CN103803533A - Preparation method of graphene - Google Patents
Preparation method of graphene Download PDFInfo
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- CN103803533A CN103803533A CN201210475304.4A CN201210475304A CN103803533A CN 103803533 A CN103803533 A CN 103803533A CN 201210475304 A CN201210475304 A CN 201210475304A CN 103803533 A CN103803533 A CN 103803533A
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- graphene
- expanded graphite
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- suspension
- graphene microplate
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Abstract
The invention is suitable for the technical field of chemical synthesis and provides a preparation method of graphene. The method comprises the following steps of preparing expanded graphite; mixing the obtained expanded graphite and an organic solvent; carrying out ultrasonic dissociation on the mixed solution of the expanded graphite and the organic solvent to obtain graphene microsheet suspension liquid; extracting a graphene microsheet from the graphene microsheet suspension liquid. The preparation method is suitable for industrially producing graphene materials in a large scale and at low cost; in addition, no any oxidative reduction process is adopted, the lattice structure of the prepared graphene is not damaged, and the quality of the obtained graphene is high; meanwhile, no any acid, alkaline or other toxic discharges are generated, and the used organic solvent can be repeatedly used and is environment-friendly.
Description
Technical field
The invention belongs to chemosynthesis technical field, relate to Graphene, relate in particular to a kind of preparation method of Graphene.
Background technology
Graphene is a kind of new carbon of broad research in recent years, is that carbon atom is arranged the Colloidal particles forming according to hexagonal.As monolayer carbon atomic plane material, Graphene can obtain by peeling off graphite material.This graphite crystal film of Graphene just becomes the focus that scientific circles and industry member are paid close attention to after being found by the scientist of University of Manchester from 2004.The thickness of Graphene only has 0.335 nanometer, is not only one the thinnest in known materials, also very firmly hard; As simple substance, it is all faster than known all conductors and semi-conductor that it at room temperature transmits the speed of electronics, and in Graphene, the travelling speed of electronics has reached 1/300 of the light velocity.Meanwhile, as monolayer carbon atomic structure, the theoretical specific surface area of Graphene is up to 2630m2/g.So high specific surface area makes to become extremely promising energy storage active material with the material based on Graphene.
At present prepare grapheme material and have following several method:
1. slight rubbing manipulation or tear tape method, this method productive rate is extremely low, is only applicable to laboratory and prepares Graphene, is not suitable for large-scale industrialization and produces.
2. heating SiC method: this method is to remove Si by heating monocrystalline 6H-SiC, decomposites graphene sheet layer on monocrystalline (0001) face.Because its thickness is determined by Heating temperature, it is more difficult that preparation big area has the Graphene of single thickness.And SiC is too expensive, and the Graphene obtaining is difficult to transfer on other substrates.
3. metal substrate chemical Vapor deposition process
Chemical Vapor deposition process is to utilize the atomic structure extension of substrate to go out Graphene, and the same with heating SiC method, the method is not suitable for for producing graphene powder material.
4. chemical dispersion method
The method is dissociated into mono-layer graphite by natural graphite powder in oxidation and reduction process.Its product has quite high Specific Surface Area Measurement (> 700m2/g), and process is relatively simple, and therefore the most applicable large-scale industrialization of the method is produced grapheme material.But its electroconductibility of partial reduction (having destroyed the high electron mobility of Graphene itself) just in redox processes, and in preparation process, produce a large amount of soda acids and dump thing, unfriendly to environment.
Summary of the invention
The object of the embodiment of the present invention is to overcome problems of the prior art, a kind of applicable low-cost industrial scale operation, high quality is provided, does not produce any poisonous graphene preparation method that dumps thing.
The embodiment of the present invention is achieved in that a kind of graphene preparation method, said method comprising the steps of: prepare expanded graphite; The expanded graphite obtaining is mixed with organic solvent; Expanded graphite organic solvent mixed solution is carried out to ultrasonic dissociating and obtain Graphene microplate suspension; And extract Graphene microplate from Graphene microplate suspension.
