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Process for producing lithium ion battery negative pole material of lithium titanate

A technology for lithium-ion batteries and negative electrode materials, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of complex synthesis process, long heat treatment time, high energy consumption, etc., and achieve simple preparation process and cheap and easy-to-obtain raw materials , the effect of broad application prospects

Inactive Publication Date: 2009-05-13
SHANGHAI UNIV
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

The traditional solid-phase reaction method is simple, but the raw materials need to be grinded and mixed for a long time, the reaction speed is slow, high heat treatment temperature and long heat treatment time are required, and the energy consumption is large. At the same time, due to the evaporation of metal lithium and lithium compounds The stoichiometric ratio of Ti and Li is difficult to control, and TiO 2 As a raw material, it is difficult to remove in the product
The product prepared by the sol-gel method has high chemical purity, good uniformity, low heat treatment temperature, and short reaction time. However, due to the use of organic raw materials in the synthesis process, the cost increases and a large amount of waste water is generated, which has a certain impact on the environment. , while the synthesis process is complex and difficult to realize industrialization

Method used

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  • Process for producing lithium ion battery negative pole material of lithium titanate
  • Process for producing lithium ion battery negative pole material of lithium titanate
  • Process for producing lithium ion battery negative pole material of lithium titanate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Lithium oxalate and anatase titanium dioxide (about 50nm) with a molar ratio of 4.5:5 were placed in an 800mL beaker, 500mL of absolute ethanol was added, mechanically stirred for 3 hours, heated to 70°C in a water bath, and stirred , the solvent was evaporated to obtain a lithium oxalate / titanium dioxide premix. The premix was calcined in the air atmosphere, first kept at 200°C for 2h, then heated to 600°C for 12h, cooled and then ground to obtain the spinel structure Li 4 Ti 5 o 12 .

[0026] The product has been detected by D / max2500PC 18KW micro-area X-ray diffractometer, and it is lithium titanate with spinel structure, such as Figure 5 (b); after the 1000HS / 3000HS laser particle analyzer test, the average particle size is 360nm; SEM photo as figure 1 shown.

Embodiment 2

[0027] Example 2: Dissolve lithium phosphate and anatase-type titanium dioxide (20-30 nm) with a molar ratio of 4.2:5 in 500 mL of deionized water, mechanically stir and pre-mix for 3 hours, and dry at 120° C. for 12 hours in a blast drying oven to obtain Lithium Phosphate / Titanium Dioxide Premix. The premix was calcined in the air atmosphere, first kept at 250°C for 3h, then heated to 800°C for 10h, cooled and then ground to obtain the spinel structure Li 4 Ti 5 o 12 .

[0028]The product has been detected by D / max2500PC 18KW micro-area X-ray diffractometer, and it is lithium titanate with spinel structure, such as Figure 5 (c); after the 1000HS / 3000HS laser particle analyzer test, the average particle size is 505nm; SEM photo as figure 2 shown.

Embodiment 3

[0029] Example 3: Lithium chloride and amorphous titanium dioxide (15-20 nm) with a molar ratio of 4.0:5 were dissolved in 500 mL of ethylene glycol, mechanically stirred and premixed for 3 hours, and spray-dried to obtain lithium chloride / titanium dioxide premixed thing. The premix was calcined in the air atmosphere, first kept at 350°C for 4h, then heated to 1000°C for 6h, cooled and then ground to obtain the spinel structure Li 4 Ti 5 o 12 .

[0030] The product has been detected by D / max2500PC 18KW micro-area X-ray diffractometer, and it is lithium titanate with spinel structure, such as Figure 5 (d); after the 1000HS / 3000HS laser particle analyzer test, the average particle size is 1035nm; SEM photo as image 3 shown.

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Abstract

The invention relates to the preparation method of Li4Ti5O12 as the negative electrode material of Li-ion battery. The preparation method comprises the following steps: dissolving nanoscale TiO2 and Li salts in a solvent at a molar ratio of 5:4 to 5:4.5, mixing completely, drying to remove the solvent to obtain a pre-mixture, heating the pre-mixture to melt the salt, soaking for 2 to 5 h, and calcining at 600 to 1,000 DEG C for 6 to 16 h to obtain Li4Ti5O12 with spinel structure and particle diameter of 0.3 to 2 mum. The preparation method has the advantages of easily-obtained raw materials, low cost, simple preparation process, low energy consumption, easy industrial production, no generation of the three wastes, no environmental pollution, and wide application prospect. By adopting a eutectic mixture as the molten medium, the preparation method can prepare high-performance and high-dispersion nanoscale Li4Ti5O12 with high specific surface area at lower temperature.

Description

technical field [0001] The invention relates to a preparation method of a negative electrode material of a lithium ion battery, in particular to a preparation method of lithium titanate, a negative electrode material of a lithium ion battery. technical background: [0002] In order to meet the urgent needs of emerging industries such as notebook computers, cameras and third-generation mobile communications for high-performance lithium-ion batteries, countries around the world have formed an upsurge in research and development of high-performance lithium-ion batteries and their key materials. Lithium-ion batteries are being Develop towards high performance (ie high specific energy, long life, safety), and low cost. Lithium-ion batteries have outstanding advantages such as high voltage, small size, light weight, high specific energy, no memory effect, no pollution, small self-discharge, and long life. They are considered to be the battery system with the best comprehensive per...

Claims

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Application Information

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IPC IPC(8): C01G23/00H01M4/58
CPCY02E60/12
Inventor 施利毅曹绍梅冯欣张大卫时雯
Owner SHANGHAI UNIV
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