CN105932281A - Preparation method for graphite anode material of lithium ion battery - Google Patents
Preparation method for graphite anode material of lithium ion battery Download PDFInfo
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- CN105932281A CN105932281A CN201610391032.8A CN201610391032A CN105932281A CN 105932281 A CN105932281 A CN 105932281A CN 201610391032 A CN201610391032 A CN 201610391032A CN 105932281 A CN105932281 A CN 105932281A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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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
- H01M4/04—Processes of manufacture in general
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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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
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Abstract
The invention discloses a preparation method for a graphite anode material of a lithium ion battery. Fine graphite powder with a small particle size and an organic carbon source are taken as raw materials; through adoption of processes such as mixing, high temperature processing, graphitizing and sieving and through mixing of the fine powder and the organic carbon source in a heating environment, coating, kneading and secondary granulating effects can be realized; and under the adhering effect of the organic carbon source, the fine powder with the small particle size forms secondary particles. The anisotropy problem of the materials is solved, and the tap density of the materials is improved. According to the method, the turnover and device residual loss of the materials are reduced, the yield is high, the processes are simple, the energy consumption is low, the environment is protected, the surface coating effects of the materials are even, and the consistency is high. The prepared anode material is characterized in anisotropy, low iron impurity content, low initial irreversible capacity, low volume expansion, high liquid absorbency, high cycle performance, high cost performance and high comprehensive performance.
Description
Technical field
The invention belongs to field of lithium ion battery, be specifically related to the preparation side of a kind of graphite negative material of lithium ion battery
Method.
Background technology
The advantages such as lithium ion battery has that high voltage, specific energy be big, life-span length and memory-less effect, thus in recent years,
3C Product, electric bicycle, energy-storage system, particularly electric automobile are used widely.Graphite negative electrodes material is current
The leading negative material of commercial Li-ion battery, it has relatively low lithium intercalation/deintercalation current potential, higher reversible capacity and money
The advantages such as source is abundant, cheap.
Lithium ion battery negative material presently mainly has the material of graphite-structure, and wherein native graphite quickly grows.
MCMB is the one of native graphite, its Stability Analysis of Structures, and specific surface area is little, and cycle performance and safety are good, but its
Cost of manufacture is high, is used as high-end ion cathode material lithium all the time.General natural graphite powder is in irregular shape,
Specific surface area is big, and degree of anisotropy is higher, causes materials processing poor performance, and the problem such as pole piece bounce-back, battery core flatulence, deformation is prominent
Go out.Therefore reducing specific surface area, improve isotropism degree, the cycle performance and the safety that improve battery core are always native graphite class
The emphasis of carbon cathode material research and development.
Chinese patent CN96198348.5 and CN03120199.6 etc., use Colophonium, petroleum tar, coal tar or they
Mixture coated graphite, asphalt pyrolysis charcoal is less than the specific surface area of Resin Char coated graphite, and the affinity of graphite to be got well,
Structure is more firm, but pitch-coating deforms because of fusing in heating process, and consumption the most also easily causes Coating Graphite Particles
Being mutually bonded, consumption is very few, and to easily cause cladding uneven, and is prone in heating process expand, and affects the electrical property of graphite.
After Chinese patent CN101162775A uses liquid phase method Colophonium and resin to be dissolved simultaneously, add graphite mixing,
Then steam solvent, finally carry out heat treatment, the mixture of Colophonium He one or more resin formation is coated on graphite
Surface, improves the cycle efficieny of graphite and cyclical stability and multiplying power property and compressible performance.But the method is in reality
Border application also there are some shortcomings, use liquid phase method to need to use organic solvent, easily cause pollution, simultaneously to solute Colophonium
Requiring the highest (quinoline insolubles content is not more than 12%), evaporation recycling design needs complicated equipment, easily causes investment
Excessive, these result in and are difficult to be applied in industrialized production.
