CN111403706A - High-gram-volume low-specific-surface-area lithium battery silicon-carbon negative electrode material and preparation method thereof - Google Patents

High-gram-volume low-specific-surface-area lithium battery silicon-carbon negative electrode material and preparation method thereof Download PDF

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CN111403706A
CN111403706A CN202010208125.9A CN202010208125A CN111403706A CN 111403706 A CN111403706 A CN 111403706A CN 202010208125 A CN202010208125 A CN 202010208125A CN 111403706 A CN111403706 A CN 111403706A
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silicon
negative electrode
electrode material
stirring
mixed solution
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李婷
冯苏宁
刘芳
李辉
顾华清
袁树兵
***
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Liyang Zichen 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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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 lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area and a preparation method thereof, wherein the preparation method comprises the following steps: adding deionized water into a beater; adding carboxyl CMC into deionized water, and stirring for 0.5-1 hour to form a first mixed solution; adding graphite into the first mixed solution, and stirring for 1-2 hours to form a second mixed solution; the second mixed solution comprises the following components in percentage by mass: graphite 0.5: 100-1.5: 100, respectively; adding the nano silicon slurry with the fourth mass into the second mixed solution, and stirring for 3-5 hours to form a third mixed solution; in the third mixed solution, the solid content of the nano silicon slurry is 6-10 percent; graphite according to mass ratio: silicon is 3:1 to 6: 1; the solid content of the third mixed solution is between 12.86 and 30.86 percent; and carrying out spray drying on the third mixed solution to prepare a powder mesh sieve, thus obtaining the lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area.

Description

High-gram-volume low-specific-surface-area lithium battery silicon-carbon negative electrode material and preparation method thereof
Technical Field
The invention relates to the technical field of battery material preparation methods, in particular to a lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area and a preparation method thereof.
Background
With the rapid popularization of lithium ion batteries in the industrial field, the requirements for high power density and high energy density are increasingly prominent.
At present, the negative electrode material of the lithium ion battery mainly takes graphite, the theoretical capacity (372mAh/g) of the negative electrode material is low, and compared with the theoretical capacity (4200mAh/g) of silicon, the negative electrode material has the advantages of good safety performance, low discharge voltage and the like. Therefore, the silicon-carbon anode material has better performance advantages, and the research and development requirements are imminent.
However, in the preparation process of the silicon-carbon cathode material, silicon is easy to agglomerate, so that the defects of large specific surface area and the like are caused. How to reduce the specific surface area of the silicon-carbon negative electrode negative material has become the focus of research in the industry.
Disclosure of Invention
The invention provides a lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area and a preparation method thereof. Adding graphite into deionized water added with a CMC thickener, stirring uniformly, adding the nano silicon slurry, stirring uniformly again, and then preparing the silicon-carbon cathode material of the lithium ion battery by spray drying, roasting in a CVD furnace and sieving. The prepared silicon-carbon negative electrode material has the advantages of uniform particle size distribution, high gram volume and low specific surface area, and the preparation method is simple in preparation process, convenient to operate and convenient for commercial popularization.
In view of the above, in a first aspect, an embodiment of the present invention provides a method for preparing a high-gram-capacity low-specific-surface-area lithium battery silicon-carbon negative electrode material, including:
adding a first mass of deionized water into a beater;
adding carboxymethyl cellulose CMC of a second mass into deionized water, and stirring for 0.5-1 hour to form a first mixed solution;
adding graphite with a third mass into the first mixed solution, and stirring for 1-2 hours to form a second mixed solution; wherein the Dv50 of the graphite is 8-15 um; in the second mixed solution, the mass ratio of CMC: graphite 0.5: 100-1.5: 100, respectively;
adding the nano silicon slurry with the fourth mass into the second mixed solution, and stirring for 3-5 hours to form a third mixed solution; wherein, in the nano silicon slurry, the solute is nano silicon with Dv50 of 40-100 nm, the solvent is isopropanol, and the solid content of the nano silicon slurry is 6-10%; in the third mixed solution, the mass ratio of graphite: silicon is 3:1 to 6: 1; the solid content of the third mixed solution is between 12.86 and 30.86 percent;
spray drying the third mixed solution to prepare powder to obtain a first mixture;
placing the first mixture into a Chemical Vapor Deposition (CVD) furnace, and roasting at 800-900 ℃ to obtain a second mixture, wherein the roasting comprises a heating process, a heat preservation process and a cooling process, nitrogen is introduced in the heating process, the flow rate is 10-15L/min, the heating rate is 5-10 ℃/min, nitrogen and acetylene are introduced in the heat preservation process, the flow rate of the introduced nitrogen is 3-6L/min, the flow rate of the introduced acetylene is 1-2L/min, the heat preservation time is 3-4 hours, the cooling process is that the nitrogen is introduced for natural cooling, and the flow rate of the introduced nitrogen is 3-6L/min;
and (3) sieving the second mixture by using a 300-mesh sieve to obtain the lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area.
