CN112614977B - Lithium ion battery optimization method based on graphene/artificial graphite composite material - Google Patents
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Abstract
A lithium ion battery optimization method based on a graphene/artificial graphite composite material is characterized in that a negative electrode of a lithium ion battery is manufactured by electrodepositing graphene on the surface of artificial graphite particles, namely, a graphene oxide dispersion liquid and an artificial stone ink powder dispersion liquid are mixed and then subjected to electrodeposition reduction, and then the graphene/artificial graphite composite material is extracted from a mixed liquid obtained by reaction. The preparation method is simple to operate, and when the prepared material is used as the lithium ion battery cathode, the material not only has higher first coulombic efficiency, but also has higher specific capacity and better rate capability.
Description
Technical Field
The invention relates to a technology in the field of graphene, in particular to a lithium ion battery optimization method based on a graphene/artificial graphite composite material.
Background
The graphene in the existing lithium ion battery electrode material is mostly applied in the form of a conductive additive, so that the comprehensive performance of the battery is improved. In the electrode material, the coating application is mostly carried out by methods such as chemical modification, ball milling, chemical vapor deposition and the like. The chemical modification process is easy to generate the phenomenon of preferential deposition of sharp corners; the ball milling method has a large reaction system and high energy consumption; the chemical vapor deposition method has low efficiency and high equipment requirement. Electrodeposition is an efficient and uniform surface treatment method, and at present, although studies are made on plating graphene on the surface of an electrode of a lithium ion battery in an electroplating mode, the graphene is acted on the surface of an electrode plate, so that the graphene cannot act on an internal material of the electrode plate, and the graphene is distributed unevenly in the electrode.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the lithium ion battery optimization method based on the graphene/artificial graphite composite material, the operation is simple, and when the prepared material is used as the negative electrode of the lithium ion battery, the lithium ion battery has high first coulombic efficiency, high specific capacity and high rate capability.
The invention is realized by the following technical scheme:
the invention relates to a lithium ion battery optimization method based on a graphene/artificial graphite composite material, which is used for manufacturing a negative electrode of a lithium ion battery based on the artificial graphite particle surface electrodeposition graphene.
Based on the artificial graphite particle surface electrodeposition of graphene, the graphene oxide dispersion liquid and the artificial stone powdered ink dispersion liquid are mixed and subjected to electrodeposition reduction, and then the graphene/artificial graphite composite material is extracted from a mixed solution obtained through reaction.
The negative electrode of the lithium ion battery is prepared by taking N-methyl pyrrolidone (NMP) as a solvent, mixing the graphene/artificial graphite composite material, conductive carbon black and polyvinylidene fluoride (PVDF), adding N-methyl pyrrolidone (NMP) as a solvent, uniformly stirring to form slurry, coating the slurry on the surface of copper foil, and drying.
The mass ratio of the graphene/artificial graphite composite material to the conductive carbon black to the polyvinylidene fluoride (PVDF) is 8:1:1.
The electrodeposition reduction adopts, but is not limited to, in an electroplating device, stainless steel as an anode, a stainless steel cylinder filled with mixed graphene oxide dispersion liquid and artificial stone toner dispersion liquid as a cathode, and voltage is applied in a stirring environment.
The voltage is preferably: 1V to 5V.
The electrodeposition treatment time is preferably: 30 s-60 min.
The stirring speed is preferably as follows: 30 to 80 revolutions per minute.
The graphene oxide dispersion liquid is obtained by ultrasonically dispersing graphene oxide in water.
The artificial stone ink powder dispersion liquid is obtained by ultrasonically dispersing artificial graphite powder in water.
The particle size of the artificial graphite powder comprises: d10：6～8 μm、D5015 to 18 μm and D90:50～60 μm。
The mass ratio of the graphene oxide in the graphene oxide dispersion liquid to the artificial graphite powder in the artificial stone ink powder dispersion liquid is 1: 20-1: 2000.
The extraction adopts, but is not limited to, suction filtration and drying treatment.
The drying is preferably carried out for 24 hours under vacuum at 60 ℃.
