CN108630462A - Nanofiber-based integrated film ultracapacitor of one kind and preparation method thereof - Google Patents
Nanofiber-based integrated film ultracapacitor of one kind and preparation method thereof Download PDFInfo
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- CN108630462A CN108630462A CN201810496063.9A CN201810496063A CN108630462A CN 108630462 A CN108630462 A CN 108630462A CN 201810496063 A CN201810496063 A CN 201810496063A CN 108630462 A CN108630462 A CN 108630462A
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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
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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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- 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
- 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 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
- H01G11/46—Metal oxides
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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
- H01G11/48—Conductive polymers
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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
- H01G11/52—Separators
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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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- 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 discloses a kind of preparation methods of nanofiber-based integrated film ultracapacitor, include the following steps：The aqueous solution of polyvinyl alcohol (PVA) is added in the aqueous dispersions of cellulose nano-fibrous (CNFs) and is uniformly dispersed, the mixed liquor of PVA and CNFs are obtained；It takes isopropanol that the mixed liquor of PVA and CNFs is added, after stirring evenly, mixed liquor is obtained into the nanofiber-based aquagel membrane of high ionic conductivity by freeze-thaw method；Conductive material and PVA are coated in nanofiber-based aquagel membrane both sides after mixing, conductive gel layer is formed again by freeze-thaw method, nanofiber-based integrated film ultracapacitor is made.There is good biocompatibility, flexibility and excellent storing up electricity performance by the integrated film ultracapacitor that this method is prepared, can be applied to wearable energy storage device field.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to a kind of nanofiber-based integrated film ultracapacitor and
Preparation method.
Background technology
Hydrogel is a kind of three-dimensional network flexible material with water-retaining property, can adsorb electrolyte as solid electrolyte
It is applied to energy storage field.A kind of natural biological of cellulose nano-fibrous (CNFs) as high length-diameter ratio and larger surface-active
Material has good biocompatibility, the physical actions such as winding and hydrogen bond can be formed with high-polymer molecular chain, to improve
The mechanics and flexility of composite material.
Ultracapacitor is a kind of new type of energy storage device between traditional capacitor and battery, has power density
The high, advantages such as the charge and discharge time is short.With the fast development of lightweight, flexibility, even wearable electronic, the energy is provided for it
Energy storage device also need to develop to flexible and efficient direction.It is conductive using nanofiber-based aquagel membrane as capacitor diaphragm
Hydrogel layer prepares integrated flexible ultracapacitor as electrode, and the Maximum Contact of electrode material and electrolyte may be implemented
Area reduces interfacial effect, improves ion transmission efficiency, excellent energy-storage property and good mechanical property, flexibility, can
Applied to fields such as wearable, portable energy-storing devices.
Invention content
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
Nanofiber-based integrated film ultracapacitor of kind and preparation method thereof.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of preparation method of nanofiber-based integrated film ultracapacitor, includes the following steps：
(1) nanofiber-based aquagel membrane is prepared using freeze-thaw method；
(2) mixed solution of conductive material and polyvinyl alcohol is prepared；
(3) mixed solution obtained by step (2) is coated uniformly on nanofiber-based aquagel membrane positive and negative two obtained by step (1)
On face, above-mentioned resulting materials are then handled by freeze-thaw method, obtain coating by diaphragm, film two sides of nanofiber-based aquagel membrane
Conductive material respectively as positive and negative electrode integrated film ultracapacitor.
Effect of the polyvinyl alcohol in step (2) mainly bonds, and conductive material is affixed to film surface, makes the electricity to be formed
It is extremely not easily to fall off, become electrode/diaphragm/electrode integrated energy storage device.In addition the polyvinyl alcohol material consistent with film main body is selected
Material reduces the interfacial effect of electrode material and diaphragm.
Above-mentioned preparation method, it is preferred that described to prepare nanofiber-based water-setting using freeze-thaw method in the step (1)
The concrete operations of glued membrane are：Polyvinyl alcohol water solution is added dropwise into cellulose nano-fibrous aqueous dispersions and stirs evenly, obtains
The mixed liquor of cellulose nano-fibrous/polyvinyl alcohol takes isopropanol that the mixed liquor of cellulose nano-fibrous/polyvinyl alcohol is added
In, using freeze-thaw method, nanofiber-based aquagel membrane is obtained after mixed liquor freeze-thaw is recycled 4~6 times.
