化工学报 ›› 2008, Vol. 59 ›› Issue (9): 2407-2411.

• 材料化学工程与纳米技术 • 上一篇    下一篇

超声水热法制备单分散球形二氧化硅及因素分析

申晓毅,翟玉春,刘岩   

  1. 东北大学材料与冶金学院
  • 出版日期:2008-09-05 发布日期:2008-09-05

Preparation of mono-disperse spherical silicon dioxide by ultrasonic hydrothermal method

SHEN Xiaoyi, ZHAI Yuchun, LIU Yan   

  • Online:2008-09-05 Published:2008-09-05

摘要: 采用超声水热法在醇水氨体系制备了单分散球形二氧化硅,其中氨作为催化剂提供强亲核剂,通过设计正交实验研究了超声波功率、反应温度、搅拌强度和反应物摩尔配比对单分散球形二氧化硅粒度的影响。研究表明随超声功率和反应物摩尔配比增加,二氧化硅粒度明显增加;随温度和搅拌强度增加二氧化硅粒度增加,但幅度较小。二氧化硅形成过程可分为水解和缩合两步,其中水解是关键步骤。采用XRD、SEM和IR对制备的样品进行表征,结果表明单分散球形二氧化硅为非晶态颗粒,粒度均匀,外形规则,且样品中含有大量羟基。

关键词:

超声水热, 单分散, 正交实验, 水解, 缩合, 非晶态

Abstract:

Mono-disperse spherical silicon dioxide was synthesized in 2-propanol-H2O-NH3 system by the ultrasonic hydrothermal method.The catalyst ammonia acted as strong nucleophilic reagent.With orthogonal experiments, the effects of ultrasonic power, reaction temperature, stirring intensity and molar ratio on the size of silicon dioxide were studied.The results indicated that the diameter of silicon dioxide increased greatly with increasing ultrasonic power and molar ratio.The size of silicon dioxide also increased with increasing temperature and stirring intensity, but with a less extent.The process of forming mono-disperse spherical silicon dioxide could be divided into two steps: hydrolysis and condensation, with hydrolysis as the key step.Mono-disperse spherical silicon dioxide was characterized with XRD, TEM, DTA and IR, and the results showed that the sample was noncrystalline with regular shape and uniform granularity and there was a large amount of hydroxyl group in the SiO2 sample.

Key words:

超声水热, 单分散, 正交实验, 水解, 缩合, 非晶态