졸겔공정에서 유기첨가제가 도입된 루타일 티타니아의 저온합성

오경석; 양재춘; 정경택; 최승철; 설용건

HWAHAK KONGHAK, Vol.33, No.5, 544-550, October, 1995

Export Citation

졸겔공정에서 유기첨가제가 도입된 루타일 티타니아의 저온합성

Low Temperature Synthesis of Rutile TiO₂ in Sol-Gel with Organic Additives

오경석, 양재춘, 정경택, 최승철, 설용건

초록

본 실험에서는 핵실렌 클리콜(HG)을 첨가하여 티타니아 겔(HG-TiO₂)을 제조하였다. 가수분해후에 얻어진 티타니아 겔(HG-TiO₂)은 밀폐된 로에서 열처리한 결과 루타일로의 상전이가 600℃부근의 저온에서 일어났다. 유기물 분해에 유리한 산소흐름 분위기하에서 충진형 관반응기로 열처리했을 때는 300℃에서도 완전한 루타일로의 상전이됨을 확인하였다. HG는 TEOT와bidentate 리간드 구조를 갖게 되고 가수분해후에도 결합이 유지됨을 FT-IR로 알 수 있었다. 또한 bidentate 리간드 구조가 가능한 에틸렌 글리콜, 아세트산, 에틸렌 디아민과 에틸 아세토아세테이트를 첨가하여 제조된 티타니아 겔을 충진반응기롤 산화분위기하의 열처리를 통해 300℃에서 루타일로의 상전이가 지배적임을 확인하였다.

Titania gel(HG-TiO₂) was prepared by the addition of hexylene glycol in sol-gel process. HG-TiO₂ gel after hydrolysis reaction showed rutile phase transformation at low temperature(600℃)under air atmosphere in a closed furnace. To promote the decomposition of organic additives incorporated into titania gel structure, packed bed reaction system with oxygen flow was attempted and the rutile phase was found at 300℃ which is lower than that of closed system. HG incorporation into TEOT was identified by using FT-IR. From the spectra, the bidentate ligand between TEOT and hexylene glycol was identified after hydrolysis reaction as well as before the TEOT hydrolysis reaction. To confirm the effect of bidentate ligand in titania gel, ethylene glycol, acetic acid, ethylenediamine and ethyl acetoacetate were added to TEOT and the rutile transformation was also confirmed at 300℃.

[References]

Yoldas BE, J. Mater. Sci., 21, 1087 (1986)
Yoldas BE, J. Am. Ceram. Soc., 65, 387 (1982)
Brinker CJ, Scherer GW, "Sol-Gel Science," Academic Press (1990)
Ulrich DR, J. Non-Cryst. Solids, 100, 174 (1988)
Pugh RJ, Bergstrom L, "Surface and Colloid Chemistry in Advanced Ceramics Processing," Marcel Dekker, Inc., New York (1994)
Jean J, Ring TA, J. Am. Ceram. Soc., 65, 1574 (1986)
Sanchez C, Livage J, Henry M, Babbnneau F, J. Non-Cryst. Solids, 100, 65 (1988)
Livage J, Mater. Res. Soc. Symp. Proc., 73, 717 (1986)
Iida Y, Ozaki S, J. Am. Ceram. Soc., 44, 120 (1961)
Mackenzie KJD, Melling PJ, Trans. J. Br. Ceram. Soc., 73, 179 (1974)
Takahashi Y, Matsuoka Y, J. Mater. Sci., 23, 2259 (1988)
Spurr RA, Myers H, Anal. Chem., 29, 760 (1957)
Ocana M, Garcia J, Serna C, J. Am. Ceram. Soc., 75, 2010 (1992)
Yamamoto A, Kambara S, J. Am. Chem. Soc., 81, 2663 (1959)
Larbot A, Laaziz I, Marignan J, Quinson J, J. Non-Cryst. Solids, 147-148, 157 (1992)
Bardley D, Mehrotra R, Gaur D, "Metal Alkoxide," Academic Press, 183-185 (1978)
Nakamoto K, "Infrared and Raman Spectra of Inorganic and Coordination Compounds," 3rd ed., John Wiley & Sons, New York (1978)
Tadanaga K, Iwami T, Tohge N, Minami T, J. Sol-Gel Sci. Tech., 3, 5 (1994)

[Referenced By]

[1] Yoldas BE, J. Mater. Sci., 21, 1087 (1986)

[2] Yoldas BE, J. Am. Ceram. Soc., 65, 387 (1982)

[3] Brinker CJ, Scherer GW, "Sol-Gel Science," Academic Press (1990)

[4] Ulrich DR, J. Non-Cryst. Solids, 100, 174 (1988)

[5] Pugh RJ, Bergstrom L, "Surface and Colloid Chemistry in Advanced Ceramics Processing," Marcel Dekker, Inc., New York (1994)

[6] Jean J, Ring TA, J. Am. Ceram. Soc., 65, 1574 (1986)

[7] Sanchez C, Livage J, Henry M, Babbnneau F, J. Non-Cryst. Solids, 100, 65 (1988)

[8] Livage J, Mater. Res. Soc. Symp. Proc., 73, 717 (1986)

[9] Iida Y, Ozaki S, J. Am. Ceram. Soc., 44, 120 (1961)

[10] Mackenzie KJD, Melling PJ, Trans. J. Br. Ceram. Soc., 73, 179 (1974)

[11] Takahashi Y, Matsuoka Y, J. Mater. Sci., 23, 2259 (1988)

[12] Spurr RA, Myers H, Anal. Chem., 29, 760 (1957)

[13] Ocana M, Garcia J, Serna C, J. Am. Ceram. Soc., 75, 2010 (1992)

[14] Yamamoto A, Kambara S, J. Am. Chem. Soc., 81, 2663 (1959)

[15] Larbot A, Laaziz I, Marignan J, Quinson J, J. Non-Cryst. Solids, 147-148, 157 (1992)

[16] Bardley D, Mehrotra R, Gaur D, "Metal Alkoxide," Academic Press, 183-185 (1978)

[17] Nakamoto K, "Infrared and Raman Spectra of Inorganic and Coordination Compounds," 3rd ed., John Wiley & Sons, New York (1978)

[18] Tadanaga K, Iwami T, Tohge N, Minami T, J. Sol-Gel Sci. Tech., 3, 5 (1994)