CN110459739A - A kind of positive electrode and preparation method thereof - Google Patents
A kind of positive electrode and preparation method thereof Download PDFInfo
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- CN110459739A CN110459739A CN201910572318.XA CN201910572318A CN110459739A CN 110459739 A CN110459739 A CN 110459739A CN 201910572318 A CN201910572318 A CN 201910572318A CN 110459739 A CN110459739 A CN 110459739A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/362—Composites
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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
- H01M4/485—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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- 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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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 present invention relates to a kind of positive electrodes and preparation method thereof, this material general formula is LiNi1-x-y-zCoxAlyZzO2Al2O3MaOb, wherein 0 x≤0.2 <, 0 y≤0.1 <, 0 < z≤0.05,0 < a≤2,0 b≤3 <.The nickel cobalt aluminium positive electrode of its preparation of the present invention, surface residual alkali amount is low, material surface Li2CO3Residual volume≤0.2%, Surface L iOH residual volume≤0.2%, improves the processing performance of cell size；DSC shows that exothermic temperature improves, and heat release area reduces, and improves the thermal stability of positive electrode；0.1C first charge-discharge efficiency improves about 2% up to 92.0% compared with prior art under button cell room temperature；High temperature cyclic performance is good, and 45 DEG C of 1C charge and discharge high temperature circulation 500 weeks, capacity retention ratio improves about 5% up to 90% or more compared with prior art.
Description
Technical field
The present invention relates to a kind of field of lithium ion battery, more particularly to a kind of positive electrode and preparation method thereof.
Background technique
In recent years, with the fast development of China's new-energy automobile market, the demand of power lithium-ion battery is driven substantially
Increase, and with the continuous improvement required lithium ion battery energy density, it is high as the positive electrode of its key components
Nickel chemical conversion is the inexorable trend of dynamic lithium battery Materials.Nickelicization significantly improves power battery energy density, it is meant that
The battery of equivalent weight can provide more carried charges, while realizing weight, reducing by hundred kilometers of power consumptions, be obviously improved
The course continuation mileage of new-energy automobile.Nickel cobalt aluminium positive electrode based on nickel content has been successfully applied in Tesla production
On Model S electrocar, in addition, world-famous power battery manufacturer AESC, Panasonic etc. all in volume production with nickel cobalt aluminium just
Pole material is the lithium ion battery of anode.
Although nickel cobalt aluminium positive electrode has obtained certain application, there are still some problems for the material.One side residual alkali
Height, is attached to positive electrode surface, and pulping process is easy water absorbent gel or is in jelly, it is difficult to be coated with；On the other hand since nickel contains
Amount is high, Li+、Ni2+Mixing is serious, and the thermostabilization of material is deteriorated；In addition, there is also first charge-discharge efficiency low and high temperatures for the material
The disadvantages of cycle performance is insufficient.
Summary of the invention
The object of the present invention is to provide a kind of positive electrode and preparation method thereof, the nickel cobalt aluminium positive electrode prepared,
Surface residual alkali amount is low, material surface Li2CO3Residual volume≤0.2%, Surface L iOH residual volume≤0.2%, improves cell size
Processing performance；DSC shows that exothermic temperature improves, and heat release area reduces, and improves the thermal stability of positive electrode；Button cell
0.1C first charge-discharge efficiency improves about 2% up to 92.0% compared with prior art under room temperature；High temperature cyclic performance is good,
45 DEG C of 1C charge and discharge high temperature circulation 500 weeks, capacity retention ratio improve about 5% up to 90% or more compared with prior art.
In order to achieve the above object, the present invention has following technical scheme:
A kind of positive electrode of the invention, this material general formula are LiNi1-x-y-zCoxAlyZzO2Al2O3MaOb,
Wherein 0 < x≤0.2,0 < y≤0.1,0 < z≤0.05,0 < a≤2,0 b≤3 <.
