CN102181877A - Graphene oxide for electrochemical reduction and preparation method of graphene - Google Patents
Graphene oxide for electrochemical reduction and preparation method of graphene Download PDFInfo
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- CN102181877A CN102181877A CN 201110103554 CN201110103554A CN102181877A CN 102181877 A CN102181877 A CN 102181877A CN 201110103554 CN201110103554 CN 201110103554 CN 201110103554 A CN201110103554 A CN 201110103554A CN 102181877 A CN102181877 A CN 102181877A
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- graphene
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- fto conductive
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Abstract
The invention belongs to the technical field of nano materials, and particularly relates to a graphene oxide for electrochemical reduction and a preparation method of graphene. The method comprises the following steps: dissolving graphite oxide in deionized water, and carrying out ultrasonic peeling to obtain a graphene oxide solution; cleaning electrodes and a glass container; adding the graphene oxide solution into the glass container; connecting one end of a copper conductor with cathode and anode materials, putting the electrodes into the graphene oxide solution, and respectively connecting the other end of the copper conductor with positive and negative poles of a direct-current stabilized voltage supply; switching on the direct-current stabilized voltage supply, wherein the voltage is controlled at 10-50V, and the temperature is controlled at 25-90 DEG C; and carrying out electrochemical reduction for 1-60 minutes, thereby obtaining the graphene. The graphene prepared by the method provided by the invention has the advantages of high quality; and the method is simple to operate, and has the advantages of low cost, high safety, no pollution, high-efficiency and the like.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to the method that the electrochemical reduction graphene oxide prepares Graphene.
Background technology
Graphene is a kind of novel two-dimensional nano material, its particular performances and at the application potential of aspects such as electrical condenser, cell image, transmitter, equipment, drug conveying and solar cell and cause extensive interest.Existing graphene preparation method comprises mechanically peel method, epitaxial growth method and chemical reduction method.In these methods, the productive rate of mechanically peel method is very low; The uneven thickness of the Graphene that epitaxial growth method obtains, so its application is limited; Chemical reduction method is generally with strong reductants such as hydrazine hydrates, though its cost is lower, hydrazine hydrate severe toxicity, easy-clear not can cause personal injury, environmental pollution and structure deteriorate.Recently, for redox graphene better, the preparation Graphene, the investigator has proposed several other methods that prepare Graphene, as hot reducing method and photo catalytic reduction method.But these methods have been brought some new problems, and hot reducing method is promptly by rapid heating graphene oxide to 1100 ° C in rare gas element, effective redox graphene, and still this method needs hot conditions, and is higher to equipment and environment requirement; The photo catalytic reduction method is promptly come redox graphene by UV-irradiation, but the thickness of the graphene film that obtains is thicker, and this will limit its performance and application.At above-mentioned these problems, combined with electrochemical reduction ultimate principle of the present invention and Green Chemistry theory, a kind of simple, convenient, feasible electrochemical reduction method is proposed, test result proves that the various aspects of performance of the Graphene that this method makes is all very excellent, and can realize the preparation of Graphene mass.
Summary of the invention
The object of the present invention is to provide a kind of simple to operate, efficient is high, is suitable for the method for preparing Graphene of large-scale production.
Graphene preparation method provided by the invention is to obtain Graphene by the electrochemical reduction graphene oxide.It combines the principle of electrochemical reduction and the electric property of Graphene excellence effectively, overcome the defective that other preparation method exists, not only effectively realized the electrochemical reduction of graphene oxide, obtain high-quality Graphene, also had advantages such as easy and simple to handle, with low cost, safety non-pollution, efficient be efficient.
The device that the inventive method relates to is seen shown in Figure 1, comprising: D.C. regulated power supply (DC regulated power supply) 1, and cathode electrode material 2, anode electrode material 3 holds graphene oxide solution (colloidal sol) in the Glass Containers 4(container).
