(中南大学 冶金科学与工程学院, 长沙 410083)
摘 要: 在充分回收含锡阳极泥有价金属的基础上, 采用从锡锑二次资源中直接提取的高纯氯锡酸铵和氯氧锑为原料, 合成了性能优良的纳米级锑掺杂二氧化锡(ATO)粉。 针对液相共沉淀法制备ATO的过程中, 锡和锑的水解不同步从而未能实现真正共沉淀掺杂的问题,以(NH4)2SnCl6和Sb4O5Cl2为原料, 采用配合-共沉淀法, 考察了反应过程中的pH、 反应温度、 掺锑浓度、 煅烧温度、前驱体洗涤次数和分散剂种类等对ATO粒度和形貌的影响, 确定了最优化条件, 即: 滴定终点pH=3, 反应温度60 ℃, 锑掺杂浓度10%(质量分数),热处理温度600 ℃,前驱体洗涤次数为6次, 采用分散剂c, 并进行了实验验证。
关键字: 锑掺杂二氧化锡; 配合-共沉淀; 纳米粉体
( School of Metallurgical Science and Technology,
Central South University, Changsha 410083, China)
Abstract: Based on the fully reclaiming of the valuable metal, pure (NH4)2SnCl6 and Sb4O5Cl2 were directly extracted form tin anode slurry, by using Sb4O5Cl2 and (NH4)2SnCl6 as precusors, fine antimony doped tin oxide(ATO) powder with excerllent performance was prepared by complex-co-precipitation, which can resolve some traditional problems when preparing ATO powder, such as conglomeration; limited material, expen sive cost and, etc. Especially, this method can make Sn4+ and Sb3+ hydrolyze at the same speed and get more even doped tin oxide. The optimal experimental condition is as: terminal pH value, reactive temperature 60 ℃, Sb doped concentration is 10%, heat treating temperature is 600 ℃, wash time is 6, and using dispersant c.
Key words: complex-co-precipitation; antimony doped tin oxide; nano-powders