CN114804094A - Nitrogen-graphene doped composite graphite negative electrode material and preparation method thereof - Google Patents
Nitrogen-graphene doped composite graphite negative electrode material and preparation method thereof Download PDFInfo
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
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Abstract
The invention discloses a nitrogen-graphene doped composite graphite cathode material and a preparation method thereof, wherein the preparation method comprises the following steps: adding a nitrogen source and graphene into an organic solvent to obtain a mixed solution A; adding the mixed solution A and graphite into a mixing device to obtain mixed solution B; carrying out heat treatment on the mixed solution B to obtain a treated material C; and loading the treated material C into a graphite device for graphitization treatment to obtain the graphite cathode material. According to the preparation method, the nitrogen source is combined with the graphene, so that the defects of low first-time efficiency, small tap density and the like of the graphene are overcome, the advantages of high conductivity, large mechanical strength and the like of the graphene are utilized, the multiplying power performance and the cycle stability of the cathode material can be effectively improved through the doping mode of the non-metal elements of the nitrogen source, the problems of low ionic conductivity, large resistance and the like of nitrogen-doped graphite in the traditional technology are solved, and the multiplying power performance and the cycle stability of the cathode material can be further improved.
Description
Technical Field
The invention relates to the technical field of new energy lithium ion battery cathode materials, in particular to a nitrogen-graphene doped composite graphite cathode material and a preparation method thereof.
Background
The traditional graphite cathode can not meet the increasing demand of high-performance power supply, therefore, the method for modifying graphite is actively explored at home and abroad to improve the capacity, the cycling stability and the high rate performance of the graphite cathode. Many factors have been shown to affect the behavior of graphite electrodes.
Proper elements are selected for doping in the graphite cathode so as to regulate and control the microstructure and the electronic structure of the graphite, the electron and ion transfer efficiency of the graphite is effectively improved, and element doping can be divided into metal element doping and non-metal element doping according to element types. At present, the commonly used metal elements include Fe, Co, Ni, Cu, Zn, Ag, etc. The doping of metal elements can improve the electronic conductivity of the graphite cathode, and some metal elements such as Sn can form an active composite material with graphite to increase lithium ion storage active sites, thereby improving the capacity. Besides metal elements, there are also some doping of non-metal elements, such as B, N, P, S, Si, etc.; there are related researchers using H 3 BO 3 B doping is carried out, the first coulombic efficiency is effectively improved, and a plurality of researchers use Si doping to prepare graphite nanosheets, so that the reversible capacity of the electrode can be greatly improved. Therefore, the doping of the non-metal elements can effectively improve the rate capability, the cycling stability and the capacity of the electrode.
Graphene is a novel negative electrode material developed in recent years, has the advantages of high conductivity, high mechanical strength and the like, is applied to the fields of lithium ion battery negative electrode materials, conductive agents and the like, but has the defects of low efficiency, low tap density and the like for the first time, and limits the application of graphene in the aspect of lithium ion batteries. At present, graphite doped with non-metallic elements such as nitrogen and the like, namely graphene, is not available, and a high-performance graphite negative electrode material is prepared.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a preparation method of a nitrogen-graphene doped composite graphite negative electrode material, which is characterized in that a non-metallic element and graphene are mixed and then doped into graphite, so that the obtained graphite negative electrode material has high cycle performance and high rate.
The invention also aims to provide the nitrogen-graphene doped composite graphite negative electrode material prepared by the preparation method.
One of the purposes of the invention is realized by adopting the following technical scheme:
a preparation method of a nitrogen-graphene doped composite graphite negative electrode material comprises the following preparation steps:
s1: adding a nitrogen source and graphene into an organic solvent, and uniformly mixing to obtain a mixed solution A;
s2: adding the mixed solution A and graphite into a mixing device, and uniformly dispersing to obtain a mixed solution B;
s3: putting the mixed solution B into heat treatment equipment for heat treatment or putting the mixed solution B into carbonization equipment for direct carbonization to obtain a treated material C;
s4: loading the treated material C into graphite equipment, and carrying out graphitization treatment in a graphitization furnace to obtain a graphitized material D;
s5: and screening the graphitized material D to obtain the graphite cathode material.
