CN104593802B - The electrochemical preparation method of graphene - Google Patents
The electrochemical preparation method of graphene Download PDFInfo
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- CN104593802B CN104593802B CN201410815658.8A CN201410815658A CN104593802B CN 104593802 B CN104593802 B CN 104593802B CN 201410815658 A CN201410815658 A CN 201410815658A CN 104593802 B CN104593802 B CN 104593802B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
Abstract
The invention discloses a kind of electrochemical preparation method of graphene, comprise the following steps：Electrode with electrocatalysis is provided, the electrode with electrocatalysis is pre-processed；Graphene oxide solution is dripped to the surface for completing have electrocatalysis electrode described in pretreatment, the electrode of graphene oxide modification is obtained after drying；The electrode that the graphene oxide is modified is immersed in the salting liquid that pH that concentration is 10mmol/L~500mmol/L is 7, regulation electrode potential is that 1.2V~2V reacts 1s~1h, obtains required graphene.The salting liquid that the electrode and pH that the electrochemical preparation method of this graphene passes through electrocatalysis are 7 is used cooperatively, and can activate the reduction reaction of graphene oxide at the lower voltage, neutral salt solution is green, configuration is simple, cheap.Relative to the electrochemical preparation method of traditional graphene, the electrochemical preparation method of this graphene prepares cost and difficulty is relatively low.
Description
Technical field
The present invention relates to a kind of electrochemical preparation method of graphene.
Background technology
Graphene (graphene) is the individual layer laminated structure that a kind of carbon atom by honeycomb-patterned ordered arrangement is formed.Graphite
Alkene has excellent electricity, calorifics and mechanical property because of its unique structure, it is expected in high-performance nano electronic device, sensing
The field such as device, nano composite material, battery and ultracapacitor, field emmision material obtains extensive use.Therefore, just go out within 2004
Existing graphene rapidly becomes the study hotspot of physics, chemistry and materialogy in recent years.
The preparation of graphene is the basis of graphene theoretical research and application study, at present the electrochemistry preparation side of graphene
Method mainly includes mechanical stripping method, epitaxial growth method, chemical vapour deposition technique (CVD), chemistry redox method, liquid phase stripping method
Deng.Chemical method receives the concern of many researchers in these methods.Chemical method reaction condition is gentle, easily controllable, fits
A large amount of preparations of graphene are closed, and there is stronger advantage in following process etc., existing many research work are also
Carried out based on this method, but chemical method preparation process is slow, and efficiency is low, and need to add hydrazine hydrate, sodium borohydride,
The noxious materials such as hydroquinones, and electroreduction rule is to obtain electronics by the oxygen-containing functional group on oxidation state graphene to be gone back
Original, it is not related to toxic chemical and preparation method is simple, course of reaction is easily controllable, cost is low, pollution-free, prepared
Graphene free from admixture quality is high, is a kind of simple, green, the graphene preparation method that can be mass-produced.
At present, traditional method that graphene is prepared by electroreduction graphene oxide, high voltage activation is generally required also
Original reaction is, it is necessary to prepare cumbersome and have corrosive acid solution or cushioning liquid as electrolyte, preparation cost and difficulty
It is higher.
The content of the invention
Based on this, it is necessary to provide a kind of electrochemical preparation method for preparing cost and the relatively low graphene of difficulty.
A kind of electrochemical preparation method of graphene, comprises the following steps：
Electrode with electrocatalysis is provided；
Graphene oxide solution is dripped into the surface with electrocatalysis electrode, graphene oxide is obtained after drying
The electrode of modification；
The electrode that the graphene oxide is modified is immersed in the salt that pH that concentration is 10mmol/L~500mmol/L is 7
In solution, regulation electrode potential is that -1.2V~-2V reacts 1s~1h, obtains required graphene.
In one embodiment, the surface of the electrode with electrocatalysis is provided with catalytic deoxidation effect
Coating.
