CN109346705A - A kind of preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure - Google Patents
A kind of preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure Download PDFInfo
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- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
A kind of preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure, belongs to anode material for lithium-ion batteries technical field.It is characterized in that first preparing presoma powder, then it is sintered presoma powder and lithium source to obtain nickel cobalt lithium aluminate cathode material, wherein presoma powder is made of core and shell two parts, and core is matrix, matrix chemical formula are as follows: Ni1‑x‑yCoxAly(OH)2；The partial size of described matrix is 1~20 μm；Shell is clad, clad chemical formula are as follows: (Ni1‑h‑ kCohMnk)1‑zMz(OH)2, wherein M is selected from one of Ti, Zr, Al, Mg, Mo, Cr, V or a variety of；Wherein h>0, k>0,1>1-h-k>0 and 0<z<0.5.The cyclical stability and high rate performance of positive electrode can be improved, and simple process, operating aspect are low in cost with the content of flexible modulation surface coating layer thickness and each element in the present invention.This method and existing industrially prepared positive forerunner's body technology are fully compatible, are effectively reduced the cost as required for modified material.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical fields, and in particular to a kind of nickel cobalt lithium aluminate of core-shell structure
The preparation method of positive electrode.
Background technique
Lithium ion battery has been widely used in various electronic equipments, is made in electric car and energy storage device
With also increasing.The service life of battery is people's concern always, and the service life depends on the positive electrode performance of battery, because
This, the performance of positive electrode is particularly important.
In numerous positive electrodes, ternary material LiNi1-x-yCoxAlyO2(NCA) with higher specific capacity, good electricity
During son and ionic conductivity and the reversible deintercalation of lithium the advantages that good structural stability, the deep favor by researcher.So
And the material, due to the fracture of positive electrode particle, dusting etc., leads to battery capacity rapid decay during charge and discharge cycles, limit
The promotion and application of the material are made.
Researchers come up with various methods around the problem of " the circulation conservation rate for how improving NCA ", comprising: surface
Modification, element doping, the synthesis of full concentration gradient etc..Research has shown that surface modification can effectively improve the cycle performance of positive electrode,
Generally, it is considered that positive electrode and electrolyte can be isolated in decorative layer, surface side reaction is avoided, meanwhile, decorative layer energy surface of stability layer
Structure hinders surface phase transformation.More crucial is a little that decorative layer must have preferable mechanical property, can prevent positive electrode particle
Fracture, otherwise, a large amount of new surfaces for being broken generation will make decorative layer lose meaning.So decorative layer should at least have following two
A performance: 1. under different voltage, has high mechanical stability, prevents positive electrode particle from cracking；2. high lithium ion conductance
Rate and electronic conductivity, are conducive to lithium ion and electronics conducts.Using performance of both this as foundation, can directly filter out comprehensive
The excellent modification composition of layer of energy, and this ingredient is coated on positive electrode particle, (element will be modified relative to traditional trial-and-error method
Oxide or hydroxide deposition are in the surface of positive electrode particle (or positive presoma), by high temperature sintering, in positive electrode particle table
Face forms one layer of decorative layer, and then assembled battery detects chemical property.The method process is complicated, heavy workload), it mentions significantly
High optimization efficiency.
The present invention has found a kind of modification layer material --- Li (Ni1-h-kCohMnk)1-zMzO2, have both high mechanics and stablize
Property and higher ion and electronic conductivity the two advantages.Therefore, material may be improved by which being coated on the surface NCA
Cycle performance.
Summary of the invention
In consideration of it, the present invention provides a kind of methods of clad for preparing controllable ingredient in positive electrode particle surface.
This method can control the ingredient of clad and the thickness of clad.
