CN105185600A - Method of preparing graphite electrode material by electrophoresis method - Google Patents
Method of preparing graphite electrode material by electrophoresis method Download PDFInfo
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- CN105185600A CN105185600A CN201510622106.XA CN201510622106A CN105185600A CN 105185600 A CN105185600 A CN 105185600A CN 201510622106 A CN201510622106 A CN 201510622106A CN 105185600 A CN105185600 A CN 105185600A
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Abstract
The present invention relates to a method of preparing a graphite electrode material by an electrophoresis method. The method comprises the steps of dispersing the graphite oxide in the water, carrying out an ultrasonic operation to obtain a graphite oxide solution; connecting a silver wire with a working electrode and then placing in the graphite oxide solution, by taking a platinum electrode as a counter electrode and the Ag/AgCl as a reference electrode, carrying out the constant voltage electrophoretic deposition to obtain a graphene oxide hydrogel; dipping the graphene oxide hydrogel in the sodium sulfate, taking out and carrying out the photo-reduction to obtain the graphite electrode material. The preparation method of the present invention is simple, has low requirements for production equipment, and is easy for the industrial production. The prepared graphite electrode material is high in conductivity, large in specific capacitance and stable in chemical property.
Description
Technical field
The invention belongs to the preparation field of electrode material, particularly a kind of method of electrophoretic preparation Graphene electrodes material.
Background technology
Graphene is known the thinnest at present, the two-dimension nano materials that hardness is maximum, and since Graphene comes out, it has just attracted the concern of numerous scholar with excellent mechanical performance and electric property.Research shows, Graphene at normal temperatures charge mobility is greater than 1500cm
2/ Vs, resistivity approximately only has 1 Ω m.Therefore, Graphene is the ideal material preparing graphene-based electrode material for super capacitor.
At present, the preparation method of Graphene mainly contains electronation graphite oxide method, thermal reduction graphene oxide method, Graphene water-gel method and activation Graphene method.Electronation graphite oxide method is the production method of current main flow, obtains Graphene electrodes in this way and has higher chemical property and high-specific surface area, but compared with theoretical value, performance still has greatly improved space.Thermal reduction graphene oxide method obtains reproducibility grapheme material by hot soarfing from the mode of graphite oxide.The Graphene specific area obtained by the method is 925m to the maximum
2/ g, under the potential scan rate of 100mV/s, ratio capacitance is approximately 120F/g.The maximum difficult problem of this technology is that high temperature is peeled off restive, and energy resource consumption is large.Graphene water-gel method utilizes reducing agent to reduce in graphite oxide suspension, is obtained by reacting three-dimensional self assembly Graphene hydrogel.Product inside is three-dimensional net structure, and be evenly distributed, pore size is between submicron order is to several microns, and product conductivity is excellent, and mechanical performance is strong.Activation Graphene method is activated by carbon nanomaterial with electrochemical techniques or chemical modification method, and the material through overactivation greatly adds specific surface and ratio capacitance.Although the Graphene function admirable that two kinds of methods next obtain, because technology is complicated, cannot directly industrially produce on a large scale.
Therefore, find one and prepare high conductivity, high-specific surface area, high stability, the method of the graphene-based electrode material of low cost improves the research emphasis of ultracapacitor electric capacity, not yet sees the report of the method preparing Graphene electrodes material with electrophoresis on filamentary silver at present.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of electrophoretic preparation Graphene electrodes material, and graphene-based electrode material conductivity prepared by the method is high, and ratio capacitance is large, stable chemical performance.
The method of a kind of electrophoretic preparation Graphene electrodes material of the present invention, comprising:
(1) graphite oxide is scattered in water, ultrasonic, obtain graphite oxide solution;
(2) filamentary silver is connected the graphite oxide solution being placed in step (1) with work electrode, be to electrode, Ag/AgCl for reference electrode with platinum electrode, constant voltage electrophoretic deposition obtains graphene oxide hydrogel; Wherein, voltage is 4 ~ 8V;
(3) be immersed in sodium sulphate by the graphene oxide hydrogel in step (2), take out, photo-reduction, obtains Graphene electrodes material.
In described step (1), ultrasonic time is 0.5 ~ 3h.
In described step (1), the concentration of graphite oxide solution is 0.5 ~ 4mg/mL.
The time of described step (2) electrophoretic deposition is 2 ~ 5min.
In described step (3), the concentration of metabisulfite solution is 1mol/L, and soak time is 1h.
In described step (3), photo-reduction is Xenon light shining reduction, and the recovery time is 6 ~ 12h.
Grapheme material prepared by the electrophoresis that the present invention sets forth has excellent mechanical property and electric property, meets the performance requirement of electrode material for super capacitor.
