以CoCl₂和SbCl₃为前驱物、NaBH₄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CoSb₃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CoSb₃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、CoSb₂和CoSb₃。在250℃保温10 min时，产物同时存在CoSb₃、CoSb₂、Sb三相；保温时间延长至20 min，CoSb₂和Sb相含量减少，产物中主相为CoSb₃相；保温时间延长至30 min可得到高纯CoSb₃相。通过Rietveld精修法对CoSb₃产物进行定量分析，CoSb₃相质量分数在90.9%以上。CoSb₃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。

CoSb₃ nano-powder is successfully synthesized by microwave solvothermal method with CoCl₂ and SbCl₃ as precursors,NaBH₄ 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 CoSb₃ 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,CoSb₂,and CoSb₃ when the reaction temperatures are 210℃,230℃,and 250℃,respectively.The products exist CoSb₃,CoSb₂ 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 CoSb₃ phase in the samples processed at 250℃ increase while the amounts of both CoSb₂ phase and Sb phase decrease.A high-purity of CoSb₃ phase can be obtained when temperature holding time extends to 30 min at 250℃.The content of CoSb₃ 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.

吴章平(1998-),男,硕士研究生,主要从事热电材料研究,1172823205@qq.com