In one embodiment, the electrode with electrocatalysis is that glass-carbon electrode, electricity that acid copper is modified are heavy
The glass-carbon electrode of product nickel modification or the glass-carbon electrode of electro-deposition cupro-nickel modification.
In one embodiment, the material of the electrode with electrocatalysis is with catalytic deoxidation effect.
In one embodiment, the electrode with electrocatalysis is copper electrode, nickel electrode or corronil electrode.
In one embodiment, in addition to particle diameter is used described there be electro-catalysis to make for the aluminum oxide of 50nm~0.3 μm
The operation being cleaned by ultrasonic after electrode sanding and polishing with ethanol, distilled water.
In one embodiment, the concentration of the graphene oxide solution is 1mg/mL~6mg/mL.
In one embodiment, graphene oxide solution is dripped to described in completion pretreatment has electrocatalysis electrode
Surface operation in, the dripping quantity of the graphene oxide solution is the μ L of 5 μ L~30.
In one embodiment, the configuration process of described graphene oxide solution is as follows：Graphene oxide is distributed to
In water, ultrasound peels off 1h~4h and obtains graphene oxide solution in ultrasonic cleaning machine.
In one embodiment, the solute for the salting liquid that the pH is 7 is Na2SO4、K2SO4、NaNO3And KNO3In extremely
Few one kind.
The salting liquid that the electrode and pH that the electrochemical preparation method of this graphene passes through electrocatalysis are 7 coordinates and made
With the reduction reaction of graphene oxide can be activated at the lower voltage, and neutral salt solution is green, configuration is simple, price
It is cheap, the electrochemical preparation method of this graphene have low-power consumption, low cost, it is quick, green the advantages of.Relative to traditional
The electrochemical preparation method of graphene, the electrochemical preparation method of this graphene prepares cost and difficulty is relatively low.
Brief description of the drawings
Fig. 1 is the flow chart of the electrochemical preparation method of the graphene of an embodiment；
Fig. 2 is the glass of the graphene oxide modification in the copper electrode and comparative example 1 of the graphene oxide modification in embodiment 1
The linear volt-ampere curve figure of carbon electrode；
Fig. 3 is obtained also for reduced graphene made from the graphene oxide in embodiment 1, embodiment 1 and comparative example 1
The C1S figures of the x-ray photoelectron power spectrum of former graphene.
Embodiment
The manufacture method of ferrite powder is described in further detail mainly in combination with drawings and the specific embodiments below.
The electrochemical preparation method of the graphene of an embodiment as shown in Figure 1, comprises the following steps：
S10, the electrode with electrocatalysis is provided, the electrode with electrocatalysis is pre-processed.
The surface of electrode with electrocatalysis is provided with the coating with catalytic deoxidation effect.Specifically, with electricity
The electrode of catalytic action can be the glass-carbon electrode of acid copper modification, the glass-carbon electrode or electro-deposition cupro-nickel of electric deposition nickel modification
The glass-carbon electrode of modification.
Or the material of the electrode with electrocatalysis is with catalytic deoxidation effect.Specifically, there is electrocatalysis
Electrode can be copper electrode, nickel electrode or corronil electrode.The operation pre-processed to electrode is：Use particle diameter for
The aluminum oxide of 50nm~0.3 μm will use ethanol, distilled water to be cleaned by ultrasonic after the electrode sanding and polishing with electrocatalysis.
The material of corronil electrode can be the corronil that copper mass percentage composition is 10%~80%.
S20, graphene oxide solution is dripped to the table with electrocatalysis electrode completed the S10 of pretreatment and obtained
Face, the electrode of graphene oxide modification is obtained after drying.
Graphene oxide can be prepared by Modified Hummers methods.
The configuration process of graphene oxide solution is as follows：Graphene oxide is distributed in water, ultrasound is peeled off 1h~4h and obtained
To graphene oxide solution.
The concentration of graphene oxide solution can be 1mg/mL~6mg/mL.
