CN105185600B - A kind of method that electrophoresis prepares Graphene electrodes material - Google Patents
A kind of method that electrophoresis prepares Graphene electrodes material Download PDFInfo
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- CN105185600B CN105185600B CN201510622106.XA CN201510622106A CN105185600B CN 105185600 B CN105185600 B CN 105185600B CN 201510622106 A CN201510622106 A CN 201510622106A CN 105185600 B CN105185600 B CN 105185600B
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Abstract
The present invention relates to a kind of method that electrophoresis prepares Graphene electrodes material, including：Graphite oxide is dispersed in water, ultrasound, obtains graphite oxide solution；Filamentary silver is connected with working electrode and is placed in graphite oxide solution, is that constant voltage electrophoretic deposition obtains graphene oxide hydrogel as reference electrode to electrode, Ag/AgCl using platinum electrode；Graphene oxide hydrogel is immersed in sodium sulphate, is taken out, photo-reduction, to obtain the final product.The preparation method of the present invention is simple, low to production equipment requirement, is easy to industrialized production；The Graphene electrodes material electric conductivity being prepared is high, and specific capacitance is big, stable chemical performance.
Description
Technical field
The invention belongs to the preparation field of electrode material, more particularly to a kind of electrophoresis prepares the side of Graphene electrodes material
Method.
Background technology
Graphene is to be currently known most thin, the two-dimension nano materials of hardness maximum, and since graphene comes out, it is just with excellent
Good mechanical performance and electric property has attracted the concern of numerous scholars.Research shows, graphene charge mobility at normal temperatures
More than 1500cm2/ Vs, resistivity only about 1 Ω m.Therefore, graphene is to prepare graphene-based electrode of super capacitor
The ideal material of material.
At present, the preparation method of graphene mainly has electronation graphite oxide method, thermal reduction graphene oxide method, graphite
Alkene water-gel method and activated graphene method.Electronation graphite oxide method is the production method of current mainstream, in this way
Obtain Graphene electrodes and possess higher chemical property and high-specific surface area, but compared with theoretical value, still have in performance
Very big room for promotion.It is that reproducibility graphene material is obtained by way of hot soarfing is from graphite oxide to heat-treat graphene oxide method
Material.The graphene specific surface area obtained with this method is up to 925m2/ g, under the potential scan rate of 100mV/s, specific capacitance
About 120F/g.The problem of technology maximum is that high temperature stripping is difficult to control, and energy consumption is big.Graphene water-gel method is
Reduced using reducing agent in graphite oxide suspension, reaction obtains three-dimensional self assembly graphene hydrogel.Inside product
For three-dimensional net structure, it is evenly distributed, pore size is in submicron order between a few micrometers, and product electrical conductivity is excellent, mechanicalness
Can be strong.Activated graphene method is to be activated carbon nanomaterial with electrochemical techniques or chemical modification method, the material pole through overactivation
Add than surface and specific capacitance greatly.The graphene function admirable that below although two methods obtain, but due to technology
Complexity, can not directly industrially be produced on a large scale.
Therefore, find one kind and prepare high conductivity, high-specific surface area, high stability, inexpensive graphene-based electrode material
The method of material is to improve the research emphasis of ultracapacitor capacitance, not yet sees prepare graphite on filamentary silver with electrophoresis at present
The report of the method for alkene electrode material.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method that electrophoresis prepares Graphene electrodes material, this method
The graphene-based electrode material electrical conductivity prepared is high, and specific capacitance is big, stable chemical performance.
The method that a kind of electrophoresis of the present invention prepares Graphene electrodes material, including：
(1) graphite oxide is dispersed in water, ultrasound, obtains graphite oxide solution；
(2) filamentary silver is connected with working electrode and be placed in the graphite oxide solution in step (1), using platinum electrode as to electricity
Pole, Ag/AgCl are reference electrode, and constant voltage electrophoretic deposition obtains graphene oxide hydrogel；Wherein, voltage is 4~8V；
(3) the graphene oxide hydrogel in step (2) is immersed in sodium sulphate, taken out, photo-reduction, obtains graphene
Electrode material.
