CN106887341A - The preparation method of three-dimensional grapheme/polyaniline array electrode material for super capacitor - Google Patents
The preparation method of three-dimensional grapheme/polyaniline array electrode material for super capacitor Download PDFInfo
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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
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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
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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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- 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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Abstract
A kind of preparation method of three-dimensional grapheme/polyaniline array electrode material for super capacitor, nickel foam prepares three-dimensional grapheme substrate as template by chemical vapour deposition technique, then slight activation process is carried out to three-dimensional grapheme, situ aggregation method growth in situ polyaniline array in three-dimensional grapheme substrate is finally utilized, obtains a kind of with high-specific surface area, high performance electrode material for super capacitor.Preparation method of the present invention is simple, and prepared electrode material polyaniline is evenly distributed, and graphene-structured is complete, and chemical property has relative to independent Graphene and is obviously improved.
Description
Technical field
The present invention relates to a kind of preparation method of three-dimensional grapheme/polyaniline array electrode material for super capacitor.
Background technology
Ultracapacitor as a kind of new electric energy storage device, energy density and power density with superelevation, compared with
The advantages of cyclical stability high.Double layer capacitor can be mainly classified as by its energy storage mechnism difference and pseudocapacitors two are big
Class.Double layer capacitor is mainly to be realized the storage of electric charge and released in electrode material surface adsorption desorption by electrolyte ion
Put.Therefore wanting to obtain energy density higher needs the electrode material to have larger specific surface area.Graphene is a kind of only single
The two-dimensional material of atomic layer level thickness, electric conductivity and excellent mechanical property with superelevation, while its specific surface area may be up to
2630 m2×g-1, therefore Graphene is considered as a kind of ideal electrode material for super capacitor.
Nearest three-dimensional grapheme causes the concern of many researchers, its three-dimensional porous structure because of its excellent performance
Bigger specific surface area can be provided, while the generation of Graphene agglomeration can be prevented, the effective electrification for improving material
Learn performance.But individually using three-dimensional grapheme as electrode material for super capacitor, due to the energy storage mechanism of its electric double layer, storage
Capacity is relatively low, it is impossible to meet actual demand.Therefore by three-dimensional grapheme and fake capacitance material, (transition metal oxide and conduction are poly-
Compound) combine, while using two kinds of performance advantages of material, as the primary hand for improving three-dimensional grapheme chemical property at present
Section.Polyaniline is a kind of electrode material for super capacitor applied widely, and its conductive energy is high, theoretical specific capacity
It is high, the advantages of synthetic method is simple and cheap.It is combined with three-dimensional grapheme and is prepared graphene/polyaniline compound electric
Focus of the pole material to be studied as current electrode material for super capacitor.Wherein, graphene oxide contains because its surface is substantial amounts of
Oxygen groups can provide avtive spot for the polymerization of aniline, it is easy to which the three-dimensional structure for forming stabilization is widely paid close attention to.(Yu
Pingping, Zhao Xin, Huang Zilong, et al. Free-standing three-dimensional
graphene and polyaniline nanowire arrays hybrid foams for highperformance
flexible and lightweight supercapacitors. Journal of materials chemistry A,
2014,2:14413-14420.) Yu et al. is immersed in nickel foam as template in the aqueous solution of graphene oxide, makes oxidation
Graphene is wrapped in foam nickel surface, is then defoamed nickel template using hydrochloric acid solution, and obtain three-dimensional by electronation
Grapheme material.Add it in aniline monomer solution, soak 180 min, add 24 h of polymerization accelerant polymerization to obtain three
Dimension grapheme/polyaniline composite material.790 F/g, and warp are can reach to its specific capacitance for carrying out electro-chemical test composite
Its capacity retention rate still can reach 80% after crossing 5000 circulations.This aspect is because Graphene is carried for the quick transmission of electronics
Passage is supplied, on the other hand because polyaniline is well-regulated to arrange the specific surface area that increased material, so as to effectively improve
The chemical property of material.(Meng Yuena, Wang Kai, Zhang Yajie, ea al. Hierarchical
porous graphene/polyaniline composite film with superior rate performance for
flexible supercapacitors, Advanced materials, 2013,25(48):6985-6990.) Meng etc.
