CN108091871A - A kind of porous spherical ternary cathode material of lithium ion battery and preparation method thereof - Google Patents
A kind of porous spherical ternary cathode material of lithium ion battery and preparation method thereof Download PDFInfo
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- CN108091871A CN108091871A CN201711454541.1A CN201711454541A CN108091871A CN 108091871 A CN108091871 A CN 108091871A CN 201711454541 A CN201711454541 A CN 201711454541A CN 108091871 A CN108091871 A CN 108091871A
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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
- 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
- H01M4/52—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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
A kind of preparation method of cellular spherical ternary cathode material of lithium ion battery, comprises the following steps, 1)Prepare the Diversity solution of nickel salt, cobalt salt and manganese salt;2)Carbon source obtains carbon ball presoma through hydro-thermal reaction, and carbon ball presoma obtains carbon ball through sintering, and obtained carbon ball is immersed in step 1)Diversity solution in;3)By step 2)Obtained mixed solution is added to ammonium hydroxide and sodium hydroxide solution cocurrent in the reaction unit containing bottom liquid, is carried out coprecipitation reaction and is obtained sodium hydroxide object presoma;4)After the sodium hydroxide presoma obtained in step 3 is washed and lithium salts carries out being thermally treated resulting in tertiary cathode material together.A kind of porous spherical tertiary cathode material good sphericity of the present invention, even particle distribution, there are higher specific surface area and tap density, and internal porous structure is suitble to the transmission of lithium ion, the high rate performance and stability of material can effectively be improved, and preparation method is simple, easily controllable, is suitble to industrialization production.
Description
Technical field
Positive electrode more particularly to a kind of porous spherical lithium ion battery ternary the present invention relates to a kind of lithium ion battery
Positive electrode and preparation method thereof.
Background technology
At present, fossil fuel is still main for electric resources.However as the mankind unreasonable exploitation and utilization, fossil
Energy day is becoming tight, environmental pollution getting worse.Therefore, new cleaning resource and regenerative resource, such as sun are developed
Energy, wind energy, tide energy etc. become the task of top priority.But then, the normal operation of power grid needs the power generation of steady and continuous, too
Positive energy, wind energy, tide energy etc. are restricted be subject to factors such as weather, place and times, are significantly limited it and on a large scale should
With and popularization.In order to solve this problem, extensive electricity storage technology becomes an important field of research.Wherein, secondary cell
Due to having higher energy density and transformation efficiency, become the prioritizing selection of extensive storing up electricity, and have extended cycle life and have
The lithium ion battery for having highest energy density is considered as most promising secondary cell.From lithium-ion electric the 1990s
Since pond successfully comes out, the application of considerable scale has been obtained in electric vehicle, mancarried electronic aid etc., but with lithium from
The continuous progress and development of sub- battery, a series of hidden danger have also gradually been exposed among the visual field of people.
According to the planning of current country, the energy density positive to the year two thousand twenty reaches 250mAh/g or even arrives 300mAh/g's
Energy density index, then the electrode material system of present commercial applications can not all be realized, therefore just need larger technology
Reform.By taking electric vehicle as an example, to run farther, must just there are the higher energy content of battery and continuation of the journey, just be widely used at present
The needs for meeting development have been difficult to for the LFP of power battery.And ternary battery higher energy density and is followed compared to having
Ring performance becomes the only selection of battery system.
Place of the positive electrode as main storage lithium ion inside current lithium ion battery, performance directly affect lithium
The performance of ion battery.However tertiary cathode material causes the high rate performance and stability of material with the continuous improvement of capacity
It is deteriorated, a hidden danger will certainly be become in the epoch of this " fast charge ".
The content of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide it is a kind of it is simple for process, reproducible,
The preparation method of of low cost, environmental-friendly lithium ion battery porous spherical tertiary cathode material.
