CN104947134A - Preparation method of porous graphene - Google Patents
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Abstract
The invention relates to a preparation method of porous graphene. The method includes the steps of dispersing graphene and graphene oxide in a phosphate buffer to obtain a mixture of graphene and graphene oxide, and conducting cyclic voltammetry scan on the mixture of graphene and graphene oxide through a three-electrode system so that a working electrode for decorating the porous graphene can be obtained, that is, the porous graphene can be obtained on the working electrode. The method is easy to operate, few in steps, rapid and low in cost.
Description
Technical field
The present invention relates to the method preparing Graphene, particularly a kind of method preparing porous graphene.
Background technology
Graphene is a kind of Two-dimensional Carbon material, it is the general designation of single-layer graphene, bilayer graphene and few layer graphene, due to the electronics of its excellence, machinery and thermal stability, the application in battery, ultracapacitor, electron device, sensor and matrix material etc. obtains the extensive concern of people.
Graphene oxide (graphene oxide) is the oxide compound of Graphene, and on graphene oxide, oxygen-containing functional group increases and makes its character more active than Graphene.
Porous graphene is a kind of Graphene of three-dimensional structure, because it has the specific surface area larger compared with Graphene, is conducive to charge capacity and catalysis; Its vesicular structure contributes to improving material mass transfer, becomes rapidly the study hotspot of the aspects such as battery, ultracapacitor, electron device, sensor and matrix material at present.
The method preparing porous graphene at present mainly contains: the methods such as solution self-assembly method, interface self-assembly method, template mediation synthesis method, but the operation of these methods is more complicated, and condition is difficult to accurate control.
Summary of the invention
Based on this, the invention provides a kind of simple to operate, step is few, the method preparing porous graphene of quick, low cost.
The preparation method of porous graphene of the present invention, comprises step:
Graphene and graphene oxide are dispersed in phosphate buffer solution, obtain the mixed solution of Graphene and graphene oxide;
With the first electrode for working electrode, adopt the mixed solution of three-electrode system to described Graphene and graphene oxide to carry out cyclic voltammetry scan, obtain the working electrode that porous graphene is modified, obtain porous graphene.
The preparation method of above-mentioned porous graphene, electrochemical method is adopted to make the graphene oxide in Graphene and graphene oxide liquid mixture be reduced to Graphene, original Graphene reconstructs and obtains porous graphene simultaneously and in mixed solution, operation steps is simple, efficiency is high, environmental protection, the porous graphene specific surface area obtained is large, active high.
Wherein, the pH value of described phosphate buffer solution is 4-6.
Wherein, described first electrode is any one in gold electrode, platinum electrode, glass-carbon electrode, Graphite Electrodes, carbon fiber electrode, carbon cloth electrode and carbon paste electrode.
Wherein, described Graphene be Graphene, any one in the Graphene that obtained by the on-the-spot redox graphene in real time of chemical reducing agent or biological reductant original position.
Wherein, described with the first electrode for working electrode, adopt the mixed solution of three-electrode system to described Graphene and graphene oxide to carry out cyclic voltammetry scan, the concrete steps obtaining the working electrode that porous graphene is modified are:
The mixed solution of described Graphene and graphene oxide is added drop-wise on described first electrode, dry, again with described first electrode be working electrode, to electrode be platinum plate electrode, reference electrode is for saturated calomel electrode, be placed in blank phosphate buffer solution (pH value is 4-6) and carry out cyclic voltammetry scan, obtain the working electrode that described porous graphene is modified.
Wherein, adopt the mixed solution of three-electrode system to described Graphene and graphene oxide to carry out cyclic voltammetry scan, the concrete steps obtaining the working electrode that porous graphene is modified also can be:
With the first electrode be working electrode, to electrode be platinum plate electrode, reference electrode for saturated calomel electrode, the mixed solution being placed in described Graphene and graphene oxide carries out cyclic voltammetry scan, obtain described porous graphene modify working electrode.
Wherein, described with the first electrode for working electrode, the scanning current potential adopting the mixed solution of three-electrode system to described Graphene and graphene oxide to carry out cyclic voltammetry scan is 0 V to-2.0 V, and sweep velocity is 10-500mV/s.
