CN108630462B - Nanofiber-based integrated thin film supercapacitor and preparation method thereof - Google Patents
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- 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
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- 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
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- H—ELECTRICITY
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- 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
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- 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
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- H—ELECTRICITY
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- 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
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- 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
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- 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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a preparation method of a nanofiber-based integrated film supercapacitor, which comprises the following steps: adding a water solution of polyvinyl alcohol (PVA) into a water dispersion of Cellulose Nanofibers (CNFs) and uniformly dispersing to obtain a mixed solution of the PVA and the CNFs; adding isopropanol into the mixed solution of PVA and CNFs, uniformly stirring, and performing freeze thawing on the mixed solution to obtain a high-ionic-conductivity nanofiber-based hydrogel membrane; and uniformly mixing the conductive material and PVA, coating the mixture on two sides of the nanofiber-based hydrogel film, and forming a conductive gel layer by a freeze-thaw method to obtain the nanofiber-based integrated film supercapacitor. The integrated film super capacitor prepared by the method has good biocompatibility, flexibility and excellent electricity storage performance, and can be applied to the field of wearable energy storage devices.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a nanofiber-based integrated thin film supercapacitor and a preparation method thereof.
Background
The hydrogel is a three-dimensional network flexible material with water retention property, and can adsorb electrolyte to be applied to the field of energy storage as solid electrolyte. The Cellulose Nanofibers (CNFs) are used as a natural biomass material with high length-diameter ratio and large surface activity, have good biocompatibility, and can form physical actions such as winding, hydrogen bonds and the like with polymer molecular chains, so that the mechanical and flexible properties of the composite material are improved.
The super capacitor is a novel energy storage device between a traditional capacitor and a battery, and has the advantages of high power density, short charging and discharging time and the like. With the rapid development of light-weight, flexible, and even wearable electronic devices, energy storage devices that provide energy to them also have developed in a flexible and efficient direction. The nanofiber-based hydrogel film is used as a capacitor diaphragm, the conductive hydrogel layer is used as an electrode, the integrated flexible supercapacitor is prepared, the maximum contact area of an electrode material and an electrolyte can be realized, the interface effect is reduced, the ion transmission efficiency is improved, the excellent energy storage performance, the good mechanical property and the good flexibility are realized, and the integrated flexible supercapacitor can be applied to the fields of wearable and portable energy storage devices.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and provides a nanofiber-based integrated thin film supercapacitor and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a nanofiber-based integrated thin film supercapacitor comprises the following steps:
(1) preparing a nanofiber-based hydrogel film by using a freeze-thaw method;
(2) preparing a mixed solution of a conductive material and polyvinyl alcohol;
(3) and (3) uniformly coating the mixed solution obtained in the step (2) on the front surface and the back surface of the nanofiber-based hydrogel film obtained in the step (1), and then treating the obtained material by a freeze-thaw method to obtain the integrated thin-film supercapacitor taking the nanofiber-based hydrogel film as a diaphragm and the conductive materials coated on the two surfaces of the film as positive and negative electrodes respectively.
The polyvinyl alcohol in the step (2) mainly has the function of bonding, and the conductive material is fixed on the surface of the film, so that the formed electrode is not easy to fall off, and the electrode/diaphragm/electrode integrated energy storage device is formed. In addition, the polyvinyl alcohol material consistent with the membrane main body is selected, so that the interface effect of the electrode material and the diaphragm is reduced.
In the preparation method, preferably, in the step (1), the specific operation of preparing the nanofiber-based hydrogel film by using a freeze-thaw method is as follows: and dropwise adding a polyvinyl alcohol aqueous solution into the cellulose nanofiber aqueous dispersion, uniformly stirring to obtain a cellulose nanofiber/polyvinyl alcohol mixed solution, adding isopropanol into the cellulose nanofiber/polyvinyl alcohol mixed solution, and performing freeze-thaw cycle on the mixed solution for 4-6 times by using a freeze-thaw method to obtain the nanofiber-based hydrogel membrane.
The polyvinyl alcohol functions in step (1) to form the host structure of the hydrogel film.
