通过水热法、火焰辅助微波法等控制氧化石墨烯(GO)的还原度,制备了一系列具有不同还原度的还原氧化石墨烯(RGO),并以这些RGO为前驱体,以六水氯化镍(NiCl2·6H2O)、2-巯基丙酸(C3H6O2S)为镍源和硫源,通过水热法合成了系列硫化镍/RGO(NS/RGO)复合材料。通过粉末X射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)和电化学工作站对材料的晶型结构、形貌特征及电化学储能性能进行了研究。结果表明:RGO的还原度高低不仅显著地影响了NS的晶型结构,而且改变了NS的形貌特征;利用超过140℃水热还原获得的RGO制得的NS/RGO复合材料中NS晶型以Ni3S4主,且形貌由棒状变成了球状;尤其,利用140℃还原获得的RGO制备的NS/RGO具有最强的电化学储能能力,比电容高达3331.6F/g。可为下一代新型电极活性材料的设计和构筑提供新思路。
In this study,the reduction degree of graphene oxide (GO) was controlled by hydrothermal method and flame-assisted microwave method to prepare a series of reduced graphene oxide (RGO) with different reduction degrees.Further,with these RGOs as precursors,nickel chloride hexahydrate (NiCl2·6H2O) and 2-mercaptopropionic acid (C3H6O2S) as nickel and sulfur sources,a series of nickel sulfide/RGO(NS/RGO) composites were synthesized by the hydrothermal method.Powder X-ray diffraction (XRD),field emission scanning electron microscopy (FE-SEM) and electrochemical workstation were used to study the crystal structure,morphology and electrochemical energy storage properties of the as-prepared materials.The results showed that the reduction degree of RGO not only significantly affected the crystal structure of NS,but also changed the morphological characteristics of NS.In the NS/RGO composite prepared from RGO obtained by hydrothermal reduction at over 140℃,the crystal forms of NS were dominated by Ni3S4,and the morphology changed from rod-like to spherical.In particular,the NS/RGO composite prepared from RGO obtained by reduction at 140℃ had the strongest electrochemical energy storage capacity,and the specific capacitance was as high as 3331.6F/g.Therefore,this study provided new insights for the design and construction of the next-generation electrode active materials.
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基金资助
贵州省科技计划项目(黔科合基础-ZK[2021]一般057);贵州省普通高等学校青年科技人才成长项目(黔教合KY字[2021]252);贵州师范学院国家自然基金项目奖励补助资金项目(纵20210108)
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