微波-超声波喷雾热解法制备超细球形ITO粉体的研究

Research on the Preparation of Superfine Spherical ITO Powders with the Method of Ultrasonic Atomization Combined Micro-wave Pyrolysis

以InCl_3·4H_2O和SnCl_2·2H_2O为原料,水为溶剂溶解作为前驱体溶液,采用微波管式炉加热联合超声波喷雾热解法制备得到ITO粉体。实验研究了不同微波热解温度和添加柠檬酸对ITO产品的微观形貌的影响,利用TG-DSC、XRD、SEM、EDS、TEM对样品的结构特征和微观形貌进行了表征分析。研究结果表明,前驱液浓度、温度和添加剂是影响氧化铟锡(ITO)粉体形貌的关键因素。得到粒径较小、分散性好和形貌呈球形的超细粉体的最佳条件为:温度650℃,前驱体原溶液浓度0.01mol/L,柠檬酸浓度0.004mol/L,载气速率0.6L/min,加入200目滤网。

With the raw materials of InCl3 · 4H2O and SnCl3 ·2H2O, the solvent of water and the mixture of them as precursor solution, the ITOpowders were prepared with the joint method of micro-wave and ultrasonic wave spray pyrolysis in a tubular furnace heated by micro wave. The influence of different micro-wave pyrolysis temperature and adding the surface active agent of ethanol on the change of microstructure has been analyzed. And the structural characteristics and microstructure of the product have been characterized with the help of TG-DSC, EDS, XRD, SEM and TEM. The results demonstrated that appropriate precursor solution concentration, temperature and proper quan- tity of additive are the key factors that have effect on the morphology of ITO powders. The extraordinarily fine ITO particles which have relatively small diameter, good dispersibility property and spherical shape morphology were pre- pared when the temperature was 650 ℃, concentration was 0. 01 mol/L, the speed of carrier gas was 0. 6 L/min, the concentration of citric acid added was 0. 004 mol/L and the a 200 mesh strainer was inserted. Key words ultrasonic atomization, indium tin oxide ultrafine powder, microwave-assisted pyrolysis, citric acid