CN111725481A - Preparation method of organic material/graphite composite negative electrode, composite negative electrode and application of composite negative electrode - Google Patents
Preparation method of organic material/graphite composite negative electrode, composite negative electrode and application of composite negative electrode Download PDFInfo
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Abstract
The invention relates to a preparation method of an organic material/graphite composite negative electrode, wherein the organic material is a mixture of one or more of organic acid/acid anhydride with a conjugated carbonyl structure, and the preparation method comprises the following steps: s1, dissolving an organic material in a solvent to obtain a first mixed solution, dispersing graphite in the solvent to obtain a second mixed solution, adding the first mixed solution into the second mixed solution, and heating and stirring until the solvent volatilizes to obtain mixed powder; and S2, placing the mixed powder in a drying oven to be dried continuously, removing residual solvent to obtain organic material/graphite composite powder, and using the organic material/graphite composite powder as an electroactive material to prepare an organic material/graphite composite negative electrode. The electrochemical performance of the composite cathode can be effectively improved by adopting different solvents or compounding the solvents.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a preparation method of an organic material/graphite composite negative electrode, the composite negative electrode and application of the composite negative electrode.
Background
The development of high-performance negative electrodes is an important way for improving the electrochemical performance of lithium ion batteries. Graphite occupies a leading position in the lithium ion battery cathode market due to the advantages of good conductivity, abundant sources, low cost, relatively small harm to the environment and the like. However, the theoretical specific capacity of the graphite is lower and is only 372mAh/g, so that the energy density and the power density of the graphite cathode are lower.
The development of an organic matter/graphite composite electrode is an effective method for improving the electrochemical performance of the negative electrode. The organic material can reversibly store lithium ions by utilizing carbonyl and conjugate effects, the capacity of storing lithium can reach 2000mAh/g, the organic material has good elasticity and flexibility, and the volume effect in the lithium intercalation and deintercalation process is small. In conclusion, the organic material has strong structural design, the energy density and the power density of the electrode can be optimized by regulating and controlling the molecular structure, and the organic material has rich sources, is clean and environment-friendly and has relatively low price. By compounding the organic material with the graphite, the organic matter can make up for the defects of low energy density and power density of the graphite, and the graphite can solve the problem of poor electronic conductivity of the organic matter. However, in the prior art, the preparation process of the organic matter/graphite composite negative electrode is single, and the organic matter, the graphite, the conductive agent and the binder are generally directly mixed for slurry stirring. The method does not solve the problems that the first irreversible lithium consumption of the organic negative electrode material is high and organic small molecules are easy to dissolve in the electrolyte.
In view of this, research on a preparation process of the organic matter/graphite composite electrode is needed to further improve the electrochemical performance of the organic matter/graphite composite negative electrode.
Disclosure of Invention
In view of the above, the present invention provides a preparation method of an organic material/graphite composite negative electrode with good electrochemical properties, a composite negative electrode and applications thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the first purpose of the invention is to provide a preparation method of an organic material/graphite composite negative electrode, wherein the organic material is a mixture of one or more of organic acid/acid anhydride with a conjugated carbonyl structure, and the preparation method comprises the following steps:
s1, dissolving an organic material in a solvent to obtain a first mixed solution, dispersing graphite in the solvent to obtain a second mixed solution, adding the first mixed solution into the second mixed solution, and heating and stirring until the solvent volatilizes to obtain mixed powder;
and S2, placing the mixed powder in a drying oven to be dried continuously, removing residual solvent to obtain organic matter material/graphite composite powder, and using the organic matter material/graphite composite powder as an electroactive material to prepare an organic matter material/graphite composite negative electrode.
Specifically, the feeding mass ratio of the organic material to the graphite is 1-30: 100.
Specifically, the solvent is one or more of ethanol, methanol, isopropanol and n-butanol.
Specifically, in S1, the heating temperature for raising the temperature is 30-100 ℃.
Specifically, in S2, the drying oven is vacuum drying or forced air drying, the drying temperature is 60-120 ℃, and the drying time is 6-24 h.
Specifically, the organic material is a mixture of one or more selected from aldehydes, ketones, carboxylic acids and carboxylic acid derivatives.
Preferably, the carboxylic acid derivative is one selected from the group consisting of an acid anhydride, an acid halide, an amide and an ester.