A kind of preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure, it is characterised in that first prepare precursor
Body, then be sintered presoma powder and lithium source to obtain nickel cobalt lithium aluminate cathode material, wherein presoma powder is by core and two, shell
It is grouped as, core is matrix, matrix chemical formula are as follows: Ni1-x-yCoxAly(OH)2, wherein x > 0, y > 0,1 > 1-x-y > 0；Described matrix
Partial size be 1~20 μm；Shell is clad, clad chemical formula are as follows: (Ni1-h-kCohMnk)1-zMz(OH)2, wherein M is selected from
One of Ti, Zr, Al, Mg, Mo, Cr, V or a variety of；H>0, k>0,1>1-h-k>0 and 0<z<0.5.
Further, the presoma powder is that clad is deposited on blapharoplast surface using coprecipitation, base
Body and clad the mass ratio of the material are (3~30): 1.
Further, the presoma powder is the suspension for first preparing blapharoplast, the suspension of blapharoplast be with
The suspension that the methods of coprecipitation, sol-gal process obtain, or the blapharoplast prepared is dispersed in water to obtain suspended
Liquid；Clad mixed solution is prepared again, clad mixed solution and precipitating reagent, complexing agent are added in suspension, with altogether
Coprecipitation mode is coated on blapharoplast surface.
Further, prepared clad solution is according to clad (Ni1-h-kCohMnk)1-zMz(OH)2Chemistry meter
Ratio is measured, soluble nickel salt, soluble cobalt, soluble manganese salt, soluble M salt are dissolved in water, obtain clad mixed solution；Packet
The total concentration of coating mixed solution intermediate ion is 0.01~2.00mol/L.
Further, the soluble M salt is one of sulfate, nitrate, chlorate and acetate or a variety of.
Further, precipitating reagent, complexing agent and clad mixed solution are added drop-wise in blapharoplast suspension, speed is added dropwise
Degree is 0.01~9.99ml/min, makes (Ni1-h-kCohMnk)1-zMz(OH)2It is deposited on blapharoplast surface, as shown in Figure 1；Control
The pH value of system reaction is 9~14；Precipitating reagent is selected from NaOH, Na2CO3One of or it is a variety of, complexing agent be selected from ammonium hydroxide, citric acid
With one of glycine or a variety of.
Further, mixed suspension is aged, is separated by solid-liquid separation, cleaned, dried, obtain Ni1-x-yCoxAly
(OH)2-(Ni1-h-kCohMnk)1-zMz(OH)2Powder.
Further, the time of mixed suspension ageing be 1~temperature for 24 hours, dry is 50~150 DEG C
Further, by the powder after drying according to the element in core and shell, with Li:(Ni+Co+Al)=(1~1.2): 1
And Li:(Ni+Co+Mn+M)=(1~1.2): 1 stoichiometric ratio calculates lithium source quality；By lithium source and preparation ground presoma
Powder is uniformly mixed；Lithium source is LiOH and Li2CO3One of or it is a variety of.
Further, presoma powder is kept the temperature into removal in 2~10 hours at 300~600 DEG C and combines water；It is warming up to 700~
950 DEG C are sintered 6~20 hours.
The present invention can regulate and control the performance of surface coating layer, improve the cyclical stability of positive electrode, and simple process, operation
Aspect, the cost of material is low, fully compatible with existing industrially prepared nickel cobalt aluminium anode forerunner's body technology, relatively low cladding
Modified cost.
Detailed description of the invention
Fig. 1,1 covered effect schematic diagram of the embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any substitution done on the essence and scope of the present invention being defined by the claims, repairs
Change, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
The present invention can also be understood completely in description.
Embodiment 1
Prepare LiNi0.8Co0.15Al0.05O2~Li (Ni0.4Co0.2Mn0.4)0.8Ti0.2O2Core-shell structured cathode material, matrix
It is 10:1 with clad the mass ratio of the material.
