水热法合成纳米花状二硫化钼及其微观结构表征  

Synthesis and characterization of flower-like Mo S_2 microspheres by hydrothermal method

作　　者：傅重源 邢淞[1] 沈涛[1] 邰博 董前民[1] 舒海波[1] 梁培[1] 

机构地区：[1]中国计量学院,光学与电子科技学院,杭州310018

出　　处：《物理学报》2015年第1期204-209,共6页Acta Physica Sinica

基　　金：国家自然科学基金(批准号:61006051;61177050);浙江省大学生科技创新活动计划(批准号:2013R409016);浙江省科技厅公益技术应用研究(批准号:2013C31068)资助的课题~~

摘　　要：本文以钼酸钠、硫代乙酰胺为前驱体,硅钨酸为添加剂,成功用水热法合成高纯度纳米花状二硫化钼.产物特性用X射线衍射(XRD)、能量色散谱(EDS)、扫描电子显微镜(SEM)进行表征.XRD和EDS图显示实验产物为二硫化钼,且其结晶度和层状堆垛良好.SEM图谱则表明二硫化钼为纳米花状结构,颗粒直径300nm左右,由几十上百片花瓣组成,每片花瓣厚度十个纳米左右.通过以硅钨酸为变量的梯度实验,研究发现,硅钨酸对于纳米花状Mo S2的形成具有重要作用,不添加硅钨酸,无法形成纳米花状Mo S2,此外,硅钨酸的剂量会影响合成Mo S2的大小和形貌.本文还对纳米花状二硫化钼的形成机理做了初步的讨论.High-purity flower-like MoS2 microspheres have been successfully synthesized by hydrothermal method using Na2MoO4 and CH3CSNH2 as precursors, and HaO40SiW12 as an additive. Samples are characterized by X-ray powder diffraction （XRD）, scanning electron microscopy （SEM）, and energy dispersive spectrometer （EDS）. XRD and EDS pat- terns show that the as-prepared samples are MoSs, which have good crystallinity with a well-stacked layered structure. SEM images show that the as-prepared MoS2 are composed of flower-like microspheres with a mean diameter about 300 nm, the structures of which are constructed from dozens of hundreds of MoS2 nano-sheet with a thickness of several nanometers. It is also found that the silicotungstic acid plays an important role in the formation of the flower-like MoSs microspheres, which could affect the size and morphology of the MoS2. Flower-like MoSs is not found in the as-prepared product without adding silicotungstic acid. A formation mechanism of MoS2 microspheres is tentatively given.

关 键 词：二硫化钼 纳米花 水热法 

分 类 号：TQ136.12[化学工程—无机化工]