Sol-Gel Process를 이용한 PMSQ/TiO<SUB>2</SUB> 복합 미립자의 합성

이동현; 구상만

Journal of the Korean Industrial and Engineering Chemistry, Vol.9, No.5, 634-638, October, 1998

Export Citation

Sol-Gel Process를 이용한 PMSQ/TiO₂ 복합 미립자의 합성

Preparation of PMSQ/TiO₂ Composite Fine Powder by Sol-Gel Process

이동현, 구상만

초록

응집이 없는 단분산의 PMSQ/TiO₂ 복합 미립자를 얻기 위하여 300 nm 크기의 TiO₂ seed가 분산되어 있는 메탄올 수용액과 MTMS (Methyltrimethoxysilane)를 메탄올에 녹인 용액을 혼합하여 TiO₂ seed 표면에서 MTMS가 가수분해 및 축합 반응이 일어나도록 유도하여 복합 미분말을 제조하였다. 촉매로 암모니아를 사용하였고, 반응온도는 실온이었으며, 모든 반응은 질소분위기에서 행하였다. 교반속도, 반응온도, [H₂O]/[MTMS], [MTMS]/[TiO₂] 등을 변화하여 입자의 크기 및 형태에 영향을 주는 인자들을 조사한 결과, [MTMS]=0.2M, [NH₄OH]=0.6M, [H₂O]/[MTMS]=100, [MTMS]/[TiO₂]=10-50이고 실온에서 서서히 교반한 경우 단분산된 약 1-2μm의 크기를 갖는 복합입자를 얻을 수 있었다. 얻어진 입자에 대한 소수성을 물에 대한 접촉각 측정을 통해 조사한 결과 거의 180도에 가까운 접촉각을 보임으로써 복합입자의 소수성이 매우 뛰어남을 확인할 수 있었다. 자외선 차폐효과도 UV 투과도 측정을 통해 조사되었다.

Monodisperse, spherical PMSQ/TiO₂ composite fine powders were prepared by modified sol-gel process where 300 nm TiO₂ fine powders were used as seed particles for hetero-condensation with hydrolyzed MTMS (Methyltrimethoxysilane). The reaction was carried out under N₂ atmosphere at ambient temperature using NH₃ as a catalyst. Methanol was used as a solvent. Powder was obtained by the filtration of the solution with a glass filter and washing with acetone. The stirring rate, reaction temperature, [H₂O]/[MTMS] and [MTMS]/[TiO₂] ratio were varied to investigate shapes and sizes of particles. Monodisperse particles of 1-2 μm diameter were obtained with [MTMS]=0.2M, [NH₃]=0.6M, [H₂O]/[MTMS]=100, [MTMS]/[TiO₂]=10-50 at ambient temperature with mild stirring condition. These composite particles had a contact angle of almost 180 degree contact angle with water, which proves their excellent hydrophobicity. The study of UV absorption spectra showd that they have UV protecting effect.

Keywords:MTMS;Titania;Core-shell;Sol-gel Process;Composite Powder

[References]

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Hanch LL, West JK, "Chemical Processing of Advanced Materials," John Wiley & Sons, Inc. (1992)
Iler RK, "The Chemistry of Silica," John Wiley (1979)
Rahaman MN, "Ceramic Processing and Sintering," Marcel Dekker Inc. (1995)
Stber W, Fink A, Bohn E, J. Colloid Interface Sci., 26, 62 (1968)
Xu Q, Anderson MA, J. Am. Ceram. Soc., 77, 1939 (1994)
Sakka S, Kamiya K, Makita K, Yamamoto Y, J. Non-Cryst. Solids, 63, 223 (1984)
Jean JH, Ring TA, Langmuir, 2, 151 (1986)
Barringer EA, Bowen HK, Communication Am. Ceram. Soc., 199 (1982)
Look JL, Zukoski CF, J. Am. Ceram. Soc., 75, 1587 (1992)
Ying JY, Benziger JB, J. Am. Ceram. Soc., 76, 2571 (1993)
Ying JY, Benziger JB, J. Am. Ceram. Soc., 76, 2561 (1993)
Tan CG, Bowen BD, Epstein N, J. Colloid Interface Sci., 118 (1987)
Bogush GH, Zukoski CF, J. Colloid Interface Sci., 40, 1 (1991)
Bogush GH, Tracy MA, Zukoski CF, J. Non-Cryst. Solids, 104, 95 (1988)
Shimizu T, Okon T, Ohba T, Inokuchi Y, U.S. Patent, 5,149,748
Koo SM, Lee DH, Ryu CS, Lee YE, J. Korean Ind. Eng. Chem., 8(2), 301 (1997)
Yoldas BE, J. Non-Cryst. Solids, 38, 81 (1988)
Van Helden AK, Jansen JW, Vrij A, J. Colloid Interface Sci., 81, 354 (1981)
Hench LL, West JK, Chem. Rev., 90, 33 (1990)
Ogihara T, Nakajima H, Yanagawa T, Ogata N, Yoshida K, J. Am. Ceram. Soc., 74, 2263 (1991)
Linberg R, Sjblom J, Sundholm G, Colloids Surf. A: Physicochem. Eng. Asp., 99, 79 (1995)
Sakka S, Kamiya K, J. Non-Cryst. Solids, 48, 31 (1982)
van Blaadern A, Vrij A, J. Colloid Interface Sci., 156, 1 (1993)
Hyun SH, Kang BS, J. Am. Ceram. Soc., 77, 3093 (1994)
Hardy AB, Rhine WE, Bowen HK, J. Am. Ceram. Soc., 76, 97 (1993)
Shih WH, Kisailus D, Wei Y, Mater. Lett., 24, 13 (1995)
Yoldas BE, J. Mater. Sci., 21, 1080 (1986)
이동현, 석사학위논문, 한양대학교 (1997)
이상덕, 석사학위논문, 한양대학교 (1997)

