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阳极氧化法制备磷酸铁锂前驱体FePO₄·2H₂O的工艺优化

Process Optimization for the Preparation of the Lithium Iron Phosphate Precursor FePO·2HO by Anodic Oxidation Method.

作者信息

Shao Yang, Liu Ziyuan, Li Chengping, Liu Ying, Zhang Zhengfu, Wan Rundong, Wang Jinsong, Yang Xiaoping, Bao Rui, Zhang Yingjie, Yi Jianhong, Dong Peng, Wang Ding

机构信息

Faculty of Materials Science and Engineering, Kunming University of Science and Technology, Kunming 650093, China.

Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming 650093, China.

出版信息

Materials (Basel). 2025 May 29;18(11):2555. doi: 10.3390/ma18112555.

Abstract

Iron phosphate (FePO·2HO) was synthesized via anodic oxidation using nickel-iron alloy composition simulates from laterite nickel ore as the anode and graphite electrodes as the cathode, with phosphoric acid serving as the electrolyte. A uniform experimental design was employed to systematically optimize the synthesis parameters including voltage, electrolyte concentration, electrolysis time, and degree of acidity or alkalinity (pH). The results indicate that the addition of cetyltrimethylammonium bromide (CTAB) surfactant effectively modulated the morphology of the anodic oxidation products. The optimized conditions were determined to be an electrolyte concentration of 1.2 mol/L, a voltage of 16 V, a pH of 1.6, an electrolysis time of 8 h, and a 3% CTAB addition. Under these conditions, the synthesized FePO·2HO exhibited enhanced performance as a lithium-ion battery precursor. Specifically, the corresponding LiFePO/C cathode delivered an initial discharge capacity of 157 mA h g at 0.2 C, retaining 99.36% capacity after 100 cycles. These findings provide valuable insights and theoretical foundations for the efficient preparation of iron phosphate precursors, highlighting the significant impact of optimized synthesis conditions on the electrochemical performance of lithium iron phosphate.

摘要

以模拟红土镍矿的镍铁合金成分为阳极、石墨电极为阴极,磷酸为电解液,通过阳极氧化法合成了磷酸铁(FePO₄·2H₂O)。采用均匀实验设计系统优化合成参数,包括电压、电解液浓度、电解时间以及酸碱度(pH值)。结果表明,添加十六烷基三甲基溴化铵(CTAB)表面活性剂有效调控了阳极氧化产物的形貌。确定优化条件为电解液浓度1.2 mol/L、电压16 V、pH值1.6、电解时间8 h以及添加3%的CTAB。在此条件下,合成的FePO₄·2H₂O作为锂离子电池前驱体表现出增强的性能。具体而言,相应的LiFePO₄/C阴极在0.2 C下的初始放电容量为157 mA h/g,100次循环后容量保持率为99.36%。这些发现为磷酸铁前驱体的高效制备提供了有价值的见解和理论基础,突出了优化合成条件对磷酸铁锂电化学性能的重大影响。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/55f7/12155975/f43a8ecc95a9/materials-18-02555-g001.jpg

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