In a preferred embodiment, the described expanded graphite of preparing, for expansible black lead is placed in to metal or ceramic crucible, under protection of inert gas, is heated to 300-900 degree, keeps temperature 10-60 to divide, and realizes fully and expanding, and is then cooled to room temperature.
In a preferred embodiment, the described expanded graphite of preparing is for to be placed in ceramic crucible or glassware by expansible black lead, with 600-1200W microwave heating 10-60 second, realizes fully and expanding, and is then cooled to room temperature.
In a preferred embodiment, described the expanded graphite obtaining and organic solvent are mixed into gained expanded graphite is placed in to container, pour organic solvent into, stir.
In a preferred embodiment, described organic solvent is at least one in NMP, DMP, toluene, chlorobenzene and trieline.
In a preferred embodiment, describedly expanded graphite organic solvent mixed solution is carried out to ultrasonic dissociating obtain Graphene microplate suspension for being the 1-24 hour that vibrates under 300-1200W condition at sonic oscillation power, Heating temperature is 20-150 degree simultaneously, obtains Graphene microplate suspension.
In a preferred embodiment, the described Graphene microplate that extracts from Graphene microplate suspension, for ultrasonic gained Graphene microplate suspension is left standstill to 0.2-5 hour, removes upper strata suspension, removes throw out, after filtration, in 80 degree baking ovens, dries.
In an embodiment of the present invention, there is following technique effect: 1, be applicable to low-cost industrial scale operation grapheme material; 2. do not adopt any redox processes, do not destroy the crystalline network of prepared Graphene, products obtained therefrom quality is high; 3. do not adopt any redox processes, do not produce any soda acid or other poisonous things that dumps, institute with an organic solvent can reuse, environmentally friendly.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
In an embodiment of the present invention, by ultrasonic method of dissociating, in solution, expanded graphite is dissociated into Graphene.Described preparation method comprises the steps:
1. prepare expanded graphite: expansible black lead is placed in to metal or ceramic crucible, under protection of inert gas, is heated to 300-900 degree, keep temperature 10-60 minute, realize fully and expanding, be then cooled to room temperature.
Or expansible black lead is placed in to ceramic crucible or glassware, with 600-1200W microwave heating 10-60 second, realizes fully and expanding, be then cooled to room temperature.
In specific embodiment, raw material is desirable crystalline flake graphite also.
2. the expanded graphite obtaining is mixed with organic solvent: gained expanded graphite is placed in to container, pours 100-1000ml organic solvent into, described organic solvent is NMP, DMP, toluene, chlorobenzene or trieline, stirs.
3. expanded graphite organic solvent mixed solution is carried out to ultrasonic dissociating and obtain Graphene microplate suspension: be the 1-24 hour that vibrates under 300-1200W condition at sonic oscillation power, heating simultaneously, temperature is 20-150 degree, obtains Graphene microplate suspension.Ultrasonic jitter time is too short in 60 minutes, to such an extent as to the effect that dispersion is dissociated is bad, and the present invention adopts concussion 1-24 hour, can effectively improve dispersion effect.The heating of taking in addition is also conducive to improve dispersion effect.
4. from Graphene microplate suspension, extract Graphene microplate: ultrasonic gained Graphene microplate suspension is left standstill to 0.2-5 hour, get upper strata suspension, remove throw out, after filtration, in 80 degree baking ovens, dry.The present invention, without centrifugal treating, saves fabrication steps, enhances productivity.
Illustrate below in conjunction with specific embodiment.
Embodiment mono-
In the present embodiment, grapheme material preparation method's implementing procedure is as follows:
Get 1g50 order expansible black lead and be placed in metal or ceramic crucible, under protection of inert gas, be heated to 900 degree, realize fully and expanding, be then cooled to room temperature.Gained expanded graphite is placed in to container, pours in 250ml NMP, stir.Be under 1200W condition, to vibrate 16 hours gained expanded graphite NMP mixed solution at sonic oscillation power, be heated to 80 degree simultaneously.Obtain Graphene microplate suspension.Sonic oscillation gained Graphene microplate suspension is left standstill to 1 hour, remove throw out, get upper strata suspension, after filtration, in 80 degree baking ovens, dry, obtain Graphene microplate.
