摘要
为提高锂离子电池正极材料前驱体磷酸铁(FePO4)的合成效率与产品性能,以硫酸亚铁和磷酸铵为原料,采用“氧化沉淀-转化”两步法制备磷酸铁,探究了氧化剂过氧化氢添加量、投料速率、反应温度等关键参数对产物粒径分布(D_(50))、纯度及铁磷比的影响。确定的优化工艺条件为:氧化阶段过氧化氢添加量为理论量的1.25倍、投料时长50 min、氧化温度40℃、氧化时间2 h,沉淀阶段磷酸铵投料时长50~55min、沉淀温度40℃,转化阶段转化温度90℃、磷酸浓度0.6 mol/L。在此条件下成功制备出D_(50)为3.0μm、杂质含量低于0.01%、Fe/P物质的量比0.997的高纯度磷酸铁。SEM与XRD表征结果显示产品为片状一次颗粒堆积而成的规则球形二次颗粒,结晶度良好。
To improve synthesis efficiency and performance of iron phosphate(FePO4)product,a precursor for cathode materials of lithium⁃ion batteries,a two⁃step process consisting of oxidation⁃precipitation,and conversion was proposed to prepare iron phosphate with ferrous sulfate and ammonium phosphate as raw materials.The effects of key parameters,such as addition amount of hydrogen peroxide(oxidant),feeding rate,and reaction temperature,on the particle size distribution(D_(50)),purity,and Fe/P ratio of the product were investigated.The optimized process conditions were determined as follows:oxidation at a temperature of 40℃for 2 h by adding hydrogen peroxide at an amount of 1.25 times the theoretical dosage and feeding material for 50 min in the oxidation stage;precipitation at a temperature of 40℃by feeding ammonium phosphate for 50~55 min in the precipitation stage;and with phosphoric acid at concentration of 0.6 mol/L and a temperature of 90℃for the conversion stage.As a result,a high⁃purity iron phosphate with D_(50) of 3.0μm,impurity content lower than 0.01%,and Fe/P at a molar ratio of 0.997 can be successfully prepared.SEM and XRD characterization results show that the product consists of regular spherical secondary particles formed with densely stacked primary lamellar crystals,presenting higher degree of crystallinity.
作者
黄欢
张仲懿
兰倩
王致富
程琦
HUANG Huan;ZHANG Zhongyi;LAN Qian;WANG Zhifu;CHENG Qi(CATARC Automotive Inspection Center(Wuhan)Co.,Ltd.,Wuhan 430056,Hubei,China;Wuhan Plastic Omnium Auto Inergy Co.,Ltd.,Wuhan 430223,Hubei,China;Yichang Brunp Recycling Technology Co.,Ltd.,Yichang 443215,Hubei,China;Yichang City Key Laboratory of Battery Recycling and Green and Low-Carbon,Yichang 443215,Hubei,China;Guangdong Provincial Key Laboratory of Battery Recycling and Reuse,Foshan 528137,Guangdong,China;The National-Local Joint Engineering Research Center for Recycling of New Energy Vehicle Traction Batteries,Foshan 528137,Guangdong,China)
出处
《矿冶工程》
北大核心
2026年第1期197-201,共5页
Mining and Metallurgical Engineering
关键词
锂离子电池
磷酸铁锂
磷酸铁
液相沉淀法
工艺优化
lithium⁃ion battery
lithium iron phosphate
iron phosphate
liquid phase precipitation
process optimization