By graphene oxide dispersion, calcium chloride and ammonia spirit mix, and are passed through carbon dioxide thereto, form graphite oxide
Alkene wraps up the three-dimensional porous structure of calcium carbonate template, then using hydrazine steam reduction graphene oxide, and is removed with hydrochloric acid solution
Calcium carbonate template obtains three-dimensional grapheme, adds it to be slowly stirred in the perchloric acid solution containing aniline monomer, Ran Houxiang
Wherein to add and react 24 h under polymerization accelerant, condition of ice bath, after product washing is dried, obtain three-dimensional grapheme/polyaniline
Composite.Due to the structure and larger specific surface area of its stabilization, composite material exhibits have gone out excellent chemical property.
In sum, three-dimensional grapheme/polyaniline composite material is prepared at present mostly with graphene oxide as raw material, then
Polyaniline is combined with the graphene oxide after reduction by chemical polymerization is prepared composite.Although graphene oxide because
There is substantial amounts of oxygen-containing functional group in its surface, for aniline polymerization provides binding site so that polyaniline is in connection even closer,
But graphene oxide in preparation process to graphene-structured destroy it is more serious, although by reduction but its electric conductivity not
Have and recovered completely, be unfavorable for the raising of electrode material chemical property.Therefore with structural integrity, morphology controllable, performance is excellent
Three-dimensional grapheme prepared by different chemical vapour deposition technique is raw material, prepares three-dimensional grapheme/carbon/polyaniline super capacitor electrode
Material is the effective means for improving its chemical property.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of three-dimensional grapheme/polyaniline array electrode of super capacitor
The preparation method of material.
A kind of preparation method of three-dimensional grapheme/polyaniline array electrode material for super capacitor of the invention is by following
What step was carried out:
First, three-dimensional grapheme is prepared:Be put in nickel foam as template in tube furnace, argon gas and hydrogen as carrier gas, by tubular type
Stove from room temperature be heated to 900 ~ 1100 DEG C insulation 30 ~ 60 min, and temperature be 900 ~ 1100 DEG C when to stove in 10 ~ 20
The speed of sccm is passed through the min of methane gas 5 ~ 10.Then tube furnace is cooled to room temperature with the speed of 80 ~ 100 DEG C/min, so
The nickel foam that obtained Graphene is wrapped up is cut into the cm of area 1 ' 1 afterwards2Square, and by poly- methyl that mass fraction is 4%
Methyl acrylate solution drips to Graphene parcel foam nickel surface by 100 ~ 150 mL consumptions every square centimeter, is protected at 200 DEG C
30 ~ 60 min of temperature, make Graphene wrap up the polymethyl methacrylate solution solidification drying of foam nickel surface, are then soaked
It it is 60 ~ 90 DEG C to temperature, concentration is 3 ~ 12 h in the hydrochloric acid solution of 3 ~ 4 mol/L, removes nickel foam therein, reusable heat third
Ketone solution removes polymethyl methacrylate therein, and is cleaned up repeatedly with deionized water, obtains three-dimensional grapheme.Then
The three-dimensional grapheme that will be cleaned up soaks 12 ~ 18 h in being moved into concentrated nitric acid solution, obtains the three-dimensional grapheme being slightly acidified;
2nd, in-situ polymerization prepares polyaniline array:Aniline monomer and ammonium persulfate are added separately to 1 isometric mol/L's
In sulfuric acid solution, 30 ~ 60 min are stirred at room temperature is completely dissolved it.The three-dimensional stone of the slight acidifying that then step one is obtained
Black alkene is placed on slide, and is dipped in 1 ~ 3 h in aniline solution, aniline monomer is connect completely with three-dimensional grapheme
Touch, 30 ~ 60 s are slowly stirred during ammonium persulfate solution finally is heated into aniline solution under condition of ice bath, then allow it in ice
0 ~ 24 h is reacted under the conditions of bath, three-dimensional grapheme/polyaniline array composite is obtained, composite is cleaned with deionized water
Totally, it is placed on and dries 6 ~ 12 h in vacuum drying chamber at 80 ~ 100 DEG C, obtains three-dimensional grapheme/polyaniline array and be combined
Material.
