CN112086299A - Flexible thin film electrode material of super capacitor and preparation method thereof - Google Patents
Flexible thin film electrode material of super capacitor and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of electrode material preparation, and discloses a flexible thin film electrode material of a super capacitor and a preparation method thereof. The preparation method comprises the following steps: mixing nano-cellulose and an electrode active substance, and adding the mixture into a foaming liquid prepared from a surfactant to obtain a mixed slurry; and then, foaming and molding the obtained mixed slurry through a foam molding process, and drying to obtain the flexible film electrode material of the supercapacitor. According to the invention, the flexible film electrode material of the supercapacitor is prepared by adopting a foam forming process, so that the nanocellulose and other electrode active substances can be fully and uniformly mixed, the flexibility, the strength and the excellent electrochemical performance of the electrode material can be ensured, and the internal structure and the specific capacity of the electrode material can be well maintained after the electrode material is bent and folded for a plurality of times; after being recycled for several times, the specific capacity of the composite material can still be kept good. Meanwhile, the foam forming process can save a large amount of fiber raw materials, water and energy consumption, and save the production cost.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a flexible film electrode material of a super capacitor and a preparation method thereof.
Background
Along with the updating and iteration of electronic products, wearable, foldable, portable and lightweight flexible electronic devices are greatly concerned by people, an energy storage device corresponding to the flexible electronic device also needs to have flexibility, and in numerous application fields, a super capacitor is taken as a unique innovative technology, has the advantages of high power density, long cycle service life and the like, and shows great market potential in the research field of flexible electronic products. In recent years, with the research in the field of flexible electronics becoming more and more intensive, most of the prior art for preparing flexible electrode materials adopt a conductive substrate to provide flexibility, for example, carbon fibers, carbon cloth, carbon nanotubes, carbon nanofibers and the like are adopted, such as Murat Cakici and the like, which use carbon fiber textile fabrics as the substrate on which coralliform MnO is uniformly grown2The prepared flexible supercapacitor electrode has 467F/g of high specific capacitance (Advanced electrochemical energy substrates on the flexible carbon fiber fabric-coated with inorganic copper-like MnO)2structured electrodes); the specific capacitance of the supercapacitor assembled by the carbon nanofibers for the people like Hongyanjiang is 114.6F/g (research on the influence of graphene doping on the electrochemical performance of the lignin-based carbon nanofibers), and the adoption of the conductive substrate has high production cost and is not beneficial to industrialization. The existing preparation process mostly adopts methods such as wet forming, vacuum filtration, magnetron sputtering, electrochemical deposition and the like, for example, the inventor of the invention uses an aqueous solution of a conductive polymer or a transition metal oxide as an electrolyte, and adopts a constant potential electrochemical deposition method to deposit the conductive polymer or the transition metal oxide on the surface of a graphene film to prepare a graphene-based composite film (a graphene-based flexible supercapacitor and a preparation method of an electrode material thereof).
The foam forming process is a novel paper sheet forming technology, foam is used as a carrier to bear fibers, so that the fibers can be well dispersed on water-based foam, the fibers are mutually overlapped, and the fibers are deposited on a forming net part by controlling the rupture of the foam to form a one-layer or multi-layer paper sheet structure.
The cellulose is a rich renewable resource on the earth, is degradable and environment-friendly, and has good film forming performance and softness, and the nano-cellulose is not only as green and environment-friendly as common cellulose but also has more excellent mechanical, optical, thermal and other properties due to small size, so that the nano-cellulose is applied to various fields.
The super capacitor combines the advantages of a battery and a traditional capacitor, has high energy density and power density, is used as a standby power supply of a plurality of instruments and equipment due to the advantages of short charging and discharging time, high cycle stability and the like, and is widely applied to a plurality of fields such as energy equipment, power and the like. The preparation of the flexible supercapacitor electrode material has great significance for the development of the flexible electrode material.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of a flexible thin film electrode material of a super capacitor.
The invention also aims to provide the flexible thin film electrode material for the super capacitor prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a flexible thin film electrode material of a super capacitor comprises the following preparation steps:
(1) mixing nano-cellulose and an electrode active substance, and then adding the mixture into a foaming liquid prepared by a surfactant;
(2) and (2) forming the mixed slurry obtained in the step (1) by using a foam forming process, and drying to obtain the flexible thin film electrode material of the super capacitor.
Preferably, the mass ratio of the nano-cellulose to the electrode active material is (30-70)% to (70-30)%.
Preferably, the size of the nano-cellulose is 10-100 nm.
Preferably, the foaming solution is prepared by adding distilled water into a surfactant, and the surfactant is polyvinyl alcohol, sodium dodecyl sulfate, sodium fatty alcohol-polyoxyethylene ether sulfate and the like.
