CN110211811A - A kind of symmetrical supercapacitor of full fake capacitance and preparation method thereof - Google Patents
A kind of symmetrical supercapacitor of full fake capacitance and preparation method thereof Download PDFInfo
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- CN110211811A CN110211811A CN201910492274.XA CN201910492274A CN110211811A CN 110211811 A CN110211811 A CN 110211811A CN 201910492274 A CN201910492274 A CN 201910492274A CN 110211811 A CN110211811 A CN 110211811A
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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
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
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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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- 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 proposes a kind of complete symmetrical supercapacitors of fake capacitance and preparation method thereof, the complete symmetrical supercapacitor of fake capacitance includes anode, cathode, collector, the diaphragm and electrolyte being set between positive and negative anodes, and the positive electrode and negative electrode are using nickel ferrite based magnetic loaded and its composite material as active material.The NiFe that the nano-carbon material (carbon nano pipe array, grapheme foam etc.) that the preparation method of the symmetrical supercapacitor of full fake capacitance is prepared in various ways supports2O4Composite material is positive and negative anodes, using KOH aqueous solution or NaOH aqueous solution as electrolyte solution, constructs the water-based complete symmetrical supercapacitor of fake capacitance.Bipolarity NiFe proposed by the present invention2O4The preparation method of electrode and full fake capacitance symmetric capacitor, simplifies the preparation process of positive and negative electrode, have the advantages that it is environmentally protective, easy to operate, be easy to prepare with scale.And the symmetrical super capacitor energy density and power density that preparation method according to the present invention obtains are high, and have good high rate performance.
Description
Technical field
The present invention relates to super capacitors more particularly to a kind of symmetrical supercapacitor of full fake capacitance and preparation method thereof.
Background technique
With society and economic further development, energy and environmental problem is increasingly subject to the concern of people.Super capacitor
Device is also known as electrochemical capacitor, is a kind of important electrochemical energy storage device, have power density is high, have extended cycle life,
Use temperature range is wide, it is environmental-friendly and can instantaneous large-current fast charging and discharging the features such as, therefore in new-energy automobile, spy
There are huge application value and market potential in the fields such as different truck, electric power, communication, national defence, consumer electronics product.So
And compared with traditional chemical cell, the lower energy density of supercapacitor strongly limits its large-scale practical application, because
This, under the premise of guaranteeing high power density, the energy density for improving supercapacitor has become the emphasis of people's research.
Usually there are two types of methods for the energy density of improvement supercapacitor, another one is the operating voltage for improving device
Kind method is to improve the specific capacitance of electrode material.The electrode material of different energy storage mechnisms is assembled into asymmetric capacitor, is utilized
The difference of positive and negative pole material polarization potential widens the operating voltage window of capacitor, is the effective way for improving capacitor working pressure
Diameter.Conventional Asymmetric Supercapacitor, usually by a fake capacitance electrode with fake capacitance characteristic with one by double electric
The carbon material electrode composition of layer energy storage.Since positive and negative electrode generallys use different preparation methods, inevitably increase
The preparation cost of supercapacitor.
Nickel ferrite based magnetic loaded (NiFe2O4) due to low in cost, environmentally friendly, and theoretical specific capacitance with higher and recognized
To be important fake capacitance material.In the inverse spinel structure dot matrix of nickel ferrite based magnetic loaded, Ni2+With half Fe3+It occupies between octahedron
Gap, and another half Fe3+Then occupy the tetrahedral interstice of dot matrix.Due to Ni2+/Ni3+And Fe3+/Fe2+Oxidation in water-medium
Reduction potential is located at positive voltage and negative voltage range, therefore NiFe2O4It is a kind of possible bipolarity fake capacitance material.?
Some researches show that NiFe2O4Electrode both can be in positive voltage window or in negative voltage window banging in aqueous electrolyte solution.
However, with NiFe2O4It is used as the symmetric capacitor that anode and negative electrode material are constructed simultaneously, has not yet to see by reporting.
Although compared with single metal oxides, NiFe2O4With higher conductivity and electro-chemical activity, but its specific capacitance
It is still unsatisfactory with high rate performance.Therefore, the growth in situ NiFe on the carbon material skeleton of graded porous structure2O4Activity
Substance is to prepare high-performance NiFe2O4The feasible method of combination electrode.