A kind of application of three-dimensional grapheme/polyaniline array electrode material for super capacitor, it is characterised in that three-dimensional graphite
Alkene/polyaniline array composite is used as electrode material for super capacitor.
Advantages of the present invention:
(1) present invention prepares the three-dimensional grapheme of excellent performance by chemical vapour deposition technique, in combination with in-situ polymerization skill
Art goes out polyaniline array in three-dimensional grapheme superficial growth, and the three-dimensional grapheme/polyaniline array for being prepared for new structure is combined
Material;
(2) composite prepared by the present invention can simultaneously play the performance advantage of Graphene and polyaniline, can simultaneously utilize two
The performance advantage of material is planted, wherein polyaniline provides larger capacity, and three-dimensional grapheme is then the polyaniline for being fixed on its surface
Quick electron propagation ducts and larger specific surface area are provided, the effective chemical property for improving material, its specific capacity can
Up to 890 F/g, far above the ultracapacitor for using graphene oxide to be prepared for raw material.
Brief description of the drawings
Fig. 1 is amplified to 100 times of stereoscan photograph for the three-dimensional grapheme prepared in embodiment 1;
Fig. 2 is amplified to 100 times of stereoscan photograph for the three-dimensional grapheme/polyaniline array prepared in embodiment 1;
Fig. 3 is amplified to 5000 times of stereoscan photograph for the three-dimensional grapheme/polyaniline array prepared in embodiment 1;
Three-dimensional grapheme prepared by the three-dimensional grapheme and embodiment 2 of Fig. 4 curves 1 and the curve 2 respectively preparation of embodiment 1/poly-
Aniline array composite material circulates Fuan curve;
Fig. 5 is the constant current charge-discharge curve of three-dimensional grapheme/polyaniline array composite prepared by embodiment 1;
Fig. 6 be example 1 prepare three-dimensional grapheme graphene/polyaniline array composite material under different current densities specific volume
Amount curve
Fig. 7 is the stable circulation linearity curve of three-dimensional grapheme/polyaniline array composite prepared by embodiment 1.
Specific embodiment
Embodiment 1
This example is contrast test, prepares three-dimensional grapheme, and specific embodiment is as follows:
It is put in nickel foam as template in tube furnace, used as carrier gas, flow is respectively 500 sccm and 200 for argon gas and hydrogen
Sccm, is heated to 1000 DEG C of 30 min of insulation, and be in temperature with the heating rate of 10 DEG C/min by tube furnace from room temperature
The min of methane gas 10 is passed through with the speed of 20 sccm in stove at 1000 DEG C.Methane gas is closed, carrier gas is continually fed into simultaneously
Tube furnace is cooled to room temperature with the speed of 100 DEG C/min, the nickel foam that obtained Graphene is wrapped up then is cut into area 1
´1 cm2Square, use quality fraction is that 4% polymethyl methacrylate solution is added dropwise by 150 mL consumptions every square centimeter
Foam nickel surface is wrapped up to Graphene, 60 min are incubated at 200 DEG C, Graphene is wrapped up the poly- methyl-prop of foam nickel surface
E pioic acid methyl ester solution solidifies drying, is then dipped into temperature for 90 DEG C, concentration be 3 mol/L hydrochloric acid solution in 12 h,
Nickel foam therein is removed, last temperature in use is that 60 DEG C of hot acetone solution removes polymethyl methacrylate therein, and
Cleaned up repeatedly with deionized water and obtain three-dimensional grapheme.
