水热LSS法制备SnO_2纳米晶工艺研究

Synthesis of SnO_2 Nanocrystalline by Hydrothermal Liquid-Solid-Solution Method

采用LSS法成功地制备出具有规则形状的SnO_2纳米晶,并系统研究了水热反应温度、[Sn^(4+)]离子浓度、水热反应釜填充比等工艺因素对SnO_2纳米晶的晶粒尺寸及相组成的影响。采用X-射线衍射仪、纳米粒度分析仪和场发射扫描电子显微镜对所制备的SnO_2纳米晶进行表征。结果表明:所制备的SnO_2由直径约为9～11 nm的具有规则形状的SnO_2纳米晶组成。SnO_2纳米晶存在明显的团聚,团聚体的平均颗粒为300 nm;随着水热反应温度的升高和[Sn^(4+)]离子浓度的增加,SnO_2纳米晶的晶粒尺寸增大;在50%～70%范围内,水热反应釜填充比对SnO_2纳米晶的影响不大。

SnO2 nanocrystalline with regular shape have been successfully prepared by the liquid-solid-solution （LSS） process. The influences of hydrothermal reaction temperature, concentrations of [Sn^4＋] and filling ratio of the autoclave on the phase composition and particle size have been investigated. The as-prepared crystalline were characterized by X-ray diffraction （XRD）, nanoparticle size analyzer （NSA） and field beaming scanning electron microscope （SEM）. It shows that the size of the as-prepared sphericity SnO2 crystalline is about 9-11 nm. The agglutination of SnO2 nanocrystalline has been observed obviously and the average grain size of the conglomeration is about 300 nm. With the increase of hydrothermal reaction temperature and concentrations of [Sn^4＋], the size of as-obtained SnO2 nanocrystalline increases. The filling ratio of the autoclave has little influence on SnO2 nanocrystalline at the range of 50%-70%.