CN104240973A - Transparent flexible supercapacitor fabric and preparation method thereof - Google Patents
Transparent flexible supercapacitor fabric and preparation method thereof Download PDFInfo
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- CN104240973A CN104240973A CN201410487054.5A CN201410487054A CN104240973A CN 104240973 A CN104240973 A CN 104240973A CN 201410487054 A CN201410487054 A CN 201410487054A CN 104240973 A CN104240973 A CN 104240973A
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Abstract
The invention belongs to the technical field of energy storage devices, and particularly relates to a transparent flexible supercapacitor fabric and a preparation method of the transparent flexible supercapacitor fabric. According to the method, oriented carbon nano tube fiber is woven into a carbon nano tube fiber fabric, a carbon nano tube/polyaniline composite fabric is obtained by depositing polyaniline on the carbon nano tube fiber fabric through an electrochemical deposition method, the surface of the composite fabric is coated with one layer of polyvinyl alcohol/phosphoric acid (PVA/H3PO4) gel electrolyte, and finally the product is assembled with the other electrode with the same structure and material so that the supercapacitor fabric can be obtained. Compared with a traditional planar capacitor, the supercapacitor fabric has the advantages of being light in weight, capable of being woven and the like; compared with other fabric capacitors, the supercapacitor fabric has the advantages of being transparent and the like; compared with a fiber supercapacitor, the supercapacitor fabric is higher in large-scale weaving capacity, and thus the supercapacitor fabric has very good application prospects.
Description
Technical field
The invention belongs to energy storage device technical field, be specifically related to a kind of transparent, flexible ultracapacitor fabric and preparation method thereof.
Background technology
Wearable mobile electronic device becomes more and more important in life of today, and will become live from now on leading gradually.Therefore, we need the corresponding energy storage device of development badly to drive these electronic devices, such as, have the ultracapacitor of high power density.In order to meet wearable demand, these ultracapacitors must have lightweight, flexibility, can weave and the advantage such as high-performance.But mostly some current researchs about ultracapacitor are heavier based on some, harder tabular material, cannot meet above demand.Recently, some research work prepare linear supercapacitor by fiber electrode.Compared with traditional plate-like structure, linear supercapacitor has flexibility, is easy to the advantage of braiding.But current linear supercapacitor is confined to the length of Centimeter Level, and the braiding of these wire devices is got up to have very large challenge, be easy to device destruction in such as braiding process.
In view of above research background and present situation, in recent years, some research work demonstrate good development trend by using textile electrode to prepare ultracapacitor fabric, meet wearable demand.Such as using other material with carbon elements such as various business-like fabric load carbon nano-tube or Graphenes as textile electrode; And for example cotton is expected that fabric direct carbonization obtains the fabric conducted electricity, obtain the ultracapacitor with superior performance with the manganese dioxide of fake capacitance on back loading.Although the preparation of these capacitor fabrics is simple, cost is low, the textile electrode used is more thick and heavy, and electric conductivity is also relatively more general, and electrode is opaque, has certain limitation in actual applications.Therefore, seek a kind ofly to have flexibility concurrently, device that is transparent, that can weave is very significant for wearable demand.
Summary of the invention
The object of the present invention is to provide a kind of transparent, flexible, efficient ultracapacitor fabric and preparation method thereof.
Ultracapacitor fabric provided by the invention, by the textile electrode material of carbon nano-tube (CNTs) fabric as capacitor; Polyvinyl alcohol/phosphoric acid (PVA/H is accompanied between the textile electrode of two same materials
3pO
4) as the electrolyte of Macromolecule glue.
The preparation method of ultracapacitor fabric provided by the invention, its concrete steps are:
(1) pass through dry spinning by carbon nano pipe array, obtain aligned carbon nanotube fiber;
(2) carbon nano-tube fibre of orientation is woven, obtain aligned carbon nanotube fabric electrode;
(3) at described carbon nano-tube fibre fabric top electrode deposition polyaniline, carbon nano-tube/poly aniline compound fabric electrode is obtained, in this, as the electrode of ultracapacitor fabric;
(4) at the space of carbon nano-tube/poly aniline compound fabric electrode and surface coating one deck PVA/H
3pO
4gel-like electrolyte;
(5) by two panels by obtained with electrolytical compound fabric electrode assembling in step (4), obtain ultracapacitor fabric.
In the present invention, described carbon nano pipe array is prepared by chemical vapour deposition technique; Described polyaniline is prepared by electrodeposition process.
