乙醇-水体系3D纳/微米球形磷酸铁的制备与表征
收稿日期: 2020-01-16
网络出版日期: 2020-06-12
Synthesis and characterization of 3D nano/micro spherical iron phosphate in ethanol-water system
Received date: 2020-01-16
Online published: 2020-06-12
提出了一种在温和条件下制备高振实密度球形磷酸铁的简单方法。制备过程中无需引入碱性物质调节pH和添加其他模板剂,仅以九水合硝酸铁[Fe(NO3)·9H2O]和磷酸(H3PO4)为原料,在乙醇-水体系中即可制备3D纳/微米球形磷酸铁(记为FPE)。采用扫描电镜(SEM)、激光粒度仪、X射线衍射仪(XRD)、热重-差式扫描量热仪(TG-DSC)、比表面积测试仪(BET)等对制备的磷酸铁进行表征分析。结果显示,制备的磷酸铁具有3D纳/微米球形结构,平均一次粒径为27.2 nm,二次粒径D50为3.75 μm。FPE的组成为二水合磷酸铁(FePO4·2H2O),纯度较高,具有介孔结构,平均孔径为2.75 nm,比表面积为22.41 cm 2/g,同时具有较高的振实密度(1.34 g/cm 3)。3D纳/微米球形磷酸铁制备方法简单,性能优异,以其为前驱体制备的磷酸铁锂(LiFePO4/C)具有较高的振实密度(1.46 g/cm 3),在0.2C倍率下的放电比容量为157.9 mA·h/g。
吴康 , 李军 , 陈明 . 乙醇-水体系3D纳/微米球形磷酸铁的制备与表征[J]. 无机盐工业, 2020 , 52(6) : 41 -45 . DOI: 10.11962/1006-4990.2019-0409
A simple method for preparing high tap density spherical iron phosphate under mild conditions was proposed.Iron phosphate with 3D nano/micro spherical structure(FPE) was prepared by using ferric nitrate[Fe(NO3)·9H2O] and phospho-ric acid(H3PO4) as raw materials in a mixed solution of ethanol and water without introducing alkaline substances for pH ad-justing and other templating agents.The obtained products were characterized by SEM,laser particle size analyzer,XRD,TG-DSC and BET.The results indicated that the iron phosphate prepared by this method had a 3D nano/micro spherical struc-ture,an average primary particle diameter of 27 nm and a secondary particle diameter D50 of 3.75 μm.The composition of FPE was iron phosphate dihydrate FePO4·2H2O with high purity.The FPE had a mesoporous structure with average pore diameter of 2.75 nm,specific surface area of 22.41 cm 2/g and high tap density of 1.34 g/cm 3,3D nano/micro spherical iron phosphate is simple to prepare and has excellent performance.The lithium iron phosphate LiFePO4/C prepared by using the precursor FPE has a high tap density of 1.46 g/cm 3,and the discharge capacity is 157.9 mA·h/g at 0.2C.
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