CN110931740A - Method for preparing lithium ion negative electrode material by using nano carbon-antimony composite material - Google Patents

Method for preparing lithium ion negative electrode material by using nano carbon-antimony composite material Download PDF

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CN110931740A
CN110931740A CN201911153621.2A CN201911153621A CN110931740A CN 110931740 A CN110931740 A CN 110931740A CN 201911153621 A CN201911153621 A CN 201911153621A CN 110931740 A CN110931740 A CN 110931740A
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nano carbon
particle size
equal
powder
composite material
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魏健
张锦俊
闵洁
张培林
庞中海
武建军
刘伟凯
吕星薄
霍有
纪永良
雷涛
徐保国
陈永贵
张彦举
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Datong Xincheng New Material 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 relates to the technical field of preparation of negative electrode materials, in particular to a method for preparing a lithium ion negative electrode material by using a nano carbon-antimony composite materialThe material has the advantages of high rigidity, weakened rigidity and higher compaction density, and the structure is formed by mixing single nano carbon-antimony composite material particles with different particle sizes, so that the material is favorable for the insertion and the separation of lithium ions, the gram capacity of a negative electrode material is further improved, and the charge and discharge capacity of the battery is increased. The lithium ion battery cathode material prepared by using the nano carbon-antimony composite material particles has a stable structure, the particle size of the cathode material is 1-30 mu m, and the true density is more than or equal to 2.5g/cm3Ash content is less than or equal to 0.15 percent, and tap density is more than or equal to 1.20g/cm3The specific surface area is less than or equal to 0.6m/g2The first discharge capacity is 370-400mAh/g, and the first discharge efficiency is more than or equal to 93 percent.

