CN106449166B - Ultracapacitor preparation method based on single-walled carbon nanotube/tungsten oxide nano composite film electrode - Google Patents
Ultracapacitor preparation method based on single-walled carbon nanotube/tungsten oxide nano composite film electrode Download PDFInfo
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Abstract
The present invention relates to a kind of ultracapacitor preparation method based on single-walled carbon nanotube/tungsten oxide nano composite film electrode, including：Under air atmosphere, the absolute ethyl alcohol precursor solution of tungsten salt and polyvinylpyrrolidone is prepared, 160~200 DEG C of 10~20h of reaction, cool down, centrifuge, wash, disperse, obtain W18O49Nanowire dispersion；Nanowire dispersion is mixed with single-walled carbon nanotube, is filtered, is washed, it is dry, obtain single-walled carbon nanotube/tungsten oxide nano composite film electrode；Composite film electrode assembles, as cathode, single-walled carbon nanotube/polyaniline film as anode, aluminum salt solution as electrolyte to obtain the final product.The inventive method achieves double layer electrodes material and fake capacitance electrode material are compound on micro-nano level, obtained ultracapacitor has excellent aluminium ion capacitive property and splendid mechanical flexibility, has further expanded the application range of ultracapacitor.
Description
Technical field
The invention belongs to the preparation field of super capacitor film electrode, it is more particularly to a kind of based on single-walled carbon nanotube/
The ultracapacitor preparation method of tungsten oxide nano composite film electrode.
Background technology
Ultracapacitor is widely studied as most having the electrochemical energy storing device of application prospect at present, according to electrochemistry
Energy storage principle is different, and the electrode material of ultracapacitor is divided into double layer electrodes material and fake capacitance electrode material.In general,
The electrical conductivity of double layer electrodes material is high, charge/discharge rates are fast, electrochemical stability is preferable, but capacitance is smaller.And counterfeit electricity
It is preferable to hold the capacitive property of electrode material, energy density is high, but there are the shortcomings that charge-discharge velocity is relatively low, stability is poor.Therefore
By above two Material cladding, with reference to the advantages of the two, nano material is especially selected, is current grind using its cooperative effect
Study carefully hot spot.
Ultracapacitor uses the solution for containing monovalent cation as electrolyte more at present, but these ion electrolyte
All there is it is fatal the shortcomings that, for example, highly acid hydrogen ion is in electrochemical reaction process, to metal oxide-type fake capacitance material
Expect that corrosivity is strong, it is relatively low to often lead to the electrochemical stability of such material, and sodium ion or potassium ion are due to ionic radius
It is larger, it is difficult to be embedded into the inside of fake capacitance electrode material, so as to cause the capacitance of such capacitor extremely low.In recent years, base
Gradually favored in the ultracapacitor of aluminium ion electrolyte be subject to people, this is primarily due to the relatively low ionic radius of aluminium ion
Cause faster solid phase dynamics, while the ion insertion of high price needs more electronics to be neutralized, so as to cause to carry at double
High specific capacitance performance.But in production, also there is a series of problems with application aspect based on aluminum ions ultracapacitor.
First, combination electrode material preparation process is complicated；Second, composite material species is single, and micro-nano structure is unfavorable for aluminium ion insertion,
So as to cause capacitive property to be affected；3rd, the ultracapacitor bending property assembled is poor, can not meet emerging at present
Wearable device etc. requirement.
The content of the invention
The technical problems to be solved by the invention are to provide one kind and are based on single-walled carbon nanotube/tungsten oxide nano THIN COMPOSITE
The ultracapacitor preparation method of membrane electrode, this method preparation process is simple, and cost is low, can realize that double layer electrodes material is (single
Wall carbon nano tube) and fake capacitance electrode material (W18O49Nano wire) structure design on nano-level, make to have two kinds of materials each
From advantage be not fully exerted, obtain excellent combination property based on aluminum ions ultracapacitor.
The present invention by simply efficiently method prepare flexible single-walled carbon nanotube/tungsten oxide W18O49Nano wire is compound
Membrane electrode, and assemble and obtain the aluminium ion ultracapacitor of high-performance high flexibility, there is very high research significance and business valency
Value.
