CN102963887A - Electrochemistry stripping and reducing integrated graphene preparation method - Google Patents
Electrochemistry stripping and reducing integrated graphene preparation method Download PDFInfo
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- CN102963887A CN102963887A CN2012105065342A CN201210506534A CN102963887A CN 102963887 A CN102963887 A CN 102963887A CN 2012105065342 A CN2012105065342 A CN 2012105065342A CN 201210506534 A CN201210506534 A CN 201210506534A CN 102963887 A CN102963887 A CN 102963887A
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Abstract
The invention relates to an electrochemistry stripping and reducing integrated graphene preparation method. The method comprises the following steps of: (1) taking graphite oxide and dissolving the graphite oxide in deionized water so as to prepare a graphite oxide solution with a concentration range of 0.1-1mg/ml; (2) adding the graphite oxide solution into a reaction container; (3) applying an alternating electric field to the graphite oxide solution; and (4) generating an electrochemistry reaction via the graphite oxide in the environment of the alternating electric field so as to generate the graphene. Compared with the prior art, the method provided by the invention has the following beneficial effects: the principle of the electrochemistry reduction and the excellent electrochemistry property of the graphene are effectively combined, so that the defects existing in other preparation methods are overcome; and the electrochemistry stripping and reducing integrated graphene preparation method not only can be used for realizing a graphene preparing method with integrated stripping and reducing, but also has the advantages of simplicity in operation, low cost, safety, no pollution and the like.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene, especially relate to electrochemical stripping and the integrated graphene preparation method of reduction.
Background technology
Graphene (rGO) is the carbon atomic layer with monatomic thickness, since 2004 come out, caused widely at numerous areas and paid close attention to that they demonstrate in fields such as optics, sensing, catalysis and electricity widely application prospect because of its unique physicochemical property.Existing graphene preparation method comprises mechanically peel method, epitaxial growth method, vapour deposition process and oxidation reduction process etc.Oxidation reduction process be with graphite oxidation, a kind of preparation method of peeling off, restoring, the method is simple to operate, cost is lower, up to now, is considered to the most economical method of manufacture Graphene.
Wherein, peeling off of graphite oxide (GO) is committed step in the whole redox processes, and common stripping means has ultrasonic wave, pyrolysis expansion to peel off, and ultrasonic peeling off not only has noise pollution, and the Graphene lateral dimension that obtains is not of uniform size; It is not high that the pyrolysis expansion stripping method is peeled off productive rate, easily causes the graphene oxide lamella to be folded into vermiform, and having relatively high expectations to equipment.Reduction is the core procedure in the whole redox processes, can make by heat, light or electric field redox graphene, and hot reducing method can destroy the structure of Graphene, and in addition, it is also higher to the requirement of equipment and environment; The thickness of the graphene film that photo-reduction obtains is thicker, and this will limit its performance and application.Existing peeling off not only, there are some problems in method of reducing itself, and with they separately research also so that the preparation process very complicated of Graphene, be unfavorable for promoting the use of, so seek a kind of efficient, environmental protection and can will peel off the experimental technique finished synchronously of reduction seem most important, especially in electrochemistry, realize this process with alternating field, yet there are no report, combined with electrochemical ultimate principle of the present invention and Green Chemistry theory, propose following simple, efficiently, the alternating field of environmental protection is peeled off method of reducing, test result proves the Graphene that this method makes, and it peels off with reduction effect all fine, and quality is higher.
Summary of the invention
Purpose of the present invention be exactly provide a kind of preparation process simply, not include in order to overcome the defective that above-mentioned prior art exists to poison learn that reagent, device are simple, the electrochemical stripping of processing ease and the integrated graphene preparation method that reduces.
Purpose of the present invention can be achieved through the following technical solutions:
Concrete action principle of the present invention is as follows: the graphite oxide particle is electronegative because the chemical groups such as carboxyl, hydroxyl, carbonyl and epoxy group(ing) ionize in the aqueous solution, after its two ends adds voltage of alternating current, particle moves anode under electric field action, when direction of an electric field changes, to be subject to reverse electric field action power, under the repeatedly effect of this reversed electric field power, graphite oxide just is stripped from into graphene oxide, graphite oxide moves to and obtains electronics on the electrode, is reduced into Graphene.
