首页|共沉淀—喷雾干燥法制备类球形磷酸铁前驱体及其性能研究

共沉淀—喷雾干燥法制备类球形磷酸铁前驱体及其性能研究

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研究了以七水合硫酸亚铁(FeSO4·7H2O)和磷酸二氢铵(NH4H2PO4)为原料,采用共沉淀—喷雾干燥法制备类球形电池级磷酸铁,考察了表面活性剂十六烷基三甲基溴化铵(CTAB)加入量、反应时间、溶液pH对磷酸铁物相和粒径的影响,并利用激光粒度仪、X射线粉末衍射仪、热重分析仪、场发射扫描电镜等对产物进行了表征.结果表明:在Fe/P物质的量比为1/1.01、CTAB加入量0.04 g、反应时间1 h、溶液pH=3.0条件下,磷酸铁粒径分布范围最小,为300～500 nm,且呈较为规则的类球形;以类球形磷酸铁作为前驱体铁源,经球磨混合烧结制备的磷酸铁锂,在0.1 C下放电比容量为150.14 mAh/g,1 C循环200次后保持率为98.9％,性能良好.
Preparation and Characterization of Spherical-like Ferric Phosphate Precursors by Co-precipitation—Spray-drying Method
The preparation of spherical-like battery-grade ferric phosphate by co-precipitation—spray-drying method was investigated using ferrous sulfate heptahydrate(FeSO4·7H2O)and ammonium dihydrogen phosphate(NH4 H2 PO4)as raw materials.The effects of the addition of the surfactant cetyltrimethyl ammonium bromide(CTAB),reaction time,and solution pH on the physical phase and particle size of ferric phosphate were examined.The products were characterized by a laser particle sizer,X-ray powder diffractometer,thermogravimetric analyzer,and field emission scanning electron microscope.The results indicate that under the conditions of a Fe/P molar ratio of 1/1.01,CTAB addition of 0.04 g,reaction time of 1 h,and solution pH of 3.0,the ferric phosphate exhibits the smallest particle size distribution,ranging from 300 to 500 nm,and displays more uniform spherical morphology.Moreover,lithium iron phosphate is prepared by ball milling,mixing and sintering,using the spherical-like ferric phosphate as the precursor iron source.The specific discharge capacity of lithium iron phosphate is 150.14 mAh/g at 0.1 C,and the retention rate is 98.9％after 200 cycles at 1 C,the performance is good.

ferric phosphateco-precipitation methodspray-dryingspherical-likelithium iron phosphatelithium batterypreparationperformance

李习达、刘礼俊、李中林、廖昌茂、李义兵

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桂林理工大学材料科学与工程学院,广西桂林 541004

桂林理工大学有色金属与材料加工新技术教育部重点实验室,广西桂林 541004

磷酸铁 共沉淀法 喷雾干燥 类球形 磷酸铁锂 锂电池 制备 性能

国家自然科学基金-联合基金-重点支持项目国家自然科学基金-青年科学基金项目广西科技计划项目(重大专项)

U23A2055752204358桂科AA22068078

2024

10.13355/j.cnki.sfyj.2024.04.014

湿法冶金
核工业北京化工冶金研究院

湿法冶金

北大核心
影响因子：0.631
ISSN：1009-2617
年,卷(期)：2024.43(4)