CN107195863A - The preparation method of nickel-cobalt-manganternary ternary anode material - Google Patents
The preparation method of nickel-cobalt-manganternary ternary anode material Download PDFInfo
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- CN107195863A CN107195863A CN201710423000.6A CN201710423000A CN107195863A CN 107195863 A CN107195863 A CN 107195863A CN 201710423000 A CN201710423000 A CN 201710423000A CN 107195863 A CN107195863 A CN 107195863A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses the preparation method of nickel-cobalt-manganternary ternary anode material, including following preparation process:Step A, obtains particle, Control granularity D50=3~8 μm are standby by lithium source sieving;Step B, the lithium source particle that step A is obtained, ternary precursor LiNi0.6Co0.2Mn0.2(OH)3And additive carries out liquid phase mixing, wet ball grinding and drying process successively, mixed powder is obtained;Step C, the mixed powder that step B is obtained is calcined 5~15h under 500~850 DEG C of temperature conditionss;Step D, the imitation frosted glass that step C is obtained is mixed with covering, and mixed material is obtained through ball-milling treatment;Step E, the mixed material that step D is obtained carries out 10~20h of after baking at 750~950 DEG C, obtains nickel-cobalt-manganternary ternary anode material.Selected, adulterated through wet-mixing by the raw material improved to additive and covering, leading to appropriate oxygen and nickel-cobalt-manganternary ternary anode material is prepared into using after baking technique, while filling secondary rate with higher capacitance and head, there is higher service life cycle.
Description
Technical field
The present invention relates to a kind of electrode material, and in particular to the preparation method of nickel-cobalt-manganternary ternary anode material.
Background technology
Lithium ion battery is widely used in the electronic product such as notebook computer and mobile phone, and by
As the energy storage equipment application of main flow to tackle current CO2 emission excess and energy supply on electric automobile
Reduce.Research main at present is concentrated on the positive electrode with more good safety and high-energy-density, and cobalt acid lithium, is made
For most representative and commercialized positive electrode because its cost is high, nowadays high toxicity and relatively low capacity are difficult to adapt to work as
The demand of modern battery.Sight is concentrated on stratiform LiNi by many researchers1-x-yCoxMnyO2(x+y < 1) positive electrode, it has
There are higher specific capacity and relatively low cost.Particularly, rich nickel dam shape LiNi1-x-yCoxMnyO2(1-x-y > 0.5) positive electrode,
Such as LiNi0.6Co0.2Mn0.2O2Receive more and more attention.However, nickel-rich positive pole material typically exhibits quick appearance
Amount decay, because easy catalytic electrolysis liquid decomposes generation gas in cation mixing and cyclic process.In addition, in high voltage
Ni4+It is readily dissolved into electrolyte, these all limit further applying for nickel-rich positive pole material.
The content of the invention
The technical problems to be solved by the invention be in the prior art nickel-cobalt-manganternary ternary anode material due to cation mixing
And easy catalytic electrolysis liquid decomposes and produces gas and cause that the capacitance of positive electrode is smaller, the life-span is shorter, mesh in cyclic process
The preparation method for being to provide nickel-cobalt-manganternary ternary anode material, by improve the raw material of additive and covering is selected, warp
Wet-mixing doping, logical appropriate oxygen are simultaneously prepared into nickel-cobalt-manganternary ternary anode material using after baking technique, with higher
While capacitance and head fill secondary rate, there is higher service life cycle.
The present invention is achieved through the following technical solutions:
The preparation method of nickel-cobalt-manganternary ternary anode material, including following preparation process:
Step A, pretreatment of raw material:Lithium source is obtained into particle through the sieving of 200~400 mesh, Control granularity D50=3~8 μm are standby
With;
Step B, pre-doping processing:Lithium source particle, the ternary precursor LiNi that the step A is obtained0.6Co0.2Mn0.2
(OH)3And additive carries out liquid phase mixing, wet ball grinding and drying process successively, mixed powder is obtained;
Step C, it is once sintered:The step B mixed powders obtained are calcined 5 under 500~850 DEG C of temperature conditionss~
15h;
Step D, pre-coated processing:The step C imitation frosted glass obtained is mixed with covering, through ball-milling treatment
Obtain mixed material;
Step E, double sintering:By the step D obtain mixed material 750~950 DEG C carry out after bakings 10~
20h, obtains nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2。
Preferably, the lithium source is lithium carbonate or lithium hydroxide.
