A preparation method of lithium titanate negative electrode material with low moisture absorption and low gas production

A technology of lithium titanate and lithium salt, which is applied in the field of preparation and application of energy storage materials, can solve the problems of rising production costs, shortening service life, aggravating gas production problems, etc., and achieves low cost, long service life, and improvement of gas production problems. Effect

Active Publication Date: 2020-05-22
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at the same time, lithium titanate also has its own defects, such as the problem of gas production. Lithium titanate is prone to react with the electrolyte and continues to produce gas in the cycle, resulting in bulging of the battery cell, performance degradation, and greatly shortened service life.
At the same time, the pH value of lithium titanate is high, and it is easy to absorb water in the air, and high moisture will further aggravate the problem of gas production. Therefore, the use of lithium titanate requires strict environmental control, which leads to an increase in its production cost.

Method used

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  • A preparation method of lithium titanate negative electrode material with low moisture absorption and low gas production
  • A preparation method of lithium titanate negative electrode material with low moisture absorption and low gas production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 0.042mol of lithium acetate (CH 3 COOLi) was dissolved in 20ml of deionized water; 17ml of 0.05mol butyl titanate solution was measured with a graduated cylinder and mixed with an equal volume of absolute ethanol, and the prepared lithium acetate solution was added dropwise under magnetic stirring to obtain a white Continue to stir the suspension for 1 hour, then transfer it to the reaction kettle for 18 hours at 180°C, cool to room temperature, centrifuge, wash and dry it, then place it in a muffle furnace for calcination at 700°C for 6 hours, and the obtained white powder is titanic acid lithium.

[0027] Lithium titanate Li prepared above 4 Ti 5 o 12 Weigh 2 g dissolved in 20 ml of deionized water with magnetic stirring, and add 5 ml of 0.5 mol / L PVP solution with a pH value of 4. The mixed solution was heated in a water bath at 60°C while stirring continuously with magnetic force to ensure uniform reaction, and stopped after 2 hours. After natural cooling,...

Embodiment 2

[0030] Weigh 0.043mol of lithium acetate (CH 3 COOLi) was dissolved in 20ml of deionized water; 17ml of 0.05mol butyl titanate solution was measured with a graduated cylinder and mixed with an equal volume of absolute ethanol, and the prepared lithium acetate solution was added dropwise under magnetic stirring to obtain a white Continue to stir the suspension for 1 hour, then transfer it to a reaction kettle for 24 hours at 150°C, cool to room temperature, centrifuge, wash and dry it, then place it in a muffle furnace for calcination at 800°C for 5 hours, and the obtained white powder is titanic acid lithium.

[0031] Lithium titanate Li prepared above 4 Ti 5 o 12 Weigh 2g, dissolve in 20ml of deionized water with magnetic stirring; add 5ml of 0.4mol / L PVP solution with a pH value of 7, heat the mixed solution in a water bath at 50°C, and keep magnetically stirring at the same time to ensure uniform reaction , stop after 6h, take out the material after natural cooling, and...

Embodiment 3

[0034] Weigh 0.044mol of lithium acetate (CH 3COOLi) was dissolved in 20ml of deionized water; 17ml of 0.05mol butyl titanate solution was measured with a graduated cylinder and mixed with an equal volume of absolute ethanol, and the prepared lithium acetate solution was added dropwise under magnetic stirring to obtain a white After the suspension was stirred for 1 hour, it was transferred to a reaction kettle for 16 hours at 160°C, cooled to room temperature, centrifuged, washed, and dried, then placed in a muffle furnace for calcination at 600°C for 6 hours, with a heating rate of 4°C / min. The obtained white powder is lithium titanate.

[0035] Lithium titanate Li prepared above 4 Ti 5 o 12 Weigh 5g dissolved in 20ml of deionized water and stir magnetically; add 5ml of 0.1mol / L PVP solution with a pH value of 6, heat the mixed solution in a water bath at 80°C, and keep magnetically stirring at the same time to ensure that the reaction is uniform. Stop after 1h, take out ...

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Abstract

The invention discloses a preparation method of a low moisture absorption and low gas production lithium titanate anode material. The method includes the steps of: preparing a titanium source and a lithium salt into a lithium titanate precursor by hydrothermal process, performing cooling, then conducting cleaning, and then subjecting the lithium titanate precursor to high temperature calcinationstreatment to obtain lithium titanate powder; dissolving lithium titanate powder in deionized water to form a lithium titanate solution, then adding a PVP (polyvinylpyrrolidone) water solution, and conducting mixing and heating to carry out coating reaction on lithium titanate and PVP in a liquid phase; and performing vacuum drying on the reactant so as to obtain a PVP coated lithium titanate material. The lithium titanate powder material prepared by hydrothermal process lowers the pH value of lithium titanate from the raw material end, thereby weakens the material water absorption, and can effectively inhibits gas production. Then PVP is employed to perform surface film coating on lithium titanate, thus lowering the lithium titanate surface residue and weakening the catalytic effect of Ti<4+> on an electrolyte solution, and preventing the electrolyte solution from being reduced and decomposed on the lithium titanate surface to produce gas.

Description

technical field [0001] The invention belongs to the field of preparation and application of energy storage materials, and in particular relates to a preparation method of a lithium titanate negative electrode material for a lithium ion battery with low moisture absorption and low gas production. Background technique [0002] Lithium titanate "zero-strain material" is being increasingly used in lithium-ion batteries due to its superior cycle performance, good rate and reliable safety. Lithium titanate has a three-dimensional lithium ion diffusion channel unique to the spinel structure, Li + The diffusion coefficient is 2*10 -8 cm 2 / S, which is more than 10 times that of graphite, makes it have obvious advantages of fast charging and good high and low temperature performance; in addition, it has good safety, long life, and environmental protection, making it suitable for electric buses, energy storage, and high-power Equipment and other fields have broad application space....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/485H01M4/62H01M10/0525
CPCH01M4/366H01M4/485H01M4/628H01M10/0525Y02E60/10
Inventor 段锐杨尘汪涛朱春林王金龙
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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