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Method for preparing lithium ionic cell anode material lithium vanadium fluorophosphate by hydro-thermal synthesis reaction

A technology for lithium vanadium phosphate and lithium ion battery, which is applied in the field of lithium vanadium phosphate lithium fluorophosphate positive electrode material prepared by hydrothermal synthesis reaction, which can solve the problem of uneven particle size distribution of synthetic materials, poor conductivity and cycle performance, and material failure. Uneven particle size distribution and other problems, to achieve the effect of inhibiting excessive growth, easy to control, and simple and convenient methods

Inactive Publication Date: 2009-06-17
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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  • Method for preparing lithium ionic cell anode material lithium vanadium fluorophosphate by hydro-thermal synthesis reaction
  • Method for preparing lithium ionic cell anode material lithium vanadium fluorophosphate by hydro-thermal synthesis reaction
  • Method for preparing lithium ionic cell anode material lithium vanadium fluorophosphate by hydro-thermal synthesis reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Dissolve 0.19mol of ammonium metavanadate, 0.21mol of lithium acetate, 0.105mol of malic acid, 0.20mol of ammonium fluoride and 0.21mol of diammonium hydrogen phosphate in water and mix them uniformly. After 1 day of reaction, the finished LiVPO is obtained after drying 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 0.1 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.

[0017] Table 1 Experimental conditions and results of Example 1

[0018] Numbering temperature reflex

Embodiment 2

[0020] Dissolve 0.20 mol ammonium metavanadate, 0.20 mol lithium fluoride, 0.10 mol adipic acid, 0.21 mol sodium fluoride and 0.20 mol ammonium dihydrogen phosphate in water and mix well, then react 1, 2, 3 and 4d, finished product LiVPO after drying 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 0.1 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.

[0021] Table 2 Experimental conditions and results of Example 2

[0022] Numbering temperature reflex

Embodiment 3

[0024] Dissolve 0.205mol of ammonium metavanadate, 0.19mol of lithium chloride, 0.095mol of citric acid, 0.19mol of potassium fluoride and 0.19mol of potassium phosphate in water, mix well, and react at 230°C, 280°C, 310°C, and 330°C respectively 4d, finished product LiVPO after drying 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 0.1 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.

[0025] Table 3 Experimental conditions and results of Example 3

[0026] Numbering temperature reflex

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Abstract

The invention discloses a method for preparing a lithium ion battery anode material, namely vanadium lithium fluophosphate, through hydrothermal synthesis reaction, which comprises: dissolving ammonium metavanadate, phosphate, organic acid, lithium salt and villaumite into water according to the mol ratio of 1.9-2.1:1.9:2.1:0.95-1.1:1.9-2.1:1.9-2.1, making the mixture react for 1 to 4 days in a hydrothermal synthesis reaction kettle at a temperature of between 200 and 350 DEG C, and drying the mixture to obtain a finished product, namely LiVPO4F. The method is simple and convenient, is easy to control, has low cost, simplifies the synthesis technology, and improves the charge and discharge performance and the cycle performance of samples.

Description

technical field [0001] The invention relates to a method for preparing lithium vanadium vanadium phosphate, a cathode material of a lithium ion battery, by a hydrothermal synthesis 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...

Claims

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Application Information

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IPC IPC(8): C01B25/455H01M4/58
CPCY02E60/12Y02E60/10
Inventor 钟胜奎赵博刘洁群姜吉琼刘乐通王健
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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