Specifically, the organic material/graphite composite negative electrode is prepared by uniformly mixing the organic material/graphite composite powder, a conductive agent and a binder, coating the mixture on a copper current collector, and rolling, slicing and drying the mixture after drying to obtain the organic material/graphite composite negative electrode; the feeding mass ratio of the organic material/graphite composite powder, the conductive agent and the binder is 5-9:1-4: 1-3.
The second purpose of the invention is to provide an organic material/graphite composite negative electrode, which is prepared by adopting the preparation method of the organic material/graphite composite negative electrode.
The third purpose of the invention is to provide an application of the organic material/graphite composite negative electrode, wherein the organic material/graphite composite negative electrode is used as a negative electrode in a lithium ion battery.
Compared with the prior art, the preparation method of the organic material/graphite composite negative electrode comprises the steps of mixing the organic material and graphite, adding the mixture into a solvent, evaporating the solvent to obtain composite powder, and using the composite powder as an active material to prepare the organic material/graphite composite negative electrode which is used as a negative electrode of a lithium ion battery. The significance of using different solvents is: by utilizing the special functional group in the solvent to react with the oxygen-containing functional group in the organic material, on one hand, the irreversible lithium consumption of the organic material in the charging and discharging process can be reduced, and the first coulombic efficiency of the electrode is improved; on the other hand, the dissolution of organic small molecules in the electrolyte can be inhibited, and the capacity retention rate of the electrode can be improved. In addition, the dispersibility, the combination degree, the morphology and the like of the organic material and the graphite can be improved by regulating and controlling the solvent, so that the electrochemical performance of the electrode is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a first charge-discharge curve of a maleic acid/graphite composite electrode corresponding to examples 1-4;
FIG. 2 is the specific discharge capacity of the first five cycles of the maleic acid/graphite composite electrode corresponding to examples 1-4;
FIG. 3 is the coulombic efficiencies of the first five cycles of the maleic acid/graphite composite electrode corresponding to examples 1-4;
FIG. 4 is a graph showing rate capability of maleic acid/graphite composite electrodes corresponding to examples 1-4.
Detailed Description
By compounding the organic material with the graphite, the organic matter can make up for the defects of low energy density and power density of the graphite, and the graphite can solve the problem of poor electronic conductivity of the organic matter. However, in the prior art, the preparation process of the organic matter/graphite composite negative electrode is single, and the organic matter, the graphite, the conductive agent and the binder are generally directly mixed for slurry stirring.
In view of this, research on a preparation process of the organic matter/graphite composite electrode is needed to further improve the electrochemical performance of the organic matter/graphite composite negative electrode.
The technical solution of the present invention will be clearly and completely described by the following detailed description. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of an organic material/graphite composite negative electrode is disclosed, wherein the organic material is a mixture of one or more of organic acid/acid anhydride with a conjugated carbonyl structure, and the preparation method comprises the following steps:
s1, dissolving an organic material (a mixture of one or more selected from aldehyde, ketone, carboxylic acid and carboxylic acid derivative (one selected from anhydride, acyl halide, amide and ester)) in a solvent (a mixed solvent of one or more selected from ethanol, methanol, isopropanol and n-butanol) to obtain a first mixed solution, dispersing graphite in the solvent (the same as the above solvent) to obtain a second mixed solution, adding the first mixed solution into the second mixed solution, raising the temperature (the heating temperature is 30-100 ℃) and stirring until the solvent volatilizes to obtain mixed powder; the feeding mass ratio of the organic material to the graphite is 1-30: 100.
And S2, placing the mixed powder in a drying oven (vacuum drying or forced air drying, drying temperature is 60-120 ℃, drying time is 6-24h), continuously drying, removing residual solvent to obtain organic material/graphite composite powder, and using the organic material/graphite composite powder as an electroactive material to prepare the organic material/graphite composite negative electrode.
An application of an organic material/graphite composite negative electrode is to apply the organic material/graphite composite negative electrode to a lithium ion battery. The organic material/graphite composite negative electrode is prepared by uniformly mixing organic material/graphite composite powder, a conductive agent and a binder, coating the mixture on a copper current collector, and rolling, slicing and drying the mixture after drying to obtain the organic material/graphite composite negative electrode; the feeding mass ratio of the organic material/graphite composite powder, the conductive agent and the binder is 5-9:1-4: 1-3.