Summary of the invention
The purpose of the present invention aims to solve the problem that the above problem, provide one kind can and meanwhile be used as in aqueous electrolyte anode and
The symmetrical supercapacitor of full fake capacitance of the fake capacitance material of cathode.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of complete symmetrical supercapacitor of fake capacitance,
Including anode, cathode, collector, the diaphragm and electrolyte being set between positive and negative anodes, the positive electrode and negative electrode with nickel ferrite based magnetic loaded and
Its composite material is active material.
As in a kind of complete symmetrical supercapacitor of fake capacitance of the invention, the electrolyte is Na2SO3、Na2SO4And
Any one in KOH aqueous solution.
As in a kind of complete symmetrical supercapacitor of fake capacitance of the invention, the concentration of the electrolyte is 0.1-10mol/
L。
As in a kind of complete symmetrical supercapacitor of fake capacitance of the invention, the collector is nickel foam.
The preparation method of the aforementioned symmetrical supercapacitor of full fake capacitance, the preparation method include electrode preparation step and
Asymmetric Supercapacitor assembling steps further include following steps before the preparation step of electrode: NiFe2O4/ carbon nano-pipe array
The preparation step of column composite material.
In preparation method as the symmetrical supercapacitor of full fake capacitance of the invention, the NiFe2O4/ carbon nano-pipe array
The preparation step of column composite material includes:
1.1, dicyclopentadienyl nickel and ferric acetyl acetonade are dissolved in acetone soln, and are successively put into carbon nano pipe array sample
Then reactor is closed reactor；
1.2, shooting flow reactor according is preheated to 40-60 DEG C, is then filled with high purity liquid carbon dioxide thereto simultaneously
It is pressurized to 9-12MPa and carbon dioxide is made to reach supercriticality, and shooting flow reactor according is heated to 115-125
DEG C, 5-7 hours are kept the temperature, the vertical carbon nanotube sample for being adsorbed with nickel, iron presoma is obtained；
1.3, the carbon nanotube-sample for being adsorbed with presoma will be transferred to quick anneal oven, is 350 DEG C true in temperature
It anneals 3 hours under empty condition, obtains NiFe2O4/ vertical carbon nanotube composite material after cooling.
In preparation method as the symmetrical supercapacitor of full fake capacitance of the invention, the NiFe2O4/ carbon nano-pipe array
The preparation step of column composite material includes:
1.1, dicyclopentadienyl nickel and ferric acetyl acetonade are dissolved in acetone soln, and are successively put into instead with grapheme foam sample
Device is answered, then closes reactor；
1.2, shooting flow reactor according is preheated to 40-60 DEG C, is then filled with high purity liquid carbon dioxide thereto simultaneously
It is pressurized to 10-12MPa and carbon dioxide is made to reach supercriticality, and shooting flow reactor according is heated to 105-120
DEG C, 5-7 hours are kept the temperature, the grapheme foam sample for being adsorbed with nickel, iron presoma is obtained；
1.3, the grapheme foam sample for being adsorbed with presoma is transferred to quick anneal oven, is 340-355 DEG C in temperature
Vacuum condition under anneal 3-3.5 hours, obtain NiFe after cooling2O4/ grapheme foam composite material.
In preparation method as the symmetrical supercapacitor of full fake capacitance of the invention, the NiFe2O4/ carbon nano-pipe array
The preparation step of column composite material includes:
1.1, the potassium ferricyanide is uniformly mixed with graphene oxide water solution, six water nickel chlorides and deionization is added later
Water, centrifugation removal supernatant liquor after stirring；
1.2, vitamin sodium is added, and transfers the solution into vial, 90-100 DEG C heat preservation 1.8-2.5 hours, from
And obtain the three-dimensional grapheme material for supporting the Prussian blue similar object of FeNi；
1.3, above-mentioned presoma is heated to 290-320 DEG C in air and keeps the temperature 1.8-2.5 hours, to obtain graphite
Alkene aeroge supports the composite material of NiFe2O4.
In preparation method as the symmetrical supercapacitor of full fake capacitance of the invention, the dicyclopentadienyl nickel and ferric acetyl acetonade
Mass percent be 1:2.
