CN111584866A - Preparation method of high-rate artificial graphite negative electrode material - Google Patents
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Abstract
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a high-rate artificial graphite cathode material, which comprises the following steps: (1) adding an alkaline compound into artificial graphite or natural graphite, heating to 80-150 ℃ in a reaction kettle, and continuously stirring for 12-24 hours for erosion; (2) cooling to room temperature, repeatedly washing with distilled water, filtering until the filtrate is neutral, and drying in a vacuum drying oven at 60-120 deg.C for 8-16 hr; (3) and (3) annealing the dried material in the step (2) in a furnace with the nitrogen source atmosphere and the temperature of 800-1400 ℃, for 2-6 hours, and finally screening the product to remove large particles to obtain the high-rate artificial graphite cathode material.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a high-rate artificial graphite negative electrode material.
Background
The lithium ion battery as a novel rechargeable battery has the advantages of small self-discharge, long cycle life, good low-temperature performance, high energy density, environmental protection, no memory and the like. With the rapid development of science and technology and the continuous improvement of living standard, people have higher requirements on batteries, namely, products such as electricity which can be charged most in the shortest time, quick charge, super quick charge and the like are produced. In the development process of lithium ion batteries, the negative electrode graphite material as a component of the lithium ion battery always occupies a significant position, and has direct influence on the electrochemical performance of the battery. However, graphite materials mostly have a layered structure or a scaly structure, graphite layers are combined by weak van der waals force, so that intercalation of solvated lithium ions and co-insertion of solvent molecules are easily caused during high-rate charge and discharge, peeling can be generated between the layers to form a new surface, an organic electrolyte is continuously reduced and decomposed on the newly formed surface to form a new SEI film, a large amount of lithium ions are consumed, the first irreversible capacity loss is increased, and the volume expansion and contraction of graphite particles are caused by the intercalation and the de-intercalation of the solvated lithium ions, so that the electric network among particles is partially interrupted, and the stability, the cycle performance and the safety performance of the graphite materials are influenced by the specific layered structure or the scaly structure of the graphite materials.
Therefore, the charging characteristics of the graphite negative electrode material, such as pore-forming, surface coating, oxidation treatment, and the like, can be greatly improved by appropriately modifying the graphite negative electrode material. Chinese patent CN108807996A introduces metal ions into the body of the nitrogen-doped carbon material, and removes the metal ions after high-temperature heat treatment to obtain the nitrogen-doped graphitized carbon material, although the process is simple, the carbonization process is easy to agglomerate, the adhesion is not uniform, the surface amorphous carbon is not uniform, and the effect is poor; chinese patent CN110841595A takes tannic acid, urea and zinc chloride as a carbon source, a nitrogen source and an activating agent respectively, takes water as a solvent, mixes the raw materials into a suspension, places the suspension in an oven for reaction for a certain time, and calcines the obtained solid sample under a nitrogen atmosphere to obtain the graphitized carbon material.
In view of the above, the invention provides a novel preparation method of a high-rate artificial graphite cathode material by innovatively improving the defects in the prior art.
Disclosure of Invention
The invention discloses a preparation method of a high-rate artificial graphite cathode material, which is characterized by comprising the following steps of:
(1) adding an alkaline compound into artificial graphite or natural graphite, heating to 80-150 ℃ in a reaction kettle, and continuously stirring for 12-24 hours for erosion;
(2) cooling to room temperature, repeatedly washing with distilled water, filtering until the filtrate is neutral, and drying in a vacuum drying oven at 60-120 deg.C for 8-16 hr;
(3) and (3) annealing the dried material in the step (2) in a furnace with the nitrogen source atmosphere and the temperature of 800-1400 ℃ for 2-6 hours, and finally screening the product to remove large particles to obtain the high-magnification artificial graphite cathode material.
Preferably, the alkali compound in step (1) is one or more of KOH and NaOH in water solution.
Adding alkali compound water solution into artificial graphite or natural graphite until graphite is completely soaked.
Preferably, the concentration of the alkali compound aqueous solution in the step (1) is 0.1-2 mol/L.
More preferably, the concentration of the alkali compound aqueous solution in the step (1) is 0.1-1 mol/L.
Further preferably, the concentration of the alkali compound aqueous solution in the step (1) is 0.1-0.5 mol/L.
Preferably, the etching of the alkali compound in the step (1) is mild etching.
Preferably, the drying temperature in the step (2) is 80-120 ℃, and the drying time is 8-12 hours.
Preferably, the nitrogen source in step (3) is urea, nitrogen or ammonia gas, preferably ammonia gas.