Preferably, the foam forming process is to perform foaming and forming in a foaming device;
preferably, the foaming liquid mixed slurry obtained in the step (1) is poured into a foaming device, the rotating speed of the foaming device is set to 800-; the foaming device is shown in figure 1, and the decay condition of the foam size can be observed by controlling the rotating speed and the foaming time;
preferably, after fully foaming, filtering the foam suspension under the pressure of 9.8-11Kpa, wherein a filtering device is shown in figure 2, and after foaming is finished, applying certain pressure to rapidly filter water to finally obtain the flexible film electrode material of the supercapacitor;
preferably, the foam molding refers to foam molding in a foaming device, and the final molded quantitative amount is 5-30 g/m2The thickness is 10 to 100 μm.
Preferably, the film material formed in the step (2) is put into an oven for drying at the temperature of 80-120 ℃, and the flexible film electrode material of the super capacitor is obtained after drying.
Preferably, the active material is at least one of graphene, manganese dioxide and polyaniline.
Preferably, the graphene refers to single-layer graphene.
Preferably, the electrode active material at least contains graphene, and the mass ratio of the graphene to the electrode active material is 3: 7-1: 1.
A flexible thin film electrode material of a super capacitor is prepared by the method.
The nano-cellulose adopted by the invention has high crystallinity and excellent mechanical property, and plays a role in supporting and reinforcing the whole flexible film electrode material of the super capacitor.
The graphene is formed by stacking carbon atoms, in sp2The hybrid crystal is arranged in a single-layer or honeycomb-shaped mode, has excellent mechanical and electrical properties due to the special structure, has a large specific surface area and has excellent double-layer capacitance performance.
The super capacitor electrode materials, namely manganese dioxide and polyaniline, are low in cost and have excellent pseudo-capacitance performance, the flexible thin film electrode material can be prepared by mixing manganese dioxide, polyaniline and graphene, the excellent double-layer capacitance performance of graphene and the excellent pseudo-capacitance performance of manganese dioxide and polyaniline can be comprehensively exerted, and the overall electrochemical performance of the flexible thin film electrode material of the super capacitor is greatly improved.
The preparation method and the obtained product have the following advantages and beneficial effects:
(1) according to the invention, the flexible film electrode material of the supercapacitor is prepared by foam molding in a foaming device by adopting a foam molding process, the nanocellulose and the electrode activity are uniformly mixed, the porosity of the obtained flexible film electrode material is high, the specific surface area of the material is large, the specific capacitance is large, the flexible film electrode material has high flexibility and excellent electrochemical properties, the flexible film electrode material can be prepared and produced on a large scale, and the flexible film electrode material has great significance for research and preparation of the flexible electrode material;
(2) the foam molding process adopted by the invention can save a large amount of fiber raw materials, water and energy consumption and save the production cost.
(3) On the basis of certain flexibility, the flexible film electrode material of the super capacitor prepared by the invention can be bent and folded for a plurality of times, and the internal structure and specific capacity of the material can be well maintained; after being recycled for several times, the specific capacity of the composite material can still be kept good. The flexible thin film electrode material of the super capacitor is shown in figure 3, has smooth surface and excellent flexibility.
(4) The surfactant used in the invention is green and degradable, does not pollute sewage and wastewater, has good film forming property, cohesiveness and emulsibility, and can control the water filtration degree by adjusting the viscosity of the slurry.
Drawings
Fig. 1 is a schematic structural view of a foaming apparatus used in the embodiment of the present invention.
Fig. 2 is a schematic structural view of a filter device used in the embodiment of the present invention.
FIG. 3 is a diagram of a flexible thin film electrode material of a supercapacitor prepared in example 6 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples and drawings, but the embodiments and the scope of the present invention are not limited thereto.
Example 1
Preparation method of flexible thin film electrode material of supercapacitor of the embodiment
(1) Adding polyvinyl alcohol (purity is more than 95%) into distilled water, preparing foaming liquid with mass concentration of 1%, mixing 30 wt% of nano-cellulose and 70 wt% of single-layer graphene (model number is SE1233, powder, manufacturer is Heizhou sixth element), adding a small amount of distilled water, mixing and pouring into foaming liquid (as shown in figure 1).
(2) Setting the rotation speed of the foaming device at 800 rpm, the foaming time at 30 minutes, applying a pressure of 9.8Kpa to filter after the foaming is finished (as shown in figure 2), and obtaining the flexible membrane electrode material with the quantitative of 30g/m2And the thickness is 10 mu m, and then the uncovered flexible thin film electrode material is put into a blast drier for drying at the drying temperature of 120 ℃ to obtain the flexible thin film electrode material of the super capacitor.
