CN110676070A - Graphene flexible supercapacitor with self-healing function and preparation method thereof - Google Patents
Graphene flexible supercapacitor with self-healing function and preparation method thereof Download PDFInfo
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 70
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000010410 layer Substances 0.000 claims abstract description 52
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 229920006299 self-healing polymer Polymers 0.000 claims abstract description 10
- 229920002635 polyurethane Polymers 0.000 claims abstract description 9
- 239000004814 polyurethane Substances 0.000 claims abstract description 9
- 229920001610 polycaprolactone Polymers 0.000 claims abstract description 8
- 239000004632 polycaprolactone Substances 0.000 claims abstract description 8
- 239000002356 single layer Substances 0.000 claims abstract description 7
- 238000004528 spin coating Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 abstract description 16
- 230000035772 mutation Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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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- 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
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Abstract
The invention discloses a graphene flexible supercapacitor with a self-healing function and a preparation method thereof, wherein the graphene flexible supercapacitor with the self-healing function comprises a graphene layer and a self-healing layer, the graphene layer is formed by a continuous single-layer or multi-layer pure graphene film, the self-healing layer is prepared by mixing polycaprolactone and polyurethane, and the preparation method of the graphene flexible supercapacitor with the self-healing function comprises the steps of firstly forming continuous graphene on the surface of a metal, then dripping or spin-coating self-healing polymers, and then corroding a metal layer to form the flexible capacitor with the continuous graphene film. The graphene flexible supercapacitor with the self-healing function, which is obtained by the invention, has the self-healing function after being bent repeatedly and greatly, is high in resistivity stability, and the capacitance performance can not have large mutation, so that the graphene flexible supercapacitor with the self-healing function can be widely applied to the technical field of large exercise amount and wearing.
Description
Technical Field
The invention relates to the technical field of super capacitors, in particular to a graphene flexible super capacitor with a self-healing function and a preparation method thereof.
Background
A super capacitor, also called an electrochemical capacitor, is a novel ideal energy storage device. It has the advantages of both traditional parallel plate capacitors and secondary batteries, such as: high capacitance, high power density, rapid charge and discharge, long cycle service life, etc. The super capacitor can be divided into an electrochemical double-layer capacitor, a pseudo capacitor and a hybrid capacitor from an energy storage mechanism.
Graphene is a two-dimensional nanomaterial formed by arranging carbon atoms in an SP2 manner, and has stable chemical properties, excellent mechanical properties, good heat and electricity conduction performance and the like. Graphene becomes a preferred material for next-generation electronic devices, and is widely applied in the fields of flexible sensing and energy storage devices. The theoretical specific surface area of the graphene can reach 2630m2/g, and the porous two-dimensional nanostructure, the stable electrochemical performance and the good conductivity determine that the graphene can be used as a good capacitance electrode material.
At present, with the need of social development, flexible electronic technology will have great influence on human society. The development of the electronic products, which is changing day by day, puts more demands on the flexible electronic technology. Flexible electronic devices need to be endowed with some more sophisticated functions to meet the demand. For example: can be highly stretched, self-healing, arbitrarily deformed, waterproof, bent, folded and the like. The research on flexible electronic devices plays a crucial role in particular in the development of current wearable electronic devices, and the research field is more and more favored by researchers.
In recent years, flexible electronic materials from healing have been pursued by researchers, and at present, a plurality of researchers endow super capacitors with self-healing functions, so that the super capacitors can be prepared to have self-healing functions under the condition that the capacitors are damaged by external machinery, and the capacitance functions of the super capacitors can be recovered. There is a report in the literature that a supercapacitors with all-round self-repairing function was developed by professor mochini. The super capacitor with the stretchable performance and the self-repairing performance is prepared by the high-definition Hualiangyo by using the stretchable and reducible graphene-based fiber spring as a stretchable electrode and using the self-repairing polyurethane material as a protective shell.
Patent CN201810296810.4 discloses a graphene supercapacitor and a manufacturing method thereof, in the method, a conductive solution is prepared by compounding graphene and a polymer, a polytetrafluoroethylene or a glass sheet is used as a template to prepare a conductive functional film, a mixed solution of polycaprolactone and polyurethane is attached to the surface of the conductive film by a dropping coating or spin coating method, and a flexible supercapacitor is prepared after drying. However, compared with a pure graphene film, the conductive layer of the flexible supercapacitor in the patent still has a larger difference in conductivity, which is also a problem commonly existing in the current flexible supercapacitors.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a graphene flexible supercapacitor with a self-healing function and a preparation method thereof, and solves the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a graphene flexible supercapacitor with a self-healing function comprises a graphene layer and a self-healing layer, and is characterized in that the graphene layer is formed by a continuous single-layer or multi-layer pure graphene film; the self-healing layer is prepared by mixing polycaprolactone and polyurethane.
