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Preparation method of carbon-coated lithium iron phosphate hollow nanospheres

A technology of carbon-coated lithium iron phosphate and lithium iron phosphate, which is applied to electrical components, battery electrodes, circuits, etc., can solve problems such as poor conductivity, low tap density, and small diffusion coefficient of lithium ions, and achieve a simple process Effect

Inactive Publication Date: 2017-12-22
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Lithium iron phosphate also has many shortcomings: one is the low tap density
Second, the conductivity is poor and the diffusion coefficient of lithium ions is small

Method used

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  • Preparation method of carbon-coated lithium iron phosphate hollow nanospheres
  • Preparation method of carbon-coated lithium iron phosphate hollow nanospheres
  • Preparation method of carbon-coated lithium iron phosphate hollow nanospheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) Preparation of lithium phosphate precursor:

[0034] Mix 20 mL of polyethylene glycol 600 and 20 mL of deionized water as a binary solvent.

[0035] Dissolve 0.008mol phosphoric acid and 0.016mol lithium hydroxide monohydrate in 15mL binary solvent, stir magnetically for 15 minutes to form a reaction system. After the reaction is completed, centrifuge at 5000rpm for 5 minutes, take the solid phase and wash it with water and ethanol 3 times respectively. Dry for 6 hours in an environment of 60°C to obtain a lithium phosphate precursor.

[0036] 2) Preparation of hollow lithium iron phosphate nanospheres:

[0037] Add 0.003 mol of the lithium phosphate precursor to 100 mL of ethylene glycol, add 0.0015 mol of ferrous chloride tetrahydrate while stirring, and sonicate for 30 minutes while stirring.

[0038] Pour the upper reaction system into a 150mL autoclave while stirring. After sealing, put it into a high-temperature blast box and heat to 180°C for 3 hours. After cooling to ...

Embodiment 2

[0042] 1) Preparation of lithium phosphate precursor:

[0043] Mix 20 mL of polyethylene glycol 600 and 60 mL of deionized water as a binary solvent.

[0044] Dissolve 0.008mol phosphoric acid and 0.024mol lithium hydroxide monohydrate in 20mL binary solvent, stir magnetically for 15 minutes to form a reaction system. After the reaction is completed, centrifuge at 5000rpm for 5 minutes, take the solid phase and wash it with water and ethanol 3 times respectively. Dry for 6 hours in a 60°C environment to obtain a lithium phosphate precursor.

[0045] 2) Preparation of hollow lithium iron phosphate nanospheres:

[0046] Add 0.002 mol of the lithium phosphate precursor to 80 mL of ethylene glycol, add 0.002 mol of ferrous chloride tetrahydrate while stirring, and sonicate for 30 minutes while stirring.

[0047] Pour the upper reaction system into a 150mL autoclave while stirring. After sealing, put it into a high-temperature blast box and heat to 180°C for 3 hours. After cooling to room t...

Embodiment 3

[0051] 1) Preparation of lithium phosphate precursor:

[0052] Mix 20 mL of polyethylene glycol 600 and 160 mL of deionized water as a binary solvent.

[0053] Dissolve 0.008mol phosphoric acid and 0.04mol lithium hydroxide monohydrate in 40mL binary solvent, stir magnetically for 15 minutes to form a reaction system. After the reaction is completed, centrifuge at 5000rpm for 5 minutes, take the solid phase and wash it with water and ethanol 3 times respectively. Dry for 6 hours in a 60°C environment to obtain a lithium phosphate precursor.

[0054] 2) Preparation of hollow lithium iron phosphate nanospheres:

[0055] Take 0.001 mol of lithium phosphate precursor and add it to 100 mL of ethylene glycol, add 0.003 mol of ferrous chloride tetrahydrate while stirring, and sonicate for 30 minutes while stirring.

[0056] Pour the upper reaction system into a 150mL autoclave while stirring. After sealing, put it into a high-temperature blast box and heat to 180°C for 3 hours. After cooling ...

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Abstract

The invention discloses a preparation method of carbon-coated lithium iron phosphate hollow nanospheres and belongs to the technical field of lithium-ion battery materials. Polyethylene glycol 600 and deionized water are mixed, the obtained mixture is mixed with phosphoric acid and lithium hydroxide monohydrate for a reaction, and a lithium phosphate precursor is obtained; the lithium phosphate precursor is mixed with ethylene glycol and ferrous chloride tetrahydrate, ultrasonic treatment is performed for 30 min, the obtained mixture is placed in an autoclave to be subjected to a sealed heating reaction, and lithium iron phosphate hollow nanospheres are prepared; the lithium iron phosphate hollow nanospheres are dipped in a sucrose aqueous solution, the dipped lithium iron phosphate hollow nanospheres are dried and calcined in a nitrogen atmosphere, and the carbon-coated lithium iron phosphate hollow nanospheres are obtained. Nano spherical lithium phosphate is taken as a self-sacrifice template, a template removal step is omitted during preparation, the method adopts a convenient process, the microstructure of lithium iron phosphate can be effectively controlled, and high-purity lithium iron phosphate hollow nanospheres can be obtained.

Description

Technical field [0001] The invention belongs to the technical field of lithium ion battery materials, and specifically relates to a preparation method of lithium iron phosphate nano hollow spheres. Background technique [0002] Lithium Iron Phosphate (LiFePO 4 ) Is ortho-lithium phosphate with an orthorhombic olivine structure and belongs to the Pbmn space group. In the crystal structure, 4 LiFePO 4 Form a unit cell, the space skeleton is made of FeO 6 Octahedron and PO 4 Tetrahedral composition, one FeO 6 The octahedron and two LiO 6 Octahedron and a PO 4 Tetrahedrons are coedges, and each PO 4 The tetrahedron is also associated with two LiO 6 Octahedrons share edges. LiO 6 The hexahedrons are connected together on the same side and parallel to the b-axis, forming a migration channel for lithium ions. [0003] The electrochemical performance of lithium iron phosphate is closely related to its structure. In the process of lithium deintercalation, after the lithium ions are remove...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M4/583
CPCH01M4/485H01M4/583Y02E60/10
Inventor 陈铭陆俊杰曹圣平姜晖赵荣芳李文龙
Owner YANGZHOU UNIV
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