The preparation method of above-mentioned porous graphene, electrochemical method is adopted to make the graphene oxide in Graphene and graphene oxide liquid mixture be reduced to Graphene, original Graphene reconstructs and obtains porous graphene simultaneously and in mixed solution, operation steps is simple, efficiency is high, environmental protection, the porous graphene specific surface area obtained is large, active high.
Accompanying drawing explanation
Fig. 1 is the step schematic diagram of the preparation method of the porous graphene of an embodiment;
Fig. 2 is the scanning electron microscope (SEM) photograph of the porous graphene that embodiment 1 obtains.
Embodiment
For the ease of understanding the present invention, below with reference to related embodiment and accompanying drawing, the present invention is described more fully.Shown below is preferred embodiment of the present invention.But the present invention can realize in many different forms, is not limited to embodiment described herein.On the contrary, provide the object of these embodiments be make the understanding of disclosure of the present invention more comprehensively thorough.
With reference to Fig. 1, the preparation method of a kind of porous graphene of the present invention, comprising:
Step S100: by graphene oxide and graphene dispersion in phosphate buffer solution, obtain the mixed solution of Graphene and graphene oxide.
Wherein in an embodiment, step S100 is specially: be dispersed in phosphate buffer solution by Graphene and graphene oxide, the concentration of Graphene in phosphate buffer solution is 1mg/mL, graphene oxide and the Graphene concentration ratio in phosphate buffer solution is 1:50-5:1, obtains the mixed solution of Graphene and graphene oxide.
Wherein in an embodiment, the pH value of phosphate buffer solution is 4-6.
Wherein in an embodiment, graphene oxide adopts Hummers legal system standby, and Hummers legal system is classical way for graphene oxide, the graphene oxide reliable in quality of preparation.Graphene is obtained by the graphene oxide that hydrazine hydrate reduction Hummers legal system is standby, and this method is classical way, the Graphene reliable in quality of preparation.
Step S200: with the first electrode for working electrode, adopts the mixed solution of three-electrode system to Graphene and graphene oxide to carry out cyclic voltammetry scan, obtains the working electrode that porous graphene is modified.
Step S200 is in cyclic voltammetry scan, and scanning current potential reaches the reduction potential of graphene oxide, and repeatedly cyclic voltammetry scan obtains the working electrode of porous graphene modification subsequently.
Wherein in an embodiment, the first electrode is any one in gold electrode, platinum electrode, glass-carbon electrode, Graphite Electrodes, carbon fiber electrode, carbon cloth electrode and carbon paste electrode.
Preferably, the first electrode is glass-carbon electrode.Wherein in an embodiment, glass-carbon electrode is carried out polishing with alumina powder on polishing cloth, clean for subsequent use in ultrasonic cleaner with dehydrated alcohol and water successively.
Wherein in an embodiment, the concrete steps of step S200 are: be added drop-wise on the first electrode by the mixed solution of Graphene and graphene oxide, dry, again with the first electrode be working electrode, to electrode be platinum plate electrode, reference electrode is for saturated calomel electrode, be placed in the blank phosphate buffer solution (pH value is 4-6) of 0.1M and carry out cyclic voltammetry scan, obtain the working electrode that porous graphene is modified.
Wherein, wherein in an embodiment, the electrolyte solution in step S200 is phosphate buffer solution.The concentration of preferred phosphate buffer solution is 0.1mol/L.
In another embodiment, the concrete steps of step S200 are: with the first electrode be working electrode, to electrode be platinum plate electrode, reference electrode is for saturated calomel electrode, the mixed solution being placed in Graphene and graphene oxide carries out cyclic voltammetry scan, obtains the working electrode that porous graphene is modified.
Wherein in an embodiment, with the first electrode for working electrode, the scanning current potential adopting the mixed solution of three-electrode system to Graphene and graphene oxide to carry out cyclic voltammetry scan is 0 V to-2.0 V, and sweep velocity is 10-500mV/s.Preferably, sweep velocity is 50mV/s.
