oxide) (PEO) to induce the phase separation and formamide (FA) to control the gelation of Al₂O₃–TiO₂ system. Appropriate amounts of PEO and formamide allow the formation of aluminium titanate xerogel with cocontinuous macroporous structure and a monolithic shape. The pore size of the resultant dried gels is in the range of 2–3 μm and the porosity is above 60%. The as-dried gel is amorphous and completely transforms into a single phase Al₂TiO₅ after heat-treated at 1300 °C. The macroporous structure is well maintained while the skeleton becomes smooth after heat-treatment.     

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 and electrochemical characterization of lithium cobalt oxide nanoparticles by modified sol–gel method

Uniformly distributed nanoparticles of LiCoO₂ have been synthesized through the simple sol–gel method in presence of neutral surfactant (Tween-80). The powders were characterized by X-ray diffractometry, transmission electron microscopy and electrochemical method including charge–discharge cycling performance. The powder calcined at a temperature of 900 °C for 5 h shows pure phase layered LiCoO₂. The results show that the particle size is reduced in presence of surfactant as compared to normal sol–gel method. Also, the sample prepared in presence of surfactant and calcined at 900 °C for 5 h shows the highest initial discharge capacity (106 mAh g^?1) with good cycling stability as compared to the sample prepared without surfactant which shows the specific discharge capacity of 50 mAh g^?1.     

Preparation and luminescent properties of Eu-doped BaTiO3 thin films by sol–gel process

Eu-doped BaTiO₃ thin films with a pseudo-cubic perovskite structure were successfully fabricated on magnesia substrates at low temperature by using a high-concentration sol–gel process, in which the newly developed gel-aging process on substrate was employed. Film microstructure, crystallinity, sintering properties and photoluminescence (PL) were investigated. The xerogel thin films exhibited strong PL associated with Eu³⁺ ions under ultraviolet excitation at room temperature; the PL was visible to naked eyes. The intensity maximum of PL was reached with doping concentration of about 8 mol%. Sintering above 600 °C caused reduction of europium, resulting in a rapid quenching of Eu³⁺ emission and enhancement of Eu²⁺ emission.     

Synthesis and thermomechanical characterization of polyimides reinforced with the sol–gel derived nanoparticles

Polyimide-based nanocomposites prepared by the in situ generation of inorganic nanoparticles (silica) through the sol–gel process were characterized by kinetics of water uptake, thermogravimetry and dynamic mechanical analysis.Silica particles turned out to possess a rather loose inner structure characterized by enhanced water diffusivities and by dynamic elasticity moduli comparable to that of the pristine, glassy PI. Thermal stability and thermomechanical properties of nanocomposites in the glassy state remained nearly the same as those of the pristine PI, while a significant reinforcement effect was observed for the rubbery PI matrix.     

Preparation of highly crystalline mesoporous TiO2 by sol–gel method combined with two-step calcining process

Mesoporous TiO₂ samples, with large specific surface area and high crystallinity, were prepared by a sol–gel method using polyethylene glycol and polyacrylamide (PAM) as composite templates and by two-step calcining process (at 500—700 °C in nitrogen and 500 °C in air). As a comparison, the sample was prepared using same composite templates by one-step calcining process (at 500 °C in air). The samples were characterised by X-ray diffraction, transmission electron microscopy, N₂ adsorption–desorption, and diffuse reflectance UV-visible absorption spectra. The results showed that when the samples were fabricated using two-step calcining process, they exhibited typical mesoporous structure, large specific surface area, and high crystallinity. The properties of samples were studied. The results showed that PAM accelerates gel rate. The crystallinity and specific surface areas of samples were increased by using two-step calcining process. Compared with the sample prepared using one-step calcining process, the visible light absorption of samples synthesised by the two-step calcining process was improved.     

Synthesis and characterization of NiO nanoparticles by sol–gel method

Nickel oxide nanoparticles have been synthesized in the presence of agarose polysaccharide by sol–gel method. The structure, morphology, optical and magnetic properties of the product was examined by X-ray diffraction, transmission electron microscopy, UV–visible spectrophotometer and superconducting quantum interference device magnetometer. The result of thermogravimetric analysis of the precursor product showed that the proper calcination temperature was 400 °C. X-ray diffraction result revealed that the obtained product was nickel oxide with face-centered cubic structure. TEM image demonstrated that the nickel oxide nanoparticles have spherical shape with size around 3 nm. Analysis of FTIR spectra confirmed the composition of product. The optical absorption band gap of the NiO nanoparticles was estimated to be 3.51 eV. Magnetic measurement showed that the nickel oxide nanoparticles exhibit superparamagnetic behavior at 300 K. Moreover, the nanoparticles show ferromagnetic interactions at 4.2 K owing to the existence of uncompensated moments on the surface of the nanoparticles.     