A kind of preparation method of positive electrode of the invention, includes the following steps:
(1) nickel cobalt aluminium hydroxide precursor is mixed with the Z compound of mass ratio 0.01%~1% in batch mixer
It is even；
(2) mixture that (1) obtains by described in is pre-sintered to obtain the nickel cobalt aluminum oxide of doping Z；
(3) product that (2) obtain by described in is uniformly mixed in batch mixer with lithium salts；
(4) product that (3) obtain by described in carries out once sintered under oxygen atmosphere；
(5) product that (4) obtain by described in is washed, is dehydrated, is dried；
(6) product that (5) obtain by described in and the aluminium compound and 0.01% for accounting for positive electrode mass ratio 0.01%~1%
~1% M compound is uniformly mixed in mixing machine；
(7) product that (6) obtain by described in carries out double sintering under oxygen atmosphere, and final positive material is obtained after screening
Material.
Wherein, Z is one of alkali metal Mg, Ca, Sr, Ba or a variety of, the source Mg in Z compound described in step (1)
MgO、Mg(OH)2At least one of, the source Ca CaO, Ca (OH)2、CaCO3At least one of, the source Sr SrCO3、Sr
(OH)2, at least one of SrO, the source Ba BaCO3、Ba(OH)2At least one of, it is calculated by the content of Z, doping exists
0.01~1wt%.
Wherein, pre-sintering temperature described in step (2) is 400-700 DEG C, and the pre-sintering time is 4-10h, pre-sintering atmosphere
For atmosphere or oxygen.
Wherein, lithium salts described in step (3) is at least one of lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate, lithium
Salt and oxide mixed proportion are 0.9-1.1:1 according to Li/ (Ni+Co+Al) molar ratio.
Wherein, 600-800 DEG C of sintering temperature, sintering time 8-20h, oxygen content 80-99.9% described in step (4).
Wherein, the mass ratio of washing water described in step (5) and material is 0.5-10:1, wash time 5-60min, washing
Temperature is 15-45 DEG C；Dewatering time 5-60min, moisture content of material≤10% after dehydration；Drying temperature is 80-100 DEG C, is done
Pathogenic dryness atmosphere is atmosphere or vacuum, moisture content of material≤1% after drying.
Wherein, aluminium compound described in step (6) is Al2O3、Al(OH)3At least one of, it is calculated by the content of Al,
The covering amount of aluminium is in 0.01~1wt%；M is one of B, Zr, Ti, La or a variety of in M compound described in step (6), and B comes
Source B2O3、H3BO3At least one of, the source Zr ZrO2, the source Ti TiO2, at least one of isopropyl titanate, the source La La2O3,
It is calculated by the content of M, the covering amount of M is in 0.01~1wt%.
Wherein, 300-700 DEG C of double sintering temperature described in step (7), sintering time 3-10h, oxygen content 30-
99.9%.
Wherein, the mixing machine is ballmillmixer or high-speed mixer, and the incorporation time is 0.5-5h.
Beneficial effect
(1) nickel cobalt aluminium positive electrode prepared by the present invention, surface residual alkali amount is low, material surface Li2CO3Residual volume≤
0.2%, Surface L iOH residual volume≤0.2% improves the processing performance of cell size；
(2) nickel cobalt aluminium positive electrode prepared by the present invention, DSC show that exothermic temperature improves, and heat release area reduces, and improves
The thermal stability of positive electrode；
(3) nickel cobalt aluminium positive electrode prepared by the present invention, 0.1C first charge-discharge efficiency is reachable under button cell room temperature
92.0%, about 2% is improved compared with prior art；
(4) nickel cobalt aluminium positive electrode prepared by the present invention, high temperature cyclic performance is good, 45 DEG C of high temperature circulations of 1C charge and discharge
500 weeks, capacity retention ratio improved about 5% up to 90% or more compared with prior art.
