CN110880599A - Preparation method of high-performance fluorinated peanut shell hard carbon electrode material - Google Patents
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Abstract
The invention discloses a preparation method of a high-performance fluorinated peanut shell hard carbon electrode material, which comprises the steps of crushing peanut shells, cleaning the crushed peanut shells with deionized water once, and removing water-soluble impurities; soaking in a KOH solution for activation, drying, pyrolyzing at high temperature for 4-6 hours under the protection of inert gas, and cooling to room temperature after pyrolysis is finished to obtain a pyrolytic carbon material; washing to be neutral, drying, grinding into powder, fluorinating the pyrolytic carbon material obtained after the step 4 by adopting a gas phase fluorination method, wherein the fluorination gas is a mixed gas of fluorine gas and nitrogen, the fluorination temperature is 200-300 ℃, the heat preservation time is 3-5 hours, and cooling is carried out after the fluorination is finished to obtain the pyrolytic carbon material; uniformly mixing the carbon fluoride material, carbon black and a binder in proportion, uniformly coating the mixture on an aluminum foil by utilizing NMP (N-methyl pyrrolidone), and drying to obtain the high-performance fluorinated peanut shell hard carbon electrode material. The carbon fluoride material with high energy density can be obtained by the method and used for the lithium primary battery, and the specific capacity of the battery can be obviously improved.
Description
Technical Field
The invention belongs to the technical field of carbon composite materials, and particularly relates to a preparation method of a high-performance fluorinated peanut shell hard carbon electrode material.
Background
In recent years, due to global demand for clean sustainable energyFor example, energy storage technology for rechargeable batteries of electric vehicles, portable electronic products, and large-scale electric energy storage devices is receiving attention. Rechargeable Lithium Ion Batteries (LIBs) dominate in the following fields. Portable electronic devices are considered to be the first choice candidates for electric vehicle energy supply. However, LIB is not suitable for large scale electrical energy storage due to limited mineral reserves and high cost of lithium-based compounds. To solve this problem, rechargeable sodium ion batteries (NIBs) have recently attracted the attention of researchers due to their low cost, abundant sodium resources. Due to the similar intercalation chemistry of lithium and sodium ions, various carbonaceous materials such as graphitic carbon, amorphous carbon (hard and soft carbons, etc., nanostructured carbon, graphene and carbon nanotubes, etc.)) have been widely used for NIB applications. Among these carbonaceous materials, hard carbon (non-graphitizing carbon) having a large interlayer distance and a disordered orientation attracts a large amount of carbonaceous materials due to its Li+/Na+The benefits of insertion-extraction, the advantages of high capacity and fast rate capability are of great interest, however its rate performance is not satisfactory. In addition, hard carbon is generally obtained by pyrolysis of important industrial products such as sucrose, glucose, polyvinyl chloride (PVC), and the like. Researchers have sought and sought suitable pyrolysis processes to improve cycle performance.
In recent years, biomass waste as a carbon source has been receiving attention because of its abundance, low cost and sustainability. Carbonaceous materials made from bamboo, peat moss, banana peel and pomelo peel have proven to be excellent electrode materials for LIB and/or NIB applications. As one of the important biomass waste products, about 600 million tons of peanut shells are produced worldwide each year, most of which are not fully utilized. Pyrolysis of peanut hulls for LIB applications has been previously studied and the resulting carbon was found to have over 380mAh g at 70 cycles-1The specific capacity of (A).
One-dimensional (1D) nanostructures provide a direct path for efficient charge transport along their microscale axis, while two very small nanoscale dimensions greatly reduce ion diffusion length. Due to its unique advantages, 1D nanostructures have fast rate capabilities and have been extensively studied for use in electrochemical energy storage devices. Carbon Nanotubes (CNTs) have unique structural and electronic properties, such as good electrical conductivity and high surface area to weight ratio and the ability to form three-dimensional conductive networks. Fluorinated carbon nanotubes (F-CNTs) can be expected to have potential use as high energy density cathode materials for Li/CFx batteries, particularly for deeply fluorinated batteries. It has been demonstrated that F-CNTs exhibit stable operating potential and Faraday yield at low discharge rates. However, carbon nanotubes are expensive and not suitable for large-scale use, and the preparation of hard carbon from biomass with wide sources becomes the research focus of many scientists.
