화학공학소재연구정보센터
Applied Chemistry, Vol.5, No.2, 83-86, October, 2001
반회분식 반응을 이용한 단분산 SiO2, TiO2, ZrO2 입자의 제조 및 입자크기와 입도분포에 영향을 미치는 인자들의 비교
Synthesis of Monodisperse SiO2, TiO2 and ZrO2 Nanopaticles using Semi-batch Reactor and Comparison of Parameters Effecting Particle Size and Particle Size Distribution
Monodisperse SiO2, TiO2, and ZrO2 nanoparticles were synthesized from tetraethyl orthosilicate (TEOS), tetraethyl orthotitanate (TEOT), zirconium IV propoxide(ZnP) dissolved in ethanol, respectively, using semibatch method which was found to be easier than a batch process in controlling the size, shape, and size distribution. In this study, a statistical experimental method was also used to compare the properties (particle size and size deviation) of the SiO2, TiO2, and ZrO2 particles according to four parameters [R(=H2O / TEOS or TEOT or ZnP), hydroxypropylcellulose (HPC) / NH3, the feed rate of the reactant, and the reaction temperature]. It was found that the optimal conditions for the preparation of SiO2, TiO2 and ZrO2 nanoparticles in a Semi-batch process were as follows ; (1) SiO2; R(=[H2O/TEOS]): 31, concentration of ammonia: 0.32 mole/l, feed rate of reactant: 17 ml/min, reaction temperature: 62 ℃. (2) TiO2; R(=[H2O/TEOT]): 16, HPC: 0.0018 g/ml, feed rate of reactant: 0.6 ml/min, reaction temperature: 30 ℃/ (3) ZrO2; R(=[H2O/ZnP]): 15, HPC: 0.0018 g/ml, feed rate of reactant: 1.3 ml/min, reaction temperature: 25 ℃. Using the above optimal conditions, particles of SiO2 (13.7 nm) and TiO2 (10.6 nm) and ZrO2 (23.0 nm) with a narrow size distribution were prepared. In addition, it was found that the main size distribution were prepared. In addition, it was found that the main parameters affecting of SiO2, TiO2 and ZrO2 nanoparticles decreased in the order of the feed rate of the reactant > NH3/ HPC > R(=H2O/ TEOT) > the reaction temperature.