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Synthesis and electrochemical properties of LiFePO4 cathode material by ionic thermal method using eutectic mixture of tetramethyl ammonium chloride–urea

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Abstract

In this study, the LiFePO4 cathode was synthesized by the ionic thermal method using the deep eutectic mixture of tetramethyl ammonium chloride and urea. The synthetic conditions were systematically investigated by orthogonal experiments, which indicate that the optimal reaction time, reaction temperature, molar ratio of Li to DES and rotate speed are 96 h, 220 °C, 1:14 and 20 r·min −1, respectively. X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM) were characterized to investigate the crystalline structure and morphology of the obtained materials, indicating well-crystallized LiFePO4 with olivine structure. And the physical properties of LiFePO4 were explored through Fourier transform infrared spectroscopy (FTIR), 57Fe Mössbauer absorption spectra and Raman spectra. An initial discharge capacity can reach 151 mAh·g−1 at 0.1C rate for LiFePO4 following by calcining at 600 °C under the optimal conditions, and it retains 125.1 mAh·g−1 after 100 cycles. These results demonstrated that the addition of ionic liquids can improve the rate performance, cycle performance and ion diffusion rate of LiFePO4.

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摘要

本文以四甲基氯化铵和尿素为原料, 采用离子热法合成了LiFePO4正极材料。通过正交实验对合成条件进行了系统的研究, 结果表明最佳反应时间、反应温度、Li与DES的摩尔比、转速分别为96h、220℃、1:14和20。通过X射线衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对所得材料的晶体结构和形貌进行了表征, 表明LiFePO4结晶良好, 具有橄榄石结构。通过傅里叶变换红外光谱(FTIR)、57Fe穆谱吸收光谱和拉曼光谱探究了LiFePO4的物理性质。在最佳条件下, LiFePO4在600℃下煅烧后, 以0.1C的速率放电, 初始放电容量可达151 mAh·g−1, 循环100次后仍可保持125.1 mAh·g−1。这些结果表明, 离子液体的加入可以提高LiFePO4的速率性能、循环性能和离子扩散速率。

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Acknowledgements

This study was financially supported by the National Natural Science Foundation of China (Nos. 51674068, 51874079, 51804035 and 11775226), the Natural Science Foundation of Hebei Province (No. E2018501091), Hebei Province Key Research and Development Plan Project (No. 19211302D), the Fundamental Research Funds for the Central Universities (Nos. N172302001, N182306001, N182312007, N182304018 and N2023040) and Research Project on Distribution of Heavy Metals in Soil and Comprehensive Utilization Technology of Tailings in Typical Iron Tailing Reservoir Areas of Hebei Province (No. 802060671901).

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Authors and Affiliations

  1. School of Materials Science and Engineering, Northeastern University, Shenyang, 110819, China

    Si-Nan Li, Shao-Hua Luo, Liu Yang, Qing Wang, Ya-Hui Zhang & Xin Liu

  2. School of Resources and Materials, Northeastern University At Qinhuangdao, Qinhuangdao, 066004, China

    Si-Nan Li, Shao-Hua Luo, Liu Yang, Qing Wang, Ya-Hui Zhang & Xin Liu

  3. Key Laboratory of Dielectric and Electrolyte Functional Material Hebei Province, Qinhuangdao, 066004, China

    Si-Nan Li, Shao-Hua Luo, Liu Yang, Qing Wang, Ya-Hui Zhang & Xin Liu

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  1. Si-Nan Li
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Correspondence to Shao-Hua Luo.

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Li, SN., Luo, SH., Yang, L. et al. Synthesis and electrochemical properties of LiFePO4 cathode material by ionic thermal method using eutectic mixture of tetramethyl ammonium chloride–urea. Rare Met. 40, 3477–3484 (2021). https://doi.org/10.1007/s12598-021-01783-4

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