The step of the graphene oxide electrochemical reduction method that the present invention proposes is as follows:
1, at first graphite oxide is dissolved in the deionized water, obtains graphene oxide solution by ultrasonic peeling off; The concentration of graphene oxide solution is 0.5 ~ 10 mg/ml;
2, cleaning electrode and Glass Containers promptly fully clean as dipolar electrode materials of yin, yang and Glass Containers with tap water, then they are put into ethanolic soln respectively, and by ultrasonic abundant cleaning, ultrasonic time is 10 ~ 30 min; Clean up with deionized water at last;
3, get an amount of above-mentioned graphene oxide solution, add in the Glass Containers;
4, an end that has a clip with copper conductor connects the cathode and anode electrode materials respectively, then electrode is put into above-mentioned graphene oxide solution and fixes, and the other end of copper conductor is connected with the positive and negative electrode of D.C. regulated power supply respectively;
5, connect power supply, control voltage is 10 ~ 50V; Controlled temperature is 25 ~ 90
oC; The electrochemical reduction time promptly makes high-quality Graphene for 1-60 min experiment.
Among the present invention, the particle diameter of described graphite oxide is 25 ~ 140 μ m;
Among the present invention, the volume of described Glass Containers is 1 ~ 100 ml;
Among the present invention, described cathode electrode material comprises: the SnO of doped with fluorine
2Conductive glass (being called for short the FTO conductive glass); TiO
2The FTO conductive glass of modifying, the FTO conductive glass that In modifies, the FTO conductive glass that ZnO Seed Layer modifies;
Among the present invention, described anode electrode material comprises; Copper sheet, carbon-point, FTO conductive glass, the FTO conductive glass that In modifies;
Electrochemical reduction graphene oxide of the present invention prepares the method for Graphene, compares with prior preparation method, has following advantage:
(1) this electrochemical reduction method does not relate to deleterious chemical reagent, and this has been avoided causing structure deteriorate, environmental pollution and hazard to person etc.;
(2) this method voltage is lower, compares safety, but can satisfy the needs of experiment fully, and this low-voltage regulated power supply is very common in the laboratory;
(3) use copper sheet, carbon-point, FTO conductive glass etc. as electrode materials, the with low cost of most of raw material is easy to get, though the price of FTO conductive glass is expensive slightly, because the amount of using seldom at every turn, so also be easy to realize;
(4) Glass Containers is transparent, the clearly variation in the observation experiment process, the convenient experimental phenomena that writes down at any time;
(5) can change the volume size of self-control Glass Containers according to the experiment needs;
(6) device is simple, facility investment is few, and raw materials cost is cheap to be easy to get, processing ease, and favorable reproducibility, suitability is strong.Be suitable for large-scale production.
Description of drawings
Fig. 1 prepares the experimental installation synoptic diagram of Graphene for the electrochemical reduction graphene oxide.
The redox graphene that electrochemical reduction obtains among Fig. 2 embodiment 1 and the Infrared spectroscopy figure of graphene oxide.
The XRD spectra of the redox graphene that electrochemical reduction obtains among Fig. 3 embodiment 1.
The redox graphene that electrochemical reduction obtains among Fig. 4 embodiment 2 and the Infrared spectroscopy figure of graphene oxide.
The XRD spectra of the redox graphene that electrochemical reduction obtains among Fig. 5 embodiment 2.
Number in the figure: 1, D.C. regulated power supply, 2, cathode electrode material, 3, anode electrode material, 4, hold the Glass Containers of graphene oxide solution.
Embodiment
Further specify the present invention below by embodiment.
Embodiment 1:Cu sheet is made anode, and FTO makes negative electrode, and the concentration of graphene oxide solution is 1mg/ml
With 30 μ m graphite oxides is raw material, graphite oxide is dissolved in the deionized water, by the ultrasonic graphene oxide solution that obtains 1mg/ml of peeling off; Fully clean copper sheet and FTO conductive glass electrode material with tap water, then they are put into ethanolic soln respectively, ultrasonic 10min cleans up with deionized water at last; Fully clean self-control rectangular parallelepiped Glass Containers with tap water, to wherein adding ethanolic soln, ultrasonic 10min rinses well with deionized water at last then; Measure the graphene oxide colloidal sol that 60ml has prepared, join in the self-control rectangular parallelepiped Glass Containers; An end that has clip with copper conductor connects copper sheet and FTO conductive glass respectively, then electrode is put into above-mentioned graphene oxide colloidal sol and fixes, and the other end of copper conductor is connected with the positive and negative electrode of D.C. regulated power supply respectively; Connect power supply, select voltage 30V, control experimental temperature 25
oC, electrochemical reduction 30min promptly makes high-quality Graphene.