Chinese patent CN102082272A uses hard charcoal precursor, soft charcoal precursor and hetero atom modifying agent, Yi Jishi
After ink mixes in proportion, first carry out cured, then carry out the most relatively low heat treatment, finally carry out secondary high-temperature
Graphitization processing, obtains the lithium ion battery negative material being coated with containing hard charcoal.But the method is owing to using in normal-temperature solid-phase condition
The lower way by the mixing of up to four kinds of powder body, is first difficult to ensure that the uniformity that multiple covering material presoma mix, next by
In two kinds of precursors, the proportion of soft charcoal precursor is too high, so also needing secondary high temperature graphitization to process, and otherwise can be because of
The degree of graphitization of soft charcoal is on the low side and causes the specific capacity of final coated graphite material on the low side.So eventually result in production
The rising of cost, it is difficult to meet the requirement that market is inexpensive to product.
Chinese patent CN201410325202.3 by by material Physical Processing, mix, mold pressing process, calcination process and ball
Changing the operations such as shaping and prepare a kind of natural graphite negative electrode material, material cycling loss is big, and production efficiency is low, and energy consumption is big, and technique is multiple
Miscellaneous.
Chinese patent CN02125715.9 utilizes the method for mist projection granulating at one layer of charcoal of graphite microparticles Surface coating, obtains interior
Portion is graphite, and outside is the carbon coated graphite microparticles of the nucleocapsid structure of charcoal, and irreversible capacity is relatively low first, and cycle performance is preferable,
But the method complex process, energy consumption is big, and production cost is high.
Chinese patent CN200510029448.7 after native graphite micropowder Surface coating organic carbon source through roasting etc.
The natural graphite negative electrode material that reason obtains, need to select the aromatic solvent such as carbolineum and washing oil as reaction promoter, carbolineum and washing oil
In containing the noxious substance such as anthracene, naphthalene, high boiling point phenols, heavy pyridine bases, acenaphthene, fluorenes, unfriendly to environment.
Summary of the invention
The purpose of the present invention is just also to solve above-mentioned technological deficiency of the prior art, it is provided that a kind of graphite cathode material
Preparation method.
The present invention specifically provides following technical scheme, the preparation method of a kind of graphite negative material of lithium ion battery, its
Comprise the steps:
(1) batch mixing: organic carbon source and graphite fine powder are added the blender with heating function by a certain percentage, be stirred continuously to
Mix homogeneously;
(2) high-temperature process: the powder body of mix homogeneously is warming up to 500~1100 DEG C, and constant temperature 3~10 hours, be subsequently cooled to
Room temperature;
(3) graphitization processing: by the material after high-temperature process 2600 DEG C of graphitization processing carried out above;
(4) screening: being sieved by the powder body after graphitization processing, collection screen blanking obtains finished product.
Organic carbon source in step (1) is asphalt, coal tar pitch, phenolic resin, polrvinyl chloride, polystyrene, phenolic aldehyde
Resin, epoxy resin one or more.
Graphite fine powder in step (1) is petroleum coke micropowder, needle coke micropowder, pitch coke micropowder, mesophase micropowder, natural
One or more in graphite microparticles, graphite fine powder mean diameter D50 is 2~10 μm.
In step (1), the weight ratio of graphite fine powder and organic carbon source is 10:(1~4).
Agitating heating temperature in step (1) is 50~300 DEG C, and mixing time is 1~12 hour.
The heating rate of step (2) is 0.5~5 DEG C/min, and cooling is to naturally cool to 200~300 DEG C, then forces cold
But to room temperature.
Step (2) and (3) are carried out under non-oxide protective atmosphere, are to be passed through the indifferent gas such as nitrogen in preparation process
Body is protected, and its gas flow is 5~30L/min.
The minus mesh collected through screening in step (4), its mean diameter D50 is 8~25 μm.
The present invention use raw material be mean diameter D50 be the graphite fine powder of 2~10 μm, select the thin of smaller particle diameter
Powder, has the features such as specific surface area is big, tap density is low.But it is just little due to its particle diameter, it is possible to shorten lithium ion and enter stone
Channel resistance between layer of ink, shows more excellent high rate performance and cryogenic property.By fine powder with organic carbon source in heating
Carry out mixed processing under environment, the effects such as cladding, kneading, secondary granulation can be played, make the fine powder of small particles at organic carbon source
Under cementation, form second particle, the problem solving each diversity of material, improves the tap density of material.