Preferably, in the spray drying powder preparation process, the air inlet temperature is 180-210 ℃, and the air exhaust temperature is 110-150 ℃.
Preferably, the graphite is expanded graphite.
Preferably, the first and second liquid crystal materials are,
the stirring is specifically as follows:
stirring is carried out at a revolution speed of 20-40r/min and a rotation speed of 2000-2500 r/min.
In a second aspect, the embodiment of the present invention provides a lithium battery silicon carbon negative electrode material with high gram capacity and low specific surface area, which is prepared by the preparation method of the lithium battery silicon carbon negative electrode material with high gram capacity and low specific surface area described in the first aspect.
According to the preparation method of the lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area, provided by the embodiment of the invention, graphite is added into deionized water added with a CMC thickener and is uniformly stirred, then nano silicon slurry is added and is uniformly stirred again, and then the lithium battery silicon-carbon negative electrode material is prepared through spray drying, roasting in a CVD furnace and sieving.
By adding CMC, the viscosity of the solution is increased, the added graphite is dispersed to prevent agglomeration, and the high-speed dispersion is carried out by using a beater when the nano silicon is added, so that the nano silicon is better dispersed on the surface of the graphite, and particularly, under the condition of high addition of the graphite silicon, the effect of the nano silicon can be more prominent, and the agglomeration of the silicon is effectively avoided. The silicon-carbon negative electrode material prepared by the method has the advantages of uniform particle size distribution, high gram volume and low specific surface area, and the preparation method is simple in preparation process, convenient to operate and convenient for commercial popularization.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
FIG. 1 is a flow chart of a method for preparing a high-gram-capacity low-specific-surface-area lithium battery silicon-carbon negative electrode material according to an embodiment of the present invention;
fig. 2 is an X-ray diffraction (XRD) pattern of the silicon carbon negative electrode material prepared in example 1 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) of the silicon-carbon negative electrode material prepared in example 1 of the present invention;
fig. 4 is a charge-discharge curve at a constant current of 0.1C after a button half cell made of the silicon-carbon negative electrode material prepared in example 1 of the present invention.
Detailed Description
The embodiment of the invention provides a preparation method of a lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area, which is described below by combining a flow chart of the preparation method of the lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area shown in fig. 1.
Referring to fig. 1, the preparation method of the silicon-carbon negative electrode material of the present invention includes the following steps:
step 110, adding deionized water with a first mass into a pulping machine;
step 120, adding carboxymethyl cellulose (CMC) of a second mass into deionized water, and stirring for 0.5-1 hour to form a first mixed solution;
specifically, the revolution speed of stirring is 20-40r/min, the rotation speed is 2000-2500r/min, and the high-speed stirring is adopted in the following preparation process.
Step 130, adding graphite with a third mass into the first mixed solution, and stirring for 1-2 hours to form a second mixed solution;
wherein the Dv50 of the graphite is 8-15 um; in the second mixed solution, the mass ratio of CMC: graphite 0.5: 100-1.5: 100, respectively; the aforementioned second and third masses are added with the respective substances following the requirement of satisfying the mass ratio. In a preferred embodiment, the graphite is in particular expanded graphite.
Step 140, adding the nano silicon slurry with the fourth mass into the second mixed solution, and stirring for 3-5 hours to form a third mixed solution;
in the nano silicon slurry, the solute is 40-100 nm of nano silicon with Dv50, the solvent is isopropanol, and the solid content of the nano silicon slurry is 6-10%.
In the third mixed solution, the mass ratio of graphite: silicon is 3:1 to 6: 1; the solid content of the third mixed solution is between 12.86 and 30.86 percent; the aforementioned first, third and fourth masses are added with the respective substances following the requirement of satisfying the mass ratio.
Step 150, spray drying the third mixed solution to prepare powder to obtain a first mixture;
specifically, in the process of spray drying and pulverizing, the air inlet temperature is 180-210 ℃, and the air exhaust temperature is 110-150 DEG C
Step 160, placing the first mixture into a Chemical Vapor Deposition (CVD) furnace to be roasted at 800-900 ℃ to obtain a second mixture;
the roasting comprises a heating process, a heat preservation process and a cooling process, wherein in the heating process, nitrogen is introduced, the flow rate is 10-15L/min, and the heating rate is 5-10 ℃/min, in the heat preservation process, nitrogen and acetylene are introduced, wherein the flow rate of the introduced nitrogen is 3-6L/min, the flow rate of the introduced acetylene is 1-2L/min, the heat preservation time is 3-4 hours, in the cooling process, the nitrogen is introduced for natural cooling, and the flow rate of the introduced nitrogen is 3-6L/min;
and 170, sieving the second mixture by using a 300-mesh sieve to obtain the lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area.
