无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ
研究与开发

乙醇-水体系3D纳/微米球形磷酸铁的制备与表征

  • 吴康 ,
  • 李军 ,
  • 陈明
展开
  • 四川大学化学工程学院,四川成都 610065
吴康(1994— ),男,硕士研究生,研究方向为化工新技术新工艺开发;E-mail: wk4372@163.com

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

  • Kang Wu ,
  • Jun Li ,
  • Ming Chen
Expand
  • School of Chemical Engineering,Sichuan University,Chengdu 610065,China

Received date: 2020-01-16

  Online published: 2020-06-12

摘要

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。

本文引用格式

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

Abstract

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.

参考文献

[1] 张克杰, 陈鹏, 谢旺旺 , 等. 磷酸铁锂优缺点及改性研究进展[J]. 无机盐工业, 2018,50(6):13-17.
[2] 李中, 洪建和, 何岗 , 等. 磷酸铁锂振实密度的研究进展[J]. 电子元件与材料, 2012,31(9):78-81.
[3] 梁广川 . 锂离子电池用磷酸铁锂正极材料[M]. 北京: 科学出版社, 2013.
[4] 伍凌, 李新海, 王志兴 , 等. 多孔前驱体渗碳制备LiFePO4/C[J].电池, 2008(3):163-165.
[5] 李文升, 樊勇利, 童书辉 , 等. 高振密球形FePO4·xH2O的合成研究[J]. 电源技术, 2013,37(6):950-952.
[6] 张震, 蒲薇华, 任建国 , 等. 控制结晶法制备球形磷酸铁的团聚尺寸模型[J]. 化学工程, 2011,39(8):20-24.
[7] 李祥 . 单分散球形磷酸铁锂粉体的制备[D]. 兰州:兰州大学, 2014.
[8] Zhang T, Xin D, Lu Y , et al. Direct precipitation for a continuous synjournal of nanoiron phosphate with high purity[J]. Industrial & Engineering Chemistry Research, 2014,53(16):6723-6729.
[9] Wang J, Wang M, Zhang T , et al. Facile synjournal of ultrafine hema-tite nanowire arrays in mixed water-ethanol-acetic acid solution for enhanced charge transport and separation[J]. ACS Applied Materi-als & Interfaces, 2018,10(15):12594-12602.
[10] Rengaraj S, Venkataraj S, Tai C , et al. Self-assembled mesoporous hierarchical-like In2S3 hollow microspheres composed of nanofi-fibers and nanosheets and their photocatalytic activity[J]. Langmuir, 2011,27(9):5534-5541.
[11] Wu Q, Liu J, Chen S , et al. Surfactant-free synjournal of SrTiO3 hi-erarchical structures in ethanol/water mixed solvent at room tem-perature[J]. CrystEngComm, 2015,17(36):6895-6900.
[12] Wang Z, Lu Y . Facile construction of high-performance amorphous FePO4/carbon nanomaterials as cathodes of lithium-ion batteri-es[J]. ACS Applied Materials & Interfaces, 2019,11(14):13225-13233.
[13] Zhao J, Ma J, Jian Z , et al. A general phase-transfer protocol for mineral acids and its application in the large-scale synjournal of highly nanoporous iron phosphate in nonaqueous solvent[J]. Indu-strial & Engineering Chemistry Research, 2012,51(37):12025-12030.
[14] Qian L, Xia Y, Zhang W , et al. Electrochemical synjournal of meso-porous FePO4 nanoparticles for fabricating high performance LiFePO4/C cathode materials[J]. Microporous and Mesoporous Materials, 2012,152:128-133.
文章导航

/