In order to solve the above technical problems, technical solution proposed by the present invention is:A kind of cellular spherical lithium ion battery ternary
The preparation method of positive electrode, comprises the following steps, and 1)Prepare the Diversity solution of nickel salt, cobalt salt and manganese salt;
2)Carbon source obtains carbon ball presoma through hydro-thermal reaction, and carbon ball presoma obtains carbon ball, and the carbon that will be obtained through sintering processes
Ball is immersed in step 1)Diversity solution in;
3)By step 2)Obtained mixed solution is added to the reaction unit containing bottom liquid with ammonium hydroxide and sodium hydroxide solution cocurrent
In, it carries out coprecipitation reaction and obtains sodium hydroxide object presoma;In the present invention, bottom liquid is sodium hydroxide and the mixed liquor of ammonium hydroxide.
4)The sodium hydroxide presoma obtained in step 3 is washed, the ternary precursor and lithium salts obtained after washing
It is heat-treated together and falls to obtain tertiary cathode material by the carbon ball sintering in hydroxide precursor.
In the present invention, first carbon source is dissolved in water, carbon ball is made by hydro-thermal reaction, sintering;Liquid is then used again
Phase infusion process is in polynary step 1)So that carbon ball is uniformly distributed in obtained complex solution;Then by mixed solution and complexing agent
(Ammonium hydroxide)And precipitating reagent(Sodium hydroxide)Presoma is obtained by the reaction.The presoma distribution of pores of chondritic produced by the present invention is equal
Even, spacing is moderate, large specific surface area.Presoma obtained and lithium salts are further processed to obtain anode material for lithium-ion batteries,
It can show high charge-discharge specific capacity, good high rate performance and long circulating stability energy.In addition, the method for the present invention it is simple for process,
It is reproducible, of low cost, environmental-friendly.
Carbon ball obtained is directly immersed in complex solution by the present invention, is conducive to each element in carbon ball by template of carbon ball
Surface homogeneous precipitation, and then obtain that sphericity is good, the homogeneous spherical presoma of particle.It is removed by being heat-treated in presoma
The porous spherical positive electrode that carbon ball obtains is conducive to lithium ion uniformly from all directions deintercalation, not only ensure that capacity, but also energy
Improve high rate performance, the problems such as stability is poor.
In the present invention, the carbon source of use dissolves and/or is dispersed in water to obtain carbon source solution, is then placed in the carbon source solution
Under confined conditions, hydro-thermal reaction is carried out;After hydro-thermal reaction, separation of solid and liquid is carried out to hydro-thermal reaction liquid, collection obtains solid,
Up to the carbon ball presoma after washing, drying, by the carbon ball presoma sintering processes, the carbon ball is made.
In the present invention, step 2)Described in carbon source be water-soluble saccharides compound, be glucose, sucrose, lignin, fiber
At least one of element, starch.Most preferably still more preferably, the carbon source is
In the present invention, step 1)The nickel of middle Diversity solution, cobalt, the ratio of manganese are 8:1:1.
In the present invention, step 1)In, the nickel salt is nickel nitrate, nickel chloride, nickel acetate, at least one of nickel sulfate,
Preferably nickel sulfate, nickel chloride.The manganese salt is manganese nitrate, manganese chloride, manganese acetate, at least one of manganese sulfate, best
It is manganese sulfate, manganese chloride.The cobalt salt is at least one of cobalt nitrate, cobalt chloride, cobalt acetate, cobaltous sulfate, preferably sulphur
Sour cobalt, cobalt chloride.
In the present invention, the step 1)The total ion concentration of obtained Diversity solution is 1mol/L-1.5mol/L, is walked
Rapid 3)Middle concentration of sodium hydroxide solution is 7.5-10mol/L, ammonia concn 6-8mol/L.
In the present invention, step 3)The charging rate of middle mixed solution is 90-150ml/min, sodium hydroxide charging rate is
30-70ml/L, ammonium hydroxide charging rate are 5-40ml/L;Preferably, step 3)The charging rate of middle mixed solution is 100-
140ml/min, sodium hydroxide charging rate are 40-60ml/min, ammonium hydroxide charging rate is 10-30ml/min, should in the range of
The grain speed of growth is stablized, good sphericity.