Preferably, the temperature in the step (3) is 1000-1200 ℃, and the annealing time is 3-4 hours.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the invention, alkaline compounds are adopted to perform an erosion action on active substances, and due to strong alkaline erosion action, more and wider pore-forming is realized, so that the insertion number of lithium ions is greatly increased, the diffusion distance of the lithium ions is greatly shortened, and the obtained graphite cathode material has good high-current charge-discharge rate performance;
(2) the pore structure is optimized, the surface alkalinity is increased, the porous carbon is endowed with rich active sites for capturing gas and organic matters, and the nitrogen doping effect is more obvious;
(3) the nitrogen element is introduced by ammonia gas in the annealing process, so that the conductivity of the material can be improved, the improvement of the rate capability of the material is facilitated, the ammonia gas is safe and sufficient in adsorption, and an autoclave is not required;
(4) the high-rate quick-charging graphite material half-cell prepared by the method has the advantages that the first discharge capacity is more than or equal to 353mAh/g, and the first efficiency is more than or equal to 93%; the charging multiplying power is more than 10C, and the capacity is kept to be more than or equal to 80 percent; the discharge multiplying power is more than 20C, and the capacity is kept to be more than or equal to 80 percent.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is an SEM image of artificial graphite used as a starting material in step 1 of the present invention.
Fig. 2 is an SEM image of the high-magnification artificial graphite negative electrode material prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. The described embodiments and their results are only intended to illustrate the invention and should not be taken as limiting the invention described in detail in the claims.
The performance parameters of the artificial graphite selected in the examples are as follows: the first discharge capacity of the half cell is 348.7mAh/g, and the first efficiency is 93.1%; the charging multiplying power is more than 1.5C, and the capacity is kept at 80%; the discharge multiplying power is more than 8C, and the capacity is kept at 80%.
Example 1
(1) Adding 0.1mol/L KOH into the artificial graphite until the graphite is completely soaked, heating the artificial graphite to 120 ℃ in a reaction kettle, and continuously stirring for 16 hours for erosion;
(2) after cooling to room temperature, the filtrate was repeatedly washed with distilled water and filtered until the filtrate was neutral (pH 7), and dried in a vacuum oven at 80 ℃ for 12 hours;
(3) annealing the dried material in the step (2) in a furnace with the atmosphere of ammonia gas and the temperature of 1200 ℃ for 3h, and finally screening the product to remove large particles to obtain the high-rate graphite anode material, wherein the performance parameters are as follows: the first discharge capacity of the half cell is 355.1mAh/g, and the first efficiency is 93.6%; the charging multiplying power is more than 10C, and the capacity is kept at 80%; the discharge rate is more than 20C, and the capacity is kept at 81 percent.
Example 2
(1) Adding 0.5mol/L KOH into the artificial graphite until the graphite is completely soaked, heating the artificial graphite to 80 ℃ in a reaction kettle, and continuously stirring the artificial graphite for 24 hours for erosion;
(2) after cooling to room temperature, the filtrate was repeatedly washed with distilled water and filtered until the filtrate was neutral (pH 7), and dried in a vacuum oven at 80 ℃ for 12 hours;
(3) annealing the dried material in the step (2) in a furnace with the atmosphere of ammonia gas and the temperature of 1000 ℃ for 4 hours, and finally screening the product to remove large particles to obtain the high-rate graphite anode material, wherein the performance parameters are as follows: the first discharge capacity of the half cell is 354.8mAh/g, and the first efficiency is 93.4%; the charging rate is more than 10C, and the capacity is kept at 81%; the discharge rate is more than 20C, and the capacity is kept at 80%.
Example 3
(1) Adding 1mol/L KOH into the artificial graphite until the graphite is completely soaked, heating the artificial graphite in a reaction kettle to 140 ℃, and continuously stirring for 14 hours for erosion;
(2) after cooling to room temperature, the filtrate was repeatedly washed with distilled water and filtered until the filtrate was neutral (pH 7), and dried in a vacuum oven at 60 ℃ for 16 hours;
(3) annealing the dried material in the step (2) in a furnace at the temperature of 1100 ℃ for 3.5 hours in the atmosphere of ammonia gas, and finally screening the product to remove large particles to obtain the high-rate graphite cathode material, wherein the performance parameters are as follows: the first discharge capacity of the half cell is 354.1mAh/g, and the first efficiency is 93.2%; the charging rate is more than 10C, and the capacity is kept at 81%; the discharge rate is more than 20C, and the capacity is kept at 82%.
Example 4
(1) Adding 0.8mol/L KOH into the artificial graphite until the graphite is completely soaked, heating the artificial graphite to 150 ℃ in a reaction kettle, and continuously stirring the artificial graphite for 12 hours for erosion;
(2) after cooling to room temperature, repeatedly washing with distilled water and filtering until the filtrate is neutral (pH 7), and drying in a vacuum oven at 120 ℃ for 8 hours;
(3) annealing the dried material in the step (2) in a furnace with the atmosphere of ammonia gas and the temperature of 1150 ℃ for 3 hours, and finally screening the product to remove large particles to obtain the high-magnification graphite cathode material, wherein the performance parameters are as follows: the first discharge capacity of the half cell is 355.2mAh/g, and the first efficiency is 93.8%; the charging multiplying power is more than 10C, and the capacity is kept at 80%; the discharge rate is more than 20C, and the capacity is kept at 82%.
