CN113054179B - Double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material and preparation method and application thereof - Google Patents

Double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material and preparation method and application thereof Download PDF

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CN113054179B
CN113054179B CN202110312402.5A CN202110312402A CN113054179B CN 113054179 B CN113054179 B CN 113054179B CN 202110312402 A CN202110312402 A CN 202110312402A CN 113054179 B CN113054179 B CN 113054179B
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asphalt
silicon
negative electrode
electrode material
double
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CN113054179A (en
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张亚光
王振
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Zhejiang Lichen New Material Technology Co ltd
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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
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method of a double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material, which is characterized in that nano silicon CVD is deposited on shaping graphite, then an outer carbon source is coated with a layer of intermediate phase carbon with controllable thickness through the thermal polycondensation reaction of asphalt, and the double-layer asphalt is coated, so that the nano silicon can be better coated, the nano silicon is prevented from being exposed and directly contacted with an electrolyte, the technical problems in the prior art are thoroughly solved, and the obtained composite silicon carbon material has high first effect, good cycle performance and good multiplying power; in terms of mechanism, the silicon-carbon material coated with the asphalt with different particle sizes for many times has good coating layer associativity, good coating effect, uniformity, stability and good conductivity after carbonization, is very beneficial to the migration of lithium ions, improves the high-rate discharge capacity and obviously improves the cycle performance.

Description

Double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material and preparation method and application thereof
Technical Field
The invention relates to the technical field of battery cathode materials, in particular to a double-particle-size asphalt multi-coating shaping graphite silicon carbon cathode material and a preparation method and application thereof.
Background
The most advanced lithium ion batteries at present have failed to meet the increasing demand for electric vehicles and large-scale energy batteries. Silicon is considered to be the most promising candidate for replacing graphite. It is the second most abundant element in the earth crust, is environment-friendly and has ultrahigh theoretical capacity (4200 mAh/g). At present, most silicon-carbon cathode materials in the market have more silicon coating methods of hot melt agent carbonization, and single coating is common, but the single carbon coating has the defects that a carbon layer is thin, the carbon layer is easy to expand and break due to volume expansion of silicon in a circulation process, and direct contact between the silicon and electrolyte causes capacity loss and potential safety hazard; in addition, the single carbon coating has unsatisfactory coating effect on porous graphite, the coating on micropores and mesopores is complete, and macropores are exposed, and the multiple coating has the advantage that the asphalt with different particle sizes can meet the coating requirement of the porous graphite.
Patent document CN110571424A discloses a method for preparing a silicon carbon material from nano silicon shaped graphite by spheroidizing equipment, wherein nano silicon is difficult to be compounded with shaped graphite, nano silicon is easy to fall off in subsequent processes, and the material has poor conductivity without being coated with soft carbon such as pitch. Poor rate multiplying performance and low first effect.
Disclosure of Invention
The invention aims to provide a double-particle-size pitch multi-coating shaping graphite silicon carbon negative electrode material and a preparation method and application thereof.
