CN105800598A - Method for preparing graphene by cutting intercalation method - Google Patents
Method for preparing graphene by cutting intercalation method Download PDFInfo
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- CN105800598A CN105800598A CN201610109503.1A CN201610109503A CN105800598A CN 105800598 A CN105800598 A CN 105800598A CN 201610109503 A CN201610109503 A CN 201610109503A CN 105800598 A CN105800598 A CN 105800598A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a method for preparing graphene by a cutting intercalation method. The method comprises the following steps: putting the graphene prepared by the intercalation method into a hydrothermal reactor employing polytetrafluoroethylene as a lining; adding a certain amount of water and hydrogen peroxide and reacting for 15 minutes to an hour at 100-180 DEG C; and taking out a sample for freeze drying after complete reaction to obtain the graphene prepared by the intercalation method after cutting. The method has the advantages of being simple and easy to operate; the overall process is environment-friendly and free of pollution; and the graphene sample with relatively uniformity in macroscopic preparation dimension can be achieved.
Description
Technical field
The present invention relates to field of preparation of graphene, be specifically related to the control preparation field based on Graphene size, prepare the cutting method of Graphene particularly to a kind of graft process.
Background technology
Graphene is prepared by promoting the important step of Graphene industrialization, and the preparation of Graphene not only includes the preparation in macroscopic quantity of Graphene, also includes the controlled synthesis of Graphene.Controlled factor mainly has the thickness of Graphene, size etc..These factors can affect the performance of Graphene to a great extent.Especially the size of Graphene, the size of Graphene can affect the electric conductivity of Graphene, thus the application of Graphene can be affected.Therefore the size controlling Graphene is most important.The method of current macroscopic preparation of graphene is mainly chemical oxidization method and graft process.The Graphene distribution of sizes that wherein prepared by chemical oxidization method is wider, and distribution of sizes is from tens nanometers to microns up to a hundred, the application affecting Graphene that this can be serious.If can to a certain extent the size of Graphene be controlled, it will promote the development of Graphene industry.
At present, in controlling Graphene size, the Graphene mainly prepared by chemical oxidization method carries out classification, and the method for classification is except centrifugally operated, and the method that also useful perforated membrane carries out classification, the media report seen has: publication number is CN104817071A.But, the clean cut separation of these methods or complicated operation or very difficult control Graphene.The size of Graphene can be controlled by the method for CVD growth, but the method for CVD can not obtain the Graphene of magnanimity to meet the needs of a lot of application.And CVD growth Graphene is relatively costly.
Graphene cost prepared by graft process is low, yield is high, but its size and thickness are bigger.These make Graphene prepared by graft process there is considerable restraint in application aspect.If the Graphene prepared by graft process carries out suitable cutting, control its thickness and size, it will promote the application of Graphene to a great extent.
Summary of the invention
Present invention aims to Graphene prepared by graft process be designed and provide a kind of method that graft process prepares Graphene that simply cuts, the size that can either control Graphene again can macroscopic preparation of graphene sample.Application further for Graphene is provided certain guarantee by this.
In order to realize foregoing invention purpose, the technical solution adopted in the present invention is as follows:
A kind of cut the method that graft process prepares Graphene, it is characterized in that the Graphene prepared by graft process puts into politef in the water heating kettle of liner, add a certain amount of water and hydrogen peroxide, at 100 DEG C～180 DEG C, reaction 15min～1h, takes out sample and carries out lyophilization and namely obtain the graft process after cutting and prepare Graphene after reacting completely.
In a preferred embodiment of the invention, the volume ratio of described water and hydrogen peroxide is 10:1～5:1.
In a preferred embodiment of the invention, the Graphene that prepared by described graft process is of a size of 80 μm.
Owing to have employed technical scheme as above, it is simple, easily operated that the present invention has method, and the advantage that whole process is environment friendly and pollution-free, it is possible to realizes the Graphene sample that preparation in macroscopic quantity size is comparatively homogeneous.
Accompanying drawing explanation
Fig. 1 is the Graphene TEM schematic diagram after the embodiment of the present invention 1 cuts.
