摘要
作为一种新型锂离子电池正极材料,氟化铁(FeF3)因具有高比容量、低成本、安全和对环境友好等优点而备受关注。但FeF3极差的导电性严重影响其电化学性能,并阻碍了其应用。本论文主要围绕提高FeF3电子电导率从而提高其电化学性能展开研究,通过添加五氧化二钒(V2O5)、乙炔黑和二硫化钼(MoS2)等导电性物质对FeF3进行改性研究。主要研究内容为:
(1)采用液相法制备了FeF3(H2O)4.5前驱体,并在惰性气体保护下,500℃加热前驱体,合成了锂离子电池正极材料FeF3。利用傅里叶红外光谱(FT-IR)、X-射线衍射(XRD)、扫描电镜(SEM)和电化学测试等技术,研究了材料的物理化学性能和电化学性能。结果表明:FeF3具有典型的正交晶系结构,并且所制备的材料粒径均匀,在0.1C倍率和电压范围为2.0~4.5 V下的首次放电比容量为115.7 mAh·g-1,经过30个循环后放电比容量降至67.7 mAh·g-1,容量保持率仅为58.5%。
(2)通过球磨混合FeF3与乙炔黑,合成了FeF3/C复合正极材料。测试结果表明:添加乙炔黑并未改变FeF3的晶体结构,但FeF3的放电比容量、循环性能及大倍率充放电性能得到了显著改善。以0.1C倍率充放电,球磨3h的样品首次放电比容量高达206.4 mAh·g-1,30个充放电循环后仍保持有179.2 mAh·g-1,容量保持率高达86.8%。以3C高倍率充放电,放电比容量仍有109 mAh·g-1。
(3)通过球磨混合FeF3与V2O5,合成了具有比FeF3电化学性能更好的FeF3/V2O5复合正极材料。其中球磨3h的样品具有最好的电化学性能,在0.1C倍率下首次放电比容量高达219 mAh·g-1,30个充放电循环后仍保持有192 mAh·g-1,容量保持率高达87.7%。
(4)通过球磨混合FeF3与MoS2,合成了FeF3/MoS2复合正极材料。测试结果表明:MoS2的添加并没有改变FeF3正极材料的电化学反应机理,对晶体结构也没有影响,但MoS2添加能显著提高FeF3的电子导电率,以0.1C放电倍率下,首次放电比容量为169.6 mAh·g-1,30个充放电循环后仍保持有141 mAh·g-1,容量保持率为83.1%。
FeF3, as a new cathode material for lithium-ion battery, has been attractive for its high capacity, low cost, safe and environmental benignity. However, its low electron conductivity impairs its electrochemical performance and prevents its applications. Therefore, improving the electron conductivity of FeF3 to enhance its electrochemical performance is the focus of the study. In this paper, the composite cathode materials of FeF3 and conductive reagents were prepared by addition of acetylene black, V2O5 and MoS2, respectively, and the physical and electrochemical performance of composites were investigated.
(1) Precursor FeF3(H2O)4.5, which was synthesized by a liquid phase reaction method, was heated in tube furnace at 500℃in inert gas to obtain FeF3. The physical and electrochemical performances of FeF3 were investigated by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), scanning electron microscope (SEM) and electrochemical tests. The results showed that FeF3 had a typical orthorhombic structure and uniform particle size, and the FeF3 electrode delivered an initial discharge capacity of 115.7 mAh·g-1 and the capacity retention at the 30th cycle was only 58.5% (67.7 mAh·g-1) at a rate of 0.1C in the voltage range of 2.0~4.5 V.
(2) The FeF3/C composites were prepared by milling the mixture of FeF3 and the conductive acetylene black. The addition of carbon did not change the crystal structure of FeF3. The discharge capacity, cycle capability and high-rate charge-discharge capability of FeF3 were all greatly improved. The FeF3/C composite milled for 3h exhibited best discharge capacity retention and highest discharge capacity in the voltage range of 2.0~4.5 V, and delivered an initial discharge capacity of 206.4 mAh·g-1 and the capacity retention at the 30th cycle was 86.8% at a rate of 0.1C. Moreover, the initial discharge capacity can reach 109 mAh·g-1 at a rate of 3C.
(3) The FeF3/V2O5 composites were prepared by milling the mixture of FeF3 and V2O5. The FeF3/V2O5 composites showed much better electrochemical performance than that of FeF3, and the FeF3/V2O5 composite milled for 3h exhibited the best electrochemical performance and highest discharge voltage plateau, highest capacity of 219 mAh·g-1 and highest capacity retention rate of about 87.7% after 30 cycles at a rate of 0.1C in the voltage range of 2.0~4.5 V.
(4) The effect of the content of molybdenum disulfide (MoS2) on the electrochemical properties of FeF3/MoS2 composite was also studied in detail. The results indicated that addition of MoS2 did not change the structure and electrochemical reaction mechanism of FeF3, and MoS2 can increase the electronic conductivity of the composites, hence to improve the electrochemical performance of FeF3. The initial discharge capacity of FeF3/MoS2 was 169.6 mAh·g-1 between 2.0~4.5 V at a rate of 0.1C, and the capacity remained as 141 mAh·g-1 after 30 cycles.
引文
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