Preparation and luminescence properties of ormosil hybrid materials doped with Tb(Tfacac)3phen complex via a sol–gel process

In this paper, silica-based transparent organic–inorganic hybrid materials were prepared via the sol–gel process. Tetraethoxysilane (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTMS) were used as the inorganic and organic precursors, respectively. The terbium complex, Tb(Tfacac)₃phen (Tfacac=1,1,1-trifluoroacetylacetone, phen=1, 10-phenanthroline) was successfully doped into organically modified silicate (ormosil) matrix derived from TEOS and GPTMS, and the luminescent properties of the resultant ormosil composite phosphors [ormosil/Tb(Tfacac)₃phen] were investigated compared with those of the Tb(Tfacac)₃phen incorporated into SiO₂ derived from TEOS (labeled as silica/Tb(Tfacac)₃phen). Both kinds of the materials show the characteristic green emission of Tb³⁺ ion. The luminescence behavior of the resultant composite products was dependent on the matrix composition. The optimized lanthanide complex concentration in the ormosil/Tb(Tfacac)₃phen was increased compared with in silica/Tb(Tfacac)₃phen. Furthermore, the lifetime of Tb³⁺ in Tb(Tfacac)₃phen, silica/Tb(Tfacac)₃phen and ormosil/Tb(Tfacac)₃phen follows the sequence: ormosil/Tb(Tfacac)₃phen>silica/Tb(Tfacac)₃phen>pure Tb(Tfacac)₃phen.     

Preparation and characterization of unique zirconia crystals within pores via a sol–gel-hydrothermal method

Unique ZrO₂ crystals within pores were prepared by a sol–gel-hydrothermal method and characterized by XRD, TG/DTA, TEM, SEM, and N₂ adsorption–desorption isotherms. Results show that the dried sol–gel was converted into monoclinic zirconia crystals after calcined above 550 °C. The crystal sizes of the zirconia single crystal were in the range of 20–70 nm. A number of irregular pores were embedded within the zirconia crystals. This unique structure was obtained due to the combination of sol–gel and hydrothermal treatments.     

Nanocrystalline sol–gel TiO2–SnO2 coatings: Preparation,characterization and photo-catalytic performance

In this study, preparation of SnO₂ (0–30 mol% SnO₂)–TiO₂ dip-coated thin films on glazed porcelain substrates via sol–gel process has been investigated. The effects of SnO₂ on the structural, optical, and photo-catalytic properties of applied thin films have been studied by X-ray diffraction, Raman spectroscopy, and scanning electron microscopy. Surface topography and surface chemical state of thin films were examined by atomic force microscopy and X-ray photoelectron spectroscopy. XRD patterns showed an increase in peak intensities of the rutile crystalline phase by increasing the SnO₂ content. The prepared Sn doped TiO₂ photo-catalyst films showed optical absorption in the visible light area exhibited excellent photo-catalytic ability for the degradation of methylene blue under visible light irradiation. Best photo-catalytic activity of Sn doped TiO₂ thin films was measured in the TiO₂–15 mol% SnO₂ sample by the Sn⁴⁺ dopants presented substitution Ti⁴⁺ into the lattice of TiO₂ increasing the surface oxygen vacancies and the surface hydroxyl groups.     

Preparation and characterization of Ba2TiSi2O8 ferroelectric films produced by sol–gel method

Fresnoite (Ba₂TiSi₂O₈, BTS) thin films were grown on polished Si(100) substrates by sol–gel method. The films were characterized using Fourier transform infrared spectroscopy (FTIR), Raman scattering spectroscopy, X-ray diffraction (XRD) and atom force microscopy (AFM). The results reveal that the crystallinity of fresnoite thin films increases and their structures become more compact as post-annealing temperature increases. Combined with XRD data, the strong FTIR peaks and Raman bands assigned to Ti–O and Si–O vibration indicate the formation of fresnoite phase in the films at a temperature of 750 °C. Besides, the AFM observation showed the films have a smooth surface, fine grains and dense structure.     

