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Preparation method of low-surface-residual-alkali nickel cobalt manganese ternary positive electrode material

A nickel-cobalt-manganese ternary and positive electrode material technology, which is applied in chemical instruments and methods, electrical components, battery electrodes, etc., can solve the problems of active lithium loss, material specific capacity reduction, and difficulty in industrialization, etc., to reduce residual alkali , reduce pH value, improve the effect of consistency and stability

Active Publication Date: 2019-07-26
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method of water washing to remove residual alkali is low cost and easy to operate, water washing will cause the loss of active lithium in the material, which will reduce the specific capacity of the material after water washing, and the material after water washing will have a negative effect on H in the air. 2 O and CO 2 become more sensitive and affect the normal use of the material
At the same time, because the nickel-cobalt-manganese ternary positive electrode material itself is alkaline and is easily corroded by acid, there are also great problems in washing with acid aqueous solution, especially in hydrometallurgical recovery technology, acid solution is often used to remove transition metals. The leaching of ions limits the use of acidic aqueous solutions. Even weak acids have a certain leaching effect, so acidic aqueous solutions are rarely used to remove residual alkali on the surface of nickel-cobalt-manganese ternary positive electrode materials.
In addition, because the material is very sensitive to moisture, the washing method used in the industry also makes the material less consistent
Other reported methods for removing residual alkali on the surface of materials, most of which are in the laboratory processing stage, cannot guarantee the consistency of materials, and it is difficult to realize industrialization

Method used

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  • Preparation method of low-surface-residual-alkali nickel cobalt manganese ternary positive electrode material
  • Preparation method of low-surface-residual-alkali nickel cobalt manganese ternary positive electrode material
  • Preparation method of low-surface-residual-alkali nickel cobalt manganese ternary positive electrode material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Step (1): take boric acid (H 3 BO 3 ) solid powder 0.006g, it was added to 100mL ethanol and stirred until dissolved to obtain a boric acid concentration of 0.001mol / L ethanol solution containing boric acid, measure 1mL for subsequent use.

[0063] Step (2): Weigh 1g of nickel-cobalt-manganese ternary cathode material LiNi 0.90 co 0.06 mn 0.04 o 2 , the material was added to 1 mL of ethanol solution containing boric acid, stirred for 1 min, filtered, and the obtained precipitate was repeatedly washed with absolute ethanol three times, and then dried in a vacuum oven at 80° C. for 2 h.

[0064] Step (3): put the dried nickel-cobalt-manganese ternary positive electrode material into a tube furnace, and calcine it in an oxygen atmosphere, calcine it at 400°C for 240 minutes, and cool it down to room temperature naturally to obtain a nickel with low residual alkali on the surface. Cobalt-manganese ternary cathode material, the obtained material is marked as NCM-1.

[...

Embodiment 2

[0073] Step (1): take boric acid (H 3 BO 3 ) solid powder 0.0025g, it was added to 5mL ethanol and stirred until dissolving to obtain a boric acid concentration of 0.008mol / L containing boric acid ethanol solution.

[0074] Step (2): Weigh 1g of nickel-cobalt-manganese ternary cathode material LiNi 0.90 co 0.06 mn 0.04 o 2 , put the material into 5 mL ethanol solution containing boric acid, stir for 5 min, filter, and rinse the obtained precipitate with absolute ethanol three times, and then dry it in a vacuum oven at 80° C. for 2 h.

[0075] Step (3): Put the dried nickel-cobalt-manganese ternary positive electrode material into a tube furnace, calcinate in an oxygen atmosphere, calcinate at 400°C for 260min, and cool naturally to room temperature to obtain a nickel with low surface residual alkali Cobalt-manganese ternary cathode material, the obtained material is marked as NCM-2.

[0076] ICP-AES test results show that the elemental composition is LiNi 0.901 co 0.05...

Embodiment 3

[0084] Step (1): take boric acid (H 3 BO 3 ) solid powder 0.0099g, it was added to 10mL ethanol and stirred until dissolving to obtain a boric acid concentration of 0.016mol / L containing boric acid ethanol solution.

[0085] Step (2): Weigh 1g of nickel-cobalt-manganese ternary cathode material LiNi 0.90 co 0.06 mn 0.04 o 2 , the material was put into 10 mL of ethanol solution containing boric acid and stirred for 5 min, filtered, and the obtained precipitate was repeatedly washed with absolute ethanol three times, and then dried in a vacuum oven at 80° C. for 2 h.

[0086] Step (3): Put the dried nickel-cobalt-manganese ternary positive electrode material into a tube furnace, calcinate it in an oxygen atmosphere, and calcinate it at 420°C for 240 minutes, then cool it naturally to room temperature to obtain a nickel with low surface residual alkali Cobalt-manganese ternary cathode material, the obtained material is marked as NCM-3.

[0087] ICP-AES test results show that ...

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Abstract

The invention relates to a preparation method of a low-surface-residual-alkali nickel cobalt manganese ternary positive electrode material and belongs to the field of chemical energy storage batteries. The preparation method includes that boric acid or citric acid is dissolved in alcohol, so that a certain amount of free-state hydrogen ions are contained in a solution; a nickel cobalt manganese ternary positive electrode material is added then, acid-alkali neutralization reaction between H+ and material surface residual alkali is utilized, and reaction intensity is regulated through stirring time, so that the residual alkali on the surface of the material can be reduced effectively, and pH value of the surface of the material is lowered; an alcohol solution is used for flushing then, so that the surface of the material is ensured to be free of residual borate ions or citrate ions; alcohol molecules probably left on the surface are removed through a two-time calcining method, so that uniformity and stability of the material are improved.

Description

technical field [0001] The invention relates to a preparation method of a nickel-cobalt-manganese ternary positive electrode material with low surface residual alkali, belonging to the field of chemical energy storage batteries. Background technique [0002] As a new generation of green power supply devices, lithium-ion batteries are widely used in people's daily life due to their high battery specific capacity, long cycle life, stable battery voltage, no memory effect, and low environmental pollution. . Nickel-cobalt-manganese ternary cathode materials currently used in lithium-ion secondary battery materials are gradually occupying an important position in the lithium-ion battery market due to their high specific capacity, high energy density and environmental friendliness. However, in order to meet the needs of the power battery market and make the battery have a higher specific capacity and higher energy density, it is necessary to continuously increase the content of n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/525H01M4/505H01M10/0525
CPCC01G53/006C01P2002/72C01P2004/03C01P2004/04C01P2006/40H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 陈刚苏岳锋陈来卢赟包丽颖李林蔚李聪谭国强王敬陈实吴锋
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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