CN110060874B - Preparation method of flexible supercapacitor electrode - Google Patents
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- 238000002360 preparation method Methods 0.000 title abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000012528 membrane Substances 0.000 claims abstract description 28
- 239000002121 nanofiber Substances 0.000 claims abstract description 22
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000007772 electrode material Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 238000004806 packaging method and process Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 23
- 239000002134 carbon nanofiber Substances 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003990 capacitor Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229920006280 packaging film Polymers 0.000 claims description 3
- 239000012785 packaging film Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 238000009987 spinning Methods 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 abstract description 15
- 239000002096 quantum dot Substances 0.000 abstract description 7
- 238000004132 cross linking Methods 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- 238000000502 dialysis Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 238000003828 vacuum filtration Methods 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
- H01G11/24—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
-
- 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
- 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
- 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
A preparation method of a flexible supercapacitor electrode comprises the steps of dispersing graphene quantum dots in an organic solvent, slowly adding the organic solvent into a high polymer precursor solution, preparing a nanofiber membrane by an electrostatic spinning method, and packaging the nanofiber membrane, carbon paper and water filter paper to form the flexible supercapacitor electrode. The graphene quantum dots prepared by the method have rich functional groups and good dispersibility in organic solvents, and the nano-fibers prepared on the basis have obvious cross-linking structures; the prepared doped graphene quantum dot nanofiber has sufficient mechanical properties, and the feasibility of the doped graphene quantum dot nanofiber as a flexible supercapacitor electrode material can be remarkably improved.
Description
Technical Field
The invention relates to a technology in the field of nano materials, in particular to an application of a nanofiber doped with graphene quantum dots prepared by an electrostatic spinning method and used as a flexible supercapacitor electrode.
Background
In recent years, with the rise of wearable devices, flexible supercapacitors have received more and more attention. For flexible supercapacitors, flexible electrodes are one of their key components. The current commercial activated carbon needs to add a conductive agent and a binder, which additionally increases the total mass of the device, thereby limiting the application of the activated carbon as a flexible electrode material. In contrast, carbon nanotubes and graphene can be prepared into flexible electrodes by physicochemical methods, but the precise process and high price limit them. Therefore, the development of a preparation method of the flexible electrode material, which has the advantages of low cost, simple preparation process, environmental protection and suitability for mass production, is urgently needed.
Disclosure of Invention
The invention provides a preparation method of a flexible supercapacitor electrode, aiming at the defects that the rate capability and the circulation stability of an electrode material are easily reduced by the existing electrostatic spinning method.
The invention is realized by the following technical scheme:
according to the invention, graphene quantum dots are dispersed in an organic solvent, slowly added into a high polymer precursor solution and used for preparing a nanofiber membrane by an electrostatic spinning method, and then the nanofiber membrane, carbon paper and water filter paper are packaged to form an electrode of a flexible supercapacitor.
The graphene quantum dots are prepared by a photo-Fenton reaction, namely, a graphite oxide aqueous solution and hydrogen peroxide are used as raw materials, and a reaction solution is subjected to rotary evaporation drying after the reaction in a photochemical reactor through a quartz tube to obtain the graphene quantum dots.
The high polymer in the high polymer precursor solution adopts any combination of polyacrylonitrile, polyvinylpyrrolidone and polymethyl methacrylate.
The graphene quantum dots are added into the high polymer precursor solution slowly, preferably by using a syringe.
The electrostatic spinning method comprises the following steps: the method adopts a 5-30kV voltage and drum type receiver, the distance between a spinning needle and the receiver is set to be 5-30cm, the injection speed of the electrostatic spinning solution is 1-10mL/h, and the rotating speed of the receiver is 500-2000 r/min.
The nanofiber membrane is preferably subjected to high-temperature heat treatment, and specifically comprises the following steps: adopting a constant-temperature blast drying box, raising the temperature to 300 ℃ at a temperature rise rate of not more than 3 ℃/min, and preserving the temperature for 10-60 min; then a vacuum crucible furnace is adopted, inert gas is introduced, the temperature is raised to 1000 ℃ at the temperature rise rate of not higher than 2 ℃/min, and the temperature is kept for 10-200 min.
The packaging means that: cutting the carbon nanofiber membrane into two pieces with the same size, respectively attaching the two pieces of carbon nanofiber membrane to carbon paper, separating the two pieces of carbon nanofiber membrane by filter paper, packaging the two pieces of PET membrane on the outer surface of the carbon paper by adopting a hot press, reserving one end of the PET membrane, slowly injecting aqueous electrolyte into an injector for standby until the electrode material is completely wetted, and then packaging the electrode material.