Embodiment bis-
In the present embodiment, grapheme material preparation method's implementing procedure is as follows:
Get 1g expansible black lead and be placed in ceramic crucible or glassware, microwave 1000W heating 30 seconds.Realize fully and expanding, be then cooled to room temperature.Gained expanded graphite is placed in to container, pours in 250ml NMP, stir.Be under 1200W condition, to vibrate 16 hours gained expanded graphite NMP mixed solution at sonic oscillation power, be heated to 80 degree simultaneously.Obtain Graphene microplate suspension.Sonic oscillation gained Graphene microplate suspension is left standstill to 1 hour, remove throw out, get upper strata suspension, after filtration, in 80 degree baking ovens, dry, obtain Graphene microplate.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. a preparation method for Graphene, is characterized in that, said method comprising the steps of:
Prepare expanded graphite;
The expanded graphite obtaining is mixed with organic solvent;
Expanded graphite organic solvent mixed solution is carried out to ultrasonic dissociating and obtain Graphene microplate suspension; And
From Graphene microplate suspension, extract Graphene microplate.
2. the method for claim 1, is characterized in that, the described expanded graphite of preparing is for to be placed in metal or ceramic crucible by expansible black lead; under protection of inert gas, be heated to 300-900 degree, keep temperature 10-60 to divide; realize fully and expanding, be then cooled to room temperature.
3. the method for claim 1, is characterized in that, the described expanded graphite of preparing is for to be placed in ceramic crucible or glassware by expansible black lead, with 600-1200W microwave heating 10-60 second, realizes fully and expanding, and is then cooled to room temperature.
4. the method for claim 1, is characterized in that, described the expanded graphite obtaining and organic solvent are mixed into gained expanded graphite is placed in to container, pours organic solvent into, stirs.
5. method as claimed in claim 4, is characterized in that, described organic solvent is at least one in NMP, DMP, toluene, chlorobenzene and trieline.
6. the method for claim 1, it is characterized in that, described by expanded graphite organic solvent mixed solution carry out ultrasonic dissociate obtain Graphene microplate suspension for sonic oscillation power be under 300-1200W condition, vibrate 1-24 little, time, Heating temperature is 20-150 degree simultaneously, obtains Graphene microplate suspension.
7. the method for claim 1, it is characterized in that, the described Graphene microplate that extracts from Graphene microplate suspension, for ultrasonic gained Graphene microplate suspension is left standstill to 0.2-5 hour, removes upper strata suspension, remove throw out, after filtration, in 80 degree baking ovens, dry.
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| CN201210475304.4A CN103803533A (en) | 2012-11-15 | 2012-11-15 | Preparation method of graphene |
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| CN201210475304.4A CN103803533A (en) | 2012-11-15 | 2012-11-15 | Preparation method of graphene |
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Cited By (5)
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| CN105731448A (en) * | 2016-05-18 | 2016-07-06 | 桂林理工大学 | Preparation method of three-dimensional nitrogen doped graphene |
| WO2018024196A1 (en) * | 2016-08-02 | 2018-02-08 | 福建新峰二维材料科技有限公司 | Preparation method for graphene nanometer material |
| CN107673341A (en) * | 2017-11-02 | 2018-02-09 | 湖南衡义材料科技有限公司 | A kind of method that large-area high-quality graphene is prepared using expansible graphite |
| CN109179390A (en) * | 2018-08-08 | 2019-01-11 | 青岛领军节能与新材料研究院 | A kind of preparation method of high-quality graphene |
| WO2019223756A1 (en) * | 2018-05-24 | 2019-11-28 | 深圳三匚科技有限公司 | Graphite material and preparation method and application thereof |
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Application publication date: 20140521 |