In the present invention, the mass content of described polyaniline in carbon nano-tube/poly aniline compound fabric is 15% ~ 60%, preferred 45-60%, more preferably 50%.
Ultracapacitor fabric of the present invention is under the current density of 1 A/g, and specific capacity can reach 272.7 F/g; And this ultracapacitor fabric transparency is good, has good flexibility, angle of bend 150 °, bending 200 lower specific capacities can retain 96.4%.。
The present invention's scanning electron microscopy (SEM) structure to device characterizes.Fig. 2 (a) is depicted as carbon nano-tube fibre fabric, after amplifying further, as shown in Fig. 2 (b), can see carbon nanotube arrangement high-sequential wherein, and have nano level space figure between carbon pipe.3(a), 3(b), 3(c) and 3(d) be respectively carbon nano-tube fibre fabric substrates 15%, 30%, high power image after the polyaniline of 40% and 50%, can find out that polyaniline is deposited on the surface of carbon nano-tube equably, carbon nanotube arrangement still keeps high-sequential.
Ultracapacitor fabric prepared by the present invention has good chemical property.Shown in Fig. 4 is the cyclic voltammetry curve of pure nano-carbon tube fabric and carbon nano-tube/poly aniline compound fabric, and the ultracapacitor fabric introducing polyaniline has obvious redox peak, illustrates that this ultracapacitor fabric has obvious fake capacitance behavior.In order to explore the impact of polyaniline content on combination electrode material specific capacity, the present invention tests the specific capacity of the compound fabric electrode with different polyaniline content, as shown in Figure 5, when polyaniline content is increased to 60% from nothing, because polyaniline has higher fake capacitance, electrode specific capacity has and improves significantly.Be increased to 272.7 F/g from 7.7 F/g of pure nano-carbon tube fabric, polyaniline content is 15%, 30, the specific capacity of the combination electrode of 40,50% and 60% is respectively 108.5,152.8,201.8,272.7 and 240.6F/g.The specific capacity of electrode shown in Fig. 6 increases along with the increase of polyaniline content, and when content is 50% reach maximum, increase polyaniline content further, electrode specific capacity has faint reduction on the contrary.Therefore, the present invention when polyaniline content is 50%, the best performance of ultracapacitor fabric.What Fig. 7 showed is different current density bottom electrode specific capacities, can find out that ultracapacitor fabric has fine capacity hold facility, stable electrochemical property.P-poly-phenyl amine content is that the chemical property of the ultracapacitor fabric of 50% has carried out exploring further subsequently, difference shown in Fig. 8 sweeps the cyclic voltammetry curve under speed, 50 mV/s are increased to from 10 mV/s when sweeping speed, redox peak can both obtain good maintenance, illustrate that this ultracapacitor fabric has good high rate performance, discharge and recharge is carried out as shown in Figure 9 under different current density, charging and discharging curve can keep good symmetry, illustrates that this ultracapacitor has higher coulombic efficiency.The fabric of ultracapacitor shown in Figure 10 is after circulation 2000 times, and electric capacity still can remain on more than 90%, and these property lists understand that ultracapacitor fabric has good electrochemical stability.
Ultracapacitor fabric prepared by the present invention has transparent, the feature such as light weight, flexibility.Be the sign to the ultracapacitor fabric transparency prepared by the present invention as shown in Figure 11 (a) shows, the ultracapacitor fabric through invention can be clear that the article after it.As Figure 11 (b) is depicted as the sign to ultracapacitor fabric light weight prepared by the present invention, the capacitor fabric of invention can hold up and not be damaged by pistil easily.The ultracapacitor fabric be depicted as prepared by the present invention as Figure 11 (c) carries out the optical photograph after bending.Be to the cyclic voltammetry curve of ultracapacitor fabric of the present invention under angle of bend is 30 °, 90 ° and 150 ° as shown in figure 12, can find out that the chemical property of bending rear ultracapacitor fabric is retentively fine, the fabric of ultracapacitor shown in Figure 13 is angle of bend 150 °, bending 200 times, the specific capacity of the electrode of ultracapacitor fabric can maintain before bending 96.4%.
In addition, super electrical equipment fabric of the present invention can carry out connecting or parallel connection comes voltage and the capacity of steering capacitor easily.Be as shown in figure 14 to super electrical equipment series connection of the present invention (3 capacitors series connection) after charging and discharging curve, the operating voltage of ultracapacitor bring up to 2.4V by the 0.8V of single capacitor.Be as shown in figure 15 to super electrical equipment parallel connection of the present invention (3 capacitor parallel connections) after charging and discharging curve, the discharge and recharge time of ultracapacitor correspondingly increases by 2 times.
