ATO粉体的水基溶胶-凝胶法合成工艺研究

Processing parameters of ATO powder prepared by water-based sol-gel method

采用水基溶胶-凝胶法合成了锑掺杂二氧化锡(ATO)粉体。采用X射线衍射(XRD)、能谱仪(EDS)、扫描电镜(SEM)、透射电镜(TEM)以及X射线光电子谱(XPS)对粉体进行了表征,探讨了ATO溶胶的制备工艺以及锡锑摩尔比(n_(Sn)/n_(Sb))对溶胶粒度和烧结粉体的形貌与物相的影响。结果表明:溶胶合成的较优条件为溶胶浓度=0.1 mol/L,水浴温度=50℃,p H=7,n_(Sn)/n_(Sb)=90/10。锡锑摩尔比对粉体的物相结构无影响。ATO粉体在n_(Sn)/n_(Sb)低于95/5时出现球形及棒状形态,其中Sn元素与Sb元素分别以Sn^(4+)、Sb^(5+)和Sb^(3+)的形式固溶于粉体中。

Antimony-doped tin dioxide powder（ATO）was synthesized by water-based sol-gel method.The morphology,phase structure and chemical state of the powders were characterized by X-Ray diffractometer（XRD）,energy disperse spectroscopy（EDS）,scanning electron microscope（SEM）,transmission electron microscope（TEM）and X-ray photoelectron spectroscopy（XPS）.The optimization processing parameters of ATO sol and the effects of antimony doping content（n_（Sn）/n_（Sb））on particle size of ATO sol and the morphology and phase structure of sintered ATO powders were investigated.The results show that the optimal parameters of ATO sol are as follows：sol concentration =0.1 mol/L,bath temperature= 50 ℃,p H=7 and n_（Sn）/n_（Sb） = 90/10.The phase structure of ATO powder has no relation with the ratio n_（Sn）/n_（Sb）.When n_（Sn）/n_（Sb） is lower than 95/5,the ATO powder with spherical and rod-like shape appears.The elements of Sn and Sb are dissolved into the ATO powder in the form of Sn^4 ＋,Sb^5 ＋ and Sb^3 ＋.