A kind of electrochemical stripping and the integrated graphene preparation method of reduction, the method may further comprise the steps:
(1) gets graphite oxide and be dissolved in the deionized water, be made into the graphite oxide solution that concentration range is 0.1～1mg/ml;
(2) graphite oxide solution is added in the reaction vessel, reaction vessel can be glass or plastic containers;
(3) in graphite oxide solution, apply alternating electric field;
(4) electrochemical reaction occurs in graphite oxide under the environment of alternating electric field, generates Graphene.
The described method that applies alternating electric field of step (3) is: by the signal generator output signal, in the signal input power amplifier, this power amplifier with detect the electrical signal frequency and be connected oscilloscope with waveform and be connected, the regulating power amplifier, select suitable voltage, waveform and frequency, electrical signal after output is amplified namely obtains alternating electric field to electrode.
The process that electrochemical reaction occurs under the environment of alternating electric field the middle graphite oxide of step (4) is: the graphite oxide particle is electronegative in the aqueous solution, under the effect of alternating electric field, the to-and-fro movement between two electrodes of graphite oxide particle, graphite oxide is stripped from and is graphene oxide, graphene oxide moves to and obtains electronics on the electrode, is reduced to Graphene.
The spacing of two electrodes is 0.5～2cm, and described electrode is copper electrode or lead electrode.
Described electrical signal is sine wave or pulse wave, and its range of frequency is 0.5～10Hz.
The time of the described electrochemical reaction of step (4) is 2～180min.
The present invention 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 integrating and peeled off the method for preparing Graphene of reducing, also had the advantages such as easy and simple to handle, with low cost, safety non-pollution.
Compared with prior art, the present invention has the following advantages:
(1) the method integrates and peels off and reduce, and the preparation process of Graphene is oversimplified;
(2) the method does not relate to poisonous chemical reagent, and this has been avoided cause damage of equipment, environmental pollution and hazard to person etc.;
(3) device required for the present invention 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.
Description of drawings
Fig. 1 is setting drawing required for the present invention;
Fig. 2 is the atomic power spectrogram of the Graphene of embodiment 1 gained;
Fig. 3 is the infrared spectrogram of graphite oxide and Graphene among the embodiment 1;
Fig. 4 is the X-ray diffraction spectrogram of graphite oxide and Graphene among the embodiment 1;
Fig. 5 is the atomic power spectrogram of the Graphene of gained among the embodiment 2;
Fig. 6 is the infrared spectrogram of graphite oxide and Graphene among the embodiment 2;
Fig. 7 is the X-ray diffraction spectrogram of graphite oxide and Graphene among the embodiment 2.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
In following examples, power amplifier can adopt HVP-300A type power amplifier, and range of regulation is 30～70, and signal generator is DG1022 type signal generator, and oscilloscope can adopt DS1052E type oscilloscope.
The device of present embodiment as shown in Figure 1, signal generator 1 connects power amplifier 2, power amplifier 2 connection electrode 4, wherein, power amplifier 2 simultaneously with detect the electrical signal frequency and be connected oscilloscope 3 with waveform and be connected, apply alternating electric field by 1 pair of graphite oxide aqueous solution 5 of signal generator.
The reaction times of present embodiment is 120 minutes.
Take 30 μ m natural graphites as raw material, utilize the standby GO of improved hummers legal system first; The GO that obtains is dissolved in the deionized water preparation 0.2mg/ml GO suspension; Self-control electrochemical reaction Glass Containers (long 4cm, wide 2cm, high 10cm) with two copper plate electrodes (wide 3.5cm, long 10cm), two copper plate electrodes are inserted in the Glass Containers, two interelectrode distance 2cm link to each other two copper sheets with the alternating field power supply, select corresponding conditions (pulse wave, frequency is 0.5Hz, dutycycle 20%, voltage 40V); The above-mentioned GO suspension 50ml for preparing is poured in the Glass Containers, and plugged reacts and stops this reaction after 120 minutes, namely gets high-quality rGO; Resulting rGO is done respectively AFM Analysis, Infrared spectroscopy and X-ray diffraction analysis, verify its reduction situation, the result is respectively such as Fig. 2, Fig. 3 and shown in Figure 4.Among the figure, a represents graphite oxide, and b represents Graphene.
