Method for preparing cathode material carbon-coated lithium titanate for lithium ion battery from metatitanic acid

A technology of carbon-coated lithium titanate and lithium-ion batteries, which is applied to battery electrodes, circuits, electrical components, etc., can solve the problems of poor electrical conductivity, increased process, difficult to remove, etc., and achieves moderate conditions, easy industrial production, and technological process simple effect

Inactive Publication Date: 2013-12-18
HUNAN UNIV
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Problems solved by technology

In addition, the intermediate product metatitanic acid H2TiO3 obtained in the process of producing nano-TiO2 by sulfuric acid method contains a certain amount of iron and chromium When using metatitanic acid to prepare battery-grade lithium titanate, these impurities must be removed first, thus increasing the process, so using metatitanic acid H2TiO3The method of preparing lithium titanate Li4Ti5O12 as a titanium source has received little attention at home and abroad
The literature "Preparation and Electrochemical Properties of Quasi-nanocrystalline Lithium Titanate" (Wang Xin, Bao Liying, Su Yuefeng, etc. "Nonferrous Metals", Volume 62, 17-21, 2010) has reported the use of metatitanic acid H2 TiO3 and lithium carbonate to prepare quasi-nanocrystalline Li4Ti5O12, and finally get is Li4Ti5O12 particles without carbon coating, so Li4Ti 5O12The disadvantage of poor electrical conductivity has not been improved, and the performance is poor
In addition, in the literature, ammonia water is used to remove metal ions contained in metatitanic acid. According to the basic principles of coordination chemistry, ammonia water is difficult to form stable complexes with iron ions, chromium ions, etc., so it is difficult to remove metatitanic acid with ammonia water. The main impurities such as iron ions and chromium ions contained in

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  • Method for preparing cathode material carbon-coated lithium titanate for lithium ion battery from metatitanic acid
  • Method for preparing cathode material carbon-coated lithium titanate for lithium ion battery from metatitanic acid
  • Method for preparing cathode material carbon-coated lithium titanate for lithium ion battery from metatitanic acid

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Embodiment 1

[0023] First, use deionized water and oxalic acid to prepare a certain concentration of oxalic acid solution, then stir and mix with metatitanic acid evenly, filter with a Buchner funnel, and rinse the filtrate with deionized water to obtain purified metatitanic acid. Lithium source Li 2 CO 3 , Purified metatitanic acid H 2 TiO 3 Mix the three raw materials with the carbon source pitch according to the following ratio, and the molar ratio of Li:Ti is 4.1:5. Add Li 2 CO 3 and H 2 TiO 3 , the amount of asphalt added is 5% of the sum of the weight of the lithium source and the titanium source; then it is fully mixed by ball milling, and the temperature is raised to 120 °C under an argon atmosphere 0 C for 3 hours at a constant temperature, then raised to 850 0 C for 12 hours, and finally cooled to room temperature.

[0024] figure 1 (a) and (b) are metatitanic acid H 2 TiO 3 Low and high magnification scanning electron micrographs of H 2 TiO 3 The size of the second...

Embodiment 2

[0026] Metatitanic acid H purified from lithium source LiOH and titanium source 2 TiO 3 Mix the three raw materials with the carbon source phenolic resin according to the following ratio, the molar ratio of Li:Ti is 4:5, add LiOH and H 2 TiO 3 , the amount of phenolic resin added is 3% of the sum of the weight of the lithium source and the titanium source, and then it is thoroughly mixed by ball milling, and then in an argon atmosphere, the temperature is raised to 180 0 C for 2 hours at a constant temperature, then raised to 700 0 C at constant temperature for 20 hours; finally cooled to room temperature.

[0027] The carbon-coated lithium titanate composite powder material was prepared by the above method, and it was used as the negative electrode active material of the lithium-ion battery to prepare a lithium-ion button-type experimental battery, and its performance was tested. The results are as follows: Figure 4 shown. in Figure 4 The voltage-specific capacity cur...

Embodiment 3

[0029] Lithium source Li 2 CO 3 , Purified metatitanic acid H 2 TiO 3 and the three raw materials of glucose as carbon source were mixed uniformly by ball milling according to the following addition ratio, and the molar ratio of Li:Ti was 4.1:5. 2 CO 3 and H 2 TiO 3 , the amount of glucose added is 5% of the sum of the weight of the lithium source and the titanium source; then under a nitrogen atmosphere, the temperature is raised to 350 0 C for 1 hour, then the temperature continued to rise to 900 0 C for another 15 hours; finally cooled to room temperature.

[0030] Carbon-coated Li was prepared by the above method 4 Ti 5 o 12 / C composite powder material is used as the negative electrode active material of lithium ion battery to prepare lithium ion button-type experimental battery, and its electrochemical performance is tested. The results are as follows Figure 5 shown. in Figure 5 The voltage-specific capacity curve of (a) shows that the first discharge / char...

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Abstract

The invention relates to a method for preparing a cathode material carbon-coated lithium titanate for a lithium ion battery from metatitanic acid. According to the method, metatitanic acid H2TiO3 is used as a titanium source, lithium carbonate or lithium hydroxide is used as a lithium source, and asphalt, phenolic resin or glucose is used as a carbon source. The carbon-coated lithium titanate Li4Ti5O12 / C can be obtained by washing metatitanic acid by oxalic acid and filtering, then uniformly mixing the three raw materials by a ball mill in a certain ratio, drying and then placing the mixture in a high-temperature heating furnace, and sintering in an inert gas shielding condition. According to the method disclosed by the invention, the selected titanium source, namely, metatitanic acid, is only about 1 / 5 of a titanium source, namely, titanium oxide TiO2 used in conventional lithium titanate preparation, so that the prepared Li4Ti5O12 / C is relatively low in cost, excellent in charge-discharge circulation performance, and capable of meeting requirements on cathode materials for lithium ion batteries. The method disclosed by the invention is simple in preparation process, easy for realization of industrial production, free from environmental pollution, and environmentally-friendly.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion battery negative electrode material, in particular to a negative electrode active material lithium titanate and a preparation method thereof. Background technique [0002] Lithium-ion batteries have been widely used in various portable appliances such as mobile phones, notebook computers, and digital cameras since their commercialization in 1991. In recent years, with the rapid development of hybrid electric vehicles and pure electric vehicles, people have put forward higher requirements for the capacity, cycle life and safety of lithium-ion batteries as power sources. At present, the negative electrode active materials of commercial lithium-ion batteries use various graphite-based carbon materials, but graphite negative electrodes are prone to precipitate lithium dendrites under high-current charging and discharging conditions, so there are potential safety hazards. Compared with graphite...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M4/62
CPCY02E60/10
Inventor 陈玉喜於洪将龚立君
Owner HUNAN UNIV
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