Detailed description of the invention
Fig. 1 is the DSC comparison frame line chart for the nickel cobalt aluminium positive electrode that the embodiment of the present invention 1 is prepared with comparative example 1；
Fig. 2 is 18650 battery high-temperatures 45 of the nickel cobalt aluminium positive electrode that the embodiment of the present invention 1,2 is prepared with comparative example
DEG C 1C charge and discharge cycles comparison frame line chart.
In figure, triangle is distributed as 1 curve distribution of embodiment；The circular curve distribution for being distributed as embodiment 2；It is square
The curve distribution for being distributed as comparative example 1 of shape.
Specific embodiment
For a further understanding of the present invention, the present invention is made below in conjunction with specification and specific preferred embodiment further
Description, but protection scope not thereby limiting the invention.
Embodiment 1
According to mass ratio Ba/Ni0.82Co0.15Al0.03(OH)2=0.5% ratio weighs nickel cobalt aluminium hydroxide respectively
Precursor and Ba (NO3)2, it is added in high speed mixer and mixes 0.5h, after mixing, 500 DEG C of pre-sinterings under air atmosphere
8h。
According to the ratio of molar ratio Li/ (Ni+Co+Al)=1.05, the pre-sintering product doped with Ba is weighed respectively
Ni0.82Co0.15Al0.03O and LiOH*H2O is added in high speed mixer and mixes 1h, after mixing, under 95% oxygen-enriched atmosphere
Firing product is crushed, is sieved by 780 DEG C of once sintered 12h.
Once sintered material is mixed with 25 DEG C of deionized waters according to the weight ratio of 1:2, is stirred continuously in a kettle
After 10min, slurry is transferred to centrifuge high speed dewatering 20min, dewatered material is transferred to vacuum by moisture content of material 8%
Baking oven, after 120 DEG C of dry 5h, moisture content of material 0.2%.
According to the ratio of mass ratio Al/ positive electrode=0.2%, B/ positive electrode=0.1%, Al is weighed respectively2O3、
H3BO3It is added in high speed mixer with the positive electrode after drying and mixes 0.5h, after mixing, 400 under 80% oxygen content
DEG C double sintering 4h obtains final doping 0.5%Ba, cladding 0.2%Al and coats the nickel cobalt aluminium anode of 0.1%B after screening
Material LiNi0.82Co0.15Al0.03O2。
Embodiment 2
Similar to embodiment 1, according to mass ratio Sr/Ni0.82Co0.15Al0.03(OH)2=0.1% ratio, weighs respectively
Nickel cobalt aluminium hydroxide precursor and SrCO3, it is pre-sintered after mixing, once sintered, washing, dehydration and baking step
It is same as Example 1.
According to the ratio of mass ratio Al/ positive electrode=0.1%, Ti/ positive electrode=0.2%, Al is weighed respectively
(OH)3、TiO2With the positive electrode mixing after drying, double sintering, final doping 0.1%Sr, cladding are obtained after screening
The nickel cobalt aluminium positive electrode LiNi of 0.1%Al and cladding 0.2%Ti0.82Co0.15Al0.03O2。
Comparative example 1
Similar to embodiment 1, according to the ratio of molar ratio Li/ (Ni+Co+Al)=1.05, nickel cobalt aluminium hydrogen-oxygen is weighed respectively
Compound precursor, LiOHH2High speed mixer is added in O, 1h is mixed, after mixing 780 DEG C under 95% oxygen-enriched atmosphere
Once sintered 12h, washing, dehydration, drying steps are with embodiment 1, and the material after drying is 400 DEG C directly under 80% oxygen content
Double sintering 4h obtains final nickel cobalt aluminium positive electrode LiNi after screening0.82Co0.15Al0.03O2。
The evaluation of positive electrode in embodiment 1,2 and comparative example 1
By following policies to a) residual alkali of obtained positive electrode and b) cell size processing performance c) thermal stability
It is evaluated.
