졸-겔법에 의한 티탄산바륨 제조에 관한 연구

황운연; 김용렬; Un-Yeon Hwangn; Yong-Ryul Kim

Korean Chemical Engineering Research, Vol.42, No.3, 338-344, June, 2004

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졸-겔법에 의한 티탄산바륨 제조에 관한 연구

Synthesis of BaTiO₃ Particles by Sol-Gel Method

황운연 ^†, 김용렬 ¹

서강대학교 화학공학과, 121-742 서울시 마포구 신수동 1
¹대진대학교 화학공학과, 487-711 경기도 포천시 선당동 11-1

Un-Yeon Hwangn^†, and Yong-Ryul Kim¹

Department of Chemical Engineering, Sogang University, 1, Sinsu-dong, Mapo-gu, Seoul 121-742, Korea
¹Department of Chemical Engineering, DaeJin University, 11-1, Sondan-dong, Poch´on, Kyonggi-do 487-711, Korea

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초록

본 연구에서는 졸-겔법을 이용하여 BaTiO₃미분체를 제조하였다. TIP에 비하여 약 4배 정도의 AcOH가 TIP분자 변형에 참가하였으며, 이와 같은 반응을 통하여 TIP의 배위체는 4에서 6으로 증가하였다. TIP와 AcOH의 반응에 의하여 생성된 티타닐아실레이트에 첨가된 물은 Ti와 monodentate로 결합되어 있던 이소프로필기를 제거하였다. Ba과 아세테이트 결합은 강염기 조건에서도 완전히 해리되지 않았으며, 따라서 최종 생성물에는 BaTiO₃상과 바륨 아세테이트와 유사한 구조를 갖는 제 2상이 공존하였다. 그리고 바륨 옥살레이트와 탄산칼륨이 중간상으로 존재하였다. [AcOH]/[TIP]의 비가 증가할수록 제조된 BaTiO₃의 결정성은 감소하였으며, 최종입자는 미세입자의 응집에 의하여 생성되었다.

In this study, spherical BaTiO₃ particles are prepared by sol-gel method. From fourier transform infrared analysis, it was found that a molar ratio of [AcOH]/[TIP] = 4 participated in TIP modification reaction and the coordination number of Ti increased to 6 by the modification reaction. Water added in the titanyl acylate removed the isopropyl groups bonded to titanium atoms by monodentate mode. From the FT-IR and XRD analysis for various solutions and barium acetate solid, it was found that Ba-OAc bonds are not readily removed even in a strong alkaline solution. BaTiO₃ and pseudo-barium acetate phases were found to coexist in as prepared powders. Barium oxalate and potassium carbonate intermediate phases formed during the thermal treatment of as-prepared powders due to decomposition of the pseudo-barium acetate phases. Crystallinity of BaTiO₃ particles decreased along with increasing [AcOH]/[TIP] ratio and the final powders were produced by aggregation of the fine particle.

Keywords:BaTiO₃;Sol-Gel Process;Barium Acetate;Alkoxide;Metal Alkoxide;Reaction Mechanism;Modification of Alkoxide

[References]

