Preparation method of nanoscale zirconium-doped lithium titanate material

A lithium zirconate titanate, nano-scale technology, which is applied in the field of electrochemical power supply material preparation, can solve the problems of low initial charge and discharge efficiency, easy reaction of electrolytes, and high cost of organic compounds, and achieves the benefits of migration and migration, shortening Heat treatment time, easy implementation effect

Inactive Publication Date: 2013-06-12
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although carbon anode materials have been greatly improved in terms of safety performance and cycle performance, there are still many disadvantages: the potential of carbon materials is very close to that of metal lithium, and when the battery is overcharged, lithium will be on the surface of the carbon electrode. Lithium dendrites are formed due to precipitation, which causes short circuit; the first charge and discharge efficiency is low, and it is easy to react with the electrolyte; there is obvious voltage hysteresis;
Its main disadvantages: high cost of organic compounds; low yield; a large amount of organic gas is volatilized; it is difficult to realize industrialization

Method used

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  • Preparation method of nanoscale zirconium-doped lithium titanate material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Disperse 34ml of tetra-n-butyl titanate in 60ml of deionized water to form A liquid; disperse 3.8g of lithium hydroxide monohydrate in 40ml of deionized water, and keep the ratio of the amount of lithium source and titanium source as no Li :n Ti =1:1.11, according to 1% of the total product mass, add 1.05ml of zirconium source solution with a zirconium ion concentration of 1mol / L to be liquid B;

[0025] 2) Under magnetic stirring, slowly add liquid B to liquid A, and stir for 30 minutes; pour the mixed solution into a high-temperature reactor, and then place it in an oven at 180°C for 12 hours. After the reaction, cool naturally to room temperature, and then carry out Suction filtration, washing with deionized water to pH=7, drying at 60°C to obtain the precursor;

[0026] 3) The obtained precursor was sintered at 750° C. for 2 hours under a nitrogen atmosphere, and the obtained product was a nanoscale lithium zirconate-doped lithium titanate material.

[0027] T...

Embodiment 2

[0031] 1) Add 10g of amorphous TiO 2 Disperse in 50ml of deionized water, which is liquid A; disperse 11.6g of lithium acetate in 50ml of deionized water, and keep the ratio of the amount of lithium source and titanium source n Li :n Ti =1:1.1, according to 0.1% of the product mass, add 0.132ml of zirconium source solution with a zirconium ion concentration of 1mol / L to be liquid B;

[0032] 2) Under magnetic stirring, slowly add liquid B to liquid A, and stir for 30 minutes; pour the mixed solution into a high-temperature reaction kettle, and then place it in a 120°C oven for 24 hours. After the reaction, cool naturally to room temperature, and then carry out Suction filtration, washing with deionized water, and drying at 120°C to obtain the precursor;

[0033] 3) The obtained precursor was sintered at 600° C. for 5 hours under a nitrogen atmosphere, and the obtained product was a nano-scale lithium zirconate-doped lithium titanate material.

[0034] The test method is con...

Embodiment 3

[0036] 1) Disperse 402g of titanium sulfate in 500ml of deionized water to form A liquid; disperse 85g of lithium acetate in 500ml of deionized water, and keep the amount ratio of lithium source and titanium source n Li :n Ti =1:1.2, add 5.27ml of zirconium source solution with a zirconium ion concentration of 1mol / L according to 0.5% of the product mass, to be liquid B;

[0037] 2) Under magnetic stirring, slowly add liquid B to liquid A, and stir for 30 minutes; pour the mixed solution into a high-temperature reactor, and then place it in a 200°C oven for 12 hours. After the reaction, cool naturally to room temperature, and then carry out Suction filtration, washing with deionized water, and drying at 100°C to obtain the precursor;

[0038] 3) The obtained precursor was sintered at 1000° C. for 1 h in a nitrogen atmosphere, and the obtained product was nano-scale zirconium-doped lithium titanate material.

[0039] The test method is consistent with that of Example 1, and t...

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Abstract

The invention discloses a preparation method of a nanoscale zirconium-doped lithium titanate material. Nanoscale lithium titanate is prepared by the method, and simultaneously is modified through doping zirconium. According to the preparation method, chemical components and grain sizes of the lithium titanate are effectively controlled by using hydro-thermal treatment, the temperature during subsequent treatment is greatly reduced, and grains are prevented from being agglomerated; and the preparation method is easy to implement in industry. The lithium titanate is doped with the zirconium in a preparation process, so that the specific discharge capacity of the material is increased at high magnification. Simultaneously, the gas expansion problem existing in the charge-discharge process of lithium titanate batteries is solved to a certain extent. The material prepared by the method has high magnification and high specific capacity and can be applied to the batteries needed for various portable electronic equipment and various electric vehicles.

Description

technical field [0001] The invention relates to a preparation method of a nanoscale zirconium-doped lithium titanate material, and belongs to the technical field of preparation of electrochemical power source materials. Background technique [0002] With the development of power batteries, lithium-ion power batteries have gradually become mainstream products. Lithium-ion battery anode materials mainly include carbon-based materials, nitrides, silicon-based materials, tin-based materials and various new alloys. Among them, carbon-based materials have been used in practice, and other materials are mostly in the laboratory research stage. Although carbon anode materials have been greatly improved in terms of safety performance and cycle performance, there are still many disadvantages: the potential of carbon materials is very close to that of metal lithium, and when the battery is overcharged, lithium will be on the surface of the carbon electrode. Precipitation and formation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485
CPCY02E60/10
Inventor 施利毅程崇领刘洪江薛鑫
Owner SHANGHAI UNIV
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