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The preparation method of sodium vanadium fluorophosphate

The technology of sodium vanadium fluorophosphate and phosphoric acid is applied in the field of preparation of spherical sodium vanadium fluorophosphate, which can solve the problems of poor electrochemical performance of materials, serious agglomeration of material particles, easy loss of fluorine elements, etc. The effect of not easy to agglomerate

Active Publication Date: 2020-12-08
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods are relatively cumbersome, long process, high synthesis temperature, serious particle agglomeration of the obtained material, easy loss of fluorine element, resulting in poor electrochemical performance of the material

Method used

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  • The preparation method of sodium vanadium fluorophosphate
  • The preparation method of sodium vanadium fluorophosphate
  • The preparation method of sodium vanadium fluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Dissolve ammonium dihydrogen phosphate and ammonium metavanadate at a molar ratio of 1:1 in deionized water, and then add oxalic acid 3 times the theoretical molar amount required for vanadium to be oxidized to trivalent vanadium, and control the total concentration to 0.5 mol / L, stirred at room temperature for 0.5h; the solution was subjected to spray pyrolysis at 600°C under an argon atmosphere (injection rate was 60ml / h, air intake volume was 3L / min), and vanadium phosphate powder was collected;

[0049] Mix the collected vanadium phosphate and sodium fluoride at a molar ratio of 1:1 and manually grind them for 1 hour, and then incubate at 500°C, 550°C, and 600°C for 4 hours in an argon atmosphere to obtain NaVPO with a spherical structure. 4 F. The obtained product was packed into a button battery to measure its charge-discharge specific capacity and rate performance, and the charge-discharge was carried out at different rates, and the first-time discharge specific...

Embodiment 2

[0053] Dissolve ammonium dihydrogen phosphate and ammonium metavanadate in deionized water at a molar ratio of 1:1, and then add oxalic acid according to 3 times the theoretical molar amount required for vanadium to be oxidized to trivalent vanadium, and control the total concentration to 0.5 mol / L, stirred at room temperature for 0.5h; the solution was subjected to spray pyrolysis at 600°C under an argon atmosphere (injection rate was 100ml / h, air intake volume was 2L / min), and vanadium phosphate powder was collected;

[0054] The collected vanadium phosphate and sodium fluoride were mixed and mechanically ground at a molar ratio of 1:1 for 0.5 h, and then placed in an argon atmosphere at 550 ° C for 4, 6, and 8 h to obtain NaVPO with a spherical structure. 4 F. The obtained product was assembled into a button battery to measure its charge-discharge specific capacity and rate performance, and the charge-discharge was carried out at different rates, and its first-time dischar...

Embodiment 3

[0058] Dissolve triammonium phosphate and vanadium pentoxide in deionized water at a molar ratio of 1:1, then add adipic acid according to 1 times the theoretical molar amount required for vanadium to be oxidized to trivalent vanadium, and control the total concentration to 0.1 mol / L, stirred at room temperature for 1 h; the solution was subjected to spray pyrolysis at 500°C under an argon atmosphere (injection rate was 110ml / h, air intake volume was 6L / min), and vanadium phosphate powder was collected;

[0059] Mix the collected vanadium phosphate, ammonium fluoride and sodium acetate according to the molar ratio of 1:1:1 and manually grind them for 2 hours, then place them in a nitrogen atmosphere at 650°C for 2 hours to obtain NaVP with a spherical structure. 4 F. Pack the obtained product into a button battery to measure its charge-discharge specific capacity and rate performance, and the discharge specific capacity at 0.1C, 1C, 2C, and 5C rates is 130, 123, 118, and 112mA...

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Abstract

The invention provides a preparation method of sodium vanadium fluorophosphate. The preparation method comprises the steps that a low-cost pentavalent inorganic vanadium source is adopted, the vanadium source, a phosphate radical source and an organic reducing agent are mixed under normal temperature and pressure, and then a spray pyrolysis method is adopted to prepare and obtain a vanadium phosphate intermediate at a low temperature and within a short period of time; and the vanadium phosphate intermediate is further mixed with a sodium source and a fluorine source in a solid phase mode, andthe sodium vanadium fluorophosphate with good crystallinity is synthesized through calcining at a low temperature and in a short period of time. The obtained sodium vanadium fluorophosphate has a spherical shape and part of the sodium vanadium fluorophosphate is in the hollow sphere form, and the particle size is small. The vanadium phosphate intermediate is prepared by the spray pyrolysis methodin the preparation process, the process flow is short, the process is simple, the productivity is large, and the production efficiency is high.

Description

technical field [0001] The invention relates to the technical field of preparation of positive electrode materials for lithium ion batteries, in particular to a method for preparing sodium vanadium fluorophosphate, especially a method for preparing spherical sodium vanadium phosphate. Background technique [0002] Currently, fossil fuels have become the main source of electricity for our lives. Carbon dioxide gas emitted from extensive use of fossil fuels has become the main cause of global warming. Therefore, humans began to seek other renewable energy sources, such as wind energy, solar energy, and nuclear energy for power generation. However, the normal operation of the grid requires continuous and stable power supply. Since solar energy and wind energy are very dependent on the environment, weather, season and location, etc., they are considered not suitable for direct integration into the grid. To overcome this problem, chemical energy storage has been given high hope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M4/136H01M10/0525
CPCH01M4/136H01M4/5825H01M10/0525Y02E60/10
Inventor 王接喜盖晓臣柴作强颜果春李新海王志兴郭华军彭文杰胡启阳
Owner CENT SOUTH UNIV
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