Fig. 2 is the Graphene TEM schematic diagram after the embodiment of the present invention 2 cuts.
Fig. 3 is the Graphene TEM schematic diagram after the embodiment of the present invention 3 cuts.
Detailed description of the invention
Following example are only detailed description of the present invention, are not intended that the restriction to the claims in the present invention protection domain.
Embodiment 1
Graphene (the being of a size of 80 μm) 20mg prepared by graft process puts into politef in the 100mL water heating kettle of liner, adds 60mL water and 10mL hydrogen peroxide, at 140 DEG C, reacts 30min, takes out sample and carry out lyophilization after reacting completely.
Characterization result is shown in accompanying drawing 1.Result proves: after cutting, Graphene is of a size of diameter 1 μm～10 μm, and comparatively uniform.
Embodiment 2
Graphene (the being of a size of 80 μm) 20mg prepared by graft process puts into politef in the 100mL water heating kettle of liner, adds 60mL water and 10mL hydrogen peroxide, at 140 DEG C, reacts 45min, takes out sample and carry out lyophilization after reacting completely.
Characterization result is shown in accompanying drawing 2.Result proves: after cutting, Graphene is of a size of diameter 800nm～2 μm, and comparatively uniform.
Embodiment 3
Graphene (the being of a size of 80 μm) 20mg prepared by graft process puts into politef in the 100mL water heating kettle of liner, adds 60mL water and 10mL hydrogen peroxide, at 180 DEG C, reacts 20min, takes out sample and carry out lyophilization after reacting completely.
Characterization result is shown in accompanying drawing 3.Result proves: after cutting, Graphene is of a size of diameter 800nm～1.5 μm, and comparatively uniform.
Claims (3)
1. one kind cuts the method that graft process prepares Graphene, it is characterized in that the Graphene prepared by graft process puts into politef in the water heating kettle of liner, add a certain amount of water and hydrogen peroxide, at 100 DEG C～180 DEG C, reaction 15min～1h, takes out sample and carries out lyophilization and namely obtain the graft process after cutting and prepare Graphene after reacting completely.
2., as claim 1 cuts the method that graft process prepares Graphene, it is characterized in that the volume ratio of described described water and hydrogen peroxide is 10:1～5:1.
3., as claim 1 or 2 cuts the method that graft process prepares Graphene, it is characterized in that Graphene prepared by described graft process is of a size of 80 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610109503.1A CN105800598B (en) | 2016-02-26 | 2016-02-26 | A method of it cutting graft process and prepares graphene |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610109503.1A CN105800598B (en) | 2016-02-26 | 2016-02-26 | A method of it cutting graft process and prepares graphene |
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| CN105800598A true CN105800598A (en) | 2016-07-27 |
| CN105800598B CN105800598B (en) | 2018-10-09 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431998A (en) * | 2011-09-20 | 2012-05-02 | 深圳市长宜景鑫投资有限公司 | Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method |
| CN102674327A (en) * | 2012-05-17 | 2012-09-19 | 哈尔滨工业大学 | Environment-friendly method for preparing water-soluble grapheme at normal temperature |
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
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2016
- 2016-02-26 CN CN201610109503.1A patent/CN105800598B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431998A (en) * | 2011-09-20 | 2012-05-02 | 深圳市长宜景鑫投资有限公司 | Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method |
| CN102674327A (en) * | 2012-05-17 | 2012-09-19 | 哈尔滨工业大学 | Environment-friendly method for preparing water-soluble grapheme at normal temperature |
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
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| CN105800598B (en) | 2018-10-09 |
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Address after: No. 26 Shengli Road, Chunjiang Street, Xinbei District, Changzhou City, Jiangsu Province, 213000 Patentee after: Changzhou Jicang Nanomaterial Technology Co.,Ltd. Address before: Building 1017 and 1019, No. 311 Yanxin Road, Huishan Economic Development Zone, Wuxi City, Jiangsu Province, 214174 (Development Zone) Patentee before: WUXI JCNANO TECHNOLOGY Co.,Ltd. |