The aqueous electrolyte adopts a sulfuric acid aqueous solution with the concentration of 1M.
The invention relates to a super capacitor which comprises an electrode material, a water-based filter paper diaphragm, a carbon paper current collector and a PET (polyethylene terephthalate) packaging film, wherein the electrode material, the water-based filter paper diaphragm, the carbon paper current collector and the PET packaging film are prepared by the method.
Technical effects
Compared with the prior art, the graphene quantum dots prepared by the method have rich functional groups and good dispersibility in an organic solvent, and the nano-fibers prepared on the basis have an obvious cross-linking structure; the prepared doped graphene quantum dot nanofiber has sufficient mechanical properties, and the feasibility of the doped graphene quantum dot nanofiber as a flexible supercapacitor electrode material can be remarkably improved.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of a doped graphene quantum dot nanofiber prepared according to the present invention;
FIG. 2 is a graph of Cyclic Voltammetry (CV) for different states of the assembled flexible supercapacitor of the present invention.
Detailed Description
Example 1
In this embodiment, an electrostatic spinning method is adopted to prepare a graphene quantum dot doped nanofiber, and the specific steps include:
the method comprises the following steps of firstly, taking a graphite oxide aqueous solution and hydrogen peroxide as raw materials, adding deionized water, placing the mixture in a photochemical reactor for reaction, carrying out vacuum filtration after the reaction is finished, and carrying out rotary evaporation drying to obtain the graphene quantum dots, wherein the method specifically comprises the following steps: taking a certain amount of graphene oxide, dispersing in deionized water to prepare a graphene oxide solution of 2mg/mL, and carrying out ultrasonic treatment for 30 min. Then 5mL of graphene oxide solution, 0.5mL of hydrogen peroxide and 70mL of deionized water are respectively added dropwise into 5 quartz tubes and placed in a photochemical reactor. And after the reaction is carried out for 37min, taking out the product, carrying out rotary evaporation at 50 ℃ for 30min, transferring the product into a dialysis bag, dialyzing for 2-3 days, carrying out rotary evaporation on the product until the product is dried, and collecting the product to obtain the graphene quantum dots.
And secondly, dispersing the graphene quantum dots in an organic solvent, ultrasonically mixing uniformly, and adding a high polymer to prepare a precursor solution, wherein the method specifically comprises the following steps: and (3) dispersing 12mg of the graphene quantum dots obtained in the first step in 5mL of DMF (dimethyl formamide), carrying out ultrasonic treatment for 1h, adding 0.6g of polyacrylonitrile and 0.6g of polymethyl methacrylate, and heating and stirring in an oil bath at 60 ℃ for 8h to obtain a precursor solution which is uniformly mixed.
Step three, preparing the nano-fiber, transferring the precursor solution into a microinjector, adjusting experimental parameters, and performing electrostatic spinning, wherein the preparation method specifically comprises the following steps: the precursor solution was transferred to a 20mL syringe, mounted on a syringe pump using a needle having an inner diameter of 1200 μm, and electrospun. Electrostatic spinning parameters: the voltage is 15kV, the distance between the needle head and the receiver is 15cm, the injection speed of the electrostatic spinning solution is 1.0mL/h, the receiver is a roller, and the rotating speed is 1000 r/min. And collecting the product after electrostatic spinning to obtain the nanofiber membrane.
And fourthly, calcining the electrostatic spinning fiber membrane in an inert atmosphere to obtain a flexible carbon nanofiber membrane, assembling the flexible carbon nanofiber membrane into a flexible supercapacitor by taking the flexible carbon nanofiber membrane as an electrode material, and carrying out electrochemical performance test, wherein the method specifically comprises the following steps: placing the electrostatic spinning nanofiber membrane in a constant-temperature blowing drying oven, heating to 180 ℃ at a heating rate of not higher than 3 ℃/min, preserving heat for 20min, heating to 270 ℃ at a heating rate of 1 ℃/min, and preserving heat for 60min to obtain a preoxidized nanofiber membrane; then placing the obtained nanofiber membrane in an inert atmosphere, raising the temperature to 800 ℃ at a heating rate of 5 ℃/min, and preserving the temperature for 120min to obtain the graphene quantum dot doped carbon nanofiber; finally, cutting the flexible carbon nanofiber membrane into two pieces of 1 multiplied by 1cm2The middle of the square electrode material is separated by filter paper, 1M sulfuric acid electrolyte is injected into the square electrode material to assemble the flexible supercapacitor, the electrochemical performance of the flexible supercapacitor is tested, and the multiplying power performance of the flexible supercapacitor is obtained by calculating according to a formula: the specific capacity is not attenuated after the current density is 320F/g when the current density is 0.25A/g and can reach 220F/g when the current density is 30A/g and the current density is 2A/g after the current density is cycled 10000 times.