The invention have the advantages that and good effect:
1, the operations such as cladding, secondary granulation, kneading are comprehensively carried out by this preparation method, decrease turnover and the equipment residual of material
Loss, productivity is high, and operation is simple, and energy consumption is low, environmental protection, material Surface coating uniform in effect, and concordance is high;
2, relatively good to raw-material orientation Resolving probiems, macroscopically isotropic, iron tramp content is low, the lithium-ion electric prepared
Pond negative material, irreversible capacity is low first, and volumetric expansion is little, and absorbency is good, and good cycle, cost performance are high, combination property
Excellent.
Accompanying drawing explanation
The negative material scanning electron microscope (SEM) photograph of Fig. 1 embodiment of the present invention 1.
The negative material full circulating battery curve chart of Fig. 2 embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the preferably embodiment of the present invention is described in further detail, but the present invention
Embodiment be not limited to this.
Embodiment 1
With native graphite fine powder as raw material (mean diameter D50 is 5 μm), asphalt (softening point is 100 DEG C) is organic carbon source,
Both mass ratioes are 10:3, weigh 100Kg native graphite fine powder and 30Kg asphalt, add reactor stirring, temperature together
For DEG C 120, mixing time is 6 hours.
It is warming up to 800 DEG C afterwards with the heating rate of 5 DEG C/min, and constant temperature 5 hours, it is then cooled to room temperature, then by material
Material is 2600 DEG C of graphitization processing carried out above.
Finally, being sieved by powder body, collection screen blanking obtains finished product.
Embodiment 2
With native graphite fine powder as raw material (mean diameter D50 is 7 μm), coal tar pitch (softening point is 150 DEG C) is organic carbon source, two
Person's mass ratio is 10:3.5, weighs 100Kg native graphite fine powder and 35Kg coal tar pitch, adds reactor stirring together, and temperature is
DEG C 170, mixing time is 5 hours.
It is warming up to 900 DEG C afterwards with the heating rate of 5 DEG C/min, and constant temperature 4 hours, it is then cooled to room temperature, then by material
Material is 2600 DEG C of graphitization processing carried out above.
Finally, being sieved by powder body, collection screen blanking obtains finished product.
Embodiment 3
With native graphite fine powder as raw material (mean diameter D50 is 6.5 μm), asphalt (softening point is 120 DEG C) is organic carbon
Source, both mass ratioes are 10:2.5, weigh 100Kg native graphite fine powder and 25Kg asphalt, add reactor stirring together,
Temperature is 150 DEG C, and mixing time is 4.5 hours.
It is warming up to 850 DEG C afterwards with the heating rate of 4 DEG C/min, and constant temperature 4 hours, it is then cooled to room temperature, then by material
Material is 2600 DEG C of graphitization processing carried out above.
Finally, being sieved by powder body, collection screen blanking obtains finished product.
Comparative example 1
Native graphite fine powder (mean diameter D50 is 5 μm) in embodiment 1.
Comparative example 2
Native graphite fine powder (mean diameter D50 is 7 μm) in embodiment 2.
Comparative example 3
Native graphite fine powder (mean diameter D50 is 6.5 μm) in embodiment 3.
Raw material in above-described embodiment and comparative example, specific targets parameter list 1.
Table 1
Electrochemical property test
For capacity first and the efficiency performance first of the raw material in inspection embodiment and comparative example, carry out by half-cell method of testing
Test, with above example and the negative material of comparative example: acetylene black: PVDF(Kynoar)=93:3:4(weight ratio), add
Appropriate NMP(N-methyl pyrrolidone) furnishing pulpous state, coat on Copper Foil, be dried through 110 DEG C of vacuum and make negative plate in 8 hours;
With metal lithium sheet for electrode, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1:1:1, and microporous polypropylene membrane is barrier film,
It is assembled into battery.Charging/discharging voltage is 0~2.0V, and charge-discharge velocity is 0.2C, carries out battery performance testing, test result
It is shown in Table 2.
