Preparation method of Co3O4 with large grain size and uniformly doped with aluminum

A technology of tricobalt tetroxide and large particle size, which is applied in the direction of cobalt oxide/cobalt hydroxide, structural parts, electrical components, etc. It can solve the problem that the uniformity of particle size distribution is not as good as that of cobalt carbonate system, the compound that is easy to separate aluminum, and the uneven incorporation of aluminum etc. to achieve excellent cycle performance, high specific capacity, and uniform particle size distribution

Active Publication Date: 2018-05-08
취저우화여우코발트뉴머터리얼컴퍼니리미티드
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of using the hydroxide system for wet doping is that the primary particles are relatively coarse and the particle size is small, only 8-10 μm. This system is difficult to prepare large particle size (above 15 μm) cobalt tetroxide
[0003] The outstanding problems of aluminum-doped cobalt tetroxide are: 1. The cobalt carbonate system is used for wet doping with aluminum. The higher the amount of aluminum doped, the more uneven the aluminum doping, and it is easy to separate aluminum compounds; Uniformity is relatively easy to solve, but it is difficult to increase the particle size, and the uniformity of particle size distribution is not as good as that of cobalt carbonate system

Method used

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  • Preparation method of Co3O4 with large grain size and uniformly doped with aluminum
  • Preparation method of Co3O4 with large grain size and uniformly doped with aluminum
  • Preparation method of Co3O4 with large grain size and uniformly doped with aluminum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] ①Dissolve aluminum sulfate into cobalt sulfate solution, and prepare mixed metal salt solutions with cobalt ion and aluminum ion concentrations of 90g / L and 0.062g / L respectively for use.

[0042] ②Inject a certain amount of pure water into the reaction kettle as the bottom liquid, add ammonium bicarbonate solution to adjust the pH value to 7.5, raise the temperature to 40°C, and mix the cobalt-aluminum mixed salt solution and the carbonic acid concentration of 230g / L at a stirring speed of 140rpm The ammonium hydrogen solution is added into the reaction kettle at the same time to cause precipitation reaction. During the feeding process, the pH value of the reaction solution is controlled at about 7.0 until the material grows to 8 μm. After the feeding is completed, the stirring is stopped. Leave the space to continue feeding, so that the crystals continue to grow;

[0043] ③Reduce the stirring speed to 30rpm, and continue feeding. During the feeding process, control th...

Embodiment 2

[0052] ①Dissolve aluminum chloride into cobalt chloride solution, and prepare mixed metal salt solutions with cobalt ion and aluminum ion concentrations of 120g / L and 0.42g / L respectively for use.

[0053] ②Inject a certain amount of pure water into the reaction kettle as the bottom liquid, add the ammonium carbonate solution to a pH value of 8.0, raise the temperature to 50°C, and add the cobalt-aluminum mixed salt solution and the ammonium carbonate solution with a concentration of 210g / L into the reaction kettle at the same time at 145rpm During the feeding process, the pH value of the reaction solution was controlled at about 7.5 until the material grew to 9 μm. After the feeding was completed, the stirring was stopped. continue to grow;

[0054] ③Reduce the stirring speed to 35rpm, and continue feeding. During the feeding process, control the pH value of the reaction solution within the range of 8.0, and the reaction temperature is 50°C. When the material reaches 85% of t...

Embodiment 3

[0064] ① Dissolve aluminum nitrate into cobalt nitrate solution, and prepare mixed metal salt solutions with cobalt ion and aluminum ion concentrations of 160g / L and 1.11g / L respectively for use.

[0065] ②Inject a certain amount of pure water into the reaction kettle as the bottom liquid, add ammonium bicarbonate solution to adjust the pH to 7.5, raise the temperature to 60°C, and add a certain concentration of cobalt-aluminum mixed salt solution and ammonium bicarbonate solution into the reaction kettle at the same time at 150rpm Precipitation reaction occurs. During the feeding process, the pH value of the reaction solution is controlled at about 7.3 until the material grows to 10 μm. After the feeding is completed, stop stirring. grow;

[0066] ③Reduce the stirring speed to 40rpm and continue feeding. During the feeding process, control the pH value of the reaction solution within the range of 7.5, and the reaction temperature is 60°C. When the material reaches 85% of the ...

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Abstract

The invention relates to a preparation method of Co3O4 with large grain size and uniformly doped with aluminum. The invention provides the preparation method of the Co3O4 which is uniformly doped withaluminum and is large in grain size and uniform in particle distribution, and the obtained Co3O4 with the large grain size and uniformly doped with aluminum can completely conform to the requirementof preparation of 4.45V high-voltage lithium cobalt oxide. According to the method, the large-grain size and aluminum-doped cobalt carbonate is synthesized by a wet method, and the problems of difficulty in enlargement of cobalt hydroxide (or hydroxyl cobalt) system grain size and non-uniform particle distribution are solved; with the regard to the problem of uniform aluminum doping of a cobalt carbonate system, a parameter is set from principle, an aluminum compound is prevented from being independently separated out and gathered, the doped Al element can be uniformly distributed in the Co3O4, the grain size reaches 15 micrometers or above, and the particle distribution is uniform; and the lithium cobalt oxide prepared from the aluminum-doped Co3O4 has high specific capacity and excellentcycle property under 4.45V.

Description

technical field [0001] The invention relates to a preparation method of battery-grade tricobalt tetroxide, in particular to a preparation method of tricobalt tetroxide for high-voltage lithium cobaltate. Background technique [0002] 3C electronic products are required to be light and compact, and the corresponding batteries need to have high energy density. Lithium cobaltate is currently the most important positive electrode material for 3C electronic products, and its energy density determines the energy density of lithium-ion batteries to a certain extent. High-voltage lithium cobalt oxide has the characteristics of high gram capacity and high voltage, and has higher energy density than conventional lithium cobalt oxide. It is the main direction of research and development of lithium cobalt oxide in the future. High-voltage lithium cobalt oxide is doped with certain metal elements in lithium cobalt oxide to improve the crystal structure stability of lithium cobalt oxide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/52C01G51/04
CPCC01G51/04C01P2002/80C01P2004/61C01P2006/40H01M4/52Y02E60/10
Inventor 田礼平刘人生陈强秦才胜虞颖周恩娄熊铜兴张凯龙
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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