The preparation method of above-mentioned porous graphene, electrochemical method is adopted to make the graphene oxide in Graphene and graphene oxide liquid mixture be reduced to Graphene, original Graphene reconstructs and obtains porous graphene simultaneously and in mixed solution, operation steps is simple, efficiency is high, environmental protection, the porous graphene specific surface area obtained is large, active high.
It is below specific embodiment.
Embodiment 1
Graphene and graphene oxide being dispersed in pH value is in the phosphate buffer solution of 4, the concentration of Graphene in 0.1mol/L phosphate buffer solution is 1mg/mL, the concentration of graphene oxide in phosphate buffer solution is 1mg/mL, obtains Graphene and graphene oxide liquid mixture.
Take glass-carbon electrode as working electrode, Graphene and graphene oxide liquid mixture dispersion are added drop-wise on glass-carbon electrode, dry, again with the glass-carbon electrode modified be working electrode, to electrode be platinum plate electrode, reference electrode is for saturated calomel electrode, be placed in 0.1mol/L pH value be 4 blank phosphate buffer solution carry out cyclic voltammetry scan, scanning current potential is 0 V to-2.0 V, and sweep velocity is 50mV/s, obtain the working electrode that porous graphene is modified, namely obtain porous graphene on the working electrode (s.
Embodiment 2
With the difference of embodiment 1, embodiment 2 is that the concentration of Graphene is 0.1 mg/mL, the pH value of phosphate buffer solution is 5, with Graphite Electrodes be working electrode, to electrode be platinum plate electrode, reference electrode is saturated calomel electrode, be placed in 0.1mol/L pH value be 5 blank phosphate buffer solution carry out cyclic voltammetry scan, scanning current potential is 0 V to-2.0 V, sweep velocity is 50mV/s, obtains the working electrode that porous graphene is modified, namely obtains porous graphene on the working electrode (s.
Embodiment 3
With the difference of embodiment 1, embodiment 3 is that the concentration of Graphene is 0.05 mg/mL, the pH value of phosphate buffer solution is 6, with carbon cloth electrode be working electrode, to electrode be platinum plate electrode, reference electrode is saturated calomel electrode, be placed in 0.1mol/L pH value be 6 blank phosphate buffer solution carry out cyclic voltammetry scan, scanning current potential is 0 V to-2.0 V, sweep velocity is 50mV/s, obtains the working electrode that porous graphene is modified, namely obtains porous graphene on the working electrode (s.
Embodiment 4
Embodiment 4 and the difference of embodiment 1 are that Graphene is the Graphene obtained by the on-the-spot redox graphene in real time of xitix original position.Be specially: graphene oxide being dispersed in pH value is in the 0.1mol/L phosphate buffer solution of 4, the concentration of graphene oxide in phosphate buffer solution is 2mg/mL, then under the condition stirred, add the xitix reaction half an hour that ultimate density is 1mg/mL, obtain Graphene and graphene oxide liquid mixture.With glass-carbon electrode be working electrode, to electrode be platinum plate electrode, reference electrode is saturated calomel electrode, be placed in gained Graphene and graphene oxide liquid mixture carries out cyclic voltammetry scan, scanning current potential is 0 V to-2.0 V, sweep velocity is 50mV/s, obtain the working electrode that porous graphene is modified, namely obtain porous graphene on the working electrode (s.
Embodiment 5
Embodiment 5 and the difference of embodiment 1 are that Graphene is the Graphene obtained by the on-the-spot redox graphene in real time of sodium borohydride original position, be specially: graphene oxide being dispersed in pH value is in the 0.1mol/L phosphate buffer solution of 5, the concentration of graphene oxide in phosphate buffer solution is 2mg/mL, then under the condition stirred, add the sodium borohydride reaction half an hour that ultimate density is 1mg/mL, obtain Graphene and graphene oxide liquid mixture.With Graphite Electrodes be working electrode, to electrode be platinum plate electrode, reference electrode is saturated calomel electrode, be placed in gained Graphene and graphene oxide liquid mixture carries out cyclic voltammetry scan, scanning current potential is 0 V to-2.0 V, sweep velocity is 50mV/s, obtain the working electrode that porous graphene is modified, namely obtain porous graphene on the working electrode (s.