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Yoko T, Kamiya K, Tanaka K, J. Mater. Sci., 25, 3922 (1990)
Sharma HB, Mansingh A, J. Mater. Sci., 33(17), 4455 (1998)
Clark IJ, Takeuchi T, Ohtori N, Sinclair DC, J. Mater. Chem., 9, 83 (1999)
Ciftci E, Rahaman MN, Shumsky M, J. Mater. Sci., 36(20), 4875 (2001)
Hennings D, Schreinemacher S, J. Eur. Ceram. Soc., 9, 41 (1992)
Davies JA, Dutremez A, J. Am. Ceram. Soc., 73, 1429 (1990)
Bhattacharjee S, Paria MK, Maiti SH, Ceram. Int., 18, 295 (1992)
Her YS, Matijevic E, Chon MC, J. Mater. Res., 11, 3121 (1996)
Gherardi P, Matijevic E, Colloids Surf., 32, 257 (1988)
Phule PP, Risbud SH, J. Mater. Sci., 25, 1169 (1990)
Cho WS, J. Phys. Chem. Solids, 59, 659 (1998)
Kao CF, Yang WD, Mater. Sci. Eng. B, 38, 127 (1996)
Doeuff S, Henry M, Sanchez C, Livage J, J. Non-Cryst. Solids, 89, 206 (1987)
Nakamoto K, "Infrared and Raman Spectra of Inorganic and Coordination Compounds," 5th ed, Wiley Press: New York (1997)
Brakley DC, Mehrotra RC, Gaur DP, "Metal Alsoxides," Academic Press, New York (1978)
Niyogi DD, Singh S, Saini A, Verma RD, J. Fluor. Chem., 66, 153 (1994)
Yoko T, Kamiya K, Tanaka K, J. Mater. Sci., 25, 3922 (1990)
Mosset A, Gautier-Luneau I, Galy L, J. Non-Cryst. Solids, 100, 339 (1988)
Lambert JB, Shurvell HF, Lightner D, Cooks RG, "Introduction to Organic Spectroscopy," New York: Macmillan, 175 (1987)
Nyquist RA, Putzig CL, Leugers MA, "Handbook of Infrared and Raman Spectra of Inorganic Compounds and Organic Salt," Vol. 4, Academic Press, 257 (1996)
Cho WS, J. Phys. Chem. Solids, 59, 659 (1998)
Kumar S, Messing GL, White WB, J. Am. Ceram. Soc., 76, 617 (1993)

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[1] Kim SW, Lee MH, Noh TY, Lee C, J. Mater. Sci., 31(14), 3643 (1996)

[2] Yoko T, Kamiya K, Tanaka K, J. Mater. Sci., 25, 3922 (1990)

[3] Sharma HB, Mansingh A, J. Mater. Sci., 33(17), 4455 (1998)

[4] Clark IJ, Takeuchi T, Ohtori N, Sinclair DC, J. Mater. Chem., 9, 83 (1999)

[5] Ciftci E, Rahaman MN, Shumsky M, J. Mater. Sci., 36(20), 4875 (2001)

[6] Hennings D, Schreinemacher S, J. Eur. Ceram. Soc., 9, 41 (1992)

[7] Davies JA, Dutremez A, J. Am. Ceram. Soc., 73, 1429 (1990)

[8] Bhattacharjee S, Paria MK, Maiti SH, Ceram. Int., 18, 295 (1992)

[9] Her YS, Matijevic E, Chon MC, J. Mater. Res., 11, 3121 (1996)

[10] Gherardi P, Matijevic E, Colloids Surf., 32, 257 (1988)

[11] Phule PP, Risbud SH, J. Mater. Sci., 25, 1169 (1990)

[12] Cho WS, J. Phys. Chem. Solids, 59, 659 (1998)

[13] Kao CF, Yang WD, Mater. Sci. Eng. B, 38, 127 (1996)

[14] Doeuff S, Henry M, Sanchez C, Livage J, J. Non-Cryst. Solids, 89, 206 (1987)

[15] Nakamoto K, "Infrared and Raman Spectra of Inorganic and Coordination Compounds," 5th ed, Wiley Press: New York (1997)

[16] Brakley DC, Mehrotra RC, Gaur DP, "Metal Alsoxides," Academic Press, New York (1978)

[17] Niyogi DD, Singh S, Saini A, Verma RD, J. Fluor. Chem., 66, 153 (1994)

[18] Yoko T, Kamiya K, Tanaka K, J. Mater. Sci., 25, 3922 (1990)

[19] Mosset A, Gautier-Luneau I, Galy L, J. Non-Cryst. Solids, 100, 339 (1988)

[20] Lambert JB, Shurvell HF, Lightner D, Cooks RG, "Introduction to Organic Spectroscopy," New York: Macmillan, 175 (1987)

[21] Nyquist RA, Putzig CL, Leugers MA, "Handbook of Infrared and Raman Spectra of Inorganic Compounds and Organic Salt," Vol. 4, Academic Press, 257 (1996)

[22] Cho WS, J. Phys. Chem. Solids, 59, 659 (1998)

[23] Kumar S, Messing GL, White WB, J. Am. Ceram. Soc., 76, 617 (1993)