Method for synthesizing SiO2 lithium ion battery cathode material lithium titanate

A technology for lithium-ion batteries and negative electrode materials, applied in battery electrodes, nanotechnology for materials and surface science, titanium compounds, etc. problem, to achieve the effect of improving rate performance and cycle performance, particle size, and high charge-discharge specific capacity

Inactive Publication Date: 2013-01-30
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industrial preparation of lithium titanate mainly adopts high-temperature solid-phase method, and is based on TiO 2 with Li 2 CO 3 Or LiOH and other raw materials are synthesized at 800-1000°C, and the reaction time is generally 12-24h. This method has a simple process and is easy to produce on a large scale, but the disadvantage is that the particle size of the product is not easy to control, and most of them are micron-sized, and the uniformity is poor , compared with fine crystals, the lithium ion intercalation reaction path of coarse grains is longer, which is not conducive to high current charge and discharge, and the high rate performance is poor

Method used

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  • Method for synthesizing SiO2 lithium ion battery cathode material lithium titanate
  • Method for synthesizing SiO2 lithium ion battery cathode material lithium titanate
  • Method for synthesizing SiO2 lithium ion battery cathode material lithium titanate

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Experimental program
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Effect test

Embodiment 1

[0021] (1) Weigh the corresponding stoichiometric precursor according to the molar ratio of 0.0172 P123: 1TEOS: 6HCl, dissolve P123 in deionized water, stir until it is completely dissolved, then add 2mol / L hydrochloric acid, and stir for 3 hours with slight heat; Slowly add TEOS dropwise. After the dropwise addition, stir at high speed in a water bath at 30°C for 24h, then transfer to a stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallize at 100°C for 24h; Wash until neutral, and dry at 100°C; heat the synthesized material to 550°C at a rate of 1°C / min in a muffle furnace, and keep it warm for 16 hours to obtain SiO with nanopores. 2 template. Nanoporous SiO 2 The scanning electron microscope image of the template is shown in figure 1 shown.

[0022] (2) Weigh a certain amount of lithium acetate and tetrabutyl titanate with a molar ratio of Li:Ti of 4.2:5, disperse them in anhydrous ethanol solvent, and slowly add them dropwise to SiO 2 On t...

Embodiment 2

[0024] (1) Weigh the corresponding stoichiometric precursor according to the molar ratio of 0.0172 P123: 1TEOS: 6HCl, dissolve P123 in deionized water, stir until it is completely dissolved, then add 2mol / L hydrochloric acid, and stir for 3 hours with slight heat; Slowly add TEOS dropwise. After the dropwise addition, stir at high speed in a water bath at 40°C for 24h, then transfer to a stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallize at 100°C for 24h; the obtained product is deionized Wash with water until neutral, and dry at 100°C; heat the synthesized material to 600°C in a muffle furnace at a rate of 1°C / min, and keep it warm for 12 hours to obtain SiO with nanopores. 2 template.

[0025] (2) Weigh a certain amount of lithium oxalate and methyl titanate with a molar ratio of Li:Ti of 4.2:5, disperse them in anhydrous ethanol solvent, and slowly add them dropwise to SiO at 120°C. 2 On the template, the precursor is obtained after evapora...

Embodiment 3

[0027] (1) Weigh the corresponding stoichiometric precursor according to the molar ratio of 0.0172 P123: 1TEOS: 6HCl, dissolve P123 in deionized water, stir until it is completely dissolved, then add 2mol / L hydrochloric acid, and stir for 3 hours with slight heat; Slowly add TEOS dropwise. After the dropwise addition, stir at high speed in a water bath at 30°C for 24h, then transfer to a stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallize at 100°C for 24h; Wash until neutral, and dry at 100°C; heat the synthesized material to 550°C at a rate of 3°C / min in a muffle furnace, and keep it warm for 16 hours to obtain SiO with nanopores. 2 template.

[0028] (2) Weigh a certain amount of lithium acetate and methyl titanate with a molar ratio of Li:Ti of 4.1:5, disperse them in anhydrous ethanol solvent, and slowly add them dropwise to SiO at 120°C. 2 On the template, the precursor is obtained after evaporating the solvent; the resulting mixture is si...

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Abstract

The invention discloses a method for synthesizing SiO2 lithium ion battery cathode material lithium titanate, which provides the method for preparing a nano lithium titanate material with excellent high rate performance and cycle performance. The method comprises the following steps: weighting a certain amount of P123, dissolving with deionized water, stirring to completely dissolve, adding 2mol / L of hydrochloric acid, performing micro-thermal agitation, slowly adding TEO drop by drop, stirring with high speed for 10-30 hours under water bath at the temperature of 20-50 DEG C, then conversing to a stainless steel reaction kettle, crystallizing for 24-28 hours at the temperature of 80-120 DEG C; using deionized water to wash the product to neutrality, drying under the temperature of 100 DEG C, heating the synthetic material in a muffle furnace with the heating speed of 1-5 DEG C / min to the temperature of 450-650 DEG C, keeping the temperature for 12-24 hours to obtain a nano mesoporous SiO2 template, heating the nano mesoporous SiO2 template to the temperature of 80-120 DEG C, dissolving a certain amount of lithium resource and titanium source by a corresponding solvent, adding into the template drop by drop, then sintering in a tube furnace under the temperature of 750-850 DEG C for 8-12 hours, removing the template by a hot highly concentrated alkali solution, washing by distilled water, drying and crushing to obtain the lithium titanate.

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 SiO of lithium titanate, a negative electrode material of a lithium ion battery. 2 Template synthesis method. Background technique [0002] At present, most lithium-ion battery negative electrode materials use various lithium-intercalated carbon materials, but the potential of the carbon electrode is very close to that of lithium. When the battery is overcharged, metal lithium is easily precipitated on the surface of the carbon electrode, forming dendrites and causing safety problems. At the same time During the repeated intercalation and deintercalation of lithium ions, the structure of carbon materials will be damaged, resulting in capacity attenuation. Spinel lithium titanate is used as the negative electrode material of lithium-ion batteries, the theoretical specific capacity is 175 mAh / g, and the actual specific capacity rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485C01G23/00B82Y30/00
CPCY02E60/122Y02E60/10
Inventor 王康平杨茂萍杨续来郭钰静谢佳
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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