The above prior art has the following disadvantages:
1. the rate capability is poor;
2. the production cost is high;
3. the capacity is small.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a high-performance fluorinated peanut shell hard carbon electrode material.
The invention is realized by the following technical scheme:
a preparation method of a high-performance fluorinated peanut shell hard carbon electrode material comprises the following steps:
step 1, crushing peanut shells, namely crushing the peanut shells to be less than 5mm, and cleaning the crushed peanut shells once by using deionized water to remove part of water-soluble impurities;
step 4, washing and drying, washing the pyrolytic carbon material to be neutral by deionized water, drying and grinding into powder;
step 5, fluorination, namely, carrying out fluorination on the pyrolytic carbon material obtained after the step 4 by adopting a gas phase fluorination method, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 15-20 vol%, the fluorination temperature is 200-300 ℃, the heat preservation time is 3-5 hours, and cooling to room temperature after the fluorination is finished to obtain the fluorinated carbon material;
and 6, preparing an electrode, namely uniformly mixing the carbon fluoride material, carbon black and a binder according to the mass ratio of 7-8: 1:1, uniformly coating the mixture on an aluminum foil by using N-methylpyrrolidone (NMP), drying the aluminum foil for 10-12 hours in a vacuum drying oven, wherein the relative vacuum degree is-110 to-90 KPa, and the temperature is 90-110 ℃, so as to obtain the high-performance fluorinated peanut shell hard carbon electrode material.
In the technical scheme, in the step 1, the peanut shell is crushed to 2-4 mm, and the crushed peanut shell is soaked in deionized water for 2-3 hours to remove part of water-soluble impurities.
In the technical scheme, in the step 2, activation, the peanut shells obtained in the step 1 are soaked in a 7 wt% KOH solution for activation for 1.5 to 3 hours, and then the peanut shells are placed in an oven at 50 to 80 ℃ for drying for 2 to 3 hours, wherein the using amount of the KOH solution is 2 to 4 times of the mass of the peanut shells;
in the technical scheme, in the step 3, the peanut shells obtained in the step 2 are pyrolyzed for 4-6 hours at 700-900 ℃ under the protection of argon, the heating rate is 5-10 ℃ per minute, and the pyrolyzed carbon materials are obtained by naturally cooling to room temperature after pyrolysis.
In the technical scheme, in the step 4, the pyrolytic carbon material is washed to be neutral by deionized water, dried for 2-3 hours at 50-80 ℃, and ground into powder after drying.
In the above technical scheme, in the step 5, the pyrolytic carbon material obtained after completion of the step 4 is placed into a fluorination furnace, the pressure in the fluorination furnace is reduced to a relative vacuum degree of-0.10 to-0.12 MPa, the temperature is increased to 200 to 300 ℃, the temperature increase rate is 5 to 10 ℃ per minute, after the temperature increase is finished, the fluorination furnace is vacuumized again to a relative vacuum degree of-0.1 to-0.12 MPa, so as to remove gas impurities such as water vapor, and a fluorinated gas is introduced until the pressure in the fluorination furnace is increased to an atmospheric pressure, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen, the volume fraction of the mixed gas is 15 to 20 vol%, the heat preservation time is 3 to 5 hours, and the temperature is reduced to room temperature after the fluorination is finished, so that the fluorinated carbon material is obtained.
In the above technical scheme, in the step 6, the binder is an aqueous solution of polyvinylidene fluoride, and the concentration of the aqueous solution of polyvinylidene fluoride is 0.1-0.2 g/ml.