According to the invention, the nitrogen source is combined with graphene, so that the defects of low first efficiency, small tap density and the like of graphene are overcome, the advantages of high conductivity, large mechanical strength and the like of graphene are utilized, the multiplying power performance and the cycle stability of the cathode material can be effectively improved by the doping mode of the non-metallic elements of the nitrogen source, meanwhile, the problems of low ionic conductivity, large resistance and the like of nitrogen-doped graphite in the traditional technology are solved by combining the nitrogen source with the graphene, and the multiplying power performance and the cycle stability of the cathode material can be further improved.
Further, in step S1, the nitrogen source is one or more of melamine, nitrilotriacetic acid, cyanamide, dicyanamide, urea, biuret, and trichloroethylamine. For example, nitrogen sources composed of melamine, cyanamide, and biuret, nitrogen sources composed of biuret and trichloroethylamine, nitrogen sources composed of melamine, nitrilotriacetic acid, and cyanamide, and the like.
Further, in step S1, the organic solvent is one or more of an oil solvent, an alcohol solvent, a ketone solvent, an alkane solvent, N-methylpyrrolidone, tetrahydrofuran, and toluene. For example, an organic solvent composed of an oil solvent, an alcohol solvent, an organic solvent composed of N-methylpyrrolidone, tetrahydrofuran, toluene, or the like.
Further, the oil solvent is one or more than two of kerosene, mineral oil and vegetable oil; the alcohol solvent is one or more than two of ethanol, methanol, ethylene glycol, isopropanol, n-octanol, allyl alcohol and octanol; the ketone solvent is one or more than two of acetone, methyl butanone, methyl isobutyl ketone, methyl ethyl ketone, methyl isopropyl ketone, cyclohexanone and methyl hexyl ketone; the alkane solvent is one or more than two of cyclohexane, normal hexane, isoheptane, 3-dimethylpentane and 3-methylhexane.
Further, in step S1, the weight ratio of the nitrogen source, graphene, and organic solvent is (0.5-0.7): (0.1-0.3): (1-2).
Further, in step S2, the graphite is artificial graphite and/or natural graphite.
Further, in step S2, the weight ratio of the mixed solution A to graphite is (0.1-0.3): 1.
Further, in step S2, the mixing device is a fusion machine or a VC100 mixer, the rotating speed is 300r/min-500r/min, and the mixing time is 1min-10 min.
Further, in step S3, the heat treatment equipment is one of a vertical kettle, a horizontal kettle, and a roller furnace, the heat treatment mode is to perform temperature rise coating by using a 400-800 ℃ curve, and the rotation frequency is 5 HZ-50 HZ; the carbonization equipment is a carbonization furnace, and the carbonization temperature is 800-1150 ℃.
Further, in step S4, the graphite equipment is an acheson graphitization furnace, and the temperature of the graphitization furnace is 2400 ℃ to 3000 ℃.
Further, in step S2, the graphite has an average particle diameter of 8.0 to 11 μm; in step S5, the graphite negative electrode material has an average particle diameter of 9.0 to 15 μm.