In the above preparation method, preferably, the mass fraction of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 1% to 10%; the mass fraction of the cellulose nanofibers in the cellulose nanofiber aqueous dispersion is 0.3-0.5%; the mass ratio of the cellulose nanofiber water dispersion to the polyvinyl alcohol aqueous solution is 1 (0.2-3). The mass fraction of the polyvinyl alcohol is lower than 1 percent, the solution is too dilute, and the film formed under the condition of the same volume is too thin; when the mass fraction of the polyvinyl alcohol is higher than 10%, the solution viscosity is too high, and the nano fibers are not easy to disperse. The mass fraction of the cellulose nano-fibers is too high, and the nano-fibers are not easy to disperse uniformly; the cellulose nano-fiber has low mass fraction and is not easy to form a film, and the cellulose nano-fiber has good film forming effect within the mass fraction range. The proportion of the polyvinyl alcohol is too large, the obtained gel film is hard, and the flexibility is reduced; the cellulose nano-fiber has an excessively large proportion, and the obtained gel film has low strength and is easy to crack.
In the preparation method, preferably, the dispersion process of dripping the polyvinyl alcohol aqueous solution into the cellulose nano-fiber aqueous dispersion is carried out under the action of ultrasonic waves with the power of 100W-150W, the dripping acceleration rate of the polyvinyl alcohol aqueous solution is 1-2 g/min, and then the mixed solution is stirred and heated for 0.5-2 hours at the temperature of 40-70 ℃. Since the viscosity of the polyvinyl alcohol aqueous solution is higher than that of the cellulose nanofiber aqueous dispersion, the polyvinyl alcohol aqueous solution is added dropwise to the cellulose nanofiber aqueous dispersion. Under the condition of 40-70 ℃, the cellulose nano-fiber and the polyvinyl alcohol can be well and uniformly dispersed, and the high-temperature degradation of the cellulose nano-fiber can not be caused.
In the above production method, the amount of the isopropyl alcohol is preferably 10 to 200% by mass of the cellulose nanofiber/polyvinyl alcohol mixed solution. The function of the isopropanol is defoaming. The addition amount of the isopropanol is too high, so that a gel film is not easy to form; if the amount is too low, the defoaming effect is hardly exhibited.
In the above preparation method, preferably, in the step (1), the culture dish is kept open all the time during the freezing-thawing process; the specific parameters of the freezing-unfreezing process are that the freezing temperature is-50 ℃ to-30 ℃, the freezing time is 2-5 hours, the unfreezing temperature is 10 ℃ to 30 ℃, and the unfreezing time is 2-5 hours.
In the preparation method, preferably, in the step (2), the specific operation of preparing the mixed solution of the conductive material and the polyvinyl alcohol is as follows: dripping a polyvinyl alcohol aqueous solution into the aqueous dispersion of the conductive material at a speed of 1-2 g/min, and uniformly stirring to obtain a conductive material/polyvinyl alcohol mixed solution; the mass fraction of the aqueous dispersion of the conductive material is 1 wt% -15 wt%; the mass fraction of the polyvinyl alcohol aqueous solution is 1 wt% -10 wt%; the mass ratio of the conductive material aqueous dispersion to the polyvinyl alcohol aqueous solution is (1-3): 1. when the mass fraction of the conductive material aqueous dispersion is too high, uniform dispersion is difficult; if the mass fraction is too low, the concentration is low, and the density of the electrode material is low. When the mass fraction of the polyvinyl alcohol aqueous solution is lower than 1%, the solution is too dilute, and the film formed under the condition of the same volume is too thin; if the mass fraction is more than 10%, the solution viscosity is too high and the dispersion of the nanofibers is not easy.
In the preparation method, preferably, in the step (2), the conductive material is Polyaniline (PANI), polypyrrole (PPy), Graphene (GR), Carbon Nanotube (CNT), and manganese dioxide (MnO)2) One kind of (1). The conductive materials have good conductivity and can be dispersed in polyvinyl alcohol solution as electrode materialThe material is coated onto a gel separator.
