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Preparation method of single crystal NCM ternary positive electrode material precursor

A technology of cathode materials and precursors, which is applied in the field of preparation of single crystal NCM ternary cathode material precursors, can solve the problems of the influence of cathode material performance, poor particle uniformity, and difficulty in sintering subsequent cathode materials.

Active Publication Date: 2021-04-23
福建常青新能源科技有限公司
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AI Technical Summary

Problems solved by technology

Due to the characteristics of the precursor seed stage in the traditional method, when preparing NCM ternary precursor products with single crystal small particles, it is easy to cause multi-level agglomeration and poor uniformity of particles in the reaction stage, resulting in subsequent sintering of positive electrode materials. Difficulty, it also has a great impact on the sintering time, which in turn causes the performance of the subsequent positive electrode material to be affected by its precursor stage

Method used

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  • Preparation method of single crystal NCM ternary positive electrode material precursor
  • Preparation method of single crystal NCM ternary positive electrode material precursor
  • Preparation method of single crystal NCM ternary positive electrode material precursor

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preparation example Construction

[0030] Please refer to Figure 4 , a method for preparing a single crystal NCM ternary positive electrode material precursor based on a particle size controllable reactor, the particle size controllable reactor comprising: a reaction unit (10) and a solid extraction unit (20); the preparation Methods include:

[0031] S1, Ni with a total concentration of 1.0-2.2mo1 / L according to the proportion x :Co y :Mn z Sulphate solution, 4-10mol / L caustic soda solution and 20% ammonia water are added into the reaction unit (10) and an inert gas is fed into the first-stage reaction at the same time, wherein the reaction conditions are: the stirring speed is 800-1100r / min , the pH is 11.50~13.00, the temperature is 40~60℃, and the inert gas flow rate is 0.1~2m 3 / h, and x+y+z=1, 1.0>x≥0.5;

[0032] S2, after measuring particle D50 = 1.5-1.8 μm, increase the ammonia value in the reactor to carry out the second-stage reaction, wherein the reaction conditions are: keep the stirring speed...

Embodiment 1

[0038] According to the molar ratio of nickel, cobalt and manganese ions as 60:20:20, prepare NiSO with a concentration of 1.6mol / L 4 、CoSO 4 , MnSO 4 For the mixed solution, use a precision metering pump to add the mixed solution, 8mol / L caustic soda solution, and 20% industrial ammonia water filtered by a 200-mesh filter cloth into the reaction vessel 12 to carry out the first-stage reaction, and the stirring speed of the reactor is 1050r / min, the pH is 12.30, the temperature is 55°C, and nitrogen is maintained at 0.2m 3 / h long pass, reaction 1.5h; In the second stage, after using the Dandong Baite 2600 model particle size analyzer to measure the particle D50=1.5 μm, control the ammonia value in the reaction vessel 12 at 3-4g / L, and control the pH to 10.60. Open the overflow valve 17, the solid lifting valve 22 and the backflow valve 27, and open the drain valve 24 by 15%, filter the mother liquor with a solid lifting device to concentrate to improve the solid content an...

Embodiment 2

[0040] According to the molar ratio of nickel, cobalt and manganese ions as 65:15:20, prepare NiSO with a concentration of 1.6mol / L 4 、CoSO 4 , MnSO 4 For the mixed solution, use a precision metering pump to add the mixed solution, 8mol / L caustic soda solution, and 20% industrial ammonia water filtered by a 200-mesh filter cloth into the reaction vessel 12 to carry out the first-stage reaction, and the stirring speed of the reactor is 1030r / min, pH is 12.22, temperature is 55°C, nitrogen gas is kept at 0.3m 3 / h long pass, reaction 1.5h; In the second stage, after using the Dandong Baite 2600 model particle size analyzer to measure the particle D50=1.5 μm, control the ammonia value in the reaction vessel 12 at 3-4g / L, and control the pH to 10.50. Open the overflow valve 17, the solid lifting valve 22 and the backflow valve 27, and open the drain valve 24 by 15%, filter the mother liquor with a solid lifting device to concentrate to improve the solid content and adjust the s...

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Abstract

The invention provides a preparation method of a single crystal NCM ternary positive electrode material precursor, which comprises the following steps of S1, adding a Nix: Coy: Mnz sulfate solution with the total concentration of 1.0-2.2 mol / L, a 4-10 mol / L caustic soda solution and 20% ammonia water into a reaction unit (10) according to a ratio, and introducing inert gas to carry out a first-stage reaction under the reaction conditions that the stirring speed is 800-1100 r / min, the pH is 11.50-13.00, the temperature is 40-60 DEG C, the inert gas flow is 0.1-2 m<3> / h, x+y+z=1, and 1.0>x> / =0.5, S2, after measuring that the particle D50 is equal to 1.5-1.8 mum, increasing the ammonia value in the reaction kettle to carry out a second-stage reaction under the reaction conditions that the stirring speed, the temperature and the airflow speed are kept unchanged, the ammonia water concentration is controlled to be 2-7 g / L, the pH is controlled to be 9.00-11.00, concentrating by utilizing a solid extraction unit (20) to increase the solid content and adjust the clear speed of a solid extractor, and finally measuring the particle D50 to be 3.8-4.5 mum and stopping the reaction, and S3, washing, drying and screening the slurry to obtain the single crystal NCM ternary positive electrode material precursor.

Description

technical field [0001] The invention relates to a preparation method of a single-crystal NCM ternary cathode material precursor. Background technique [0002] With the rapid development of the lithium battery industry and the use of new energy vehicles in the transportation field, high-nickel NCM ternary cathode materials have always been considered the most mainstream development direction. However, in recent years, natural problems of domestic new energy vehicles have frequently occurred. The high-nickel ternary material system is quite controversial in the market. Affected by this, single-crystal NCM cathode materials with better safety performance have gradually become the focus of domestic cathode material companies. In order to meet the future application of nickel-cobalt-lithium-manganese-oxide ternary materials in small high-energy-density lithium-ion batteries for power batteries and electronic products, the development direction of NCM nickel-cobalt-lithium-mangan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/505H01M4/525H01M10/0525
CPCC01G53/006H01M4/505H01M4/525H01M10/0525C01P2004/03C01P2006/10C01P2006/11C01P2006/12C01P2004/61C01P2006/82C01P2006/80Y02E60/10
Inventor 张刚康杰石小东张东学江福茂王楚明晁锋刚沈陆彬钟庆磊黄萍黄伟超颜志梁
Owner 福建常青新能源科技有限公司
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