Graphene oxide solution is dripped in the operation on the surface with electrocatalysis electrode for completing pretreatment, oxidation
The dripping quantity of graphene solution is the μ L of 5 μ L~30.
S30, the electrode that graphene oxide that S20 is obtained is modified is immersed in into concentration is 10mmol/L~500mmol/L's
PH is in 7 salting liquid, and regulation electrode potential is that -1.2V~-2V reacts 1s~1h, obtains required graphene.
The solute for the salting liquid that pH is 7 is Na2SO4、K2SO4、NaNO3And KNO3At least one of.
The salting liquid that the electrode and pH that the electrochemical preparation method of this graphene passes through electrocatalysis are 7 coordinates and made
With the reduction reaction of graphene oxide can be activated at the lower voltage, and neutral salt solution is green, configuration is simple, price
It is cheap, the electrochemical preparation method of this graphene have low-power consumption, low cost, it is quick, green the advantages of.
It is specific embodiment below.
Embodiment 1
Graphene oxide prepared by Modified Hummers methods is distributed in water, peeled off in 500W Vltrasonic devices
2h obtains the graphene oxide solution that concentration is 1.2mg/mL.
It is the aluminum oxide of 50nm~0.3 μm by a diameter of 3mm copper electrode sanding and polishing to use particle diameter, then with ethanol,
Distilled water is cleaned by ultrasonic, and completes the pretreatment of copper electrode.
The graphene oxide solution that 6 μ L concentration are 1.2mg/mL is dripped to the surface for the copper electrode for completing pretreatment, so
Copper electrode is dried at room temperature for afterwards to obtain the copper electrode of graphene oxide modification.
The copper electrode that graphene oxide is modified is immersed in the Na that concentration is 0.1mol/L2SO4In solution, then 0~-
Linear voltammetric scan is carried out in 1.5V potential range.Substantially there is cathode current when potential is -0.7V, reached in -1.2V
To peak value.Regulation electrode potential is -1.3V, reacts 5s, obtains required graphene.
Embodiment 2
Graphene oxide prepared by Modified Hummers methods is distributed in water, peeled off in 500W Vltrasonic devices
2h obtains the graphene oxide solution that concentration is 1.2mg/mL.
It is the aluminum oxide of 50nm~0.3 μm by diameter 3mm glass-carbon electrode sanding and polishing to use particle diameter, then with ethanol,
Distilled water is cleaned by ultrasonic.
Glass-carbon electrode is immersed to 0.5mol/L CuSO4In solution, the acid copper in the range of 0V~-0.6V, copper is obtained
The glass-carbon electrode of modification.
The graphene oxide solution that 6 μ L concentration are 1.2mg/mL is dripped to the surface of the glass-carbon electrode of copper modification, Ran Hou
The glass-carbon electrode of graphene oxide-copper modification is dried to obtain at room temperature.
The glass-carbon electrode of graphene oxide-copper modification is immersed in 0.1mol/L Na2SO4In solution, then 0.0~-
Linear voltammetric scan is carried out in 1.5V potential range；Substantially there is cathode current when potential is -0.72V, in -1.23V
Reach peak value.Regulation electrode potential is -2V, reacts 1s, obtains required graphene.
Embodiment 3
Graphene oxide prepared by Modified Hummers methods is distributed in water, peeled off in 500W Vltrasonic devices
2h obtains the graphene oxide solution that concentration is 1.0mg/mL.
It is the aluminum oxide of 50nm~0.3 μm by a diameter of 3mm copper electrode sanding and polishing to use particle diameter, then with ethanol,
Distilled water is cleaned by ultrasonic, and completes the pretreatment of copper electrode.
The graphene oxide solution that 10 μ L concentration are 1.0mg/mL is dripped to the surface for the copper electrode for completing pretreatment, so
Copper electrode is dried at room temperature for afterwards to obtain the copper electrode of graphene oxide modification.
The copper electrode that graphene oxide is modified is immersed in the Na that concentration is 0.1mol/L2SO4In solution, regulation electrode electricity
Gesture is -1.25V, reacts 5s, obtains required graphene.
