球状ZnSe纳晶的微波辅助元素溶剂热合成与表征
Microwave-assisted Elemental Solvothermal Synthesis and Characterization of Sphere-like ZnSe Nanocrystals
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摘要: 采用微波辅助的元素溶剂热法,以Zn,Sc等单质为Zn源和Se源,en(en=乙二胺)为螯合剂,N2H4·H2O为还原性助剂,在160℃下反应4小时,合成了直径为0-100nm、分散性较好、高度结晶的球形ZnSe纳晶;采用XKD,SEM等手段对所合成的产物进行了表征,结果发现,反应温度和反应时间等反应条件共同控制着ZnSe纳晶的形貌.通过对其反应过程及机理的分析,结果表明,获得平均直径为60nm、高度结晶的球形ZnSe纳晶的优化反应条件是用en做螯合剂,N2J4·H2O为还原性助剂,反应温度为160℃,时间为4小时;并且球状ZnSe纳晶是在N2微泡上集聚而成的.Abstract: Well dispersed and high crystallized sphere-like ZnSe nanocrystals with diameter of 50-100nm have been synthesized by a microwave-assisted elemental solvothermal method with element Zinc and Selenium as reaction sources,en(en=ethylenediamine) as the chelating reagent,and N2H4·H2O as reductive assistant at 160℃ for 4 hours; The as-synthesized ZnSe nanocrystals were characterized by X-ray diffraction(XRD) and scanning electron microscopy(SEM).It was found that the shape of ZnSe nanocrystals was controlled by the reaction temperature and time.Through the reaction process and possible mechanism analysis,the results showed that the preferable reaction conditions in which high crystallized sphere-like ZnSe nanocrystals with mean diameter of 60nm could be successfully obtained were using en as the chelating reagent and N2H4·H2O as reductive assistant at 160℃ for 4 hours and sphere-like ZnSe nanocrystals came from the aggregation of ZnSe nanocrystals on the surface of N2 microbubble.