졸-겔법에 의한 mullite합성시 건조 첨가제가 건조 및 소성에 미치는 영향

함영민; 홍영호; 최승일

Journal of the Korean Industrial and Engineering Chemistry, Vol.4, No.3, 497-504, September, 1993

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졸-겔법에 의한 mullite합성시 건조 첨가제가 건조 및 소성에 미치는 영향

Effects of Drying Agents on the Drying and Calcination in Synthesis of Mullite by Sol-Gel Process

함영민, 홍영호, 최승일

초록

본 연구는 고온 구조재료 및 전자재료로 주목받고 있는 복합산화물인 mullite(3Al₂O₃·2SiO₂)를 금속알콕사이드에 의한 졸-겔법으로 합성함에 있어서 재활용품으로서의 aluminium foil을 aluminium 금속원으로 사용하여 알루미늄 알콕사이드를 제조하고 Si(OC₂H₅)₄와 혼합하여 가수분해 단계에서 건조조절화학첨가제(Drying Control Chemical Additives, DCCA)를 첨가함으로써 건조시간을 단축시키려는 시도를 하였으며 이러한 DCCA가 mullite 물성에 어떠한 영향을 주는지 검토하고자 하였다. 이때 DCCA로 N, N-dimethyl formamide (DMF), Glycerol, 1, 4-Dioxane과 Oxalic acid가 첨가되었으며 건조된 겔을 각 온도별로 소성하여 TG-DTA, FT-IR, XRD 및 SEM을 사용하여 결정의 전이과정 및 각 소성온도에서의 결정상태 등을 관찰하였다. DCCA를 첨가하여 건조시킨 결과 0.1mole의 DMF를 첨가하였을 경우 DCCA를 첨가하지 않았을 때보다 건조시간이 1/2 정도 단축되었으며 분석결과 mullite의 결정형성에 큰 영향을 미치지 않았음을 확인하였다.

The effect of DCCA (Drying Control Chemical Additives) on the drying of gel was investigated in order to determine an optimum drying condition of mullite precursor through sol-gel process. Aluminium sec-butoxide was synthesized from aluminium foil and then mullite powders were synthesized from Tetra-ethyl-ortho-silicate (TEOS) and the aluminium sec-butoxide. N, N-dimethyl formamide (DMF), Glycerol, 1, 4-Dioxane, and Oxalic acid were used as DCCA. Mullite powders that were calcined at 200, 900, 1100, and 1250℃ for 2hr were analysed by XRD, TG-DTA, FT-IR, and SEM in order to investigate structural change and characteristics of calcined powders. The results of this work showed that the drying time of gel was reduced to about half in the presence of 0.1mol DMF compared with the absence of DCCA and also calcined powders were obtained without remarkable structural change despite of the addition of DCCA.

[References]

Brindley GW, Nakahira M, J. Am. Ceram. Soc., 42, 311 (1959)
Chakravorty AK, Ghosh DK, J. Am. Ceram. Soc., 71, 978 (1988)
Kanzanki S, Tabata H, J. Am. Ceram. Soc., 68, C6 (1985)
Komaneri S, Suwa Y, Roy R, J. Am. Ceram. Soc., 69, C155 (1986)
Pask JA, Zhang XW, Tomsia AP, Yoldas BE, J. Am. Ceram. Soc., 70, 704 (1987)
Ismail MGMU, Nasaki Z, Somiya S, J. Am. Ceram. Soc., 70, C7 (1987)
Rahaman MN, DeJonghe LC, Shinde SL, Tewari PH, J. Am. Ceram. Soc., 71, C338 (1988)
Tucker DS, Sparks JS, Esker DC, J. Am. Ceram. Bull., 69, 1971 (1990)
Sakka S, J. Non-Cryst. Solids, 73, 651 (1985)
Sakka S, Kamiya K, J. Non-Cryst. Solids, 48, 31 (1982)
Wilson G, Heathcote R, J. Am. Ceram. Bull., 69, 1137 (1990)
Hench LL, Ulrich DR, "Science of Ceramic Chemical Processing," John Wiley and Sons, New York, 52 (1986)
Adachi T, Sakka S, J. Non-Cryst. Solids, 99, 118 (1988)
Wolfrum SM, J. Mater. Sci. Lett., 6, 706 (1987)
Scherer GW, J. Non-Cryst. Solids, 107, 135 (1989)
Kim CE, J. Korean Ceram. Soc., 25, 585 (1988)
Mackenzie KJD, J. Am. Ceram. Soc., 55, 68 (1972)
Low IM, Mcpherson R, J. Mater. Sci., 24, 926 (1989)
Hoffman DW, Roy R, Komaneri S, J. Am. Ceram. Soc., 67, 468 (1984)

[Referenced By]

[1] Brindley GW, Nakahira M, J. Am. Ceram. Soc., 42, 311 (1959)

[2] Chakravorty AK, Ghosh DK, J. Am. Ceram. Soc., 71, 978 (1988)

[3] Kanzanki S, Tabata H, J. Am. Ceram. Soc., 68, C6 (1985)

[4] Komaneri S, Suwa Y, Roy R, J. Am. Ceram. Soc., 69, C155 (1986)

[5] Pask JA, Zhang XW, Tomsia AP, Yoldas BE, J. Am. Ceram. Soc., 70, 704 (1987)

[6] Ismail MGMU, Nasaki Z, Somiya S, J. Am. Ceram. Soc., 70, C7 (1987)

[7] Rahaman MN, DeJonghe LC, Shinde SL, Tewari PH, J. Am. Ceram. Soc., 71, C338 (1988)

[8] Tucker DS, Sparks JS, Esker DC, J. Am. Ceram. Bull., 69, 1971 (1990)

[9] Sakka S, J. Non-Cryst. Solids, 73, 651 (1985)

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

[11] Wilson G, Heathcote R, J. Am. Ceram. Bull., 69, 1137 (1990)

[12] Hench LL, Ulrich DR, "Science of Ceramic Chemical Processing," John Wiley and Sons, New York, 52 (1986)

[13] Adachi T, Sakka S, J. Non-Cryst. Solids, 99, 118 (1988)

[14] Wolfrum SM, J. Mater. Sci. Lett., 6, 706 (1987)

[15] Scherer GW, J. Non-Cryst. Solids, 107, 135 (1989)

[16] Kim CE, J. Korean Ceram. Soc., 25, 585 (1988)

[17] Mackenzie KJD, J. Am. Ceram. Soc., 55, 68 (1972)

[18] Low IM, Mcpherson R, J. Mater. Sci., 24, 926 (1989)

[19] Hoffman DW, Roy R, Komaneri S, J. Am. Ceram. Soc., 67, 468 (1984)