Embodiment 4
Graphene oxide prepared by Modified Hummers methods is distributed in water, peeled off in 500W Vltrasonic devices
2h obtains the graphene oxide solution that concentration is 1.0mg/mL.
It is the aluminum oxide of 50nm~0.3 μm by diameter 3mm glass-carbon electrode sanding and polishing to use particle diameter, then with ethanol,
Distilled water is cleaned by ultrasonic.
Glass-carbon electrode is immersed to 0.5mol/L CuSO4In solution, the acid copper in the range of 0V~-0.6V, copper is obtained
The glass-carbon electrode of modification.
The graphene oxide solution that 5 μ L concentration are 1.0mg/mL is dripped to the surface of the glass-carbon electrode of copper modification, Ran Hou
The glass-carbon electrode of graphene oxide-copper modification is dried to obtain at room temperature.
The glass-carbon electrode of graphene oxide-copper modification is immersed in 0.1mol/L Na2SO4In solution, electrode potential is adjusted
For -1.3V, 2s is reacted, obtains required graphene.
Comparative example 1
Graphene oxide prepared by Modified Hummers methods is distributed in water, peeled off in 500W Vltrasonic devices
2h obtains the graphene oxide solution that concentration is 1.2mg/ml.
It is the aluminum oxide of 50nm~0.3 μm by a diameter of 3mm glass-carbon electrode sanding and polishing to use particle diameter, then uses second
Alcohol, distilled water are cleaned by ultrasonic.
The graphene oxide solution that 6 μ L concentration are 1.2mg/ml is dripped to the surface of glass-carbon electrode, then by electrode in room
The glass-carbon electrode of graphene oxide modification is dried to obtain under temperature.
The glass-carbon electrode that graphene oxide is modified is immersed in 0.1mol/L Na2SO4In solution, then 0.0~-
Linear voltammetric scan is carried out in 2.0V potential range.Substantially there is cathode current when potential is -0.9V, reached in -1.7V
To peak value.Regulation electrode potential is -2V, reacts 5s, obtains required graphene.
Comparative example 2
Graphene oxide prepared by Modified Hummers methods is distributed in water, peeled off in 500W Vltrasonic devices
2h obtains the graphene oxide solution that concentration is 1.2mg/ml.
It is the aluminum oxide of 50nm~0.3 μm by a diameter of 3mm glass-carbon electrode sanding and polishing to use particle diameter, then uses second
Alcohol, distilled water are cleaned by ultrasonic.
The graphene oxide solution that 6 μ L concentration are 1.2mg/ml is dripped to the surface of glass-carbon electrode, then by electrode in room
The glass-carbon electrode of graphene oxide modification is dried to obtain under temperature.
The glass-carbon electrode that graphene oxide is modified is immersed in 0.1mol/L Na2SO4In solution.Adjust electrode potential for-
1.7V, 10s is reacted, obtains required graphene.
Fig. 2 is the glass of the graphene oxide modification in the copper electrode and comparative example 1 of the graphene oxide modification in embodiment 1
The linear volt-ampere curve figure of carbon electrode, wherein, three electrode chem workstations are that Pt pieces are to electrode to electrode, reference electrode
Ag/AgCl electrodes, electrolyte are 0.1M Na2SO4Solution, obtain Fig. 2.
As seen from Figure 2, the copper electrode of the graphene oxide modification in embodiment 1 substantially goes out when potential is -0.7V
Existing cathode current, peak value is reached in -1.2V；The glass-carbon electrode of graphene oxide modification in comparative example 1 is -0.9V in potential
There is cathode current in Shi Mingxian, and peak value is reached in -1.7V.
As seen from Figure 2, the copper electrode modified in embodiment 1 by using graphene oxide, can reduce oxygen reduction
Electrode potential needed for graphite alkene.