According to the preparation method of the lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area, provided by the embodiment of the invention, graphite is added into deionized water added with a CMC thickener and is uniformly stirred, then nano silicon slurry is added into the deionized water and is uniformly stirred again, and then the nano silicon slurry is subjected to spray drying, CVD furnace roasting and sieving to prepare the lithium battery silicon-carbon negative electrode material.
By adding CMC, the viscosity of the solution is increased, the added graphite is dispersed to prevent agglomeration, and the high-speed dispersion is carried out by using a beater when the nano silicon is added, so that the nano silicon is better dispersed on the surface of the graphite, and particularly, under the condition of high addition of the graphite silicon, the effect of the nano silicon can be more prominent, and the agglomeration of the silicon is effectively avoided. The silicon-carbon negative electrode material prepared by the method has the advantages of uniform particle size distribution, high gram volume and low specific surface area, and the preparation method is simple in preparation process, convenient to operate and convenient for commercial popularization.
The preparation process of the present invention is further illustrated in detail by the following specific examples.
Example 1
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Fig. 2 is an X-ray diffraction (XRD) pattern of the silicon carbon negative electrode material prepared in example 1 of the present invention, from which XRD diffraction peaks, it can be seen that the peaks of the silicon carbon negative electrode material are diffraction peaks of silicon, indicating that no SiC is generated. Fig. 3 is a Scanning Electron Microscope (SEM) of the silicon-carbon negative electrode material prepared in example 1 of the present invention, and it can be seen from the SEM that the nano-silicon is effectively dispersed on the expanded graphite.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent was as follows:dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC), wherein a mixed electrolyte of 1:1:1:1 is assembled into a CR2025 type button half cell in a vacuum glove box by adopting a polypropylene microporous membrane as a diaphragm, and the cell is discharged to 5mV at a constant current of 0.1C, then discharged to 5mV at a constant current of 0.02C and charged to 1.5V at a constant current of 0.1C.
Fig. 3 is a charge-discharge curve at a constant current of 0.1C after a button half cell made of the silicon-carbon negative electrode material prepared in example 1 of the present invention. The gram capacity is 691.5 mAh/g.
The particle size distribution, specific surface area, gram capacity and first cycle efficiency data obtained by the test of the silicon carbon anode material prepared in the embodiment are shown in the following table 1.
Figure BDA0002421875220000061
TABLE 1
Example 2
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 64.65kg of deionized water and adding into a pulping machine;
b, weighing 60g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 12kg of expanded graphite (Dv50 ═ 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 3
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 84.97kg of deionized water and adding into a pulping machine;
b, weighing 75g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 15kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 4
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
A, weighing 106.3kg of deionized water and adding into a beater;
b, weighing 90g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 18kg of graphite (Dv50 ═ 8.2um) and adding into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Is prepared byMixing the silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 5
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 90g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black(SP) mixing according to the mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on a copper foil, drying the copper foil for 24 hours in vacuum at 80 ℃ to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and using L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 6
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 135g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, and adding NMP (1-methyl-2-pyrrolidone)) Preparing the mixture into slurry, uniformly coating the slurry on a copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare an experimental battery pole piece, and then taking a lithium piece as a counter electrode and using L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 7
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 54.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 30kg of nano-silicon solution with the solid content of 10% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on a copper foil, and performing vacuum coating at 80 DEG CDrying for 24 hours to obtain the experimental battery pole piece, and taking a lithium piece as a counter electrode and using L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 8
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 20r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on a copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare the battery pole piece for experiments. Then using lithium sheet as counter electrodeUsing L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 9
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 20r/min, rotating for 2000r/min, and stirring for 30 min;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6A four-component mixed solvent according to carbonic acidEthylene Ester (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC), wherein the mixed electrolyte is 1:1:1:1, a polypropylene microporous membrane is used as a diaphragm, a CR2025 type button half cell is assembled in a vacuum glove box, and the button half cell is discharged to 5mV at a constant current of 0.1C, then discharged to 5mV at a constant current of 0.02C and charged to 1.5V at a constant current of 0.1C.
