• 한국세라믹학회지
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• 제34권2호
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• pp.216-224
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• 1997

TEOS와 에탄올의 양을 고정하고 H2O/TEOS의 몰비가 2.6-59.0이 되는 범위에서 염산촉매를 사용하여 다공성 실리카 세라믹을 제조하였다. 서로 다른 조성의 솔 9종을 만든 후 젤화시간 측정, TG/DTA에 의한 건조시료의 열분석 및 FT-IR과 X-ray diffractometer에 의한 중간생성물의 특성분석을 수행하였고 50$0^{\circ}C$까지 열처리한 시료의 FT-IR에 의한 SiO2폴리머 분석, N2-adsorption isotherm을 이용한 비표면적과 기공크기분포 조사 및 TEM에 의한 SiO2폴리머의 형태와 기공의 변화를 조사하였다. 적용된 조성 및 촉매의 농도에서 최소 젤화반응시간은 TEOS1몰달 물의 양이 약 11몰에서, 가장 높은 중합도는 약 8-18몰에서, 그리고 가장 큰 비표면적값은 약 11몰에서 보였다. 이것은 물의 양이 약 11몰일 때 중합반응이 가장 빠르게 진행하였음을 의미한다. 결론적으로, 물의 양이 증가함에 따라서 약 11몰까지는 반응이 빠르게 진행되나 그 이상의 물이 사용될 경우 과잉의 물이 반응저해요인으로 작용하여 젤화시간의 지연 및 비표면적의 감소를 보인다.

• Bulletin of the Korean Chemical Society
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• 제22권7호
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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.

• 한국결정성장학회지
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• 제11권2호
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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.

• 공업화학
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• 제8권2호
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• pp.301-307
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• 1997

응집이 없는 단분산의 $SiO_2/TiO_2$ 복합 미립자를 얻기 위하여 $TiO_2$seed가 분산되어 있는 에탄올 수용액과 TEOS (Tetraethyl Orthosilicate)를 에탄올에 녹인 용액을 혼합하여 $TiO_2$ 주위에서 TEOS가 가수분해 및 축합 반응이 일어나도록 유도하여 복합 미분말을 제조하였다. 촉매로 암모니아를 사용하였고, 반응온도는 실온이었다. 반응변수는 TEOS의 농도, 암모니아의 농도, $TiO_2$ seed의 크기 및 양이었다. 응집이 없는 복합 미립자를 얻기 위한 최적조건은 [TEOS]=0.3M, [$NH_4OH$]=0.7M, $TiO_2$ seed의 크기가 200~300 nm이었고, 이때 $0.8{\sim}0.9{\mu}m$의 입자크기를 갖는 복합입자를 얻을 수 있었다.

• 한국재료학회지
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• 제11권9호
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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.

• 한국세라믹학회지
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• 제36권9호
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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.

• 공업화학
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• 제25권3호
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• pp.286-291
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• 2014

본 연구에서는 기체 분리를 위한 제올라이트 세라믹 멤브레인 제조에 적합한 입자크기와 형상을 갖춘 나노크기의 제올라이트를 TPAOH : $SiO_2$ : $H_2O$의 적합한 조성으로 합성하였으며 그 특성을 분석하였다. 실리카 원으로는 TEOS, LUDOX AS-40, CAB-O-SIL을 사용하고, TPAOH와 함께 출발물질로 하여 특정 조성의 TPAOH, $SiO_2$, $H_2O$ gel을 합성하고, $NaH_2PO_4$ 및 다양한 산 염기를 결정화 촉진제로 사용하였다. 합성시간을 단축할 수 있는 방법의 일환으로 저온에서 2단계 온도 변화법을 적용한 수열합성법으로 TPA-Silicalite-1을 합성하였으며 XRD, SEM, BET, TGA 등을 사용하여 분석하였다. 그 결과, 2단계 온도 변화법을 사용하고, 결정화 촉진제로서 $NaH_2PO_4$를 사용하였을 때가 최적의 합성 조건으로 입자크기100 nm, 비표면적 $416m^2/g$의 TPA-Silicalite-1 분말을 제조할 수 있었다.

• 한국세라믹학회지
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• 제28권5호
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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.

• 한국재료학회지
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• 제23권4호
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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.

• 한국세라믹학회지
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• 제39권2호
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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.