In order to achieve the above object, in a first aspect, the present invention provides a method for preparing a graphite silicon carbon anode material with double-particle-size pitch by multiple coating shaping, which is characterized by comprising the following steps:
(1) placing the shaped graphite with the average grain diameter of 15-22 mu m of D50 in a chemical vapor deposition furnace, pumping to a vacuum state, filling inert protective gas at the rate of 10-100L/h, heating to 400-1000 ℃ at the rate of 1-15 ℃/min, heating to a set temperature, filling silicon source gas at the rate of 10-100L/h, keeping the temperature for 0.5-10h, closing a silicon source gas pipeline, entering an automatic cooling program, cooling to normal temperature, and taking out to obtain the shaped graphite for depositing the nano silicon;
(2) uniformly stirring and mixing the shaped graphite deposited with the silicon in the step (1) with the asphalt at the stirring speed of 500-1000r/min for 10-30min, and keeping the temperature to room temperature along with the stable temperature of circulating water; the mass percentage of the nano silicon deposition is 0.5-10 percent and the mass percentage of the asphalt is 1-10 percent based on the total amount of the shaping graphite;
(3) putting the mixture in the step (2) into a tank type atmosphere furnace for asphalt carbonization reaction, opening a vacuum pump, pumping the furnace to negative pressure of-0.05 to-0.1 MPa, backfilling protective gas until positive pressure is 0-0.1MPa and gas flow is 20-80L/min, setting a heating program, heating at 3-5 ℃/min, respectively keeping at 200 ℃, 350 ℃ for 30-60min and at 800-;
(4) and (3) crushing and grinding the carbonized product in the step (3), sieving the crushed carbonized product by a 600-mesh and 800-mesh sieve, placing the crushed carbonized product in a mixer for stirring, adding asphalt with the average particle size of 5-10 mu m in an equal proportion D50, repeating the step (3) when the stirring condition is consistent with that in the step (2), and taking out the crushed and sieved shaped graphite silicon carbon negative electrode material coated with the asphalt for multiple times after cooling to room temperature.
Preferably, in the step (1), the average particle size of the shaped graphite D50 is specifically 15-20 μm, and the silicon source gas is one or a mixture of more of silane, dichlorosilane, trichlorosilane, and silicon tetrachloride.
Preferably, in the step (1), the average particle size of the post-deposition shaped graphite D50 is 17-20 μm.
Preferably, in the step (2), the asphalt is one of mesophase asphalt and clean coal asphalt.
Preferably, in the step (2), the asphalt D50 has an average particle size of 3-5 μm.
Preferably, in the step (2), the asphalt is purified coal asphalt, the ash content of the purified coal asphalt is less than 100ppm, the quinoline insoluble content of the purified coal asphalt is not higher than 30 percent, and the softening point of the purified coal asphalt is 60-150 ℃.
Preferably, in the step (2), the asphalt is mesophase asphalt, and the mesophase asphalt comprises naphthalene series, petroleum series and coal series, the relative molecular weight is 400-6000, the content of the wide range mesophase is more than 80%, and the softening point is 200-320 ℃.
Preferably, in step (3), the protective gas is one or more of nitrogen, helium, xenon, radon, neon and argon.
In a second aspect, the technical scheme of the present invention provides a double-particle-size pitch multi-coating shaping graphite silicon carbon negative electrode material prepared by the preparation method in any one of the above technical schemes.
In a third aspect, the technical solution of the present invention provides an application of the double-particle-size pitch multi-coating shaping graphite silicon carbon negative electrode material as a negative electrode material of a lithium ion battery.
In summary, the technical scheme of the preparation method of the graphite silicon carbon anode material with double-particle-size asphalt for multiple coating and shaping has the following beneficial effects: according to the invention, the nano-silicon CVD is deposited on the shaping graphite, then the outer carbon source is coated with a layer of intermediate phase carbon with controllable thickness through the thermal polycondensation reaction of the asphalt, and the double-layer asphalt coating can better coat the nano-silicon to avoid the exposure of the nano-silicon and directly contact with the electrolyte, so that the technical problems in the prior art are thoroughly solved, and the obtained composite silicon-carbon material has high first-effect, good cycle performance and good multiplying power. In terms of mechanism, the silicon-carbon material coated with the asphalt with different particle sizes for many times has good coating layer associativity, good coating effect, uniformity, stability and good conductivity after carbonization, is very beneficial to the migration of lithium ions, improves the high-rate discharge capacity and obviously improves the cycle performance.
In order to make the present invention and other objects, advantages, features and functions more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a comparison of the graphitic silicon carbon anode materials prepared in example 1 and comparative example 1, a is the dual particle size pitch coated graphitic silicon carbon anode material prepared in example 1; b is the graphite silicon carbon negative electrode material coated by single-grain size asphalt in comparative example 1;
fig. 2 is a graph of capacity retention after 100 cycles of examples 1 and 2 and comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a preparation method of a double-particle-size pitch multi-coating shaping graphite silicon carbon negative electrode material.