The counter electrode of the lithium ion battery adopts but is not limited to metal lithium; the separator adopts but is not limited to a microporous polypropylene film; the electrolyte solution is prepared by, but not limited to, mixing lithium hexafluorophosphate with ethylene carbonate, diethyl carbonate, and methyl ethyl carbonate, and preferably mixing lithium hexafluorophosphate with ethylene carbonate, diethyl carbonate, and methyl ethyl carbonate at the same concentration in a volume ratio of 1:1: 1.
The lithium ion battery is preferably assembled in a glove box filled with high-purity argon.
Technical effects
According to the invention, the graphene layer is deposited on the surface of the high-curvature artificial graphite powder by using an electrodeposition technology, so that the initial coulombic efficiency, specific capacity and rate capability of the artificial graphite powder are effectively improved.
Drawings
FIG. 1 is a SEM photograph of the artificial graphite powder in example 1;
FIG. 2 is a SEM image of the graphene/artificial graphite composite material in example 1;
FIG. 3 is a first charge-discharge curve of a battery prepared by using the artificial graphite powder as a negative electrode material in example 1;
fig. 4 is a first charge-discharge curve of the graphene/artificial graphite composite material as a negative electrode material in example 1.
The specific implementation mode is as follows: example 1
The embodiment comprises the following steps:
adding 1g of artificial graphite powder into 100mL of deionized water, and stirring for 30 min; and adding 1mg of graphene oxide into 100mL of deionized water, ultrasonically stirring for 30min, mixing with the stirred artificial graphite dispersion liquid, and putting into an electroplating device. And carrying out electrodeposition treatment for 1 min under the voltage of 1V, stirring at the speed of 30 r/min, then carrying out suction filtration, and drying in a vacuum drying oven at the temperature of 80 ℃ for 12h to obtain the graphene/artificial graphite composite material.
And secondly, mixing the graphene/artificial graphite composite material, the conductive carbon black and the polyvinylidene fluoride (PVDF) according to a mass ratio of 8:1:1 by taking N-methylpyrrolidone (NMP) as a solvent to obtain a mixture serving as an embodiment, mixing untreated artificial graphite, the conductive carbon black and the PVDF to obtain a comparative example, respectively stirring uniformly to obtain slurry, coating the slurry on the surface of the copper foil, then performing vacuum drying at 110 ℃ for 12 hours, and tabletting to obtain a negative plate with the diameter of 10 mm.
And thirdly, taking metal lithium as a reference counter electrode, taking a microporous polypropylene film as a diaphragm, and taking 1mol/L lithium hexafluorophosphate/ethylene carbonate, diethyl carbonate and methyl ethyl carbonate (in a volume ratio of 1:1:1) as electrolyte. A 2025 button cell battery was assembled in a glove box filled with high purity argon. And (5) standing for 12h, and then carrying out electrochemical performance test.
And the simulated battery adopts a blue battery test system to carry out charge and discharge performance test. And carrying out charge and discharge performance tests on the untreated artificial graphite and the treated graphene/artificial graphite composite material within the voltage range of 0.1-3V by using different discharge current densities (0.2, 0.5, 1, 2, 5A/g).
The charge and discharge performance test result shows that: the comparative example had a first coulombic efficiency of about 72.1% and specific discharge capacities at 0.2A/g and 5A/g of about 375 and 27 mAh/g, respectively. The first coulombic efficiency of the graphene/artificial graphite composite material electrode treated by the embodiment is 81.1%, and the specific discharge capacities at 0.2A/g and 5A/g are about 446 mAh/g and 80 mAh/g respectively.
Example 2
The embodiment comprises the following steps:
adding 1g of artificial graphite into 100mL of deionized water, and stirring for 30 min. And adding 5mg of graphene oxide into 100mL of deionized water, ultrasonically stirring for 30min, mixing with the stirred artificial graphite dispersion liquid, and putting into an electroplating device. And performing electrodeposition treatment for 5 min under the voltage of 1V, stirring at the speed of 40 rpm, performing suction filtration, and drying in a vacuum drying oven at the temperature of 80 ℃ for 12h to obtain the graphene/artificial graphite composite material.
And secondly, mixing the graphene/artificial graphite composite material, conductive carbon black and polyvinylidene fluoride (PVDF) according to a mass ratio of 8:1:1 by taking N-methylpyrrolidone (NMP) as a solvent, uniformly stirring to form slurry, coating the slurry on the surface of copper foil, then performing vacuum drying at 110 ℃ for 12 hours, and tabletting to obtain the negative plate with the diameter of 10 mm.