Using x-ray photoelectron spectroscopy to reduced graphene made from the graphene oxide in embodiment 1, embodiment 1
And reduced graphene made from comparative example 1 carries out elementary analysis, obtains Fig. 3.
As seen from Figure 3, the degree of oxidation of the graphene oxide raw material in embodiment 1 and comparative example 1 is very high,
286.8eV combination energy position has very strong C-O peaks.And the C-O peaks of reduced graphene made from embodiment 1 and comparative example 1
Intensity substantially weakens, and illustrates that graphene oxide has obtained effective reduction.Meanwhile embodiment 1 and the obtained reduction stone of comparative example 1
The C-O peaks contrast of black alkene, it is found that the C-O peaks of embodiment 1 disappear substantially, and there be a certain degree of guarantor at the C-O peaks of comparative example 1
Stay.So as to illustrate that the reduction intensity of reduced graphene made from embodiment 1 is preferable, purity is higher.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
1. a kind of electrochemical preparation method of graphene, it is characterised in that comprise the following steps：
Electrode with electrocatalysis is provided；
Graphene oxide solution is dripped to the surface of the electrode with electrocatalysis, obtaining graphene oxide after drying repaiies
The electrode of decorations；
The electrode that the graphene oxide is modified is immersed in the salting liquid that the pH that concentration is 10mmol/L ~ 500mmol/L is 7
In, regulation electrode potential is that -1.2V ~ -2V reacts 1s ~ 1h, obtains required graphene；
The electrode with electrocatalysis is copper electrode, nickel electrode or corronil electrode.
2. the electrochemical preparation method of graphene as claimed in claim 1, it is characterised in that also include using particle diameter as 50nm
~ 0.3 μm of aluminum oxide will use ethanol, distilled water to be cleaned by ultrasonic behaviour after the electrode sanding and polishing with electrocatalysis
Make.
3. the electrochemical preparation method of graphene as claimed in claim 1, it is characterised in that the graphene oxide solution
Concentration is 1mg/mL ~ 6mg/mL.
4. the electrochemical preparation method of graphene as claimed in claim 3, it is characterised in that drip to graphene oxide solution
In the operation for completing the surface of the electrode with electrocatalysis of pretreatment, the dripping quantity of the graphene oxide solution
For the μ L of 5 μ L ~ 30.
5. the electrochemical preparation method of the graphene as described in claim 1,3 or 4, it is characterised in that described graphite oxide
The configuration process of alkene solution is as follows：Graphene oxide is distributed in water, ultrasound is peeled off 1h ~ 4h and aoxidized in ultrasonic cleaning machine
Graphene solution.
6. the electrochemical preparation method of graphene as claimed in claim 1, it is characterised in that the pH is 7 salting liquid
Solute is Na2SO4、K2SO4、NaNO3And KNO3At least one of.
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| CN105331999B (en) * | 2015-10-13 | 2017-10-24 | 湖南农业大学 | The preparation method of hollow plumbago alkene |
| CN107215867B (en) * | 2016-03-22 | 2019-05-10 | 中国科学院金属研究所 | A kind of method that serialization prepares graphene oxide microplate |
| TR201603935A2 (en) | 2016-03-28 | 2017-10-23 | Yuecel Sahin | A METHOD FOR PRODUCING GRAFEN BASED ELECTRODE |
| CN106319576B (en) * | 2016-09-13 | 2018-08-28 | 合肥工业大学 | A kind of room temperature prepares two electrode electro Chemical reduction methods of silver-graphene nanocomposite |
| CN106676562B (en) * | 2016-12-13 | 2019-02-05 | 西安交通大学 | A method of graphene is prepared by electrochemical process reduction |
| CN109142482A (en) * | 2018-09-30 | 2019-01-04 | 辽宁大学 | Polypyrrole/stannic oxide/graphene nano material and its preparation method and application of divalent nickel compounds modification |
| CN114525522A (en) * | 2022-01-21 | 2022-05-24 | 江苏斯迪克新材料科技股份有限公司 | Graphene oxide waste conversion and recovery device and method |
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