Example 10
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 1 hour;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared from Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC), and fluoro carbonAnd (3) assembling a CR2025 type button half cell in a vacuum glove box by using a polypropylene microporous membrane as a diaphragm, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 11
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 2 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by mixing Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) with 1:1:1:1, and using polypropylene microporous membraneThe diaphragm is assembled into a CR2025 button half cell in a vacuum glove box, and the cell is discharged to 5mV at a constant current of 0.1C, then discharged to 5mV at a constant current of 0.02C, and charged to 1.5V at a constant current of 0.1C.
Example 12
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of graphite (Dv50 ═ 8.2um) and adding the graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 4 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by assembling CR2025 type button half-cell in a vacuum glove box by using a polypropylene microporous membrane as a diaphragm according to an electrolyte mixed by Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) in a ratio of 1:1:1:1,and discharged to 5mV at constant current 0.1C, then discharged to 5mV at constant current 0.02C, and charged to 1.5V at constant current 0.1C.
Example 13
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 100nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent adopts an electrolyte mixed by Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) in a ratio of 1:1:1:1, adopts a polypropylene microporous membrane as a diaphragm, is assembled into a CR2025 type button half cell in a vacuum glove box, and discharges to 5mV at a constant current of 0.1C and then discharges to 5mV at a constant current of 0.02C0.1C to 1.5V.
Example 14
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 210 ℃ and the air outlet temperature is 150 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 15
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 15L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 16
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen to evacuate the CVD furnace for 1.5 hours, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 17
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 210 ℃ and the air outlet temperature is 150 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 900 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 18
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 10 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 19
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen to evacuate the CVD furnace for 1.5 hours, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 4 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 20
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 6L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 6L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 21
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
Weighing 44.31kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 900 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 2L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 22
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
A, weighing 52.65kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 ═ 15um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
Example 23
The embodiment provides a preparation method of a silicon-carbon negative electrode material for a lithium ion battery.
A, weighing 14.63kg of deionized water and adding into a pulping machine;
b, weighing 45g of CMC, adding into the beater, revolving for 40r/min, rotating for 2500r/min, and stirring for 30 min;
c, weighing 9kg of expanded graphite (Dv50 is 8.2um) and adding the expanded graphite into the beater in the step B, and stirring for 1.5 hours;
d, adding 40kg of nano-silicon solution with the solid content of 7.5% into the mixture obtained in the step C, wherein the Dv50 of the nano-silicon is 40nm, the organic solvent in the nano-silicon solution is isopropanol, and stirring for 3 hours;
e: d, spray drying the mixture obtained in the step D, wherein the air inlet temperature is 180 ℃, and the air exhaust temperature is 110 ℃;
f, roasting the mixture obtained in the step E in a CVD furnace at a nitrogen flow rate of 10L/min, introducing nitrogen, exhausting the CVD furnace for 1 hour, heating to 800 ℃ at a heating rate of 5 ℃/min, simultaneously introducing nitrogen and acetylene at a nitrogen flow rate of 3L/min and an acetylene flow rate of 1L/min, preserving heat for 3 hours, closing the acetylene, and naturally cooling under the condition of the nitrogen flow rate of 3L/min;
and G, sieving the mixture obtained after cooling in the step F by using a 300-mesh sieve to obtain the silicon-carbon negative electrode material for the lithium ion battery.