Description

Method for preparing lithium ion negative electrode material by using nano carbon-antimony composite material
Technical Field
The invention relates to the technical field of preparation of negative electrode materials, in particular to a method for preparing a lithium ion negative electrode material by using a nano carbon-antimony composite material.
Background
The lithium ion battery negative electrode material is divided into a carbon material and a non-carbon material, the carbon material is divided into a graphite carbon material and an amorphous carbon graphite material, and the graphite carbon material mainly comprises natural graphite, artificial graphite, modified graphite or a mixture; amorphous carbon graphitic materials include, as graphitizable carbon materials (hard carbons): coke, mesocarbon microbeads and the like and hard-to-graphitize carbon materials (soft carbon) including carbon fibers, epoxy resin and phenolic resin are used as main materials; non-carbon materials include tin-based materials, silicon-based materials, oxides, titanium-based materials, and the like.
As a novel chemical power supply, the lithium ion battery has become the key point of development of countries in the world in the field of new energy materials at present due to high output voltage, high specific energy, long cycle life, small self-discharge, safety, no memory effect and environmental friendliness. The natural graphite also has the characteristics of low tap density and high specific surface area, and is not ideal as a raw material for preparing a cathode material. The common artificial graphite has the defects of high specific surface area, low tap density, poor particle morphology, low discharge capacity and the like, is not suitable for being directly used as a condition for preparing a negative electrode material, and if the artificial graphite needs to be used, modification is needed, the improvement of the structural stability of the graphite cannot be ensured, and the production cost is also increased.
The negative electrode materials of lithium ion batteries that are currently commercially available are graphite and other forms of carbon materials. The theoretical capacity of the graphite is only 372mAh g-1And the lithium intercalation potential is lower, which limits the application range. Isotropic graphite materials have excellent properties such as electrical conductivity, thermal conductivity, resistance to corrosion, self-lubricity, and the like, are easier to process than metal materials, and are widely used as conductive materials and structural materials in many fields such as electronics, machinery, semiconductors, and the like. Compared with carbon materials such as graphite, some antimony-based alloys have ideal lithium intercalation potential, higher mass ratio and volume specific capacity, and very wide application prospect.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for preparing a lithium ion negative electrode material by using a nano carbon-antimony composite material.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for preparing a lithium ion negative electrode material by using a nano carbon-antimony composite material comprises the following steps:
s1, preparing a nano carbon material solution: the nano carbon material solution is prepared by dispersing purified graphite material into concentrated sulfuric acid at 0 +/-5 ℃, and adding KMnO4Stirring for 30-60 minutes, raising the temperature to 40-50 ℃, adding deionized water which is 3-8 times of the volume of the stirred mixture, continuing stirring for 20-40 minutes, performing centrifugal separation, washing with an HCl aqueous solution with the mass concentration of 5%, deionized water and acetone, ultrasonically dispersing the mixture in the deionized water, and fully stirring to obtain a nano carbon material solution with the nano carbon material content of 20-50 mmol/L;
s2, preparation of an antimony-containing solution: providing SbCl according to the atomic ratio of Sb, Ni and Co of 1 to (0.3-0.5) to (0.2-0.3)3、NiSO4And CoSO4Mixing the precursor solution with anhydrous glycol to prepare an antimony-containing precursor solution with the concentration of 0.10-0.15mol/L calculated by Sb;
s3, preparing the nano carbon-antimony composite material: adding an antimony-containing solution in S2 into a nano carbon material solution in S1 to form a mixed solution, wherein the volume ratio of the mixed solution to the nano carbon material solution is 1 (1-2), and adding KBH into the mixed solution4Heating to 200-300 ℃ under a sealed condition, reacting for 12-24 hours, naturally cooling to room temperature after the reaction is finished, collecting a powdery reaction product, sequentially washing with deionized water and absolute ethyl alcohol, and drying to obtain composite material powder;
s4, grinding the nano carbon-antimony composite material in the S3 in a grinding equipment machine;
s5, coating: placing the nano carbon-antimony composite material and the coating material in S4 in an impregnation tank, and impregnating for 8-15h at the temperature of 280-650 ℃ and under the pressure of 7-12KPa to obtain a mixed material;
s6, roasting: placing the mixed material in the S5 into a roasting furnace for roasting and carbonization;
