CN110911665A - Boron and nitrogen doped lithium ion battery negative electrode material and preparation method thereof - Google Patents
Boron and nitrogen doped lithium ion battery negative electrode material and preparation method thereof Download PDFInfo
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- CN110911665A CN110911665A CN201911149943.XA CN201911149943A CN110911665A CN 110911665 A CN110911665 A CN 110911665A CN 201911149943 A CN201911149943 A CN 201911149943A CN 110911665 A CN110911665 A CN 110911665A
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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
- H01M4/58—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- 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
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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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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 provides a preparation method of a boron and nitrogen doped lithium ion battery cathode material, which comprises the following steps: 1) mixing melamine, ammonium borate, ethyl orthosilicate, hydrochloric acid, deionized water and ethanol to obtain colloidal precursor solution; 2) heating the colloidal precursor solution obtained in the step 1) to convert the colloidal precursor solution into compound particles, washing and drying to obtain an intermediate product; 3) and (3) carbonizing the intermediate product in the step 2) in an inert atmosphere, and performing ball milling treatment on the carbonized product doped with graphite to obtain the boron and nitrogen doped lithium ion battery cathode material. The preparation method provided by the invention is simple in process, and the prepared cathode material shows stable electrochemical cycling stability and rate capability.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a boron and nitrogen doped lithium ion battery cathode material and a preparation method thereof.
Background
At present, graphite is widely used as a commercial lithium ion battery cathode material, but the theoretical capacity of the graphite cathode material is only 372mA · h/g, the capacity is lower in the actual use process, and the requirements of people on the high-capacity and high-stability lithium ion battery electrode material cannot be met. Silicon as an electrode material of a lithium ion battery with great potential has a theoretical capacity as high as 4200mA · h/g, but practical application of the silicon is greatly limited by low conductivity and volume effect in the charging and discharging processes. Related researches find that the introduction of elements such as boron, nitrogen and the like has more or less influence on the capacity or stability of the electrode material.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a preparation method of a boron and nitrogen doped lithium ion battery cathode material.
The purpose of the invention can be realized by the following technical scheme: a preparation method of a boron and nitrogen doped lithium ion battery negative electrode material comprises the following steps:
1) mixing melamine, ammonium borate, ethyl orthosilicate, hydrochloric acid, deionized water and ethanol to obtain colloidal precursor solution;
2) heating the colloidal precursor solution obtained in the step 1) to convert the colloidal precursor solution into compound particles, washing and drying to obtain an intermediate product;
3) and (3) carbonizing the intermediate product in the step 2) in an inert atmosphere, doping a certain proportion of graphite into the carbonized product, and performing ball milling treatment to obtain the boron and nitrogen doped lithium ion battery cathode material.
On the basis of the technical scheme, the invention can further have the following specific selection or optimized selection.
Specifically, the mixing is performed under room temperature conditions for 1 hour.
Specifically, the dosage ratio of the melamine, the ammonium borate, the ethyl orthosilicate, the hydrochloric acid, the deionized water and the ethanol is that each gram of melamine corresponds to 0.6-1.2g of the ammonium borate, 2-3g of the ethyl orthosilicate, 1-2mL of the hydrochloric acid, 10-20mL of the deionized water and 10-20mL of the ethanol; wherein the concentration of hydrochloric acid is 0.05-0.15M.
Specifically, the heating refers to placing the colloidal precursor solution into a heating furnace for heating, wherein the heating furnace is a muffle furnace, the heating temperature is 400-.
Specifically, the washing refers to washing 3-5 times by deionized water. The drying refers to heating and drying at a higher temperature, and conventional laboratory drying parameters are adopted. The washing uses an excess of deionized water, typically 3-5 times the material being washed.
Specifically, the intermediate product is heated and carbonized in an inert atmosphere, wherein the heating and carbonization refer to the carbonization of the intermediate product in a vacuum tube type atmosphere furnace, the heating temperature is 800-950 ℃, the heating rate is 5-10 ℃/min, the heat preservation time is 2-4h, and the inert atmosphere is nitrogen or argon.
Specifically, the doping amount of the graphite is 10-35% by mass of the obtained boron and nitrogen doped lithium ion battery negative electrode material, and the ball milling treatment time is 1-3 h. Specifically, the doping amount of the graphite is 10-35% of the whole mass, the mass of the intermediate product is 65-90%, namely the mass ratio of the graphite to the intermediate product is 10-35: 65-90.
In addition, the invention also provides the boron and nitrogen doped lithium ion battery cathode material prepared by the preparation method of the boron and nitrogen doped lithium ion battery cathode material.
In addition, the invention also provides application of the boron and nitrogen doped lithium ion battery negative electrode material in a lithium battery.
Compared with the prior art, the invention has the beneficial effects that:
(1) the three raw materials of melamine, ammonium borate and tetraethoxysilane in the method provided by the invention are common raw materials in industry, the price is low, and the preparation method is simple in process and suitable for industrial large-scale production.
(2) The boron and nitrogen doped lithium ion battery cathode material prepared by the method has extremely strong cycle stability and rate capability.