In the reaction process, the color of solution is deepened gradually by original yellowish brown; After reaction finished, solution was aterrimus, with one deck atrament, had the membranaceous material of one deck black on the negative electrode FTO conductive glass on the positive C u sheet; Especially understand the dope of assembling some black near the negative pole in the solution.Samplings respectively such as black dopes in Cu sheet and FTO conductive glass, solution, the solution, do Infrared spectroscopy and XRD test after the processing respectively.Fig. 2 is the Infrared spectroscopy figure of electrochemical reduction graphene oxide and graphene oxide.The absorption peak that occurs a plurality of oxygen-containing functional groups among the Infrared spectroscopy figure of graphene oxide is as hydroxyl OH (~ 3575cm
-1With ~ 1400cm
-1), epoxy group(ing) C-O-C (~ 1225 cm
-1), carbonyl C=O (~ 1892 cm
-1).In the infrared spectrogram of electrochemical reduction graphene oxide, hydroxyl OH (~ 3575 cm
-1), carbonyl C=O (~ 1892 cm
-1) all disappear substantially, have only OH (~ 1400cm
-1) and C-O-C (~ 1225 cm
-1) also there is very poor absorption, this explanation reduction effect is relatively good.Fig. 3 is the XRD spectra of electrochemical reduction graphene oxide; Among the figure 34
o, 38
o, 52
o, 62
oWith 65
oNear diffraction peak is (101), (200), (211), (310) and (301) face of corresponding FTO respectively.43
oNear have the diffraction peak of faint graphite oxide (100) face, and 10
oNear the main peak of graphite oxide (002) face disappears, 26
oVery sharp very strong diffraction peak appears in the place, and is close with the diffraction peak position of graphite, and this explanation graphene oxide is reduced to Graphene to a great extent.
Embodiment 2:Cu sheet is made anode, and FTO makes negative electrode, and the concentration of graphene oxide solution is 2mg/ml
With 30 μ m graphite oxides is raw material, is dissolved in the deionized water, by the ultrasonic graphene oxide solution that obtains 2mg/ml of peeling off; Fully clean copper sheet and FTO conductive glass electrode material with tap water, then they are put into ethanolic soln respectively, ultrasonic 10min cleans up with deionized water at last; Fully clean self-control rectangular parallelepiped Glass Containers with tap water, to wherein adding ethanolic soln, ultrasonic 10min rinses well with deionized water at last then; Measure the graphene oxide colloidal sol that 60ml has prepared, join in the self-control rectangular parallelepiped Glass Containers; An end that has clip with copper conductor connects copper sheet and FTO conductive glass respectively, then electrode is put into above-mentioned graphene oxide colloidal sol and fixes, and the other end of copper conductor is connected with the positive and negative electrode of D.C. regulated power supply respectively; Connect power supply, select voltage 30V, control experimental temperature 25
oC, electrochemical reduction 30min promptly makes high-quality Graphene.
