溶剂热法合成硫化镉微晶工艺研究

Study on the Synthetic Technology of CdS Microcrystals by Solvothermal Method

以氯化镉为前驱体,硫化钠、硫代乙酰胺、硫脲等为硫源,乙二醇、乙醇等为溶剂,通过溶剂热法制备硫化镉微晶。设计L9(34)正交试验,探讨了反应温度、反应时间等对硫化镉微晶大小和形貌的影响。所得产物经离心、洗涤、干燥后,用纳米粒度仪分别测定各产物的平均粒径,同时用扫描电子显微镜测定部分产物的大小和形貌,并用极差分析法找寻最佳合成工艺。结果表明:以硫代乙酰胺为硫源,乙二醇为溶剂,反应温度为100℃,反应时间为10 h,可得到直径为0.5~0.7μm的片状硫化镉晶体。该方法工艺简单,反应条件温和,制备的硫化镉晶体大小分布均匀,形貌单一。

Sadmium sulfide(CdS)microcrystals were prepared by solvothermal method using cadmium chloride as precur⁃sor,sodium sulfide,thioacetamide and thiourea as sulfur sources,ethylene glycol and ethanol as solvent.The L9(34)orthogo⁃nal experiments were designed to investigate the effects of reaction temperature and reaction time on the size and morpholo⁃gy of CdS microcrystals.After centrifugation,washing and drying,the average particle size of each product was determined by nanoparticle size analyzer,and the size and morphology of some products were measured by scanning electron micro⁃scope simultaneously,and the best synthesis process was found by range analysis.The results show that:using thioacet⁃amide as sulfur source,ethylene glycol as solvent,reaction temperature of 100℃,reaction time of 10 h,the plate-shaped CdS crystal with diameter of 0.5~0.7μm can be obtained.The method is simple,mild reaction conditions,uniform size dis⁃tribution and single morphology of CdS crystal.