Effect of the polyvinyl alcohol in step (1) is to form the agent structure of aquagel membrane.
Above-mentioned preparation method, it is preferred that in the polyvinyl alcohol water solution mass fraction of polyvinyl alcohol be 1%~
10%；Cellulose nano-fibrous mass fraction is 0.3%~0.5% in the cellulose nano-fibrous aqueous dispersions；Fiber
The mass ratio of plain nanofiber aqueous dispersions and polyvinyl alcohol water solution is 1:(0.2~3).Polyvinyl alcohol mass fraction is less than
1% solution is too dilute, formed lepthymenia in the case of same volume；Polyvinyl alcohol mass fraction is higher than 10%, then solution viscosity is excessively high,
It is not easy to the dispersion of nanofiber.Cellulose nano-fibrous mass fraction is excessively high, and nanofiber is not easy to be uniformly dispersed；Cellulose is received
Rice fiber quality score is too low, is not easy to form a film, this cellulose nano-fibrous mass fraction range film-formation result is preferable.Polyvinyl alcohol
Ratio is excessive, and gained gel mould is partially hard, and flexibility reduces；Cellulose nano-fibrous ratio is excessive, and gained gel film-strength is low, is easy to
Rupture.
Above-mentioned preparation method, it is preferred that the dropwise addition polyvinyl alcohol into cellulose nano-fibrous aqueous dispersions is water-soluble
The dispersion process of liquid is carried out in the case where power is the ul-trasonic irradiation of 100W~150W, polyvinyl alcohol water solution drop rate 1
Then above-mentioned mixed liquor is stirred and is heated 0.5~2 hour under the conditions of 40 DEG C~70 DEG C by~2g/min.Due to polyvinyl alcohol
Solution viscosity is more than cellulose nano-fibrous aqueous dispersions, therefore polyvinyl alcohol is added dropwise into cellulose nano-fibrous aqueous dispersions
Aqueous solution.It is cellulose nano-fibrous to be preferably uniformly dispersed with polyvinyl alcohol under the conditions of 40 DEG C~70 DEG C, and will not draw
Play cellulose nano-fibrous high temperature degradation.
Above-mentioned preparation method, it is preferred that the additive amount of the isopropanol is cellulose nano-fibrous/polyvinyl alcohol
The 10%~200% of liquid quality.The effect of isopropanol is defoaming.Isopropanol adding too much so that be not easy into gel mould；Addition
Measure it is too low, almost without defoaming effect.
Above-mentioned preparation method, it is preferred that in the step (1), in the step (1), freeze-thaw process culture dish
Remain open；The design parameter of freeze-thaw process is that cryogenic temperature is -50 DEG C~-30 DEG C, and cooling time is 2~5 small
When, thaw point is 10 DEG C~30 DEG C, and thawing time is 2~5 hours.
Above-mentioned preparation method, it is preferred that in the step (2), the mixing for preparing conductive material and polyvinyl alcohol
The concrete operations of solution are：Polyvinyl alcohol water solution is added dropwise simultaneously with the rate of 1~2g/min into the aqueous dispersions of conductive material
It stirs evenly, obtains the mixed solution of conductive material/polyvinyl alcohol；The mass fraction of the aqueous dispersions of the conductive material is
1wt%~15wt%；The mass fraction of the polyvinyl alcohol water solution is 1wt%~10wt%；Conductive material aqueous dispersions with
Polyvinyl alcohol water solution mass ratio is (1~3)：1.The mass fraction of conductive material aqueous dispersions is excessively high, then is difficult to be uniformly dispersed；
The too low then concentration of mass fraction is low, and it is low to make the density after electrode material.The mass fraction of polyvinyl alcohol water solution is less than 1%,
Then solution is too dilute, formed lepthymenia in the case of same volume；Mass fraction is higher than 10%, then solution viscosity is excessively high, is not easy to receive
The dispersion of rice fiber.
