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Preparation method of single crystal type high-nickel ternary layered positive electrode material

A positive electrode material and ternary material technology, which is applied in the field of preparation of high-nickel ternary positive electrode materials, can solve problems such as high temperature flatulence, affecting electrochemical performance, and poor thermal stability

Inactive Publication Date: 2021-03-30
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, the ternary NCM (NCA) materials that can be seen on the market are all micron-sized secondary balls formed by the agglomeration of fine primary particles. This type of secondary spherical particles has the following problems: poor compaction density. Under high pressure, the secondary ball will be broken, the internal particles will be directly exposed to the electrolyte, and the side reaction will be aggravated. Side reactions occur on the surface, resulting in more inert rock-salt phases, which affect the electrochemical performance; in addition, the secondary spherical particles also have problems such as high temperature flatulence and capacity recovery during charging and discharging.
[0004] The researchers tried to make LiNi x co y m 1-x-y o 2 The material is made into a single crystal morphology to solve the above-mentioned problems, and many solutions have been proposed, but it is inevitable that they are not well considered in the calcination process. In their reports, the sintering temperature is above 900 ° C. Although this temperature It is suitable for low-nickel (x<0.5) ternary single crystals, but high-nickel materials will have poor thermal stability and severe cation mixing at high temperatures, so high-nickel and low-nickel cannot be directly generalized

Method used

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  • Preparation method of single crystal type high-nickel ternary layered positive electrode material
  • Preparation method of single crystal type high-nickel ternary layered positive electrode material
  • Preparation method of single crystal type high-nickel ternary layered positive electrode material

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Experimental program
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Effect test

Embodiment 1

[0024] The single crystal structure ternary cathode material LiNi was prepared according to the following steps 0 8 co 0.1 mn 0.1 o 2 .

[0025] 1) 2.41g Co 3 o 4 , 1.45g LiOH·H 2 O and 9.10 g KNO 3 Grind and mix well to obtain mixture A. Put the above mixture A in an alumina crucible, pre-fire it in a muffle furnace at 500°C for 5h, then raise the temperature to 750°C and keep it for 15h, then cool to room temperature, and the obtained product is deionized After washing with water for several times, suction filtration, and drying at 120 °C for 24 h, single crystal LiCoO was obtained 2 matrix.

[0026] 2) Weigh 57.04g NiCl 2 ·6H 2 O, 5.94 g MnCl 2 4H 2 O and 11.33g LiOH·H 2 O, with the above 2.94g LiCoO 2 The matrix was ground and mixed evenly to obtain mixture B.

[0027] 3) Press the above mixture B into tablets, the pressure is 20MPa, the tableting time is 2min, put into a crucible and calcined in a tube furnace under an oxygen atmosphere, pre-calcined at 500...

Embodiment 2

[0030] The single crystal structure ternary cathode material LiNi was prepared according to the following steps 0 6 co 0.2 mn 0.2 o 2 .

[0031] 1) Weigh 2.41g Co 3 o 4 , 1.45g LiOH·H 2O and 5.26g NaCl were thoroughly ground and mixed uniformly to obtain mixture A, which was placed in an alumina crucible, pre-fired in a muffle furnace at 500°C for 5h, then raised to 850°C for 15h, then cooled to room temperature, and The obtained product was washed several times with deionized water, filtered with suction, and dried at 120 °C for 24 h to obtain single crystal LiCoO 2 matrix.

[0032] 2) Weigh 23.65g NiSO 4 ·6H 2 O, 5.07g MnSO 4 ·H 2 O and 4.43g Li 2 CO 3 , with the above 2.94gLiCoO 2 The matrix is ​​ground and mixed evenly.

[0033] 3) Press the above mixture into tablets with a pressure of 20 MPa and a tablet pressing time of 2 minutes, put it into a crucible and calcinate it in an oxygen atmosphere in a tube furnace, pre-calcine at 650°C for 5 hours, then rais...

Embodiment 3

[0036] The single crystal structure ternary cathode material LiNi was prepared according to the following steps 0 5 co 0.2 mn 0.3 o 2 .

[0037] 1) 2.41g Co 3 o 4 , 1.45g LiOH·H 2 O and 6.71g KCl were thoroughly ground and mixed uniformly to obtain mixture A, which was placed in an alumina crucible, pre-fired in a muffle furnace at 500°C for 5h, then raised to 800°C for 15h, then cooled to room temperature, and The obtained product was washed several times with deionized water, filtered with suction, and dried at 120 °C for 24 h to obtain single crystal LiCoO 2 matrix.

[0038] 2) Weigh 21.81g Ni(NO 3 ) 2 ·6H 2 O, 11.30g Mn(NO 3 ) 2 4H 2 O and 4.43g Li 2 CO 3 , with the above 2.94g LiCoO 2 The matrix was ground and mixed evenly to obtain mixture B.

[0039] 3) Press the above mixture B into tablets with a pressure of 20 MPa and a tablet pressing time of 2 minutes, put it into a crucible and calcinate it in an oxygen atmosphere in a tube furnace, pre-calcine at...

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Abstract

The invention designs a preparation method of a single crystal type high-nickel ternary layered positive electrode material LiNixCoyM1-x-yO2 (x is more than or equal to 0.5 and less than or equal to 0.95, y is more than or equal to 0.025 and less than or equal to 0.2, and M is one or two of Mn and Al). Monocrystalline lithium cobalt oxide is prepared through a molten salt method, then nickel, manganese (aluminum) and a certain amount of lithium source are supplemented, and ternary monocrystalline particles are obtained. The method has the advantages that (1) a new thought is provided and can be suitable for preparing the high-nickel monocrystalline ternary material, and the problems that the thermal stability of the high-nickel material becomes poor and cation mixed arrangement is intensified due to the too high sintering temperature are solved; and (2) the LiCoO2 and the LiNixCoyM1-x-yO2 are both of a layered structure, a LiCoO2 single crystal matrix is very easy to prepare through amolten salt method, and the single crystal LiNixCoyM1-x-yO2 positive electrode material is obtained through mutual diffusion of other supplementary elements in a solid phase under proper external conditions.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a preparation method of a high-nickel ternary positive electrode material with a single crystal morphology. Background technique [0002] At present, lithium-ion batteries have been widely used in various fields due to their unique advantages, but at the same time, the improvement of their energy density has become the most concerned issue of various energy fields and scientific researchers. Improve energy density, but the service life of lithium-ion batteries will also be greatly reduced, which is not suitable for industrialization and civilian popularization. [0003] Cathode material is an important part of lithium-ion batteries. Compared with other cathode materials, ternary cathode materials with high energy density have obvious advantages. NCM (NCA) materials give full play to the three elements of nickel, cobalt, and manganese (aluminum). Synergi...

Claims

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Application Information

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IPC IPC(8): C01G53/00H01M4/485H01M4/505H01M4/525
CPCC01G53/006C01P2004/03C01P2006/40H01M4/485H01M4/505H01M4/525Y02E60/10
Inventor 张联齐廖建国张洪周宋大卫时喜喜李春亮
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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