In the preparation method, preferably, in the step (3), the amount of the mixed solution obtained in the step (2) uniformly coated on the front and back surfaces of the nanofiber-based hydrogel film obtained in the step (1) is 50-200 mg/100mm of single-side coating2(ii) a The step of treating the obtained material by a freeze thawing method is to freeze-thaw the obtained material for 4-6 times; the specific parameters of the freezing-unfreezing process are that the freezing temperature is-50 ℃ to-30 ℃, the freezing time is 2-5 hours, the unfreezing temperature is 10 ℃ to 30 ℃, and the unfreezing time is 2-5 hours.
As a general inventive concept, the invention also provides a nanofiber-based integrated thin film supercapacitor obtained by the preparation method.
Compared with the prior art, the invention has the advantages that:
(1) the nanofiber-based hydrogel film adopted by the invention is non-toxic and degradable, has good biocompatibility, high flexibility and excellent ionic conductivity. The realization of high ionic conductivity is benefited by abundant sulfonic acid groups on the surface of the nano-cellulose, which can ionize carriers for ion transmission, namely hydrogen ions.
(2) Compared with the existing super capacitor, the integrated thin film super capacitor prepared by the invention reduces the interface effect between the electrode material and the diaphragm, has high flexibility, is convenient to carry and store, and has simple and convenient preparation method and lower cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is an ion conductivity of the nanofiber-based hydrogel film prepared in example 1 of the present invention. (the ionic conductivity of the nanofiber-based hydrogel membrane in the figure is 3.55X 10-2S-1M, ion conductivity of pure polyvinyl alcohol hydrogel film 1.20X 10-2S-1·m)。
Fig. 2 is a photograph of the nanofiber-based integrated thin film supercapacitor prepared in example 2 of the present invention and a cyclic voltammetry characteristic curve of the thin film supercapacitor.
Fig. 3 is a constant current charge and discharge curve of the nanofiber-based integrated thin film supercapacitor prepared in example 2 of the present invention.
Detailed Description
In order to facilitate understanding of the invention, the invention will be described more fully and in detail with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a preparation method of a nanofiber-based integrated film supercapacitor, which comprises the following steps:
(1) 10g of 5% polyvinyl alcohol (PVA) aqueous solution is weighed, added into 20g of 0.5% cellulose nanofiber aqueous dispersion in a dropwise manner in ultrasonic, and stirred uniformly at 50 ℃ to obtain a mixed solution of CNFs and PVA.
(2) And (2) dropwise adding 30g of isopropanol into the mixed solution of the CNFs and the PVA obtained in the step (1), uniformly stirring at 50 ℃ without bubbles, and cooling to room temperature. Pouring 10g of the mixed solution into a culture dish with the diameter of 6cm, keeping the culture dish in an open state all the time, freezing for 2h at the temperature of minus 40 ℃, unfreezing for 2h at the temperature of 20 ℃, and circulating for 5 times to obtain the nanofiber-based hydrogel membrane. The ionic conductivity of the nanofiber-based hydrogel membrane is shown in fig. 1.
(3) 10g of 10% Polyaniline (PANI) aqueous suspension and 7.5g of 5% PVA solution were mixed uniformly to obtain a PANI/PVA mixed solution.
(4) Coating the PANI/PVA mixed solution obtained in the step (3) on two sides (the single-side coating amount is 50-200 mg/100 mm) of the nanofiber-based hydrogel film obtained in the step (2)2) Freezing for 2h at-40 ℃, unfreezing for 2h at 20 ℃, and performing freeze-thaw cycling for 5 times to obtain the nanofiber-based integrated film supercapacitor.
Example 2:
the invention relates to a preparation method of a nanofiber-based integrated film supercapacitor, which comprises the following steps:
(1) 5g of 10% PVA aqueous solution is weighed, added dropwise into 25g of 0.5% cellulose nanofiber aqueous dispersion in ultrasonic, and stirred uniformly at 45 ℃ to obtain a mixed solution of CNFs and PVA.
