Preparation of silica nanoparticles: determination of the optimal synthesis conditions for small and uniform particles

Preparation of silica nanoparticles: determination of the optimal synthesis conditions for small and uniform particles
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DOI:
10.1016/s0927-7757(01)00683-5
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发表时间:
2002-02
期刊:
Colloids and Surfaces A: Physicochemical and Engineering Aspects
影响因子:
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通讯作者:
S. Park;Ki Do Kim;H. Kim
S. Park;Ki Do Kim;H. Kim
中科院分区:
其他
文献类型:
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作者:
S. Park;Ki Do Kim;H. Kim

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采用半间歇法将原硅酸四乙酯 (TEOS) 溶解在乙醇中制备二氧化硅纳米颗粒,以控制颗粒特性。本工作还采用统计实验方法根据四个参数(R=[H2O]/[TEOS])、氨(NH3)浓度、反应物进料速率、反应温度]比较了SiO2颗粒的性能(粒径和SD)。通过我们的实验,我们获得了尺寸范围为10至350 nm的单分散二氧化硅颗粒。结果表明,半间歇法制备窄粒径分布SiO2纳米颗粒的最佳合成条件为: (R=[H2O]/[TEOS],30–55;氨(NH3)浓度,0.2–0.35 mol l−1;反应物进料速率,13–17 cm3min−1;反应温度,55–65°C)。采用上述最佳条件同时制备出最小粒径(30 nm)和SD(<±5 nm)的颗粒。使用最佳合成条件测量的实验结果与模拟值非常吻合,并获得了最小的尺寸(直径~10 nm)。此外,我们还发现制备SiO2纳米颗粒时参数对粒径和SD的影响按以下顺序增加:反应温度,(R=[H2O]/[TEOS]);氨(NH3)的浓度,反应物的进料速率。
Silica nanoparticles were prepared from tetraethylortho-silicate (TEOS) dissolved in ethanol by using a semi-batch process in order to control the particle properties. In this work, the statistical experimental method was also used to compare the properties (particle size and SD) of the SiO2particles according to the four parameters (R=[H2O]/[TEOS]), concentration of ammonia (NH3), the feed rate of reactant, reaction temperature]. We have obtained monodispersed silica particles having size ranging from 10 to 350 nm by our experiment. It was found that the optimal synthesis conditions for the preparation of SiO2nanoparticles with narrow size distribution in semi-batch process were as follows; (R=[H2O]/[TEOS], 30–55; concentration of ammonia (NH3), 0.2–0.35 mole l−1; feed rate of reactant, 13–17 cm3min−1; reaction temperature, 55–65°C). The above-mentioned optimal conditions were used to prepare the particles with minimum particle size (30 nm) and its SD (<±5 nm), simultaneously. Experimental results measured by using the optimal synthesis conditions were in a good agreement with simulated value and the smallest size (∼10 nm in diameter) was obtained. Also, we found that the effect of parameters on the particle size and SD in the preparation of SiO2nanoparticles was increased in the following order; reaction temperature, (R=[H2O]/[TEOS]); concentration of ammonia (NH3), feed rate of reactant.