CN103833026A - Preparation method of graphene nanoribbon - Google Patents
Preparation method of graphene nanoribbon Download PDFInfo
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- CN103833026A CN103833026A CN201210491188.5A CN201210491188A CN103833026A CN 103833026 A CN103833026 A CN 103833026A CN 201210491188 A CN201210491188 A CN 201210491188A CN 103833026 A CN103833026 A CN 103833026A
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- methylimidazole
- ethyl
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Abstract
The invention belongs to the field of preparation of carbon-nano materials and discloses a preparation method of graphene nanoribbon. The preparation method comprises the following steps of: preparing a carbon-nano working electrode, selecting a lead plate as a counter electrode, selecting Hg/Hg2SO4 as a reference electrode and selecting ion liquid as electrolyte; soaking the three electrodes into the electrolyte; applying forward voltage, then applying backward voltage and obtaining a mixture with the graphene nanoribbon and the ion liquid; filtering, cleaning and drying the mixture and obtaining the graphene nanoribbon. The preparation method provided by the invention has the advantages that the preparation process is simple, the reaction speed and the quality of products can be controlled by controlling the level of the voltage, and by utilizing the ion liquid as the electrolyte, re-aggregation of the peeled graphene nanoribbon can be effectively prevented and the preparation efficiency can be improved.
Description
Technical field
The present invention relates to carbon nanomaterial preparation, relate in particular to a kind of preparation method of graphene nanobelt.
Background technology
The kind of carbon material has the soccerballene (C60 etc.) of zero dimension, carbon nanotube, the carbon nanofiber etc. of one dimension, the Graphene of two dimension, three-dimensional graphite, diamond etc., graphene nanobelt not only has the performance of Graphene, also possess some special performances, for example its length-to-diameter ratio is larger, can, up to thousands of times, can replace copper conductor at integrated circuit connection, further improve integrated level, also can carry out modification to its structure and be prepared into switch device.But due to size control difficulty in graphene nanobelt preparation process, yield poorly at present, thereby limited its application.
Summary of the invention
Problem to be solved by this invention is to provide the preparation method of the graphene nanobelt that a kind of preparation process is simple, output is high.
Technical scheme of the present invention is as follows:
A preparation method for graphene nanobelt, comprises the steps:
The carbon nanotube of diameter 10～120nm is pressed into carbon nanometer wall sheet as working electrode, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, ionic liquid is as electrolytic solution;
By described working electrode, electrode, reference electrode are put into and are filled the electrolyzer of described electrolytic solution and be fully immersed in described electrolytic solution, working electrode is applied to the voltage of 0.1～20V, keep 0.1～10 hour, then described working electrode is applied to reverse voltage-20～-0.1V, keep 0.1～10 hour, just obtain the mixture of graphene nanobelt and ionic liquid;
Described mixture filters mixed solution after supercentrifuge separates unstripped carbon nanotube, the filter residue obtaining filters repeatedly through organic solvent again, clean, filter with ethanol, acetone, deionized water etc. respectively again, the filter residue and drying of collecting, to constant weight, is obtained to described graphene nanobelt.
The preparation method of described graphene nanobelt, preferably, the specification of described carbon nanometer wall sheet is 75*40*7mm
3.
The preparation method of described graphene nanobelt, preferably, described ionic liquid is selected 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole fluoroform sulfimide, 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid, 1-ethyl-3-methylimidazole trifluoroacetic acid, 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon, 1-ethyl-3-methylimidazole five acetyl fluoride imines, 1-ethyl-3-methylimidazole two cyaniding nitrogen, 1-ethyl-3, 5-methylimidazole fluoroform sulfimide, 1, 3-diethyl-4-methylimidazole fluoroform sulfimide and 1, at least one in 3-diethyl-5-Methylimidazole fluoroform sulfimide.
The preparation method of described graphene nanobelt, preferably, organic solvent when described filter residue filtration treatment is 1-Methyl-2-Pyrrolidone or DMF.
The preparation method of described graphene nanobelt, preferably, described filter residue and drying processing is at 60～100 ℃, to carry out in vacuum drying oven.