And thirdly, taking metal lithium as a reference counter electrode, taking a microporous polypropylene film as a diaphragm, and taking 1mol/L lithium hexafluorophosphate/ethylene carbonate, diethyl carbonate and methyl ethyl carbonate (in a volume ratio of 1:1:1) as electrolyte. A 2025 button cell battery was assembled in a glove box filled with high purity argon. And (5) standing for 12h, and then carrying out electrochemical performance test.
And the simulated battery adopts a blue battery test system to carry out charge and discharge performance test. And (3) carrying out charge and discharge performance tests on the treated graphene/artificial graphite composite material within the voltage range of 0.1-3V by using different discharge current densities (0.2, 0.5, 1, 2, 5A/g).
The charge and discharge performance test result shows that: the first coulombic efficiency of the treated graphene/artificial graphite composite material electrode is 82.3%, and the specific discharge capacities at 0.2A/g and 5A/g are 457 and 74 mAh/g respectively.
Example 3
The embodiment comprises the following steps:
adding 2g of artificial graphite into 100mL of deionized water, and stirring for 30 min. And adding 1mg of graphene oxide into 100mL of deionized water, ultrasonically stirring for 30min, mixing with the stirred artificial graphite dispersion liquid, and putting into an electroplating device. And performing electrodeposition treatment for 10min under the voltage of 2V, stirring at the speed of 80 rpm, performing suction filtration, and drying in a vacuum drying oven at the temperature of 80 ℃ for 12h to obtain the graphene/artificial graphite composite material.
And secondly, mixing the graphene/artificial graphite composite material, conductive carbon black and polyvinylidene fluoride (PVDF) according to a mass ratio of 8:1:1 by taking N-methylpyrrolidone (NMP) as a solvent, uniformly stirring to form slurry, coating the slurry on the surface of copper foil, then performing vacuum drying at 110 ℃ for 12 hours, and tabletting to obtain the negative plate with the diameter of 10 mm.
And thirdly, taking metal lithium as a reference counter electrode, taking a microporous polypropylene film as a diaphragm, and taking 1mol/L lithium hexafluorophosphate/ethylene carbonate, diethyl carbonate and methyl ethyl carbonate (in a volume ratio of 1:1:1) as electrolyte. A 2025 button cell battery was assembled in a glove box filled with high purity argon. And (5) standing for 12h, and then carrying out electrochemical performance test.
And the simulated battery adopts a blue battery test system to carry out charge and discharge performance test. And (3) carrying out charge and discharge performance tests on the treated graphene/artificial graphite composite material within the voltage range of 0.1-3V by using different discharge current densities (0.2, 0.5, 1, 2, 5A/g).
The charge and discharge performance test result shows that: the first coulombic efficiency of the treated graphene/artificial graphite composite material electrode is 80.7%, and the specific discharge capacities at 0.2A/g and 5A/g are respectively 464 mAh/g and 78 mAh/g.
Example 4
The embodiment comprises the following steps:
adding 2g of artificial graphite into 100mL of deionized water, and stirring for 30 min. 100mg of graphene oxide is added into 100mL of deionized water, ultrasonic stirring is carried out for 30min, and then the mixture and the stirred artificial graphite dispersion liquid are mixed and put into an electroplating device. And performing electrodeposition treatment for 20min under the voltage of 4V, stirring at the speed of 60 r/min, performing suction filtration, and drying in a vacuum drying oven at the temperature of 80 ℃ for 12h to obtain the graphene/artificial graphite composite material.
And secondly, mixing the graphene/artificial graphite composite material, conductive carbon black and polyvinylidene fluoride (PVDF) according to a mass ratio of 8:1:1 by taking N-methylpyrrolidone (NMP) as a solvent, uniformly stirring to form slurry, coating the slurry on the surface of copper foil, then performing vacuum drying at 110 ℃ for 12 hours, and tabletting to obtain the negative plate with the diameter of 10 mm.
And thirdly, taking metal lithium as a reference counter electrode, taking a microporous polypropylene film as a diaphragm, and taking 1mol/L lithium hexafluorophosphate/ethylene carbonate, diethyl carbonate and methyl ethyl carbonate (in a volume ratio of 1:1:1) as electrolyte. A 2025 button cell battery was assembled in a glove box filled with high purity argon. And (5) standing for 12h, and then carrying out electrochemical performance test.