With saturation Ag/AgCl electrodes as reference electrode, platinum filament is above-mentioned dry three-dimensional grapheme/polyaniline to electrode
Array composite material is working electrode, and Electrochemical Detection is carried out to it under conditions of 1 mol/L sulfuric acid solutions are as electrolyte.
As shown in Figure 1, it can be seen that the three-dimensional grapheme of preparation shows three-dimensional UNICOM's structure, graphenic surface light Slipped Clove Hitch
Structure is complete.
Embodiment 2
It is put in nickel foam as template in tube furnace, used as carrier gas, flow is respectively 500 sccm and 200 for argon gas and hydrogen
Sccm, is heated to 1000 DEG C of 30 min of insulation, and be in temperature with the heating rate of 10 DEG C/min by tube furnace from room temperature
The min of methane gas 10 is passed through with the speed of 20 sccm in stove at 1000 DEG C.Methane gas is closed, carrier gas is continually fed into simultaneously
Tube furnace is cooled to room temperature with the speed of 100 DEG C/min, the nickel foam that obtained Graphene is wrapped up then is cut into area 1
´1 cm2Square, use quality fraction is that 4% polymethyl methacrylate solution is added dropwise by 150 mL consumptions every square centimeter
Foam nickel surface is wrapped up to Graphene, 60 min are incubated at 200 DEG C, Graphene is wrapped up the poly- methyl-prop of foam nickel surface
E pioic acid methyl ester solution solidifies drying, is then dipped into temperature for 90 DEG C, concentration be 3 mol/L hydrochloric acid solution in 12 h,
Nickel foam therein is removed, last temperature in use is that 60 DEG C of hot acetone solution removes polymethyl methacrylate therein, and
Cleaned up repeatedly with deionized water and obtain three-dimensional grapheme.Then it is molten that the three-dimensional grapheme that will be cleaned up is moved into concentrated nitric acid
18 h are soaked in liquid, the three-dimensional grapheme being slightly acidified is obtained.
46.5 mL aniline monomers and 28.3 mg ammonium persulfates are added separately to the 40mL sulfuric acid that concentration is 1 mol/L molten
In liquid, 30 min are stirred at room temperature is completely dissolved it.The three-dimensional grapheme of the slight acidifying that then step one is obtained is placed
On slide, and 3 h in above-mentioned aniline solution are dipped in, aniline monomer is completely attached to three-dimensional grapheme, so
60 s are slowly stirred during ammonium persulfate solution is heated into aniline solution under condition of ice bath afterwards, relief its under condition of ice bath
24 h are reacted, three-dimensional grapheme/polyaniline array composite is obtained, by it after composite is cleaned up with deionized water
It is placed in vacuum drying chamber and 6 h is dried at 80 DEG C, obtains three-dimensional grapheme/polyaniline array composite.
Such as Fig. 2, shown in 3, one layer of polyaniline array of vertical-growth, Graphene and polyphenyl are contained on three-dimensional grapheme surface
Amine is closely combined together, and forms three-dimensional grapheme/polyaniline array composite.
With saturation Ag/AgCl electrodes as reference electrode, platinum filament is above-mentioned dry three-dimensional grapheme/polyaniline to electrode
Array composite material is working electrode, and Electrochemical Detection is carried out to it under conditions of 1 mol/L sulfuric acid solutions are as electrolyte.
Curve 1 as shown in Figure 4 and curve 2 are respectively three-dimensional prepared by the three-dimensional grapheme and embodiment 2 of the preparation of embodiment 1
Graphene/polyaniline array composite material circulates Fuan curve, as can be seen from the figure the three-dimensional graphite under same scan speed
Alkene/polyaniline array composite can store more electric charges, show more preferable capacitive property, such as Fig. 5, right shown in 6
Three-dimensional grapheme polyaniline array composite carries out constant current charge-discharge test under conditions of current density is 1 ~ 10 A/g, from
Even if it can be seen that composite has remained in that specific capacity higher at higher current densities in figure, it was demonstrated that composite has
Good rate capability, Fig. 7 is to be circulated stability test to material under the current density of 2 A/g, can from figure
The capacity retention rate gone out in the material after 1000 times circulate can reach 80%, show preferable cyclical stability.
