室温固相合成球形氧化锆纳米晶体  

Preparationof spherical zirconium oxidenano-crystals by solid state reaction at room temperature

作　　者：姜求宇[1] 吴文伟[1] 廖森[1] 谭国进[1] 梁信源[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004

出　　处：《无机盐工业》2005年第11期20-22,共3页Inorganic Chemicals Industry

基　　金：广西教育厅科研项目(桂教科研字2002第316号)

摘　　要：用碳酸铵与氯氧化锆作原料,在适量表面活性剂聚乙二醇辛基苯基醚(OP乳化剂)的存在下,在室温下充分混合研磨得到反应混合物,洗去其中的可溶性无机盐后烘干得到前驱体,前驱体经热分解即可得到球形氧化锆纳米晶体。基于均匀设计、逐步回归分析及最优化计算,对纳米氧化锆的固相合成条件进行优化,所获取的优化工艺条件为:氯氧化锆取10 mmol时,反应物碳酸铵与氯氧化锆的物质的量比等于1.4∶1;表面活性剂用量40μL;研磨时间40 m in;热分解温度500℃及热分解时间120 m in。在此条件下合成的氧化锆晶体粉末颗粒均匀、团聚弱,其一次粒子的平均粒径约20 nm,收率为95%。The precursor mixture was obtained by grinding ZrOCl2 · 8H2O and （NH4）2CO3 with surfactant OP thoroughly at room temperature. Then soluble inorganic salts were removed by washing with water. After drying, the spherical zirconium oxide nano - crystals were obtained when the dried precursor was pyrolyzed. Based on the uniform design and stepwise regression and optimization calculation, the optimization parameters for the preparation of the zirconium oxide nano - crystals by solid state reaction were obtained, i.e. ,with 10 mmol ZrOCl2 · 8H2O, n[ （ NH4 ）2CO3 ] ： n（ ZrOCl2 · 8H2O） = 1.4 ： 1 , volume of surfactant OP 40 μL, and grinding time 40 min, and pyrolysis temperature 500 ℃, and pyrolysis time 120 min. Under such conditions, the uniform zirconium oxide powder was obtained, and the average grain size of primary grain was about 20 nm, and the yield was up to 95%.

关 键 词：氧化锆 纳米晶 室温固相反应 

分 类 号：TQ134.1[化学工程—无机化工]