本文应用碳热还原法,以廉价的FeCl3.6H2O、LiOH.H2O和NH4H2PO4为原料,以淀粉为还原剂和碳源,经600 oC烧结制备了LiFePO4/C复合材料,方法重现性好且易规模化. 采用X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)测试材料结构,观察材料形貌. 结果表明,经600 oC烧结10 h所得产物具有纯相的橄榄石型晶体结构、良好的结晶性和规整的球状形貌,粒径为60 ~ 100 nm,包覆LiFePO4晶粒的碳层厚度为2 nm左右,碳含量为5%(by mass). 材料的振实密度高达1.3 g.cm-3,在0.2C倍率下首次放电比容量为162 mAh.g-1,在0.5C、1C、2C、5C和10C倍率下首次放电比容量分别为143、135、127、116和105 mAh.g-1,10C倍率下500周期循环,其比容量仍有81 mAh.g-1.
The LiFePO4/C composite electrode material was synthesized by a moderate in situ carbothermal reduction method at 600 °C using FeCl3.6H2O, LiOH.H2O, and NH4H2PO4 as starting materials, soluble starch sol as a carbon source and a reducing agent. This method is readily reproducible and possibly feasible to carry out large-scale synthesis. The structure and morphology of the LiFePO4/C samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The synthesized LiFePO4/C composite was in pure phase of olivine-type, shows highly crystalline and spherical morphology with the particle sizes in the range of 60 ~ 100 nm. The thickness of the carbon film could be as thin as about 2 nm for the isolated LiFePO4/C particles, and the amount of carbon introduced into the composite was about 5% (by mass). The measured tap density of LiFePO4/C composite was as high as 1.3 g.cm-3 and the initial discharge capacities of LiFePO4/C composite reached 162, 143, 135, 127, 116 and 105 mAh?g-1 at 0.2C, 0.5C, 1C, 2C, 5C and 10C rates, respectively. Remarkably, even after 500 cycles at 10C, the capacity of 81 mAh.g-1 could be obtained.