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Spherical high-nickel cobalt-free single crystal precursor and preparation method thereof

A precursor, high-nickel technology, applied in chemical instruments and methods, inorganic chemistry, nickel compounds, etc., can solve the problems of high-nickel-cobalt-free precursors with high crystallinity, unfavorable sintering single crystallization, small specific surface, etc. The effect of improving the rate and cycle performance, reducing the single crystallization, and improving the ratio table

Active Publication Date: 2021-06-11
SHAANXI COAL & CHEM TECH INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that the high-nickel-cobalt-free precursor prepared by the conventional co-precipitation method has high crystallinity and small specific surface area, which is not conducive to sintering single crystallization, the present invention provides a spherical high-nickel-cobalt-free single crystal precursor and The preparation method effectively improves the ratio of the precursor, reduces the crystallinity of the material, and improves the sphericity of the small particle size precursor, which is beneficial to the consistency of the sintering process and the single crystallization of the sintering process.

Method used

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  • Spherical high-nickel cobalt-free single crystal precursor and preparation method thereof
  • Spherical high-nickel cobalt-free single crystal precursor and preparation method thereof
  • Spherical high-nickel cobalt-free single crystal precursor and preparation method thereof

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Effect test

Embodiment 1

[0030] Step 1. Raw material solution preparation: Nickel sulfate and manganese sulfate are prepared into a 2mol / L solution according to the molar ratio of 0.90:0.08, and a sodium metaaluminate solution of 0.1mol / L is prepared as a doping solution, and sodium hydroxide is dissolved to a concentration of 10mol / L lye; use 13mol / L ammonia solution as complexing agent.

[0031] Step 2. Preparation of reaction bottom liquid: Add the prepared lye and ammonia solution into a reaction kettle filled with nitrogen and half a kettle of water. The reaction kettle adopts paddles with paddle diameter / kettle diameter = 0.60 to adjust the pH of the bottom liquid The value is 13.0, the ammonia concentration in the reaction bottom solution is controlled to be 10g / L, the stirring speed is controlled at 500rpm, and the temperature is controlled at 40°C.

[0032] Step 3, the reaction starts, the nickel-manganese mixed salt, aluminum salt, lye and ammonia solution are added to the reaction kettle eq...

Embodiment 2

[0037] Step 1. Raw material solution preparation: nickel sulfate and manganese sulfate are prepared into a 2mol / L solution according to the molar ratio of 0.60:0.35, and a magnesium sulfate solution of 0.1mol / L is prepared as a doping solution, and sodium hydroxide is dissolved to a concentration of 10mol / L lye; use 13mol / L ammonia solution as complexing agent.

[0038] Step 2, preparation of the reaction bottom liquid: add the prepared lye and ammonia solution into the reactor filled with half a kettle of water with nitrogen, and the reactor adopts paddles with paddle diameter / kettle diameter = 0.65 to adjust the pH of the bottom liquid The value is 12.5, the ammonia concentration is 4g / L, the stirring speed is controlled at 300rpm, and the temperature is controlled at 20°C.

[0039] Step 3, the reaction starts, the nickel-manganese mixed salt, magnesium salt, lye and ammonia solution are added to the reaction kettle equipped with the reaction bottom liquid at the same time,...

Embodiment 3

[0044] Step 1. Raw material solution preparation. Nickel nitrate and manganese nitrate are prepared into a 2mol / L solution according to the molar ratio of 0.80:0.17, and a zirconium nitrate solution of 0.1mol / L is prepared as a doping solution, and sodium hydroxide is dissolved to a concentration of 10mol / L. L of lye; use 13mol / L of ammonia solution as complexing agent.

[0045] Step 2. Preparation of reaction bottom liquid: Add the prepared lye and ammonia solution into a reactor filled with nitrogen and half a pot of water. The reactor adopts paddle diameter / kettle diameter=0.55 to adjust the pH of the bottom liquid The value is 12.5, the ammonia concentration is 6g / L, the stirring speed is controlled at 400rpm, and the temperature is controlled at 30°C.

[0046] Step 3, the reaction starts, the nickel-manganese mixed salt, zirconium salt, lye and ammonia solution are added to the reaction kettle equipped with the reaction bottom liquid at the same time, the ammonia concentr...

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Abstract

The invention discloses a spherical high-nickel cobalt-free single crystal precursor and a preparation method thereof, a low coprecipitation reaction temperature of 20-40 DEG C is adopted, the crystallinity of the precursor is effectively reduced and the specific surface of the precursor is improved by increasing the feeding speed section by section, changing the pH value and the like, in addition, a long-diameter paddle is adopted, the paddle diameter / kettle diameter is 0.50-0.65, the stirring strength is improved, and the dispersity and sphericity of the single crystal precursor are improved. The process is simple, the process is easy to control, the method is suitable for large-scale production, the prepared high-nickel cobalt-free single crystal precursor is good in dispersity and sphericity, the specific surface area is larger than or equal to 20 m < 2 > / g, the crystallinity is low, the half-peak width FWHM101 of the precursor obtained through XRD testing is larger than or equal to 0.8, and sintering single crystallization is obvious.

Description

technical field [0001] The invention belongs to the technical field of positive electrode materials for lithium ion batteries, in particular to a spherical high-nickel and cobalt-free single crystal precursor and a preparation method thereof. Background technique [0002] Since cobalt is a scarce resource, the price of cobalt fluctuates greatly. In order to get rid of the monopoly control of resources, the development of cobalt-free products is technically accelerated. The advantage of high-nickel and cobalt-free materials is that the scarce cobalt element is removed, material cost is reduced, nickel content is increased, and the specific capacity of the material is increased. At the same time, the increase in manganese content can stabilize the structure. However, the increase in nickel content and the complete absence of cobalt lead to adverse results such as poor electrical conductivity, severe lithium-nickel mixing, and poor thermal stability. Especially when the high-ni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/485H01M4/505H01M4/525H01M10/0525
CPCC01G53/006H01M4/505H01M4/525H01M4/485H01M10/0525C01P2002/72C01P2004/03C01P2006/12C01P2006/40Y02E60/10
Inventor 张诚寇亮陈微微孙静张超王继峰
Owner SHAANXI COAL & CHEM TECH INST
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