CN108448088A - A kind of modified tertiary cathode material and preparation method thereof, lithium ion battery - Google Patents
A kind of modified tertiary cathode material and preparation method thereof, lithium ion battery Download PDFInfo
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- 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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- 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
- H01M4/48—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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- 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 modified tertiary cathode material and preparation method thereof, lithium ion batteries.The preparation method be using the covering liquid containing graphene and water soluble polymer to tertiary cathode material carry out cladding processing to get;The water soluble polymer is one or more in polyvinylpyrrolidone, diallyl dimethyl ammoniumchloride, kayexalate.The preparation method of modified tertiary cathode material provided by the invention carries out cladding processing using graphene and water soluble polymer to tertiary cathode material, and water soluble polymer can improve the surface-clinging ability of graphene, improve the cladding stability of graphene;Simultaneously, the surface coating layer that gained is modified tertiary cathode material contains graphene and water soluble polymer, dispersibility and structural stability of the positive electrode when further battery makes can be improved in the water soluble polymers such as polyvinylpyrrolidone, to enable the self-characteristic of graphene and ternary material to give full play to.
Description
Technical field
The invention belongs to electrode material fields, and in particular to a kind of modified tertiary cathode material and preparation method thereof, lithium from
Sub- battery.
Background technology
Lithium ion battery is the green clean energy resource and energy storage means of great competitiveness, and is expected to solve the present energy
The important means of crisis and greenhouse effects.Lithium ion battery has lot of advantages, for example battery capacity is higher, power density
Height, stable operating voltage, the features such as having extended cycle life, therefore have received widespread attention.With Sony release in 1991
After commercial Li-ion battery, lithium ion battery technology is rapidly developed, in fields such as portable electronic products, electric vehicles
It is widely used.
The energy density of lithium ion battery is primarily limited to the specific capacity of positive electrode, tertiary cathode material
(LiNixCoyMnzO2, x+y+z=1) and because having the characteristics that good specific capacity, environmental-friendly, become research heat in recent years
Point.But current ternary material itself there is also some problems, as first charge-discharge efficiency is low, structural stability is poor, poorly conductive,
High rate performance plays difference etc. under high-pressure solid.
Surface coating modification is one of the effective means for improving ternary material performance.Publication No. is the special of CN106450279A
Profit application disclose a kind of preparation method of graphene coated nickel cobalt manganese anode material for lithium-ion batteries, be with nickel source, cobalt source,
Manganese source, lithium source, ammonium hydroxide are raw material, then formulated suspension is added PDDA reactions, prepares positive electrode material precursor, then will be positive
Material precursor carries out carbonization treatment, obtains the tertiary cathode material of graphene coated modification.This method is to utilize coprecipitation
Positive electrode material precursor is prepared, then prepares modified anode material using high-temperature calcination, preparation process is relatively complicated, graphite
The cladding stability of alkene is poor.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of modified tertiary cathode material, are deposited to solve existing method
Graphene cladding stability difference problem.The present invention is additionally providing modification ternary that above-mentioned preparation method obtains just simultaneously
Pole material and the lithium ion battery for using the modification tertiary cathode material.
To achieve the above object, the technical solution adopted in the present invention is:
A kind of preparation method of modified tertiary cathode material, includes the following steps:Using containing graphene and high water solubility
The covering liquid of molecule to tertiary cathode material carry out cladding processing to get;The water soluble polymer be polyvinylpyrrolidone,
It is one or more in diallyl dimethyl ammoniumchloride, kayexalate.
The preparation method of modified tertiary cathode material provided by the invention, using graphene and water soluble polymer to ternary
Positive electrode carries out cladding processing, and water soluble polymer can improve the surface-clinging ability of graphene, improve the packet of graphene
Cover stability;Meanwhile the surface coating layer of gained modification tertiary cathode material contains graphene and water soluble polymer, polyethylene
Dispersibility and structural stability of the positive electrode when further battery makes can be improved in the water soluble polymers such as pyrrolidones, to
The self-characteristic of graphene and ternary material is set to give full play to.