In the technical scheme, in the step 6, electrode preparation, the carbon fluoride material, carbon black and 0.1 g/ml aqueous solution of polyvinylidene fluoride are uniformly mixed according to the mass ratio of 8:1:1, N-methyl pyrrolidone (NMP) is uniformly coated on an aluminum foil, and the aluminum foil is dried in a vacuum drying oven for 12 hours at the relative vacuum degree of-0.1 MPa and the temperature of 110 ℃ to obtain the high-performance fluorinated peanut shell hard carbon electrode material.
A preparation method of a high-performance fluorinated peanut shell hard carbon electrode material comprises the following steps:
step 1, crushing peanut shells, namely crushing the peanut shells to be less than 3mm, and soaking the crushed peanut shells in deionized water for 2 hours to remove part of water-soluble impurities;
step 4, washing and drying, namely washing the pyrolytic carbon material to be neutral by using deionized water, drying for 3 hours at 80 ℃, and grinding into powder after drying;
step 5, fluorination, namely putting the pyrolytic carbon material obtained after the completion of the step 4 into a fluorination furnace, reducing the pressure in the fluorination furnace to-0.1 MPa of relative vacuum degree, heating to 300 ℃, heating at a heating rate of 10 ℃ per minute, vacuumizing the fluorination furnace again to-0.1 MPa of relative vacuum degree after the heating is finished so as to remove gas impurities such as water vapor, introducing a fluorinated gas until the pressure in the fluorination furnace is increased to one atmospheric pressure, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 15-20 vol%, keeping the temperature for 4 hours, and reducing the temperature to room temperature after the fluorination is finished so as to obtain the fluorinated carbon material;
and 6, preparing an electrode, namely uniformly mixing the carbon fluoride material with carbon black and a polyvinylidene fluoride aqueous solution with the concentration of 0.1 g/ml according to the mass ratio of 8:1:1, uniformly coating the mixture on an aluminum foil by utilizing N-methylpyrrolidone (NMP), drying the mixture for 12 hours in a vacuum drying oven at the relative vacuum degree of-0.1 MPa and the temperature of 110 ℃, and obtaining the high-performance fluorinated peanut shell hard carbon electrode material.
The high-performance fluorinated peanut shell hard carbon electrode material prepared by the preparation method of the high-performance fluorinated peanut shell hard carbon electrode material.
The invention has the advantages and beneficial effects that: high capacity and low cost.
Drawings
FIG. 1 is a cyclic voltammogram of example 1 of the present invention.
The solid line, the dot-dash line and the dotted line represent the cyclic voltammetry curves of 1 st, 2 nd and 3 rd times, respectively. The upper three curves represent the reduction peaks and the lower three curves represent the oxidation peaks.
FIG. 2 is a constant current charge and discharge curve of example 1 of the present invention.
The charging curves sequentially correspond to a 1 st charging curve, a 2 nd charging curve, a 3 rd charging curve, a 5 th charging curve and a 10 th charging curve from right to left.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
Example one
A preparation method of a high-performance fluorinated peanut shell hard carbon electrode material comprises the following steps:
step 1, crushing peanut shells, namely crushing the peanut shells to be less than 3mm, and soaking the crushed peanut shells in deionized water for 2 hours to remove part of water-soluble impurities;
step 4, washing and drying, namely washing the pyrolytic carbon material to be neutral by using deionized water, drying for 3 hours at 80 ℃, and grinding into powder after drying;
step 5, fluorination, namely putting the pyrolytic carbon material obtained after the completion of the step 4 into a fluorination furnace, reducing the pressure in the fluorination furnace to-0.1 MPa of relative vacuum degree, heating to 300 ℃, heating at a heating rate of 10 ℃ per minute, vacuumizing the fluorination furnace again to-0.1 MPa of relative vacuum degree after the heating is finished so as to remove gas impurities such as water vapor, introducing a fluorinated gas until the pressure in the fluorination furnace is increased to one atmospheric pressure, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 15 vol%, keeping the temperature for 4 hours, and reducing the temperature to room temperature after the fluorination is finished so as to obtain the pyrolytic carbon material;
and 6, preparing an electrode, namely placing 80mg of the carbon fluoride material and 10mg of carbon black in a mortar for fully grinding, then dropwise adding a few drops of N-methyl pyrrolidone (NMP) to form viscous slurry, adding 100 microliters of 0.1 gram/milliliter aqueous solution of polyvinylidene fluoride by using a liquid transfer gun, continuously grinding, pouring the slurry on an aluminum foil, padding a layer of plastic diaphragm on the aluminum foil, rolling the electrode slurry by using a rolling pin, and placing the electrode slurry in a vacuum drying oven for drying for 12 hours at the relative vacuum degree of-0.1 MPa and the temperature of 110 ℃ to obtain the high-performance fluorinated peanut shell hard carbon electrode material.