It is prepared by a kind of ultracapacitor based on single-walled carbon nanotube/tungsten oxide nano composite film electrode of the present invention
Method, including：
(1) under air atmosphere, the absolute ethyl alcohol precursor solution containing tungsten salt and polyvinylpyrrolidone is prepared, is transferred to
In water heating kettle, 160~200 DEG C of 10~20h of reaction, cooled to room temperature, centrifuges, and washs, and disperses, obtains W18O49Nano wire
Dispersion liquid；
(2) by the W in step (1)18O49Nanowire dispersion is sufficiently mixed with single-walled carbon nanotube, is filtered, and is washed, and is done
It is dry, obtain flexible single-walled carbon nanotube/W18O49Nano wire composite film electrode；
(3) by single-walled carbon nanotube/W in step (2)18O49Nano wire composite film electrode is received as cathode, single wall carbon
Mitron/polyaniline film is as anode, and as electrolyte, assembling, obtains being based on single-walled carbon nanotube/W aluminum salt solution18O49Receive
The flexible aluminium ion ultracapacitor of rice noodles composite film electrode.
The concentration of tungsten salt is 0.2~1.2mg/ml in precursor solution in the step (1), polyvinylpyrrolidone it is dense
Spend for 5~50 μ g/ml.
Tungsten salt is tungsten hexachloride in the step (1).
Ambient humidity is 20~70% in the process for preparation of precursor solution in the step (1).
W in the step (1)18O49The concentration of nanowire dispersion is 1~5mg/ml.
W in the step (1)18O49The solvent of nanowire dispersion is deionized water.
W in the step (2)18O49The mass ratio of nano wire and single-walled carbon nanotube is 2:1~5:1.
The concentration of aluminum salt solution is 0.5~1.5mol/L in the step (3).
The aluminum salt solution is aluminium chloride, aluminum sulfate, aluminum nitrate aqueous solution or the carbonic allyl ester solution of aluminum perchlorate.
Single-walled carbon nanotube/polyaniline film is bibliography (ACS Nano, 2010,4,2445) in the step (3)
It is prepared.
Beneficial effect
(1) preparation method of the invention is simple, and cost is low, is adapted to large-scale production；
(2) present invention realizes both answering on nano-level by the way that both dispersion liquids directly are mixed the method filtered
Close, the nanometer line network with superior structural of formation, experiment is provided for further open Novel super capacitor thin-film material
And theoretical foundation；
(3) both dispersion liquids are directly mixed, filter obtained flexible single-walled carbon nanotube/W by the present invention18O49Nano wire
Composite film electrode not only improves the small deficiency of single-walled carbon nanotube specific capacitance, while also overcomes transition metal oxide and follow
The shortcomings that ring stability is poor, power density is small, what is assembled has high electrochemistry height based on aluminium ion ultracapacitor
Performance, prospect is widely applied in energy storage device field.
Brief description of the drawings
Fig. 1 is W prepared by embodiment 118O49The stereoscan photograph of nano wire；
Fig. 2 is single-walled carbon nanotube/W prepared by embodiment 118O49The stereoscan photograph of nano wire composite film electrode；
Fig. 3 is single-walled carbon nanotube/W prepared by embodiment 118O49Aluminium chloride of the nano wire composite film electrode in 1M is molten
Constant current charge-discharge curve in liquid；
Fig. 4 is single-walled carbon nanotube/W prepared by embodiment 118O49Aluminium chloride of the nano wire composite film electrode in 1M is molten
Capacity retention after repeatedly being circulated in liquid；
Fig. 5 is the constant current charge-discharge for the aluminium ion ultracapacitor that embodiment 1 is assembled using the aluminium chloride of 1M as electrolyte
Curve；
Specific capacitance conservation rate of the aluminium ion ultracapacitor that Fig. 6 is assembled by embodiment 1 under multiple bending condition.
Embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Embodiment 1
In humidity is 50% air ambient, polyvinylpyrrolidone and tungsten hexachloride are respectively put into ethanol solution
Middle stirring, obtains the precursor solution containing 7 μ g/ml polyvinylpyrrolidones and 0.75mg/ml tungsten hexachlorides, solution is put
It is placed in water heating kettle, when 180 DEG C of insulations 18 are small, cooled to room temperature, adds in deionized water after centrifuge washing, obtain
3mg/ml W18O49Nanowire dispersion.By the suspension containing 15mg single-walled carbon nanotubes and the above-mentioned W of 15ml18O49Nano wire point
Dispersion liquid mixing, suction filtration, washing are dried to obtain single-walled carbon nanotube/W18O49Nano wire flexible composite film electrode.Answered what is obtained
Film is closed as cathode, single-walled carbon nanotube/polyaniline film as anode, 1mol/L aluminum chloride aqueous solutions as electrolyte,
Assembling obtains aluminium ion ultracapacitor.Fig. 1 is the W prepared18O49The stereoscan photograph of nano wire, it can be seen that W18O49Nanometer
Line has higher draw ratio, a diameter of 5nm~25nm.Fig. 2 is the single-walled carbon nanotube/W prepared18O49Nano wire THIN COMPOSITE
The stereoscan photograph of membrane electrode, it can be seen that carbon nanotubes and W18O49Nano wire is intertwined to form network, and has multi-stage porous
Hole structure, ensure that good ion transmission is shifted with electronics.Fig. 3 is the single wall carbon of preparation in 1mol/L liquor alumini chloridis
Nanotube/W18O49The constant current charge-discharge diagram of nano wire composite film electrode, it can be seen that composite film electrode has high area
Specific capacitance and there is good discharge and recharge invertibity.Fig. 4 is the cyclical stability figure of composite film electrode, it can be seen that combination electrode
With high cyclical stability, Fig. 5 is the constant current of the aluminium ion ultracapacitor assembled using the aluminium chloride of 1M as electrolyte
Charging and discharging curve, it can be seen that prepared aluminium ion ultracapacitor has longer discharge time, illustrates that its higher energy is close
Degree.The specific capacitance conservation rate that Fig. 6 is the aluminium ion ultracapacitor that is assembled under multiple bending condition, illustrates that the aluminium ion surpasses
Level capacitor has high mechanical flexibility.
Embodiment 2
In humidity is 20% air ambient, polyvinylpyrrolidone and tungsten hexachloride are respectively put into ethanol solution
Middle stirring, obtains the precursor solution containing 7 μ g/ml polyvinylpyrrolidones and 0.2mg/ml tungsten hexachlorides, solution is put
It is placed in water heating kettle, when 160 DEG C of insulations 18 are small, cooled to room temperature, adds in deionized water after centrifuge washing, obtain
3mg/ml W18O49Nanowire dispersion.By the suspension containing 15mg single-walled carbon nanotubes and the above-mentioned W of 15ml18O49Nano wire point
Dispersion liquid mixing, suction filtration, washing are dried to obtain single-walled carbon nanotube/W18O49Nano wire flexible composite film electrode.Answered what is obtained
Film is closed as cathode, single-walled carbon nanotube/polyaniline film as anode, 1mol/L aluminum nitrate aqueous solutions as electrolyte,
Assembling obtains aluminium ion ultracapacitor.Since the amount of tungsten hexachloride in precursor solution significantly reduces, and and polyvinyl pyrrole
Alkanone mass ratio substantially reduces, and soaking time has reduced in addition so that obtained W18O49Nano wire is compared with embodiment 1
Average diameter substantially reduces；But due to the connection function of single-walled carbon nanotube suspension so that obtained single-walled carbon nanotube/
W18O49Nano wire composite film electrode still has good film forming, but specific capacitance slightly reduces, and the aluminium ion assembled is super
Capacitor power density is also declined slightly.