In the reaction process, the color of solution is deepened gradually by original yellowish brown; After reaction finished, solution was aterrimus, with one deck atrament, had the membranaceous material of one deck black on the negative electrode FTO conductive glass on the positive C u sheet; Especially understand the dope of assembling some black near the negative pole in the solution.Samplings respectively such as black dopes in Cu sheet and FTO conductive glass, solution, the solution, do infrared after the processing respectively and test such as XRD.Fig. 4 is the Infrared spectroscopy figure of electrochemical reduction graphene oxide and graphene oxide.The absorption peak that occurs a plurality of oxygen-containing functional groups in the graphene oxide is as hydroxyl OH (~ 3575 cm
-1With ~ 1400cm
-1), epoxy group(ing) C-O-C (~ 1225 cm
-1), carbonyl C=O (~ 1892 cm
-1).In the electrochemical reduction graphene oxide, OH (~ 3575 cm
-1), C=O (~ 1892 cm
-1) all disappear substantially, have only epoxy group(ing) C-O-C (~ 1225 cm
-1) and hydroxyl (~ 1400cm
-1) also there is very poor absorption, this explanation reduction effect is relatively good.Fig. 5 is the XRD spectra of electrochemical reduction graphene oxide.Among the figure 10
oNear the diffraction peak completely dissolve of graphene oxide (100) face, the diffraction peak of Graphene can clearly see that show, graphene oxide is reduced fully near 26 °.
Claims (3)
1. an electrochemical reduction graphene oxide is characterized in that to prepare the method for Graphene concrete steps are:
(1), at first graphite oxide is dissolved in the deionized water, the particle diameter of graphite oxide is 25 ~ 140 μ m; Obtain graphene oxide solution by ultrasonic peeling off; The concentration of graphene oxide solution is 0.5 ~ 10 mg/ml;
(2), cleaning electrode and Glass Containers;
(3), get an amount of above-mentioned graphene oxide solution, in the adding Glass Containers;
(4), the end that has a clip with copper conductor connects negative electrode, anode respectively, then electrode put into above-mentioned graphene oxide solution and fixes, the other end of copper conductor is connected with the positive and negative electrode of D.C. regulated power supply respectively;
(5), connect power supply, control voltage is 10 ~ 50V; Controlled temperature is 25 ~ 90
oC; The electrochemical reduction time is 1-60 min, promptly makes high-quality Graphene.
2. method according to claim 1 is characterized in that described cathode electrode material is: the SnO of doped with fluorine
2Conductive glass; Or TiO
2The FTO conductive glass of modifying, or the FTO conductive glass of In modification, or the FTO conductive glass of ZnO Seed Layer modification.
3. method according to claim 1 is characterized in that described anode electrode material is the FTO conductive glass that copper sheet, carbon-point, FTO conductive glass or In modify.
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| CN102645421A (en) * | 2012-04-21 | 2012-08-22 | 吉林大学 | Method of in-situ assembly, electrochemical reduction and representation of graphene oxide |
| CN102745676A (en) * | 2012-07-05 | 2012-10-24 | 吉林大学 | Method for preparing graphene and polyoxometalate composite through electrochemical reduction |
| CN102817057A (en) * | 2012-08-02 | 2012-12-12 | 上海交通大学 | Graphene oxide/conducting polymer composite coating and preparation method thereof |
| CN102963887A (en) * | 2012-11-30 | 2013-03-13 | 同济大学 | Electrochemistry stripping and reducing integrated graphene preparation method |
| CN103528928A (en) * | 2013-10-24 | 2014-01-22 | 南开大学 | Method for sensing single-cell based on graphene |
| CN104140096A (en) * | 2014-07-25 | 2014-11-12 | 同济大学 | Method for manufacturing graphene roll |
| CN104655698A (en) * | 2015-02-15 | 2015-05-27 | 浙江理工大学 | Graphene/graphene oxide microarray electrode as well as preparation method and application thereof |
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| CN105088261A (en) * | 2014-05-14 | 2015-11-25 | 国能纳米科技有限公司 | Preparation method of graphene |
| CN106319576A (en) * | 2016-09-13 | 2017-01-11 | 合肥工业大学 | Two-electrode electrochemical reduction method for preparing silver-graphene nano composite material at indoor temperature |
