Regulating nucleation method during crystallization of nickel-cobalt-manganese precursor

A nickel-cobalt-manganese and precursor technology, applied in chemical instruments and methods, nickel compounds, structural parts, etc., can solve the problems such as not being widely promoted and applied, the particle size distribution cannot be controlled, and the stability of the reactor fluid is poor, etc. Achieve significant nucleation effect, control the nucleation method is simple and efficient, and reduce the effect of process control

Active Publication Date: 2019-03-05
HUNAN SHANSHAN ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned patents all mentioned the use of multi-reactor series or parallel mode to solve the problem of particle size distribution in the precursor preparation process, but the multi-reactor series-parallel mode has insufficient equipment investment, and the process switching is complicated. The stability is poor, so it has not been widely promoted and applied in industrial production.
In the Chinese patent document CN102725232A, the single-pot mode is used, and the principle of process switching is used. Although the mode of nucleation first and then growth can avoid the disadvantages of the multi-pot series-parallel production mode, it can only be produced in a single-pot interval, and the production efficiency is low. Preparation of precursors with narrow particle size distribution, the particle size distribution cannot be adjusted

Method used

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  • Regulating nucleation method during crystallization of nickel-cobalt-manganese precursor
  • Regulating nucleation method during crystallization of nickel-cobalt-manganese precursor
  • Regulating nucleation method during crystallization of nickel-cobalt-manganese precursor

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Embodiment 1

[0040] A nickel cobalt lithium manganate precursor, the molecular formula of the nickel cobalt lithium manganate precursor is Ni 0.8 co 0.1 mn 0.1 (OH) 2 , the particle size of the secondary particle aggregate of the nickel cobalt lithium manganese oxide precursor, D10=6.03 μm, D50=12.28 μm, D90=21.86 μm, particle size distribution span=1.29, and its preparation method includes the following steps:

[0041] (1) Under the protection of nitrogen, add the nickel-cobalt-manganese salt solution, ammonia solution and lye into the closed reaction kettle with bottom liquid to carry out stirring reaction; the specific operation is as follows: prepare nickel-cobalt-manganese salt solution, ammonia solution and Alkaline solution, wherein the nickel-cobalt-manganese salt solution is Ni:Co:Mn=8:1:1, a mixed solution of nickel salt, cobalt salt and manganese salt with a total metal ion concentration of 2mol / L, and the concentration of ammonia solution is 13mol / L, the lye is 10mol / L sodi...

Embodiment 2

[0052] A nickel cobalt lithium manganate precursor, the molecular formula of the nickel cobalt lithium manganate precursor is Ni 0.85 co 0.1 mn 0.05 (OH) 2 , the particle size of the secondary particle aggregate of the nickel cobalt lithium manganese oxide precursor, D10=6.36 μm, D50=12.4 μm, D90=20.68 μm, particle size distribution span=1.15, and its preparation method includes the following steps:

[0053] (1) Add nickel-cobalt-manganese salt solution, ammonia solution and lye into a closed reaction kettle equipped with bottom liquid to carry out stirring reaction; the specific operation is as follows: prepare nickel-cobalt-manganese salt solution, ammonia solution and lye, wherein, The nickel-cobalt-manganese salt solution is a mixed solution of Ni:Co:Mn=8.5:1:0.5, the total concentration of metal ions is 2mol / L, nickel salt, cobalt salt and manganese salt, the concentration of ammonia solution is 13mol / L, and the concentration of lye Before adding 10mol / L sodium hydroxi...

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Abstract

The invention discloses a regulating nucleation method during crystallization of a nickel-cobalt-manganese precursor. The method comprises the following steps: (1) adding a nickel-cobalt-manganese salt solution, an ammonia solution and an alkali solution into a closed reaction kettle containing a base liquid for a reaction; and (2) monitoring D50 and span values of particles generated in the reaction kettle; when the span value is smaller than 1, adding a nucleation feeding liquid to the reaction kettle, performing continuous stirring for the reaction, and monitoring the span value of the particles generated in the reaction kettle continuously; when the span value reaches a preset value, stopping adding the nucleation feeding liquid; and after the span value is lower than the preset value,adding the nucleation feeding liquid to the reaction kettle again, terminating the reaction until the D50 and span values of the particles generated in the reaction kettle reach a target particle size and the preset value separately, collecting materials, and then performing subsequent treatment so as to obtain the nickel-cobalt-manganese precursor, wherein the nucleation feeding liquid is a mixed solution of the nickel-cobalt-manganese salt solution and the ammonia solution, and span = (D90-D10) / D50.

Description

technical field [0001] The invention belongs to the field of lithium-ion battery materials, and in particular relates to a method for regulating nucleation during the crystallization process of a cathode material precursor. Background technique [0002] With the rapid development of digital electronic products and electric vehicles, the battery market has put forward higher requirements for the performance of lithium-ion batteries. The current commercialized lithium battery cathode materials include lithium cobaltate, lithium manganate, lithium iron phosphate, and nickel-cobalt lithium manganate. Due to the advantages of high discharge capacity and good cycle performance, lithium nickel cobalt manganese oxide has gradually increased its proportion in the application of positive electrode materials. With the increase of nickel content, the capacity per gram of lithium nickel cobalt manganese oxide will increase accordingly, so It has become the consensus of the lithium batte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/505H01M4/525H01M10/0525
CPCC01G53/006C01P2004/01C01P2004/61C01P2006/40H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 陈九华晁锋刚彭威杨志石慧谭欣欣李旭
Owner HUNAN SHANSHAN ENERGY TECH CO LTD
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