Preferably, the graphene layer is formed by chemical vapor deposition.
Preferably, the thickness of the graphene layer is 1-1000 nm.
A preparation method of a graphene flexible supercapacitor with a self-healing function comprises the following steps:
s1: continuously depositing a graphene film layer on a metal substrate by using a chemical vapor deposition method, and preparing the metal substrate with graphene deposited on the surface at the preparation temperature of 550 ℃ by using a continuous tunnel furnace;
s2: dissolving polycaprolactone and polyurethane in a mass ratio of 1:1 by using an organic solvent, and stirring to prepare a self-healing polymer solution;
s3: dropping or spin-coating a self-healing polymer solution on the graphene film layer I of the metal substrate with the surface deposited with the graphene prepared in S1, baking, and volatilizing an organic solvent to obtain a three-layer structure film of the metal substrate-graphene-self-healing polymer layer;
s4: and (3) soaking the three-layer structure film obtained in the step (S3) in a corrosive liquid at the temperature of 60-80 ℃, removing the metal substrate, washing with water, and drying at the temperature of 70-90 ℃ for 0.5-1h to obtain the graphene flexible supercapacitor with the self-healing function.
Preferably, the metal substrate in step S1 is copper or aluminum, and has a thickness of 10um or more.
Preferably, the organic solvent in step S2 is one or more of N, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, tetrahydrofuran, or N-methylpyrrolidone.
Preferably, the reaction temperature in the step S2 is 50-90 ℃, and the stirring time is 15-120 min.
Preferably, the graphene thin film layer in step S3 is a single-layer or multi-layer stacked structure.
Preferably, the baking temperature in the step S3 is 50-90 ℃, and the baking time is 1-2 h.
The invention has the beneficial effects that: the graphene flexible supercapacitor with the self-healing function, which is obtained by the invention, has the self-healing function after being bent repeatedly and greatly, is high in resistivity stability, and the capacitance performance can not have large mutation, so that the graphene flexible supercapacitor can be widely applied to the technical field of large exercise amount and wearing.
Drawings
FIG. 1 is a schematic cross-sectional view of a super capacitor according to the present invention;
FIG. 2 is a block diagram of a method for manufacturing a supercapacitor according to the present invention;
in the figure, 1-graphene layer, 2-self-healing layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, 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 invention.
Referring to fig. 1, the present invention provides a graphene flexible supercapacitor with a self-healing function, which includes a graphene layer (1) and a self-healing layer (2), and is characterized in that the graphene layer (1) is formed by a continuous, single-layer or multi-layer pure graphene film; the self-healing layer (2) is prepared by mixing polycaprolactone and polyurethane.
Further, the graphene layer (1) is prepared by a chemical vapor deposition method.
Further, the thickness of the graphene layer (1) is 1-1000 nm.
Referring to fig. 2, the invention provides a preparation method of a graphene flexible supercapacitor with a self-healing function, which includes the following steps:
s1: continuously depositing a graphene film layer on a metal substrate by using a chemical vapor deposition method, and preparing the metal substrate with graphene deposited on the surface at the preparation temperature of 550 ℃ by using a continuous tunnel furnace;
s2: dissolving polycaprolactone and polyurethane in a mass ratio of 1:1 by using an organic solvent, and stirring to prepare a self-healing polymer solution;
s3: dropping or spin-coating a self-healing polymer solution on the graphene film layer I of the metal substrate with the surface deposited with the graphene prepared in S1, baking, and volatilizing an organic solvent to obtain a three-layer structure film of the metal substrate-graphene-self-healing polymer layer;
s4: and (3) soaking the three-layer structure film obtained in the step (S3) in a corrosive liquid at the temperature of 60-80 ℃, removing the metal substrate, washing with water, and drying at the temperature of 70-90 ℃ for 0.5-1h to obtain the graphene flexible supercapacitor with the self-healing function.
Further, the metal substrate in step S1 is copper or aluminum, and has a thickness of 10um or more.
Further, the organic solvent in step S2 is one or more of N, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, tetrahydrofuran, or N-methylpyrrolidone.
Further, the reaction temperature in the step S2 is 50-90 ℃, and the stirring time is 15-120 min.
Further, the graphene thin film layer in step S3 is a single-layer or multi-layer stacked structure.