For the cycle performance of the raw material in inspection embodiment and comparative example, test by the method for testing of full battery, use
Upper embodiment and the negative material of comparative example: SP:SBR(solid content 50%): CMC=94:2.5:1.5:2(weight ratio), add appropriate
Deionized water mix homogeneously furnishing pulpous state, is applied on Copper Foil, and at 90 DEG C, evacuation is dried;By LiFePO4 powder: SP:KS-6:
PVDF=92:3.5:2:2.5(weight ratio), do after solvent mix homogeneously sizes mixing with NMP, be applied on aluminium foil, at 100 DEG C
Evacuation is dried;By dried positive and negative electrode pole piece through roll-in, cut-parts, winding, fluid injection, sealing, formation process, make phosphorus
Acid ferrum lithium power type 4244130 type Soft Roll resultant battery (nominal capacity is 2.5Ah), barrier film is Celgard2400, and electrolyte is
1M LiPF6 DMC:EC:DEC, uses battery check device to be circulated the detection of performance, and test result is shown in Table 2.
Table 2
From table 1, table 2 it can be seen that the negative material properties obtained by each embodiment is superior to comparative example.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert
Being embodied as of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of present inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to the present invention's
Protection domain.
Claims (8)
1. a preparation method for graphite negative material of lithium ion battery, it comprises the steps:
(1) batch mixing: organic carbon source and graphite fine powder are added the blender with heating function by a certain percentage, be stirred continuously to
Mix homogeneously;
(2) high-temperature process: the powder body of mix homogeneously is warming up to 500~1100 DEG C, and constant temperature 3~10 hours, be subsequently cooled to
Room temperature;
(3) graphitization processing: by the material after high-temperature process 2600 DEG C of graphitization processing carried out above;
(4) screening: being sieved by the powder body after graphitization processing, collection screen blanking obtains finished product.
2. according to the preparation method of a kind of graphite negative material of lithium ion battery described in claim 1, it is characterised in that: step
Suddenly the organic carbon source in (1) is asphalt, coal tar pitch, phenolic resin, polrvinyl chloride, polystyrene, phenolic resin, asphalt mixtures modified by epoxy resin
One or more of fat.
3. according to the preparation method of a kind of graphite negative material of lithium ion battery described in claim 1, it is characterised in that: step
Suddenly during the graphite fine powder in (1) is petroleum coke micropowder, needle coke micropowder, pitch coke micropowder, mesophase micropowder, native graphite micropowder
One or more, graphite fine powder mean diameter D50 is 2~10 μm.
4. according to the preparation method of a kind of graphite negative material of lithium ion battery described in claim 1, it is characterised in that: step
Suddenly in (1), the weight ratio of graphite fine powder and organic carbon source is 10:(1~4).
5. according to the preparation method of a kind of graphite negative material of lithium ion battery described in claim 1, it is characterised in that: step
Suddenly the agitating heating temperature in (1) is 50~300 DEG C, and mixing time is 1~12 hour.
6. according to the preparation method of a kind of graphite negative material of lithium ion battery described in claim 1, it is characterised in that: step
Suddenly the heating rate of (2) is 0.5~5 DEG C/min, and cooling is to naturally cool to 200~300 DEG C, then forces to be cooled to room temperature.
7. according to the preparation method of a kind of graphite negative material of lithium ion battery described in claim 1, it is characterised in that: step
Suddenly (2) and (3) are carried out under non-oxide protective atmosphere, are to be passed through the noble gases such as nitrogen in preparation process to protect
Protecting, its gas flow is 5~30L/min.
8. according to the preparation method of a kind of graphite negative material of lithium ion battery described in claim 1, it is characterised in that: step
Suddenly the minus mesh collected through screening in (4), its mean diameter D50 is 8~25 μm.
