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A method of producing lithium ion battery positive pole material fluorine Lithium Vanadium Phosphate by microwave rapid reaction

A lithium-ion battery, lithium vanadium phosphate technology, applied in the field of lithium vanadium phosphate, can solve the problems of poor conductivity and cycle performance, uneven particle size distribution of synthetic materials, uneven particle size distribution of materials, etc., and achieve easy control , Inhibit excessive growth, the method is simple and convenient

Inactive Publication Date: 2009-06-03
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrogen reduction method uses pure H 2 As a reducing agent, due to the H 2 It is very dangerous due to its flammable and explosive properties, which is not conducive to industrial production
Moreover, the particle size distribution of the synthesized material is not uniform, and the electrical conductivity is low.
The two-step carbothermal reduction method adopts two-step reactions to synthesize, the process is complicated, and the synthesis conditions are harsh, and the prepared materials have uneven particle size distribution, poor conductivity and cycle performance

Method used

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  • A method of producing lithium ion battery positive pole material fluorine Lithium Vanadium Phosphate by microwave rapid reaction
  • A method of producing lithium ion battery positive pole material fluorine Lithium Vanadium Phosphate by microwave rapid reaction
  • A method of producing lithium ion battery positive pole material fluorine Lithium Vanadium Phosphate by microwave rapid reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] After mixing 0.095mol of vanadium pentoxide powder, 0.21mol of lithium acetate, 0.105mol of malic acid, 0.20mol of ammonium fluoride and 0.21mol of diammonium hydrogen phosphate, under the protection of nitrogen at 450°C, 550°C, 650°C, Sinter at 750°C for 10 minutes respectively, and the finished product LiVPO will be obtained after cooling 4 F. The obtained products were analyzed by X-ray diffraction, showing that they were all LiVPO 4 F, without any impurity phase, the particle size of the product obtained by SEM is about 2 μm. The obtained product was assembled into an experimental button battery to measure its charge-discharge specific capacity and cycle performance. The charge-discharge was carried out at a rate of 1C. The initial discharge capacity and the discharge capacity after 30 cycles are shown in Table 1.

[0018] Table 1 Experimental conditions and results of Example 1

[0019] serial number Sintering temperature

Embodiment 2

[0021] After mixing 0.10mol of vanadium pentoxide powder with 0.20mol of lithium fluoride, 0.10mol of adipic acid, 0.21mol of sodium fluoride and 0.20mol of ammonium dihydrogen phosphate, they were sintered at 650°C under the protection of argon for 10, 20, 30 and 40 minutes, after cooling, the finished LiVPO 4 F. The obtained products were analyzed by X-ray diffraction, showing that they were all LiVPO 4 F, without any impurity phase, the particle size of the product obtained by SEM is about 2 μm. The obtained product was assembled into an experimental button battery to measure its charge-discharge specific capacity and cycle performance. The charge-discharge was carried out at a rate of 1C. The initial discharge capacity and the discharge capacity after 30 cycles are shown in Table 2.

[0022] Table 2 Experimental conditions and results of Example 2

[0023] serial number Sintering temperature

Embodiment 3

[0025] After mixing 0.105mol of vanadium pentoxide powder, 0.19mol of lithium chloride, 0.095mol of citric acid, 0.19mol of potassium fluoride and 0.19mol of potassium phosphate, under the protection of argon at 480°C, 580°C, 680°C, Sinter at 750°C for 40 minutes respectively, and the finished product LiVPO will be obtained after cooling 4 F. The obtained products were analyzed by X-ray diffraction, showing that they were all LiVPO 4 F, without any impurity phase, the particle size of the product obtained by SEM is about 2 μm. The obtained product was assembled into an experimental button battery to measure its charge-discharge specific capacity and cycle performance. The charge-discharge was carried out at a rate of 1C. The initial discharge capacity and the discharge capacity after 30 cycles are shown in Table 3.

[0026] Table 3 Experimental conditions and results of Example 3

[0027] serial number Sintering temperature

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Abstract

The present invention discloses a method of producing lithium ion battery positive pole material fluorine Lithium Vanadium Phosphate by microwave rapid reaction. First evenly mix vanadic oxide powder, phosphates, organic acid, lithium salt and villaumite in molar ratio 0. 95-1.1:1.9-2.1:0.95-1.1:1. 9-2.1:1.9-2.1 respectively. Then sinter the mixture in a microwave reactor for 10 to 40 minutes in 450 EDG C to 750 EDG C under noble gas protection, and get completed product LiVPO4F after cooling. The invention is simple and convenient, easy controlled and cost low which simplifies the synthesizing process and improves charge-discharge performance and circulates performance of sample.

Description

technical field [0001] The invention relates to a method for preparing lithium vanadium vanadium phosphate, a cathode material of a lithium ion battery, through rapid microwave reaction. Background technique [0002] Lithium-ion secondary batteries have many excellent characteristics, and have been widely used in portable electronic products, communication tools, electric vehicles, and energy storage devices. The performance of lithium-ion batteries depends largely on the cathode material. Among them, lithium vanadium fluorophosphate (LiVPO) in the vanadium-based cathode material 4 F) Due to its good reversible performance, rich sources of raw materials, high specific capacity (theoretical capacity is 156mAh / g), and high platform ratio (4.2V vs Li + / Li) and other advantages have attracted great attention. But the following disadvantages hinder its practical application: (1) V in synthesis 3+ easily oxidized to V 5+ , it is not easy to obtain single-phase LiVPO 4 F; 2)...

Claims

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Application Information

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IPC IPC(8): C01B25/455H01M4/58
Inventor 钟胜奎李伟刘洁群
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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