As can be seen from Figure 2, rGO thickness is about 0.45nm, and lateral dimension is single-layer graphene between 1～3um substantially.This Graphene has formed the shape as a kind of " snowflake " in reduction process.
Among Fig. 3, the absorption peak that occurs among the GO is respectively OH (3400cm
-1), C=O (1720cm
-1), C=C (1620cm
-1), C-H (1300cm
-1), C-O-C (1060cm-1).Behind the electrochemical reduction, the absorption peak OH (3400cm among the rGO
-1), C=O (1720cm
-1), C=C (1620cm
-1), C-O-C (1060cm-1) disappears substantially, only has C-H (1300cm
-1) also there is very faint absorption, this explanation reduction effect is relatively good.
Among Fig. 4, GO is after peeling off reduction, and the main peak of GO (002) face disappears near 2 θ=～10 °, ° locates to occur weak and wide diffraction peak in 2 θ=26, and this explanation GO is reduced to rGO to a great extent.
The device of present embodiment as shown in Figure 1,90 minutes reaction times.
Take 30 μ m natural graphites as raw material, utilize the standby GO of improved hummers legal system first; The GO that obtains is dissolved in the deionized water preparation 0.2mg/ml GO suspension; Self-control electrochemical reaction Glass Containers (long 4cm, wide 2cm, high 10cm) and two copper plate electrodes (wide 3.5cm, long 10cm) insert two copper plate electrodes in the Glass Containers two interelectrode distance 2cm; Two copper sheets are linked to each other with the alternating field power supply, select corresponding conditions (pulse wave, frequency are 0.5Hz, dutycycle 20%, voltage 40V); The above-mentioned GO suspension 50ml for preparing is poured in the Glass Containers, and plugged reacts and stops this reaction after 90 minutes, namely gets high-quality rGO;
Resulting rGO is done respectively AFM Analysis, Infrared spectroscopy and X-ray diffraction analysis, verify its reduction situation, the result is respectively such as Fig. 5, Fig. 6 and shown in Figure 7.
As seen from Figure 5, rGO thickness is about 0.8nm, and lateral dimension is more or less the same with single-layer graphene thickness between 2～4um.
Among Fig. 6, the absorption peak that occurs among the GO is respectively OH (3400cm
-1), C=O (1720cm
-1), C=C (1620cm
-1), C-H (1300cm
-1), C-O-C (1060cm
-1).Behind the electrochemical reduction, the absorption peak OH (3400cm among the rGO
-1), C=O (1720cm
-1), C-O-C (1060cm-1) disappears substantially, only has C-O-C (1060cm
-1) and C=C (1580cm
-1) locate also to exist a little absorption, this explanation reduction effect is relatively good.
Among Fig. 7, GO is after peeling off reduction, and the main peak of GO (002) face disappears near 2 θ=10 °, ° locates to occur weak and wide diffraction peak in 2 θ=26, near the diffraction peak that has faint GO (100) face 2 θ=43 °, this explanation GO major part is reduced to rGO.
A kind of electrochemical stripping and the integrated graphene preparation method of reduction, the method may further comprise the steps:
(1) gets graphite oxide and be dissolved in the deionized water, be made into the graphite oxide solution that concentration range is 0.1mg/ml;
(2) graphite oxide solution is added in the reaction vessel, reaction vessel can be glass or plastic containers;
(3) in graphite oxide solution, apply alternating electric field;
(4) electrochemical reaction occurs in graphite oxide under the environment of alternating electric field, generates Graphene.
