LiFePO4_C复合材料的制备过程和氧化过程研究.doc

  LiFePO4/C 复合材料的制备过程和氧化过程 研究# 李金才，姜洪英，顾大伟，李冀蜀，沈临江** 5 10 15 20 25 30 35 40 （南京工业大学理学院，南京 210009） 摘要：采用 XRD 测试技术对不同煅烧温度条件下所得的 LiFePO4/C（LFP/C）产物和不同温 度氧化处理 LFP/C 的产物进行了研究，并结合差热分析（DTA）对含碳 LFP 前驱体和 700 煅烧制备的 LFP/C 样品的测试结果，研究了 LFP/C 的制备过程和 LFP/C 在空气气氛下的氧 化过程。实验结果表明，含碳 LFP 前驱体在 350 - 400 区间完全分解。当煅烧温度提升至 400时，含碳 LFP 前驱体分解产生的 FeO、Li4P2O7 和 H4P2O7 反应生成 LFP。当煅烧温度 升至 600 时可得到无杂相的 LFP。进一步提高反应温度有利于 LFP 结晶度的提高。LFP 的最佳煅烧温度应控制在 700 附近。LFP/C 样品中的 LFP 在 250 - 550 温度区间被氧化 为 β-Li3Fe2(PO4)3 和 α-Fe2O3。LFP/C 样品中的碳在 750 时被完全氧化。从提高实验准确度 考虑，采用热重法对 LFP/C 进行碳含量测定时应尽可能将测试温度覆盖到 750 。 关键词：磷酸铁锂；制备过程；氧化过程；X 射线衍射；差热分析 中图分类号：TM912.9 Study on the preparation process and oxidation process of LiFePO4/C composites LI Jincai, JIANG Hongying, GU Dawei, LI Jishu, SHEN Linjiang (School of Sciences, Nanjing University of Technology, NanJing 210009) Abstract: LiFePO4/C(LFP/C) samples were synthesized at different calcination temperatures and LFP/C oxidation products were prepared by oxidating LFP/C at different temperature. X-ray diffraction(XRD) patterns were studied. The preparation process and oxidation process in air atmosphere of LFP/C were analyzed and discussed with the test of XRD and Differential thermal analysis(DTA) for carbonaceous LFP precursor and LFP/C samples calcinated at 700℃. The experimental results show that carbonaceous LFP precursor was decomposed completely in the range of 350 - 400 ℃. LFP was produced by FeO, Li4P2O7 and H4P2O7 decomposed from carbonaceous LFP precursor when the calcination temperature reached 400 ℃. LFP without impurity phase was obtained when the calcination temperature reached 600 ℃. Increasing reaction temperature contributed to improvement of crystallinity of LFP. The best calcination temperature of LFP should be controlled at about 700 ℃. LFP in LFP/C sample was oxidized to β-Li3Fe2(PO4)3 and α-Fe2O3 between 250 ℃ and 550 ℃. The carbon in LFP/C sample was oxidized completely at 750 ℃. In consideration of experimental accuracy, the test temperature reached 7