The preparation method of graphene nanobelt provided by the invention, preparation process is simple, can control speed of response and product quality by controlling voltage swing, utilize ionic liquid to do electrolytic solution and can effectively prevent from again reuniting after graphene nanobelt from peeling off, improve preparation efficiency; By selecting carbon nanotube diameter and length, can control diameter Distribution and the length-to-diameter ratio of graphene nanobelt, reliability is high; Required equipment is all common chemical industry equipment, saves research and development equipment cost, is applicable to scale operation.
Accompanying drawing explanation
Fig. 1 is graphene nanobelt SEM figure prepared by embodiment 1.
Embodiment
The preparation method of graphene nanobelt provided by the invention, its preparation process is as follows:
S1, the carbon nanotube of 10～120nm is pressed into 75*40*7mm
3the carbon nanometer wall sheet of (about 2g) is as working electrode, using stereotype as to electrode, and Hg/Hg
2sO
4as reference electrode, ionic liquid is as electrolytic solution;
S2, by working electrode, three electrodes such as electrode, reference electrode are put into and are filled the electrolyzer of described electrolytic solution and be fully immersed in electrolytic solution, working electrode is applied to the voltage of 0.1～20V, keep 0.1～10 hour, then apply working electrode reverse voltage-20～-0.1V, keep 0.1～10 hour, just obtain the mixture of graphene nanobelt and ionic liquid;
S3, mixture filter mixed solution after supercentrifuge separates unstripped carbon nanotube, the filter residue obtaining filters repeatedly through organic solvent again, preferably 3～6 times, clean, filter with ethanol, acetone, deionized water etc. respectively again, the filter residue of collecting is dried in vacuum drying oven to constant weight at 60～100 ℃ and can obtains graphene nanobelt.
The preparation method of described graphene nanobelt, preferably, ionic liquid is preferably 1-ethyl-3-methylimidazole Tetrafluoroboric acid (EtMeImBF
4), 1-ethyl-3-methylimidazole fluoroform sulfimide (EtMeImN (CF
3sO
2)
2), 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid (EtMeImCF
3sO
3), 1-ethyl-3-methylimidazole trifluoroacetic acid (EtMeImCF
3cO
2), 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon (EtMeImC (CF
3sO
2)
3), 1-ethyl-3-methylimidazole five acetyl fluoride imines (EtMeIm N (C
2f
5sO
2)
2), 1-ethyl-3-methylimidazole two cyaniding nitrogen (EtMeImN (CN)
2), 1-ethyl-3,5-methylimidazole fluoroform sulfimide (1-Et-3,5-Me
2imN (CF
3sO
2)
2), 1,3-diethyl-4-methylimidazole fluoroform sulfimide (1,3-Et
2-4-MeImN (CF
3sO
2)
2) 1,3-diethyl-5-Methylimidazole fluoroform sulfimide (1,3-Et
2-5-MeImN (CF
3sO
2)
2) at least one.
The preparation method of described graphene nanobelt, preferably, the organic solvent adopting when filter residue filtration treatment is preferably: 1-Methyl-2-Pyrrolidone (NMP) or DMF (DMF); NMP, DMF can effectively remove ionic liquid.
The preparation method of graphene nanobelt provided by the invention, preparation process is simple, can control speed of response and product quality by controlling voltage swing, utilize ionic liquid to do electrolytic solution and can effectively prevent from again reuniting after graphene nanobelt from peeling off, improve preparation efficiency.By selecting carbon nanotube diameter and length, can control diameter Distribution and the length-to-diameter ratio of graphene nanobelt, reliability is high.Required equipment is all common chemical industry equipment, saves research and development equipment cost, is applicable to scale operation.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
1. the carbon nanotube that is 10～20nm by diameter is pressed into 75*40*7mm
3the graphite flake of (about 2g) is as working electrode, using stereotype as to electrode, and Hg/Hg
2sO
4as reference electrode, EtMeImBF
4as electrolytic solution, three electrodes are put into electrolyzer and are fully immersed in electrolytic solution, working electrode is applied to the voltage of 10V, keep 0.5 hour, then working electrode is applied to reverse voltage-10V, keep 0.5 hour, just obtain graphene nanobelt and EtMeImBF
4the mixture of ionic liquid.After supercentrifuge separates unstripped carbon nanotube, mixed solution is filtered, the filter residue obtaining filters 6 times through NMP again, clean, filter with ethanol, acetone, deionized water etc. respectively again, the filter residue of collecting is dried in vacuum drying oven to constant weight at 60 ℃ and can obtains graphene nanobelt, as shown in Figure 1.