Preferably, lithium source and the mol ratio of ternary precursor 1.02~1.20.
Preferably, described additive is Mg (NO3)2、Al(NO3)3And NH4One or more mixtures in F;And addition
The addition of agent is the 0.1%~10.0% of theoretical product quality.
Preferably, the medium that liquid phase mixing and ball milling are used in the step B is distilled water or absolute ethyl alcohol, Ball-milling Time
For 1~4h.
Preferably, in the step C, purity oxygen is continually fed into roasting process, oxygen flow is 10~30L/min.
Preferably, in the step D, using 1~4h of dry ball milling, Control granularity D50=9~14um.
Preferably, the covering is Al2O3、Li3PO4, one or more mixtures in silicic acid and aluminium isopropoxide;Its
The addition of covering is the 0.1%~10.0% of theoretical product quality.
The present invention compared with prior art, has the following advantages and advantages:
Nickel-cobalt-manganternary ternary anode material is due to easy catalytic electrolysis liquid in cation mixing and cyclic process in the prior art
Decompose and produce gas and cause that the capacitance of positive electrode is smaller, the life-span is shorter.The nickel-cobalt-manganese ternary positive pole material that the present invention is provided
The preparation method of material, is selected by the raw material improved to additive and covering, is adulterated through wet-mixing, led to appropriate oxygen and adopt
Be prepared into nickel-cobalt-manganternary ternary anode material with after baking technique, while filling time rate with higher capacitance and head, have compared with
High service life cycle.And preparation section is simple, easy industrialization and with higher capacity, 0.1C capacity >
190mAh/g。
Brief description of the drawings
Accompanying drawing described herein is used for providing further understanding the embodiment of the present invention, constitutes one of the application
Point, do not constitute the restriction to the embodiment of the present invention.In the accompanying drawings:
Fig. 1 is the preparation flow structural representation of nickel-cobalt-manganternary ternary anode material of the present invention.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, with reference to embodiment and accompanying drawing, to this
Invention is described in further detail, and exemplary embodiment and its explanation of the invention is only used for explaining the present invention, does not make
For limitation of the invention.
Embodiment 1
The preparation technology flow for the nickel-cobalt-manganternary ternary anode material that the present invention is provided is as shown in figure 1, concrete operation step is:
Step A, pretreatment of raw material:Lithium hydroxide raw material is obtained into particle, the μ of Control granularity D50=3~8 through the sieving of 200 mesh
M is standby;
Step B, pre-doping processing:By the lithium hydroxide feed particles of step A acquisitions, ternary precursor
LiNi0.6Co0.2Mn0.2(OH)3And Mg (NO3)2Add using high-speed mixer progress liquid phase mixing in distilled water, it is to be mixed uniform
Liquid phase mixture is carried out afterwards directly to carry out ball milling 1h, ball milling is finished in the dry machine of disk, the drying process under 90 DEG C of temperature conditionss,
Obtain mixed powder;Wherein Li and (Ni+Co+Mn) mol ratio are 1.1:1, Mg (NO3)2Addition quality be theoretical product matter
The 0.1% of amount;
Step C, it is once sintered:The mixed powder roller kilns progress that the step B is obtained is once sintered, with 10 DEG C/min
500 DEG C of insulation 10h are warming up to, oxygen are continually fed into sintering process, uninterrupted is 10L/min;
Step D, pre-coated processing:The imitation frosted glass and Al that the step C is obtained2O3Powder is uniformly mixed, through ball milling 1h
Processing obtains mixed material;Wherein Al2O3Addition quality be the 0.45% of theoretical product quality, the μ of Control granularity D50=9~14
m;
Step E, double sintering:The mixed material that the step D is obtained is warming up to 850 DEG C in roller kilns with 10 DEG C/min
It is incubated 12h;Double sintering products obtained therefrom is sieved and except iron, the magnetisable material content that control removes after iron in material is less than
60ppb, except the material after iron carries out batch mixed, sieving and packaging and storage, final be made obtains nickel-cobalt-manganternary ternary anode material
LiNi0.6Co0.2Mn0.2O2Finished product.