s7, graphitizing: placing the carbonized mixed material in S6 in a graphitization furnace for graphitization purification for 500 hours at the time of 450-;
s8, classifying the pulse into the pulse width less than 100, the wavelength 500-2000nm, processing the material after the final purification into the required particle size by the laser pulse.
Further, the graphite material, concentrated sulfuric acid and KMnO4The mass ratio of (1-5) to (10-20) to (5-15).
Further, the graphite material is a mixture of nano carbon powder and carbon black, and the weight ratio of the nano carbon powder to the carbon black is 60:40-65: 35; the specific preparation method of the graphite material comprises the following steps: weighing the powder, uniformly mixing the powder together, putting the powder into a ball milling tank, introducing argon gas for protection, then carrying out ball milling for 8 hours at the rotating speed of 500-800r/min, rotating for 30min and stopping for 10 min.
Further, the particle size of the nano carbon powder is 1-20 μm, and the volume density is more than or equal to 1.80g/cm3The resistivity is less than or equal to 8 mu omega m, the breaking strength is more than or equal to 30Mpa, and the compressive strength is more than or equal to 60 Mpa; wherein the particle size is 1-5 μm accounting for 30% of the weight, the particle size is 5-10 μm accounting for 20% of the weight, the particle size is 10-15 μm accounting for 30% of the weight, and the particle size is 15-20 μm accounting for 20% of the weight; the purity of the carbon black is 99%, and the particle size is 1-40 mu m; wherein the particle size is 1-10 μm and accounts for 20% of the weight of the powder; the particle size is 10-20 μm and accounts for 30% of the weight of the powder; the particle size is 20-30 μm and accounts for 30% of the weight of the powder; the particle size is 30-40 μm and accounts for 20% of the weight of the powder.
Furthermore, the coating material adopts medium-temperature coal pitch, the softening point is 83-88 ℃, the coking value is more than or equal to 52%, the ash content is less than or equal to 0.20%, and the quinoline insoluble substance is less than or equal to 0.20%.
Further, the weight ratio of the nano carbon-antimony composite material to the coating material is 75:25-80:20, preferably 72-80: 20-28.
Further, the KBH4The mol ratio of the Sb in the mixed solution is 1 (1-2);
further, the milled particle size of S4 is classified to leave the material required for production, wherein the particle size is 1-10 μm accounting for 25% of the weight; the particle size is 10-20 μm and accounts for 15% of the weight of the powder; the particle size is 20-30 μm and accounts for 15% of the weight of the powder; the particle size is 30-40 μm accounting for 25% of the weight of the powder; the particle size is 40-50 μm and accounts for 20% of the total weight
Further, the baking of S6 is carried out with temperature programming: the heating rate is 2.5 ℃/h and 80h at the temperature of 120-320 ℃; the heating rate is 3.5 ℃/h and 57h at the temperature of 320-520 ℃; at the temperature of 520 ℃ and 820 ℃, the heating rate is 4 ℃/h and 75 h; at the temperature of 820-.
Furthermore, the particle size of the negative electrode material is 1-30 μm, and the true density is more than or equal to 2.5g/cm3Ash content is less than or equal to 0.15 percent, and tap density is more than or equal to 1.20g/cm3The specific surface area is less than or equal to 0.6m/g2The first discharge capacity is 370-400mAh/g, and the first discharge efficiency is more than or equal to 93 percent.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for preparing a lithium ion negative electrode material by using a nano carbon-antimony composite material, which improves the graphitization process, carries out deep graphitization purification, and has the advantages of high comprehensive performance, weakened rigidity and higher compaction density of the prepared battery, and the structure is formed by mixing single nano carbon-antimony composite material particles with different particle sizes. The lithium ion battery cathode material prepared by using the nano carbon-antimony composite material particles has a stable structure, the particle size of the cathode material is 1-30 mu m, and the true density is more than or equal to 2.5g/cm3Ash content is less than or equal to 0.15 percent, and tap density is more than or equal to 1.20g/cm3The specific surface area is less than or equal to 0.6m/g2The first discharge capacity is 370-400mAh/g, and the first discharge efficiency is more than or equal to 93 percent. The cathode material has the characteristics of high quality, strong reliability, high energy density, long service life, high utilization rate of the anode, high first discharge efficiency and the like.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
A method for preparing a lithium ion negative electrode material by using a nano carbon-antimony composite material comprises the following steps:
s1, preparing a nano carbon material solution: the nano carbon material solution is prepared by dispersing purified graphite material into concentrated sulfuric acid at 0 +/-5 ℃, and adding KMnO4Stirring for 30-60 minutes, raising the temperature to 40-50 ℃, adding deionized water which is 3-8 times of the volume of the stirred mixture, continuing stirring for 20-40 minutes, performing centrifugal separation, washing with an HCl aqueous solution with the mass concentration of 5%, deionized water and acetone, ultrasonically dispersing the mixture in the deionized water, and fully stirring to obtain a nano carbon material solution with the nano carbon material content of 20-50 mmol/L; the mass ratio of the graphite material to the concentrated sulfuric acid to the KMnO4 is (1-5) to (10-20) to (5-15)