Compared with prior art, advantages of the present invention are as follows: the present invention utilizes NiFe2O4Middle Ni2+With Fe3+Oxidation-reduction potential
Difference, propose with NiFe2O4For ambipolar fake capacitance active material, to support NiFe2O4C-base composte material be it is positive and negative
Pole constructs the symmetrical supercapacitor of full fake capacitance using aqueous solution as electrolyte.Method proposed by the present invention, avoids just
Negative electrode material uses cost increase caused by Different Preparation, the symmetrical supercapacitor being prepared in the process of the present invention
With can have broad application prospects with the voltage window and energy density compared with asymmetric capacitor.
Detailed description of the invention
Fig. 1 is NiFe in the embodiment of the present invention one2O4Scanning electron microscope (SEM) figure of/vertical carbon nanotube composite material.
Fig. 2 is NiFe in the embodiment of the present invention one2O4Transmission electron microscope (TEM) figure of/vertical carbon nanotube composite material.
Fig. 3 is NiFe in the embodiment of the present invention one2O4The XRD spectrum of/vertical carbon nanotube combination electrode.
Fig. 4 is cyclic voltammetry curve of the assembled symmetric capacitor under different scanning rates in the embodiment of the present invention one.
Fig. 5 is that the cyclic voltammetric of the symmetrical supercapacitor that assembles in the embodiment of the present invention one under different scanning rates is bent
Line.
Fig. 6 is that constant current charge-discharge of the symmetrical supercapacitor under different current densities in the embodiment of the present invention one is bent
Line.
Fig. 7 is energy density-power density curve of the symmetrical supercapacitor in the embodiment of the present invention one.
Specific embodiment
The technical solution adopted in the present invention is further described below in conjunction with schematic diagram.
A kind of embodiment 1: complete symmetrical supercapacitor of fake capacitance comprising anode, cathode, collector, be set to it is positive and negative
Diaphragm and electrolyte between pole, the positive electrode and negative electrode are using nickel ferrite based magnetic loaded and its composite material as active material.Full fake capacitance pair
The structure of supercapacitor is claimed to belong to the known prior art, not in this to go forth.
The preparation method of the symmetrical supercapacitor of the present embodiment the following steps are included:
Step 1: NiFe2O4The preparation of/carbon nano-tube array composite material:
The ferric acetyl acetonade of the dicyclopentadienyl nickel of 30mg and 60mg is dissolved in 1ml acetone soln, and and carbon nano pipe array
Sample is successively put into reactor, then closes reactor.Shooting flow reactor according is preheated to 50 DEG C, is then filled thereto
Enter high purity liquid carbon dioxide and being pressurized to 10MPa makes carbon dioxide reach supercriticality, and by shooting flow reactor according
120 DEG C are heated to, 6 hours is kept the temperature, obtains the vertical carbon nanotube sample for being adsorbed with nickel, iron presoma.Presoma will be adsorbed with
Carbon nanotube-sample be transferred to quick anneal oven, anneal 3 hours in the case where temperature is 350 DEG C of vacuum condition, is obtained after cooling down
NiFe2O4/ vertical carbon nanotube composite material.
Fig. 1 is NiFe2O4Scanning electron microscope (SEM) figure of/vertical carbon nanotube composite material.
Fig. 2 is NiFe2O4Transmission electron microscope (TEM) figure of/vertical carbon nanotube composite material.
Fig. 3 is NiFe2O4The XRD spectrum of/vertical carbon nanotube combination electrode.
Step 2: the preparation of electrode:
After sample preparation, by NiFe2O4/ vertical carbon nanotube composite material is removed from silicon wafer, and is transferred to nickel foam
On collector, applies the pressure compacting flakiness of 3MPa and be cut to suitable dimension.
Step 3: assembling Asymmetric Supercapacitor:
The NiFe that step 2 is obtained2O4/ vertical carbon nanotube electrode be used as positive and negative anodes, with slightly larger than electrode it is aqueous every
Film paper separates, and is immersed in the KOH solution of 2mol/L and is assembled into Asymmetric Supercapacitor.
Fig. 4 is cyclic voltammetry curve of the assembled symmetric capacitor under different scanning rates.
Electro-chemical test
After combination electrode prepares, its cyclic voltammetry curve is tested in the KOH solution of 2mol/L, as shown in figure 4, the electricity
It pole can the steady operation in the voltage range of -1.2~0V and 0~0.6V respectively.
