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Preparation method of spherical lithium ion battery positive electrode material LiVPO4F

A technology for lithium-ion batteries and cathode materials, applied in the preparation of cathode materials for lithium-ion batteries, in the field of spherical lithium-ion battery cathode materials LiVPO4F, can solve the problems of difficult preparation of pure-phase LiVPO, complex synthesis process, low electronic conductivity, etc., to achieve Conducive to the effect of transmission de-embedding and simplifying the experimental process

Active Publication Date: 2014-06-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] LiVPO 4 Although F has a three-dimensional framework structure, its ionic conductivity is greatly improved, but its synthesis process is complicated, and pure phase LiVPO 4 F is difficult to prepare and has low electronic conductivity, which severely limits its electrochemical performance during high-rate charge and discharge.

Method used

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  • Preparation method of spherical lithium ion battery positive electrode material LiVPO4F
  • Preparation method of spherical lithium ion battery positive electrode material LiVPO4F
  • Preparation method of spherical lithium ion battery positive electrode material LiVPO4F

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh 0.91g of vanadium pentoxide, 1.15g of diammonium hydrogen phosphate, 0.13g of lithium fluoride, and 1.4g of citric acid, add 1000mL of deionized water, dissolve them in the autoclave, and adjust the pH to 3. The heating temperature is 300°C, the heating time is 15H, and the internal pressure of the autoclave is 4MPa; cool to room temperature, take out and filter, and dry the filtered product in a vacuum oven at 80°C. Fully grind the dried powder in an agate mortar, then place it in a sintering furnace, and sinter it at 600°C, 650°C, 700°C, 750°C for 2 hours under an argon atmosphere, and then naturally cool down to room temperature to obtain the finished product LiVPO 4 F. The obtained product was analyzed by XRD, in which pure phase LiVPO was obtained at 600°C and 650°C 4 F, the products obtained at other temperatures have Li 3 V 2 (PO 4 ) 3 and V 2 o 3 Miscellaneous. The microscopic morphology of the obtained materials was detected by SEM. The obtained ...

Embodiment 2

[0029] Weigh 0.91g of vanadium pentoxide, 1.15g of diammonium hydrogen phosphate, 0.13g of lithium fluoride, and 1.4g of citric acid, add 1000mL of deionized water, dissolve them in the autoclave, and adjust the pH to 3. The heating temperature is 300°C, the heating time is 15H, and the internal pressure of the autoclave is 4MPa; cool to room temperature, take out and filter, and dry the filtered product in a vacuum oven at 80°C. Fully grind the dried powder in an agate mortar, then place it in a sintering furnace, sinter at 650°C under an argon atmosphere for 0.5h, 2h, 4h, 6h, and then cool down naturally to room temperature to obtain the finished product LiVPO 4 F. Gained product all obtains pure phase LiVPO through XRD analysis 4 F. The microscopic morphology of the obtained materials detected by SEM is spherical, and the size of the spherical materials gradually increases with the prolongation of sintering time. The obtained product was assembled into an experimental bu...

Embodiment 3

[0033] Weigh 0.91g of vanadium pentoxide, 1.15g of diammonium hydrogen phosphate, 0.13g of lithium fluoride, 1.4g of citric acid, add 1000mL of deionized water, dissolve them in the autoclave, adjust the pH=1, 6, 8 , 12. The heating temperature of the autoclave is 300°C, the heating time is 15H, and the internal pressure of the autoclave is 4MPa; cool to room temperature, take out and filter, and dry the filtered product in a vacuum oven at 80°C. The dried powder was fully ground in an agate mortar, then placed in a sintering furnace, sintered at 650°C for 2 hours under an argon atmosphere, and then cooled naturally to room temperature to obtain the finished LiVPO 4 F. Gained product all obtains pure phase LiVPO through XRD analysis 4 F, through SEM detection, only the microscopic morphology of the material obtained from No. 1 is spherical, and the others have no special morphology. . The obtained product was assembled into an experimental button battery to measure its char...

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Abstract

The invention discloses a preparation method of a spherical lithium ion battery positive electrode material fluorine lithium vanadium phosphate (LiVPO4F), which belongs to the technical field of a lithium ion battery. The preparation method is characterized in that the lithium ion battery positive electrode material LiVPO4F is prepared by a liquid-phase high-temperature high-pressure method. The preparation method comprises the specific steps of placing a lithium source, a vanadium source and a phosphorous source in a stoichiometric ratio of 1:1:1 into a high-pressure reaction kettle, adding an organic carbon source as a reducing agent, adjusting the pH value to be 3 with deionized water as a solvent, heating the mixture for 15h under the condition that the pressure is 4MPa and the temperature is 300 DEG C to obtain a precursor of the spherical LiVPO4F; grinding and tabletting the spherical LiVPO4F, placing an amorphous precursor into a tubular sintering furnace, sintering at the temperature of 650 DEG C under a non-oxidization atmosphere for 2h, and cooling the precursor to the room temperature to obtain the spherical positive electrode material LiVPO4F. The synthesis method is simple and easy to control, the appearance of the material is unique, and the electrochemical performance is excellent.

Description

technical field [0001] The invention relates to a method for preparing a positive electrode material of a lithium ion battery, in particular to a method for preparing a spherical lithium ion battery positive electrode material LiVPO by using liquid phase high temperature and high pressure technology. 4 F's method. It belongs to the technical field of lithium ion batteries. Background technique [0002] LiVPO 4 F is a new type of cathode material for lithium-ion batteries. LiVPO 4 F inherits the advantages of polyanion lithium-ion battery positive electrode material safety, environmental protection, good thermal stability, and LiVPO 4 The special spatial 3D network structure of F provides a good shuttle channel for the deintercalation process of lithium ions, so it has excellent charge and discharge performance and high rate performance. At the same time, the addition of fluorine can reduce the surface erosion of the electrode material by the electrolyte, so that the mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397
CPCY02E60/122H01M4/1397H01M4/5825H01M10/0525H01M2004/021H01M2004/028Y02E60/10
Inventor 张宝郑俊超韩亚东张佳峰
Owner CENT SOUTH UNIV