S2, preparation of an antimony-containing solution: providing SbCl according to the atomic ratio of Sb, Ni and Co of 1 to (0.3-0.5) to (0.2-0.3)3、NiSO4And CoSO4Mixing the precursor solution with anhydrous glycol to prepare an antimony-containing precursor solution with the concentration of 0.10-0.15mol/L calculated by Sb;
s3, preparing the nano carbon-antimony composite material: adding an antimony-containing solution in S2 into a nano carbon material solution in S1 to form a mixed solution, wherein the volume ratio of the mixed solution to the nano carbon material solution is 1 (1-2), and adding KBH into the mixed solution4，KBH4The mol ratio of the Sb in the mixed solution is 1 (1-2); heating to 200-300 ℃ under a sealed condition, reacting for 12-24 hours, naturally cooling to room temperature after the reaction is finished, collecting a powdery reaction product, sequentially washing with deionized water and absolute ethyl alcohol, and drying to obtain composite material powder;
s4, grinding the nano carbon-antimony composite material in the S3 in a grinding equipment machine, and grading the ground particle size to leave the material required for production, wherein the particle size is 1-10 mu m and accounts for 25% of the weight of the material; the particle size is 10-20 μm and accounts for 15% of the weight of the powder; the particle size is 20-30 μm and accounts for 15% of the weight of the powder; the particle size is 30-40 μm accounting for 25% of the weight of the powder; the particle size is 40-50 μm and accounts for 20% of the total weight
S5, coating: placing the nano carbon-antimony composite material and the coating material in S4 in an impregnation tank, and impregnating for 8-15h at the temperature of 280-650 ℃ and under the pressure of 7-12KPa to obtain a mixed material; the weight ratio of the nano carbon-antimony composite material to the coating material is 75:25-80:20, preferably 72-80: 20-28.
S6, roasting: placing the mixed material in the S5 into a roasting furnace for roasting and carbonization, and carrying out temperature programming in the roasting process: the heating rate is 2.5 ℃/h and 80h at the temperature of 120-320 ℃; the heating rate is 3.5 ℃/h and 57h at the temperature of 320-520 ℃; at the temperature of 520 ℃ and 820 ℃, the heating rate is 4 ℃/h and 75 h; at the temperature of 820-
S7, graphitizing: placing the carbonized mixed material in S6 in a graphitization furnace for graphitization purification for 500 hours at the time of 450-;
s8, classifying the pulse into the pulse width less than 100, the wavelength 500-2000nm, processing the material after the final purification into the required particle size by the laser pulse.
In the embodiment, the graphite material is a mixture of nano carbon powder and carbon black, and the weight ratio of the mixture to the carbon black is 60:40-65: 35; the specific preparation method of the graphite material comprises the following steps: weighing the powder, uniformly mixing the powder together, putting the powder into a ball milling tank, introducing argon gas for protection, then carrying out ball milling for 8 hours at the rotating speed of 500-800r/min, rotating for 30min and stopping for 10 min. The particle size of the nano carbon powder is 1-20 mu m, and the volume density is more than or equal to 1.80g/cm3The resistivity is less than or equal to 8 mu omega m, the breaking strength is more than or equal to 30Mpa, and the compressive strength is more than or equal to 60 Mpa; wherein the particle size is 1-5 μm accounting for 30% of the weight, the particle size is 5-10 μm accounting for 20% of the weight, the particle size is 10-15 μm accounting for 30% of the weight, and the particle size is 15-20 μm accounting for 20% of the weight; the purity of the carbon black is 99%, and the particle size is 1-40 mu m; wherein the particle size is 1-10 μm and accounts for 20% of the weight of the powder; the particle size is 10-20 μm and accounts for 30% of the weight of the powder; the particle size is 20-30 μm and accounts for 30% of the weight of the powder; the particle size is 30-40 μm and accounts for 20% of the weight of the powder.
In the embodiment, the coating material adopts medium-temperature coal tar pitch, the softening point is 83-88 ℃, the coking value is more than or equal to 52%, the ash content is less than or equal to 0.20%, and the quinoline insoluble substance is less than or equal to 0.20%.
In this example, the prepared anode material has a particle size of 1-30 μm and a true density of 2.5g/cm or more3Ash content is less than or equal to 0.15 percent,tap density is more than or equal to 1.20g/cm3The specific surface area is less than or equal to 0.6m/g2The first discharge capacity is 370-400mAh/g, and the first discharge efficiency is more than or equal to 93 percent.
Although only the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art, and all changes are encompassed in the scope of the present invention.