Preparation method is specific as follows:
(1) according to cladding composition of layer, solution, concentration 0.1mol/L, wherein NiSO are prepared4·6H2O is 0.032 mol/
L, MnSO4·H2O is 0.032mol/L, CoSO4·7H2O is 0.016mol/L, Ti (SO4)2For 0.02mol/L.Above-mentioned salt is molten
It in deionized water, and stirs evenly, H is added dropwise2SO4, its pH value is adjusted to 2 or so and obtains mixing salt solution；
(2) dispersion liquid for configuring blapharoplast, by presoma matrix Ni0.8Co0.15Al0.05(OH)2Deionization is added in particle
In water, every liter of 0.2mol containing blapharoplast.PH value is adjusted to 12 or so, then places it on magnetic stirring apparatus and is stirred continuously,
Mixing speed is 900rpm, forms uniform suspension；
(3) by the measurement mixing salt solution of solute molar ratio 10 in blapharoplast in suspension and clad solution, configuration
Three is instilled the dispersion liquid of blapharoplast, rate of addition by the ammonium hydroxide of 0.5mol/L and the NaOH solution of 1mol/L simultaneously, at the same speed
For 1ml/min；
(4) after the reaction was completed to completion of dropwise addition, ripening is carried out for 24 hours to it, after precipitating completely, by precipitating spend from
Sub- water cleaning filters out precipitating, being placed on 80 DEG C of drying box is completely dried it when the pH value of suspension is 10；
(5) then by the precipitating and LiOHH after drying2O is uniformly mixed with the mass ratio of the material 1:1.05.By the mixture
It is placed in 500 DEG C of environment and keeps the temperature removal in 4 hours in conjunction with water, being then sintered to obtain for 10 hours at 800 DEG C has special component packet
The positive electrode of coating.
Embodiment 2
Prepare LiNi0.8Co0.15Al0.05O2~Li (Ni0.4Co0.2Mn0.4)0.9Zr0.1O2Core-shell structured cathode material, matrix
It is 10:1 with clad the mass ratio of the material.
Preparation method is specific as follows:
(1) according to cladding composition of layer, solution, concentration 0.1mol/L, wherein NiSO are prepared4·6H2O is 0.036 mol/
L, MnSO4·H2O is 0.036mol/L, CoSO4·7H2O is 0.018mol/L, Zr (SO4)2For 0.01mol/L.Above-mentioned salt is molten
In deionized water, and stir evenly mixing salt solution；
(2) dispersion liquid for configuring blapharoplast, by presoma matrix Ni0.8Co0.15Al0.05(OH)2Deionization is added in particle
In water, every liter of 0.2mol containing blapharoplast.PH value is adjusted to 12 or so, then places it on magnetic stirring apparatus and is stirred continuously,
Mixing speed is 900rpm, forms uniform suspension；
(3) by the measurement mixing salt solution of solute molar ratio 10 in blapharoplast in suspension and clad solution, configuration
Three is instilled the dispersion liquid of blapharoplast, rate of addition by the ammonium hydroxide of 0.5mol/L and the NaOH solution of 1mol/L simultaneously, at the same speed
For 1ml/min；
(4) after the reaction was completed to completion of dropwise addition, ripening is carried out for 24 hours to it, after precipitating completely, by precipitating spend from
Sub- water cleaning filters out precipitating, being placed on 80 DEG C of drying box is completely dried it when the pH value of suspension is 10；
(5) then by the precipitating and LiOHH after drying2O is uniformly mixed with the mass ratio of the material 1:1.05.By the mixture
It is placed in 500 DEG C of environment and keeps the temperature removal in 4 hours in conjunction with water, being then sintered to obtain for 10 hours at 800 DEG C has special component packet
The positive electrode of coating.
Claims (10)
1. a kind of preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure, it is characterised in that presoma powder is first prepared,
It is sintered presoma powder and lithium source to obtain nickel cobalt lithium aluminate cathode material again, wherein presoma powder is by core and shell two parts group
At core is matrix, matrix chemical formula are as follows: Ni1-x-yCoxAly(OH)2, wherein x > 0, y > 0,1 > 1-x-y > 0；The grain of described matrix
Diameter is 1~20 μm；Shell is clad, and clad chemical formula is (Ni1-h-kCohMnk)1-zMz(OH)2, wherein M be selected from Ti, Zr,
One of Al, Mg, Mo, Cr, V or a variety of；Wherein h>0, k>0,1>1-h-k>0 and 0<z<0.5.
