에탄올의 수분함량에 따라 합성된 Condensed Ethyl Silicate의 물성에 관한 연구

노재성; 홍성수; 서신석

Journal of the Korean Industrial and Engineering Chemistry, Vol.7, No.1, 91-100, February, 1996

Export Citation

에탄올의 수분함량에 따라 합성된 Condensed Ethyl Silicate의 물성에 관한 연구

A Study on the Properties of Condensed Ethyl Silicate Synthesized according to Water Contents in Ethanol

노재성, 홍성수, 서신석

초록

사염화실리콘에 에틸알콜의 수분함랑을 2.5, 5.0, 7.0wt.%로 달리하여 축중합된 에틸실리케이트(CES : condensed ethylsilicate)용액들을 합성하였다. 용액의 졸-겔 전이 거동 조사를 위하여 시간경과에 따른 용액의 부피, 밀도, SiO₂ 함량, 본성점도 및 수평균분자량변화를 측정하였으며, 용액의 고분자 형상을 본성점도와 수평균분자랑 관계로부터 간접적으로 알아보았다. 에틸알콜의 수분함량을 7.0wt.%로 하여 합성한 CES-3는 수분함량이 2.5wt.%, 5.0wt.%인 CES-1, CES-2와 다른 졸-겔 전이 거동을 보였으며, 복합산화물계 요업재료 제조시에 TEOS의 가수분해 속도를 조절하기위하여 부분가수분해 시킨 PHT(Partially Hydrolysed TEOS)와 유사한 거동을 보였다. Mark-Hawink가 제시한 [η]=KMn^α식에 의한 CES 및 PHT의 고분자형상은, 지수 α값이 0.53∼0.84로 용액 모두 선상 혹은 사슬상 고분자로 나타났으며, 이상의 졸-겔 거동과 고분자형상에 대한 비교 실험 결과로부터 CES-3는 PHT와 매우 유사한 물성을 가지고 있어 복합산화물계 요업재료의 원료로 사용될수 있는 가능성이 높은것으로 나타났다.

Condensed ethyl silicate(CES) solutions were prepared from SiCl₄ and ethanol which is different in water content(2.5, 5.0 and 7.0wt.% ). To investigate the sol-gel transition behaviors of CES and PHT(partially hydrolyzed TEOS) solutions, the measurement of volume change, density, SiO₂ content, intrinsic viscosity and number average molecular weight were conducted with elapsed time. The polymer shapes of CES were discussed from the relation between the intrinsic viscosity[η] and the number average molecular weight(Mn). CES-3 prepared from ethanol containing 7.0wt.% H₂O had different sol-gel transition behaviors from CES-1 (2.5wt.% H₂O) and CES-2(5.Owt.% H₂O), but similar behaviors to those of PHT which is used for controlling the hydrolysis rata of TEOS when composite ceramic materials were manufactured from silicon alkoxides. On the basis of Mark-Hawink relation, [η] = KMn^α, the polymer shape of CES solutions were determined linear siloxane polymers because all solutions had α values in the range from 0.53 to 0.84. Especially, CES-3 showed to be a favorable raw materials for composite ceramics due to its similar properties to those of PHT.

[References]

Bradley DC, Abdel Halim FM, Wardlaw W, J. Chem. Soc., 3450 (1950)
Bradley DC, Methrotra RC, Wardlaw W, J. Chem. Soc., 4204 (1952)
Bradley DC, Methrotra RC, Wardlaw W, J. Chem. Soc., 5020 (1952)
Kamiya K, Yoko T, Suzuki H, J. Non-Cryst. Solids, 93, 407 (1987)
노재성, 양현수, 조헌영, 요업재료의 과학과 기술, 8, 67 (1993)
Rho JS, Yang HS, Cho HY, Cho TW, J. Korean Ind. Eng. Chem., 4(2), 240 (1993)
노재성, 조헌영, 홍성수, 조태웅, 충남대학교 산업기술연구소 논문집, 8, 127 (1983)
Saito H, Suzuki H, Yogyo-Kyokai-Shi, 95, 697 (1987)
KleinLC, "Sol-Gel Technology for Thin Film, Fibers, Preforms, Electronics and Speciality Shapes," 50, Noyes Publications, New Jersey (1988)
Lentz CW, Inorg. Chem., 3, 574 (1968)
Currel BR, Parsonage JR, J. Macromol. Sci.-Chem., 16, 141 (1981)
Bogush GH, Tracy MA, J. Non-Cryst. Solids, 104, 95 (1988)
Murtagh MJ, Graham EK, J. Am. Ceram. Soc., 69, 775 (1986)
Brinker CJ, Keefer KD, Schaefer DW, Ashley CS, J. Non-Cryst. Solids, 48, 47 (1982)
Kamiya K, Yoko T, J. Mater. Sci., 21, 842 (1986)
Sakka S, Kamya K, J. Non-Cryst. Solids, 48, 31 (1982)
Huggins ML, J. Am. Chem. Soc., 64, 2716 (1942)
Budley WJ, Mark H, "High Molecular Weight Organic Compounds," R.E. Burk and O. Grunmitt, ed., Interscience Publisher, New York, 7 (1949)
Tsuchida H, "Science of Polymers," 85, Baihukan Publishing Company, Tokyo (1975)
Kamiya K, Yoko T, Sakka S, Yogyo-Kyokai-Shi, 92, 345 (1984)

[1] Bradley DC, Abdel Halim FM, Wardlaw W, J. Chem. Soc., 3450 (1950)

[2] Bradley DC, Methrotra RC, Wardlaw W, J. Chem. Soc., 4204 (1952)

[3] Bradley DC, Methrotra RC, Wardlaw W, J. Chem. Soc., 5020 (1952)

[4] Kamiya K, Yoko T, Suzuki H, J. Non-Cryst. Solids, 93, 407 (1987)

[5] 노재성, 양현수, 조헌영, 요업재료의 과학과 기술, 8, 67 (1993)

[6] Rho JS, Yang HS, Cho HY, Cho TW, J. Korean Ind. Eng. Chem., 4(2), 240 (1993)

[7] 노재성, 조헌영, 홍성수, 조태웅, 충남대학교 산업기술연구소 논문집, 8, 127 (1983)

[8] Saito H, Suzuki H, Yogyo-Kyokai-Shi, 95, 697 (1987)

[9] KleinLC, "Sol-Gel Technology for Thin Film, Fibers, Preforms, Electronics and Speciality Shapes," 50, Noyes Publications, New Jersey (1988)

[10] Lentz CW, Inorg. Chem., 3, 574 (1968)

[11] Currel BR, Parsonage JR, J. Macromol. Sci.-Chem., 16, 141 (1981)

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

[13] Murtagh MJ, Graham EK, J. Am. Ceram. Soc., 69, 775 (1986)

[14] Brinker CJ, Keefer KD, Schaefer DW, Ashley CS, J. Non-Cryst. Solids, 48, 47 (1982)

[15] Kamiya K, Yoko T, J. Mater. Sci., 21, 842 (1986)

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

[17] Huggins ML, J. Am. Chem. Soc., 64, 2716 (1942)

[18] Budley WJ, Mark H, "High Molecular Weight Organic Compounds," R.E. Burk and O. Grunmitt, ed., Interscience Publisher, New York, 7 (1949)

[19] Tsuchida H, "Science of Polymers," 85, Baihukan Publishing Company, Tokyo (1975)

[20] Kamiya K, Yoko T, Sakka S, Yogyo-Kyokai-Shi, 92, 345 (1984)