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A kind of preparation method of polynuclear core-shell structure phosphate series composite positive electrode material for lithium ion battery

A composite cathode material, lithium-ion battery technology, applied in battery electrodes, positive electrodes, secondary batteries, etc., can solve the problems of slow ion transmission, low electronic conductivity, etc., and achieve the improvement of kinetic factors and kinetic factors. Effect

Active Publication Date: 2017-12-19
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, among these polyanionic phosphate-based positive electrode materials, including LiFePO, which has been commercialized or may be commercialized 4 , LiMnPO 4 , LiVPO 4 F, Li 3 V 2 (PO 4 ) 3 etc. are limited by kinetic factors such as low electronic conductivity and slow ion transport in practical applications.

Method used

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  • A kind of preparation method of polynuclear core-shell structure phosphate series composite positive electrode material for lithium ion battery
  • A kind of preparation method of polynuclear core-shell structure phosphate series composite positive electrode material for lithium ion battery
  • A kind of preparation method of polynuclear core-shell structure phosphate series composite positive electrode material for lithium ion battery

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Embodiment 1

[0022] With lithium carbonate, vanadium pentoxide, diammonium hydrogen phosphate, and lithium fluoride as raw materials, LiVPO in the obtained composite positive electrode material 4 F. Li 3 V 2 (PO 4 ) 3 with LiVOPO 4 The molar ratio is 0.1:0.4:0.5, and mix evenly; then add the reducing agent oxalic acid to the mixed material, according to the molar ratio of oxalic acid and vanadium source is 3:1, add and mix, mechanical ball mill for 8 hours, and then turn it to vacuum drying The powder was dried in an oven, fully ground the powder in an agate mortar, pressed into tablets, heat-treated at 750°C for 6 hours in an argon atmosphere, then naturally cooled to 350°C and sintered in an air atmosphere for 1 hour, and finally cooled naturally to room temperature to obtain 0.1 LiVPO 4 F 0.4Li 3 V 2 (PO 4 ) 3 0.5LiVOPO 4 of composite materials. The resulting product was formed into a button battery to measure its charge-discharge specific capacity and cycle performance. The ...

Embodiment 2

[0024] With lithium carbonate, vanadium pentoxide, diammonium hydrogen phosphate, and lithium fluoride as raw materials, LiVPO in the obtained composite positive electrode material 4 F. Li 3 V 2 (PO 4 ) 3 with LiVOPO 4 The molar ratio is 0.2:0.4:0.4, and mix evenly; then add the reducing agent oxalic acid to the mixed material, according to the molar ratio of oxalic acid and vanadium source is 3:1, add and mix, mechanical ball mill for 8 hours, and then turn it to vacuum drying The powder was dried in an oven, fully ground the powder in an agate mortar, pressed into tablets, heat-treated at 750°C for 4 hours in an argon atmosphere, then naturally cooled to 350°C and sintered in an air atmosphere for 2 hours, and finally cooled naturally to room temperature to obtain 0.2 LiVPO 4 F 0.4Li 3 V 2 (PO 4 ) 3 0.4LiVOPO 4 of composite materials. The resulting product was formed into a button battery to measure its charge-discharge specific capacity and cycle performance. The...

Embodiment 3

[0026] With lithium carbonate, vanadium pentoxide, diammonium hydrogen phosphate, and lithium fluoride as raw materials, LiVPO in the obtained composite positive electrode material 4 F. Li 3 V 2 (PO 4 ) 3 with LiVOPO 4 The molar ratio is 0.4:0.4:0.2, and mix evenly; then add reducing agent oxalic acid to the mixed material, according to the molar ratio of oxalic acid and vanadium source is 3:1, add and mix, mechanical ball mill for 8 hours, and then turn it to vacuum drying The powder was dried in an oven, fully ground the powder in an agate mortar, pressed into tablets, heat-treated at 750°C for 2 hours in an argon atmosphere, then naturally cooled to 350°C and sintered in an air atmosphere for 4 hours, and finally cooled naturally to room temperature to obtain 0.4 LiVPO 4 F 0.4Li 3 V 2 (PO 4 ) 3 0.2LiVOPO4 of composite materials. The resulting product was formed into a button battery to measure its charge-discharge specific capacity and cycle performance. The first...

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Abstract

The invention discloses a preparation method of a multi-core type phosphate compound positive electrode material with a core-shell structure for a lithium ion battery, and belongs to the technical field of lithium ion batteries. The preparation method is characterized in that the compound positive electrode material xLiVPO4F yLi3V2(PO4)3 (1-x-y)LiVOPO4 of the lithium ion battery is prepared by adopting a chemical reduction-solid phase sintering technology. The preparation method comprises the following steps: (1), blending raw materials; (2), adding a carbon source as a reducing agent, mechanically activating and then drying in a vacuum drying oven to obtain a compound precursor; (3), calcining the compound precursor obtained in the step (2) in a sintering furnace under a non-oxidation atmosphere at a temperature of 600-800 DEG C for 1-24 hours, naturally cooling to 300-700 DEG C, and sintering for 1-10 hours to obtain the multi-core type compound positive electrode material xLiVPO4F yLi3V2(PO4)3 (1-x-y)LiVOPO4 with the core-shell structure. According to the compound positive electrode material prepared by adopting the preparation method, components of cores, formed by a selfoxidation-reduction reaction, sequentially comprise LiVPO4F, Li3V2(PO4)3 and LiVOPO4 from inside to outside, and an outermost layer is of a carbon-coated microstructure. The multi-core type phosphate compound positive electrode material is special in structure components, excellent in electrochemical performance, multiple in charging and discharging platforms, easily controllable in charge state, and suitable for a power battery.

Description

technical field [0001] The invention relates to a preparation method of a lithium-ion battery positive electrode material, in particular to a method for preparing a lithium-ion battery multi-nuclear core-shell structure phosphate-based composite positive electrode material using a "chemical reduction-solid phase sintering" technology. It belongs to the technical field of lithium ion batteries. Background technique [0002] With the advent of the electronic information age, in order to meet the increasing energy demand of various mobile devices, the development of high-performance secondary lithium-ion batteries with long life, high specific power, low cost, and no pollution has become the current research trend. Lithium-ion battery cathode materials are the key components of lithium-ion batteries, and the development of cheap, high-cycle performance, and high-safety cathode materials is currently a global research hotspot. Phosphate-based cathode materials have become the f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
CPCH01M4/364H01M4/5825H01M10/0525H01M2004/028Y02E60/10
Inventor 郑俊超张宝韩亚东张佳峰
Owner CENT SOUTH UNIV
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