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Preparation method of low moisture absorption and low gas production lithium titanate anode material

A technology of lithium titanate and lithium salt, which is applied in the field of preparation and application of energy storage materials, can solve problems such as shortened service life, aggravated gas production problems, and increased production costs, achieving long service life, improved gas production problems, and low cost Effect

Active Publication Date: 2018-03-16
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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  • Preparation method of low moisture absorption and low gas production lithium titanate anode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0027] The lithium titanate Li prepared above 4 Ti 5 O 12 Weigh 2g dissolved in 20ml of deionized water and stir magnetically, and add 5ml of a 0.5mol / L PVP solution with a pH of 4. The mixed solution was heated in a 60°C water bath while continuously magnetically stirred to ensure that the reaction proceeded evenly. After 2 hours, the mixture was stopped. After natural cooling, the mater...

Embodiment 2

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

[0031] The lithium titanate Li prepared above 4 Ti 5 O 12 Weigh 2g, dissolve it in 20ml of deionized water and stir it magnetically; and add 5ml of 0.4mol / L PVP solution with a pH of 7, and heat the mixed solution in a water bath at 50℃ while continuously magnetically stirring to ensure uniform reaction. , Stop after 6h, take out the material after natural cooling, and vacuum dry...

Embodiment 3

[0034] Weigh 0.044mol of lithium acetate (CH 3 COOLi) Dissolve in 20ml of deionized water; measure 17ml of 0.05mol butyl titanate solution with a graduated cylinder and mix with an equal volume of absolute ethanol, add the prepared lithium acetate solution dropwise to it under magnetic stirring to obtain a white After the suspension, continue to stir for 1 hour and then transfer to a reaction kettle at 160°C for 16 hours, cool to room temperature, and place it in a muffle furnace to calcinate at 600°C for 6 hours after centrifugation, washing and drying. The heating rate is 4°C / min. The white powder obtained is lithium titanate.

[0035] The lithium titanate Li prepared above 4 Ti 5 O 12 Weigh 5g dissolved in 20ml of deionized water and stir it magnetically; add 5ml of a 0.1mol / L PVP solution with a pH of 6 and heat the mixed solution in a water bath at 80°C while continuously magnetically stirring to ensure that the reaction proceeds evenly. Stop after 1 hour, take out the mater...

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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 particularly 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 used more and more in lithium-ion batteries because of its superior cycle performance, good rate performance 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 diffused in graphite, which makes it have obvious fast charging advantages and good high and low temperature performance; coupled with good safety, long life, and green environmental protection, it is used in electric buses, energy storage, high power Equipment and other fields have broad application spac...

Claims

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Application Information

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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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