(2) And (2) dropwise adding 25g of isopropanol into the mixed solution obtained in the step (1), uniformly stirring at 45 ℃ without bubbles, and cooling to room temperature. And pouring 7g of the mixed solution into a culture dish with the diameter of 6cm, keeping the culture dish in an open state all the time, freezing for 3 hours at the temperature of minus 40 ℃, unfreezing for 3 hours at the room temperature (20 ℃), and circulating for 4 times to obtain the nanofiber-based hydrogel membrane.
(3) Uniformly mixing 5g of 10% aqueous suspension of Carbon Nanotubes (CNT) with 5g of 5% PVA solution to obtain a CNT/PVA mixed solution;
uniformly mixing 5g of 10% Polyaniline (PANI) aqueous suspension and 5g of 5% PVA solution to obtain a PANI/PVA mixed solution;
(4) respectively coating the PANI/PVA and CNT/PVA mixed solution obtained in the step (3) on the front side and the back side of the nanofiber-based hydrogel membrane obtained in the step (2) (the single-side coating amount is 50-200 mg/100 mm)2) The CNT/PVA side served as the negative electrode and the PANI/PVA side as the positive electrode. Freezing for 3h at-40 ℃, unfreezing for 3h at room temperature (20 ℃), and performing freeze-thaw cycling for 4 times to obtain the nanofiber-based integrated thin film supercapacitor. The nanometer fiber-based integrated film super capacitor is 0.5M Na2SO4Cyclic voltammetry characteristics and galvanostatic charge-discharge curves in the electrolyte are shown in fig. 2 and 3.
Example 3:
the invention relates to a preparation method of a nanofiber-based integrated film supercapacitor, which comprises the following steps:
(1) weighing 15g of 8% PVA aqueous solution, dropwise adding the aqueous solution into 15g of 0.3% cellulose nanofiber aqueous dispersion in ultrasonic, and uniformly stirring at 55 ℃ to obtain a mixed solution of CNFs and PVA.
(2) 20g of isopropanol is weighed and added into the mixed solution obtained in the step (1) dropwise, and after the mixture is stirred uniformly at 55 ℃ and is free of bubbles, the temperature is reduced to room temperature. Pouring 6g of the mixed solution into a culture dish with the diameter of 6cm, keeping the culture dish in an open state all the time, freezing for 2h at the temperature of minus 40 ℃, unfreezing for 2h at the temperature of 20 ℃, and circulating for 4 times to obtain the nanofiber-based hydrogel membrane.
(3) 6g of an aqueous suspension of 10% polypyrrole (PPy) was mixed uniformly with 6g of a 5% PVA solution to obtain a PPy/PVA mixed solution.
(4) Coating the PPy/PVA mixed solution obtained in the step (3) on two sides (the single-side coating amount is 50-200 mg/100 mm) of the nanofiber-based hydrogel film obtained in the step (2)2) Freezing for 2h at-40 ℃, unfreezing for 2h at 20 ℃, and performing freeze-thaw cycling for 4 times to obtain the nanofiber-based integrated film supercapacitor.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included outside the protection scope of the present invention.
Claims (8)
1. A preparation method of a nanofiber-based integrated thin film supercapacitor is characterized by comprising the following steps:
(1) preparing a nanofiber-based hydrogel film by using a freeze-thaw method;
(2) preparing a mixed solution of a conductive material and polyvinyl alcohol;
(3) uniformly coating the mixed solution obtained in the step (2) on the front and back surfaces of the nanofiber-based hydrogel film obtained in the step (1), and then treating the obtained material by a freeze-thaw method to obtain an integrated thin-film supercapacitor taking the nanofiber-based hydrogel film as a diaphragm and conducting materials coated on the two surfaces of the film as positive and negative electrodes respectively;
in the step (1), the specific operation of preparing the nanofiber-based hydrogel film by using a freeze-thaw method is as follows: dropwise adding a polyvinyl alcohol aqueous solution into the cellulose nanofiber aqueous dispersion, uniformly stirring to obtain a cellulose nanofiber/polyvinyl alcohol mixed solution, adding isopropanol into the cellulose nanofiber/polyvinyl alcohol mixed solution, and performing freeze-thaw cycle on the mixed solution for 4-6 times by using a freeze-thaw method to obtain a nanofiber-based hydrogel membrane; the mass fraction of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 1-10%; the mass fraction of the cellulose nanofibers in the cellulose nanofiber aqueous dispersion is 0.3-0.5%; the mass ratio of the cellulose nanofiber water dispersion to the polyvinyl alcohol aqueous solution is 1 (0.2-3).