Example 2
The embodiment specifically comprises the following steps:
step 1, taking a certain amount of graphene oxide, dispersing the graphene oxide in deionized water to prepare a graphene oxide solution of 2mg/mL, and carrying out ultrasonic treatment for 30 min. Then 5mL of graphene oxide solution, 0.5mL of hydrogen peroxide and 70mL of deionized water are respectively added dropwise into 5 quartz tubes and placed in a photochemical reactor. And after the reaction is carried out for 37min, taking out the product, carrying out rotary evaporation at 50 ℃ for 30min, transferring the product into a dialysis bag, dialyzing for 2-3 days, carrying out rotary evaporation on the product until the product is dried, and collecting the product to obtain the graphene quantum dots.
And 2, taking 60mg of the graphene quantum dots obtained in the step 1, dispersing the graphene quantum dots in 5mL of DMF (dimethyl formamide), carrying out ultrasonic treatment for 1h, adding 0.6g of polyacrylonitrile and 0.6g of polymethyl methacrylate, and heating and stirring the mixture in an oil bath at the temperature of 60 ℃ for 8h to obtain a precursor solution which is uniformly mixed.
And 3, transferring the precursor solution into a 20mL injector, using a needle with the inner diameter of 1200 mu m, clamping the precursor solution on an injection pump, and carrying out electrostatic spinning. Electrostatic spinning parameters: the voltage is 18kV, the distance between the needle head and the receiver is 15cm, the injection speed of the electrostatic spinning solution is 1.0mL/h, the receiver is a roller, and the rotating speed is 1000 r/min. And collecting the product after electrostatic spinning to obtain the flexible carbon nanofiber membrane.
A flexible supercapacitor electrode material was prepared in the same manner as in the fourth step of example 1.
The foregoing embodiments may be modified in many different ways by those skilled in the art without departing from the spirit and scope of the invention, which is defined by the appended claims and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (5)
1. A super capacitor is characterized by comprising an electrode, a water-based filter paper diaphragm, a carbon paper current collector and a PET packaging film; the electrode is formed by dispersing graphene quantum dots in an organic solvent, slowly adding the organic solvent into a high polymer precursor solution, preparing a nanofiber membrane by an electrostatic spinning method, and packaging the nanofiber membrane, carbon paper and water filter paper;
the electrostatic spinning method comprises the following steps: adopting a 5-30kV voltage drum type receiver, setting the distance between a spinning needle head and the receiver to be 5-30cm, the injection speed of the electrostatic spinning solution to be 1-10mL/h, and the rotating speed of the receiver to be 500-2000 r/min;
the packaging means that: cutting the carbon nanofiber membrane into two pieces with the same size, attaching the two pieces of carbon nanofiber membrane to carbon paper respectively, separating the two pieces of carbon nanofiber membrane by using filter paper, packaging the two pieces of PET membrane on the outer surface of the carbon paper by using a hot press, reserving one end of the PET membrane, and slowly injecting aqueous electrolyte into an injector until an electrode material is completely wetted, and then packaging the electrode material;
the graphene quantum dots are prepared by a photo-Fenton reaction, namely, a graphite oxide aqueous solution and hydrogen peroxide are used as raw materials, and a reaction solution is subjected to rotary evaporation drying after the reaction in a photochemical reactor through a quartz tube to obtain the graphene quantum dots.
2. The supercapacitor according to claim 1, wherein the high polymer in the high polymer precursor solution is a combination of polyacrylonitrile, polyvinylpyrrolidone and polymethyl methacrylate.
3. The supercapacitor according to claim 1, wherein the slow addition is performed by adding the graphene quantum dots to the polymer precursor solution using a syringe.
4. The super capacitor as claimed in claim 1, wherein the nanofiber membrane is subjected to a high temperature heat treatment, and specifically comprises: adopting a constant-temperature blast drying box, raising the temperature to 300 ℃ at a temperature rise rate of not more than 3 ℃/min, and preserving the temperature for 10-60 min; then a vacuum crucible furnace is adopted, inert gas is introduced, the temperature is raised to 1000 ℃ at the temperature rise rate of not higher than 2 ℃/min, and the temperature is kept for 10-200 min.
5. The supercapacitor according to claim 1, wherein the aqueous electrolyte is a 1M aqueous solution of sulfuric acid.
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| CN106024421B (en) * | 2016-05-11 | 2018-03-02 | 常州大学 | A kind of preparation of chitosan-based porous carbon materials of graphene quantum dot and its capacitive property research |
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