固相剪切磨盘碾磨法制备四氧化三铁/氮掺杂石墨烯复合材料及其在锂离子电池中的应用

Preparation of Fe_3O_4/Nitrogen-doped Graphene Composite via Solid-state Shear Pan-milling Method and Its Application in Lithium Ion Battery

固相剪切磨盘碾磨法是一种基于全固相反应、不同于传统球磨方法制备微纳米基功能复合材料的新方法。本文以石墨和纳米四氧化三铁为原料,三聚氰胺为氮掺杂剂,采用固相剪切磨盘碾磨法,成功制备了四氧化三铁/氮掺杂石墨烯复合材料(Fe_3O_4/N-G)。通过X射线衍射(XRD)、拉曼光谱(RM)、透射电镜(TEM)、X射线光电子能谱(XPS)、比表面积(BET)测试和电化学测试对样品结构、形貌和电化学性能进行表征。测试结果显示:该方法能够在将石墨剥离成少数层石墨烯的同时,实现石墨烯的氮掺杂以及与Fe_3O_4的均匀复合,最终制得Fe_3O_4/N-G复合材料;将该复合材料作为锂离子电池负极材料,表现出优异的循环稳定性,在100mA·g-1的电流密度下经过100次循环后,Fe_3O_4/N-G可逆比容量保持在869 mAh·g-1,远高于纯Fe_3O_4的78mAh·g-1。该方法为制备石墨烯基复合电极材料提供了绿色环保、简便易行的新方法。

Different from traditional ball milling,solid-state shear pan-milling is an innovative approach that enables the synthesis of functional micro-and nano-composites.When graphite and nanometer scale Fe 3O 4 are applied as the raw material and melamine as the nitrogen doping agent,a composite of Fe 3O 4 and N-doped graphene(Fe 3O 4/N-G)could be successfully synthesized by employing the solid-state shearing pan-milling method.After characterization by X-ray diffraction(XRD),Raman spectroscopy(RM),transmission electronic microscopy(TEM),X-ray photoelectron spectroscopy(XPS),Brunauer,Emmett and Teller analysis(BET)and electrochemical measurements,it is found that graphite could be exfoliated into few-layered graphene while simultaneously doped by nitrogen and composited with Fe 3O 4 uniformly.When applied as an anode for lithium ion battery,an excellent cycling stability with a reversible capacity of 869 mAh·g-1 after 100 cycles at 100 mA·g-1 is delivered,which is far superior to pristine Fe 3O 4 with only 78 mAh·g-1 retained.The technique provides a green,and facile method for the preparation of graphene based composite electrode materials.