And the simulated battery adopts a blue battery test system to carry out charge and discharge performance test. And (3) carrying out charge and discharge performance tests on the treated graphene/artificial graphite composite material within the voltage range of 0.1-3V by using different discharge current densities (0.2, 0.5, 1, 2, 5A/g).
The charge and discharge performance test result shows that: the first coulombic efficiency of the graphene/artificial graphite composite material electrode after the treatment is 83.4%, and the specific discharge capacities at 0.2A/g and 5A/g are respectively 477 mAh/g and 84 mAh/g.
Example 5
The embodiment comprises the following steps:
adding 1g of artificial graphite into 100mL of deionized water, and stirring for 30 min. And adding 5mg of graphene oxide into 100mL of deionized water, ultrasonically stirring for 30min, mixing with the stirred artificial graphite dispersion liquid, and putting into an electroplating device. And performing electrodeposition treatment for 30s under the voltage of 3V, stirring at the speed of 50 r/min, performing suction filtration, and drying in a vacuum drying oven at the temperature of 80 ℃ for 12h to obtain the graphene/artificial graphite composite material.
And secondly, mixing the graphene/artificial graphite composite material, conductive carbon black and polyvinylidene fluoride (PVDF) according to a mass ratio of 8:1:1 by taking N-methylpyrrolidone (NMP) as a solvent, uniformly stirring to form slurry, coating the slurry on the surface of copper foil, then performing vacuum drying at 110 ℃ for 12 hours, and tabletting to obtain the negative plate with the diameter of 10 mm.
② taking metal lithium as a reference counter electrode, a microporous polypropylene film as a diaphragm and 1mol/L lithium hexafluorophosphate/ethylene carbonate, diethyl carbonate and methyl ethyl carbonate (volume ratio is 1:1:1) as electrolyte. A 2025 button cell battery was assembled in a glove box filled with high purity argon. And (5) standing for 12h, and then carrying out electrochemical performance test.
And the simulated battery adopts a blue battery test system to carry out charge and discharge performance test. And (3) carrying out charge and discharge performance tests on the treated graphene/artificial graphite composite material within the voltage range of 0.1-3V by using different discharge current densities (0.2, 0.5, 1, 2, 5A/g).
The charge and discharge performance test result shows that: the first coulombic efficiency of the treated graphene/artificial graphite composite material electrode is 82.8%, and the specific discharge capacities at 0.2A/g and 5A/g are respectively 482 mAh/g and 91 mAh/g.
Example 6
The embodiment comprises the following steps:
adding 0.5g of artificial graphite into 100mL of deionized water, and stirring for 30 min. And adding 1mg of graphene oxide into 100mL of deionized water, ultrasonically stirring for 30min, mixing with the stirred artificial graphite dispersion liquid, and putting into an electroplating device. And carrying out electrodeposition treatment for 60min under the voltage of 5V, stirring at the speed of 40 rpm, then carrying out suction filtration, and drying in a vacuum drying oven at the temperature of 80 ℃ for 12h to obtain the graphene/artificial graphite composite material.
And secondly, mixing the graphene/artificial graphite composite material, conductive carbon black and polyvinylidene fluoride (PVDF) according to a mass ratio of 8:1:1 by taking N-methylpyrrolidone (NMP) as a solvent, uniformly stirring to form slurry, coating the slurry on the surface of copper foil, then performing vacuum drying at 110 ℃ for 12 hours, and tabletting to obtain the negative plate with the diameter of 10 mm.
And thirdly, taking metal lithium as a reference counter electrode, taking a microporous polypropylene film as a diaphragm, and taking 1mol/L lithium hexafluorophosphate/ethylene carbonate, diethyl carbonate and methyl ethyl carbonate (in a volume ratio of 1:1:1) as electrolyte. A 2025 button cell battery was assembled in a glove box filled with high purity argon. And (5) standing for 12h, and then carrying out electrochemical performance test.
And the simulated battery adopts a blue battery test system to carry out charge and discharge performance test. And (3) carrying out charge and discharge performance tests on the treated graphene/artificial graphite composite material within the voltage range of 0.1-3V by using different discharge current densities (0.2, 0.5, 1, 2, 5A/g).