It using the modification tertiary cathode material of the clad structure, is substantially improved with the compatibility of electrolyte, electricity can be optimized
Pond electrochemical reaction efficiency reduces internal resistance, and diallyl dimethyl ammoniumchloride, polystyrene sulphur are selected in water soluble polymer
When sour sodium, the two belongs to Ionomer in the electrolytic solution, further combined with the graphite with excellent ductility and electric conductivity
When alkene material, the electric conductivity and lithium ion transport rate of positive electrode can be significantly improved, and then improves gram appearance of positive electrode
Amount plays, and optimizes the cycle performance of battery.
Preferably, water soluble polymer includes polyvinylpyrrolidone and diallyl dimethyl ammoniumchloride, polyphenyl second
At least one of alkene sodium sulfonate.These types of water-soluble high-molecular material plays surfactant in the preparation process of modified material
Effect, on the one hand, its long chain, which can be coated on ternary NCM particle surfaces and prevent from being formed by particle, reunites,
On the other hand these types of high molecular material also has good adsorptivity to graphene so that graphene can be good at being coated on
The surface of ternary NCM materials.
In covering liquid, the mass content of graphene is 20%-50%.The mass content of water soluble polymer is 3%-6%.
The content of graphene in covering liquid, water soluble polymer is controlled in above range, graphene in clad, water-soluble high score can be made
The proportioning of son is reasonable, and electric conductivity, the structural stability that gained is modified tertiary cathode material reach best.
The solvent selection that covering liquid uses is not particularly limited, and can form the covering liquid of stable uniform, and then improve packet
The solvent for covering effect can be used.Preferably, solvent used in the covering liquid is water, ethyl alcohol, propyl alcohol, N, N- dimethyl methyls
It is one or more in amide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone, dimethyl sulfoxide (DMSO).
Covering liquid belongs to liquid-solid two phase system, after raw material being mixed using conventional method, can further using ultrasound, shake
The techniques such as dynamic improve the mixing homogeneity of covering liquid.Preferably, the covering liquid is prepared by method comprising the following steps:
Graphene dispersing solution and water soluble polymer are mixed, ultrasonic disperse uniformly to get.The power of the ultrasonic disperse is 100-
200W, time 30-60min.
During prepared by above-mentioned covering liquid, the prior art can be used in the preparation of graphene dispersing solution, or directly uses
Existing graphene dispersion liquid product.Preferably, the graphene dispersing solution is prepared by method comprising the following steps:It will
Graphene and solvent mixing, ultrasonic disperse uniformly to get.When prepared by graphene dispersing solution, the power of ultrasonic disperse is 100-
200W, time 30-60min.It is given full play to for characteristics such as the ductility, electric conductivity and machinability that enable graphene,
Preferably, the piece number of plies of the graphene is 1-8 layers.The graphene of this type belongs to customary commercial, can pass through commercially available routine
Channel obtains.
In the preparation process of above-mentioned modified tertiary cathode material, numerous embodiments can be used in cladding processing, such as pass through
Cladding processing is completed in multiple immersion, drying process, or directly using by the way of spray drying come realize it is capable of being industrialized soon
Speed prepares cladding product.The above cladding processing procedure processing procedure it is simple, be easy to industrializing implementation in terms of all have it is certain
Advantage.Here the present invention additionally provides a kind of cladding processing method, which can be improved the covered effect of covering liquid,
The substance of removal cladding binding force weakness, to keep structural stability, the repeatability of cladding product good.It is i.e. preferred, institute
It is to mix covering liquid and tertiary cathode material to state cladding processing, ultrasonic disperse processing.It is further preferred that cladding processing step
In rapid, the power of the ultrasonic disperse is 100-200W, time 60-120min.
In the scheme of above-mentioned preferred cladding processing, in order to improve coating efficiency, it is preferred that the addition of tertiary cathode material
Measure is 3-6 times of institute's graphene-containing quality in covering liquid.Tertiary cathode material is nickle cobalt lithium manganate or passes through other metallic elements
The modification ternary material of doping.The molecular formula of tertiary cathode material is LiNixCoyMnzO2, wherein x+y+z=1.
In the scheme of above-mentioned preferred cladding processing, ultrasonic disperse treated system is Unstable Systems, after standing point
Layer, lower layer's solid formation is the tertiary cathode material of coating modification.Following post-processing means can be used, to being obtained after cladding processing
Modification tertiary cathode material detached, obtain final products.I.e.:After ultrasonic disperse processing, stands to being layered, pour out upper layer
After liquid phase, lower layer's substance is centrifuged, then washed to centrifuging gained solid formation, dried and change to get described
Property tertiary cathode material.Preferably, the rotating speed of the centrifugation is 1000-3000r/min.