The second purpose of the invention is realized by adopting the following technical scheme:
the nitrogen-graphene doped composite graphite negative electrode material is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method, the nitrogen source is combined with the graphene, so that the defects of low initial efficiency, small tap density and the like of the graphene are overcome, the advantages of high conductivity, large mechanical strength and the like of the graphene are utilized, the multiplying power performance and the cycle stability of the cathode material can be effectively improved through the doping mode of the non-metal elements of the nitrogen source, meanwhile, the problems of low ionic conductivity, large resistance and the like of nitrogen-doped graphite in the traditional technology are solved through the combination of the nitrogen source and the graphene, and the multiplying power performance and the cycle stability of the cathode material can be further improved.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
Example 1
A preparation method of a nitrogen-graphene doped composite graphite negative electrode material comprises the following preparation steps:
s1: grinding 300g of artificial graphite material mechanically to obtain graphite powder with the average particle size of 8.0-11 mu m;
s2: mixing the following components in parts by weight: 2:1, adding a nitrogen source consisting of melamine, cyanamide and biuret and graphene into N-methyl pyrrolidone, and uniformly mixing to obtain a mixed solution A; wherein the weight ratio of the nitrogen source to the graphene to the N-methyl pyrrolidone is 0.5:0.1: 1;
s3: adding the mixed solution A and graphite powder into a fusion machine according to the weight ratio of 0.1:1 to uniformly disperse the mixed solution A and the graphite powder, wherein the rotating speed is 500r/min, and the mixing time is 5min to obtain mixed solution B;
s4: putting the mixed solution B into a vertical kettle for heat treatment, and heating and coating according to a curve of 400-800 ℃ to obtain a treated material C;
s5: loading the treated material C into an Acheson graphitizing furnace, and carrying out heat treatment in the graphitizing furnace at the temperature of 2800 ℃ to obtain a graphitized material D;
s6: and screening the graphitized material D to obtain the graphite negative electrode material with the average particle size of 9.0-15 mu m.
Example 2
A preparation method of a nitrogen-graphene doped composite graphite negative electrode material comprises the following preparation steps:
s1: grinding 300g of natural graphite mechanically to obtain graphite powder with the average particle size of 8.0-11 mu m;
s2: adding a nitrogen source consisting of biuret and trichloroethylamine in a ratio of 1:1 and graphene into methyl isobutyl ketone, and uniformly mixing to obtain a mixed solution A; wherein the weight ratio of the nitrogen source to the graphene to the methyl isobutyl ketone is 0.5:0.1: 1;
s3: adding the mixed solution A and graphite powder into a fusion machine according to the weight ratio of 0.2:1 to uniformly disperse the mixed solution A and the graphite powder, wherein the rotating speed is 500r/min, and the mixing time is 5min to obtain mixed solution B;
s4: putting the mixed solution B into a vertical kettle for heat treatment, and heating and coating according to a curve of 400-800 ℃ to obtain a treated material C;
s5: loading the treated material C into an Acheson graphitizing furnace, and carrying out heat treatment in the graphitizing furnace at the temperature of 2800 ℃ to obtain a graphitized material D;
s6: and screening the graphitized material D to obtain the graphite negative electrode material with the average particle size of 9.0-15 mu m.
Example 3
A preparation method of a nitrogen-graphene doped composite graphite negative electrode material comprises the following preparation steps:
s1: grinding 300g of artificial graphite material mechanically to obtain graphite powder with the average particle size of 8.0-11 mu m;
s2: adding a nitrogen source consisting of melamine, nitrilotriacetic acid and cyanamide in a ratio of 1:1:1 and graphene into cyclohexane, and uniformly mixing to obtain a mixed solution A; wherein the weight ratio of the nitrogen source to the graphene to the cyclohexane is 0.5:0.3: 2;
s3: adding the mixed solution A and graphite powder into a fusion machine according to the weight ratio of 0.3:1 to uniformly disperse the mixed solution A and the graphite powder, wherein the rotating speed is 500r/min, and the mixing time is 5min to obtain mixed solution B;
s4: putting the mixed solution B into a vertical kettle for heat treatment, and heating and coating according to a curve of 400-800 ℃ to obtain a treated material C;
s5: loading the treated material C into an Acheson graphitizing furnace, and carrying out heat treatment in the graphitizing furnace at the temperature of 2800 ℃ to obtain a graphitized material D;
s6: and screening the graphitized material D to obtain the graphite negative electrode material with the average particle size of 9.0-15 mu m.