The charge and discharge performance test result shows that: the first coulombic efficiency of the treated graphene/artificial graphite composite material electrode is 83.7%, and the specific discharge capacities at 0.2A/g and 5A/g are respectively 495 mAh/g and 96 mAh/g.
Through the experiment, the first coulombic efficiency of the lithium ion battery consisting of the graphene/artificial graphite composite material electrode treated by the method is improved by 8.6-11.6%, the specific capacity of the lithium ion battery under the current density of 0.2A/g is improved by 71 mAh/g-120mAh/g, and the specific capacity of the lithium ion battery under the current density of 5A/g is improved by 47 mAh/g-69 mAh/g.
The foregoing embodiments may be modified in many different ways by those skilled in the art without departing from the spirit and scope of the invention, which is defined by the appended claims and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. A lithium ion battery optimization method based on a graphene/artificial graphite composite material is characterized in that a negative electrode of a lithium ion battery is manufactured by electrodepositing graphene on the surface of artificial graphite particles;
carrying out electrodeposition reduction on the graphene based on the surface of the artificial graphite particles after mixing a graphene oxide dispersion liquid and an artificial stone ink powder dispersion liquid, and extracting a graphene/artificial graphite composite material from a mixed solution obtained by reaction;
the electrodeposition reduction adopts stainless steel as an anode and a stainless steel cylinder filled with mixed graphene oxide dispersion liquid and artificial stone ink powder dispersion liquid as a cathode in an electroplating device, and applies voltage between the anode and the cathode in a stirring environment;
the voltage is as follows: 1V to 5V; the electrodeposition treatment time is as follows: 30 s-60 min.
2. The method for optimizing the lithium ion battery based on the graphene/artificial graphite composite material as claimed in claim 1, wherein the negative electrode of the lithium ion battery is prepared by taking N-methyl pyrrolidone (NMP) as a solvent, mixing the graphene/artificial graphite composite material, conductive carbon black and polyvinylidene fluoride (PVDF), adding N-methyl pyrrolidone (NMP) as a solvent, uniformly stirring to form slurry, coating the slurry on the surface of copper foil, and drying.
3. The method for optimizing the lithium ion battery based on the graphene/artificial graphite composite material as claimed in claim 2, wherein the mass ratio of the graphene/artificial graphite composite material to the conductive carbon black to the polyvinylidene fluoride (PVDF) is 8:1:1.
4. The method for optimizing a lithium ion battery based on graphene/artificial graphite composite material according to claim 1, wherein the particle size of the artificial graphite particles comprises: d10：6～8 μm、D5015 to 18 μm and D90:50～60 μm。
5. The optimization method of the lithium ion battery based on the graphene/artificial graphite composite material, according to claim 1, is characterized in that the mass ratio of the graphene oxide in the graphene oxide dispersion liquid to the artificial graphite powder in the artificial stone toner dispersion liquid is 1: 20-1: 2000.
6. The method for optimizing the lithium ion battery based on the graphene/artificial graphite composite material as claimed in claim 1, wherein the extraction is performed by suction filtration and drying.
7. The method for optimizing the lithium ion battery based on the graphene/artificial graphite composite material according to claim 1, wherein a counter electrode of the lithium ion battery is made of metal lithium; the diaphragm adopts a microporous polypropylene film; the electrolyte was prepared by mixing lithium hexafluorophosphate/ethylene carbonate, diethyl carbonate, and methylethyl carbonate at the same concentration in a volume ratio of 1:1: 1.
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| CN102583354B (en) * | 2012-03-09 | 2015-05-20 | 合肥工业大学 | Method for preparing graphene film through electroplating deposition method |
| US10879534B2 (en) * | 2013-12-12 | 2020-12-29 | Rensselaer Polytechnic Institute | Porous graphene network electrodes and an all-carbon lithium ion battery containing the same |
| CN106283150A (en) * | 2015-05-11 | 2017-01-04 | 深圳中宇昭日科技有限公司 | A kind of electro-deposition graphene conductive corrosion-resistant material preparation method for material |
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| CN105350054A (en) * | 2015-11-25 | 2016-02-24 | 哈尔滨工业大学 | Method for modifying nano-carbon material on surface of secondary battery diaphragm through electrophoretic deposition |
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