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Method for low temperature preparing lithium ion battery positive pole material fluorophosphoric acid vanadium lithium

A lithium-ion battery, lithium vanadium fluorophosphate technology, applied in battery electrodes, circuits, electrode manufacturing, etc., can solve the problem of poor electrical conductivity and cycle performance, uneven particle size distribution of synthetic materials, uneven particle size distribution of materials, etc. problem, to achieve the effect of easy control, suppression of excessive growth, and simple and convenient method

Inactive Publication Date: 2008-08-27
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.
Due to the relatively high reaction temperature required by the high-temperature carbothermal reduction method, the particle size distribution of the synthesized material is uneven, and the electrical conductivity and cycle performance are not good.

Method used

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  • Method for low temperature preparing lithium ion battery positive pole material fluorophosphoric acid vanadium lithium
  • Method for low temperature preparing lithium ion battery positive pole material fluorophosphoric acid vanadium lithium
  • Method for low temperature preparing lithium ion battery positive pole material fluorophosphoric acid vanadium lithium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Heat 0.1mol vanadium pentoxide powder to 600°C, keep the temperature for 4 hours to make it melt, and then quickly pour it into a container filled with water to form a brownish red solution, which can be formed after standing for 16 hours. 2 o 5 ·nH 2 O wet gel. The wet gel was washed to remove most of the moisture, then vacuum-dried at 70° C. for 16 hours, and ground to obtain vanadium pentoxide gel powder. Mix the prepared vanadium pentoxide gel powder with 0.2mol of lithium acetate, 0.2mol of ammonium fluoride, 0.2mol of diammonium hydrogen phosphate and 0.24mol of acetylene black, and then place them at 400°C, 500°C, and Sintering at 600°C and 700°C for 5 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 1 μm. The obtained product was assembled into an experimental button battery to me...

Embodiment 2

[0021] Heat 0.1mol vanadium pentoxide powder to 900°C, keep the temperature constant for 1 hour to melt the vanadium pentoxide, then quickly pour it into a container filled with water to form a brownish-red solution, and leave the solution for 12 hours to form V 2 o 5 ·nH 2 O wet gel. Wash the wet gel to remove most of the moisture, then vacuum-dry it at 90° C. for 12 hours, and grind it to obtain vanadium pentoxide gel powder. After mixing the prepared vanadium pentoxide gel powder with 0.2mol lithium fluoride, 0.2mol sodium fluoride, 0.2mol ammonium dihydrogen phosphate and 0.24mol acetylene black, they were sintered at 600°C under the protection of argon for 5 , 10, 15 and 20h, 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 1 μm. The obtained product was assembled into an experimental butt...

Embodiment 3

[0025] Heat 0.1mol vanadium pentoxide powder to 800°C, keep the temperature constant for 2 hours to melt it, then quickly pour it into a container filled with water to form a brown-red solution, and the solution can be formed after standing for 4 hours. 2 o 5 ·nH 2 O wet gel. The wet gel was washed to remove most of the water, then vacuum-dried at 100° C. for 8 hours, and ground to obtain vanadium pentoxide gel powder. After mixing the prepared vanadium pentoxide gel powder with 0.2mol lithium chloride, 0.2mol potassium fluoride, 0.2mol potassium phosphate and 0.24mol acetylene black, they were heated at 450°C and 550°C under the protection of argon , 650°C, 700°C sintering for 20h, 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 1 μm. The obtained product was assembled into an experimental button bat...

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Abstract

The invention discloses a method for preparing anode material vanadium lithium fluoroalkylphosphate of a lithium -ion cell at low temperature, comprising the steps of: (1) heating vanadic oxide powder to six hundred to nine hundred DEG C; allowing to melt at a constant temperature for one to four hours and pouring into a container with water rapidly to form a brown-red solution; letting the solution stand for four to sixteen hours to form wet gel V2O5.nH2O; washing the wet gel, removing most of moisture, keeping drying for four to sixteen hours in a vacuum ambient of seventy to one hundred DEG C and grinding to obtain vanadic oxide powder. (2) Mixing the vanadic oxide powder obtained through the preparation method with Lithium, villiaumite, phosphates and acetylene black evenly at mol ratio of one to two to two to two to two point four, sintering for five to twenty hours at temperature between four hundred and seven hundred DEG C under the protection of an inert gas and cooling to obtain a finished product of LiVPO4F. The preparation method is easy and simple, easy to control and low in cost, reduces sintering temperature and improves the charging and discharging performance and cycle performance of samples.

Description

technical field [0001] The invention relates to a low-temperature method for preparing lithium vanadium phosphate, a cathode material of a lithium ion battery. 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 (4.2Vvs 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 ions in LiVPO 4 Di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/48H01M4/04C04B35/622
CPCY02E60/10
Inventor 钟胜奎刘长久王健
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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