CN105428082B - Stretchable ultracapacitor based on nitrogen-doped carbon nanometer pipe array/polyurethane combination electrode and preparation method thereof - Google Patents
Stretchable ultracapacitor based on nitrogen-doped carbon nanometer pipe array/polyurethane combination electrode and preparation method thereof Download PDFInfo
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- CN105428082B CN105428082B CN201510987928.8A CN201510987928A CN105428082B CN 105428082 B CN105428082 B CN 105428082B CN 201510987928 A CN201510987928 A CN 201510987928A CN 105428082 B CN105428082 B CN 105428082B
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Abstract
The invention belongs to ultracapacitor field, specially a kind of stretchable ultracapacitor based on N doping aligned carbon nanotube array/polyurethane combination electrode and preparation method thereof.The method comprises the steps of firstly, preparing a kind of N doping aligned carbon nanotube array, and by drop-coating in its strata urethane of surface recombination one, peel off from substrate to obtain N doping aligned carbon nanotube array/polyurethane combination electrode after natural drying, layer of gel electrolyte is coated in the N doping aligned carbon nanotube array side of combination electrode, finally assembles to obtain stretchable ultracapacitor by two pieces of combination electrodes for scribbling gel electrolyte.Ultracapacitor prepared by the present invention can maintain 98.9% capacity in the case of stretching 400%, and still to maintain 96% capacity after 200% amount of tension repeated stretching 1000 times.Stretchable ultracapacitor prepared by the present invention has broad application prospects in fields such as flexible electronic devices.
Description
Technical field
The invention belongs to supercapacitor technologies field, and in particular to one kind is based on nitrogen-doped carbon nanometer pipe array/poly- ammonia
Stretchable ultracapacitor of ester combination electrode and preparation method thereof.
Background technology
Flexible, stretchable electronic equipment turn into modern electronics an important development direction, they electronic skin,
Intelligent clothing, flexible display etc. have broad application prospects [1-3].Ultracapacitor is due to its high specific capacitance, height
The features such as power density and high service life cycle, it is the preferable energy storage system of numerous electronic equipments [4-6].So
And the electrode material that conventional Super capacitor uses is usually that rigidity is non-stretchable, and electrolyte is usually liquid, therefore this
A little ultracapacitors are difficult to meet future electronic Flexible Equipment, stretchable demand.
To realize the flexible extensible of ultracapacitor, there is researcher to use elastomeric polymer film to be received for substrate with carbon
Mitron or conducting polymer etc. are active material, and are prepared for ultracapacitor [7] with reference to solid electrolyte.This kind of super capacitor
Utensil has bending flexibility, and certain tensility energy very well.Can not resist excessive stretching yet with electrode material should
Become, therefore limit the tensile property of ultracapacitor, still can not meet actual demand.In recent years, researcher passes through again
The preparation method of pre-stretching, first elastomeric polymer substrate is pre-stretched, then active material such as CNT even load is arrived
In elastic substrates in pretensioned state, unloading pulling force rear electrode material is shunk with polymeric substrates and forms pleated structure,
So that the tensile property of electrode material further improves.2013, single wall carbon nano-tube film was supported on prestretching by Niu etc.
Stretch on the PDMS membrane under state, after removing the tensile stress on PDMS membrane, obtain the list of fold
Wall carbon nano-tube film electrode.Using polyvinyl alcohol sulfuric acid as gel electrolyte, sandwich structure is assembled into by two polar stacks,
Stretchable ultracapacitor is prepared.The ultracapacitor can reach 120% amount of tension [8].Patent " application number：
201510165881.7 " load to spongy graphene/nickel particle compound in the elastic substrates of pre-stretching, after recovering deformation
Stretchable elastomer/electrode composite material is made, and according to the knot of elastomer/electrode/solid electrolyte/electrode/elastomer
Structure is prepared for stretchable ultracapacitor [9].
The above method achieves certain effect in terms of stretchable ultracapacitor is prepared.However, due to this prestretching
The mode stretched needs to apply prestressing force, is not suitable for actual large-scale production.Simultaneously as the limitation of electrode material in itself, difficult
Further to improve the amount of tension of ultracapacitor so that its use under the conditions of extreme stretcher strain is restricted.Cause
This, prepares a kind of more preferable ultracapacitor of tensile property by a kind of simple method and becomes area research person and constantly chase after
The target asked.
The content of the invention
It is an object of the invention to provide one kind to have big amount of tension（Reach 400%）Stretchable ultracapacitor system
Preparation Method.
