• Korean Journal of Materials Research
• /
• v.9 no.8
• /
• pp.804-809
• /
• 1999

Silica films were prepared on Si single crystal substrates by a sol-gel process without DMF using TEOS as a starting material. Films were fabricated by spin coating technique. For films having a composition of TEOS : HCI(1:0.05mol), gelation time, the thickness of films, the formation of cracks and the microstructure of the films were investigated as a function of the molar ratio of $CH_3OH and H_2O$. With 8mol $CH_3OH$, the longest gelation time was measured to be 640hr. The thickness of the coated films was decreased with increasing content of $CH_3OH$. The films were sintered at $500^{\circ}C$ for 1hr with a heating rate of $0.6^{\circ}C$/min. The coated films showed worm-like grains and partially cracked microstructures at an amount of $CH_3OH$ 2mol and 4mol. The addition of more than 8 mole of $CH_2OH$ resulted in crack-free silica films. This suggests that crack-free films can be fabricated by controlling the surface tension energy of the sol solutions without DMF.

• Korean Chemical Engineering Research
• /
• v.45 no.6
• /
• pp.611-618
• /
• 2007

We demonstrate the sol-gel coating technique of colloidal clusters for producing hollow micro-particles with complex morphologies. Cross-linked amidine polystyrene (PS) microspheres were synthesized by emulsifier-free emulsion copolymerization of styrene and divinylbenzene. The amidine PS particles were self-organized inside toluene-in-water emulsion droplets to produce large quantities of colloidally stable clusters. These clusters were coated with thin silica shell by sol-gel reaction of tetraethylorthosilicate (TEOS) and ammonia, and the organic polystyrene cores were removed by calcination at high temperature to generate nonspherical hollow micro-particles with complex morphologies. This process can be used to prepare hollow particles with shapes such as doublets, tetrahedra, icosahedra, and others.

• Journal of the Korean Ceramic Society
• /
• v.34 no.2
• /
• pp.216-224
• /
• 1997

Porous silica ceramics were prepared(with HCI catalyst) using H2O/TEOS molar ratios of 2.6~59.0, with the EtOH/TEOS ratio fixed. After preparing 9 kinds of sol, the followings were investigated; measurement of the gelation time, thermal analyses by TG/DTA, property analyses of the intermediates by FT-IR and X-ray diffractometry with dried samples, analyses of SiO2 polymer by FT-IR, the investigation of specific sur-face area and pore size distribution by N2-adsorption isotherm, and structural change of SiO2 polymer and pore morphology by TEM observation, with samples heat-treated to 50$0^{\circ}C$. In the concentrations of in-vestigated compositions and catalyst, gelation time showed a minimum at ca. 11 moles of water per one mole of TEOS, the highest degree of polymerization at ca. 8-18 moles, and the largest specific surface area at ca. 11 moles, which means that the polymerization proceeded fastest at ca. 11 moles of water. In con-clusion, the more water used, the faster the polymerization reaction up to ca. 11 moles, but more than ca. 11 moles of water caused retardation of gelation and resultant reduction of specific surface area.

• Polymer(Korea)
• /
• v.29 no.2
• /
• pp.156-160
• /
• 2005

$\alpha,\omega-Vinyl$ poly (dimethyl-methylphenyl) siloxane prepolymer (VPMPS ) was prepared by the equilibrium polymerization of octamethylcyclotetrasiloxane $(D_4)$, 1,3,5-trimethyl-1,3,5-triphenylcyclotrisiloxane $(D_3^{Me,Ph)$, and 1,1,3,3-tetramethyl-1,3-divinyldisiloxane (MVS). And also, of $\alpha,\omega-hydrogen$ poly(dimethyl-methyl)siloxane prepolymer (HPDMS) as end blocker was prepared from octamethylcyclotetrasiloxane $(D_4)$, 1,3,5-trimethylcyclotrisiloxane $(D_3^:Me,H})$, and 1,1,3,3-tetramethyldisiloxane (MS). Nickel ferrite nanoparticles having spinel magnetic material was prepared by the sol-gel method using PAA as a chelating agent. Poly(organosiloxane) rubber nanocomposite containing silica and nickel ferrite ultrafine powder modified with 1,3-divinyltetramethyldisilazane (VMS) was prepared by compounding VPMPS, HPDMS, and catalyst in high speed dissolver. The mechanical properties, heat dissipating away characteristics, and volume resistivities for POX-30 and POX-50 were measured.

• Korean Chemical Engineering Research
• /
• v.48 no.3
• /
• pp.332-336
• /
• 2010

Ionic liquid immobilized on mesoporous amorphous silica was prepared from the coupling of 1-(triethoxysilylpropyl)-3-n-alkyl-imidzolium halides with tetraethyl orthosilicate(TEOS) through template-free condensation under strong acidic conditions. The immobilized 1-n-butyl-3-methyl imidazolium bromide ionic liquid on amorphous silica(BMImBr-AS) was proved to be an effective heterogeneous catalyst for the synthesis of dimethyl carbonate(DMC) from transesterification of ethylene carbonate(EC) with methanol. High temperature, high carbon dioxide pressure and long reaction time were favorable for the reactivity of BMImBr-AS. Kinetic studies based on two step reactions revealed that the proposed reaction model fitted well the experimental data. The apparent activation energy was estimated to be 67.4 kJ/mol.