The method that step (3) applies alternating electric field is: by the signal generator output signal, in the signal input power amplifier, this power amplifier with detect the electrical signal frequency and be connected oscilloscope with waveform and be connected, the regulating power amplifier, select suitable voltage, waveform and frequency, electrical signal after output is amplified namely obtains alternating electric field to electrode.The spacing of two electrodes is 0.5cm, and electrode is copper electrode, and electrical signal is sinusoidal wave, and its frequency is 0.5Hz.
The process that electrochemical reaction occurs under the environment of alternating electric field the middle graphite oxide of step (4) is: the graphite oxide particle is electronegative in the aqueous solution, under the effect of alternating electric field, the to-and-fro movement between two electrodes of graphite oxide particle, graphite oxide is stripped from and is graphene oxide, graphene oxide moves to and obtains electronics on the electrode, is reduced to Graphene.The time of step (4) electrochemical reaction is 2min.
A kind of electrochemical stripping and the integrated graphene preparation method of reduction, the method may further comprise the steps:
(1) gets graphite oxide and be dissolved in the deionized water, be made into the graphite oxide solution that concentration range is 1mg/ml;
(2) graphite oxide solution is added in the reaction vessel, reaction vessel can be glass or plastic containers;
(3) in graphite oxide solution, apply alternating electric field;
(4) electrochemical reaction occurs in graphite oxide under the environment of alternating electric field, generates Graphene.
The method that step (3) applies alternating electric field is: by the signal generator output signal, in the signal input power amplifier, this power amplifier with detect the electrical signal frequency and be connected oscilloscope with waveform and be connected, the regulating power amplifier, select suitable voltage, waveform and frequency, electrical signal after output is amplified namely obtains alternating electric field to electrode.The spacing of two electrodes is 2cm, and electrode is copper electrode, and electrical signal is sinusoidal wave, and its frequency is 10Hz.
The process that electrochemical reaction occurs under the environment of alternating electric field the middle graphite oxide of step (4) is: the graphite oxide particle is electronegative in the aqueous solution, under the effect of alternating electric field, the to-and-fro movement between two electrodes of graphite oxide particle, graphite oxide is stripped from and is graphene oxide, graphene oxide moves to and obtains electronics on the electrode, is reduced to Graphene.The time of step (4) electrochemical reaction is 180min.
Claims (5)
1. an electrochemical stripping and the integrated graphene preparation method of reduction is characterized in that the method may further comprise the steps:
(1) gets graphite oxide and be dissolved in the deionized water, be made into the graphite oxide solution that concentration range is 0.1～1mg/ml;
(2) graphite oxide solution is added in the reaction vessel;
(3) in graphite oxide solution, apply alternating electric field;
(4) electrochemical reaction occurs in graphite oxide under the environment of alternating electric field, generates Graphene.
A kind of electrochemical stripping according to claim 1 and the reduction integrated graphene preparation method, it is characterized in that, the described method that applies alternating electric field of step (3) is: by the signal generator output signal, in the signal input power amplifier, this power amplifier with detect the electrical signal frequency and be connected oscilloscope with waveform and be connected, the regulating power amplifier, the electrical signal after output is amplified namely obtains alternating electric field to electrode.
3. a kind of electrochemical stripping according to claim 2 and the integrated graphene preparation method of reduction is characterized in that the spacing of two electrodes is 0.5～2cm, and described electrode is copper electrode or lead electrode.
4. a kind of electrochemical stripping according to claim 2 and the integrated graphene preparation method of reduction is characterized in that described electrical signal is sine wave or pulse wave, and its range of frequency is 0.5～10Hz.
5. a kind of electrochemical stripping according to claim 1 and the integrated graphene preparation method of reduction is characterized in that the time of the described electrochemical reaction of step (4) is 2～180min.