In sum, the present invention prepares a kind of Novel super capacitor fabric of transparent, flexible, light weight first, the high specific capacity of the ultracapacitor fabric of carbon nano-tube/poly aniline compound reaches 272.7 F/g, still can keep original 96.4% after bending 200 times.Simultaneously, ultracapacitor fabric of the present invention is first by work that transparent, flexible, light weight and stitchability are integrated in one, this is very crucial and important for wearable energy storage device, also for other wearable electrooptical devices of development and electronic device provide the effective way with universality, there is significant application value.
Accompanying drawing explanation
Fig. 1 is ultracapacitor fabric preparation process schematic diagram of the present invention.
Fig. 2 is the stereoscan photograph of pure nano-carbon tube textile electrode.Wherein, (a) pure nano-carbon tube fabric; (b) pure nano-carbon tube fabric enlarged drawing.
Fig. 3 is the high power stereoscan photograph of carbon nano-tube/poly aniline compound fabric.Wherein, (a) polyaniline content is 15%; B () polyaniline content is 30%; C () polyaniline content is 40%; D () polyaniline content is 50%.
Fig. 4 is that the ultracapacitor fabric of pure nano-carbon tube fabric and carbon nano-tube/poly aniline compound fabric is sweeping the cyclic voltammetry curve under fast 20 mV/s.
Fig. 5 is the constant current charge-discharge curve of ultracapacitor fabric under 1A/g current density of the carbon nano-tube/poly aniline compound fabric of different polyaniline content.
The specific capacity of ultracapacitor fabric of Fig. 6 carbon nano-tube/poly aniline compound fabric and the relation of polyaniline content.
Fig. 7 is the specific capacity of ultracapacitor fabric under different charging and discharging currents density of pure nano-carbon tube fabric and carbon nano-tube/poly aniline compound fabric.
Fig. 8 to be polyaniline content be 50% the cyclic voltammetry curve of ultracapacitor fabric under difference sweeps speed.
Fig. 9 to be polyaniline content be 50% the constant current charge-discharge curve of ultracapacitor fabric under different charging and discharging currents density.
Figure 10 to be polyaniline content be 50% ultracapacitor fabric under 1A/g current density, carry out the chemical property of long-acting circulation.
Figure 11 is the optical photograph that ultracapacitor fabric property characterizes.Wherein, the optical photograph of (a) characterizing transparent; B () characterizes the optical photograph of lightweight; C () characterizes flexible optical photograph.
Figure 12 is the cyclic voltammetry curve of ultracapacitor fabric after bending different angles.
Figure 13 be ultracapacitor fabric under 150 ° of angle of bend specific capacity conservation rate with the change of number of bends.
Figure 14 is the constant current charge-discharge curve of ultracapacitor fabric under same current density of single ultracapacitor fabric and 3 series connection.
Figure 15 is single ultracapacitor fabric and 3 the constant current charge-discharge curves of ultracapacitor fabric under same current density in parallel.
Embodiment
Prepare aligned carbon nanotube fiber according to prior art, namely by so-called chemical vapor deposition for carbon nanotubes array, then prepare corresponding fiber by dry spinning.Concrete way is in a quartz tube furnace, to be coated with Fe (1.2 nm)/Al
2o
3the silicon chip of (3 nm) as catalyst, using ethylene gas as carbon source, with Ar and H
2gaseous mixture, as carrier gas, is warming up to 740
oc, carbon nano-tube starts growth, and growth time controls at 10-20 min.After obtaining spinnable carbon nano pipe array, with the edge pull-out carbon nano-tube film of blade from carbon nano pipe array, the carbon nano-tube film of superposition 5-15 layer, then obtains carbon nano-tube fibre, finally by carbon nano-tube fibre woven into fabric with motor with the twisting of the rotational speed of 1000 rpm.
Polyaniline in textile electrode material is prepared by electrodeposition process, is namely reference electrode with Ag/AgCl, Pt sheet is the H of aniline to electrode, 0.1 M and 1 M
2sO
4the aqueous solution is electrolyte, carbon nano-tube fibre fabric is work electrode, can obtain the carbon nano-tube/poly aniline compound fabric electrode with certain content polyaniline under 0.75 V after carrying out potentiostatic electrodeposition certain hour; Wherein, obtain by the time that electro-deposition is different the carbon nano-tube/poly aniline combination electrode that five kinds of polyaniline content are respectively 15%, 30%, 40%, 50% and 60%, for experiment.