| CN106591871A (en) * | 2016-12-01 | 2017-04-26 | 燕园众欣纳米科技（北京）有限公司 | Method for preparing graphene through electrochemical in-situ oxidation and reduction |
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| CN108878171A (en) * | 2018-07-27 | 2018-11-23 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Core-sheath-type Flexible graphene fibre supercapacitors and its electroluminescent reducing preparation method |
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| CN101634032A (en) * | 2009-08-14 | 2010-01-27 | 南京大学 | Green and fast electrochemical preparation method for graphene |
| CN101797502A (en) * | 2010-03-24 | 2010-08-11 | 南京大学 | Preparation method of noble metal-graphene nanometer composite |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101634032A (en) * | 2009-08-14 | 2010-01-27 | 南京大学 | Green and fast electrochemical preparation method for graphene |
| CN101797502A (en) * | 2010-03-24 | 2010-08-11 | 南京大学 | Preparation method of noble metal-graphene nanometer composite |
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| CN102645421B (en) * | 2012-04-21 | 2013-11-27 | 吉林大学 | Method of in-situ assembly, electrochemical reduction and representation of graphene oxide |
| CN102645421A (en) * | 2012-04-21 | 2012-08-22 | 吉林大学 | Method of in-situ assembly, electrochemical reduction and representation of graphene oxide |
| CN102745676B (en) * | 2012-07-05 | 2014-03-12 | 吉林大学 | Method for preparing graphene and polyoxometalate composite through electrochemical reduction |
| CN102745676A (en) * | 2012-07-05 | 2012-10-24 | 吉林大学 | Method for preparing graphene and polyoxometalate composite through electrochemical reduction |
| CN102817057A (en) * | 2012-08-02 | 2012-12-12 | 上海交通大学 | Graphene oxide/conducting polymer composite coating and preparation method thereof |
| CN102817057B (en) * | 2012-08-02 | 2016-07-06 | 上海交通大学 | Graphene oxide/conducting polymer composite deposite and preparation method thereof |
| CN102963887A (en) * | 2012-11-30 | 2013-03-13 | 同济大学 | Electrochemistry stripping and reducing integrated graphene preparation method |
| CN102963887B (en) * | 2012-11-30 | 2015-01-14 | 同济大学 | Electrochemistry stripping and reducing integrated graphene preparation method |
| CN103528928A (en) * | 2013-10-24 | 2014-01-22 | 南开大学 | Method for sensing single-cell based on graphene |
| CN105088261B (en) * | 2014-05-14 | 2017-10-20 | 国能纳米科技有限公司 | The preparation method of graphene |
| CN105088261A (en) * | 2014-05-14 | 2015-11-25 | 国能纳米科技有限公司 | Preparation method of graphene |
| CN104140096A (en) * | 2014-07-25 | 2014-11-12 | 同济大学 | Method for manufacturing graphene roll |
| CN104140096B (en) * | 2014-07-25 | 2016-04-20 | 同济大学 | A kind of preparation method of graphene roll |
| CN104692670A (en) * | 2015-02-13 | 2015-06-10 | 北京欣奕华科技有限公司 | Graphene film and preparation method thereof |
| CN104655698B (en) * | 2015-02-15 | 2017-07-25 | 浙江理工大学 | Graphene/graphene oxide tiny array electrode and preparation method and application |
| CN104655698A (en) * | 2015-02-15 | 2015-05-27 | 浙江理工大学 | Graphene/graphene oxide microarray electrode as well as preparation method and application thereof |
| CN106319576A (en) * | 2016-09-13 | 2017-01-11 | 合肥工业大学 | Two-electrode electrochemical reduction method for preparing silver-graphene nano composite material at indoor temperature |
| 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 |
| CN106591871A (en) * | 2016-12-01 | 2017-04-26 | 燕园众欣纳米科技（北京）有限公司 | Method for preparing graphene through electrochemical in-situ oxidation and reduction |
| CN106676562A (en) * | 2016-12-13 | 2017-05-17 | 西安交通大学 | Method for preparing high-quality graphene through electrochemical reduction |
| CN108767210A (en) * | 2018-04-27 | 2018-11-06 | 西安理工大学 | A kind of electrochemical preparation method of self-supporting graphene/sulphur positive plate |
| CN108878171A (en) * | 2018-07-27 | 2018-11-23 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Core-sheath-type Flexible graphene fibre supercapacitors and its electroluminescent reducing preparation method |
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Application publication date: 20110914 |