2. The method according to claim 1, wherein the dispersion of the aqueous dispersion of cellulose nanofibers by dropwise addition of the aqueous solution of polyvinyl alcohol is carried out by ultrasonic waves of 100 to 150W power at an acceleration rate of 1 to 2g/min, and the mixture is stirred and heated at 40 to 70 ℃ for 0.5 to 2 hours.
3. The method according to claim 1, wherein the amount of the isopropyl alcohol added is 10 to 200% by mass of the mixed solution of cellulose nanofibers and polyvinyl alcohol.
4. The method according to claim 1, wherein in the step (1), the freeze-thaw process culture dish is always kept open; the specific parameters of the freezing-unfreezing process are that the freezing temperature is-50 ℃ to-30 ℃, the freezing time is 2-5 hours, the unfreezing temperature is 10 ℃ to 30 ℃, and the unfreezing time is 2-5 hours.
5. The preparation method according to claim 1, wherein in the step (2), the specific operation of preparing the mixed solution of the conductive material and the polyvinyl alcohol is: dripping a polyvinyl alcohol aqueous solution into the aqueous dispersion of the conductive material at a speed of 1-2 g/min, and uniformly stirring to obtain a conductive material/polyvinyl alcohol mixed solution; the mass fraction of the aqueous dispersion of the conductive material is 1 wt% -15 wt%; the mass fraction of the polyvinyl alcohol aqueous solution is 1 wt% -10 wt%; the mass ratio of the aqueous dispersion of the conductive material to the aqueous solution of polyvinyl alcohol is (1-3): 1.
6. the method according to claim 1, wherein in the step (2), the conductive material is one of polyaniline, polypyrrole, graphene, carbon nanotube, and manganese dioxide.
7. The preparation method according to claim 1, wherein in the step (3), the mixed solution obtained in the step (2) is uniformly coated on the front and back surfaces of the nanofiber-based hydrogel membrane obtained in the step (1) in an amount of 50-200 mg/100mm coated on one surface2(ii) a The step of treating the obtained material by a freeze thawing method is to freeze-thaw the obtained material for 4-6 times; the specific parameters of the freezing-unfreezing process are that the freezing temperature is-50 ℃ to-30 ℃, the freezing time is 2-5 hours, the unfreezing temperature is 10 ℃ to 30 ℃, and the unfreezing time is 2-5 hours.
8. The nanofiber-based integrated thin film supercapacitor obtained by the preparation method according to any one of claims 1 to 7.
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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 |
| CN111504519B (en) * | 2020-04-20 | 2022-03-01 | 河北工业大学 | Flexible cable type touch sensor |
| CN111505065B (en) * | 2020-04-20 | 2023-04-18 | 河北工业大学 | Interdigital counter electrode type flexible touch sensor based on super-capacitor sensing principle and preparation method thereof |
| CN111504520B (en) * | 2020-04-20 | 2022-05-24 | 河北工业大学 | Integrated flexible stretchable touch sensor based on super-capacitor sensing principle |
| CN111499999B (en) * | 2020-06-02 | 2022-06-21 | 河北工业大学 | Polyvinyl alcohol sponge with high tensile rate and preparation method thereof |
| CN113150314B (en) * | 2021-01-26 | 2023-08-11 | 上海工程技术大学 | Composite gel electrolyte material with interpenetrating network porous structure, preparation and application thereof |
| CN114605674B (en) * | 2022-04-22 | 2023-06-16 | 福州大学 | Polyaniline composite flexible conductive hydrogel with high specific capacitance and preparation method thereof |
| CN115360024A (en) * | 2022-08-10 | 2022-11-18 | 五邑大学 | Super capacitor and preparation method and application thereof |
| CN115376839B (en) * | 2022-09-22 | 2024-01-12 | 闽江学院 | Method for preparing super capacitor by packaging flexible nanocellulose film |
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