In the present invention, step 3)The PH of middle coprecipitation reaction be 10-12, ammonium ion concentration be 5-9g/L, should in the range of
Be conducive to evengranular growth, good dispersion avoids particle agglomeration.Reaction temperature is 50-60 °C, speed of agitator 200-
400r/min。
8th, the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, feature
It is:Step 4)The ternary precursor obtained after middle lithium salts and washing is according to 1.05:1 ratio mixing, under oxygen atmosphere first
Pre-sintering 2-5h, is carbonized under conditions of 300-500 DEG C, and temperature is preferably 400-450 DEG C, then is warming up to 700-1000 DEG C
Under conditions of be sintered 12-16h, by be sintered remove presoma in carbon ball, the porous spherical ternary material needed.At this
In invention, the temperature setting of sintering under condition collaboration in front, can make the even pore distribution of positive electrode obtained,
Away from moderate, porosity height, large specific surface area, good conductivity.During heating, heating rate is 1-10 DEG C/min;It is best
It is the regularity that 3-8 DEG C/min is more advantageous to ensureing material morphology structure in the preferred heating rate.
The present invention also provides a kind of lithium ion battery porous spherical tertiary cathode material, in porous spherical, the D50 of granularity
For 10-12um, tap density 1.8-2.5g/cm3, specific surface area 4-7g/m2。
A kind of porous spherical tertiary cathode material good sphericity of invention, even particle distribution have higher ratio
Surface area and tap density, and internal porous structure is suitble to the transmission of lithium ion, can effectively improve the high rate performance of material
And stability, and preparation method is simple, easily controllable, is suitble to industrialization production.
Compared with prior art, the advantage of the invention is that:
1)The present invention is directly dispersed in carbon ball obtained in material solution, obtains the internal spherical presoma for being inlaid with carbon ball.
Positive electrode is thermally treated resulting in afterwards.The positive electrode has chondritic, and internal porous.By the material be used as lithium from
The anode of sub- battery has excellent electric property.
2)In preparation method of the present invention, the carbon ball is as template while and pore creating material.Pass through the carbon ball and original
Expect under the collaboration of the conditions such as concentration, pH, ammonium root concentration rotating speed, hole can be controlled in suitable scope, and then be obviously improved system
The chemical property of the positive electrode obtained.
3)The positive electrode of the present invention can be used for preparing steady with high specific discharge capacity, excellent high rate performance and long circulating
The lithium ion battery of qualitative energy.
4)The present invention the carbon material method for preparing operation is simple and reliable, it is reproducible, workable, environmental-friendly, into
This is cheap, has wide industrial applications prospect.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of ternary anode material precursor made from embodiment 1(SEM).
Fig. 2 is the capacity circulating efficiency chart of porous spherical tertiary cathode material made from embodiment 1.
Specific embodiment
For the ease of understanding the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
A kind of preparation method of porous spherical ternary cathode material of lithium ion battery, comprises the following steps:Step 1), according to
Ni:Co:Mn=8:1:1 ratio prepares nickel salt, cobalt salt, the Diversity solution of manganese salt, total ion concentration 1mol/L-
1.5mol/L;
Step 2), the water-soluble carbon source solution of 0.1-4g/L is configured, carbon ball forerunner is obtained in 150-200 °C of lower hydro-thermal reaction 10-15h
Body is protected and carbon ball presoma is sintered 9-12h under 1000-1200 °C obtains carbon ball under gas shielded and be immersed in the polynary of a
In solution;
Step 3), the mixed solution of b obtained above and the sodium hydroxide cocurrent of 6-8mol/L ammonium hydroxide and 7.5-10mol/L are added
Enter into the reaction unit containing bottom liquid, adjust mixing complex solution charging rate for 100-140ml/min, sodium hydroxide into
Expect that speed is 40-60ml/min, ammonium hydroxide charging rate is 10-30ml/min.Reaction temperature is 50-60 °C, rotating speed 200-
400r/min.PH is 10-12, and ammonium ion concentration carries out coprecipitation reaction for 5-9g/L and obtains hydroxide precursor.
