铜铟硫纳米粒子的改进溶剂热法合成与表征

Improved solvothermal synthesis and characterization of copper indium sulfide nanoparticles

采用溶剂热法和单一前体法相结合的改进方法,以二乙基二硫代氨基甲酸铜和二乙基二硫代氨基甲酸铟配合物为前体,乙二胺或油胺为表面修饰剂,成功地合成了铜铟硫纳米粒子.研究了表面修饰剂与前体的摩尔配比、反应时间、反应温度以及弱还原性添加剂对产物形貌结构的影响,采用XRD,SEM等测试方法对产物进行了结构表征.结果表明,在乙二胺和铜的物质的量比为10∶1或者油胺和铜的物质的量比为5∶1,反应温度为180℃,反应时间为8 h,能够得到具有较好的粒度和晶度的铜铟硫纳米粒子.单一前体法和溶剂热法相结合的复合方法能有效地控制最终产物组成元素的物质的量比,可以推广到其他二元、三元硫族化合物的制备之中.

Copper indium sulfide nanoparticles were successfully synthesized through the combination of single source precoursor method and solvothermal method.Copper diethyldithiocarbamate and indium diethyldithiocarbamate were used as precursors.Ethylene diamine and oleylamine were used as capping ligands.The impact of the molar ratio of ligand to precursor,the reaction time,the reaction temperature and the reductive additives were studied.XRD（X-ray diffraction） and SEM（scanning electron microscope） were used to characterize the as-synthesized products.The results show that the CuInS2 nanoparticles with good size and crystallinity can be synthesized with ethylene diamine to precursor ratio of 10∶1 or oleylamine to precursor ratio of 5∶1,and 8 h reation under 180 ℃.The final product compoistion can be effectively controlled by this combined method,which could be further applied to the preparation of other binary or ternary chalcogenides.