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A kind of preparation method of sodium vanadyl fluorophosphate cathode material for sodium ion battery

A technology for sodium vanadyl fluorophosphate and sodium ion batteries, which is applied in battery electrodes, positive electrodes, secondary batteries, etc. It can solve the problems of large material particles, irregular material appearance, and small product volume, and achieve particle size distribution. Uniformity, high product consistency, and mild reaction conditions

Active Publication Date: 2022-03-22
湖南钠邦新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sol-gel method has a complicated process, large drying shrinkage, and the obtained material has irregular appearance and is easy to agglomerate; the product obtained by the hydrothermal method is small, the purity is not high, and the particle distribution is uneven. Carry out solid-phase carbon encapsulation treatment on the obtained precipitate, the operation process is cumbersome, and the carbon encapsulation effect is not good
The solid-phase method is simple to operate, but the prepared material has large particles, uneven distribution, poor cycle stability and rate performance
Secondly, the preparation method of sodium vanadyl fluorophosphate is obtained by one-step synthesis, and there are problems such as the morphology of the material, the control of particle size, and the ease of agglomeration in the one-step synthesis.
[0006] In summary, there are still many deficiencies in the preparation methods of sodium vanadyl fluorophosphate reported at present, and there is still a lot of room for improvement in the electrical properties of the prepared sodium vanadyl fluorophosphate

Method used

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  • A kind of preparation method of sodium vanadyl fluorophosphate cathode material for sodium ion battery
  • A kind of preparation method of sodium vanadyl fluorophosphate cathode material for sodium ion battery
  • A kind of preparation method of sodium vanadyl fluorophosphate cathode material for sodium ion battery

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Embodiment 1

[0062] Add 2g of vanadium pentoxide to 48ml of deionized water, add 12ml of phosphoric acid (V / P molar ratio is 1:7~8), heat and stir at 80°C for 30 minutes to obtain a mixed solution, and put the solution at 500°C under argon Spray pyrolysis was carried out under air atmosphere (injection rate was 90ml / h, air intake rate was 4.5L / min), and vanadyl phosphate powder was collected (XRD showed that it was δ-VOPO 4 ), sodium fluoride, sodium acetate and vanadyl phosphate are compounded according to Na, F, vanadyl phosphate according to the chemical formula, and citric acid (citric acid / vanadyl phosphate molar ratio is 3:2) and 10ml of dispersant (alcohol or acetone), at a rotational speed of 650rpm, ball mill for 12 hours to obtain a precursor, the precursor was dried at 80°C for 2 hours, then pulverized, heated to 650°C for 8 hours under an argon atmosphere, and cooled to obtain sodium vanadyl fluorophosphate;

Embodiment 2

[0064] Add 2g of vanadium pentoxide to 48ml of deionized water, add 12ml of phosphoric acid (V / P molar ratio is 1:7~8), heat and stir at 80°C for 30 minutes to obtain a mixed solution, and put the solution at 100°C under argon Spray drying was carried out under air atmosphere (the air intake rate was 15L / min), and the vanadyl phosphate powder was collected after sintering at a temperature of 750°C (XRD showed that it was δ-VOPO 4 ), sodium fluoride, sodium acetate and vanadyl phosphate are compounded according to Na, F, vanadyl phosphate according to the chemical formula, and citric acid (citric acid / vanadyl phosphate molar ratio is 3:2) and 10ml of dispersant (alcohol or acetone), at a rotational speed of 650rpm, ball mill for 12 hours to obtain a precursor, the precursor was dried at 80°C for 2 hours, then pulverized, heated to 650°C for 8 hours under an argon atmosphere, and cooled to obtain sodium vanadyl fluorophosphate;

Embodiment 3

[0066] Add 2g of vanadium pentoxide into 48ml of deionized water, add 12ml of phosphoric acid (V / P molar ratio is 1:7~8), heat and stir at 80°C for 30 minutes to obtain a mixed solution, and co-mix the solution at 50°C Precipitate (the dropping rate is 15ml / h), then sinter at a temperature of 750°C, and collect vanadyl phosphate powder (XRD shows that it is δ-VOPO 4 ), sodium fluoride, sodium acetate and vanadyl phosphate are compounded according to Na, F, vanadyl phosphate according to the chemical formula, and citric acid (citric acid / vanadyl phosphate molar ratio is 3:2) and 10ml of dispersant (alcohol or acetone), at a rotational speed of 650rpm, ball mill for 12 hours to obtain a precursor, the precursor was dried at 80°C for 2 hours, then pulverized, heated to 650°C for 8 hours under an argon atmosphere, and cooled to obtain sodium vanadyl fluorophosphate;

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Abstract

The invention belongs to the technical field of positive electrode materials for sodium ion batteries, and specifically discloses a preparation method of sodium vanadyl fluorophosphate positive electrode materials for sodium ion batteries. A fluorine source, a sodium source, and vanadyl phosphate are mixed to obtain a mixture, and then in a protective atmosphere, Roast at 650-900°C to get it. The preparation method of the present invention innovatively pre-converts the P source and the vanadium source in advance, and it is found that converting it into vanadyl phosphate, and then mixing it with the fluorine source and the sodium source, can unexpectedly significantly improve the electrical properties of the prepared material, In particular, the initial capacity performance and cycle stability of the material are significantly improved.

Description

technical field [0001] The invention relates to the field of preparation of positive electrode materials for sodium ion batteries, in particular to a method for preparing sodium vanadyl fluorophosphate by a liquid phase-solid phase method. Background technique [0002] As a socially dominant electrochemical energy storage device, lithium-ion batteries have achieved good results in portable electronics (laptops, smart mobile devices, tablets, etc.), electric vehicles, and plug-in hybrid electric vehicles. application. At the same time, sodium-ion batteries have also received widespread attention due to their rich reserves of sodium resources and environmental friendliness. The research and development of sodium-ion batteries can alleviate the limited development of batteries caused by the shortage of lithium resources to a certain extent, and are considered to be the next generation of electric vehicles. It is an ideal choice for automobile power supply and large-scale energ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/455H01M4/58H01M10/054
CPCC01B25/455H01M4/582H01M4/5825H01M10/054H01M2004/028C01P2004/52C01P2004/62Y02E60/10
Inventor 张治安王涛胜孙学文赖延清张凯洪波李劼
Owner 湖南钠邦新能源有限公司
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