Claims (4)
1. a kind of preparation method of three-dimensional grapheme/polyaniline array electrode material for super capacitor, it is characterised in that three-dimensional stone
The preparation method of black alkene/carbon/polyaniline super capacitor electrode material is carried out according to the following steps:
First, three-dimensional grapheme is prepared:Be put in nickel foam as template in tube furnace, argon gas and hydrogen as carrier gas, by tubular type
Stove from room temperature be heated to 900 ~ 1100 DEG C insulation 30 ~ 60 min, and temperature be 900 ~ 1100 DEG C when to stove in 10 ~ 20
The speed of sccm is passed through the min of methane gas 5 ~ 10, tube furnace then is cooled into room temperature with the speed of 80 ~ 100 DEG C/min, so
The nickel foam that obtained Graphene is wrapped up is cut into the cm of area 1 ' 1 afterwards2Square, and by poly- methyl that mass fraction is 4%
Methyl acrylate solution drips to Graphene parcel foam nickel surface by 100 ~ 150 mL consumptions every square centimeter, is protected at 200 DEG C
30 ~ 60 min of temperature, make Graphene wrap up the polymethyl methacrylate solution solidification drying of foam nickel surface, are then soaked
It it is 60 ~ 90 DEG C to temperature, concentration is 3 ~ 12 h in the hydrochloric acid solution of 3 ~ 4 mol/L, removes nickel foam therein, reusable heat third
Ketone solution removes polymethyl methacrylate therein, and is cleaned up repeatedly with deionized water, obtains three-dimensional grapheme, then
The three-dimensional grapheme that will be cleaned up soaks 12 ~ 18 h in being moved into concentrated nitric acid solution, obtains the three-dimensional grapheme being slightly acidified;
2nd, in-situ polymerization prepares polyaniline array:Aniline monomer and ammonium persulfate are added separately to 1 isometric mol/L's
In sulfuric acid solution, 30 ~ 60 min are stirred at room temperature is completely dissolved it, the three-dimensional stone of the slight acidifying for then obtaining step one
Black alkene is placed on slide, and is dipped in 1 ~ 3 h in aniline solution, aniline monomer is connect completely with three-dimensional grapheme
Touch, 30 ~ 60 s are slowly stirred during ammonium persulfate solution finally is heated into aniline solution under condition of ice bath, then allow it in ice
0 ~ 24 h is reacted under the conditions of bath, three-dimensional grapheme/polyaniline array composite is obtained, composite is cleaned with deionized water
Totally, it is placed on and dries 6 ~ 12 h in vacuum drying chamber at 80 ~ 100 DEG C, obtains three-dimensional grapheme/polyaniline array and be combined
Material.
2. the preparation side of a kind of three-dimensional grapheme/polyaniline array electrode material for super capacitor according to claim 1
Method, it is characterised in that tube furnace is heated to 900 ~ 1100 DEG C, argon gas with the heating rate of 10 DEG C/min from room temperature in step one
500 sccm and 200sccm are respectively with the flow of hydrogen.
3. the preparation side of a kind of three-dimensional grapheme/polyaniline array electrode material for super capacitor according to claim 1
Method, it is characterised in that the aniline monomer and the mol ratio of persulfuric acid weighed in step 2 are 4:1, ice bath temperature is 0 ~ -5 DEG C.
4. the application of a kind of three-dimensional grapheme/polyaniline array electrode material for super capacitor, it is characterised in that three-dimensional grapheme/
Polyaniline array composite is used as electrode material for super capacitor.
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CN108428864A (en) * | 2018-03-02 | 2018-08-21 | 合肥国轩高科动力能源有限公司 | A kind of sulphur carbon composite anode material and preparation method thereof |
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