CN113178548A - Pre-sodium graphene negative pole piece, preparation method thereof and sodium ion battery - Google Patents
Pre-sodium graphene negative pole piece, preparation method thereof and sodium ion battery Download PDFInfo
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- CN113178548A CN113178548A CN202110462318.1A CN202110462318A CN113178548A CN 113178548 A CN113178548 A CN 113178548A CN 202110462318 A CN202110462318 A CN 202110462318A CN 113178548 A CN113178548 A CN 113178548A
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Abstract
The application provides a preparation method of a pre-sodium graphene negative electrode piece, the pre-sodium graphene negative electrode piece and a sodium ion battery, wherein the preparation method comprises the following steps: dissolving polycyclic aromatic hydrocarbon and a film forming additive in an aprotic polar solvent, and adding excessive metal sodium to enable the polycyclic aromatic hydrocarbon to react completely to generate polycyclic aromatic hydrocarbon sodium to prepare a solution; and soaking the graphene negative pole piece in the solution for 5s-3 min. This application is through polycyclic aromatic hydrocarbon sodium and film forming additive's combined action, preformed one deck electronic insulation, ionic conduction and insoluble surface SEI membrane on graphite alkene negative pole piece, and the SEI membrane that produces with the battery circulation can the collaborative work, protects sodium ion battery's negative pole better to promote sodium ion battery's each item performance. The method is simple and safe, easy to implement and not easy to generate byproducts.
Description
Technical Field
The application relates to the technical field of batteries, in particular to a preparation method of a pre-sodium graphene negative electrode plate, the pre-sodium graphene negative electrode plate prepared by the preparation method and a sodium ion battery applying the negative electrode plate.
Background
Due to the abundance of sodium resources, sodium ion batteries have become a promising alternative to lithium ion batteries, especially in future large-scale energy storage systems.
Carbon has high conductivity, controllable microstructure and surface chemical properties, and is an excellent cathode for preparing sodium ion batteries. Low specific surface area disordered carbons tend to exhibit poor rate capability and low reversible capacity due to low ion diffusion rates and limited sodium storage sites. And the high-specific-surface-area carbon deposits such as reduced graphene oxide and the like have abundant sodium storage active sites and a two-dimensional structure for enhancing ion diffusion, so that the two-dimensional structure is widely researched. However, reduced graphene oxide generally exhibits a low initial coulombic efficiency due to unavoidable electrolyte decomposition and other side reactions.
The effect of improving the first coulombic efficiency can be achieved by adjusting the components of an SEI (Solid Electrolyte Interface) by optimizing the Electrolyte or adjusting the defect structure by adjusting the carbonization temperature, but the effect is limited. Therefore, researchers have proposed a variety of pre-sodium methods to improve the first coulombic efficiency, including the addition of metallic sodium, the addition of sacrificial salts such as sodium salts, and electrochemical methods. However, the direct addition of highly flammable and explosive sodium metal causes serious safety hazards; adding Na3N (sodium nitride), Na3P (sodium phosphide) and other sacrificial salts are easy to generate unwanted byproducts; the electrochemical method requires disassembly of the battery, and is complicated in process and not easy to implement.
Disclosure of Invention
In view of this, a preparation method of a pre-sodium graphene negative electrode plate is needed to be provided to solve the problems that the pre-sodium method in the prior art has potential safety hazards, is easy to generate byproducts, and is complex in operation and not easy to implement.
In addition, a pre-sodiumized graphene negative electrode plate and a sodium ion battery are also needed to be provided.
An embodiment of the application provides a preparation method of a pre-sodium graphene negative electrode piece, which comprises the following steps:
preparing a graphene negative pole piece;
dissolving polycyclic aromatic hydrocarbon and a film forming additive in an aprotic polar solvent, and adding excessive metal sodium to enable the polycyclic aromatic hydrocarbon to react completely to generate polycyclic aromatic hydrocarbon sodium to prepare a solution;
soaking the graphene negative pole piece in the solution for 5s-3 min;
and washing the graphene negative electrode piece soaked in the solution for multiple times by using the aprotic polar solvent to obtain the pre-sodium graphene negative electrode piece.
In one embodiment, the polycyclic aromatic hydrocarbon includes one or more of biphenyl, biphenylene, polyphenylaliphatic hydrocarbon, and polycyclic aromatic hydrocarbon.
In one embodiment, the film forming additive includes a cyclic carbonate having a fluoro group and a chain carbonate having a fluoro group.