In the invention, the conductive agent is acetylene black, and the binder is carboxymethyl cellulose and styrene butadiene rubber in a mass ratio of 1: 1.
The invention is further illustrated and discussed below in the following specific examples and comparative examples.
s1, dissolving 0.25g of maleic acid in 10g of ethanol to obtain a first mixed solution, dispersing 1g of graphite in 10g of ethanol to obtain a second mixed solution, adding the first mixed solution into the second mixed solution, stirring at room temperature for 30min, heating and stirring to 80 ℃ until the solvent volatilizes to obtain mixed powder;
and S2, placing the mixed powder in an air-blast drying oven (the drying temperature is 60 ℃ and the drying time is 12 hours) to continue drying, removing residual solvent to obtain organic material/graphite composite powder, and using the organic material/graphite composite powder as an electroactive material to prepare an organic material/graphite composite negative electrode.
And the organic matter material/graphite composite negative electrode is used for preparing a lithium ion battery.
Example 2 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as that in example 1 except that: the solvent is methanol.
Example 3 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: the solvent is isopropanol.
Example 4 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: the solvent is n-butanol.
Example 5 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: the solvent is compounded by water and ethanol, wherein the volume ratio is 3: 7.
Example 6 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: the solvent is compounded by water and ethanol, wherein the volume ratio is 1: 1.
Example 7 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: the solvent is compounded by water and ethanol, wherein the volume ratio is 7: 3.
Example 8 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: maleic acid was 0.05 g.
Example 9 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: maleic acid was 0.1 g.
Example 10 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: maleic acid was 0.15 g.
Example 11 this example provides a method for preparing an organic material/graphite composite anode, which is substantially the same as in example 1, except that: maleic acid was 0.2 g.
Comparative example 1 this comparative example provides a method of preparing an organic material/graphite composite anode, which is substantially the same as example 1, except that: the solvent is acetone.
Comparative example 2 this comparative example provides a method of preparing an organic material/graphite composite anode, which is substantially the same as example 1, except that: maleic acid was 0.5 g.
Comparative example 3 this comparative example provides a prior artThe preparation method of the organic material/graphite composite negative electrode in the technology comprises the following steps of uniformly mixing an organic lithium storage material, graphite, a conductive agent, a binder and a dispersing agent in deionized water to prepare electrode slurry, coating the electrode slurry on a copper foil current collector, drying and then using 2MPa/cm2The obtained product is pressed, cut and dried for 16 hours at 120 ℃ under the vacuum condition, and the composite electrode is obtained and used for preparing a lithium ion battery by using a negative electrode.
The electrochemical properties of the negative electrodes of lithium ion batteries assembled with the composite electrodes obtained in examples 1 to 11 and comparative examples 1 to 3 were measured as follows (electrode ratio: organic material/graphite composite powder: conductive agent: binder: 7:2:1 wt%, with metallic lithium as the counter electrode)
The electrochemical performance of the electrode can be effectively improved by compounding the solvent. Comparing different solvents: when ethanol is used as a solvent, the first coulombic efficiency of the electrode is highest; when n-butanol is used as a solvent, the capacity retention ratio of the electrode is the best. This is because maleic acid contains a carboxylic acid functional group, and under heating conditions, a part of the alcohol solvent reacts with maleic acid to form an ester by dehydration, which not only reduces irreversible lithium consumption of the carboxylic acid functional group during charging and discharging, but also suppresses dissolution of maleic acid in the electrolyte.
The electrochemical performance of the assembled lithium ion battery negative electrode formed by mixing the organic matter/graphite composite powder prepared in examples 1 to 4 is shown in fig. 1 to 4.
As can be seen from the data in fig. 1, with different solvents, the polarization order of the electrodes is ethanol < isopropanol < methanol < n-butanol. As can be seen from the data in fig. 2, the discharge specific capacity of the electrodes with different solvents is ordered ethanol > isopropanol > methanol > n-butanol. As can be seen from the data in fig. 3, with different solvents, the coulombic efficiency order of the electrode is ethanol > methanol > isopropanol > n-butanol. As can be seen from the data in fig. 4, the electrode has the highest specific discharge capacity when ethanol is used as the solvent, but has the highest capacity retention rate when n-butanol is used as the solvent, at different current densities.
