반응매개체로 사용한 염산과 반응시간이 TiO<sub>2</sub> 분말제조에 미치는 영향

이정훈; 양영석; Jeong Hoon Lee; Yeong Seok Yang

Journal of the Korean Industrial and Engineering Chemistry, Vol.14, No.2, 224-229, April, 2003

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반응매개체로 사용한 염산과 반응시간이 TiO₂ 분말제조에 미치는 영향

Effect of HCl Used as Reaction Medium and Reaction Time on the Synthesis of Titanium Dioxide Powder

이정훈, 양영석 ^†

우석대학교 화학공학과, 전북 561-701

Jeong Hoon Lee, and Yeong Seok Yang^†

Department of Chemical Engineering, Woosuk University, Wan-ju, Jeon-buk 561-701, Korea

E-mail:

초록

다양한 농도의 염산으로 제조한 TiOCl₂ 수용액으로부터 반응시간에 따라 침전반응으로 TiO₂를 제조하였다. 1.0 M과 4.0 M 염산을 사용하여 얻은 분말의 결정구조는 순수한 루틸상이고, 2.0 M ~ 3.5 M에서는 브루카이트상과 루틸상의 혼합상이 생성되었다. 브루카이트상이 지배적인 결정구조를 이루는 TiO₂ 제조를 위한 용액의 적정 Cl^-1_total: Ti⁺⁴의 비율이 존재하며, TiOCl₂ 수용액의 Ti⁺⁴농도가 증가할수록 브루카이트상이 생성되기 위한 Cl^-1_total: Ti⁺⁴의 비율이 감소하였다. 브루카이트상 TiO₂는 반응시간의 증가에 따라 루틸상으로 직접 상변화가 진행되었다. 또한, 염산농도가 증가할수록 Ti⁺⁴이 TiO₂로 전환되는데 필요한 산소의 공급원인 H₂O의 양이 상대적으로 작아서 침전반응이 느리게 진행되었으며, 생성효율의 증가를 위해서는 반응시간의 증가가 필요하였다.

TiO₂ was synthesized by precipitation from aqueous TiOCl₂ solution, which was prepared by using HCl at various concentrations and reaction time. Pure rutile type TiO₂ was obtained when the concentration of HCl solution was 1.0 M and 4.0 M, while a mixture of rutile and brookite was obtained at 2.0 ~ 3.5 M HCl. There was optimum ratio of Cl^-1_total: Ti⁺⁴ in obtaining brookite-type TiO₂, and the ratio decreased with increased Ti⁺⁴ concentration. The bookite transformed directly to rutile phase with increase of the reaction time only. The precipitation was delayed with increase of HCl concentration because the amount of H₂O, which in necessary for the conversion of Ti⁺⁴ to TiO₂, was relatively reduced. Therefore, in order to increase the productive efficiency it was required longer reaction time.

Keywords:TiCl₄;TiO₂;brookite;precipitation;HCl

[References]

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Pottier A, Chaneac C, Tronc E, Mazerolles L, Jolivet J, J. Mater. Chem., 11, 1116 (2001)
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[1] Zheng Y, Shi E, Chen Z, Li W, Hu X, J. Mater. Chem., 11, 1547 (2001)

[2] Pottier A, Chaneac C, Tronc E, Mazerolles L, Jolivet J, J. Mater. Chem., 11, 1116 (2001)

[3] Kim SJ, Park SD, Jeong YH, J. Am. Ceram. Soc., 82(4), 927 (1999)

[4] Gao L, Zhang Q, Mater. Trans., 42(8), 1676 (2001)

[5] Wang CC, Ying JY, Chem. Mater., 11(11), 3113 (1999)

[6] Nam HD, Lee BH, Kim SJ, Jung CH, Lee JH, Park SD, Jpn. J. Appl. Phys., 37, 4603 (1998)

[7] Park SD, Cho YH, Kim WW, Kim SJ, J. Solid State Chem., 146, 230 (1999)

[8] Zhang Q, Gao L, Guo J, J. Eur. Ceram. Soc., 20, 2153 (2000)

[9] Yang J, Mei S, Ferreira JM, J. Am. Ceram. Soc., 83(6), 1361 (2000)

[10] Ye X, Sha J, Jiao Z, Zhang L, Nanostructure Mater., 8(7), 919 (1997)

[11] Kominami H, Kohno M, Kera Y, J. Mater. Chem., 10, 1151 (2000)

[12] Tompsett GA, Bowmaker GA, Cooney RP, Metson JB, Rodgers KA, SEakins JM, J. Raman Spectroscopy., 26, 50 (1995)

[13] Zheng YQ, Erwei S, Cui SX, Li WJ, Hu XF, J. Mater. Sci. Lett., 19(16), 1445 (2000)

[14] Cheng H, Ma J, Zhao Z, Qi L, Chem. Mater., 7, 663 (1995)