In one embodiment, the film-forming additive comprises one or more of fluoroethylene carbonate, difluoroethylene carbonate, and fluoromethyl carbonate.
In one embodiment, the aprotic polar solvent comprises one or more of dimethylformamide, dimethylsulfoxide, acetone, tetrahydrofuran, and dimethylether.
In one embodiment, the concentration of the polycyclic aromatic hydrocarbon sodium is 0.05 to 3mol/L and the concentration of the film forming additive is 0.05 to 1 mol/L.
In one embodiment, the preparation of the graphene negative electrode plate comprises the following steps:
mixing reduced graphene oxide, ketjen black and polyvinylidene fluoride according to parts by weight of 80, 10 and 10, and dissolving the mixture in methyl pyrrolidone to obtain negative active material slurry;
and coating the negative active material slurry on a copper foil, vacuum drying, and blanking to obtain the graphene negative pole piece.
The application also provides a pre-sodium graphene negative electrode plate which is prepared by the preparation method of any one of the above.
In one embodiment, the pre-sodiated graphene negative electrode sheet comprises a solid electrolyte interface film.
The application also provides a sodium ion battery, which comprises a positive plate, a negative plate, electrolyte and a diaphragm, wherein the negative plate is the pre-sodium graphene negative plate.
This application is through polycyclic aromatic hydrocarbon sodium and film forming additive's combined action, preformed one deck electronic insulation, ionic conduction and insoluble surface SEI membrane on graphite alkene negative pole piece, and the SEI membrane that produces with the battery circulation can the collaborative work, protects sodium ion battery's negative pole better to promote sodium ion battery's each item performance. The method is simple and safe, easy to implement and not easy to generate byproducts.
Drawings
The present application will be described in further detail with reference to the following drawings and detailed description.
Fig. 1A is a scanning electron microscope image of the common graphene negative electrode sheet prepared in comparative example 1.
Fig. 1B is a scanning electron microscope image of the pre-sodiumized graphene negative electrode sheet prepared in example 1 of the present application.
Fig. 2 is an ac impedance profile of a pre-sodium battery prepared in example 1 of the present application and a general battery prepared in comparative example 1.
Fig. 3 is a graph comparing the first charge and discharge curves of the pre-sodium treated battery prepared in example 1 of the present application and the general battery prepared in comparative example 1.
Fig. 4 is a graph comparing rate performance of a pre-sodium battery prepared in example 1 of the present application and a general battery prepared in comparative example 1.
Fig. 5 is a graph comparing the first charge and discharge curves of the pre-sodium treated battery prepared in example 2 of the present application and the general battery prepared in comparative example 1.
Fig. 6 is a graph comparing the first charge and discharge curves of the pre-sodium treated battery prepared in example 3 of the present application and the general battery prepared in comparative example 1.
Fig. 7 is a graph comparing the first charge and discharge curves of the pre-sodium treated battery prepared in example 4 of the present application and the general battery prepared in comparative example 1.
The following detailed description will further describe embodiments of the present application in conjunction with the above-described figures.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely with reference to the drawings in the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. 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 application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the embodiments of this application belong. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the present application.
An embodiment of the application provides a preparation method of a pre-sodium graphene negative electrode piece, which comprises the following steps:
preparing a graphene negative pole piece;
dissolving polycyclic aromatic hydrocarbon and a film forming additive in an aprotic polar solvent, and adding excessive metal sodium to enable the polycyclic aromatic hydrocarbon to react completely to generate polycyclic aromatic hydrocarbon sodium to prepare a solution;
soaking the graphene negative pole piece in the solution for 5s-3 min;
and washing the graphene negative electrode piece soaked in the solution for multiple times by using the aprotic polar solvent to obtain the pre-sodium graphene negative electrode piece.
Further, the graphene negative electrode piece is prepared by the following steps: mixing 80 parts, 10 parts and 10 parts of reduced graphene oxide (negative active material), Ketjen black (conductive agent) and polyvinylidene fluoride (PVDF, binder) by weight, and dissolving the mixture in methyl pyrrolidone to obtain negative active material slurry; and coating the negative active material slurry on a copper foil, performing vacuum drying at 110 ℃, and blanking into a circle with the diameter of 12mm to obtain the graphene negative pole piece. It can be understood that the preparation method of the graphene negative electrode plate can also be other conventional preparation methods in the art, for example, the conductive agent and/or the adhesive can also be selected from other substances, the methylpyrrolidone can also be replaced by other applicable solvents, the ratio of the substances can also be adjusted, and the like.