Stretchable ultracapacitor provided by the present invention, it is compound with N doping aligned carbon nanotube array/polyurethane
Symmetrical ultracapacitor of the film as electrode material.
Stretchable ultracapacitor provided by the present invention, its preparation method comprise the following steps that：
（1）Aligned carbon nanotube array is prepared by chemical vapour deposition technique；
（2）By chemical vapour deposition technique on aligned carbon nanotube array further growth nitrogen-doped graphene layer, system
Standby N doping aligned carbon nanotube array；
（3）By polyurethane solutions drop coating on N doping aligned carbon nanotube array, peeled off after natural drying from substrate,
Obtain N doping aligned carbon nanotube array/polyurethane combination electrode；
（4）Layer of gel electrolyte is coated in the N doping aligned carbon nanotube array side of combination electrode, and by two pieces
The combination electrode assembling of gel electrolyte is scribbled, obtains stretchable ultracapacitor.
The concrete operations of each step are as follows：
（1）Chemical vapour deposition technique prepares aligned carbon nanotube array.
It is Al that a Rotating fields are deposited on silicon chip by electron beam evaporation deposition instrument2O3/ Fe catalyst, wherein Al2O3's
Thickness is that 2-20 nm, Fe thickness are 0.5-1.5 nm.By chemical vapour deposition technique, carrier gas, ethene conduct are used as by the use of argon gas
Carbon source, hydrogen synthesize height-oriented carbon nano pipe array as reducing agent on the silicon chip of catalyst is coated with advance.Wherein argon
Gas gas flow is 350-450 sccm, and ethylene gas flow is 60-120 sccm, and hydrogen gas flow is 30-90
sccm.Reaction temperature is 700-800 DEG C, and the reaction time is 10-15 min.
（2）Prepare N doping aligned carbon nanotube array.
By chemical vapour deposition technique, by the use of argon gas as carrier gas, acetonitrile as carbon and nitrogen source, hydrogen as reducing agent,
Further growth nitrogen-doped graphene layer on the aligned carbon nanotube array of above-mentioned preparation, obtains N doping aligned carbon nanotube battle array
Row；Wherein argon gas flow is 90-130 sccm, and acetonitrile gas flow is 30-50 sccm, and hydrogen gas flow is 5-
20 sccm.Reaction temperature is 1000-1100 DEG C, and the reaction time is 5-60 min.
（3）Prepare N doping aligned carbon nanotube array/polyurethane combination electrode.
Polyurethane is cut into slices and is dissolved in mass fraction 5%-20% in DMF, strong stirring, obtains poly- ammonia
Ester solution.By resulting polyurethane solutions drop coating in step（2）The N doping aligned carbon nanotube array surface of preparation, vacuum
It is evacuated 5-10 min.It is peeled off from substrate after natural drying, obtains N doping aligned carbon nanotube/polyurethane compound electric
Pole.
（4）Assemble stretchable ultracapacitor.
On the surface of the N doping aligned carbon nanotube side of N doping aligned carbon nanotube array/polyurethane combination electrode
Layer of polyethylene alcohol phosphoric acid gel electrolyte is coated, and two pieces of combination electrodes for scribbling gel electrolyte are assembled to obtain stretchable
Ultracapacitor.
Preparation process schematic diagram such as Fig. 1 and Fig. 2 institutes of the N doping aligned carbon nanotube array/polyurethane composite membrane
Show.
The assembly structure diagram of the stretchable ultracapacitor is as shown in Figure 3.
Compared with prior art, the technological means such as the novelty of its technology is to be pre-stretched can be direct by the present invention
Prepare the stretchable super capacitor based on N doping aligned carbon nanotube array/polyurethane combination electrode with big amount of tension
Device.CNT in N doping aligned carbon nanotube array has very strong Van der Waals force between each other so that it is being stretched
During can closely link together, the ultracapacitor of preparation can bear very big tensile deformation.Stretching
98.9% capacity is maintained in the case of 400%, and still to maintain 96% capacity after 200% amount of tension repeated stretching 1000 times.
Stretchable ultracapacitor prepared by the present invention is in fields such as flexible electronic devices, in terms of being particularly applied to extreme tensile deformation
Have broad prospects.
Brief description of the drawings
Fig. 1 is aligned carbon nanotube preparation process schematic diagram.
Fig. 2 is the preparation process schematic diagram of N doping aligned carbon nanotube/polyurethane composite membrane.