Embodiment 2
The preparation technology flow for the nickel-cobalt-manganternary ternary anode material that the present invention is provided is as shown in figure 1, concrete operation step is:
Step A, pretreatment of raw material:Lithium hydroxide raw material is obtained into particle, the μ of Control granularity D50=3~8 through the sieving of 200 mesh
M is standby;
Step B, pre-doping processing:By the lithium hydroxide feed particles of step A acquisitions, ternary precursor
LiNi0.6Co0.2Mn0.2(OH)3、Al(NO3)3And NH4F is added in distilled water using high-speed mixer progress liquid phase mixing, waits to mix
Liquid phase mixture is subjected to directly progress ball milling 3h after closing uniformly, ball milling is finished in the dry machine of disk, done under 120 DEG C of temperature conditionss
Dry processing, obtains mixed powder;Wherein Li and (Ni+Co+Mn) mol ratio are 1.12:1, Al (NO3)3Addition quality for reason
By 0.6%, NH of product quality4F addition quality is the 0.4% of theoretical product quality;
Step C, it is once sintered:The mixed powder roller kilns progress that the step B is obtained is once sintered, with 10 DEG C/min
600 DEG C of insulation 8h are warming up to, oxygen are continually fed into sintering process, uninterrupted is 20L/min;
Step D, pre-coated processing:The step C imitation frosted glass obtained is uniformly mixed with isopropanol aluminium powder powder, passed through
Ball milling 2h processing obtains mixed material;Wherein the addition quality of isopropanol aluminium powder is the 0.65% of theoretical product quality, controls grain
Spend D50=9~14 μm;
Step E, double sintering:The mixed material that the step D is obtained is warming up to 950 DEG C in roller kilns with 10 DEG C/min
It is incubated 12h;Double sintering products obtained therefrom is sieved and except iron, the magnetisable material content that control removes after iron in material is less than
60ppb, except the material after iron carries out batch mixed, sieving and packaging and storage, final be made obtains nickel-cobalt-manganternary ternary anode material
LiNi0.6Co0.2Mn0.2O2Finished product.
Embodiment 3
Step A, pretreatment of raw material:Lithium hydroxide raw material is obtained into particle, the μ of Control granularity D50=3~8 through the sieving of 200 mesh
M is standby;
Step B, pre-doping processing:By the lithium hydroxide feed particles of step A acquisitions, ternary precursor
LiNi0.6Co0.2Mn0.2(OH)3With Al (NO3)3Add using high-speed mixer progress liquid phase mixing in absolute ethyl alcohol, it is to be mixed equal
Liquid phase mixture is subjected to directly progress ball milling 4h after even, ball milling finished in the dry machine of disk, under 100 DEG C of temperature conditionss at drying
Reason, obtains mixed powder;Wherein Li and (Ni+Co+Mn) mol ratio are 1.20:1, Al (NO3)3Addition quality produced to be theoretical
The 0.8% of quality;
Step C, it is once sintered:The mixed powder roller kilns progress that the step B is obtained is once sintered, with 10 DEG C/min
850 DEG C of insulation 5h are warming up to, oxygen are continually fed into sintering process, uninterrupted is 25L/min;
Step D, pre-coated processing:The imitation frosted glass and Li that the step C is obtained3PO4Uniformly mixed with silicic acid material,
Handled through ball milling 4h and obtain mixed material;Wherein Li3PO4Addition quality be the 0.75% of theoretical product quality, the addition of silicic acid
Quality is the 0.25% of theoretical product quality, Control granularity D50=9~14 μm;
Step E, double sintering:The mixed material that the step D is obtained is warming up to 750 DEG C in roller kilns with 10 DEG C/min
It is incubated 20h;Double sintering products obtained therefrom is sieved and except iron, the magnetisable material content that control removes after iron in material is less than
60ppb, except the material after iron carries out batch mixed, sieving and packaging and storage, final be made obtains nickel-cobalt-manganternary ternary anode material
LiNi0.6Co0.2Mn0.2O2Finished product
Comparative example 1
Nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2Preparation method it is same as Example 2, difference is:Step
Rapid B, in pre-doping processing, lithium hydroxide feed particles that step A is obtained, ternary precursor LiNi0.6Co0.2Mn0.2(OH)3、
Al(NO3)3And NH4F adds high-speed mixer and carries out dry-mixed, ball milling, no drying steps.