Embodiment 3
In humidity is 20% air ambient, polyvinylpyrrolidone and tungsten hexachloride are respectively put into ethanol solution
Middle stirring, obtains the precursor solution containing 5 μ g/ml polyvinylpyrrolidones and 1.2mg/ml tungsten hexachlorides, solution is put
It is placed in water heating kettle, when 180 DEG C of insulations 18 are small, cooled to room temperature, adds in deionized water after centrifuge washing, obtain
5mg/ml W18O49Nanowire dispersion.By the suspension containing 10mg single-walled carbon nanotubes and the above-mentioned W of 10ml18O49Nano wire point
Dispersion liquid mixing, suction filtration, washing are dried to obtain single-walled carbon nanotube/W18O49Nano wire flexible composite film electrode.Answered what is obtained
Film is closed as cathode, single-walled carbon nanotube/polyaniline film is as anode, and 0.5mol/L aluminum nitrate aqueous solutions are as electrolysis
Liquid, assembling obtain aluminium ion ultracapacitor.Since the amount of tungsten hexachloride in precursor solution increased, and with polyethylene pyrrole
Pyrrolidone mass ratio improves, obtained W18O49Nano wire average diameter compared with embodiment 1 slightly increases, and draw ratio is obvious
Reduce, decline so that the nanometer line network resulted in is flexible, the electricity in multiple BENDING PROCESS of aluminium ion ultracapacitor
Hold conservation rate to decline；Due to W in mixed liquor18O49Nano wire improves a lot with single-walled carbon nanotube mass ratio, reduces film
Whole conductivity, simultaneously because W18O49Nanowire diameter slightly increases, draw ratio reduces, and causes active material specific surface area
Reduce, so that its specific capacitance is slightly reduced with embodiment 1, simultaneously because the reduction of concentration of electrolyte, aluminium ion super capacitor
Device power density is also declined slightly.
Embodiment 4
In humidity is 70% air ambient, polyvinylpyrrolidone and tungsten hexachloride are respectively put into ethanol solution
Middle stirring, obtains the precursor solution containing 50 μ g/ml polyvinylpyrrolidones and 1.2mg/ml tungsten hexachlorides, solution is put
It is placed in water heating kettle, when 160 DEG C of insulations 18 are small, cooled to room temperature, adds in deionized water after centrifuge washing, obtain
5mg/ml W18O49Nanowire dispersion.By the suspension containing 10mg single-walled carbon nanotubes and the above-mentioned W of 10ml18O49Nano wire point
Dispersion liquid mixing, suction filtration, washing are dried to obtain single-walled carbon nanotube/W18O49Nano wire flexible composite film electrode.Answered what is obtained
Film is closed as cathode, single-walled carbon nanotube/polyaniline film is as anode, and 0.5mol/L aluminum sulfate aqueous solutions are as electrolysis
Liquid, assembling obtain aluminium ion ultracapacitor.Due to tungsten hexachloride amount showed increased in precursor solution, so as to get W18O49
Nano wire average diameter compared with embodiment 1 increased, simultaneously because the raising of polyvinylpyrrolidone amount, causes
W18O49Nanowire surface has wrapped up excessive macromolecule, is unfavorable for electric transmission；Due to W in mixed liquor18O49Nano wire and single wall
Carbon nanotube mass ratio increases so that single-walled carbon nanotube compound quantity is less, and composite film electrode electric conductivity declines, electronics
Transmission is obstructed, and causes single-walled carbon nanotube/W18O49Nano wire laminated film capacitive character is poor, aluminium ion ultracapacitor power
Density is also declined slightly.
Embodiment 5
In humidity is 50% air ambient, polyvinylpyrrolidone and tungsten hexachloride are respectively put into ethanol solution
Middle stirring, obtains the precursor solution containing 5 μ g/ml polyvinylpyrrolidones and 0.75mg/ml tungsten hexachlorides, solution is put
It is placed in water heating kettle, when 160 DEG C of insulations 10 are small, cooled to room temperature, adds in deionized water after centrifuge washing, obtain
5mg/ml W18O49Nanowire dispersion.By the suspension containing 25mg single-walled carbon nanotubes and the above-mentioned W of 10ml18O49Nano wire point
Dispersion liquid mixing, suction filtration, washing are dried to obtain single-walled carbon nanotube/W18O49Nano wire flexible composite film electrode.Answered what is obtained
It is molten as anode, the propene carbonate of 1.5mol/L aluminum perchlorates as cathode, single-walled carbon nanotube/polyaniline film to close film
Liquid obtains aluminium ion ultracapacitor as electrolyte, assembling.The reduction of polyvinylpyrrolidone amount causes in precursor solution
The one-dimensional growth of nano wire is obstructed, therefore obtained W18O49Nano wire average diameter compared with embodiment 1 slightly improves, and also leads
The mechanical stability of aluminium ion ultracapacitor is caused to decline；Due to W in mixed liquor18O49The matter of nano wire and single-walled carbon nanotube
Amount reduces than, its specific capacitance is slightly below embodiment 1, and aluminium ion ultracapacitor power density is also declined slightly.