Example 1
The embodiment 1 provides a method for preparing a graphite silicon carbon anode material with double-particle-size pitch for multiple coating and shaping, which specifically comprises the following steps:
(1) placing shaped graphite (1600 g) with the average grain diameter of 17 mu m of D50 in a chemical vapor deposition furnace, pumping to a vacuum state, filling nitrogen at the rate of 12L/h, heating to 420 ℃ at the rate of 8 ℃/min, filling silane at the rate of 25L/h after heating to 420 ℃, carrying out program heat preservation for 2h, closing a silicon source gas pipeline, entering an automatic cooling program, cooling to normal temperature, and taking out to obtain the shaped graphite for depositing nano silicon;
(2) 900g of shaping graphite of deposited silicon is mixed with 100g of mesophase pitch, the average grain diameter of D50 is 5.72 mu m, the rotating speed is 900r/min, the stirring time is 20min, the temperature is kept to the room temperature along with the stable temperature of circulating water, and the shaping graphite is taken out after the material mixing is finished;
(3) putting the mixture in the step (2) into a tank-type atmosphere furnace for pitch carbonization reaction, opening a vacuum pump, pumping the furnace to negative pressure (-0.1 MPa), backfilling nitrogen gas until positive pressure is 0.1MPa, wherein the gas flow is 80L/min, setting a heating program, heating at 3 ℃/min, respectively keeping the temperature at 200 ℃, 350 ℃ for 60min and 900 ℃ for 180 min;
(4) and (3) crushing and grinding the carbonized product obtained in the step (3), sieving the crushed carbonized product through a 800-mesh sieve, placing the crushed carbonized product into a mixer, adding 111g of mesophase pitch into the mixer, wherein the average particle size of D50 is 10.27 mu m, stirring the mixture under the condition consistent with that of the step (2), repeating the step (3), and taking out the crushed and sieved shaped graphite silicon carbon negative electrode material coated with the pitch for multiple times after cooling to room temperature.
Example 2
The embodiment 1 provides a method for preparing a graphite silicon carbon anode material with double-particle-size pitch for multiple coating and shaping, which specifically comprises the following steps:
(1) placing shaped graphite (1600 g) with the average grain diameter of 17 mu m of D50 in a chemical vapor deposition furnace, pumping to a vacuum state, filling nitrogen at the rate of 12L/h, heating to 420 ℃ at the rate of 8 ℃/min, filling silane at the rate of 25L/h after heating to 420 ℃, carrying out program heat preservation for 2h, closing a silicon source gas pipeline, entering an automatic cooling program, cooling to normal temperature, and taking out to obtain the shaped graphite for depositing nano silicon;
(2) 900g of shaping graphite of deposited silicon is mixed with 100g of mesophase pitch, the average grain diameter of D50 is 10.27 mu m, the rotating speed is 900r/min, the stirring time is 20min, the temperature is kept to the room temperature along with the stable temperature of circulating water, and the shaping graphite is taken out after the material mixing is finished;
(3) putting the mixture in the step (2) into a tank type atmosphere furnace for pitch carbonization reaction, opening a vacuum pump, pumping the furnace to negative pressure (-0.1 MPa), backfilling nitrogen gas until positive pressure is 0.1MPa, wherein the gas flow is 80L/min, setting a heating program, heating at 3 ℃/min, and respectively keeping the temperature at 200 ℃, 350 ℃ for 60min and at 800-;
(4) and (3) crushing and grinding the carbonized product obtained in the step (3), sieving the crushed carbonized product through a 800-mesh sieve, placing the crushed carbonized product into a mixer, adding 111g of mesophase pitch into the mixer, wherein the average particle size of D50 is 5.72 mu m, stirring the mixture under the condition consistent with that of the step (2), repeating the step (3), and taking out the crushed and sieved shaped graphite silicon carbon negative electrode material coated with the pitch for multiple times after cooling to room temperature.