Fig. 3 is the assembly structure diagram of stretchable ultracapacitor.
Fig. 4 is the surface sweeping electron microscope of aligned carbon nanotube array in embodiment.
Fig. 5 is the transmission electron microscope figure of N doping aligned carbon nanotube in embodiment.
Fig. 6 is the optical photograph of N doping aligned carbon nanotube array/polyurethane composite membrane in embodiment.
Fig. 7 is constant current charge-discharge curve of the stretchable ultracapacitor under different current densities in embodiment.
Fig. 8 is the lasting charge-discharge test of stretchable ultracapacitor in embodiment.
Fig. 9 is capacitance variations curve of the stretchable ultracapacitor under the conditions of different stretch in embodiment.
Figure 10 is stretchable ultracapacitor in embodiment with capacitance variations curve during 200% amount of tension repeated stretching.
Embodiment
Below in conjunction with specific implementation case, exemplary explanation and help further understand the present invention, but case study on implementation has
Body details does not represent technical scheme whole under present inventive concept, therefore should not be construed as pair merely to the explanation present invention
The restriction of the total technical scheme of the present invention, some in technical staff, unsubstantiality increase without departing from present inventive concept and
Change, such as simply change or replace with the technical characteristic with same or similar technique effect, belong to present invention protection model
Enclose.
（1）Prepare aligned carbon nanotube array.
It is Al that a Rotating fields are deposited on silicon chip by electron beam evaporation deposition instrument2O3/ Fe catalyst, wherein Al2O3's
Thickness is 3 nm, and Fe thickness is 1.2 nm.By chemical vapour deposition technique, by the use of argon gas as carrier gas, ethene is as carbon source, hydrogen
Gas synthesizes height-oriented carbon nano pipe array as reducing agent on the silicon chip of catalyst is coated with advance.Wherein argon gas
Flow is 400 sccm, and ethylene gas flow is 90 sccm, and hydrogen gas flow is 60 sccm.Reaction temperature is 740 DEG C,
Reaction time is 10 min.Its scanning electron microscope (SEM) photograph is as shown in figure 4, as can be observed from Figure, CNT is height-oriented and tight
Close grows together.
（2）Prepare N doping aligned carbon nanotube array.
By chemical vapour deposition technique, by the use of argon gas as carrier gas, acetonitrile as carbon and nitrogen source, hydrogen as reducing agent,
Further growth nitrogen-doped graphene layer on the aligned carbon nanotube array of above-mentioned preparation, obtains N doping aligned carbon nanotube battle array
Row.Wherein argon gas flow is 110 sccm, and acetonitrile gas flow is 40 sccm, and hydrogen gas flow is 10 sccm.
Reaction temperature is 1060 DEG C, and the reaction time is 20 min.Wherein, the transmission electron microscope figure of N doping aligned carbon nanotube is such as
Shown in Fig. 5, it can be seen that the tube wall diameter of the N doping aligned carbon nanotube can be increased to from several nanometers tens to
Hundreds of nanometers.
（3）Prepare N doping aligned carbon nanotube array/polyurethane composite membrane.
Polyurethane is cut into slices and is dissolved in mass fraction 20% in DMF, the h of strong stirring 24, obtains poly- ammonia
Ester solution.By resulting polyurethane solutions drop coating in step（1）The N doping aligned carbon nanotube array surface of preparation, vacuum
It is evacuated 5 min.It is peeled off from substrate after natural drying and obtains N doping aligned carbon nanotube/polyurethane composite membrane.Its light
It is as shown in Figure 6 to learn photo.
（4）Assemble stretchable ultracapacitor.
Applied on the surface of the N doping aligned carbon nanotube side of N doping aligned carbon nanotube array/polyurethane composite membrane
Layer of gel electrolyte is covered, and two pieces of composite membranes for scribbling gel electrolyte are assembled to obtain stretchable ultracapacitor.Wherein,
Gel electrolyte is the aqueous solution of polyvinyl alcohol phosphoric acid, and the mass ratio of polyvinyl alcohol and phosphoric acid is 1:1.5.
Experiment test shows, the stretchable ultracapacitor of above-mentioned preparation is 0.05,0.1 in constant current charge-discharge electric current,
0.2,0.4,0.8 mAcm-2Under conditions of, its area specific capacitance is respectively 37.6,31.1,23.6,18.6,14.2 mFcm-2
（Fig. 7）.And it has good stability, after continuous discharge and recharge 10000 times, 91.6% capacitance is still maintained（Fig. 8）.I
Further test its tensile property, as shown in Figures 9 and 10.The ultracapacitor of above-mentioned preparation can be in the feelings of stretching 400%
98.9% capacity is maintained under condition（Fig. 9）, and still to maintain 96% capacity after 200% amount of tension repeated stretching 1000 times（Figure 10）.