Above-mentioned preparation method, it is preferred that in the step (2), the conductive material is polyaniline (PANI), polypyrrole
(PPy), graphene (GR), carbon nanotube (CNT) and manganese dioxide (MnO2) in one kind.These types of conductive material electric conductivity
It is relatively good, it is dispersed in poly-vinyl alcohol solution and is coated on gelatin membrane as electrode material.
Above-mentioned preparation method, it is preferred that in the step (3), mixed solution obtained by step (2) is coated uniformly on step
Suddenly the amount on nanofiber-based aquagel membrane tow sides obtained by (1) is that single side coats 50~200mg/100mm2；It is described to pass through
Freeze-thaw method processing resulting materials refer to carrying out freeze-thaw 4~6 times to resulting materials；The design parameter of freeze-thaw process is
Cryogenic temperature is -50 DEG C~-30 DEG C, and cooling time is 2~5 hours, and thaw point is 10 DEG C~30 DEG C, and thawing time is 2~5
Hour.
The inventive concept total as one, the present invention also provides a kind of nanofiber-based one that above-mentioned preparation method obtains
Change film ultracapacitor.
Compared with the prior art, the advantages of the present invention are as follows：
(1) the nanofiber-based aquagel membrane that the present invention uses is not only nontoxic, degradable, has good bio-compatible
Property, also very high flexibility and excellent ionic conductivity.The realization of high ionic conductivity has benefited from nano-cellulose surface
Abundant sulfonic acid group, it is ionizable go out for ion transmission carrier --- hydrogen ion.
(2) the integrated film ultracapacitor prepared by the present invention compares existing ultracapacitor, reduces electrode
Interfacial effect between material and diaphragm, and have very high flexibility, easy to carry and preserve, preparation method is easy, cost compared with
It is low.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the ionic conductivity of the nanofiber-based aquagel membrane prepared by the embodiment of the present invention 1.(Nanowire in figure
The ionic conductivity of Wiki aquagel membrane is 3.55 × 10-2S-1The ionic conductivity of m, pure polyvinyl alcohol hydrogel film is
1.20×10-2S-1·m)。
Fig. 2 is the photo and the film of nanofiber-based integrated film ultracapacitor prepared by the embodiment of the present invention 2
The Cyclic voltamogram curve of ultracapacitor.
Fig. 3 is the constant current charge-discharge of nanofiber-based integrated film ultracapacitor prepared by the embodiment of the present invention 2
Curve.
Specific implementation mode
To facilitate the understanding of the present invention, the present invention is done below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but protection scope of the present invention is not limited to following specific examples.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of preparation method of nanofiber-based integrated film ultracapacitor of the present invention, includes the following steps：
(1) aqueous solution for weighing 5% polyvinyl alcohol of 10g (PVA) is added dropwise to 0.5% cellulose nanometers of 20g in ultrasound
In the aqueous dispersions of fiber, 50 DEG C stir evenly after obtain the mixed liquor of CNFs and PVA.
(2) 30g isopropanols are weighed to be added dropwise to CNFs obtained by step (1) and in PVA mixed liquors, stir evenly at 50 DEG C and nothing
After bubble, it is cooled to room temperature.It takes 10g mixed liquors to pour into the culture dish of Ф 6cm, so that culture dish is remained open state, -40
2h is freezed at DEG C, thaw 2h at 20 DEG C, recycles 5 times, obtains nanofiber-based aquagel membrane.Nanofiber-based aquagel membrane from
Electron conductivity is as shown in Figure 1.
(3) aqueous suspension of 10g10% polyanilines (PANI) is uniformly mixed with 7.5g 5%PVA solution, obtains PANI/
The mixed solution of PVA.
(4) PANI/PVA mixed solutions obtained by step (3) are coated in nanofiber-based aquagel membrane two obtained by step (2)
(single side coated weight is 50~200mg/100mm for side2), 2h is freezed at -40 DEG C, thaw 2h at 20 DEG C, such Frozen-thawed cycled 5 times
After obtain nanofiber-based integrated film ultracapacitor.