The porous graphene that embodiment 1 obtains is made sem test, obtains scanning electron microscope (SEM) photograph as shown in Figure 2.As shown in Figure 2, the specific surface area of gained porous graphene is large.
Each technical characteristic of the above embodiment can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics does not exist contradiction, be all considered to be the scope that this specification sheets is recorded.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (6)
1. a preparation method for porous graphene, is characterized in that comprising step is:
Graphene and graphene oxide are dispersed in phosphate buffer solution, obtain the mixed solution of Graphene and graphene oxide;
With the first electrode for working electrode, adopt the mixed solution of three-electrode system to described Graphene and graphene oxide to carry out cyclic voltammetry scan, obtain the working electrode that porous graphene is modified, obtain porous graphene.
2. the preparation method of porous graphene according to claim 1, is characterized in that, the pH value of described phosphate buffer solution is 4-6.
3. the preparation method of porous graphene according to claim 1, is characterized in that, described first electrode is any one in gold electrode, platinum electrode, glass-carbon electrode, Graphite Electrodes, carbon fiber electrode, carbon cloth electrode and carbon paste electrode.
4. the preparation method of porous graphene according to claim 1, is characterized in that, described Graphene is Graphene, any one in the Graphene that obtained by the on-the-spot redox graphene in real time of chemical reducing agent or biological reductant original position.
5. the preparation method of porous graphene according to claim 1, it is characterized in that, described with the first electrode for working electrode, adopt the mixed solution of three-electrode system to described Graphene and graphene oxide to carry out cyclic voltammetry scan, the concrete steps obtaining the working electrode that porous graphene is modified are:
The mixed solution of described Graphene and graphene oxide is added drop-wise on described first electrode, dry, again with described first electrode be working electrode, to electrode be platinum plate electrode, reference electrode is for saturated calomel electrode, being placed in pH value is that the blank phosphate buffer solution of 4-6 carries out cyclic voltammetry scan, obtains the working electrode that described porous graphene is modified.
6. the preparation method of porous graphene according to claim 1, it is characterized in that, described with the first electrode for working electrode, adopt the mixed solution of three-electrode system to described Graphene and graphene oxide to carry out cyclic voltammetry scan, the concrete steps obtaining the working electrode that porous graphene is modified are:
With the first electrode be working electrode, to electrode be platinum plate electrode, reference electrode for saturated calomel electrode, the mixed solution being placed in described Graphene and graphene oxide carries out cyclic voltammetry scan, obtain described porous graphene modify working electrode.
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| CN107271505A (en) * | 2017-06-01 | 2017-10-20 | 赵云飞 | Composite electrode and preparation method thereof, Quercetin sensor |
| CN110453260A (en) * | 2019-08-23 | 2019-11-15 | 厦门大学 | A kind of wearable sensors and preparation method thereof for sweat detection |
| CN114324545A (en) * | 2022-01-07 | 2022-04-12 | 三只松鼠股份有限公司 | Reduced graphene oxide sensor, preparation method thereof and method for rapidly detecting capsaicin content |
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| CN106978606A (en) * | 2016-11-30 | 2017-07-25 | 哈尔滨工业大学（威海） | A kind of high heat conduction graphene/titanium composite material and preparation method thereof |
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| CN107083557A (en) * | 2017-02-21 | 2017-08-22 | 鑑道生命科技有限公司 | A kind of equipment of utilization graphene high-efficiency oxygen and hydrogen-rich ionized water |
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| CN110453260A (en) * | 2019-08-23 | 2019-11-15 | 厦门大学 | A kind of wearable sensors and preparation method thereof for sweat detection |
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| CN114324545A (en) * | 2022-01-07 | 2022-04-12 | 三只松鼠股份有限公司 | Reduced graphene oxide sensor, preparation method thereof and method for rapidly detecting capsaicin content |
| CN114324545B (en) * | 2022-01-07 | 2024-05-28 | 三只松鼠股份有限公司 | Reduced graphene oxide sensor, preparation method thereof and method for rapidly detecting capsaicin content |
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