Mixing the prepared silicon-carbon negative electrode material with a binder CMC, Styrene Butadiene Rubber (SBR) and conductive carbon black (SP) according to a mass ratio of 70:10:10:10, preparing the mixture into slurry by using NMP (1-methyl-2-pyrrolidone), uniformly coating the slurry on copper foil, and performing vacuum drying at 80 ℃ for 24 hours to prepare a battery pole piece for experiments, and then using a lithium piece as a counter electrode and L iPF of 1.1 mol/L6The four-component mixed solvent is prepared by adopting a mixed electrolyte of Ethylene Carbonate (EC), dimethyl carbonate (DMC), Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) as 1:1:1:1, adopting a polypropylene microporous membrane as a diaphragm, assembling into a CR2025 type button half cell in a vacuum glove box, and discharging to 5mV at a constant current of 0.1C, then discharging to 5mV at a constant current of 0.02C, and charging to 1.5V at a constant current of 0.1C.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (5)

1. A preparation method of a lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area is characterized by comprising the following steps:
adding a first mass of deionized water into a beater;
adding carboxymethyl cellulose CMC of a second mass into deionized water, and stirring for 0.5-1 hour to form a first mixed solution;
adding graphite with a third mass into the first mixed solution, and stirring for 1-2 hours to form a second mixed solution; wherein the Dv50 of the graphite is 8-15 um; in the second mixed solution, the mass ratio of CMC: graphite 0.5: 100-1.5: 100, respectively;
adding the nano silicon slurry with the fourth mass into the second mixed solution, and stirring for 3-5 hours to form a third mixed solution; wherein, in the nano silicon slurry, the solute is nano silicon with Dv50 of 40-100 nm, the solvent is isopropanol, and the solid content of the nano silicon slurry is 6-10%; in the third mixed solution, the mass ratio of graphite: silicon is 3:1 to 6: 1; the solid content of the third mixed solution is between 12.86 and 30.86 percent;
spray drying the third mixed solution to prepare powder to obtain a first mixture;
placing the first mixture into a Chemical Vapor Deposition (CVD) furnace, and roasting at 800-900 ℃ to obtain a second mixture, wherein the roasting comprises a heating process, a heat preservation process and a cooling process, nitrogen is introduced in the heating process, the flow rate is 10-15L/min, the heating rate is 5-10 ℃/min, nitrogen and acetylene are introduced in the heat preservation process, the flow rate of the introduced nitrogen is 3-6L/min, the flow rate of the introduced acetylene is 1-2L/min, the heat preservation time is 3-4 hours, the cooling process is that the nitrogen is introduced for natural cooling, and the flow rate of the introduced nitrogen is 3-6L/min;
and (3) sieving the second mixture by using a 300-mesh sieve to obtain the lithium battery silicon-carbon negative electrode material with high gram capacity and low specific surface area.
2. The preparation method of claim 1, wherein the air inlet temperature is 180 ℃ to 210 ℃ and the air outlet temperature is 110 ℃ to 150 ℃ during the spray drying powder preparation process.
3. The method of claim 1, wherein the graphite is expanded graphite.
4. The preparation method according to claim 1, wherein the stirring is specifically:
stirring is carried out at a revolution speed of 20-40r/min and a rotation speed of 2000-2500 r/min.
5. A high-gram-capacity low-specific-surface-area lithium battery silicon-carbon negative electrode material prepared by the preparation method of the high-gram-capacity low-specific-surface-area lithium battery silicon-carbon negative electrode material as claimed in any one of claims 1 to 4.
CN202010208125.9A 2020-03-23 2020-03-23 High-gram-volume low-specific-surface-area lithium battery silicon-carbon negative electrode material and preparation method thereof Pending CN111403706A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102769139A (en) * 2012-08-10 2012-11-07 深圳市斯诺实业发展有限公司永丰县分公司 Preparation method of high power capacity lithium ion battery cathode material
CN103474667A (en) * 2013-08-16 2013-12-25 深圳市贝特瑞新能源材料股份有限公司 Silicon-carbon composite negative electrode material for lithium ion battery and preparation method thereof
CN105355870A (en) * 2015-10-22 2016-02-24 清华大学深圳研究生院 Expanded graphite and nano-silicon composite material, preparation method thereof, electrode plate and battery
CN106025221A (en) * 2016-06-24 2016-10-12 广东省稀有金属研究所 Preparation method for silicon/carbon/graphite composite negative electrode material
KR20180094747A (en) * 2017-02-16 2018-08-24 강원대학교산학협력단 Negative active material for lithium secondary battery, method for preparing the same and lithium secondary battery comprising thereof
CN110649236A (en) * 2019-09-24 2020-01-03 中国科学院化学研究所 Porous silicon-carbon composite material and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102769139A (en) * 2012-08-10 2012-11-07 深圳市斯诺实业发展有限公司永丰县分公司 Preparation method of high power capacity lithium ion battery cathode material
CN103474667A (en) * 2013-08-16 2013-12-25 深圳市贝特瑞新能源材料股份有限公司 Silicon-carbon composite negative electrode material for lithium ion battery and preparation method thereof
CN105355870A (en) * 2015-10-22 2016-02-24 清华大学深圳研究生院 Expanded graphite and nano-silicon composite material, preparation method thereof, electrode plate and battery
CN106025221A (en) * 2016-06-24 2016-10-12 广东省稀有金属研究所 Preparation method for silicon/carbon/graphite composite negative electrode material
KR20180094747A (en) * 2017-02-16 2018-08-24 강원대학교산학협력단 Negative active material for lithium secondary battery, method for preparing the same and lithium secondary battery comprising thereof
CN110649236A (en) * 2019-09-24 2020-01-03 中国科学院化学研究所 Porous silicon-carbon composite material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘漫红 等: "《纳米材料及其制备技术》", 31 August 2014 *
谢凯 等: "《新一代锂二次电池技术》", 31 August 2013 *

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