Embodiment 2：
A kind of preparation method of nanofiber-based integrated film ultracapacitor of the present invention, includes the following steps：
(1) aqueous solution for weighing 5g 10%PVA is added dropwise to the cellulose nano-fibrous moisture of 25g 0.5% in ultrasound
In dispersion liquid, 45 DEG C stir evenly after obtain the mixed liquor of CNFs and PVA.
(2) 25g isopropanols are weighed to be added dropwise in mixed solution obtained by step (1), 45 DEG C stir evenly and it is still after, cooling
To room temperature.It takes 7g mixed liquors to pour into the culture dish of Ф 6cm, culture dish is made to remain open state, freezed at -40 DEG C
3h, thaw under room temperature (20 DEG C) 3h, recycles 4 times, obtains nanofiber-based aquagel membrane.
(3) aqueous suspension of 5g10% carbon nanotubes (CNT) is uniformly mixed with 5g 5%PVA solution, obtains CNT/PVA
Mixed solution；
The aqueous suspension of 5g10% polyanilines (PANI) is uniformly mixed with 5g 5%PVA solution, obtains PANI/PVA's
Mixed solution；
(4) PANI/PVA and CNT/PVA mixed solutions obtained by step (3) are respectively coated on Nanowire obtained by step (2)
(single side coated weight is 50~200mg/100mm to the positive and negative both sides of Wiki aquagel membrane2), the sides CNT/PVA are as cathode, PANI/
The sides PVA are as anode.3h is freezed at -40 DEG C, thaw 3h under room temperature (20 DEG C), and nanometer is obtained after such Frozen-thawed cycled 4 times
Fiber base integration film ultracapacitor.Nanofiber-based integration film ultracapacitor is in 0.5M NaSO4In electrolyte
Cyclic voltamogram curve and constant current charge-discharge curve it is as shown in Figures 2 and 3.
Embodiment 3：
A kind of preparation method of nanofiber-based integrated film ultracapacitor of the present invention, includes the following steps：
(1) aqueous solution for weighing 15g 8%PVA is added dropwise to the cellulose nano-fibrous moisture of 15g 0.3% in ultrasound
In dispersion liquid, 55 DEG C stir evenly after obtain the mixed liquor of CNFs and PVA.
(2) 20g isopropanols are weighed to be added dropwise in mixed solution obtained by step (1), 55 DEG C stir evenly and it is still after, cooling
To room temperature.It takes 6g mixed liquors to pour into the culture dish of Ф 6cm, culture dish is made to remain open state, freezed at -40 DEG C
2h, thaw at 20 DEG C 2h, recycles 4 times, obtains nanofiber-based aquagel membrane.
(3) aqueous suspension of 6g10% polypyrroles (PPy) is uniformly mixed with 6g 5%PVA solution, obtains PPy/PVA's
Mixed solution.
(4) PPy/PVA mixed solutions obtained by step (3) are coated in nanofiber-based aquagel membrane two obtained by step (2)
(single side coated weight is 50~200mg/100mm for side2), 2h is freezed at -40 DEG C, thaw 2h at 20 DEG C, such Frozen-thawed cycled 4 times
After obtain nanofiber-based integrated film ultracapacitor.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should be included in except protection scope of the present invention.
Claims (10)
1. a kind of preparation method of nanofiber-based integrated film ultracapacitor, which is characterized in that include the following steps：
(1) nanofiber-based aquagel membrane is prepared using freeze-thaw method；
(2) mixed solution of conductive material and polyvinyl alcohol is prepared；
(3) mixed solution obtained by step (2) is coated uniformly on nanofiber-based aquagel membrane tow sides obtained by step (1)
On, above-mentioned resulting materials are then handled by freeze-thaw method, obtain coating by diaphragm, film two sides of nanofiber-based aquagel membrane
Integrated film ultracapacitor of the conductive material respectively as positive and negative electrode.