Example 4
A preparation method of a nitrogen-graphene doped composite graphite negative electrode material comprises the following preparation steps:
s1: grinding 300g of artificial graphite material mechanically to obtain graphite powder with the average particle size of 8.0-11 mu m;
s2: adding dicyandiamide and graphene into allyl alcohol, and uniformly mixing to obtain a mixed solution A; wherein the weight ratio of dicyandiamide to graphene to allyl alcohol is 0.7:0.3: 2;
s3: adding the mixed solution A and graphite powder into a fusion machine according to the weight ratio of 0.2:1 to uniformly disperse the mixed solution A and the graphite powder, wherein the rotating speed is 500r/min, and the mixing time is 5min to obtain mixed solution B;
s4: putting the mixed solution B into a carbonization furnace for direct carbonization at the carbonization temperature of 1000 ℃ to obtain a treated material C;
s5: putting the treated material C into an Acheson graphitizing furnace, and carrying out heat treatment in the graphitizing furnace at the temperature of 2800 ℃ to obtain a graphitized material D;
s6: and screening the graphitized material D to obtain the graphite negative electrode material with the average particle size of 9.0-15 mu m.
Comparative example 1
A preparation method of a graphite negative electrode material comprises the following preparation steps:
s1: grinding 300g of artificial graphite material mechanically to obtain graphite powder with the average particle size of 8.0-11 mu m;
s2: putting graphite powder into an Acheson graphitizing furnace, and carrying out heat treatment in the graphitizing furnace at the temperature of 2800 ℃ to obtain a graphitized material D;
s3: and screening the graphitized material D to obtain the graphite cathode material.
Comparative example 2
A preparation method of a graphite negative electrode material comprises the following preparation steps:
s1: grinding 300g of artificial graphite material mechanically to obtain graphite powder with the average particle size of 8.0-11 mu m;
s2: adding dicyandiamide into allyl alcohol, and uniformly mixing to obtain a mixed solution A; wherein the weight ratio of dicyandiamide to allyl alcohol is 0.7: 2;
s3: adding the mixed solution A and graphite powder into a fusion machine according to the weight ratio of 0.2:1 to uniformly disperse the mixed solution A and the graphite powder, wherein the rotating speed is 500r/min, and the mixing time is 5min to obtain mixed solution B;
s4: putting the mixed solution B into a carbonization furnace for direct carbonization at the carbonization temperature of 1000 ℃ to obtain a treated material C;
s5: putting the treated material C into an Acheson graphitizing furnace, and carrying out heat treatment in the graphitizing furnace at the temperature of 2800 ℃ to obtain a graphitized material D;
s6: and screening the graphitized material D to obtain the graphite negative electrode material with the average particle size of 9.0-15 mu m.
Comparative example 3
A preparation method of a graphite negative electrode material comprises the following preparation steps:
s1: grinding 300g of artificial graphite material mechanically to obtain graphite powder with the average particle size of 8.0-11 mu m;
s2: adding graphene into allyl alcohol, and uniformly mixing to obtain a mixed solution A; wherein the weight ratio of the graphene to the allyl alcohol is 0.3: 2;
s3: adding the mixed solution A and graphite powder into a fusion machine according to the weight ratio of 0.2:1 to uniformly disperse the mixed solution A and the graphite powder, wherein the rotating speed is 500r/min, and the mixing time is 5min to obtain mixed solution B;
s4: putting the mixed solution B into a carbonization furnace for direct carbonization at the carbonization temperature of 1000 ℃ to obtain a treated material C;
s5: loading the treated material C into an Acheson graphitizing furnace, and carrying out heat treatment in the graphitizing furnace at the temperature of 2800 ℃ to obtain a graphitized material D;
s6: and screening the graphitized material D to obtain the graphite negative electrode material with the average particle size of 9.0-15 mu m.
Performance testing
The materials prepared in the comparative example and the example are taken and tested for capacity retention at 50 cycles at 0.5 and capacity retention at 3C relative to 0.1C.
The test method comprises the following steps: the test was performed by a half-cell test method, in which N-methylpyrrolidone (NMP) was added to the negative electrode material and polyvinylidene fluoride (PVdF) of the above examples and comparative examples at a mass ratio of 9:1 to prepare a slurry, which was coated on a copper foil, and a negative electrode sheet was prepared by drying, film punching and film pressing. And (3) taking a metal lithium foil as a counter electrode, taking an electrolyte as 1MLiPF6/(PC + DMC) to be 1:1, and taking a polypropylene film (Celgard 2325) as a diaphragm to assemble the battery. The charging and discharging voltage is 0-1.5V, the charging and discharging speed is 0.1C and 0.5C, the battery performance is tested, and the test results are shown in the following table.