Comparative example 1
The comparative example 1 provides a preparation method of a graphite silicon carbon anode material with double-particle-size asphalt coated and shaped for multiple times, which specifically comprises the following steps:
(1) placing shaped graphite (1600 g) with the average grain diameter of 17 mu m of D50 in a chemical vapor deposition furnace, pumping to a vacuum state, filling nitrogen at the rate of 12L/h, heating to 420 ℃ at the rate of 8 ℃/min, filling silane at the rate of 25L/h after heating to 420 ℃, carrying out program heat preservation for 2h, closing a silicon source gas pipeline, entering an automatic cooling program, cooling to normal temperature, and taking out to obtain the shaped graphite for depositing nano silicon;
(2) mixing 800g of the silicon-deposited reshaping graphite with 200g of mesophase pitch, wherein the average grain diameter of D50 is 5.72 mu m, the rotating speed is 900r/min, the stirring time is 20min, the temperature is kept to room temperature along with the stable temperature of circulating water, and the silicon-deposited reshaping graphite is taken out after the material mixing is finished;
(3) and (3) putting the mixture obtained in the step (2) into a tank-type atmosphere furnace for pitch carbonization reaction, opening a vacuum pump, pumping the furnace to negative pressure (-0.1 MPa), backfilling nitrogen gas until positive pressure is 0.1MPa, setting a heating program, heating at 3 ℃/min, keeping the temperature at 200 ℃, 350 ℃ for 60min and at 800-900 ℃ for 180min, respectively, and taking out, grinding, crushing and screening the mixture to obtain the multi-pitch-coated shaped graphite silicon carbon negative electrode material after cooling to room temperature.
Application example
In the preparation of all pole pieces, carbon black (SP) is used as a conductive agent, sodium carboxymethyl cellulose (CMC) is used as a binder, and the mass ratio of the conductive agent to the synthesized active material is 1: 1: 8, mixing and dissolving the mixture in deionized water and a small amount of alcohol, and magnetically stirring for more than 8 hours to prepare uniformly dispersed battery slurry for later use. And (3) uniformly coating the battery slurry on the surface of an electrode (the cut foam copper or copper foil), carrying out vacuum drying at 85 ℃ for 12h, tabletting and weighing for later use. The electrochemical performance of the electrodes was tested by assembling a button-type half cell (CR 2025) using a glove box (model Mbraun) from Labstar, Germany. The button half cell assembly completely adopts a lithium sheet as a counter electrode, a foam nickel sheet as a buffer gasket, and the water oxygen content of the manufacturing environment is respectively as follows: water concentration < 2 ppm, oxygen concentration < 2 ppm. The electrolyte used was 1M LiPF6 dissolved in EC and DMC organic solvents. Cell cycle formation was tested on novice devices.
Examples 1-2 and comparative example 1 were characterized by the following method
The morphology of the electron microscope image of the invention is tested by adopting American Saimer Feishell Phonomation 5
The specific surface area was tested using a Tristar3020 full-automatic specific surface area and porosity analyzer from Mac instruments USA.
TABLE 1 characterization test result of double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material
First discharge capacity (mAh/g) First effect (%) Capacity retention ratio at 100 weeks (%) BET（m2/g）
Example 1 620 92 89.8 1.3325
Example 2 609 90.2 88.2 1.3513
Comparative example 1 587 88.5 81.4 2.2411
Referring to fig. 1-2 and table 1, it can be seen from examples 1-2 and comparative example 1 that the mesophase pitch-coated composite silicon carbon material has high first efficiency and good cycle performance. By comparing fig. 1, it can be found that asphalt with different particle sizes can be completely coated on the surface of the silicon-carbon material by multiple coating, and the specific surface area is combined, so that the effect of coating silicon on the graphite surface of the embodiment is stronger than that of the comparative example 1.