A high voltage difference exists between the reduced graphene oxide and the polycyclic aromatic hydrocarbon sodium, the reduced graphene oxide receives electrons of the polycyclic aromatic hydrocarbon, sodium ions are combined with oxygen-containing functional groups on the surface of the reduced graphene oxide, and the sodium ions are effectively induced to form a surface SEI film under the action of the film forming additive. The preformed SEI film and the SEI film generated by battery circulation can work cooperatively to better protect the negative electrode of the sodium-ion battery.
Further, the reduced graphene oxide is prepared by a Hummers method. Specifically, the steps of the Hummers method are generally as follows: a 250mL reaction bottle is assembled in an ice-water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 2g of graphite powder and 1g of sodium nitrate is added under stirring, 6g of potassium permanganate is added in times, the reaction temperature is controlled not to exceed 20 ℃, and the mixture is stirred and reacted for a period of time; then heating to about 35 ℃, and continuing stirring for 30 min; slowly adding a certain amount of deionized water, continuously stirring for 20min, adding a proper amount of hydrogen peroxide to reduce residual oxidant to make the solution become bright yellow, filtering while the solution is hot, and washing with 5% HCl solution and deionized water until no sulfate radical is detected in the filtrate; and finally, putting the filter cake into a vacuum drying oven at 60 ℃ for full drying, and storing for later use. The surface of the prepared reduced graphene oxide contains a plurality of oxygen-containing functional groups.
In some embodiments, the polycyclic aromatic hydrocarbon includes one or more of biphenyl, biphenylene, polyphenylaliphatic hydrocarbon, and polycyclic aromatic hydrocarbon.
In some embodiments, the film forming additive comprises a cyclic carbonate having a fluoro group and a chain carbonate having a fluoro group.
Further, the film forming additive comprises one or more of fluoroethylene carbonate, difluoroethylene carbonate and fluoromethyl carbonate. The film-forming additive is effective to induce sodium ions to preform a layer of electronically insulating, ionically conducting, and insoluble surface SEI film.
In some embodiments, the aprotic polar solvent comprises one or more of dimethylformamide, dimethylsulfoxide, acetone, tetrahydrofuran, and dimethyl ether.
In some embodiments, the concentration of the polycyclic aromatic hydrocarbon sodium is 0.05 to 3mol/L and the concentration of the film forming additive is 0.05 to 1 mol/L.
The present application will be described in further detail with reference to specific embodiments.
Example 1
Reduced graphene oxide (negative electrode active material), ketjen black (conductive agent), and polyvinylidene fluoride (PVDF, binder) were mixed in parts by weight of 80, 10, and dissolved in a solvent NMP (methyl pyrrolidone), to obtain negative electrode active material slurry. And coating the negative active material slurry on a copper foil serving as a working electrode current collector, drying in a vacuum drier at 110 ℃, and blanking into a circle with the diameter of 12mm to obtain the graphene negative pole piece.
Dissolving 0.005mol of naphthalene (polycyclic aromatic hydrocarbon in polycyclic aromatic hydrocarbon) and 0.0005mol of fluoroethylene carbonate (film forming additive) in 10mL of dimethyl ether (aprotic polar solvent), and adding excessive metal sodium to obtain a solution; then soaking the reduced graphene oxide cathode in the solution for 10 s; and finally, washing the graphene negative pole piece soaked in the solution for several times by using dimethyl ether.
Assembling the graphene negative pole piece into a button type power supply in a glove box filled with argon according to the following sequencePool: the graphene anode plate comprises a positive electrode shell, a gasket, an electrolyte, a diaphragm, an electrolyte, a sodium sheet, a gasket, an elastic sheet and a negative electrode shell, wherein the electrolyte on two sides of the diaphragm is 30 mu L, the electrolyte solvent is dimethyl ether (DME), and the sodium salt is sodium hexafluorophosphate (NaPF) with the concentration of 1M6) The cell was compacted for testing using a button cell sealer with the positive casing down and the negative casing up.
Example 2
The difference from example 1 is: the naphthalene is replaced by biphenyl, the dimethyl ether is replaced by tetrahydrofuran, and the soaking time is changed to 3 min. The rest is the same as the embodiment 1, and the description is omitted.
Example 3
The difference from example 1 is: the amount of naphthalene added was changed to 0.03mol and fluoroethylene carbonate was changed to fluoromethyl carbonate. The rest is the same as the embodiment 1, and the description is omitted.