Drawings
FIG. 1 is an electron microscope scanning image of the cathode material of the boron and nitrogen doped lithium ion battery prepared by the invention;
FIG. 2 is a diagram of electrochemical performance of the boron and nitrogen doped lithium ion battery negative electrode material prepared by the invention.
Detailed Description
For a better understanding of the present invention, the following further illustrates the present invention with reference to the accompanying drawings and specific examples, but the present invention is not limited to the following examples.
The invention provides a preparation method of a boron and nitrogen doped lithium ion battery cathode material, which comprises the following steps:
1) mixing melamine, ammonium borate, ethyl orthosilicate, hydrochloric acid, deionized water and ethanol to obtain colloidal precursor solution;
2) heating the colloidal precursor solution obtained in the step 1) to convert the colloidal precursor solution into compound particles, washing and drying to obtain an intermediate product;
3) and (3) carbonizing the intermediate product in the step 2) in an inert atmosphere, doping a certain proportion of graphite into the carbonized product, and performing ball milling treatment to obtain the boron and nitrogen doped lithium ion battery cathode material.
On the basis of the technical scheme, the invention can further have the following specific selection or optimized selection.
Specifically, the mixing is performed under room temperature conditions for 1 hour.
Specifically, the dosage ratio of the melamine, the ammonium borate, the ethyl orthosilicate, the hydrochloric acid, the deionized water and the ethanol is that each gram of melamine corresponds to 0.6-1.2g of the ammonium borate, 2-3g of the ethyl orthosilicate, 1-2mL of the hydrochloric acid, 10-20mL of the deionized water and 10-20mL of the ethanol; wherein the concentration of hydrochloric acid is 0.05-0.15M.
Specifically, the heating refers to placing the colloidal precursor solution into a heating furnace for heating, wherein the heating furnace is a muffle furnace, the heating temperature is 400-.
Specifically, the washing is 3-5 times of washing with deionized water of 3-5 times. The drying refers to heating and drying at a higher temperature, and conventional laboratory drying parameters are adopted.
Specifically, the step of carbonizing in an inert atmosphere refers to that the intermediate product is put into a vacuum tube type atmosphere furnace for carbonizing, the heating temperature is 800-950 ℃, the heating rate is 5-10 ℃/min, the heat preservation time is 2-4h, and the inert atmosphere is nitrogen or argon.
Specifically, the doping amount of the graphite is 10-35% by mass of the obtained boron and nitrogen doped lithium ion battery negative electrode material, and the ball milling treatment time is 1-3 h.
In addition, the invention also provides a boron and nitrogen doped lithium ion battery cathode material prepared by the preparation method of the boron and nitrogen doped lithium ion battery cathode material.
In addition, the invention also provides application of the boron and nitrogen doped lithium ion battery negative electrode material in a lithium battery.
Example 1
1.8g of melamine, 1.24g of ammonium borate, 4.2g of ethyl orthosilicate, 2mL of 0.05M hydrochloric acid, 15mL of deionized water and 15mL of ethanol were mixed and stirred at room temperature for 1 hour to obtain a colloidal precursor solution. And transferring the colloidal precursor solution into a muffle furnace, heating at 450 ℃, heating at a rate of 10 ℃/min, and keeping the temperature for 2h to convert the colloidal precursor solution into compound particles. And transferring the compound particles into a vacuum tube type nitrogen atmosphere furnace, heating at the rate of 10 ℃/min and the temperature of 900 ℃, keeping the temperature for 3 hours, cooling along with the furnace, and ball-milling the obtained sample and 20% graphite for 1 hour to obtain the boron and nitrogen doped lithium ion battery cathode material.
Example 2
1.8g of melamine, 1.5g of ammonium borate, 3.6g of ethyl orthosilicate, 2mL of 0.1M hydrochloric acid, 10mL of deionized water and 10mL of ethanol were mixed and stirred at room temperature for 1 hour to obtain a colloidal precursor solution. And transferring the colloidal precursor solution into a muffle furnace, heating at 400 ℃, heating at a rate of 12 ℃/min, and keeping the temperature for 1h to convert the colloidal precursor solution into compound particles. And transferring the compound particles into a vacuum tube type argon atmosphere furnace, heating at the rate of 5 ℃/min and the temperature of 800 ℃, keeping the temperature for 2 hours, cooling along with the furnace, and ball-milling the obtained sample and 10% graphite for 2 hours to obtain the boron and nitrogen doped lithium ion battery cathode material.
Example 3
1.8g of melamine, 1.8g of ammonium borate, 4.68g of ethyl orthosilicate, 2mL of 0.05M hydrochloric acid, 12mL of deionized water and 12mL of ethanol were mixed and stirred at room temperature for 1 hour to obtain a colloidal precursor solution. And transferring the colloidal precursor solution into a muffle furnace, heating to 470 ℃, heating at the rate of 8 ℃/min, and keeping the temperature for 3h to convert the colloidal precursor solution into compound particles. And transferring the compound particles into a vacuum tube type nitrogen atmosphere furnace, heating at the rate of 8 ℃/min and the temperature of 850 ℃, keeping the temperature for 4 hours, cooling along with the furnace, and ball-milling the obtained sample and 35% graphite for 3 hours to obtain the boron and nitrogen doped lithium ion battery cathode material.
