Influence of sintering temperature on the properties of Li4Ti5O12 anode material for lithium-ion batteries
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摘要: 采用钛酸四丁酯为钛源、一水合氢氧化锂为锂源,利用水热法制备锂离子电池负极材料Li4Ti5O12(LTO),研究了水热后不同烧结温度对LTO相组成、微观形貌及电化学性能的影响。结果表明:当煅烧温度分别为500、550、600、650、700℃时,烧结LTO均为尖晶石型;500、550、600℃烧结LTO的微观形貌为纳米片状结构,当温度升高到650℃时,LTO出现纳米棒状结构,随着温度继续升高,LTO在700℃时生成较厚的纳米片状结构;当烧结温度为650℃时,LTO的比表面积为94.5907 m2·g-1,气孔体积为0.9663 mL·g-1,此时Li4Ti5O12的放电比容量达到最大值240 mAh·g-1;电流密度100 mA·g-1、循环260次条件下,LTO容量保持率达96.45%,电流密度为1和2 A·g-1、循环1000次条件下,LTO容量保持率达92.97%和77.21%。Abstract: The Li4Ti5O12 (LTO) anode materials for lithium-ion batteries were prepared by hydrothermal method in this paper, using tetrabutyl titanate as the titanium source and lithium hydroxide monohydrate as the lithium source. The influence of sintering temperature on the phase composition, microstructures, and electrochemical properties of LTO was investigated. The results show that the spinel LTO is formed at 500, 550, 600, 650, and 700℃, respectively. The microstructures of LTO are present as the nanosheets sintered at 500, 550, and 600℃, the nanorods sintered at 650℃, and the thicker nonosheets sintered at 700℃. The LTO exhibits the high specific surface area of 94.5907 m2·g-1, the good pore volume of 0.9663 mL·g-1, and the highest initial discharge capacity of 240 mAh·g-1 sintered at 650℃. Additionally, the LTO has an excellent cycling performance with capacity retention ratio of 96.45% after 260 cycles at 100 mA·g-1, and the capacity retention ratio of 92.97% and 77.21% after 1000 cycles at 1 and 2 A·g-1, respectively.
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Key words:
- lithium ion battery /
- anode material /
- sintering temperature /
- microstructure /
- electrochemical property
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表 1 不同烧结温度下LTO样品的比表面积和孔体积
Table 1. Specific surface area and pore volume of LTO samples sintered at different temperatures
温度/℃ 比表面积/(m2·g-1) 孔体积/(mL·g-1) 500 37.1633 0.2552 550 71.3419 0.8075 600 85.3326 0.8623 650 94.5907 0.9663 700 45.8839 0.4178 表 2 不同烧结温度下不同电流密度时LTO样品的放电比容量
Table 2. Discharge capacities of LTO samples sintered at different temperatures in different current densities
温度/℃ 放电比容量/(mAh·g-1) 20 mA·g-1 100 mA·g-1 500 m A·g-1 1 A·g-1 2 A·g-1 4 A·g-1 500 142.0 112.9 95.8 86.7 72.7 56.7 550 164.2 141.1 125.1 115.9 103.3 83.4 600 222.4 175.1 152.0 143.6 133.5 119.0 650 240.0 203.8 190.1 184.3 172.6 150.0 700 231.1 177.1 159.6 147.0 133.4 129.3 表 3 不同烧结温度下电解液电阻(RE)和电荷迁移电阻(RCT)数值
Table 3. Electrolyte resistance (RE) and charge transfer resistance (RCT) at different sintering temperatures
温度/℃ RE/Ω RCT/Ω 500 2.71 211.29 550 2.10 127.30 600 4.39 192.01 650 1.80 69.20 700 2.36 93.04 -
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