化学液相共沉淀法制备ITO纳米粉体的工艺研究

研究了以4N铟、锡锭为原料，以25%氨水为沉淀剂，采用点滴法滴加氨水的方式来制备铟锡氧化物 (ITO)纳米粉体的化学液相共沉淀法。考察了反应初始铟浓度、反应温度、反应终点pH值和前驱体老化时间对ITO粉体粒径的影响。运用X射线衍射(XRD)、差热-热重分析(DTA-TG)、透射电镜(TEM)、场发射扫描电镜(SEM)等检测手段对粉体进行了表征。在液相中加入1%的硅酸钠、反应温度为60 ℃、反应终点pH值为8、老化时间为2 h、煅烧制度为4 h、800 ℃的工艺条件下，所制得的ITO粉体具有立方晶系结构，粉体粒径在20～40 nm之间，呈球形，颗粒均匀，且分散性能良好。该方法与以前的方法相比，原料来源简单，共沉淀工艺改善，反应条件更加温和，工艺设备简单，污染小，成本低，产品质量高，为ITO纳米粉体合成探索一条新的工艺路线。

Study on Preparing Nanosized ITO Powder by Chemical Liquid Phase Coprecipitation Process

Indium tin oxide (ITO) nanopowder was synthesized by liquid chemical co-precipitation process using 4 N indium and tin ingots as material and ammonia (25% wt) as precipitator. The study investigated the effect of the initial concentration of indium ion，reaction temperature, pH of reaction end and aging time of precursor on the size of ITO powder. The powder was characterized by means of X-ray diffraction (XRD), differential thermal analysis, thermogravimetric analysis (DTA-TG), transmission electron microscopy (TEM) and field-emission scanning electron microscope(SEM). At 1% sodium silicate, a reaction temperature of 60 ℃, a final reaction pH of 8, an aging time of 2 h and a calcination temperature of 800 ℃ for 4 h, the ITO powder particulates obtained are of cubic crystalline structure, 20～40 nm sized, spherical, uniform and well dispersed. Compared with the previous ones, this process has the advantages of easy-to-get raw material, improved co-precipitation, moderate reaction, simple process equipment, small pollution, low cost and high quality, providing a new process route for the synthesis of nanosized ITO powder.