And (4) cutting the high-performance fluorinated peanut shell hard carbon electrode material into a 12mm round piece, and assembling the round piece into the button cell. The battery is assembled by a positive electrode cover, a negative electrode cover, a lithium sheet, a diaphragm, a positive electrode sheet (a high-performance fluorinated peanut shell hard carbon electrode material wafer) and an electrolyte (LiPF6 is used as a solute, and a solvent is diethyl carbonate and dimethyl carbonate in a volume ratio of 1: 1) and is tested.
As can be seen from the cyclic voltammetry curves of fig. 1:
the solid line is the first scan, and from the upper convex part of the oxidation peak curve, it can be known that the SEI (solid electrolyte membrane) film is formed, and in the cycle thereafter, the curve is smooth, indicating that the electrode reaction is normally proceeding, and the cycle performance is stable.
As can be seen from the constant current charge-discharge curve of fig. 2:
the first discharge cycle can show that the capacity reaches 350mAh/g, which indicates that the fluorinated peanut shell pyrolytic hard carbon has high specific capacity, and the capacity is kept about 200mAh/g in the subsequent discharge test, and the reduction reason is probably caused by the reduction of the number of active sites inserted by lithium ions due to the lattice distortion of the fluorinated carbon.
The embodiment has the advantages that the carbon fluoride material with high energy density can be obtained, and the carbon fluoride material can be used for the lithium primary battery and can obviously improve the specific capacity of the battery.
Example 2
A preparation method of a high-performance fluorinated peanut shell hard carbon electrode material comprises the following steps:
step 1, crushing peanut shells, namely crushing the peanut shells to be less than 5mm, and soaking the crushed peanut shells in deionized water for 3 hours to remove part of water-soluble impurities;
step 4, washing and drying, namely washing the pyrolytic carbon material to be neutral by using deionized water, drying for 3 hours at 60 ℃, and grinding into powder after drying;
step 5, fluorination, namely putting the pyrolytic carbon material obtained after the completion of the step 4 into a fluorination furnace, reducing the pressure in the fluorination furnace to-0.12 MPa of relative vacuum degree, heating to 300 ℃, heating at a heating rate of 10 ℃ per minute, vacuumizing the fluorination furnace again to-0.12 MPa of relative vacuum degree after the heating is finished so as to remove gas impurities such as water vapor, introducing a fluorinated gas until the pressure in the fluorination furnace is increased to one atmospheric pressure, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 20 vol%, keeping the temperature for 5 hours, and reducing the temperature to room temperature after the fluorination is finished so as to obtain the pyrolytic carbon material;
and 6, preparing an electrode, namely placing 80mg of the carbon fluoride material and 10mg of carbon black in a mortar for fully grinding, then dropwise adding a few drops of N-methyl pyrrolidone (NMP) to form viscous slurry, adding 100 microliters of 0.1 gram/milliliter aqueous solution of polyvinylidene fluoride by using a liquid transfer gun, continuously grinding, pouring the slurry on an aluminum foil, padding a layer of plastic diaphragm on the aluminum foil, rolling the electrode slurry by using a rolling pin, and placing the electrode slurry in a vacuum drying oven for drying for 12 hours at the relative vacuum degree of-0.1 MPa and the temperature of 110 ℃ to obtain the high-performance fluorinated peanut shell hard carbon electrode material.