Claims (10)

1. A method for preparing a lithium ion negative electrode material by using a nano carbon-antimony composite material is characterized by comprising the following steps of:
s1, preparing a nano carbon material solution: the nano carbon material solution is prepared by dispersing purified graphite material into concentrated sulfuric acid at 0 +/-5 ℃, and adding KMnO4Stirring for 30-60 minutes, raising the temperature to 40-50 ℃, adding deionized water which is 3-8 times of the volume of the stirred mixture, continuing stirring for 20-40 minutes, performing centrifugal separation, washing with an HCl aqueous solution with the mass concentration of 5%, deionized water and acetone, ultrasonically dispersing the mixture in the deionized water, and fully stirring to obtain a nano carbon material solution with the nano carbon material content of 20-50 mmol/L;
s2, preparation of an antimony-containing solution: providing SbCl according to the atomic ratio of Sb, Ni and Co of 1 to (0.3-0.5) to (0.2-0.3)3、NiSO4And CoSO4Mixing the precursor solution with anhydrous glycol to prepare an antimony-containing precursor solution with the concentration of 0.10-0.15mol/L calculated by Sb;
s3, preparing the nano carbon-antimony composite material: adding an antimony-containing solution in S2 into a nano carbon material solution in S1 to form a mixed solution, wherein the volume ratio of the mixed solution to the nano carbon material solution is 1 (1-2), and adding KBH into the mixed solution4Heating to 200-300 ℃ under a sealed condition, reacting for 12-24 hours, naturally cooling to room temperature after the reaction is finished, collecting a powdery reaction product, sequentially washing with deionized water and absolute ethyl alcohol, and drying to obtain composite material powder;
s4, grinding the nano carbon-antimony composite material in the S3 in a grinding equipment machine;
s5, coating: placing the nano carbon-antimony composite material and the coating material in S4 in an impregnation tank, and impregnating for 8-15h at the temperature of 280-650 ℃ and under the pressure of 7-12KPa to obtain a mixed material;
s6, roasting: placing the mixed material in the S5 into a roasting furnace for roasting and carbonization;
s7, graphitizing: placing the carbonized mixed material in S6 in a graphitization furnace for graphitization purification for 500 hours at the time of 450-;
s8, classifying the pulse into the pulse width less than 100, the wavelength 500-2000nm, processing the material after the final purification into the required particle size by the laser pulse.
2. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: the graphite material, concentrated sulfuric acid and KMnO4The mass ratio of (1-5) to (10-20) to (5-15).
3. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: the graphite material is a mixture of nano carbon powder and carbon black, and the weight ratio of the nano carbon powder to the carbon black is 60:40-65: 35; the specific preparation method of the graphite material comprises the following steps: weighing the powder, uniformly mixing the powder together, putting the powder into a ball milling tank, introducing argon gas for protection, then carrying out ball milling for 8 hours at the rotating speed of 500-800r/min, rotating for 30min and stopping for 10 min.
4. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: the particle size of the nano carbon powder is 1-20 mu m, and the volume density is more than or equal to 1.80g/cm3The resistivity is less than or equal to 8 mu omega m, the breaking strength is more than or equal to 30Mpa, and the compressive strength is more than or equal to 60 Mpa; wherein the particle size is 1-5 μm accounting for 30% of the total weight, the particle size is 5-10 μm accounting for 20% of the total weight, the particle size is 10-15 μm accounting for 30% of the total weight, and the particle size is 15-20 μm accounting for 15-20 μm20% of; the purity of the carbon black is 99%, and the particle size is 1-40 mu m; wherein the particle size is 1-10 μm and accounts for 20% of the weight of the powder; the particle size is 10-20 μm and accounts for 30% of the weight of the powder; the particle size is 20-30 μm and accounts for 30% of the weight of the powder; the particle size is 30-40 μm and accounts for 20% of the weight of the powder.
5. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: the coating material adopts medium-temperature coal pitch, the softening point is 83-88 ℃, the coking value is more than or equal to 52%, the ash content is less than or equal to 0.20%, and the quinoline insoluble substance is less than or equal to 0.20%.
6. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: the weight ratio of the nano carbon-antimony composite material to the coating material is 75:25-80: 20.
7. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: the KBH4The molar ratio of the Sb in the mixed solution is 1 (1-2).
8. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: classifying the milled particle size of S4 to obtain material with particle size of 1-10 μm 25 wt%; the particle size is 10-20 μm and accounts for 15% of the weight of the powder; the particle size is 20-30 μm and accounts for 15% of the weight of the powder; the particle size is 30-40 μm accounting for 25% of the weight of the powder; the particle size is 40-50 μm and accounts for 20% of the weight of the powder.
9. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the baking of S6 is carried out for temperature programming: the heating rate is 2.5 ℃/h and 80h at the temperature of 120-320 ℃; the heating rate is 3.5 ℃/h and 57h at the temperature of 320-520 ℃; at the temperature of 520 ℃ and 820 ℃, the heating rate is 4 ℃/h and 75 h; at the temperature of 820-.
10. The method for preparing the lithium ion anode material by using the nano carbon-antimony composite material as claimed in claim 1, wherein the method comprises the following steps: the particle size of the negative electrode material is 1-30 mu m, and the true density is more than or equal to 2.5g/cm3Ash content is less than or equal to 0.15 percent, and tap density is more than or equal to 1.20g/cm3The specific surface area is less than or equal to 0.6m/g2The first discharge capacity is 370-400mAh/g, and the first discharge efficiency is more than or equal to 93 percent.
CN201911153621.2A 2019-11-22 2019-11-22 Method for preparing lithium ion negative electrode material by using nano carbon-antimony composite material Pending CN110931740A (en)

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CN109244389A (en) * 2018-08-21 2019-01-18 大同新成新材料股份有限公司 A method of ion cathode material lithium is prepared using selenium graphene composite material

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CN103066253A (en) * 2012-12-26 2013-04-24 上海锦众信息科技有限公司 Preparation method for graphene-antimony composite material used for lithium ion battery
CN107732216A (en) * 2017-11-07 2018-02-23 大同新成新材料股份有限公司 A kind of method that ion cathode material lithium is prepared using C/C composite material granulars
CN108862272A (en) * 2018-08-21 2018-11-23 大同新成新材料股份有限公司 A method of expanded graphite is prepared using graphene oxide, nano-carbon powder
CN109244389A (en) * 2018-08-21 2019-01-18 大同新成新材料股份有限公司 A method of ion cathode material lithium is prepared using selenium graphene composite material

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