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Carbon-coated LiVPO4F positive electrode material as well as preparation and application thereof

A cathode material and carbon coating technology, applied in the field of carbon-coated LiVPO4F cathode material preparation, can solve problems such as difficulty in synthesizing pure phase LiVPO, achieve excellent electrochemical performance, improve electronic conductivity, and improve the effect of crystal phase purity

Active Publication Date: 2021-03-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem that the present invention mainly solves is for above-mentioned synthetic pure phase LiVPO 4 F more difficult problem while providing a fluoropolymer assisted synthesis of pure phase LiVPO 4 F / C method, LiVPO prepared 4 F has high phase purity and excellent electrochemical performance as a cathode material for lithium-ion batteries

Method used

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  • Carbon-coated LiVPO4F positive electrode material as well as preparation and application thereof
  • Carbon-coated LiVPO4F positive electrode material as well as preparation and application thereof
  • Carbon-coated LiVPO4F positive electrode material as well as preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: Taking oxalic acid, vanadium pentoxide, ammonium dihydrogen phosphate, lithium fluoride, glucose, and PTFE as initial raw materials. First weigh 3.396g of oxalic acid and dissolve it in 50ml of deionized water, stir the oxalic acid solution in an 80°C water bath for 0.5h, then weigh 2.129g of vanadium pentoxide and add it to the above oxalic acid solution and continue stirring for 0.5h; then weigh 1.345g of ammonium dihydrogen phosphate, 0.318g of lithium fluoride and 0.5g of glucose were added to the above solution, and the stirring was continued for 6h to obtain a blue colloidal liquid, which was dried at 120°C for 24h; After pre-sintering at 350 °C for 5 h in the atmosphere, it was mixed with 3.792 g of PTFE and sintered at 800 °C for 5 h to obtain a pure phase of carbon-coated LiVPO 4 F positive electrode material, the particle size is 0.5-3 microns, the obtained product is a pure phase after XRD analysis, and the carbon mass content in the material is...

Embodiment 2

[0029] Embodiment 2: Taking oxalic acid, ammonium metavanadate, phosphoric acid, lithium fluoride, PVDF, and glucose as initial raw materials. First weigh 3.396g of oxalic acid and dissolve it in 50ml of deionized water, stir the oxalic acid solution in an 80°C water bath for 0.5h, then weigh 1.368g of ammonium metavanadate and add it to the above oxalic acid solution and continue stirring for 0.5h; then weigh 1.147g of phosphoric acid, 0.318g of lithium fluoride and 0.5g of glucose were added to the above solution, and the stirring was continued for 8h to obtain a blue colloidal liquid, which was dried at 120°C for 48h; After pre-sintering at ℃ for 8 h, it was mixed with 1.515 g of PVDF and sintered at 750 °C for 5 h to obtain a pure phase of carbon-coated LiVPO 4 F cathode material. The particle size is 0.5-3 microns. The obtained product is a pure phase after XRD analysis. The carbon content in the material is about 5%. The carbon-coated LiVPO 4 F, super P and PVDF are pr...

Embodiment 3

[0030] Embodiment 3: Taking oxalic acid, vanadium pentoxide, ammonium dihydrogen phosphate, lithium fluoride, and PTFE as initial raw materials. First weigh 3.396g of oxalic acid and dissolve it in 50ml of deionized water, stir the oxalic acid solution in an 80°C water bath for 0.5h, then weigh 1.368g of ammonium metavanadate and add it to the above oxalic acid solution and continue stirring for 0.5h; then weigh Add 1.345g of ammonium dihydrogen phosphate and 0.318g of lithium fluoride to the above solution, and continue to stir for 6h to obtain a blue colloidal liquid, which is dried at 120°C for 12h; the dried product is heated at 350°C under an argon atmosphere After pre-sintering for 6 h, it was mixed with 2.215 g of PTFE and sintered at 650 °C for 4 h to obtain a pure phase of carbon-coated LiVPO 4 F positive electrode material, the particle size is 0.5-3 microns, the obtained product is a pure phase after XRD analysis, and the carbon content in the material is about 5%. ...

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Abstract

The invention discloses a preparation method of a carbon-coated LiVPO4F positive electrode material. The preparation method comprises the following steps: adding oxalic acid, citric acid or ascorbic acid into deionized water to form a transparent solution, sequentially adding a vanadium source, a lithium source, a phosphorus source and a fluorine source according to the molar ratio of 1:1:1:1 at the temperature of 20-90 DEG C, conducting uniform mixing in the solution, conducting reacting for 1-12h to form a colloidal solution, and conducting drying at the temperature of 70-140 DEG C for 6-48hto obtain a solid product; carrying out heat treatment on the dried solid product in an inert atmosphere at the temperature of 300-500 DEG C for 1-12h to obtain an intermediate product; and mixing the intermediate product with a fluorine-containing polymer (PTFE, PVDF or PCTFE) accounting for 5%-100% of the mass of the intermediate product, carrying out ball milling for 1-24 hours, and conductingsintering in an inert atmosphere at the temperature of 500-800 DEG C for 1-12 hours to obtain the pure-phase LiVPO4F / C positive electrode material. The carbon-coated LiVPO4F material prepared by theinvention has high crystalline phase purity, and the introduction of the fluorine-containing polymer not only can be used as an additional fluorine source to effectively improve the crystalline phasepurity of the material, but also can be used as a carbon source to coat the surface of LiVPO4F to improve the electron conductivity of the material, thereby obtaining excellent electrochemical properties.

Description

Technical field [0001] The invention relates to the field of lithium-ion battery cathode materials, and specifically to a carbon-coated LiVPO 4 Preparation method of F cathode material. Background technique [0002] Lithium-ion batteries have been widely used as the main power source for portable electronic devices, communication tools, and electric vehicles. In lithium-ion batteries, the cathode material plays a very important role in its performance. Lithium vanadium fluorophosphate (LiVPO 4 F) As a new type of polyanion cathode material, due to its high theoretical specific capacity (156mAh g -1 ), higher voltage platform (~4.2V), excellent thermal stability and other characteristics, it has good development potential; the team led by J. Barker synthesized LiVPO for the first time in 2003 through a solid-phase method 4 F, proving that it has good electrochemical properties. But pure phase LiVPO 4 The synthesis conditions of F are relatively harsh, and a rapid coolin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455C01B32/05H01M4/58H01M4/62H01M10/0525
CPCC01B25/455C01B32/05H01M4/5825H01M4/625H01M10/0525C01P2004/80C01P2004/61C01P2004/62Y02E60/10
Inventor 郑琼李先锋张华民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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