And (4) cutting the high-performance fluorinated peanut shell hard carbon electrode material into a 12mm round piece, and assembling the round piece into the button cell. The battery is assembled by a positive electrode cover, a negative electrode cover, a lithium sheet, a diaphragm, a positive electrode sheet (a high-performance fluorinated peanut shell hard carbon electrode material 12mm round sheet) and an electrolyte (LiPF6 is used as a solute, and a solvent is diethyl carbonate to dimethyl carbonate in a volume ratio of 1: 1) and is tested.
Example 3
A preparation method of a high-performance fluorinated peanut shell hard carbon electrode material comprises the following steps:
step 1, crushing peanut shells, namely crushing the peanut shells to be less than 2mm, and soaking the crushed peanut shells in deionized water for 3 hours to remove part of water-soluble impurities;
step 4, washing and drying, namely washing the pyrolytic carbon material to be neutral by using deionized water, drying for 3 hours at 70 ℃, and grinding into powder after drying;
step 5, fluorination, namely putting the pyrolytic carbon material obtained after the completion of the step 4 into a fluorination furnace, reducing the pressure in the fluorination furnace to-0.10 MPa of relative vacuum degree, heating to 300 ℃ at a heating rate of 10 ℃ per minute, vacuumizing the fluorination furnace again to-0.10 MPa of relative vacuum degree after the heating is finished so as to remove gas impurities such as water vapor, introducing a fluorinated gas until the pressure in the fluorination furnace is increased to one atmosphere, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 18 vol%, and keeping the temperature for 3.5 hours, and reducing the temperature to room temperature after the fluorination is finished so as to obtain the fluorinated carbon material;
and 6, preparing an electrode, namely placing 80mg of the carbon fluoride material and 10mg of carbon black in a mortar for fully grinding, then dropwise adding a few drops of N-methyl pyrrolidone (NMP) to form viscous slurry, adding 100 microliters of 0.1 gram/milliliter aqueous solution of polyvinylidene fluoride by using a liquid transfer gun, continuously grinding, pouring the slurry on an aluminum foil, padding a layer of plastic diaphragm on the aluminum foil, rolling the electrode slurry by using a rolling pin, and placing the electrode slurry in a vacuum drying oven for drying for 12 hours at the relative vacuum degree of-0.1 MPa and the temperature of 110 ℃ to obtain the high-performance fluorinated peanut shell hard carbon electrode material.
And (4) cutting the high-performance fluorinated peanut shell hard carbon electrode material into a 12mm round piece, and assembling the round piece into the button cell. The battery is assembled by a positive electrode cover, a negative electrode cover, a lithium sheet, a diaphragm, a positive electrode sheet (a high-performance fluorinated peanut shell hard carbon electrode material 12mm round sheet) and an electrolyte (LiPF6 is used as a solute, and a solvent is diethyl carbonate to dimethyl carbonate in a volume ratio of 1: 1) and is tested.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. A preparation method of a high-performance fluorinated peanut shell hard carbon electrode material is characterized by comprising the following steps:
step 1, crushing peanut shells, namely crushing the peanut shells to be less than 5mm, and cleaning the crushed peanut shells once by using deionized water to remove part of water-soluble impurities;
step 2, activating, namely soaking the peanut shells obtained in the step 1 in a 5-7 wt% KOH solution for activation, and then drying, wherein the using amount of the KOH solution is 2-4 times of the mass of the peanut shells;
step 3, performing pyrolysis, namely pyrolyzing the peanut shells obtained in the step 2 for 4-6 hours at 700-900 ℃ under the protection of inert gas, and cooling to room temperature after pyrolysis is completed to obtain a pyrolytic carbon material;
step 4, washing and drying, washing the pyrolytic carbon material to be neutral by deionized water, drying and grinding into powder;
step 5, fluorination, namely, carrying out fluorination on the pyrolytic carbon material obtained after the step 4 by adopting a gas phase fluorination method, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 15-20 vol%, the fluorination temperature is 200-300 ℃, the heat preservation time is 3-5 hours, and cooling to room temperature after the fluorination is finished to obtain the fluorinated carbon material;
and 6, preparing an electrode, namely uniformly mixing the carbon fluoride material, carbon black and a binder according to the mass ratio of 7-8: 1:1, uniformly coating the mixture on an aluminum foil by using N-methylpyrrolidone (NMP), drying the aluminum foil for 10-12 hours in a vacuum drying oven, wherein the relative vacuum degree is-110 to-90 KPa, and the temperature is 90-110 ℃, so as to obtain the high-performance fluorinated peanut shell hard carbon electrode material.