Fig. 5 is cyclic voltammetry curve of the symmetrical supercapacitor of assembling under different scanning rates.The symmetrical super electricity
Container can be with steady operation under the voltage window of 0~1.8V, and similar curve is shown under different sweep speeds
Shape shows its preferable capacitive property.
Fig. 6 is constant current charge-discharge curve of the symmetrical supercapacitor under different current densities.
The charging process curve and discharge process curve of the capacitor have symmetry, illustrate there is good capacitive character
Energy.
Fig. 7 is energy density-power density curve of symmetrical supercapacitor.When the power density of device is 0.92kW/
When kg, energy density highest 36.5Wh/kg.
Embodiment 2: the preparation method of the symmetrical supercapacitor of the present embodiment the following steps are included:
By the ferric acetyl acetonade of the dicyclopentadienyl nickel of 30mg and 30mg be dissolved in 1ml acetone soln and with grapheme foam sample
It successively is put into reactor, then closes reactor.Shooting flow reactor according is preheated to 50 DEG C, is then filled with height thereto
Pure liquid carbon dioxide and being pressurized to 12MPa makes carbon dioxide reach supercriticality, and shooting flow reactor according is heated
To 100 DEG C, 6 hours are kept the temperature, the grapheme foam sample for being adsorbed with nickel, iron presoma is obtained.The graphite of presoma will be adsorbed with
Alkene foam sample is transferred to quick anneal oven, anneals 3 hours in the case where temperature is 350 DEG C of vacuum condition, obtains after cooling
NiFe2O4/ grapheme foam composite material.
With NiFe2O4/ grapheme foam is positive and negative anodes, and the KOH aqueous solution of 3mol/L is that electrolyte assembles symmetrical super capacitor
Device.The symmetrical supercapacitor obtained according to the preparation method of this implementation, quality specific capacitance are 72F/g, and energy density is
32.4Wh/kg。
Embodiment 3: the preparation method of the Asymmetric Supercapacitor of the present embodiment the following steps are included:
The 0.1mmol potassium ferricyanide is uniformly mixed with 10ml graphene oxide water solution (4mg/ml), 1mmol is added later
Six water nickel chlorides and 20ml deionized water be centrifuged in removal in 5 minutes after 500 turns are stirred one hour with the speed of 10,000 rpm
Layer clear liquid.Finally, the vitamin sodium of 198mg is added, and above-mentioned solution is transferred in the vial of 50ml, keeps the temperature 2 at 95 DEG C
Hour, to obtain the three-dimensional grapheme material for supporting the Prussian blue similar object of FeNi.Finally, in air by above-mentioned presoma
It is heated to 300 DEG C and keeps the temperature 2 hours, so that obtaining graphene aerogel supports NiFe2O4Composite material.
Under the pressure of 3MPa, appropriate composite material is pressed in foam nickel surface, can be obtained NiFe2O4The airsetting of/graphene
Gel electrode material.Using the electrode material as positive and negative anodes, the KOH aqueous solution of 6mol/L is that electrolyte assembles symmetrical supercapacitor.
The symmetrical supercapacitor obtained according to the preparation method of this implementation, quality specific capacitance are 66F/g, energy density 29.7Wh/
kg。
To sum up, in each embodiment provided by the invention, the symmetrical supercapacitor of full fake capacitance of the offer of embodiment one to three
Preparation method, the NiFe that the nano-carbon material prepared in various ways (carbon nano pipe array, grapheme foam etc.) supports2O4
Composite material is positive and negative anodes, using KOH aqueous solution or NaOH aqueous solution as electrolyte solution, constructs water-based full fake capacitance and symmetrically surpasses
Grade capacitor.
Bipolarity NiFe proposed by the present invention2O4The preparation method of electrode and full fake capacitance symmetric capacitor, simplifies positive and negative
The preparation process of electrode, have the advantages that it is environmentally protective, easy to operate, be easy to prepare with scale.And system according to the present invention
The symmetrical super capacitor energy density and power density that Preparation Method obtains are high, and have good high rate performance, application prospect
It is wide.
The above is only a preferred embodiment of the present invention, does not play the role of any restrictions to the present invention.Belonging to any
Those skilled in the art, in the range of not departing from technical solution of the present invention, to the invention discloses technical solution and
Technology contents make the variation such as any type of equivalent replacement or modification, belong to the content without departing from technical solution of the present invention, still
Within belonging to the scope of protection of the present invention.
