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Preparation method of lithium titanate negative electrode material with controllable particle size for lithium battery

A negative electrode material and particle size technology, applied in the field of lithium titanate negative electrode material preparation, to achieve high capacity, uniform and controllable particle size, and high cycle stability

Inactive Publication Date: 2018-05-22
天津普兰能源科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problem to be solved by the present invention is to provide a preparation method of lithium titanate negative electrode material with controllable particle size for lithium batteries, which solves the problem of titanium dioxide accumulation and can effectively control the particle size of lithium titanate

Method used

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  • Preparation method of lithium titanate negative electrode material with controllable particle size for lithium battery
  • Preparation method of lithium titanate negative electrode material with controllable particle size for lithium battery
  • Preparation method of lithium titanate negative electrode material with controllable particle size for lithium battery

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preparation example Construction

[0024] In order to solve this problem, the present invention proposes a method for preparing a lithium titanate negative electrode material with a controllable particle size for lithium batteries, which includes: the first step is to combine the lithium source, titanium source, surfactant, complexing agent, and The buffer reagent is dissolved in water; the second step is to hydrothermally react the product of the first step at 120-200℃ for 12-24 hours; the third step is to dry the product of the second step; the fourth step is to remove the product of the third step Calcined at 700-900℃ for 2-12h. In this method, the addition of a buffer reagent can stabilize the pH of the solution during the reaction, and make the hydrolysis rate of organic titanium constant, so that the size of the titanium dioxide particles generated can be uniform. The added complexing agent is complexed with the hydrolyzed titanium, which can control the hydrolysis rate of the organotitanium source, and pr...

Embodiment 1

[0035] Dissolve 5.8g polyoxyethylene sorbitan palmitate and 9.58g lithium hydroxide into 180g water, then add 38.7g 30wt% H 2 O 2 , Stir for 15min to obtain material 1; take 97.2g of tetrabutyl titanate and slowly add dropwise to material 1 under stirring to obtain material 2; add 1.885g of ammonium carbonate to material 2, and then put it into a 500ml hydrothermal reactor In the process, keep the temperature at 180°C for 12h to obtain material 3; spray dry to obtain material 4; calcinate material 4 at 750°C under nitrogen protection for 8 hours to obtain lithium titanate material for lithium batteries.

[0036] Observe the obtained lithium titanate material using scanning electron microscope, such as figure 1 This is a scanning electron micrograph of the lithium titanate material obtained in this example.

[0037] The lithium titanate material prepared in this embodiment is used as an active material to prepare a lithium ion battery. Using N-methylpyrrolidone as the solvent, the l...

Embodiment 2

[0040] Dissolve 6.4g of octylphenol polyoxyethylene ether and 9.58g of lithium hydroxide into 180g of water, then add 192.4g of isopropanol and stir for 15min to obtain material 1; take 65.6g of tetraethyl titanate and slowly add dropwise to the stirring state Add 3.85g of ammonium bicarbonate to material 2 and put it in a 500ml hydrothermal reactor, keep it at a constant temperature of 150°C for 24h to obtain material 3, which is spray-dried to obtain material 4; Material 4 is calcined at 800°C for 6 hours under the protection of argon to obtain lithium titanate materials for lithium batteries.

[0041] Observe the obtained lithium titanate material using scanning electron microscope, such as figure 2 This is a scanning electron micrograph of the lithium titanate material obtained in this example.

[0042] The lithium titanate material prepared in this embodiment is used as an active material to prepare a lithium ion battery. Using N-methylpyrrolidone as the solvent, the lithium...

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Abstract

The invention provides a preparation method of a lithium titanate negative electrode material with controllable particle size for a lithium battery. The preparation method comprises the steps of 1, dissolving a lithium source, a titanium source, a surfactant, a complexing agent and a buffer agent in water; 2, performing hydrothermal reaction on the product in the first step for 12-24 hours under 120-200 DEG C; 3, drying the product of the second step; and 4, roasting the product of the third step for 2-12 hours under 700-900 DEG C. By the preparation method, the hydrolysis rate of organic titanium can be effectively controlled, and the lithium titanate material with uniform and controllable particle size, obtained by preparation, has high cycle stability, high capacity, high-rate charge-discharge performance and high safety.

Description

Technical field [0001] The invention belongs to the technical field of lithium battery electrode materials, and in particular relates to a method for preparing a lithium titanate negative electrode material with a controllable particle size for a lithium battery. Background technique [0002] As a lithium battery anode material, the unit cell volume hardly changes during the charge and discharge process of lithium titanate. It is known as a "zero strain" material. It has good cycling, high rate charge and discharge, low temperature and safety performance, and has a wide range Application prospects. [0003] However, the lithium titanate prepared by the commonly used solid-phase synthesis technology has problems such as coarse particles, uneven particle size, low conductivity, and Ti-O bonds that cause carbonate solvates in the electrolyte to decompose and expand, which seriously affects lithium titanate. Industrial applications. In order to further improve this defect, some schol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M10/0525C01G23/00
CPCC01G23/003H01M4/485H01M10/0525Y02E60/10
Inventor 陈永胜黄晓艳随东
Owner 天津普兰能源科技有限公司
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