Embodiment 6
In humidity is 70% air ambient, polyvinylpyrrolidone and tungsten hexachloride are respectively put into ethanol solution
Middle stirring, obtains the precursor solution containing 50 μ g/ml polyvinylpyrrolidones and 0.2mg/ml tungsten hexachlorides, solution is put
It is placed in water heating kettle, when 200 DEG C of insulations 20 are small, cooled to room temperature, adds in deionized water after centrifuge washing, obtain
5mg/ml W18O49Nanowire dispersion.By the suspension containing 25mg single-walled carbon nanotubes and the above-mentioned W of 10ml18O49Nano wire point
Dispersion liquid mixing, suction filtration, washing are dried to obtain single-walled carbon nanotube/W18O49Nano wire flexible composite film electrode.Answered what is obtained
Film is closed as cathode, single-walled carbon nanotube/polyaniline film as anode, 1mol/L aluminum chloride aqueous solutions as electrolyte,
Assembling obtains aluminium ion ultracapacitor.Although precursor solution has fraction hydrolysis under high humility, due to being led as structure
Raising to the polyvinylpyrrolidone amount of effect, so as to get W18O49Nano wire average diameter phase compared with embodiment 1
Seemingly, but nanowire surface has more polymeric PTC materials, and electric transmission is obstructed, so as to cause single-walled carbon nanotube/W18O49Nano wire
The specific capacitance of flexible composite film electrode is less than embodiment 1, and aluminium ion ultracapacitor power density is also declined slightly.
Claims (9)
1. one kind is based on single-walled carbon nanotube/tungsten oxide W18O49The ultracapacitor preparation method of nano wire composite film electrode,
Including：
(1) under air atmosphere, the absolute ethyl alcohol precursor solution containing tungsten salt and polyvinylpyrrolidone is prepared, 160~200 DEG C
10~20h is reacted, is cooled down, is centrifuged, is washed, disperses, obtains tungsten oxide W18O49Nanowire dispersion；
(2) by the W in step (1)18O49Nanowire dispersion is mixed with single-walled carbon nanotube, is filtered, and is washed, dry, obtains list
Wall carbon nano tube/W18O49Nano wire composite film electrode；
(3) by single-walled carbon nanotube/W in step (2)18O49Nano wire composite film electrode as cathode, single-walled carbon nanotube/
Polyaniline film is as anode, and as electrolyte, assembling, obtains being based on single-walled carbon nanotube/W aluminum salt solution18O49Nano wire is answered
Close the ultracapacitor of membrane electrode.
2. one kind according to claim 1 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that in the step (1) in precursor solution the concentration of tungsten salt for 0.2~
1.2mg/ml, the concentration of polyvinylpyrrolidone is 5~50 μ g/ml.
3. one kind according to claim 2 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that the tungsten salt is tungsten hexachloride.
4. one kind according to claim 1 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that ambient humidity is in the process for preparation of precursor solution in the step (1)
20%~70%.
5. one kind according to claim 1 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that W in the step (1)18O49The concentration of nanowire dispersion is 1~5mg/
ml。
6. one kind according to claim 1 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that W in the step (1)18O49The solvent of nanowire dispersion is deionized water.
7. one kind according to claim 1 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that W in the step (2)18O49The mass ratio of nano wire and single-walled carbon nanotube
For 2:1~5:1.
8. one kind according to claim 1 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that the concentration of aluminum salt solution is 0.5~1.5mol/L in the step (3).
9. one kind according to claim 8 is based on single-walled carbon nanotube/tungsten oxide W18O49Nano wire composite film electrode
Ultracapacitor preparation method, it is characterised in that the aluminum salt solution is aluminum chloride aqueous solution, aluminum sulfate aqueous solution, aluminum nitrate
Aqueous solution or the carbonic allyl ester solution of aluminum perchlorate.
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| CN106847544B (en) * | 2017-03-10 | 2019-05-03 | 东华大学 | A kind of preparation method of high specific capacitance flexible super capacitor negative electrode material |
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| CN115346803A (en) * | 2022-08-03 | 2022-11-15 | 昆明理工大学 | W 18 O 49 Carbon paper composite electrode material and preparation method thereof |
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