The natural graphite is adopted to replace the artificial graphite, and the high multiplying power of the graphite cathode material can also be improved.
Comparative example 1
(1) Adding 0.1mol/L KOH into the artificial graphite until the graphite is completely soaked, heating the artificial graphite to 120 ℃ in a reaction kettle, and continuously stirring for 16 hours for erosion;
(2) after cooling to room temperature, the filtrate was repeatedly washed with distilled water and filtered until the filtrate was neutral (pH 7), and dried in a vacuum oven at 80 ℃ for 12 hours;
(3) adding a proper amount of urea into the dried material in the step (2), dissolving the urea in water to form a suspension, magnetically stirring the suspension for 30min, transferring the suspension into an oven to react for 20 hours at 110 ℃, annealing the suspension in a furnace at 1200 ℃ in the atmosphere of nitrogen for 3 hours, and finally screening the product to remove large particles to obtain the high-rate graphite cathode material, wherein the performance parameters are as follows: the first discharge capacity of the half cell is 350.3mAh/g, and the first efficiency is 93.2%; the charging multiplying power is more than 5C, and the capacity is kept at 80%; the discharge multiplying power is more than 12C, and the capacity is kept at 80%.
Comparative example 2
(1) Adding 5mol/L KOH into the artificial graphite until the graphite is completely soaked, heating the artificial graphite to 120 ℃ in a reaction kettle, and continuously stirring for 16 hours for corrosion;
(2) after cooling to room temperature, the filtrate was repeatedly washed with distilled water and filtered until the filtrate was neutral (pH 7), and dried in a vacuum oven at 80 ℃ for 12 hours;
(3) annealing the dried material in the step (2) in a furnace with the atmosphere of ammonia gas and the temperature of 1200 ℃ for 3h, and finally screening the product to remove large particles to obtain the high-rate graphite anode material, wherein the performance parameters are as follows: the first discharge capacity of the half cell is 349.0mAh/g, and the first efficiency is 93.6%; the charging multiplying power is more than 8C, and the capacity is kept at 80%; the discharge rate is more than 10C, and the capacity is kept at 81%.
Claims (10)
1. A preparation method of a high-rate artificial graphite negative electrode material is characterized by comprising the following steps:
(1) adding an alkaline compound into artificial graphite or natural graphite, heating to 80-150 ℃ in a reaction kettle, and continuously stirring for 12-24 hours for erosion;
(2) cooling to room temperature, repeatedly washing with distilled water, filtering until the filtrate is neutral, and drying in a vacuum drying oven at 60-120 deg.C for 8-16 hr;
(3) and (3) annealing the dried material in the step (2) in a furnace with the nitrogen source atmosphere and the temperature of 800-1400 ℃ for 2-6 hours, and finally screening the product to remove large particles to obtain the high-magnification artificial graphite cathode material.
2. The preparation method according to claim 1, wherein the alkali compound in step (1) is an aqueous solution of one or more of KOH and NaOH.
3. The production method according to claim 1, wherein the step (1) is to add an aqueous solution of a basic compound to the artificial graphite or the natural graphite until the graphite is completely impregnated.
4. The process according to claim 2, wherein the concentration of the aqueous solution of the basic compound in the step (1) is 0.1 to 2 mol/L.
5. The process according to claim 2, wherein the concentration of the aqueous solution of the basic compound in the step (1) is 0.1 to 1 mol/L.
6. The process according to claim 2, wherein the concentration of the aqueous solution of the basic compound in the step (1) is 0.1 to 0.5 mol/L.
7. The method according to claim 1, wherein the etching of the basic compound in step (1) is mild etching.
8. The method according to claim 1, wherein the drying temperature in the step (2) is 80 to 120 ℃ and the drying time is 8 to 12 hours.
9. The method according to claim 1, wherein the nitrogen source in step (3) is urea, nitrogen or ammonia gas.
10. The method as claimed in claim 1, wherein the temperature in step (3) is 1000-1200 ℃ and the annealing time is 3-4 hours.
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Cited By (3)
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| CN113611855A (en) * | 2021-07-30 | 2021-11-05 | 山东大学 | Water-soluble inorganic salt modified graphite material and preparation method and application thereof |
| CN113782837A (en) * | 2021-08-03 | 2021-12-10 | 东风悦达起亚汽车有限公司 | Preparation method of high-quality graphene battery |
| CN114068880A (en) * | 2021-11-22 | 2022-02-18 | 安徽科达新材料有限公司 | Preparation method of high-efficiency energy-saving graphite cathode |
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