On the sol–gel synthesis and characterization of strontium ferrite ceramic material

A simple oxalate based sol–gel process has been described to produce a highly stable anion deficient strontium ferrite for separation of oxygen from air. The method involves metal nitrates and oxalic acid precursors with ethanol and water as solvents, gel formation, digestion for 4 h, drying at 150 °C for 24 h, and finally decomposition at 800 °C in air. The resulting material (i) exhibits a single perovskite-type cubic (SrFeO_3?ξ; ξ ～ 0.13) phase with a_o = 3.862 ± 0.002 Å, (ii) contains both the Fe⁴⁺ and Fe³⁺ species in 2.8:1 ratio, (iii) undergoes Fe⁴⁺ → Fe³⁺ reduction upon heating at 650 °C in rare gas ambient and transition to an orthorhombic phase with a ～ a_o√2, b ～ 4a_o, c ～ a_o√2, which reverts back to cubic phase with oxygen uptake at elevated temperatures, and (iv) acts as filter for air with excellent oxygen permeation, typical flux density value being 2.45 ml/cm² min at 1000 °C.     

Preparation of a hierarchically porous AlPO4 monolith via an epoxide-mediated sol–gel process accompanied by phase separation

Abstract

Monolithic aluminum phosphate (AlPO₄) with a macro–mesoporous structure has been successfully prepared via the sol–gel process accompanied by phase separation in the presence of poly(ethylene oxide) (PEO). Gelation of the system has been mediated by propylene oxide (PO), while PEO induces a phase separation. The dried gel is amorphous, whereas the crystalline tridymite phase precipitates upon heating above 1000 °C. Heat treatment does not spoil the macroporous morphology of the AlPO₄ monoliths. Nitrogen adsorption–desorption measurements revealed that the skeletons of the dried gels possess a mesostructure with a median pore size of about 30 nm and a surface area as high as 120 m² g^?1. Hydrothermal treatment before heat treatment can increase the surface area to 282 m² g^?1.     

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).     

Preparation of mullite fibres by sol–gel processes using aluminium carboxylates and tetraethylorthosilicate

Abstract

Mullite fibres were prepared using aluminium carboxylates (ACs) and tetraethylorthosilicate by sol–gel process. ACs were synthesised from dissolution aluminium in a mixture of formic acid and glacial acetic acid using aluminium chloride hexahydrate as catalyst. The optimum condition for obtaining ACs is as follows: the molar ratio of aluminium, formic acid and acetic acid was 1∶3∶2·26 and aluminium chloride hexahydrate was 10 wt-%. All the Al and Si components were mixed at the molecular level and linear molecules were formed in the precursor sol. The dried gel fibres completely transformed to mullite fibres at 1200°C and the calcinated fibres had a smooth surface and uniform diameter.     

Synthesis and characterization of superfine pure tetragonal nanocrystalline sulfated zirconia powder by a non-alkoxide sol–gel route

Nanocrystalline sulfated zirconia powder was prepared by a non-alkoxide sol–gel route using acidic condition (pH 1–2). The samples had superfine crystallites and pure tetragonal phase at 700 °C. Zr(acac)₄ was used as zirconium precursor due to a better retention of sulfate species and H₂SO₄ 0.5 M was used as sulfating agent. Fourier transform infrared (FT-IR) spectra have shown Zr–O–Zr and sulfate bonds. Crystal phase and crystallite size have been determined by X-ray Diffraction (XRD) analysis. Besides, the morphology of the samples has been investigated by field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). The optical properties of the samples have been analyzed using photoluminescence (PL) spectroscopy, too. All the analyses consistently have shown fairly uniform nanoparticles (calcined at 600 and 700 °C) with very small size and pure tetragonal phase with crystallite size between 5 and 10 nm.     

Synthesis of high purity hydroxyapatite nanopowder via sol–gel combustion process

A polymeric sol–gel combustion method has been used to synthesize nanocrystalline hydroxyapatite (HA) powder from calcium nitrate and triethyl phosphate with the addition of NH₄OH. The sol–gel combustion process generates phase-pure nanocrystalline HA powder, as characterized using Fourier transform infrared (FTIR), X-ray diffraction (XRD), and transmission electron microscopy (TEM). Sintering of the HA powder compact at 1200°C for 2 h leads to a 93% theoretical dense ceramic body. This method offers an easy route for the preparation of phase-pure nanocrystalline HA powder.