Example 2
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials are 40 wt% of nanocellulose and 60 wt% of single-layer graphene, and other steps are completely the same.
Example 3
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials are 50 wt% of nanocellulose and 50 wt% of single-layer graphene, and other steps are completely the same.
Example 4
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials comprise 60 wt% of nanocellulose and 40 wt% of single-layer graphene, and other steps are completely the same.
Example 5
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials are 70 wt% of nanocellulose and 30 wt% of single-layer graphene, and other steps are completely the same.
The performance test results of the flexible thin film electrode material of the supercapacitor obtained in the above examples 1 to 5 are shown in table 1:
TABLE 1
| Examples | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (omega/sq) |
| 1 | 3072.31 | 154.83 | 8.33 |
| 2 | 3126.64 | 101.42 | 11.57 |
| 3 | 3842.59 | 82.63 | 15.39 |
| 4 | 3524.33 | 57.38 | 27.44 |
| 5 | 3348.96 | 36.29 | 52.26 |
The performance test results of the flexible film electrode material of the super capacitor obtained in the above examples 1-5 after folding and cyclic charge and discharge 1000 are shown in table 2:
TABLE 2
The specific capacitance value test results of the supercapacitor flexible thin film electrode material obtained in the above example 1 at different scanning rates are shown in table 3:
TABLE 3
| Scanning Rate (mv/s) | 10 | 30 | 50 | 70 | 90 |
| Specific capacitance value (F/g) | 154.83 | 95.64 | 68.40 | 42.97 | 26.54 |
Each performance index in the above tables 1 and 2 was measured at a scanning rate of 10 mv/s.
From the results in table 1, it can be seen that the elastic modulus in example 1 also reaches a larger value, and the specific capacitance and the sheet resistance of the flexible film material are better than those of other examples, i.e. the amount of graphene is larger than that of nanocellulose, so that the flexible film material has a larger specific capacity and a lower sheet resistance, which is a preferred example.
From the results in table 2, it can be seen that the performance indexes of the flexible thin film electrode materials of the super capacitor prepared in examples 1 to 5 are kept good after the flexible thin film electrode materials are folded for 1000 times and are circularly charged and discharged for 1000 times.
From the results in table 3, it can be seen that the specific capacitance value of the flexible thin film electrode material of the super capacitor obtained in the invention is greatly influenced by the scanning rate, the performance of the flexible thin film electrode material of the super capacitor is better at a low scanning rate, and the service life of the electrode material is longer.
Examples 6 to 11 are preparation examples of the flexible thin film electrode material of the supercapacitor:
example 6
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials comprise 30 wt% of nanocellulose, 50 wt% of single-layer graphene and 20 wt% of manganese dioxide, and other steps are completely the same.
The prepared flexible thin film electrode material of the hierarchical capacitor is shown in figure 3.
Example 7
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials comprise 30 wt% of nanocellulose, 40 wt% of single-layer graphene and 30 wt% of manganese dioxide, and other steps are completely the same.
Example 8
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials comprise 30 wt% of nanocellulose, 30 wt% of single-layer graphene and 40 wt% of manganese dioxide, and other steps are completely the same.
The performance test results of the flexible thin film electrode materials of the super capacitors obtained in the above examples 6 to 8 are shown in table 4:
TABLE 4
| Examples | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (omega/sq) |
| 6 | 3175.38 | 185.78 | 13.71 |
| 7 | 3096.98 | 139.94 | 22.25 |
| 8 | 2985.40 | 125.47 | 35.31 |
The performance test results of the flexible film electrode material of the super capacitor obtained in the above examples 6 to 8 after folding and 1000 times of cyclic charge and discharge are shown in table 5:
TABLE 5
Each performance index in the above tables 4 and 5 was measured at a scanning rate of 10 mv/s.
From the results in table 4, on the basis of the examples 1 to 5, the specific capacity of the flexible thin film electrode material of the supercapacitor obtained by foam molding in the examples 6 to 8 after adding a part of manganese dioxide is greatly improved compared with that in the examples 1 to 5, which is the result of the comprehensive effect of the manganese dioxide pseudo-capacitance and the graphene double electric layer capacitance, and the comprehensive performance of the flexible thin film electrode material of the supercapacitor can be effectively improved by adding a small amount of manganese dioxide.
From the results in table 5, it can be seen that the performance indexes of the supercapacitor flexible thin film electrode materials prepared in examples 6 to 8 can be kept good in all aspects after 1000 times of folding and 1000 times of cyclic charge and discharge.
Example 9
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials comprise 30 wt% of nanocellulose, 50 wt% of single-layer graphene and 20 wt% of polyaniline, and other steps are completely the same.