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Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106654269A (en) * | 2017-01-06 | 2017-05-10 | 江西紫宸科技有限公司 | Graphite negative electrode material used for power lithium ion battery and preparation method and application of graphite negative electrode material |
CN106675054A (en) * | 2017-01-04 | 2017-05-17 | 赣州市瑞富特科技有限公司 | Blend asphalt for coating graphite anode material |
WO2017206544A1 (en) * | 2016-06-03 | 2017-12-07 | 田东 | Method for preparing artificial graphite anode material for lithium ion battery |
CN107619047A (en) * | 2017-09-22 | 2018-01-23 | 江苏亮盈科技股份有限公司 | A kind of preparation method of the compound ion cathode material lithium of isotropism |
CN107808955A (en) * | 2017-10-27 | 2018-03-16 | 湖南工业大学 | A kind of absorbent charcoal material with spherical structure and its preparation method and application |
CN107845810A (en) * | 2017-10-26 | 2018-03-27 | 深圳市斯诺实业发展股份有限公司 | A kind of soft or hard carbon of lithium ion battery is modified the preparation method of negative material |
CN108231423A (en) * | 2017-12-08 | 2018-06-29 | 上海奥威科技开发有限公司 | Lithium-ion capacitor negative material particle and preparation method thereof |
CN109265166A (en) * | 2018-12-10 | 2019-01-25 | 江苏省陶瓷研究所有限公司 | A method of preparing injection moulding zirconia ceramics feeding |
CN109956471A (en) * | 2019-04-26 | 2019-07-02 | 溧阳紫宸新材料科技有限公司 | The process for being granulated or coating for graphite cathode material |
CN110407189A (en) * | 2019-07-04 | 2019-11-05 | 山西沁新能源集团股份有限公司 | Coal needle coke and preparation method thereof, lithium ion battery negative material and lithium ion battery |
CN110600715A (en) * | 2019-10-17 | 2019-12-20 | 石家庄尚太科技有限公司 | Graphite cathode composite material of lithium ion battery and preparation method thereof |
CN111653739A (en) * | 2020-04-28 | 2020-09-11 | 万向一二三股份公司 | Method for preparing high-cycle-performance SiO negative electrode material of lithium battery |
CN113488635A (en) * | 2021-05-24 | 2021-10-08 | 长沙矿冶研究院有限责任公司 | Isotropic heat treatment negative electrode material coating method and preparation method of long-cycle negative electrode material |
CN114628650A (en) * | 2021-09-06 | 2022-06-14 | 万向一二三股份公司 | Material for improving quick charge performance of lithium ion battery and preparation method thereof |
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CN109956471A (en) * | 2019-04-26 | 2019-07-02 | 溧阳紫宸新材料科技有限公司 | The process for being granulated or coating for graphite cathode material |
CN110407189A (en) * | 2019-07-04 | 2019-11-05 | 山西沁新能源集团股份有限公司 | Coal needle coke and preparation method thereof, lithium ion battery negative material and lithium ion battery |
CN110407189B (en) * | 2019-07-04 | 2020-08-21 | 山西沁新能源集团股份有限公司 | Coal needle coke and preparation method thereof, lithium ion battery cathode material and lithium ion battery |
CN110600715A (en) * | 2019-10-17 | 2019-12-20 | 石家庄尚太科技有限公司 | Graphite cathode composite material of lithium ion battery and preparation method thereof |
CN110600715B (en) * | 2019-10-17 | 2021-06-04 | 石家庄尚太科技股份有限公司 | Graphite cathode composite material of lithium ion battery and preparation method thereof |
CN111653739A (en) * | 2020-04-28 | 2020-09-11 | 万向一二三股份公司 | Method for preparing high-cycle-performance SiO negative electrode material of lithium battery |
CN113488635A (en) * | 2021-05-24 | 2021-10-08 | 长沙矿冶研究院有限责任公司 | Isotropic heat treatment negative electrode material coating method and preparation method of long-cycle negative electrode material |
CN114628650A (en) * | 2021-09-06 | 2022-06-14 | 万向一二三股份公司 | Material for improving quick charge performance of lithium ion battery and preparation method thereof |
CN114628650B (en) * | 2021-09-06 | 2024-01-05 | 万向一二三股份公司 | Material for improving quick charge performance of lithium ion battery and preparation method thereof |
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