Ultrasonic time is 0.5~3h in the step (1).
The concentration of graphite oxide solution is 0.5~4mg/mL in the step (1).
The time of step (2) electrophoretic deposition is 2~5min.
The concentration of metabisulfite solution is 1mol/L, soaking time 1h in the step (3).
Photo-reduction reduces for Xenon light shining in the step (3), and the recovery time is 6~12h.
Grapheme material prepared by the electrophoresis that the present invention illustrates has excellent mechanical property and electric property, meets super
The performance requirement of level capacitor electrode material.
By adjusting graphene solution concentration and the electrophoretic deposition time of various concentrations, the graphene of different qualities can obtain
Base electrode material.
Beneficial effect
The preparation method of the present invention is simple, low to production equipment requirement, is easy to industrialized production；The graphene being prepared
Electrode material electrical conductivity is high, and specific capacitance is big, stable chemical performance.
Brief description of the drawings
Fig. 1 is the schematic diagram that three-electrode method prepares Graphene electrodes material in invention；
Fig. 2 is the Graphene electrodes material that electrophoretic deposition obtains in embodiment 1；
Fig. 3 is the SEM pictures of the Graphene electrodes material prepared in embodiment 1；
Fig. 4 is the cyclic voltammetry curve of Graphene electrodes material in embodiment 1；
Fig. 5 is the SEM pictures of Graphene electrodes material in embodiment 2.
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
0.20g graphite oxides are weighed at room temperature, are added 100mL deionized waters and are obtained the solution of 2mg/mL, are ultrasonically treated 2h
Form finely dispersed solution.The long 5cm of filamentary silver of a diameter of 0.5mm is chosen, with three electrodes on electrochemical workstation CHI760
Method (such as Fig. 1), add constant voltage 8V, the electrophoretic deposition time is 2min, obtains graphene oxide hydrogel.The oxygen that will be obtained
Graphite alkene hydrogel takes out the metabisulfite solution 1h for being immersed in 1mol/L, and taking-up is placed on progress photo-reduction 6h under xenon lamp, obtains
To Graphene electrodes material (such as Fig. 2).Fig. 3 is the scanning electron microscopic picture of Graphene electrodes material manufactured in the present embodiment, can be with
Find out：Buckle condition is integrally presented in the pattern of graphene, and the smooth no obscission in surface, shows that mechanical strength is good,
There are trickle hole, aperture is about 10 μm for gully depths, is conducive to electrolyte and enters material internal structure, is given full play to double
Electric layer performance.Fig. 4 is the cyclic voltammetry curve figure for preparing electrode material, it can be seen that：The Graphene electrodes material charging and
The process of electric discharge illustrates that it has very high charge storage, specific capacitance C=is obtained by calculation there are redox peaks
218.8F/g。
Embodiment 2
0.20g graphite oxides are weighed at room temperature, are added 100mL deionized waters and are obtained the solution of 2mg/mL, are ultrasonically treated 2h
Form finely dispersed solution.The long 5cm of filamentary silver of a diameter of 0.5mm is chosen, with three electrodes on electrochemical workstation CHI760
Method (such as Fig. 1), add constant voltage 4V, the electrophoretic deposition time is 2min, obtains graphene oxide hydrogel.The oxygen that will be obtained
Graphite alkene hydrogel takes out the metabisulfite solution 1h for being immersed in 1mol/L, and taking-up is placed on progress photo-reduction 6h under xenon lamp, obtains
To Graphene electrodes material.Fig. 5 is the scanning electron microscopic picture of Graphene electrodes material manufactured in the present embodiment, it can be seen that：Stone
Buckle condition is integrally presented in the pattern of black alkene, and with respect to example 1 (Fig. 3), the stacking of graphene film Rotating fields is loose, easily comes off,
The Graphene electrodes material that structure is preferable, performance is more stable it follows that the voltage Gao Shihui of electrophoretic deposition is obtained.