Step 4), above-mentioned presoma is centrifuged, washed and dried, and takes lithium salts:Ternary precursor=1.05:1 is mixed
It closes, first in 400-450 °C of pre-sintering 2-5h under oxygen atmosphere, then is warming up to 700-1000 °C and is sintered 12-16h to get to institute
The porous spherical ternary material stated obtains the tertiary cathode material of porous spherical.
Embodiment 1
Configure the sulfate liquor that total concentration of metal ions is 1.5mol/L(Ni:Co:Mn=8:1:1), the grape of 2g is weighed first
Sugar is dissolved in deionized water, by hydro-thermal reaction and heat treatment, is obtained hard carbon microballoon and is dispersed in mixed solution.It will be above-mentioned
Mixed solution is flowed into together with ammonium hydroxide and sodium hydroxide in the reaction kettle containing sodium hydroxide and ammonia water mixture, adjusts reaction kettle
Rotating speed is 300r/min, and temperature is 55 degree.It is 6-8g/L, pH 12 to adjust mother liquor ammonium root concentration, makes to have mixed in solution
Even each component comes out according to chemical dosage ratio co-precipitation.Lithium hydroxide is taken afterwards:Presoma=1.05:1, in oxygen gas
First in 400-450 °C of pre-sintering 2h under atmosphere, then 800-1000 °C of sintering 15h is warming up to get to the porous spherical ternary
Material.
Porous spherical material manufactured in the present embodiment is used as working electrode, lithium piece is to electrode, is assembled into button cell,
Under the multiplying power of 1C, chemical property is tested.The scanning electron microscope (SEM) photograph of the ternary anode material precursor of the present embodiment(SEM)Such as figure
Shown in 1.The capacity circulating efficiency chart of the porous spherical tertiary cathode material of the present embodiment is as shown in Figure 2.
From test result, lithium electricity prepared by this example is just having good chemical property;It is first under the multiplying power of 1C
It is 88% to enclose coulombic efficiency, after 50 circle of Xun Huan, remains to keep the specific capacity of 185mA/g.
Comparative example 1
Configure the sulfate liquor that total concentration of metal ions is 1.5mol/L(Ni:Co:Mn=8:1:1), by above-mentioned solution together with ammonia
Water and sodium hydroxide are added to the reaction kettle containing sodium hydroxide and ammonia water mixture, and it is 300r/min to adjust reaction kettle rotating speed,
Temperature is 55 degree.It is 6-8g/L, pH 12 to adjust mother liquor ammonium root concentration, makes each component in solution by evenly mixing according to change
Dose ratio co-precipitation is learned to come out.Lithium hydroxide is taken afterwards:Presoma=1.05:1, first at 400-450 °C under oxygen atmosphere
Pre-sintered 2h, then 800-1000 °C of sintering 15h is warming up to get to spherical tertiary cathode material.
Spheroidal material manufactured in the present embodiment is used as working electrode, lithium piece is to electrode, button cell is assembled into, in 1C
Multiplying power under, test chemical property.
From test result, lithium electricity anode chemical property prepared by this example is poor;Under the multiplying power of 1C, first circle coulomb
Efficiency is 72%, after 50 circle of Xun Huan, is only capable of keeping the specific capacity of 132mA/g.