Example 4
The difference from example 1 is: naphthalene is replaced by 1-4 triphenyl and dimethyl ether is replaced by acetone. The rest is the same as the embodiment 1, and the description is omitted.
Comparative example 1
The difference from example 1 is that: after the graphene negative pole piece is prepared, the button cell is directly assembled without pre-sodium treatment (namely, without solution soaking, washing and other treatment). The rest is the same as the embodiment 1, and the description is omitted.
The negative electrode plates prepared in example 1 and comparative example 1 were subjected to a scanning electron microscope test, the pre-sodium batteries and the common batteries prepared in example 1 and comparative example 1 were subjected to an ac impedance spectrum scanning test, and the pre-sodium batteries prepared in examples 1 to 4 and the common batteries prepared in comparative example 1 were subjected to a blue light tester.
A Scanning Electron Microscope (SEM) image of the common graphene negative electrode sheet prepared in comparative example 1 is shown in fig. 1A, and a scanning electron microscope image of the pre-sodium graphene negative electrode sheet prepared in example 1 is shown in fig. 1B. As can be seen from fig. 1A and 1B, compared to a common graphene negative electrode plate, a layer of SEI appears on the pre-sodium graphene negative electrode plate. The reason is that high voltage difference exists between the reduced graphene oxide and the polycyclic aromatic hydrocarbon sodium, the reduced graphene oxide receives electrons of the polycyclic aromatic hydrocarbon, sodium ions are combined with oxygen-containing functional groups on the surface of the reduced graphene oxide, and the sodium ions are effectively induced to form a surface SEI film under the action of the film-forming additive.
The ac impedance profile scan results of the pre-sodium treated cell prepared in example 1 and the conventional cell prepared in comparative example 1 are shown in fig. 2. The alternating current impedance map is roughly divided into an arc section and a straight line section, wherein the arc section represents charge transfer impedance, and the smaller the curvature radius of the arc section is, the smaller the charge transfer impedance is; the straight line segment represents the diffusion resistance, and the higher the slope of the straight line segment, the smaller the diffusion resistance. As can be seen from fig. 2, the radius of curvature of the circular arc segment of the pre-sodium cell prepared in example 1 is smaller than that of comparative example 1, indicating that the charge transfer resistance of the pre-sodium cell in example 1 is lower than that of the general cell in comparative example 1; the slope of the straight line segment of the pre-sodium cell prepared in example 1 is higher than that of comparative example 1, indicating that the diffusion resistance of the pre-sodium cell in example 1 is lower than that of the general cell in comparative example 1. The charge transfer resistance and diffusion resistance in example 1 were lower than those in comparative example 1, demonstrating that the preformed SEI film optimizes the battery.
As can be seen from the charge and discharge curves of fig. 3, the first charge specific capacity of the general battery in comparative example 1 is 417mAh/g, the first discharge specific capacity is 325mAh/g, and the first coulombic efficiency (first discharge specific capacity/first charge specific capacity) is 78.0%. The first charge specific capacity of the pre-sodium battery of example 1 was 320mAh/g, the first discharge specific capacity was 310mAh/g, and the first coulombic efficiency was 96.8%. The first coulombic efficiency of the pre-sodium battery is improved from 78.0% to 96.8%, and the fact that the irreversible decomposition and other side reactions of the electrolyte in the first circulation process are successfully inhibited through pre-sodium treatment is shown.
As can be seen from the comparison of rate performance tests in fig. 4, the rate performance of the pre-sodium cell of example 1 was greatly improved, maintaining a specific capacity of 198.5mAh/g even at a current density of 5A/g, indicating that the pre-formed SEI film optimized the pre-sodium cell and worked in concert with the SEI film produced by cycling the pre-sodium cell.
The first charge and discharge test was performed on the pre-sodium cell prepared in example 2 and the general cell prepared in comparative example 1, and the test results are shown in fig. 5, in which the first coulombic efficiency of the pre-sodium cell was improved from 78.0% to 132.8%.
The first charge and discharge test was performed on the pre-sodium battery prepared in example 3 and the general battery prepared in comparative example 1, and the test results are shown in fig. 6, in which the first coulombic efficiency of the pre-sodium battery was improved from 78.0% to 97.0%.
The first charge and discharge test was performed on the pre-sodium battery prepared in example 4 and the general battery prepared in comparative example 1, and the test results are shown in fig. 7, in which the first coulombic efficiency of the pre-sodium battery was improved from 78.0% to 99.2%.