Claims (6)
1. a kind of method that electrophoresis prepares Graphene electrodes material, including：
(1) graphite oxide is dispersed in water, ultrasound, obtains graphite oxide solution；
(2) filamentary silver is connected with working electrode and be placed in the graphite oxide solution in step (1), using platinum electrode as to electrode, Ag/
AgCl is reference electrode, and constant voltage electrophoretic deposition obtains graphene oxide hydrogel；Wherein, voltage is 4~8V；
(3) the graphene oxide hydrogel in step (2) is immersed in sodium sulphate, taken out, photo-reduction, obtains Graphene electrodes
Material.
2. the method that a kind of electrophoresis according to claim 1 prepares Graphene electrodes material, it is characterised in that the step
(1) ultrasonic time is 0.5~3h in.
3. the method that a kind of electrophoresis according to claim 1 prepares Graphene electrodes material, it is characterised in that the step
(1) concentration of graphite oxide solution is 0.5~4mg/mL in.
4. the method that a kind of electrophoresis according to claim 1 prepares Graphene electrodes material, it is characterised in that the step
(2) time of electrophoretic deposition is 2~5min.
5. the method that a kind of electrophoresis according to claim 1 prepares Graphene electrodes material, it is characterised in that the step
(3) concentration of metabisulfite solution is 1mol/L, soaking time 1h in.
6. the method that a kind of electrophoresis according to claim 1 prepares Graphene electrodes material, it is characterised in that the step
(3) photo-reduction reduces for Xenon light shining in, and the recovery time is 6~12h.
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| CN106596682B (en) * | 2016-12-28 | 2019-03-19 | 上海应用技术大学 | A kind of hydrospace detection Go-Nafion composite membrane Ag/AgCl reference electrode and preparation method |
| CN111261418A (en) * | 2020-01-21 | 2020-06-09 | 江苏大学 | Method for preparing high-purity graphene film, electrode and capacitor |
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| CN102051651A (en) * | 2011-01-11 | 2011-05-11 | 湖南大学 | Preparation method of graphene film |
| CN102560415A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院上海硅酸盐研究所 | Three-dimensional graphene/metal line or metal wire composite structure and preparation method thereof |
| CN103219163A (en) * | 2013-04-15 | 2013-07-24 | 苏州大学 | Super capacitor fiber electrode and manufacturing method thereof |
| CN103436939A (en) * | 2013-08-19 | 2013-12-11 | 南京航空航天大学 | Foam metal-graphene composite material and preparation method thereof |
| CN104036969A (en) * | 2014-06-27 | 2014-09-10 | 西南大学 | Novel battery super capacitor electrode material with high power density and high energy density and preparing method thereof |
| CN104451925A (en) * | 2014-11-21 | 2015-03-25 | 东华大学 | Water-soluble polymer/graphene composite fiber as well as preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140137471A (en) * | 2013-05-21 | 2014-12-03 | 인제대학교 산학협력단 | Electrochemical method of graphene oxide deposition, graphene oxide deposited substrate made by the same, and electric device including the same |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051651A (en) * | 2011-01-11 | 2011-05-11 | 湖南大学 | Preparation method of graphene film |
| CN102560415A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院上海硅酸盐研究所 | Three-dimensional graphene/metal line or metal wire composite structure and preparation method thereof |
| CN103219163A (en) * | 2013-04-15 | 2013-07-24 | 苏州大学 | Super capacitor fiber electrode and manufacturing method thereof |
| CN103436939A (en) * | 2013-08-19 | 2013-12-11 | 南京航空航天大学 | Foam metal-graphene composite material and preparation method thereof |
| CN104036969A (en) * | 2014-06-27 | 2014-09-10 | 西南大学 | Novel battery super capacitor electrode material with high power density and high energy density and preparing method thereof |
| CN104451925A (en) * | 2014-11-21 | 2015-03-25 | 东华大学 | Water-soluble polymer/graphene composite fiber as well as preparation method and application thereof |
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