It is related in the scheme of ultrasonic disperse above-mentioned, can be used the high-power types such as supersonic cleaning machine, cell disruptor super
Sound mixing arrangement come realize high-volume, more stable ultrasonic disperse processing.
The preparation method of above-mentioned modified tertiary cathode material provided by the invention, relative to traditional vapor deposition, high temperature
The methods of calcining, technological process greatly simplifies, and implementation cost is lower, can also meet the requirement of high-volume, industrialized production.
The present invention also provides use modified tertiary cathode material made from above-mentioned preparation method.
It is water-soluble with graphene and polyvinylpyrrolidone etc. using modified tertiary cathode material made from above-mentioned preparation method
The high molecular mixture of property improves the stability of clad structure so that electric conductivity, ductility of graphene etc. as clad
Characteristic is given full play to, and the agglomeration of positive electrode is reduced, and dispersibility is obviously improved, and then also makes material entirety
Electric conductivity and lithium ion transport rate also significantly improve.
The present invention also provides the lithium ion batteries for using above-mentioned modified tertiary cathode material.
On the basis of above-mentioned modified tertiary cathode material, lithium ion battery can be prepared according to the conventional method of the prior art
Then lithium ion battery is made with conventional cathode, electrolyte assembling in anode.
Based on the performance characteristics of above-mentioned modified tertiary cathode material, the lithium-ion electric of the modification tertiary cathode material is used
The deficiencies of pond, ternary material self structure stability is poor, high rate performance plays difference under poorly conductive, high-pressure solid, is obviously changed
It is apt to, prepared capacity of lithium ion battery performance, high rate performance, cycle performance are obviously improved.
Specific implementation mode
Embodiments of the present invention are described further with reference to specific embodiment.In following embodiment, polyethylene
The molecular weight of pyrrolidones is 30000, is purchased from Aladdin reagent Co., Ltd;The molecular weight of diallyl dimethyl ammoniumchloride
It is 70000, is purchased from Aladdin reagent Co., Ltd;The molecular weight of kayexalate is 70000, purchased from the cruel that biology in Anhui
Engineering Co., Ltd.
Embodiment 1
The modification tertiary cathode material of the present embodiment, is prepared using following steps:
1) graphene that the piece number of plies is 1-8 layers is added to the water, after stirring evenly, the ultrasonic disperse under the power of 150W
30min obtains the graphene suspension that the mass content of graphene is 30%;
2) polyvinylpyrrolidone is added into graphene suspension, after stirring evenly, the ultrasound point under the power of 150W
30min is dissipated, the covering liquid that the mass content of polyvinylpyrrolidone is 3% is obtained;
3) nickel-cobalt-manganese ternary material (LiNi is added into covering liquid0.6Co0.2Mn0.2O2), the quality of nickel-cobalt-manganese ternary material
It is 3 times of institute's graphene-containing quality in graphene suspension, the ultrasonic disperse 60min under the power of 150W, it is quiet after ultrasonic disperse
It sets to layering, after pouring out upper phase, lower layer's substance migration centrifuge is detached with rotating speed 2000r/min, then to separation
Gained solid formation washed, dry to get.
Embodiment 2
The modification tertiary cathode material of the present embodiment, is prepared using following steps:
1) graphene that the piece number of plies is 1-8 layers is added in n,N-Dimethylformamide, after stirring evenly, 150W's
Ultrasonic disperse 45min under power obtains the graphene suspension that the mass content of graphene is 40%;
2) diallyl dimethyl ammoniumchloride is added into graphene suspension, after stirring evenly, in the power of 150W
Lower ultrasonic disperse 45min obtains the covering liquid that the mass content of diallyl dimethyl ammoniumchloride is 5%;
3) nickel-cobalt-manganese ternary material (LiNi is added into covering liquid0.6Co0.2Mn0.2O2), the quality of nickel-cobalt-manganese ternary material
It is 5 times of institute's graphene-containing quality in graphene suspension, the ultrasonic disperse 100min under the power of 150W, it is quiet after ultrasonic disperse
It sets to layering, after pouring out upper phase, lower layer's substance migration centrifuge is detached with rotating speed 1500r/min, then to separation
Gained solid formation washed, dry to get.