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Cited By (11)
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|---|---|---|---|---|
| CN103215628A (en) * | 2013-04-17 | 2013-07-24 | 中国石油大学(华东) | Method for electro-chemical compounding of graphene and metallic oxide |
| CN103762096A (en) * | 2014-01-07 | 2014-04-30 | 同济大学 | Method for manufacturing grapheme paper used for flexible electrode material |
| CN103834993A (en) * | 2014-01-07 | 2014-06-04 | 同济大学 | Preparation method of graphene dendritic crystals and graphene dendritic crystals thereof |
| CN103879998A (en) * | 2013-12-27 | 2014-06-25 | 杭州金马能源科技有限公司 | Device for preparing graphene through large-scale electrochemical efficient stripping |
| CN104140096A (en) * | 2014-07-25 | 2014-11-12 | 同济大学 | Method for manufacturing graphene roll |
| CN105181660A (en) * | 2015-06-24 | 2015-12-23 | 中国科学院宁波材料技术与工程研究所 | Method for preparing graphene fluorescence quantum dots through electrochemical pulse |
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| CN110272040A (en) * | 2018-03-15 | 2019-09-24 | 中国人民解放军军事科学院防化研究院 | A kind of preparation method of high-purity graphene oxide |
| US10787746B2 (en) | 2014-10-13 | 2020-09-29 | Haibo Xu | Graphene oxide prepared by electrochemically oxidizing and cutting end face of carbon-based three-dimensional material and method therefor |
| CN112607729A (en) * | 2020-12-23 | 2021-04-06 | 中钢集团南京新材料研究院有限公司 | Device for stripping graphene by using alternating electric field and using method thereof |
| CN113249740A (en) * | 2021-06-21 | 2021-08-13 | 广西师范大学 | Method for preparing graphene by electrochemical continuous and synchronous stripping and reduction |
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| CN103215628B (en) * | 2013-04-17 | 2015-11-18 | 中国石油大学(华东) | A kind of method of electrochemical copolymerization Graphene and metal oxide |
| CN103215628A (en) * | 2013-04-17 | 2013-07-24 | 中国石油大学(华东) | Method for electro-chemical compounding of graphene and metallic oxide |
| CN103879998A (en) * | 2013-12-27 | 2014-06-25 | 杭州金马能源科技有限公司 | Device for preparing graphene through large-scale electrochemical efficient stripping |
| CN103762096A (en) * | 2014-01-07 | 2014-04-30 | 同济大学 | Method for manufacturing grapheme paper used for flexible electrode material |
| CN103834993A (en) * | 2014-01-07 | 2014-06-04 | 同济大学 | Preparation method of graphene dendritic crystals and graphene dendritic crystals thereof |
| 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 |
| US10787746B2 (en) | 2014-10-13 | 2020-09-29 | Haibo Xu | Graphene oxide prepared by electrochemically oxidizing and cutting end face of carbon-based three-dimensional material and method therefor |
| CN105181660A (en) * | 2015-06-24 | 2015-12-23 | 中国科学院宁波材料技术与工程研究所 | Method for preparing graphene fluorescence quantum dots through electrochemical pulse |
| CN105181660B (en) * | 2015-06-24 | 2018-08-21 | 中国科学院宁波材料技术与工程研究所 | The method that electrochemistry pulse prepares graphene fluorescence quantum |
| CN107628609A (en) * | 2016-07-18 | 2018-01-26 | 鸡西市昌隆石墨制品有限公司 | The manufacture method and graphene of number of plies controllable grapheme |
| CN110272040A (en) * | 2018-03-15 | 2019-09-24 | 中国人民解放军军事科学院防化研究院 | A kind of preparation method of high-purity graphene oxide |
| CN110272040B (en) * | 2018-03-15 | 2022-11-11 | 中国人民解放军军事科学院防化研究院 | Preparation method of high-purity graphene oxide |
| CN112607729A (en) * | 2020-12-23 | 2021-04-06 | 中钢集团南京新材料研究院有限公司 | Device for stripping graphene by using alternating electric field and using method thereof |
| CN113249740A (en) * | 2021-06-21 | 2021-08-13 | 广西师范大学 | Method for preparing graphene by electrochemical continuous and synchronous stripping and reduction |
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