Claims (9)
1. a kind of symmetrical supercapacitor of full fake capacitance comprising anode, cathode, collector, be set between positive and negative anodes every
Film and electrolyte, which is characterized in that the positive electrode and negative electrode are using nickel ferrite based magnetic loaded and its composite material as active material.
2. a kind of complete symmetrical supercapacitor of fake capacitance according to claim 1, which is characterized in that the electrolyte is
Na2SO3、Na2SO4And any one in KOH aqueous solution.
3. a kind of complete symmetrical supercapacitor of fake capacitance according to claim 1, which is characterized in that the electrolyte it is dense
Degree is 0.1-10mol/L.
4. a kind of complete symmetrical supercapacitor of fake capacitance according to claim 1, which is characterized in that the collector is bubble
Foam nickel.
5. a kind of preparation method of the symmetrical supercapacitor of fake capacitance complete as described in claim any one of 1-4, the preparation method
Preparation step and Asymmetric Supercapacitor assembling steps including electrode, which is characterized in that electrode preparation step it
Before further include following steps: NiFe2O4The preparation step of/carbon nano-tube array composite material.
6. preparation method according to claim 5, which is characterized in that the NiFe2O4/ carbon nano-tube array composite material
Preparation step include:
1.1, dicyclopentadienyl nickel and ferric acetyl acetonade are dissolved in acetone soln, and are successively put into and react with carbon nano pipe array sample
Then device is closed reactor；
1.2, shooting flow reactor according is preheated to 40-60 DEG C, is then filled with high purity liquid carbon dioxide thereto and pressurizeed
Make carbon dioxide reach supercriticality to 9-12MPa, and shooting flow reactor according is heated to 115-125 DEG C, protects
It is 5-7 hours warm, obtain the vertical carbon nanotube sample for being adsorbed with nickel, iron presoma；
1.3, the carbon nanotube-sample for being adsorbed with presoma will be transferred to quick anneal oven, the vacuum item for being 350 DEG C in temperature
It anneals 3 hours under part, obtains NiFe2O4/ vertical carbon nanotube composite material after cooling.
7. preparation method according to claim 5, which is characterized in that the NiFe2O4/ carbon nano-tube array composite material
Preparation step include:
1.1, dicyclopentadienyl nickel and ferric acetyl acetonade are dissolved in acetone soln, and are successively put into and react with grapheme foam sample
Then device is closed reactor；
1.2, shooting flow reactor according is preheated to 40-60 DEG C, is then filled with high purity liquid carbon dioxide thereto and pressurizeed
Make carbon dioxide reach supercriticality to 10-12MPa, and shooting flow reactor according is heated to 105-120 DEG C, protects
It is 5-7 hours warm, obtain the grapheme foam sample for being adsorbed with nickel, iron presoma；
1.3, the grapheme foam sample for being adsorbed with presoma is transferred to quick anneal oven, is 340-355 DEG C true in temperature
It anneals 3-3.5 hours under empty condition, obtains NiFe after cooling2O4/ grapheme foam composite material.
8. preparation method according to claim 5, which is characterized in that the NiFe2O4/ carbon nano-tube array composite material
Preparation step include:
1.1, the potassium ferricyanide is uniformly mixed with graphene oxide water solution, six water nickel chlorides and deionized water is added later, stirs
Centrifugation removal supernatant liquor after mixing；
1.2, vitamin sodium is added, and transfers the solution into vial, 90-100 DEG C heat preservation 1.8-2.5 hours, to obtain
The three-dimensional grapheme material of the Prussian blue similar object of FeNi must be supported；
1.3, above-mentioned presoma is heated to 290-320 DEG C in air and keeps the temperature 1.8-2.5 hours, to obtain graphene gas
Gel supports the composite material of NiFe2O4.
9. preparation method according to claim 6 or 7, which is characterized in that the quality of the dicyclopentadienyl nickel and ferric acetyl acetonade
Percentage is 1:2.
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| CN114496585A (en) * | 2022-01-21 | 2022-05-13 | 西安电子科技大学 | High-performance supercapacitor composite electrode material based on carbon nanotube array and preparation method thereof |
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