A) residual alkali
The positive electrode 20g weighed is added in 100ml pure water, and after stirring at normal temperature 20min, filtering pipettes 50ml filter
Liquid is used phenolphthalein and methyl red as indicator, is titrated with the HCl of 0.2mol/L, respectively when according to different indicator discoloration
The HCl volume of consumption calculates the residual alkali amount Li of positive electrode2CO3%, LiOH%.
B) cell size processing performance
Obtained positive electrode and PVDF, CNT, SP and NMP are configured to cell size, by slurry in 25 DEG C of temperature, phase
To placing in the environment of humidity 60%, observation is primary per hour, records slurry into the jelly time.
C) thermal stability
Obtained positive electrode is fabricated to CR2016 button cell, 0.1C charge and discharge two weeks, then 0.1C charges to 4.3V；
The battery that will be filled with electricity is disassembled in glove box, takes out pole piece, is placed in dried and clean and the aluminium crucible the inside with coordinative composition of equipments,
Positive electrode is face-up, then adds 1uL electrolyte on material, covers crucible cover, and carry out differential scanning calorimeter is sealed
Test；Nitrogen atmosphere, Range of measuring temp is from room temperature to 400 DEG C, hermetical testing, 2 DEG C/min of heating rate.
Battery behavior evaluation: by following policies to the d of obtained positive electrode) first charge-discharge efficiency and e) high temperature
Cycle performance is evaluated.
D) first charge-discharge efficiency
Obtained positive electrode is fabricated to CR2016 button cell, places 1h, it, will be relative to after open-circuit voltage is stablized
The current density of anode is set as 0.1C and carries out charge and discharge, and charge cutoff voltage 4.25V after standing 10min, is discharged to cut-off electricity
2.75V is pressed, capacity at this time is evaluated as initial discharge capacity, and calculate first charge-discharge efficiency.
E) high temperature cyclic performance
Obtained positive electrode is fabricated to 18650 cylindrical batteries, carries out conventional chemical conversion after the completion of cylindrical battery preparation,
Battery after chemical conversion is subjected to loop test in 45 DEG C of insulating boxs, circulating ratio selects 1C charge and discharge to carry out, circulating battery 500
Data are recorded after secondary, and calculate capacity retention ratio.
Evaluation
The preparation condition and residual alkali of 1 particle powder of table, cell size processing performance and first charge-discharge efficiency test result
As it can be seen from table 1 compared with comparative example 1, according to the nickel cobalt aluminium anode for the embodiment 1,2 that the present invention is prepared
Material, residual alkali significantly reduce, and cell size extends at the jelly time, and processing performance is obviously improved, while first charge-discharge efficiency
Improve about 2%.
From attached drawing 1 as can be seen that compared with comparative example 1, according to the nickel cobalt aluminium anode for the embodiment 1 that the present invention is prepared
Material, DSC exothermic temperature improve, and heat release area reduces, and improve the thermal stability of positive electrode.
From attached drawing 2 as can be seen that compared with comparative example 1, the nickel cobalt aluminium for the embodiment 1,2 being prepared according to the present invention is just
Pole material, 500 weeks circulation conservation rates are increased to 92% or so from 87% or so.
It is compared by embodiment and comparative example, illustrates to increase the residual alkali for being pre-sintered and reducing positive electrode, improve battery
The processing performance of slurry；Doped alkali metal can reduce Li+、Ni2+Mixing improves the thermal stability of positive electrode；Surface carries out double
Cladding, cladding B or Ti make surface form fast-ionic conductor, improve lithium ion diffusion rate, to improve first charge-discharge effect
Rate, while Al is coated, the side reaction between positive electrode and electrolyte is further suppressed, the high temperature circulation of positive electrode is improved
Energy.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the invention is not limited to described above, that is, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow
It could implement.It should be clear to those skilled in the art, any improvement in the present invention, to each raw material of product of the present invention
Equivalence replacement and addition, the selection of concrete mode of auxiliary element etc., all fall within protection scope of the present invention and the open scope
Within.
