Method for preparing lithium ion battery anode material vanadium lithium fluophosphate by one-step solid phase reaction

A lithium ion battery and lithium vanadium fluorophosphate technology, applied in the field of lithium vanadium phosphate, can solve the problems of uneven particle size distribution of synthetic materials, poor electrical conductivity and cycle performance, uneven particle size distribution of materials, etc. The effect of growing up, easy to control, simple and convenient method

Inactive Publication Date: 2008-12-10
GUILIN UNIVERSITY OF TECHNOLOGY
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  • 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 ion battery anode material vanadium lithium fluophosphate by one-step solid phase reaction
  • Method for preparing lithium ion battery anode material vanadium lithium fluophosphate by one-step solid phase reaction
  • Method for preparing lithium ion battery anode material vanadium lithium fluophosphate by one-step solid phase reaction

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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 ascorbic acid, 0.20mol of ammonium fluoride and 0.21mol of diammonium hydrogen phosphate, they were respectively heated at 450°C, 550°C, 650°C, Sintering at 750°C for 3 hours, then finished LiVPO 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 0.2 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] Experimental condition and result of table 1 embodiment 1

[0019] Numbering

Embodiment 2

[0021] Mix 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, and then sinter at 650°C under the protection of argon. 6, 9 and 12h, the finished product liVPO 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 0.2 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] Experimental condition and result of table 2 embodiment 2

[0023] Numbering

Embodiment 3

[0025] Mix 0.105mol of vanadium pentoxide powder with 0.19mol of lithium chloride, 0.095mol of citric acid, 0.19mol of potassium fluoride and 0.19mol of potassium phosphate. ℃, 750℃ sintering for 12h, after cooling, the finished product 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 0.2 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] Experimental condition and result of table 3 embodiment 3

[0027] Numbering

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Abstract

The invention discloses a method for producing fluorophoshoric acid vanadium lithium of lithium iron battery positive pole material at low temperature by one-step solid phase reaction, comprising the step of: uniformly blending vanadic oxide powders, phosphate, organic acid, lithium salts with villaumite to sinter for 3 to 12 hours under the protection of inert gases, consequently the final product LiVPO4F is obtained after cooling; the invention is simple and convenient in usage, easy in control and low in cost, and simplifies the synthesis process and promotes the discharge and charge performance and circulation performance of samples.

Description

technical field [0001] The invention relates to a method for preparing lithium vanadium phosphate, a cathode material of a lithium ion battery, by one-step solid phase 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) Lithium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/04C04B35/622B01J19/00
CPCY02E60/10
Inventor 钟胜奎刘乐通王健刘洁群姜吉琼
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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