微波溶剂热法快速合成CoSb_(3)纳米粉体的工艺研究  

Research on rapid synthesis of CoSb_(3)nano powder by microwave solvothermal method

作　　者：吴章平 关春龙[1] 赵志伟[1] 赵小苗 陈倩倩 史丽萍[2] WU Zhang-ping;GUAN Chun-long;ZHAO Zhi-wei;ZHAO Xiao-miao;CHEN Qian-qian;SHI Li-ping(School of Material Science&Engineering,Henan University of Technology,Zhengzhou 450007,China;National Key Laboratory of Science and Technology on Advanced Composites in Special Environments,Harbin Institute of Technology,Harbin 150001,China)

机构地区：[1]河南工业大学材料科学与工程学院,河南郑州450007 [2]哈尔滨工业大学,特种环境复合材料技术国防科技重点实验室,黑龙江哈尔滨150001

出　　处：《现代化工》2022年第11期145-149,154,共6页Modern Chemical Industry

基　　金：特种环境复合材料技术国防科技重点实验室基金(6142905203114);河南省科技厅科技攻关项目(212102210114)。

摘　　要：以CoCl_(2)和SbCl_(3)为前驱物、NaBH_(4)为还原剂、无水乙醇和聚乙二醇(200)为溶剂,采用微波溶剂热法合成了CoSb_(3)纳米粉体,并考察了反应温度、前驱物的摩尔比以及保温时间对CoSb_(3)纳米粉体的影响。通过XRD、SEM、TEM、激光粒度仪分别对样品的物相、形貌、晶粒尺寸进行表征。结果表明,当反应温度分别为210、230℃和250℃时,样品的主相分别为CoSb、CoSb_(2)和CoSb_(3)。在250℃保温10 min时,产物同时存在CoSb_(3)、CoSb_(2)、Sb三相;保温时间延长至20 min,CoSb_(2)和Sb相含量减少,产物中主相为CoSb_(3)相;保温时间延长至30 min可得到高纯CoSb_(3)相。通过Rietveld精修法对CoSb_(3)产物进行定量分析,CoSb_(3)相质量分数在90.9%以上。CoSb_(3)样品的晶体形貌为小颗粒球状,晶粒分布均匀,平均晶粒尺寸为33 nm。CoSb_(3) nano-powder is successfully synthesized by microwave solvothermal method with CoCl_(2) and SbCl_(3) as precursors,NaBH_(4) as reductant,and absolute ethanol and polyethylene glycol(200)as solvent.The effects of reaction temperature,molar ratio of precursor and temperature holding time on CoSb_(3) nano-powder are investigated.The samples'phase,morphology,and grain size are characterized by means of XRD,SEM,TEM,and Laser particle size analyzer.It is shown that main phases of the sample are CoSb,CoSb_(2),and CoSb_(3) when the reaction temperatures are 210℃,230℃,and 250℃,respectively.The products exist CoSb_(3),CoSb_(2) and Sb phases simultaneously when the temperature has been kept at 250℃for 10 min.If the temperature holding time is extended from 10 min to 20 min,the amount of CoSb_(3) phase in the samples processed at 250℃increase while the amounts of both CoSb_(2) phase and Sb phase decrease.A high-purity of CoSb_(3) phase can be obtained when temperature holding time extends to 30 min at 250℃.The content of CoSb_(3) phase is more than 90.9%through calculation by the Rietveld refinement method.The as-obtained powder is mainly composed of spherical particles with a mean diameter of approximately 33 nm.

关 键 词：微波溶剂热法 纳米粉体 热电材料 方钴矿 CoSb_(3) 

分 类 号：TN304[电子电信—物理电子学]