乙醇-水体系3D纳/微米球形磷酸铁的制备与表征

doi:10.11962/1006-4990.2019-0409

Abstract

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.

Key words: ethanol-water system, spherical iron phosphate, nano/micro structure

CLC Number:

Wu Kang,Li Jun,Chen Ming. Synthesis and characterization of 3D nano/micro spherical iron phosphate in ethanol-water system[J]. Inorganic Chemicals Industry, 2020, 52(6): 41-45.

Figures/Tables 6

References 14

[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.

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Inorganic Acid-Base-Salt Committee of CIESC

Synthesis and characterization of 3D nano/micro spherical iron phosphate in ethanol-water system

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