Embodiment 3
The modification tertiary cathode material of the present embodiment, is prepared using following steps:
1) graphene that the piece number of plies is 1-8 layers is added in N-Methyl pyrrolidone, after stirring evenly, in the work(of 150W
Ultrasonic disperse 60min under rate obtains the graphene suspension that the mass content of graphene is 50%;
2) kayexalate is added into graphene suspension, after stirring evenly, the ultrasound point under the power of 150W
60min is dissipated, the covering liquid that the mass content of kayexalate is 6% is obtained;
3) nickel-cobalt-manganese ternary material (LiNi is added into covering liquid0.6Co0.2Mn0.2O2), the quality of nickel-cobalt-manganese ternary material
It is 6 times of institute's graphene-containing quality in graphene suspension, the ultrasonic disperse 120min under the power of 150W, it is quiet after ultrasonic disperse
It sets to layering, after pouring out upper phase, lower layer's substance migration centrifuge is detached with rotating speed 3000r/min, then to separation
Gained solid formation washed, dry to get.
Embodiment 4-6
The modification tertiary cathode material of embodiment 4, preparation process is substantially the same manner as Example 3, differs only in step 2)
In, polyvinylpyrrolidone and diallyl dimethyl ammoniumchloride, the mass content of the two are added into graphene suspension
Respectively 2% and 3%.
The modification tertiary cathode material of embodiment 5, preparation process is substantially the same manner as Example 3, differs only in step 2)
In, polyvinylpyrrolidone and kayexalate are added into graphene suspension, the mass content of the two is respectively 2%
With 3%.
The modification tertiary cathode material of embodiment 6, preparation process is substantially the same manner as Example 3, differs only in step 2)
In, polyvinylpyrrolidone, diallyl dimethyl ammoniumchloride and kayexalate are added into graphene suspension,
The mass content of three is respectively 2%, 2% and 2%.
Test example
This test example presses matter with the modification tertiary cathode material obtained by embodiment 1-6, with conductive agent CNT, binder PVDF
Measure ratio 9.7:1:1.3 are added into N-Methyl pyrrolidone, are sufficiently mixed, prepare positive electrode slurries, by positive electrode slurries
Coated on aluminium foil, lithium ion cell positive is prepared through techniques such as drying, roll-in, slices.By graphite, conductive agent SP, binder
CMC, binder SBR in mass ratio 9.5:1:1.5:2.5 are added into a certain amount of deionized water, prepare negative material slurries, will
Negative material slurries are coated on copper foil, and negative electrode of lithium ion battery is prepared through techniques such as drying, roll-in, slices.With a concentration of
The LiPF of 1mol/L6(solvent is volume ratio EC to solution:The 1 of DMC:The mixed solvent of 1 composition) it is electrolyte.By anode, cathode,
Electrolyte is assembled into the lithium ion battery of 5Ah, the electrochemistry of the lithium ion battery of each embodiment and comparative example by the prior art
It can, wherein the testing conditions of cycle performance are under conditions of test voltage 2.75~4.25V of range, with the electric current of 1C (5A)
Charge-discharge test is carried out to battery, the results are shown in Table 1.
Comparative example 1 is non-modified nickel-cobalt-manganese ternary material (LiNi0.6Co0.2Mn0.2O2), comparative example 2 is single graphite
Nickel-cobalt-manganese ternary material (the LiNi that alkene is modified0.6Co0.2Mn0.2O2), the method for specific method of modifying reference implementation example 1 carries out.
Comparative example 1, comparative example 2 positive electrode on the basis of, prepare corresponding lithium ion battery with reference to the above method.