By regulating graphene solution concentration and the electrophoretic deposition time of variable concentrations, the graphene-based electrode material of different quality can be obtained.
beneficial effect
Preparation method of the present invention is simple, requires low, be easy to suitability for industrialized production to production equipment; The Graphene electrodes material electric conductivity prepared is high, and ratio capacitance is large, stable chemical performance.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that in invention, three-electrode method prepares Graphene electrodes material;
Fig. 2 is the Graphene electrodes material that in embodiment 1, electrophoretic deposition obtains;
Fig. 3 is the SEM picture of the Graphene electrodes material of preparation in embodiment 1;
Fig. 4 is the cyclic voltammetry curve of Graphene electrodes material in embodiment 1;
Fig. 5 is the SEM picture of Graphene electrodes material in embodiment 2.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Take 0.20g graphite oxide under room temperature, add the solution that 100mL deionized water obtains 2mg/mL, ultrasonic process 2h forms finely dispersed solution.Choose the long 5cm of filamentary silver that diameter is 0.5mm, with three electrode method (as Fig. 1) on electrochemical workstation CHI760, add constant voltage 8V, the electrophoretic deposition time is 2min, obtains graphene oxide hydrogel.The graphene oxide hydrogel obtained is taken out the metabisulfite solution 1h being immersed in 1mol/L, take out under being placed on xenon lamp and carry out photo-reduction 6h, obtain Graphene electrodes material (as Fig. 2).Fig. 3 is the scanning electron microscopic picture of Graphene electrodes material prepared by the present embodiment, can find out: the pattern entirety of Graphene presents buckle condition, smooth surface is smooth without obscission, show that mechanical strength is good, trickle hole is there is in depths, gully, aperture is approximately 10 μm, is conducive to electrolyte and enters into material internal structure, gives full play to electric double layer performance.Fig. 4 is the cyclic voltammetry curve figure preparing electrode material, can find out: this Graphene electrodes material exists redox peak in the process of charging and discharging, illustrates that it has very high charge storage, by calculating ratio capacitance C=218.8F/g.
Embodiment 2
Take 0.20g graphite oxide under room temperature, add the solution that 100mL deionized water obtains 2mg/mL, ultrasonic process 2h forms finely dispersed solution.Choose the long 5cm of filamentary silver that diameter is 0.5mm, with three electrode method (as Fig. 1) on electrochemical workstation CHI760, add constant voltage 4V, the electrophoretic deposition time is 2min, obtains graphene oxide hydrogel.The graphene oxide hydrogel obtained is taken out the metabisulfite solution 1h being immersed in 1mol/L, take out under being placed on xenon lamp and carry out photo-reduction 6h, obtain Graphene electrodes material.Fig. 5 is the scanning electron microscopic picture of Graphene electrodes material prepared by the present embodiment, can find out: the pattern entirety of Graphene presents buckle condition, relative example 1 (Fig. 3), graphene film Rotating fields stacking loose, easily come off, it can thus be appreciated that the voltage Gao Shihui of electrophoretic deposition obtains the Graphene electrodes material that structure is better, performance is more stable.
Claims (6)
1. a method for electrophoretic preparation Graphene electrodes material, comprising:
(1) graphite oxide is scattered in water, ultrasonic, obtain graphite oxide solution;
(2) filamentary silver is connected the graphite oxide solution being placed in step (1) with work electrode, be to electrode, Ag/AgCl for reference electrode with platinum electrode, constant voltage electrophoretic deposition obtains graphene oxide hydrogel; Wherein, voltage is 4 ~ 8V;
(3) be immersed in sodium sulphate by the graphene oxide hydrogel in step (2), take out, photo-reduction, obtains Graphene electrodes material.
2. the method for a kind of electrophoretic preparation Graphene electrodes material according to claim 1, is characterized in that, in described step (1), ultrasonic time is 0.5 ~ 3h.
3. the method for a kind of electrophoretic preparation Graphene electrodes material according to claim 1, is characterized in that, in described step (1), the concentration of graphite oxide solution is 0.5 ~ 4mg/mL.
4. the method for a kind of electrophoretic preparation Graphene electrodes material according to claim 1, is characterized in that, the time of described step (2) electrophoretic deposition is 2 ~ 5min.
5. the method for a kind of electrophoretic preparation Graphene electrodes material according to claim 1, is characterized in that, in described step (3), the concentration of metabisulfite solution is 1mol/L, and soak time is 1h.
6. the method for a kind of electrophoretic preparation Graphene electrodes material according to claim 1, is characterized in that, in described step (3), photo-reduction is Xenon light shining reduction, and the recovery time is 6 ~ 12h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106596682A (en) * | 2016-12-28 | 2017-04-26 | 上海应用技术大学 | Go-Nafion composite film Ag/AgCl reference electrode for ocean exploration and preparation method thereof |
| 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 |
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| CN103219163A (en) * | 2013-04-15 | 2013-07-24 | 苏州大学 | Super capacitor fiber electrode and manufacturing method thereof |
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| 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 |
| 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 |
| 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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Patent Citations (7)
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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 |
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| 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 |
| 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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| CN106596682A (en) * | 2016-12-28 | 2017-04-26 | 上海应用技术大学 | Go-Nafion composite film Ag/AgCl reference electrode for ocean exploration and preparation method thereof |
| 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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| CN105185600B (en) | 2018-05-15 |
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