Embodiment 2 ~ 11, adopts following form 1 form, and its step of preparation process is identical with embodiment 1, and corresponding processing parameter and processing condition refer in following table 1.
Table 1
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (5)
1. a preparation method for graphene nanobelt, is characterized in that, comprises the steps:
The carbon nanotube of diameter 10～120nm is pressed into carbon nanometer wall sheet as working electrode, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, ionic liquid is as electrolytic solution;
By described working electrode, electrode, reference electrode are put into and are filled the electrolyzer of described electrolytic solution and be fully immersed in described electrolytic solution, working electrode is applied to the voltage of 0.1～20V, keep 0.1～10 hour, then described working electrode is applied to reverse voltage-20～-0.1V, keep 0.1～10 hour, just obtain the mixture of graphene nanobelt and ionic liquid;
Described mixture filters mixed solution after supercentrifuge separates unstripped carbon nanotube, the filter residue obtaining filters repeatedly through organic solvent again, clean, filter with ethanol, acetone, deionized water etc. respectively again, the filter residue and drying of collecting, to constant weight, is obtained to described graphene nanobelt.
2. the preparation method of graphene nanobelt according to claim 1, is characterized in that, the specification of described carbon nanometer wall sheet is 75*40*7mm
3.
3. the preparation method of graphene nanobelt according to claim 1, it is characterized in that, described ionic liquid is selected 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole fluoroform sulfimide, 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid, 1-ethyl-3-methylimidazole trifluoroacetic acid, 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon, 1-ethyl-3-methylimidazole five acetyl fluoride imines, 1-ethyl-3-methylimidazole two cyaniding nitrogen, 1-ethyl-3, 5-methylimidazole fluoroform sulfimide, 1, 3-diethyl-4-methylimidazole fluoroform sulfimide and 1, at least one in 3-diethyl-5-Methylimidazole fluoroform sulfimide.
4. the preparation method of graphene nanobelt according to claim 1, is characterized in that, organic solvent when described filter residue filtration treatment is 1-Methyl-2-Pyrrolidone or DMF.
5. the preparation method of graphene nanobelt according to claim 1, is characterized in that, described filter residue and drying processing is at 60～100 ℃, to carry out in vacuum drying oven.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924257A (en) * | 2013-01-15 | 2014-07-16 | 海洋王照明科技股份有限公司 | Graphene nanoribbons and preparation method thereof |
| CN109321932A (en) * | 2018-10-30 | 2019-02-12 | 深圳大学 | Graphene and the preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010022164A1 (en) * | 2008-08-19 | 2010-02-25 | William Marsh Rice University | Preparation of graphene nanoribbons from carbon nanotubes |
| CN101913599A (en) * | 2010-08-13 | 2010-12-15 | 东华大学 | Method for preparing graphene nanobelt |
| WO2012035551A1 (en) * | 2010-09-14 | 2012-03-22 | Council Of Scientific & Industrial Research | Electrochemical process for synthesis of graphene |
| CN102807213A (en) * | 2012-08-30 | 2012-12-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for electrochemically preparing graphene |
-
2012
- 2012-11-27 CN CN201210491188.5A patent/CN103833026A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010022164A1 (en) * | 2008-08-19 | 2010-02-25 | William Marsh Rice University | Preparation of graphene nanoribbons from carbon nanotubes |
| CN101913599A (en) * | 2010-08-13 | 2010-12-15 | 东华大学 | Method for preparing graphene nanobelt |
| WO2012035551A1 (en) * | 2010-09-14 | 2012-03-22 | Council Of Scientific & Industrial Research | Electrochemical process for synthesis of graphene |
| CN102807213A (en) * | 2012-08-30 | 2012-12-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for electrochemically preparing graphene |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924257A (en) * | 2013-01-15 | 2014-07-16 | 海洋王照明科技股份有限公司 | Graphene nanoribbons and preparation method thereof |
| CN109321932A (en) * | 2018-10-30 | 2019-02-12 | 深圳大学 | Graphene and the preparation method and application thereof |
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Application publication date: 20140604 |