A kind of preparation method and application of lithium vanadium fluorophosphate

A technology of composite vanadium lithium fluorophosphate and vanadium source, which is applied in the direction of carbon preparation/purification, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of side reactions and product purity reduction, and achieve small particle size and crystal phase purity High, to avoid the effect of volatilization

Active Publication Date: 2022-07-08
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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  • A kind of preparation method and application of lithium vanadium fluorophosphate
  • A kind of preparation method and application of lithium vanadium fluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

[0031] The prepared mixed solution A was placed in an oven at 100 degrees to dry for 12 hours, and after being taken out for grinding and grinding, it was placed in a tube furnace at 750 °C with an argon atmosphere for 6 hours at a constant temperature, and then the black carbon composite vanadium phosphate was obtained by taking out, grinding and grinding. Powder (VPO 4 @C);

[0032] the resulting VPO 4 @C is mixed with 0.05mol ammonium fluoride, 0.05mol lithium hydroxide, and 80ml of water to obtain mixed solution B, and mixed solution B is placed in a 180-degree reactor for 48h of solvothermal reaction, s...

Embodiment 2

[0034] V 2 O 3 LiVPO prepared by @C as precursor 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, and stir mechanically at 80°C for 10 hours to obtain mixed solution A; the mass of citric acid is 50% of the mass of ammonium metavanadate;

[0036] The prepared mixed solution A was placed in an oven at 100 degrees to dry for 12 hours, and after being taken out for grinding and grinding, it was placed in a tube furnace at 750 °C with an argon atmosphere for 6 hours at a constant temperature, and the black V was taken out for grinding and grinding. 2 O 3 @C powder;

[0037] the resulting V 2 O 3 @C is mixed with 0.05mol ammonium fluoride, 0.05mol ammonium dihydrogen phosphate, 0.05mol lithium hydroxide, and 80ml water to obtain mixed solution B, which is placed in a 180-degree reactor for 48h of solvothermal reaction , suction filtration, drying and grinding to obtain LiVPO 4 F@C powd...

Embodiment 3

[0039] VPO 4 LiVPO prepared by @C as precursor 4 F@C

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

[0041] The prepared mixed solution A was placed in an oven at 100 degrees for drying for 12 hours, and after being taken out for grinding and grinding, it was placed in a tube furnace at 600 °C with an argon atmosphere for 10 hours at a constant temperature, and the black carbon composite vanadium phosphate was obtained by taking out and grinding for grinding. Powder (VPO 4 @C);

[0042] the resulting VPO 4@C is mixed with 0.05mol ammonium fluoride, 0.05mol lithium hydroxide, and 80ml of water to obtain mixed solution B, and mixed solution B is placed in a 180-degree reactor for 48h of solvothermal reaction,...

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Abstract

The present invention provides a preparation method of lithium vanadium fluorophosphate and application thereof. The method of the present invention is summarized into two steps. The first step is to prepare carbon-coated vanadium phosphate (VPO) by a sol-gel method. 4 @C) or carbon-coated vanadium trioxide (V 2 O 3 @C); the second step is low-temperature solvothermal preparation of carbon composite LiVPO 4 F. First step to prepare carbon-coated VPO using sol-gel method 4 @C or V 2 O 3 @C, carbon composite precursors with small particle size and uniform distribution can be obtained. The present invention adopts low-temperature hydrothermal synthesis of LiVPO through the second step 4 F, on the one hand, effectively avoids the volatilization of F, and prepares high-purity LVPF materials at low temperature; Obtained LiVPO 4 F@C powders have nanoscale morphologies, high crystal phase purity, and excellent performance close to the theoretical specific capacity at low magnifications.

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 fluorophosphate. Background technique [0002] The cathode material of lithium-ion batteries is the key to determining the energy density of the battery. The preferred cathode material should have high operating voltage, high capacity and stable structure. Among the many cathode materials, lithium vanadium fluorophosphate (LiVPO) 4 F, abbreviated as LVPF) has attracted wide attention due to its high voltage (4.2V), high theoretical specific capacity (153mAh / g), and stable structure. However, the intrinsic 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 a carbon source in the process of sol-gel method, solid phase or wet phase ball milling to form a car...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58C01B25/455C01B32/05H01M4/62H01M10/0525
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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