Preparation method and application of lithium vanadium fluorophosphate

A technology for compounding lithium vanadium fluorophosphate and vanadium source is applied in the preparation/purification of carbon, chemical instruments and methods, phosphorus compounds, etc., and can solve problems such as side reactions and reduction of product purity.

Active Publication Date: 2021-05-28
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

The high-temperature sintering process undergoes a slow cooling process, and the resulting product is prone to side reactions at around 500 degrees (LiVPO 4 F is easily decomposed into lithium vanadium phosphate and VF gas), which reduces the purity of the prepared product

Method used

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  • Preparation method and application of lithium vanadium fluorophosphate
  • Preparation method and application of lithium vanadium fluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] VPO 4 Preparation of LiVPO as precursor by @C 4 F@C

[0030] Mix 0.05mol ammonium metavanadate, 0.05mol ammonium dihydrogen phosphate, and an appropriate amount of citric acid in a beaker filled with 200ml of water, and stir mechanically at 80°C for 10 hours to obtain mixed solution A; the mass of citric acid is ammonium metavanadate 40% of mass;

[0031] Put the prepared mixed solution A in an oven at 100 degrees to dry for 12 hours, take it out and pulverize it, put it in a tube furnace with an argon atmosphere at 750 ° C for 6 hours at a constant temperature, take it out and grind it to obtain black carbon-composite vanadium phosphate Powder (VPO 4 @C);

[0032] The resulting VPO 4 @C is mixed with 0.05mol ammonium fluoride, 0.05mol lithium hydroxide, and 80ml water to obtain a mixed solution B, and the mixed solution B is placed in a 180-degree reaction kettle for 48 hours of solvothermal reaction, suction filtered, and dried. LiVPO can be obtained by grinding...

Embodiment 2

[0034] V 2 o 3 Preparation of LiVPO as precursor by @C 4 F@C

[0035] Put 0.05mol ammonium metavanadate and an appropriate amount of citric acid into a beaker containing 200ml of water and mix them, and mechanically stir at 80°C for 10 hours to obtain a mixed solution A; the mass of citric acid is 50% of the mass of ammonium metavanadate;

[0036] Put the prepared mixed solution A in a 100-degree oven to dry for 12 hours, take it out and pulverize it, put it in a tube furnace with an argon atmosphere at 750 ° C for 6 hours, take it out and pulverize it to obtain black V 2 o 3 @C powder;

[0037] The resulting V 2 o 3 Mix @C with 0.05mol ammonium fluoride, 0.05mol ammonium dihydrogen phosphate, 0.05mol lithium hydroxide, and 80ml water to obtain a mixed solution B, and place the mixed solution B in a reactor at 180 degrees for 48 hours of solvothermal reaction , suction filtration, drying, and grinding to obtain LiVPO 4 F@C powder;

Embodiment 3

[0039] VPO 4 @C is the precursor to prepare LiVPO 4 F@C

[0040] Mix 0.05mol ammonium metavanadate, 0.05mol ammonium dihydrogen phosphate, and an appropriate amount of citric acid in a beaker filled with 200ml of water, and stir mechanically at 80°C for 10 hours to obtain mixed solution A; the mass of citric acid is ammonium metavanadate 40% of mass;

[0041] Put the prepared mixed solution A in an oven at 100 degrees to dry for 12 hours, take it out and pulverize it, put it in a tube furnace with an argon atmosphere at 600 ° C for 10 hours at a constant temperature, take it out and pulverize it to obtain black carbon-composite vanadium phosphate Powder (VPO 4 @C);

[0042] The resulting VPO 4@C is mixed with 0.05mol ammonium fluoride, 0.05mol lithium hydroxide, and 80ml water to obtain a mixed solution B, and the mixed solution B is placed in a 180-degree reaction kettle for 48 hours of solvothermal reaction, suction filtered, and dried. LiVPO can be obtained by grindin...

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Abstract

The invention provides a preparation method and application of lithium vanadium fluorophosphate, and the method provided by the invention is summarized into two steps: 1, preparing carbon-coated vanadium phosphate (VPO4 (at) C) or carbon-coated vanadium trioxide (V2O3 (at) C) by a sol-gel method; and 2, preparing the carbon composite LiVPO4F through a low-temperature solvothermal method. In the first step, the sol-gel method is used for preparing carbon-coated VPO4 (at) C or V2O3 (at) C, and a carbon composite precursor with small particle size and uniform distribution can be obtained. In the second step, low-temperature hydrothermal synthesis of LiVPO4F is adopted, on one hand, volatilization of F is effectively avoided, and a high-purity LVPF material is prepared at low temperature; on the other hand, the crystallization phase formation of the LVPF is realized, and the volatilization of F at high temperature to generate impurities is avoided. The obtained LiVPO4F (at) C powder has nanoscale morphology, is very high in crystalline phase purity, and has excellent performance close to theoretical specific capacity at low magnification.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrode materials, and in particular relates to a preparation method and application of lithium vanadium phosphate. Background technique [0002] The cathode material of a lithium-ion battery is the key to determining the energy density of the battery. The preferred cathode material should have high working voltage, high capacity and stable structure. Among many cathode materials, lithium vanadium fluorophosphate (LiVPO 4 F, referred to as LVPF for short) has attracted extensive attention due to its high voltage (4.2V), high theoretical specific capacity (153mAh / g), and stable structure. However, the inherent conductivity of the above compounds is low, which limits their performance. In order to improve the electrical conductivity of the material, the commonly used method is to add carbon source to form a carbon composite lithium vanadium phosphate compound through the sol-gel met...

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
CPCC01B25/455C01B32/05H01M4/5825H01M4/625H01M10/0525C01P2006/40C01P2004/03C01P2002/72C01P2006/80Y02E60/10
Inventor 郑琼李先锋韩建鑫凌模翔张华民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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