According to the preparation method of the double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material, the nano silicon CVD is deposited on the shaping graphite, the outer carbon source is coated with the intermediate phase carbon with controllable thickness through the thermal polycondensation reaction of the asphalt, the double-layer asphalt is coated, the nano silicon can be better coated, the nano silicon is prevented from being exposed and directly contacted with the electrolyte, the technical problems in the prior art are thoroughly solved, and the obtained composite silicon carbon material is high in first effect, good in cycle performance and good in multiplying power. In terms of mechanism, the silicon-carbon material coated with the asphalt with different particle sizes for many times has good coating layer associativity, good coating effect, uniformity, stability and good conductivity after carbonization, is very beneficial to the migration of lithium ions, improves the high-rate discharge capacity and obviously improves the cycle performance.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (6)

1. A preparation method of a double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material is characterized by comprising the following steps of:
(1) placing the shaped graphite with the average grain diameter of 15-22 mu m of D50 in a chemical vapor deposition furnace, pumping to a vacuum state, filling inert protective gas at the rate of 10-100L/h, heating to 400-1000 ℃ at the rate of 1-15 ℃/min, heating to a set temperature, filling silicon source gas at the rate of 10-100L/h, keeping the temperature for 0.5-10h, closing a silicon source gas pipeline, entering an automatic cooling program, cooling to normal temperature, and taking out to obtain the shaped graphite for depositing the nano silicon;
(2) uniformly stirring and mixing the shaped graphite deposited with the silicon in the step (1) with the asphalt at the stirring speed of 500-1000r/min for 10-30min, and keeping the temperature to room temperature along with the stable temperature of circulating water; the nano silicon deposition mass percentage is 0.5-10 percent, the asphalt mass percentage is 1-10 percent, and the average grain diameter of the asphalt D50 is 3-5 mu m; the asphalt is mesophase asphalt, and the mesophase asphalt comprises naphthalene series, petroleum series and coal series, the relative molecular weight of the mesophase asphalt is 400-6000, the content of the wide-area mesophase is more than 80 percent, and the softening point is 200-320 ℃;
(3) putting the mixture in the step (2) into a tank type atmosphere furnace for asphalt carbonization reaction, opening a vacuum pump, pumping the furnace to negative pressure of-0.05 to-0.1 MPa, backfilling protective gas until positive pressure is 0-0.1MPa and gas flow is 20-80L/min, setting a heating program, heating at 3-5 ℃/min, respectively keeping at 200 ℃, 350 ℃ for 30-60min and at 800-;
(4) and (3) crushing and grinding the carbonized product in the step (3), sieving the crushed carbonized product by a 600-mesh and 800-mesh sieve, placing the crushed carbonized product in a mixer for stirring, adding asphalt with the average particle size of 5-10 mu m in an equal proportion D50, repeating the step (3) when the stirring condition is consistent with that in the step (2), and taking out the crushed and sieved shaped graphite silicon carbon negative electrode material coated with the asphalt for multiple times after cooling to room temperature.
2. The method for preparing the double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material as claimed in claim 1, wherein in the step (1), the average particle size of the shaping graphite D50 is 15-20 μm; the silicon source gas is one or a mixture of silane, dichlorosilane, trichlorosilane and silicon tetrachloride.
3. The method for preparing the double-particle-size asphalt multi-coating shaped graphite silicon carbon negative electrode material as claimed in claim 1, wherein in the step (1), the average particle size of the shaped graphite D50 is 17-20 μm.
4. The method for preparing the double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material as claimed in claim 1, wherein in the step (3), the protective gas is one or more of nitrogen, helium, xenon, radon, neon and argon.
5. The double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material prepared by the preparation method of any one of claims 1 to 4.
6. The use of the double-particle-size pitch multi-coating shaped graphitic silicon carbon negative electrode material according to claim 5 as a negative electrode material of a lithium ion battery.
CN202110312402.5A 2021-03-24 2021-03-24 Double-particle-size asphalt multi-coating shaping graphite silicon carbon negative electrode material and preparation method and application thereof Active CN113054179B (en)

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