The selection of parameters and the results of the tests in examples 1 to 4 and comparative example 1 are shown in table 1.
TABLE 1
This application is through polycyclic aromatic hydrocarbon sodium and film forming additive's combined action, preformed one deck electronic insulation, ionic conduction and insoluble surface SEI membrane on graphite alkene negative pole piece, and the SEI membrane that produces with the battery circulation can the collaborative work, protects sodium ion battery's negative pole better to promote sodium ion battery's each item performance. The method is simple and safe, easy to implement and not easy to generate byproducts.
Although the embodiments of the present application have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the embodiments of the present application.
Claims (10)
1. A preparation method of a pre-sodium graphene negative electrode piece is characterized by comprising the following steps:
preparing a graphene negative pole piece;
dissolving polycyclic aromatic hydrocarbon and a film forming additive in an aprotic polar solvent, and adding excessive metal sodium to enable the polycyclic aromatic hydrocarbon to react completely to generate polycyclic aromatic hydrocarbon sodium to prepare a solution;
soaking the graphene negative pole piece in the solution for 5s-3 min;
and washing the graphene negative electrode piece soaked in the solution for multiple times by using the aprotic polar solvent to obtain the pre-sodium graphene negative electrode piece.
2. The method for preparing the pre-sodium graphene negative electrode plate according to claim 1, wherein the polycyclic aromatic hydrocarbon comprises one or more of biphenyl, biphenylene, polyphenylaliphatic hydrocarbon and polycyclic aromatic hydrocarbon.
3. The method for preparing the pre-sodium graphene negative electrode sheet according to claim 1, wherein the film forming additive comprises cyclic carbonate having a fluorine group and chain carbonate having a fluorine group.
4. The method of making the pre-sodiated graphene negative electrode sheet of claim 3, wherein the film forming additive comprises one or more of fluoroethylene carbonate, difluoroethylene carbonate, and fluoromethyl carbonate.
5. The method for preparing the pre-sodium graphene negative electrode plate according to claim 1, wherein the aprotic polar solvent comprises one or more of dimethylformamide, dimethyl sulfoxide, acetone, tetrahydrofuran and dimethyl ether.
6. The preparation method of the pre-sodium graphene negative electrode plate according to claim 1, wherein the concentration of the polycyclic aromatic hydrocarbon sodium is 0.05-3mol/L, and the concentration of the film forming additive is 0.05-1 mol/L.
7. The preparation method of the pre-sodium graphene negative electrode plate according to claim 1, wherein the step of preparing the graphene negative electrode plate comprises the following steps:
mixing reduced graphene oxide, ketjen black and polyvinylidene fluoride according to parts by weight of 80, 10 and 10, and dissolving the mixture in methyl pyrrolidone to obtain negative active material slurry;
and coating the negative active material slurry on a copper foil, vacuum drying, and blanking to obtain the graphene negative pole piece.
8. A pre-sodiumized graphene negative pole piece is characterized in that the pre-sodiumized graphene negative pole piece is prepared by the preparation method of any one of claims 1 to 7.
9. The pre-sodiated graphene negative electrode sheet of claim 8, wherein said pre-sodiated graphene negative electrode sheet comprises a solid electrolyte interface film.
10. A sodium ion battery comprising a positive plate, a negative plate, an electrolyte and a diaphragm, wherein the negative plate is the pre-sodiumized graphene negative plate of claim 8 or 9.
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| CN115763947A (en) * | 2022-11-07 | 2023-03-07 | 南开大学 | Ampere-hour-grade sodium ion soft package battery |
| WO2023186165A1 (en) * | 2022-04-02 | 2023-10-05 | 华为技术有限公司 | Sodium-ion battery, and preparation method therefor and use thereof |
| CN117254120A (en) * | 2023-11-10 | 2023-12-19 | 中自环保科技股份有限公司 | Sodium ion battery and pre-sodium treatment method thereof |
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| WO2023186165A1 (en) * | 2022-04-02 | 2023-10-05 | 华为技术有限公司 | Sodium-ion battery, and preparation method therefor and use thereof |
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| CN117254120A (en) * | 2023-11-10 | 2023-12-19 | 中自环保科技股份有限公司 | Sodium ion battery and pre-sodium treatment method thereof |
| CN117254120B (en) * | 2023-11-10 | 2024-02-02 | 中自环保科技股份有限公司 | Sodium ion battery and pre-sodium treatment method thereof |
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