Claims (9)
1. a kind of preparation method of cellular spherical ternary cathode material of lithium ion battery, it is characterised in that:Comprise the following steps, 1)
Prepare the Diversity solution of nickel salt, cobalt salt and manganese salt;
2)Carbon source obtains carbon ball presoma through hydro-thermal reaction, and carbon ball presoma obtains carbon ball, and the carbon that will be obtained through sintering processes
Ball is immersed in step 1)Diversity solution in;
3)By step 2)Obtained mixed solution is added to the reaction unit containing bottom liquid with ammonium hydroxide and sodium hydroxide solution cocurrent
In, it carries out coprecipitation reaction and obtains sodium hydroxide object presoma;
4)The sodium hydroxide presoma obtained in step 3 is washed, the ternary precursor and lithium salts obtained after washing is together
It is heat-treated and falls to obtain tertiary cathode material by the carbon ball sintering in hydroxide precursor.
2. the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Step 2)Described in carbon source be glucose, sucrose, lignin, cellulose, at least one of starch.
3. the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Step 1)The nickel of middle Diversity solution, cobalt, the ratio of manganese are 8:1:1.
4. the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Step 1)In, the nickel salt is at least one of nickel nitrate, nickel chloride, nickel acetate, nickel sulfate;The manganese salt is nitric acid
At least one of manganese, manganese chloride, manganese acetate, manganese sulfate;The cobalt salt is cobalt nitrate, in cobalt chloride, cobalt acetate, cobaltous sulfate
At least one.
5. the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
The step 1)The total ion concentration of obtained Diversity solution be 1mol/L-1.5mol/L, step 3)Middle sodium hydroxide is molten
Liquid concentration is 7.5-10mol/L, ammonia concn 6-8mol/L.
6. the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Step 3)The charging rate of middle mixed solution is 90-150ml/min, sodium hydroxide charging rate is 30-70ml/L, ammonium hydroxide charging
Speed is 5-40ml/L.
7. the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Step 3)The PH of middle coprecipitation reaction is 10-12, and ammonium ion concentration is 5-9g/L, and reaction temperature is 50-60 °C, speed of agitator
For 200-400r/min.
8. the preparation method of cellular spherical ternary cathode material of lithium ion battery according to claim 1, it is characterised in that:
Step 4)The ternary precursor obtained after middle lithium salts and washing is according to 1.05:1 ratio mixing, first in 300- under oxygen atmosphere
Pre-sintering 2-5h under conditions of 500 DEG C, then it is sintered 12-16h under conditions of being warming up to 700-1000 DEG C.
9. a kind of lithium ion battery porous spherical tertiary cathode material obtained such as claim 1-8 any one of them preparation methods
Material, it is characterised in that:The tertiary cathode material is in porous spherical, and granularity D50 is 10-12um, tap density 1.8-2.5g/
cm3, specific surface area 4-7g/m2。
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CN109052490A (en) * | 2018-07-09 | 2018-12-21 | 华中科技大学 | A kind of ternary cathode material of lithium ion battery and preparation method thereof |
CN109301186A (en) * | 2018-09-10 | 2019-02-01 | 清远佳致新材料研究院有限公司 | A kind of tertiary cathode material and preparation method thereof of cladded type porous structure |
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CN109786695A (en) * | 2018-12-29 | 2019-05-21 | 合肥融捷能源材料有限公司 | A kind of high magnification nickel-cobalt lithium manganate cathode material and preparation method thereof |
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CN109052490A (en) * | 2018-07-09 | 2018-12-21 | 华中科技大学 | A kind of ternary cathode material of lithium ion battery and preparation method thereof |
CN109301186B (en) * | 2018-09-10 | 2020-09-15 | 清远佳致新材料研究院有限公司 | Coated porous ternary cathode material and preparation method thereof |
CN109301186A (en) * | 2018-09-10 | 2019-02-01 | 清远佳致新材料研究院有限公司 | A kind of tertiary cathode material and preparation method thereof of cladded type porous structure |
CN109638248A (en) * | 2018-12-10 | 2019-04-16 | 北方奥钛纳米技术有限公司 | A kind of preparation method of porous triple material, porous triple material and half-cell |
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