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Method for preparing anode material lithium vanadium phosphate by adopting quenching

A technology of lithium vanadium fluorophosphate and cathode material, applied in battery electrodes, electrical components, circuits, etc., can solve the difficulty of diffusion and migration of lithium ions and electrons, affect the high-rate charge and discharge performance of materials, and limit the substantiality of lithium vanadium fluorophosphate. application and other issues, to achieve the effect of shortening the diffusion distance, excellent high-rate charge-discharge performance, and improved electrical conductivity

Inactive Publication Date: 2012-03-21
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, CN200910113804.1 discloses a sol-gel method to prepare titanium-doped lithium vanadium phosphate lithium ion battery positive electrode material, which is to mix ammonium metavanadate, lithium salt, phosphate, fluorine salt and metal ester in molar ratio of 1-1.15: 1-1.15: 1-1.15: 1-1.15: 0.10-0.25 After mixing evenly, sintering at 400°C-700°C for 5-20h under the protection of inert gas, the finished product LiVPO4F is obtained after cooling; most of these methods Natural cooling or other slow cooling methods are adopted. On the one hand, this slow cooling method is easy to generate impurities in the synthesized materials. On the other hand, the particles of the synthesized materials are relatively large, which makes the diffusion and migration of lithium ions and electrons in the materials. become difficult, thus affecting the high rate charge and discharge performance of the material
These all limit the substantive application of lithium vanadium phosphate

Method used

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  • Method for preparing anode material lithium vanadium phosphate by adopting quenching
  • Method for preparing anode material lithium vanadium phosphate by adopting quenching
  • Method for preparing anode material lithium vanadium phosphate by adopting quenching

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Mix 0.1mol of vanadium pentoxide, 0.2mol of ammonium dihydrogen phosphate, 0.105mol of lithium carbonate, 0.2mol of hydrofluoric acid and 0.2mol of citric acid through high-energy ball milling, then dry at 80°C, and then put them into tubes In a type furnace, under an argon atmosphere, the temperature was calcined at 500°C for 0.5 hours, and then the high-temperature charge was quickly placed in liquid nitrogen at -193°C, dry ice at -80°C, and water at 0°C. Diffraction analysis shows triclinic crystal system, which is LiVPO 4 F's

[0018] structure. The particle size obtained by SEM is about 50nm. The obtained product was assembled into a button battery and charged and discharged at a rate of 10C. The first discharge capacity under different conditions is shown in Table 1:

[0019] Table 1

[0020]

Embodiment 2

[0022] Mix 0.1 mol of vanadium dioxide, 0.1 mol of lithium fluoride, 0.1 mol of triammonium phosphate and 1 mol of oxalic acid under high-energy ball milling conditions, dry at 60°C, and then put them into a tube furnace, under hydrogen atmosphere, The temperature was calcined at a constant temperature of 700°C for 0.5h, and then the high-temperature charge was quickly placed in 40°C water to quench for 1min, 20min and 1h. The obtained material was analyzed by X-ray diffraction as a triclinic crystal system, namely LiVPO 4 The structure of F. The particle size obtained by SEM is about 80nm. The resulting product was assembled into a button battery and charged and discharged at a rate of 10C. The first discharge capacity under different conditions is shown in Table 2:

[0023] Table 2

[0024]

Embodiment 3

[0026] Mix 0.1mol of ammonium metavanadate, 0.051 of lithium oxide, 0.1mol of diammonium hydrogen phosphate, 0.1mol of hydrofluoric acid and 0.2mol of sucrose through high-energy ball milling, dry at 120°C, and then put them into a tube furnace. Under the atmosphere, it was calcined at a constant temperature of 800°C for 5 hours, and then the high-temperature charge was quickly placed in dry ice at -87°C for 1 minute, and the obtained material was analyzed by X-ray diffraction as a triclinic crystal system, namely LiVPO 4 The structure of F. The particle size can be found to be about 100nm by SEM. The obtained product was assembled into a button battery and charged and discharged at a rate of 10C, and the specific capacity of the first discharge was 138mAh·g -1 .

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Abstract

The invention relates to a method for preparing anode material lithium vanadium phosphate by adopting quenching, which comprises the following steps: mixing a lithium source compound, a vanadium source compound, a phosphorus source compound and a fluoride at a molar ratio of lithium : vanadium : phosphorus : fluorine = (1-1.05):1:1:1, adding a carbon source at a molar ratio of the carbon source : the vanadium source compound = 1:1-10:1, performing high-energy ball-milling for uniform mixing to obtain a precursor mixture, drying the precursor mixture, placing the dried precursor mixture in a non-oxidizing atmosphere and heating to 500-1000 DEG C, performing constant-temperature calcination for 0.5-48 h, rapidly transferring the high-temperature powder to a low-temperature medium (-209-40 DEG C), and allowing rapid quenching for a period from 1 min to 1 h to obtain lithium vanadium phosphate powder. The lithium vanadium phosphate powder prepared by using the quenching method provided by the invention has nano size, uniform particle size distribution, and excellent large-multiplying factor charging / discharging performance.

Description

technical field [0001] The invention relates to a preparation method of lithium vanadium phosphate, a cathode material of a lithium ion battery, in particular to a method for preparing lithium vanadium phosphate by a rapid cooling method. Background technique [0002] LiVPO4F is a new cathode material for lithium-ion batteries. It has the advantages of stable structure, up to 4.2V charge and discharge platform, and good cycle performance. It is considered to be a promising lithium-ion battery cathode material and is expected to be used in electric vehicles powered by lithium-ion batteries. Its prospects are immeasurable. Traditional LiVPO 4 F preparation methods mainly include the following: high temperature solid phase sintering method, carbothermal reduction method, sol-gel method, hydrothermal method and so on. For example, CN200910113804.1 discloses a sol-gel method to prepare titanium-doped lithium vanadium phosphate lithium ion battery positive electrode material, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 郑俊超张宝张明
Owner CENT SOUTH UNIV
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