Further, the baking temperature in the step S3 is 50-90 ℃, and the baking time is 1-2 h.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. A graphene flexible supercapacitor with a self-healing function comprises a graphene layer (1) and a self-healing layer (2), and is characterized in that the graphene layer (1) is formed by a continuous single-layer or multi-layer pure graphene film; the self-healing layer (2) is prepared by mixing polycaprolactone and polyurethane.
2. The graphene flexible supercapacitor with a self-healing function according to claim 1, wherein: the graphene layer (1) is prepared by a chemical vapor deposition method.
3. The method of claim 1, wherein: the thickness of the graphene layer (1) is 1-1000 nm.
4. A preparation method of a graphene flexible supercapacitor with a self-healing function is characterized by comprising the following steps:
s1: continuously depositing a graphene film layer on a metal substrate by using a chemical vapor deposition method, and preparing the metal substrate with graphene deposited on the surface at the preparation temperature of 550 ℃ by using a continuous tunnel furnace;
s2: dissolving polycaprolactone and polyurethane in a mass ratio of 1:1 by using an organic solvent, and stirring to prepare a self-healing polymer solution;
s3: dropping or spin-coating a self-healing polymer solution on the graphene film layer I of the metal substrate with the surface deposited with the graphene prepared in S1, baking, and volatilizing an organic solvent to obtain a three-layer structure film of the metal substrate-graphene-self-healing polymer layer;
s4: and (3) soaking the three-layer structure film obtained in the step (S3) in a corrosive liquid at the temperature of 60-80 ℃, removing the metal substrate, washing with water, and drying at the temperature of 70-90 ℃ for 0.5-1h to obtain the graphene flexible supercapacitor with the self-healing function.
5. The preparation method of the graphene flexible supercapacitor with the self-healing function according to claim 4, wherein the preparation method comprises the following steps: the metal substrate in step S1 is copper or aluminum, and has a thickness of 10um or more.
6. The preparation method of the graphene flexible supercapacitor with the self-healing function according to claim 4, wherein the preparation method comprises the following steps: the organic solvent in step S2 is one or more of N, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, tetrahydrofuran, or N-methylpyrrolidone.
7. The preparation method of the graphene flexible supercapacitor with the self-healing function according to claim 4, wherein the preparation method comprises the following steps: the reaction temperature in the step S2 is 50-90 ℃, and the stirring time is 15-120 min.
8. The preparation method of the graphene flexible supercapacitor with the self-healing function according to claim 4, wherein the preparation method comprises the following steps: the graphene thin film layer in step S3 is a single-layer or multi-layer stacked structure.
9. The preparation method of the graphene flexible supercapacitor with the self-healing function according to claim 4, wherein the preparation method comprises the following steps: the baking temperature in the step S3 is 50-90 ℃, and the baking time is 1-2 h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009126758A (en) * | 2007-11-26 | 2009-06-11 | Institute Of National Colleges Of Technology Japan | Surface-modified carbon material and its forming method |
| CN105590703A (en) * | 2016-03-10 | 2016-05-18 | 中国科学院重庆绿色智能技术研究院 | Preparation method of graphical three-dimensional graphene/polyurethane flexible conductive film |
| CN105679678A (en) * | 2016-03-18 | 2016-06-15 | 武汉华星光电技术有限公司 | Preparation method for graphene thin film transistor |
| CN107275121A (en) * | 2017-07-12 | 2017-10-20 | 广东工业大学 | A kind of ultracapacitor with self-healing and preparation method thereof |
| CN108735524A (en) * | 2018-03-30 | 2018-11-02 | 广东工业大学 | A kind of dilute flexible super capacitor of graphite of the self-healing of high elongation deformation and its preparation method and application |
-
2019
- 2019-10-18 CN CN201910995526.0A patent/CN110676070A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009126758A (en) * | 2007-11-26 | 2009-06-11 | Institute Of National Colleges Of Technology Japan | Surface-modified carbon material and its forming method |
| CN105590703A (en) * | 2016-03-10 | 2016-05-18 | 中国科学院重庆绿色智能技术研究院 | Preparation method of graphical three-dimensional graphene/polyurethane flexible conductive film |
| CN105679678A (en) * | 2016-03-18 | 2016-06-15 | 武汉华星光电技术有限公司 | Preparation method for graphene thin film transistor |
| CN107275121A (en) * | 2017-07-12 | 2017-10-20 | 广东工业大学 | A kind of ultracapacitor with self-healing and preparation method thereof |
| CN108735524A (en) * | 2018-03-30 | 2018-11-02 | 广东工业大学 | A kind of dilute flexible super capacitor of graphite of the self-healing of high elongation deformation and its preparation method and application |
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