Example 10
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials comprise 30 wt% of nanocellulose, 40 wt% of single-layer graphene and 30 wt% of polyaniline, and other steps are completely the same.
Example 11
Compared with the preparation method of the flexible thin film electrode material of the supercapacitor in the embodiment 1, the preparation method of the flexible thin film electrode material of the supercapacitor is different in that the raw materials comprise 30 wt% of nanocellulose, 30 wt% of single-layer graphene and 40 wt% of polyaniline, and other steps are completely the same.
The performance test results of the flexible thin film electrode materials of the super capacitors obtained in the above examples 9 to 11 are shown in table 6:
TABLE 6
| Examples | Modulus of elasticity (Mpa) | Specific capacity (F/g) | Surface resistance (omega/sq) |
| 9 | 3574.38 | 103.41 | 17.84 |
| 10 | 3884.67 | 118.91 | 19.51 |
| 11 | 3763.28 | 161.47 | 25.54 |
The performance test results of the flexible film electrode material for the super capacitor obtained in the above examples 9 to 11 after folding and 1000 times of cyclic charge and discharge are shown in table 7:
TABLE 7
Each performance index in the above tables 6 and 7 was measured at a scanning rate of 10 mv/s.
From the results in table 6, on the basis of the embodiments 1 to 5, after polyaniline is added in the embodiments 9 to 11, the specific capacity of the flexible thin film electrode material of the super capacitor obtained by wet forming is greatly improved compared with the embodiments 1 to 5, which is the result of the comprehensive effect of the pseudo capacitance of the polyaniline and the electric double layer capacitance of the graphene, and the comprehensive performance of the flexible thin film electrode material of the super capacitor can be effectively improved by adding part of the polyaniline.
From the results in table 7, it can be seen that the performance indexes of the supercapacitor flexible thin film electrode materials prepared in examples 9 to 11 can be kept good in all aspects after 1000 times of folding and 1000 times of cyclic charge and discharge.
From the above results, it can be seen that the flexible thin film electrode material for the supercapacitor prepared by the invention can exert respective pseudo-capacitance performance by adding manganese dioxide and polyphenyl, and improve the electrochemical performance of the flexible composite thin film electrode material for the supercapacitor, and examples 6 to 8 are superior to examples 9 to 11, that is, the electrochemical performance of the flexible composite thin film electrode material after adding manganese dioxide is superior to that of the flexible composite thin film electrode material after adding polyaniline.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a flexible thin film electrode material of a super capacitor is characterized by comprising the following preparation steps:
(1) mixing nano-cellulose and an electrode active substance, and then adding the mixture into a foaming liquid prepared by a surfactant;
(2) and (2) forming the mixed slurry obtained in the step (1) by using a foam forming process, and drying to obtain the flexible thin film electrode material of the super capacitor.
2. The preparation method of the flexible thin film electrode material for the supercapacitor as claimed in claim 1, wherein the mass ratio of the nanocellulose to the electrode active material is (30-70)% to (70-30)%.
3. The preparation method of the flexible thin film electrode material for the supercapacitor, according to claim 1, wherein the size of the nanocellulose is 10-100 nm.
4. The preparation method of the flexible film electrode material of the supercapacitor, according to claim 1, wherein the foaming solution is prepared by adding distilled water to a surfactant, and the surfactant is polyvinyl alcohol, sodium dodecyl sulfate or sodium fatty alcohol-polyoxyethylene ether sulfate.
5. The preparation method of the flexible thin film electrode material for the supercapacitor according to claim 1, wherein the electrode active material is at least one of graphene, manganese dioxide and polyaniline.
6. The preparation method of the flexible thin film electrode material for the supercapacitor according to claim 5, wherein the graphene is single-layer graphene.
7. The preparation method of the flexible thin-film electrode material for the supercapacitor according to claim 5, wherein the electrode active material at least contains graphene, and the mass ratio of the graphene to the electrode active material is 3: 7-1: 1.
8. the preparation method of the flexible thin-film electrode material for the supercapacitor according to claim 1, wherein the foam forming process comprises foaming and forming in a foaming device, the rotating speed of the foaming is set to be 800-1500 rpm, the foaming time is 20-30 minutes, the forming is filtration forming, and the quantitative amount is 5-30 g/m2The thickness is 10 to 100 μm, and the pressure of the filtration is 9.8 to 11 kpa.
9. The preparation method of the flexible thin film electrode material for the supercapacitor according to claim 1, wherein the drying temperature is 80-120 ℃.
10. A flexible thin film electrode material for a super capacitor, which is prepared by the method of any one of claims 1 to 9.
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| CN115360024A (en) * | 2022-08-10 | 2022-11-18 | 五邑大学 | Super capacitor and preparation method and application thereof |
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