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

• Bulletin of the Korean Chemical Society
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• v.22 no.7
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• pp.678-684
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• 2001

Porous silica-pillared montmorillonites were prepared by simultaneous intercalation of dodecylamine-TEOS [tetraethylorthosilicate, Si(OC2H5)4] into the H-montmorillonite and intragallery amine-catalyzed hydrolysis of TEOS. Mixtures of the H-montmorillonite, dodecylamine and TEOS at molar ratios of 1 : 2 : 15-30 and 1 : 2-6 : 20 resulted to swollen and viscous gel once at room temperature, allowing intercalation compounds which dodecylamine and TEOS were simultaneously intercalated into interlayer of H-montmorillonite. The hydrolysis of the gallery TEOS was conducted in water solution for 40 min at room temperature, affording siloxane-pillared H-montmorillonite. Calcination of samples at 500 $^{\circ}C$ in air resulted in silica-pillared montmorillonite with large specific surface areas between 403 and 577 m2 /g, depending on the reaction stoichiometry. The reaction at H-montmorillonite : dodecylamine : TEOS reaction stoichiometries of 1 : 2 : 15 and 1 : 4 : 20 resulted in high specific surface areas and mesopores with a narrow pore size distribution. Result indicates that the intragallery-amine catalyze the hydrolysis of gallery-TEOS and simultaneously have a role of gallery-templated micellar assemblies.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.11 no.2
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• pp.67-70
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• 2001

Nanosize $SiO_2$composite particles have been synthesized within reverse micelle via metal alkoxide hydrolysis and condensation. The size of the particles can be controlled by manipulating the relative rates of the hydrolysis and condensation reactions of tetraethoxysilane (TEOS) within the microemulsion. The average size of synthesized particles was about in the size range 14~30nm. The effects of synthesis parameters, such as the molar ratio of water to TEOS, the molar ratio of water to surfactant, and the amount of base catalyst, are discussed.

• Applied Chemistry for Engineering
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• v.8 no.2
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• pp.301-307
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• 1997

Monodisperse, spherical $SiO_2/TiO_2$ composite fine powders were prepared by modified Sol-Gel process which $TiO_2$ fine Powders was used as a seed particles for condensation of TEOS (Tetraethyl Orthosilicate). The reaction was carried out under $N_2$ atmosphere at ambient temperature using $NH_3$ as a catalyst. Ethanol was used as a solvent. Drying process was carried out with vacuum trap which cooled by liquid $N_2$. The reaction variables were the concentration of TEOS, the concentration of ammonia, the size of $TiO_2$ seed and molar ratio of $SiO_2/TiO_2$. The optimum condition for the preparation of $SiO_2/TiO_2$ composite fine powders without agglomeration was [TEOS]=0.3M, [$NH_3$]=0.7M, size of $SiO_2/TiO_2$ seed = 200~300nm.

• Korean Journal of Materials Research
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• v.11 no.9
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• pp.740-744
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• 2001

The $Y_2SiO_5:Ce$ phosphors were synthesized by sol-gel technique in order to improve the performance of blue emitting phosphors for field emission display(FED). The resulted$Y_2SiO_5:Ce$ phosphors enhanced the emission intensity. In addition, calcination temperature of sol-gel technique(1300~140$0^{\circ}C$) was lower than that of the solid state reaction(>1$600^{\circ}C$). Under 365 nm and low voltage electron excitations. $Ce^{3+}$ -activated $Y_2SiO_5$phosphors showed blue emission band with a range of 400~ 430nm. Especially, 2mol% $Ce^{3+}$ doped $Y_2SiO_5:Ce$phosphors showed the maximum emission intensity. We have also controlled drying temperature of wet gel, pH, and $H_2O$/TEOS molar ratio for the optimum condition of TEOS hydrolysis.

• Journal of the Korean Ceramic Society
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• v.36 no.9
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• pp.893-900
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• 1999

Silica films were prepared on Si single crystal substrates by sol-gel process using TEOS as starting materials. Films were fabricated by a spin coating technique. Sol solutions were prepared by varying the compositions of CH3OH, H2O and DMF with fixed molar ratio of TEOS=1, HCl=0.05(mol). Wetting behavior viscosity of solutions gelation time thickness of films and cracking behavior were investigated with the various solution compositions. Wetting behaviors of solutions depended on the solution compositions mixing method and mixing rate. The optimum composition of sol was TEOS : DMF ; CH3OH: H2O :HCl=1:2:4:4:0.05(mol) and the mixing rate of solution was optimized at 1 ml/min. Viscosity of solutions were controlled by choosing a reaction time(elapsed time after mixing) at a room temperature so that we could get up to 800nm thick film The surface roughness was getting poor when thickness of films was thicker than 500nm. Thickness of coated films were increased with decreasing amount of CH3OH. The best surface roughness was obtained at the content of CH3OH 4 mol. The shortest gelation time was obtained with the content of CH3OH 8 mol. Crack-free filkms were fabricated when sintered at 500$^{\circ}C$ for 1 hr with heating rate of 0.6$^{\circ}C$/min.