Bibliography
[1]Kim R., Kim D., Xiao J. L., et al. Nature Mater., 2010, 9: 929-937.
[2]Liang J. J., Li L., Niu X. F., et al. Nature Photon., 2013, 7:
817-824.
[3]Lipomi D. J., Tee B. C. K., Vosgueritchian M., et al. Adv. Mater.,
2011, 23: 1771-1775.
[4]Zhang N., Zhou W. Y., Zhang Q., et al. Nanoscale, 2015, 7: 12492-12497.
[5]Chen X. L., Lin H. J., Chen P. N., et al. Adv. Mater., 2014, 26,
4444-4449.
[6]Chen T., Xue Y. H., Roy A. K., et al. ACS Nano, 2014, 8: 1039-1046.
[7]Chen T., Peng H. S., Durstock M., et al. Sci. Rep., 2014, 4: 3612-3619.
[8]Niu Z. Q., Dong H. B., Zhu B. W., Adv. Mater., 2013, 25, 1058-1064.
[9] Yang Cheng, Bi Yiqing, Lu Jing, Chinese patents, 201510165881.7,2015-09-02. are waited.
Claims (5)
1. a kind of preparation method of stretchable ultracapacitor, it is characterised in that the capacitor is to be orientated carbon nanometer with N doping
Symmetrical ultracapacitor of the pipe array/polyurethane composite membrane as electrode material, is comprised the following steps that：
（1）Aligned carbon nanotube array is prepared by chemical vapour deposition technique；
（2）By chemical vapour deposition technique on aligned carbon nanotube array further growth nitrogen-doped graphene layer, obtain nitrogen
Adulterate aligned carbon nanotube array；
（3）Peel off and obtain from substrate by polyurethane solutions drop coating on N doping aligned carbon nanotube array, after natural drying
N doping aligned carbon nanotube array/polyurethane combination electrode；
（4）Layer of gel electrolyte is coated in the N doping aligned carbon nanotube array side of combination electrode, and two pieces are scribbled
The combination electrode of gel electrolyte assembles to obtain stretchable ultracapacitor.
2. the preparation method of stretchable ultracapacitor as claimed in claim 1, it is characterised in that step（1）In, chemical gas
For phase sedimentation using argon gas as carrier gas, ethene is 350-450 as reducing agent, wherein argon gas flow as carbon source, hydrogen
Sccm, ethylene gas flow are 60-120 sccm, and hydrogen gas flow is 30-90 sccm；Reaction temperature is 700-800
DEG C, the reaction time is 10-15 min.
3. the preparation method of stretchable ultracapacitor as claimed in claim 1, it is characterised in that step（2）In, chemical gas
For phase sedimentation using argon gas as carrier gas, acetonitrile is 90- as reducing agent, wherein argon gas flow as carbon and nitrogen source, hydrogen
130 sccm, acetonitrile gas flow are 30-50 sccm, and hydrogen gas flow is 5-20 sccm；Reaction temperature is 1000-
1100 DEG C, the reaction time is 5-60 min.
4. the preparation method of stretchable ultracapacitor as claimed in claim 1, it is characterised in that step（3）In, it is described poly-
The mass fraction of urethane solution is 5%-20%, and solvent is DMF.
5. the preparation method of stretchable ultracapacitor as claimed in claim 1, it is characterised in that step（4）In, it is described solidifying
Glue electrolyte is polyvinyl alcohol phosphoric acid electrolyte.
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| 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 |
| CN106803462A (en) * | 2016-11-30 | 2017-06-06 | 同济大学 | A kind of flexible extensible ultracapacitor and its preparation based on graphene composite film |
| CN107093520B (en) * | 2017-03-03 | 2019-01-01 | 清华大学深圳研究生院 | Three layers of integrated flexible film supercapacitor of one kind and preparation method thereof |
| TWI745229B (en) * | 2020-11-10 | 2021-11-01 | 友達光電股份有限公司 | Pixel brightness compensation structure of stretchable display |
| CN116375005A (en) * | 2023-04-11 | 2023-07-04 | 厦门大学 | Efficient carbon nano tube vertical array hybridization stripping method |
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