2. preparation method according to claim 1, which is characterized in that described to be prepared using freeze-thaw method in the step (1)
The concrete operations of nanofiber-based aquagel membrane are：Polyvinyl alcohol water solution is added dropwise simultaneously into cellulose nano-fibrous aqueous dispersions
It stirs evenly, obtains the mixed liquor of cellulose nano-fibrous/polyvinyl alcohol, take isopropanol that cellulose nano-fibrous/poly- second is added
In the mixed liquor of enol, using freeze-thaw method, nanofiber based aquagel is obtained after mixed liquor freeze-thaw is recycled 4~6 times
Film.
3. preparation method according to claim 2, which is characterized in that the matter of polyvinyl alcohol in the polyvinyl alcohol water solution
It is 1%~10% to measure score；Cellulose nano-fibrous mass fraction is 0.3% in the cellulose nano-fibrous aqueous dispersions
~0.5%；The mass ratio of cellulose nano-fibrous aqueous dispersions and polyvinyl alcohol water solution is 1:(0.2~3).
4. preparation method according to claim 2, which is characterized in that described to be dripped into cellulose nano-fibrous aqueous dispersions
The dispersion process of Polyvinyl alcohol aqueous solution is carried out in the case where power is the ul-trasonic irradiation of 100W~150W, polyvinyl alcohol water
Then above-mentioned mixed liquor is stirred and is heated 0.5~2 hour under the conditions of 40 DEG C~70 DEG C by solution 1~2g/min of drop rate.
5. preparation method according to claim 2, which is characterized in that the additive amount of the isopropanol is cellulose Nanowire
The 10%~200% of dimension/polyvinyl alcohol liquid quality.
6. preparation method according to claim 2, which is characterized in that in the step (1), freeze-thaw process culture
Ware remains open；The design parameter of freeze-thaw process is that cryogenic temperature is -50 DEG C~-30 DEG C, and cooling time is 2~5
Hour, thaw point is 10 DEG C~30 DEG C, and thawing time is 2~5 hours.
7. preparation method according to claim 1, which is characterized in that in the step (2), the preparation conductive material with
The concrete operations of the mixed solution of polyvinyl alcohol are：It is added dropwise and is gathered with the rate of 1~2g/min into the aqueous dispersions of conductive material
Vinyl alcohol aqueous solution simultaneously stirs evenly, and obtains the mixed solution of conductive material/polyvinyl alcohol；The aqueous dispersions of the conductive material
Mass fraction be 1wt%~15wt%；The mass fraction of the polyvinyl alcohol water solution is 1wt%~10wt%；Conduction material
Expect that aqueous dispersions and polyvinyl alcohol water solution mass ratio are (1~3)：1.
8. preparation method according to claim 1, which is characterized in that in the step (2), the conductive material is polyphenyl
One kind in amine, polypyrrole, graphene, carbon nanotube and manganese dioxide.
9. preparation method according to claim 1, which is characterized in that in the step (3), will be mixed obtained by step (2)
It is that single side coats 50~200mg/ that solution, which is coated uniformly on the amount on nanofiber-based aquagel membrane tow sides obtained by step (1),
100mm2；It is described that handle resulting materials by freeze-thaw method refer to carrying out freeze-thaw 4~6 times to resulting materials；Freeze-thaw
The design parameter of process is that cryogenic temperature is -50 DEG C~-30 DEG C, and cooling time is 2~5 hours, and thaw point is 10 DEG C~30
DEG C, thawing time is 2~5 hours.
10. the nanofiber-based integrated film ultracapacitor obtained such as claim 1-9 any one of them preparation methods.
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| CN110993360A (en) * | 2019-11-25 | 2020-04-10 | 广西大学 | Preparation method of integrated electrode composite material and flexible supercapacitor |
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| CN113150314A (en) * | 2021-01-26 | 2021-07-23 | 上海工程技术大学 | Composite gel electrolyte material with interpenetrating network porous structure and preparation and application thereof |
| CN114605674A (en) * | 2022-04-22 | 2022-06-10 | 福州大学 | High-specific-capacitance polyaniline composite flexible conductive hydrogel and preparation method thereof |
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| CN115376839A (en) * | 2022-09-22 | 2022-11-22 | 闽江学院 | Method for preparing supercapacitor by packaging flexible nano cellulose membrane |
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