Compared with the preparation method of the prior art of the comparative example 3, the preparation method has the advantages that maleic acid and graphite are mixed in different solvents, and the interaction between the solvents and the maleic acid is utilized, so that on one hand, the irreversible lithium consumption of the maleic acid in the charging and discharging processes can be effectively reduced, and the first coulombic efficiency of the electrode is improved; on the other hand, the dissolution of maleic acid in the electrolyte can be suppressed to some extent, and the capacity retention rate of the electrode can be improved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of an organic material/graphite composite negative electrode is characterized in that the organic material is one or a mixture of more of organic acid/acid anhydride with a conjugated carbonyl structure, and the preparation method comprises the following steps:
s1, dissolving an organic material in a solvent to obtain a first mixed solution, dispersing graphite in the solvent to obtain a second mixed solution, adding the first mixed solution into the second mixed solution, and heating and stirring until the solvent volatilizes to obtain mixed powder;
and S2, placing the mixed powder in a drying oven to be dried continuously, removing residual solvent to obtain organic matter material/graphite composite powder, and using the organic matter material/graphite composite powder as an electroactive material to prepare an organic matter material/graphite composite negative electrode.
2. The method for preparing the organic material/graphite composite negative electrode according to claim 1, wherein: the feeding mass ratio of the organic material to the graphite is 1-30: 100.
3. The method for preparing the organic material/graphite composite negative electrode according to claim 1, wherein: the solvent is one or more of ethanol, methanol, isopropanol and n-butanol.
4. The method for preparing the organic material/graphite composite negative electrode according to claim 1, wherein: in S1, the heating temperature for raising the temperature is 30-100 ℃.
5. The method for preparing the organic material/graphite composite negative electrode according to claim 1, wherein: and S2, drying in a vacuum drying oven or in a forced air drying oven at 60-120 ℃ for 6-24 h.
6. The method for preparing the organic material/graphite composite negative electrode according to claim 1, wherein: the organic material is a mixture consisting of one or more of aldehyde, ketone, carboxylic acid and carboxylic acid derivative.
7. The method for preparing the organic material/graphite composite negative electrode according to claim 6, wherein: the carboxylic acid derivative is one selected from acid anhydride, acid halide, amide and ester.
8. The method for preparing the organic material/graphite composite negative electrode according to claim 1, wherein: the organic material/graphite composite negative electrode is prepared by the specific steps of uniformly mixing the organic material/graphite composite powder, a conductive agent and a binder, coating the mixture on a copper current collector, and rolling, slicing and drying the mixture after drying to obtain the organic material/graphite composite negative electrode; the feeding mass ratio of the organic material/graphite composite powder, the conductive agent and the binder is 5-9:1-4: 1-3.
9. An organic matter material/graphite composite negative electrode is characterized in that: the organic material/graphite composite negative electrode as claimed in any one of claims 1 to 8.
10. The application of the organic material/graphite composite negative electrode is characterized in that: the organic material/graphite composite negative electrode according to claim 9 is used as a negative electrode in a lithium ion battery.
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Citations (3)
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| CN105514394A (en) * | 2016-01-26 | 2016-04-20 | 苏州大学 | Modification method for lithium-ion battery graphite cathode material |
| CN108711623A (en) * | 2018-05-30 | 2018-10-26 | 欣旺达电子股份有限公司 | Lithium ion battery, negative plate, composite graphite negative electrode material and preparation method thereof |
| CN110323435A (en) * | 2019-07-11 | 2019-10-11 | 苏州大学 | Organic material/graphite composite negative pole, preparation method and lithium ion battery |
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| CN105514394A (en) * | 2016-01-26 | 2016-04-20 | 苏州大学 | Modification method for lithium-ion battery graphite cathode material |
| CN108711623A (en) * | 2018-05-30 | 2018-10-26 | 欣旺达电子股份有限公司 | Lithium ion battery, negative plate, composite graphite negative electrode material and preparation method thereof |
| CN110323435A (en) * | 2019-07-11 | 2019-10-11 | 苏州大学 | Organic material/graphite composite negative pole, preparation method and lithium ion battery |
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| RUITIAN GUO等: "A novel itaconic acid-graphite composite anode for enhanced lithium storage in lithium ion batteries", 《CARBON》 * |
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