TABLE 1
| Item | First coulombic efficiency (%) | 5C Capacity Retention (%) |
| Example 1 | 97.32 | 56.34 |
| Example 2 | 96.82 | 57.89 |
| Example 3 | 97.62 | 56.59 |
| Example 4 | 96.21 | 58.31 |
| Comparative example 1 | 95.67 | 50.46 |
| Comparative example 2 | 96.57 | 53.62 |
| Comparative example 3 | 94.36 | 48.68 |
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Claims (10)
1. A preparation method of a nitrogen-graphene doped composite graphite negative electrode material is characterized by comprising the following preparation steps:
s1: adding a nitrogen source and graphene into an organic solvent, and uniformly mixing to obtain a mixed solution A;
s2: adding the mixed solution A and graphite into a mixing device, and uniformly dispersing to obtain a mixed solution B;
s3: putting the mixed solution B into heat treatment equipment for heat treatment or putting the mixed solution B into carbonization equipment for direct carbonization to obtain a treated material C;
s4: loading the treated material C into graphite equipment, and carrying out graphitization treatment in a graphitization furnace to obtain a graphitized material D;
s5: and screening the graphitized material D to obtain the graphite cathode material.
2. The method for preparing the nitrogen-graphene doped composite graphite anode material according to claim 1, wherein in step S1, the nitrogen source is one or more of melamine, nitrilotriacetic acid, cyanamide, dicyandiamide, urea, biuret, and trichloroethylamine.
3. The method for preparing the nitrogen-graphene doped composite graphite anode material according to claim 1, wherein in step S1, the organic solvent is one or more of an oil solvent, an alcohol solvent, a ketone solvent, an alkane solvent, N-methylpyrrolidone, tetrahydrofuran, and toluene.
4. The preparation method of the nitrogen-graphene doped composite graphite negative electrode material according to claim 3, wherein the oil solvent is one or more than two of kerosene, mineral oil and vegetable oil; the alcohol solvent is one or more than two of ethanol, methanol, ethylene glycol, isopropanol, n-octanol, allyl alcohol and octanol; the ketone solvent is one or more than two of acetone, methyl butanone, methyl isobutyl ketone, methyl ethyl ketone, methyl isopropyl ketone, cyclohexanone and methyl hexyl ketone; the alkane solvent is one or more than two of cyclohexane, normal hexane, isoheptane, 3-dimethylpentane and 3-methylhexane.
5. The method for preparing the nitrogen-graphene doped composite graphite anode material according to claim 1, wherein in the step S1, the weight ratio of the nitrogen source to the graphene to the organic solvent is (0.5-0.7): (0.1-0.3): (1-2).
6. The method for preparing the nitrogen-graphene doped composite graphite anode material according to claim 1, wherein in the step S2, the graphite is artificial graphite and/or natural graphite.
7. The method for preparing a nitrogen-graphene doped composite graphite anode material according to claim 1, wherein in step S2, the weight ratio of mixed solution A to graphite is (0.1-0.3): 1.
8. The method for preparing the nitrogen-graphene doped composite graphite anode material according to claim 1, wherein in step S2, the mixing device is a fusion machine or a VC100 mixer, the rotation speed is 300r/min to 500r/min, and the mixing time is 1min to 10 min.
9. The method for preparing the nitrogen-graphene doped composite graphite anode material according to claim 1, wherein in step S3, the heat treatment equipment is one of a vertical kettle, a horizontal kettle and a roller furnace, the heat treatment mode is to perform temperature rise coating by using a curve of 400-800 ℃, and the rotation frequency is 5 HZ-50 HZ; the carbonization equipment is a carbonization furnace, and the carbonization temperature is 800-1150 ℃; in step S4, the graphite equipment is an acheson graphitization furnace, and the temperature of the graphitization furnace is 2400 ℃ to 3000 ℃.
10. A nitrogen-graphene doped composite graphite negative electrode material, characterized in that the graphite negative electrode material is prepared by the preparation method according to any one of claims 1 to 9.
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