Comparative example 2
Nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2Preparation method it is same as Example 2, difference is:Step
Additive uses Al in rapid B2O3。
Comparative example 3
Nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2Preparation method it is same as Example 2, difference is:Step
In rapid C, carry out in air atmosphere once sintered.
Comparative example 4
Nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2Preparation method it is same as Example 2, difference is:Step
In rapid C, the flow for being continually fed into oxygen is 60L/min.
Comparative example 5
Nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2Preparation method it is same as Example 2, difference is:Nothing
Step D and step E.
Performance test:
By obtained finished product, acetylene black and PVDF with mass ratio 90:4:6 are well mixed, and are dispersed in appropriate NMP and obtain
Uniform anode sizing agent, is coated onto on aluminium foil, the vacuum bakeout 12h at 80 DEG C, through roll-in, and positive plate is made.With lithium piece
For negative pole, obtained positive plate is positive pole, using 1mol/L LiPF6/ (EC+DMC+EMC) (mass ratio 1: 1: 1) mixed solutions as
Electrolyte, is assembled into CR2032 type button cells in glove box, and battery passes through 10h standing, is tested at blue electric (CT2001A)
0.1C charge-discharge tests are carried out in system (charging and discharging currents density is 16mA/g, and charging/discharging voltage scope is 3.0~4.4V)
Lithium battery standard cycle life test is provided with according to IEC.
IEC regulation lithium battery standard cycle life tests are:
Battery is put to 3.0V/ branch with 0.2C, and 1C constant-current constant-voltage chargings to 4.2V, the μ A of cut-off current 50 are shelved 1 hour
Afterwards, then with 0.2C 3.0V (a circulation) iterative cycles are discharged to 500 times.
Test result is as shown in table 1:
The performance test results of sample prepared by the embodiment 1~3 of table 1 and comparative example 1~5
Above-described embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc. all should be included
Within protection scope of the present invention.
Claims (8)
1. the preparation method of nickel-cobalt-manganternary ternary anode material, it is characterised in that including following preparation process:
Step A, pretreatment of raw material:Lithium source is obtained into particle through the sieving of 200~400 mesh, Control granularity D50=3~8 μm are standby;
Step B, pre-doping processing:Lithium source particle, the ternary precursor LiNi that the step A is obtained0.6Co0.2Mn0.2(OH)3And
Additive carries out liquid phase mixing, wet ball grinding and drying process successively, obtains mixed powder;
Step C, it is once sintered:The step B mixed powders obtained are calcined 5~15h under 500~850 DEG C of temperature conditionss;
Step D, pre-coated processing:The step C imitation frosted glass obtained is mixed with covering, obtained through ball-milling treatment
Mixed material;
Step E, double sintering:The mixed material that the step D is obtained carries out 10~20h of after baking at 750~950 DEG C,
Obtain nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2。
2. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that the lithium source is carbon
Sour lithium or lithium hydroxide.
3. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that before lithium source and ternary
Drive the mol ratio 1.02~1.20 of body.
4. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that described additive
For Mg (NO3)2、Al(NO3)3And NH4One or more mixtures in F;And the addition of additive is theoretical product quality
0.1%~10.0%.
5. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that in the step B
The medium that liquid phase is mixed and ball milling is used is distilled water or absolute ethyl alcohol, and Ball-milling Time is 1~4h.
6. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that in the step C,
Purity oxygen is continually fed into roasting process, oxygen flow is 10~30L/min.
7. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that in the step D,
Using 1~4h of dry ball milling, Control granularity D50=9~14um.
8. the preparation method of nickel-cobalt-manganternary ternary anode material according to claim 1, it is characterised in that the covering is
Al2O3、Li3PO4, one or more mixtures in silicic acid and aluminium isopropoxide;The addition of its covering is theoretical product quality
0.1%~10.0%.
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