Claims (10)
1. a kind of positive electrode, it is characterised in that: this material general formula is LiNi1-x-y-zCoxAlyZzO2·Al2O3·MaOb, wherein 0
< x≤0.2,0 < y≤0.1,0 < z≤0.05,0 < a≤2,0 b≤3 <.
2. a kind of preparation method of positive electrode as described in claim 1, characterized by the following steps:
(1) nickel cobalt aluminium hydroxide precursor is uniformly mixed in batch mixer with the Z compound of mass ratio 0.01%~1%；
(2) mixture that (1) obtains by described in is pre-sintered to obtain the nickel cobalt aluminum oxide of doping Z；
(3) product that (2) obtain by described in is uniformly mixed in batch mixer with lithium salts；
(4) product that (3) obtain by described in carries out once sintered under oxygen atmosphere；
(5) product that (4) obtain by described in is washed, is dehydrated, is dried；
(6) product that (5) obtain by described in account for positive electrode mass ratio 0.01%~1% aluminium compound and 0.01%~
1% M compound is uniformly mixed in mixing machine；
(7) product that (6) obtain by described in carries out double sintering under oxygen atmosphere, and final positive electrode is obtained after screening.
3. the preparation method as described in right 2, it is characterised in that: in Z compound described in step (1) Z be alkali metal Mg, Ca,
One of Sr, Ba or a variety of, the source Mg MgO, Mg (OH)2At least one of, the source Ca CaO, Ca (OH)2、CaCO3In
At least one, the source Sr SrCO3、Sr(OH)2, at least one of SrO, the source Ba BaCO3、Ba(OH)2At least one of,
It is calculated by the content of Z, doping is in 0.01~1wt%.
4. the preparation method as described in right 2, it is characterised in that: pre-sintering temperature described in step (2) is 400-700 DEG C, pre-burning
The knot time is 4-10h, and pre-sintering atmosphere is atmosphere or oxygen.
5. the preparation method as described in right 2, it is characterised in that: lithium salts described in step (3) is lithium carbonate, lithium hydroxide, acetic acid
At least one of lithium, lithium nitrate, lithium salts and oxide mixed proportion are 0.9-1.1:1 according to Li/ (Ni+Co+Al) molar ratio.
6. the preparation method as described in right 2, it is characterised in that: 600-800 DEG C of sintering temperature described in step (4), sintering time
8-20h, oxygen content 80-99.9%.
7. the preparation method as described in right 2, it is characterised in that: the mass ratio of washing water described in step (5) and material is 0.5-10:
1, wash time 5-60min, wash temperature are 15-45 DEG C；Dewatering time 5-60min, moisture content of material after dehydration≤
10%；Drying temperature is 80-100 DEG C, and dry atmosphere is atmosphere or vacuum, moisture content of material≤1% after drying.
8. the preparation method as described in right 2, it is characterised in that: aluminium compound described in step (6) is Al2O3、Al(OH)3In
At least one is calculated by the content of Al, and the covering amount of aluminium is in 0.01~1wt%；In M compound described in step (6) M be B,
One of Zr, Ti, La or a variety of, the source B B2O3、H3BO3At least one of, the source Zr ZrO2, the source Ti TiO2, isopropanol
At least one of titanium, the source La La2O3, calculated by the content of M, the covering amount of M is in 0.01~1wt%.
9. the preparation method as described in right 2, it is characterised in that: 300-700 DEG C of double sintering temperature described in step (7), sintering
Time 3-10h, oxygen content 30-99.9%.
10. the preparation method as described in right 2, it is characterised in that the mixing machine be ballmillmixer or high-speed mixer, it is described
Incorporation time is 0.5-5h.
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| CN111952590A (en) * | 2020-07-08 | 2020-11-17 | 河南科隆新能源股份有限公司 | Lithium ion battery positive electrode material for improving safety and cycle performance and preparation method thereof |
| CN113651373A (en) * | 2021-10-19 | 2021-11-16 | 河南科隆新能源股份有限公司 | Anode material with uniform porous structure and preparation method thereof |
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