2. The method for preparing the high-performance fluorinated peanut shell hard carbon electrode material as claimed in claim 1, wherein in the step 1, the peanut shell is crushed to 2-4 mm, and the crushed peanut shell is soaked in deionized water for 2-3 hours to remove part of water-soluble impurities.
3. The preparation method of the high-performance fluorinated peanut shell hard carbon electrode material as claimed in claim 1, wherein in the step 2, activation, the peanut shell obtained in the step 1 is soaked in 7 wt% KOH solution for activation for 1.5-3 hours, and then is dried in an oven at 50-80 ℃ for 2-3 hours, and the amount of the KOH solution is 2-4 times of the mass of the peanut shell.
4. The preparation method of the high-performance fluorinated peanut shell hard carbon electrode material as claimed in claim 1, wherein in the step 3, the peanut shell obtained in the step 2 is pyrolyzed at 700-900 ℃ for 4-6 hours under the protection of argon gas, the temperature rise rate is 5-10 ℃ per minute, and the pyrolyzed carbon material is obtained by naturally cooling to room temperature after pyrolysis.
5. The method for preparing the high-performance fluorinated peanut shell hard carbon electrode material as claimed in claim 1, wherein in the step 4, the pyrolytic carbon material is washed to be neutral by deionized water, dried for 2-3 hours at 50-80 ℃, and ground into powder after being dried.
6. The method for preparing a high-performance fluorinated peanut shell hard carbon electrode material as claimed in claim 1, wherein in the step 5, the pyrolytic carbon material obtained after the step 4 is completed is placed into a fluorination furnace, the pressure in the fluorination furnace is reduced to a relative vacuum degree of-0.10 to-0.12 MPa, the temperature is raised to 200 to 300 ℃, the temperature raising rate is 5 to 10 ℃ per minute, the fluorination furnace is vacuumized again to a relative vacuum degree of-0.1 to-0.12 MPa after the temperature raising is finished, gas impurities such as water vapor and the like are removed, the pressure in the fluorination furnace is increased to one atmosphere by introducing fluorinated gas, the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 15 to 20 vol%, the heat preservation time is 3 to 5 hours, and the temperature is reduced to room temperature after the fluorination is finished, so that the fluorinated carbon material is obtained.
7. The method for preparing the high-performance fluorinated peanut shell hard carbon electrode material as claimed in claim 1, wherein in the step 6, the binder is an aqueous solution of polyvinylidene fluoride, and the concentration of the aqueous solution of polyvinylidene fluoride is 0.1-0.2 g/ml.
8. The preparation method of the high-performance fluorinated peanut shell hard carbon electrode material as claimed in claim 1, wherein in the step 6, the electrode is prepared by uniformly mixing the carbon fluoride material, carbon black and 0.1 g/ml polyvinylidene fluoride aqueous solution according to a mass ratio of 8:1:1, uniformly coating the mixture on an aluminum foil by using N-methylpyrrolidone (NMP), and drying the mixture in a vacuum drying oven for 12 hours at a relative vacuum degree of-0.1 MPa and a temperature of 110 ℃ to obtain the high-performance fluorinated peanut shell hard carbon electrode material.