The chemical property of the lithium ion battery of 1 each embodiment and comparative example of table compares
Number | First circle specific capacity, mAh/g | Specific capacity after 200 circle of cycle, mAh/g |
Embodiment 1 | 5.196 | 5.014 |
Embodiment 2 | 5.165 | 4.963 |
Embodiment 3 | 5.136 | 4.972 |
Embodiment 4 | 5.094 | 4.930 |
Embodiment 5 | 5.149 | 4.996 |
Embodiment 6 | 5.182 | 5.022 |
Comparative example 1 | 5.068 | 4.839 |
Comparative example 2 | 5.125 | 4.904 |
As shown in Table 1, relative to the lithium ion battery of comparative example, due to modified tertiary cathode material obtained by the present invention
The comprehensive of the performances such as electric conductivity, lithium ion transport rate, structural stability, the dispersibility of material improves, prepared lithium ion
The electrochemical reaction internal resistance of battery is small, and electron conduction and ionic conductivity are excellent, the volumetric properties of battery, high rate performance and follows
Ring performance is obviously improved.
In the other embodiment of the modification tertiary cathode material of the present invention, solvent used in covering liquid can be in the present invention
It is replaced, adjusts in the solvent type of restriction;Tertiary cathode material can be nickle cobalt lithium manganate (such as nickel cobalt manganese of other proportionings
111, nickel cobalt manganese 523);The power of ultrasonic disperse and time can be adaptively adjusted in the framework of the present definition, can be obtained
To with the comparable modified tertiary cathode material of embodiment and lithium ion battery.
Claims (10)
1. a kind of preparation method of modified tertiary cathode material, which is characterized in that include the following steps:Using containing graphene and
The covering liquid of water soluble polymer to tertiary cathode material carry out cladding processing to get;The water soluble polymer is polyethylene
It is one or more in pyrrolidones, diallyl dimethyl ammoniumchloride, kayexalate.
2. the preparation method of modified tertiary cathode material as described in claim 1, which is characterized in that in covering liquid, graphene
Mass content be 20%-50%.
3. the preparation method of modified tertiary cathode material as claimed in claim 1 or 2, which is characterized in that water-soluble in covering liquid
Property high molecular mass content be 3%-6%.
4. the preparation method of modified tertiary cathode material as described in claim 1, which is characterized in that the covering liquid is used
Solvent be water, ethyl alcohol, propyl alcohol, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone, dimethyl
It is one or more in sulfoxide.
5. the preparation method of modified tertiary cathode material as described in claim 1, which is characterized in that the covering liquid is by including
The method of following steps is prepared:Graphene dispersing solution and water soluble polymer are mixed, ultrasonic disperse uniformly to get.
6. the preparation method of modified tertiary cathode material as described in claim 1, which is characterized in that the cladding processing be by
Covering liquid and tertiary cathode material mixing, ultrasonic disperse processing.
7. the preparation method of modified tertiary cathode material as claimed in claim 6, which is characterized in that the work(of the ultrasonic disperse
Rate is 100-200W, time 60-120min.
8. the preparation method of modified tertiary cathode material as claimed in claim 6, which is characterized in that the matter of tertiary cathode material
Measure is 3-6 times of institute's graphene-containing quality in covering liquid.
9. one kind modified tertiary cathode material made from preparation method described in claim 1.
10. a kind of lithium ion battery using modified tertiary cathode material as claimed in claim 9.
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CN109742357B (en) * | 2019-01-03 | 2021-12-10 | 浙江锋锂新能源科技有限公司 | Composite anode material, preparation method thereof and anode plate containing anode material |
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CN112164774A (en) * | 2020-09-08 | 2021-01-01 | 合肥国轩高科动力能源有限公司 | Composite high-nickel ternary cathode material and preparation method thereof |
CN112331826A (en) * | 2020-10-23 | 2021-02-05 | 华南师范大学 | Modified lithium ion battery positive electrode material and preparation method and application thereof |
CN112186167A (en) * | 2020-10-28 | 2021-01-05 | 陕西彩虹新材料有限公司 | Preparation method of template-method-coated high-nickel ternary cathode material for lithium ion battery |
CN112563504A (en) * | 2020-12-09 | 2021-03-26 | 北京理工大学重庆创新中心 | Method for regulating and controlling surface transmission efficiency of lithium battery anode material and obtained anode material |
CN113716623A (en) * | 2021-08-27 | 2021-11-30 | 中国地质大学(武汉) | High-nickel ternary material LiNi0.80Co0.15Al0.05O2Coating method of |
CN113716623B (en) * | 2021-08-27 | 2022-07-19 | 中国地质大学(武汉) | High-nickel ternary material LiNi0.80Co0.15Al0.05O2Coating method of |
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