2. the preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 1, which is characterized in that described
Presoma powder is that clad is deposited on blapharoplast surface using coprecipitation, and matrix is with clad the mass ratio of the material
(3~30): 1.
3. the preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 1 or 2, feature exist
In the presoma powder is the suspension for first preparing blapharoplast, and the suspension of blapharoplast is solidifying with coprecipitation, colloidal sol
The suspension that glue method method obtains, or be dispersed in water the blapharoplast prepared to obtain suspension；It is mixed that clad is prepared again
Solution is closed, clad mixed solution and precipitating reagent, complexing agent are added in suspension, matrix is coated in a manner of co-precipitation
Particle surface.
4. the preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 3, which is characterized in that institute
The clad solution of preparation is according to clad (Ni1-h-kCohMnk)1-zMz(OH)2Stoichiometric ratio, by soluble nickel salt, can
Dissolubility cobalt salt, soluble manganese salt, soluble M salt are dissolved in water, obtain clad mixed solution；Clad mixed solution intermediate ion
Total concentration is 0.01~2.00mol/L.
5. the preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 4, which is characterized in that can
Dissolubility M salt is one of sulfate, nitrate, chlorate and acetate or a variety of.
6. the preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 3, which is characterized in that will
Precipitating reagent, complexing agent and clad mixed solution are added drop-wise in blapharoplast suspension, and rate of addition is 0.01~9.99ml/
Min makes (Ni1-h-kCohMnk)1-zMz(OH)2It is deposited on blapharoplast surface, the pH value for controlling reaction is 9~14；Precipitating reagent
Selected from NaOH, Na2CO3One of or it is a variety of, complexing agent is selected from one of ammonium hydroxide, citric acid and glycine or a variety of.
7. the preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 6, which is characterized in that will
Mixed suspension is aged, is separated by solid-liquid separation, is cleaned, is dried, and Ni is obtained1-x-yCoxAly(OH)2-(Ni1-x-yCoxMny)1- zMz(OH)2Powder.
8. the preparation method of the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 7, which is characterized in that old
The time of change is 1~for 24 hours, dry temperature is 50~150 DEG C.
9. the nickel cobalt lithium aluminate cathode material of core-shell structure according to claim 1, which is characterized in that according in core and shell
Element, with Li:(Ni+Co+Al)=(1~1.2): 1 and Li:(Ni+Co+Mn+M)=(1~1.2): 1 stoichiometry
Than calculating lithium source amount；Lithium source is uniformly mixed with the presoma powder of preparation；Lithium source is LiOH and Li2CO3One of or it is more
Kind.
10. the nickel cobalt lithium aluminate cathode material preparation method of core-shell structure according to claim 1, which is characterized in that institute
Stating sintering is that presoma powder is kept the temperature removal in 2~10 hours at 300~600 DEG C to combine water；It is warming up to 700~950 DEG C of sintering 6
~20 hours.
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| CN111799457A (en) * | 2020-07-30 | 2020-10-20 | 广东邦普循环科技有限公司 | Pre-lithiation-treated lithium ion positive electrode material and preparation method and application thereof |
| CN112047395A (en) * | 2020-09-10 | 2020-12-08 | 江西智锂科技有限公司 | Method for preparing lithium-nickel-cobalt-aluminum composite oxide lithium battery anode material with core |
| CN113258041A (en) * | 2021-03-31 | 2021-08-13 | 上海空间电源研究所 | Lithium ion battery anode material with layered structure, preparation method and lithium ion battery |
| CN113437265A (en) * | 2020-03-23 | 2021-09-24 | 飞翼新能源公司 | Positive active material for lithium battery and preparation method thereof |
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Application publication date: 20190215 |