PVA and H
3pO
4gel electrolyte is prepared by the following method, first by 1 g PVA 98
ostir 1 h in C oil bath, be then cooled to room temperature, add 1 g concentrated phosphoric acid (mass fraction is 85 wt%).
The preparation of ultracapacitor fabric, first by the space of carbon nano-tube/poly aniline compound fabric electrode and surface coating one deck PVA/H
3pO
4gel-like electrolyte; Then two panels is scribbled the assembling of electrolytical textile electrode, obtain ultracapacitor fabric.
The structure of device is characterized by scanning electron microscopy (Hitachi, FE-SEM S-4800 operated at 1 kV).Constant current charge-discharge Arbin multi-channel electrochemical tester (Arbin, MSTAT-5 V/10 mA/16 Ch) completes.Cyclic voltammetry is completed by electrochemical workstation (CHI 660D).
Ultracapacitor fabric prepared by the present invention, compared to conventional planar shape capacitor, have quality light, the advantage such as can to weave; Compared to other fabric capacitor devices, there is the advantages such as transparent; Compared to fibrous ultracapacitor, there is better extensive braiding ability, thus there is good application prospect.
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Claims (4)
1. a preparation method for transparent, flexible ultracapacitor fabric, is characterized in that concrete steps are as follows:
(1) pass through dry spinning by carbon nano pipe array, obtain aligned carbon nanotube fiber;
(2) carbon nano-tube fibre of orientation is woven, obtain aligned carbon nanotube fabric electrode;
(3) at described carbon nano-tube fibre fabric top electrode deposition polyaniline, carbon nano-tube/poly aniline compound fabric electrode is obtained, in this, as the electrode of ultracapacitor fabric;
(4) in the space of carbon nano-tube/poly aniline compound fabric electrode and surface coating layer of polyethylene alcohol/phosphoric acid gel-like electrolyte;
(5) by two panels by obtained with electrolytical compound fabric electrode assembling in step (4), obtain ultracapacitor fabric.
2. the preparation method of ultracapacitor fabric transparent, flexible as claimed in claim 1, is characterized in that the mass content of described polyaniline in carbon nano-tube/poly aniline compound fabric is 15% ~ 60%.
3. transparent, the flexible ultracapacitor fabric prepared by the preparation method described in claim 1 or 2.
4. ultracapacitor fabric transparent, flexible as claimed in claim 3 can application in Woven electronic device in flexibility.
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| CN105140048A (en) * | 2015-09-11 | 2015-12-09 | 复旦大学 | Method for preparing composite fiber-shaped capacitors continuously |
| CN105780242A (en) * | 2016-05-04 | 2016-07-20 | 东华大学 | Carbon nanotube fabric with multi-scale pore structure and preparation method thereof |
| CN106024420A (en) * | 2016-05-03 | 2016-10-12 | 常州工程职业技术学院 | Preparation method of graphene-containing energy storage polymer electrode sheet |
| CN106449135A (en) * | 2016-07-11 | 2017-02-22 | 同济大学 | Stretchable capacitor based on ordered carbon nanotube composite film and preparation method of stretchable capacitor |
| CN106548875A (en) * | 2016-11-03 | 2017-03-29 | 东华大学 | A kind of transparent ultracapacitor of all-solid-state flexible and its prepare and apply |
| CN106971865A (en) * | 2017-04-28 | 2017-07-21 | 东华大学 | A kind of Polymerization of Polyaniline/carbon Nanotube with high specific capacitance/bafta composite and flexible electrode and its preparation and application |
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| CN109950049A (en) * | 2019-04-09 | 2019-06-28 | 华南师范大学 | The composite material and preparation method and application of carbon nano-tube fibre and nitrogen oxidation tungsten |
| CN110468588A (en) * | 2019-08-21 | 2019-11-19 | 安徽工程大学 | A kind of preparation method of polyaniline coating knitted fabric strain transducer |
| CN112420400A (en) * | 2020-11-11 | 2021-02-26 | 华北电力大学（保定） | Preparation method of super-hydrophobic self-repairing flexible supercapacitor |
| CN114284074A (en) * | 2021-12-29 | 2022-04-05 | 东华大学 | Carbon nanotube/cotton mixed woven fabric material and preparation and application thereof |
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