Example 4
1.8g of melamine, 2.05g of ammonium borate, 4.86g of ethyl orthosilicate, 2mL of 0.08M hydrochloric acid, 18mL of deionized water and 18mL of ethanol were mixed and stirred at room temperature for 1 hour to obtain a colloidal precursor solution. And transferring the colloidal precursor solution into a muffle furnace, heating at 500 ℃, heating at a rate of 15 ℃/min, and keeping the temperature for 1.5h to convert the colloidal precursor solution into compound particles. And transferring the compound particles into a vacuum tube type nitrogen atmosphere furnace, heating at the rate of 10 ℃/min and the temperature of 950 ℃, keeping the temperature for 4 hours, cooling along with the furnace, and ball-milling the obtained sample and 25% graphite for 2.5 hours to obtain the boron and nitrogen doped lithium ion battery cathode material.
Example 5
1.8g of melamine, 2.14g of ammonium borate, 5.4g of ethyl orthosilicate, 2mL of 0.15M hydrochloric acid, 20mL of deionized water and 20mL of ethanol were mixed and stirred at room temperature for 1 hour to obtain a colloidal precursor solution. And transferring the colloidal precursor solution into a muffle furnace, heating at 400 ℃, heating at a rate of 10 ℃/min, and keeping the temperature for 3h to convert the colloidal precursor solution into compound particles. And transferring the compound particles into a vacuum tube type nitrogen atmosphere furnace, heating at the rate of 5 ℃/min and the temperature of 800 ℃, keeping the temperature for 3.5h, cooling along with the furnace, and ball-milling the obtained sample and 15% graphite for 1.5h to obtain the boron and nitrogen doped lithium ion battery cathode material.
The boron and nitrogen doped lithium ion battery cathode material prepared by the invention has extremely strong cycle stability and rate capability, and is compared with the existing lithium ion battery cathode material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A preparation method of a boron and nitrogen doped lithium ion battery negative electrode material is characterized by comprising the following steps:
1) mixing melamine, ammonium borate, ethyl orthosilicate, hydrochloric acid, deionized water and ethanol to obtain colloidal precursor solution;
2) heating the colloidal precursor solution obtained in the step 1) to convert the colloidal precursor solution into compound particles, washing and drying to obtain an intermediate product;
3) and (3) carbonizing the intermediate product in the step 2) in an inert atmosphere, and performing ball milling treatment on the carbonized product doped with graphite to obtain the boron and nitrogen doped lithium ion battery cathode material.
2. The preparation method of the boron and nitrogen doped lithium ion battery negative electrode material according to claim 1, characterized by comprising the following steps: the mixing means stirring at room temperature for 1 hour.
3. The preparation method of the boron and nitrogen doped lithium ion battery negative electrode material according to claim 1, characterized by comprising the following steps: the dosage ratio of the melamine, the ammonium borate, the ethyl orthosilicate, the hydrochloric acid, the deionized water and the ethanol is that each gram of melamine corresponds to 0.6-1.2g of ammonium borate, 2-3g of ethyl orthosilicate, 1-2mL of hydrochloric acid, 10-20mL of deionized water and 10-20mL of ethanol; wherein the concentration of hydrochloric acid is 0.05-0.15M.
4. The preparation method of the boron and nitrogen doped lithium ion battery negative electrode material according to claim 1, characterized by comprising the following steps: the heating refers to putting the colloidal precursor solution into a heating furnace for heating, wherein the heating furnace is a muffle furnace, the heating temperature is 400-500 ℃, the heating rate is 8-15 ℃/min, and the heat preservation time is 1-3 h.
5. The preparation method of the boron and nitrogen doped lithium ion battery negative electrode material according to claim 1, characterized by comprising the following steps: the washing is 3-5 times by using deionized water.
6. The preparation method of the boron and nitrogen doped lithium ion battery negative electrode material according to any one of claims 1 to 5, characterized by comprising the following steps: the step of carbonizing in an inert atmosphere refers to the step of putting the intermediate product into a vacuum tube type atmosphere furnace for heating and carbonizing, wherein the heating and carbonizing temperature is 800-950 ℃, the heating rate is 5-10 ℃/min, the heat preservation time is 2-4h, and the inert atmosphere is nitrogen or argon.
7. The preparation method of the boron and nitrogen doped lithium ion battery negative electrode material according to any one of claims 1 to 5, characterized by comprising the following steps: the doping amount of the graphite is 10-35% by mass of the obtained boron and nitrogen doped lithium ion battery negative electrode material, and the ball milling treatment time is 1-3 h.
8. A boron and nitrogen doped lithium ion battery negative electrode material, which is prepared by the preparation method of the boron and nitrogen doped lithium ion battery negative electrode material as claimed in any one of claims 1 to 7.
9. Use of the boron and nitrogen doped lithium ion battery negative electrode material of claim 8 in a lithium battery.
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| CN114843470A (en) * | 2022-05-10 | 2022-08-02 | 长沙理工大学 | Preparation method of boron and lanthanum co-modified MCMB as lithium ion battery cathode material |
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