9. A preparation method of a high-performance fluorinated peanut shell hard carbon electrode material is characterized by comprising the following steps:
step 1, crushing peanut shells, namely crushing the peanut shells to be less than 3mm, and soaking the crushed peanut shells in deionized water for 2 hours to remove part of water-soluble impurities;
step 2, activating, namely soaking the peanut shells obtained in the step 1 in a 7 wt% KOH solution for 2 hours, and then drying the peanut shells in an oven at 80 ℃ for 2 hours, wherein the using amount of the KOH solution is 2-4 times of the mass of the peanut shells;
step 3, performing pyrolysis, namely pyrolyzing the peanut shells obtained in the step 2 for 5 hours at 800 ℃ under the protection of inert gas, wherein the heating rate is 5-10 ℃ per minute, and cooling to room temperature after pyrolysis is completed to obtain a pyrolytic carbon material;
step 4, washing and drying, namely washing the pyrolytic carbon material to be neutral by using deionized water, drying for 3 hours at 80 ℃, and grinding into powder after drying;
step 5, fluorination, namely putting the pyrolytic carbon material obtained after the completion of the step 4 into a fluorination furnace, reducing the pressure in the fluorination furnace to-0.1 MPa of relative vacuum degree, heating to 300 ℃, heating at a heating rate of 10 ℃ per minute, vacuumizing the fluorination furnace again to-0.1 MPa of relative vacuum degree after the heating is finished so as to remove gas impurities such as water vapor, introducing a fluorinated gas until the pressure in the fluorination furnace is increased to one atmospheric pressure, wherein the fluorinated gas is a mixed gas of fluorine gas and nitrogen gas, the volume fraction of the fluorine gas in the mixed gas is 15-20 vol%, keeping the temperature for 4 hours, and reducing the temperature to room temperature after the fluorination is finished so as to obtain the fluorinated carbon material;
and 6, preparing an electrode, namely uniformly mixing the carbon fluoride material with carbon black and a polyvinylidene fluoride aqueous solution with the concentration of 0.1 g/ml according to the mass ratio of 8:1:1, uniformly coating the mixture on an aluminum foil by utilizing N-methylpyrrolidone (NMP), drying the mixture for 12 hours in a vacuum drying oven at the relative vacuum degree of-0.1 MPa and the temperature of 110 ℃, and obtaining the high-performance fluorinated peanut shell hard carbon electrode material.
10. A high performance fluorinated peanut shell hard carbon electrode material prepared by the method of preparing a high performance fluorinated peanut shell hard carbon electrode material according to any one of claims 1 to 9.
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| CN112002881A (en) * | 2020-07-30 | 2020-11-27 | 国网浙江省电力有限公司电力科学研究院 | Hard carbon composite material and preparation method and application thereof |
| CN112331848A (en) * | 2020-11-10 | 2021-02-05 | 厦门永力鑫新能源科技有限公司 | Carbon fluoride material with core-shell structure, preparation method thereof and lithium battery |
| CN113422059A (en) * | 2021-06-17 | 2021-09-21 | 贵州梅岭电源有限公司 | High-voltage carbon fluoride composite cathode material and preparation method thereof |
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| CN113451561B (en) * | 2021-08-30 | 2022-02-15 | 北京壹金新能源科技有限公司 | Silicon-based composite material and preparation method and application thereof |
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| CN116632233A (en) * | 2023-07-19 | 2023-08-22 | 成都锂能科技有限公司 | High-performance sodium ion battery doped hard carbon negative electrode material and preparation method thereof |
| CN116632233B (en) * | 2023-07-19 | 2023-09-29 | 成都锂能科技有限公司 | High-performance sodium ion battery doped hard carbon negative electrode material and preparation method thereof |
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