• Applied Chemistry for Engineering
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• v.25 no.3
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• pp.286-291
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• 2014

In this study, nanosized TPA-silicalite-1 was synthesized with a suitable molar composition of TPAOH: $SiO_2$: $H_2O$ for the development of zeolite ceramic membranes to utilize as gas separation. As silica sources, TEOS, LUDOX AS-40 and CAB-O-SIL were used with the starting material of TPAOH. $NaH_2PO_4$, and a variety of acids and bases were used as promoters after TPAOH, $SiO_2$, $H_2O$ gel synthesis. To decrease synthesis time, a two step temperature change method was applied to the synthesis of TPA-silicalite-1 at a low temperature. TPA-silicalite-1 synthesized was analyzed with XRD, SEM, BET and TGA. As a result, TPA-silicalite-1 powders with a particle size of 100 nm and a specific surface area of $416m^2/g$ were obtained as optimum synthesis conditions when the two stage temperature change method was used with $NaH_2PO_4$ as promoter.

• Journal of the Korean Ceramic Society
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• v.28 no.5
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• pp.365-372
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• 1991

LAS (lithium aluminosilicate) sol was synthesized using the hydrolysis-condensation reaction of TEOS, chelated Al(OBus)3 and Li-salt with H2O in alcohol (EtOH+2-Propanol) medium. Effects of important reaction parameters on the properties of sol and gel-derived LAS were examined. The crystallization of the sol-gel derived LAS with ${\beta}$-spodumene composition began at ∼600$^{\circ}C$, and a series of polymorphic transformations occurred as temperature was increased to 1100$^{\circ}C$: amorphous LAS\longrightarrowhexagonal LiAl(SiO3)2\longrightarrow${\beta}$-spodumene. Lowering Li content in the gel enhanced densification and retarded the crystallization significantly. Optimum reaction conditions of LAS sol formation for thin coating applications were derived from rheological measurements, and these can be summarized as: H2O/total alkoxides molar ratio=4, pH=∼2.5, and aging time of ∼250h.

• Korean Journal of Materials Research
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• v.23 no.4
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• pp.246-249
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• 2013

Nano-sized ${\beta}$-SiC nanoparticles were synthesized combined with a sol-gel process and a carbothermal process. TEOS and carbon black were used as starting materials for the silicon source and carbon source, respectively. $SiO_2$ nanoparticles were synthesized using a sol-gel technique (Stober process) combined with hydrolysis and condensation. The size of the particles could be controlled by manipulating the relative rates of the hydrolysis and condensation reactions of tetraethyl orthosilicate (TEOS) within the micro-emulsion. The average particle size and morphology of synthesized silicon dioxide was about 100nm and spherical, respectively. The average particles size and morphology of the used carbon black powders was about 20nm and spherical, respectively. The molar ratio of silicon dioxide and carbon black was fixed to 1:3 in the preparation of each combination. $SiO_2$ and carbon black powders were mixed in ethanol and ball-milled for 12 h. After mixing, the slurries were dried at $80^{\circ}C$ in an oven. The dried powder mixtures were placed in alumina crucibles and synthesized in a tube furnace at $1400{\sim}1500^{\circ}C$ for 4 h with a heating rate of $10^{\circ}C$/min under flowing Ar gas (160 cc/min) and furnace cooling down to room temperature. SiC nanoparticles were characterized by XRD, TEM, and SAED. The XRD results showed that high purity beta silicon carbide with excellent crystallinity was synthesized. TEM revealed that the powders are spherical shape nanoparticles with diameters ranging from 15 to 30 nm with a narrow distribution.

• Journal of the Korean Ceramic Society
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• v.39 no.2
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• pp.113-119
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• 2002

The effect of ultrasonic radiation is reported for silica-poly(ethylene glycol) system prepared without the solvent using sol-gel processing by varying various parameters such as ultrasonic irradiation time, PEG content and HCl/TEOS molar ratio. The property of sonogel is compared with classic gel which has been prepared with ethanol as a solvent by traditional sol-gel processing. SEM, BET, DTA-TGA, density and Vickers hardness measurements are carried out for analyzing the samples. The gelation time is found strongly dependent on radiation time, PEG content and pH value, and has been discussed on the basis of existing theories. The $SiO_2-10$ & 20 wt% PEG sonogel exhibited superior optical, physical and gel properties as compared to the classic gel, hence, found suitable for device applications. The ultrasonic radiation increased the density and surface area, and also reduced the pore size which is well supported by the shift in the peak of DTA curve. The DTA thermogram was found similar to that of pure silica gel.