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[2] Hanch LL, West JK, "Chemical Processing of Advanced Materials," John Wiley & Sons, Inc. (1992)

[3] Iler RK, "The Chemistry of Silica," John Wiley (1979)

[4] Rahaman MN, "Ceramic Processing and Sintering," Marcel Dekker Inc. (1995)

[5] Stber W, Fink A, Bohn E, J. Colloid Interface Sci., 26, 62 (1968)

[6] Xu Q, Anderson MA, J. Am. Ceram. Soc., 77, 1939 (1994)

[7] Sakka S, Kamiya K, Makita K, Yamamoto Y, J. Non-Cryst. Solids, 63, 223 (1984)

[8] Jean JH, Ring TA, Langmuir, 2, 151 (1986)

[9] Barringer EA, Bowen HK, Communication Am. Ceram. Soc., 199 (1982)

[10] Look JL, Zukoski CF, J. Am. Ceram. Soc., 75, 1587 (1992)

[11] Ying JY, Benziger JB, J. Am. Ceram. Soc., 76, 2571 (1993)

[12] Ying JY, Benziger JB, J. Am. Ceram. Soc., 76, 2561 (1993)

[13] Tan CG, Bowen BD, Epstein N, J. Colloid Interface Sci., 118 (1987)

[14] Bogush GH, Zukoski CF, J. Colloid Interface Sci., 40, 1 (1991)

[15] Bogush GH, Tracy MA, Zukoski CF, J. Non-Cryst. Solids, 104, 95 (1988)

[16] Shimizu T, Okon T, Ohba T, Inokuchi Y, U.S. Patent, 5,149,748

[17] Koo SM, Lee DH, Ryu CS, Lee YE, J. Korean Ind. Eng. Chem., 8(2), 301 (1997)

[18] Yoldas BE, J. Non-Cryst. Solids, 38, 81 (1988)

[19] Van Helden AK, Jansen JW, Vrij A, J. Colloid Interface Sci., 81, 354 (1981)

[20] Hench LL, West JK, Chem. Rev., 90, 33 (1990)

[21] Ogihara T, Nakajima H, Yanagawa T, Ogata N, Yoshida K, J. Am. Ceram. Soc., 74, 2263 (1991)

[22] Linberg R, Sjblom J, Sundholm G, Colloids Surf. A: Physicochem. Eng. Asp., 99, 79 (1995)

[23] Sakka S, Kamiya K, J. Non-Cryst. Solids, 48, 31 (1982)

[24] van Blaadern A, Vrij A, J. Colloid Interface Sci., 156, 1 (1993)

[25] Hyun SH, Kang BS, J. Am. Ceram. Soc., 77, 3093 (1994)

[26] Hardy AB, Rhine WE, Bowen HK, J. Am. Ceram. Soc., 76, 97 (1993)

[27] Shih WH, Kisailus D, Wei Y, Mater. Lett., 24, 13 (1995)

[28] Yoldas BE, J. Mater. Sci., 21, 1080 (1986)

[29] 이동현, 석사학위논문, 한양대학교 (1997)

[30] 이상덕, 석사학위논문, 한양대학교 (1997)