微波溶剂热法快速合成CoSb₃ 纳米粉体的工艺研究

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.