CN103569999B - A kind of preparation method of Graphene - Google Patents
A kind of preparation method of Graphene Download PDFInfo
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- CN103569999B CN103569999B CN201210248634.XA CN201210248634A CN103569999B CN 103569999 B CN103569999 B CN 103569999B CN 201210248634 A CN201210248634 A CN 201210248634A CN 103569999 B CN103569999 B CN 103569999B
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Abstract
The invention provides the preparation method of a kind of Graphene, comprise the following steps: glucide is mixed with graphite oxide in mass ratio 0.01～0.2:1, add deionized water, ultrasonic 30～60 minutes, obtain the mixed solution of glucide and graphene oxide；Mixed solution is filtered, after the filtering residue obtained is dried 12 ~ 24 hours at 60 ~ 80 DEG C, is placed in reacting furnace；Heating reaction furnace, to 300～600 DEG C, is incubated and reacts for 10～30 minutes, after question response terminates, be cooled to room temperature, opens reacting furnace, collects solid product, and this solid product is Graphene.The graphene preparation method that the present invention provides, preparation technology is simple, it is easy to accomplish large-scale industrial produces, and the Graphene prepared has loose structure, and crystal structure is complete, functional, can be applicable to quieter material, gas adsorption material etc..
Description
Technical field
The present invention relates to field of preparation of graphene, particularly relate to the system of a kind of Graphene with loose structure
Preparation Method.
Background technology
Graphene is that peace moral strong K sea nurse (Andre K.Geim) of Univ Manchester UK in 2004 etc. finds
A kind of Two-dimensional Carbon atomic crystal.Owing to structure and the photoelectric property of its uniqueness become material with carbon element, nanometer
The study hotspot in the fields such as technology, Condensed Matter Physics and functional material, has attracted many scientific workers.Single
Layer graphene has excellent conduction, heat conductivility and low thermal coefficient of expansion, and its theoretical specific surface area
Up to 2630m2/ g (A Peigney, Ch Laurent, et al.Carbon, 2001,39,507), can be used for effect
Transistor, electrode material, composite, liquid crystal display material, sensor etc..Prepare Graphene at present
Method mainly have graphite breakaway (Novoselov K S, Geim A K, et al.Science 2004,306,666),
Chemistry redox method [D A Dikin, et al.Nature 2007,448,457；Sasha Stankovich,
Dmitriy A Dikin, Richard D Piner, et al.Carbon 2007,45,1558], ultrasonic stripping method
(Guohua Chen, Wengui Weng, Dajun Wu, et al.Carbon.2004,42,753) and chemical gaseous phase
Sedimentation (Alexander N, Obraztsov.Nature nanotechnology.2009,4,212) etc..These
Method presently, there are the place of some shortcomings, such as complicated process of preparation, is difficult to prepare the Graphene of specific morphology
Deng, Chinese patent CN 101993056 A, CN 102107868 A etc. both provide the preparation of porous graphene
Method, but the operation of these methods is excessively complicated.
Summary of the invention
For solving the problems referred to above, it is desirable to provide the preparation method of a kind of Graphene, the method can be quick
Effectively prepare yield height, hole enriches, Graphene of good performance, and prepared porous graphene can be applied
In quieter material, gas adsorption material etc..
The preparation method of the Graphene that the present invention provides, comprises the following steps:
(1) glucide is mixed with graphite oxide in mass ratio 0.01～0.2:1, adds deionized water,
Ultrasonic 30～60 minutes, obtain the mixed solution of described glucide and graphene oxide；
(2) described mixed solution is filtered, after the filtering residue obtained is dried 12～24 hours at 60～80 DEG C,
It is placed in reacting furnace；
(3) heat described reacting furnace to 300～600 DEG C, be incubated and react for 10～30 minutes, question response
After end, being cooled to room temperature, open reacting furnace, collect solid product, this solid product is Graphene.
Step (1) is the process preparing glucide with the mixed solution of graphene oxide.By glucide with
After graphite oxide mixing, utilizing Ultrasound Instrument by mixture ultrasonic disperse in water, graphite oxide is ultrasonic to be peeled off into
Graphene oxide.
Preferably, glucide is sucrose, glucose, fructose, maltose or starch.
Preferably, the concentration of mixed solution is 0.1～10g/L.
Step (2), for filtering glucide and graphene oxide mixed solution, obtains filtering residue and is dried place
The process of reason.Graphene oxide is by glucide solution immersion so that surface of graphene oxide and interlayer are equal
Even it is attached with substantial amounts of glucide.
Preferably, filter residue and drying is placed on quartz boat, and quartz boat is placed in reacting furnace.
Step (3) is the process that pyroreaction generates Graphene.
Under the high temperature of 300～600 DEG C, graphene oxide is decomposed, and decomposites aqueous vapor, carbon dioxide etc.
Gas, and generate Graphene, meanwhile, glucide is also because of pyrolytic, carbonization and stay abundant
Hole, also can fill up the carbon atom disappearance produced in graphene oxide catabolic process simultaneously, reduce Graphene
Defect, thus the Graphene for preparing of the present invention has loose structure and Conductivity Ratio general oxidation-reduction method institute
Obtaining Graphene electrical conductivity high, aperture is 50～500nm, and the thickness of Graphene is 1～5nm.
The method preparing Graphene that the present invention provides, with graphite oxide as raw material, preparation technology is simple, raw material
Wide material sources, low cost, it is easy to accomplish large-scale industrial produces；Whole process does not use any chemical reagent,
Substantially without to environment, it is achieved that prepared by the green non-pollution of Graphene；And by system of the present invention
The Graphene that Preparation Method prepares has loose structure, and crystal structure is complete, and hole is abundant uniformly, can be applicable to
Quieter material, gas adsorption material etc..
Accompanying drawing explanation
Fig. 1 is the Graphene SEM figure obtained by the embodiment of the present invention one.
Detailed description of the invention
The following stated is the preferred embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, this
A little improvements and modifications are also considered as protection scope of the present invention.
Embodiment one
The preparation method of a kind of Graphene, comprises the following steps:
(1) sucrose and graphite oxide are mixed during 0.1:1 joins beaker in mass ratio, add go from
Sub-water, is placed in beaker in Ultrasound Instrument ultrasonic 60 minutes, obtains sucrose and graphite oxide that concentration is 10g/L
The mixed solution of alkene；
(2) mixed solution is filtered, after the filtering residue obtained is dried 24 hours at 60 DEG C, takes out and be placed in stone
On Ying Zhou, and quartz boat is moved in reacting furnace；
(3) heating reaction furnace is to 300 DEG C, is incubated and reacts for 20 minutes, after question response terminates, the coldest
But to room temperature, collecting solid product, this solid product is the Graphene with loose structure.
The aperture of the Graphene of the present embodiment gained loose structure is 50～300nm.
Fig. 1 is the Graphene SEM figure obtained by the embodiment of the present invention one.From figure 1 it appears that graphite
Alkene is the most successfully prepared, and obtained Graphene thickness is 1～5nm, and has abundant multi-level hole
Structure, aperture is 50～300nm.
Embodiment two
The preparation method of a kind of Graphene, comprises the following steps:
(1) glucose and graphite oxide being mixed during 0.2:1 joins beaker in mass ratio, addition is gone
Ionized water, is placed in beaker in Ultrasound Instrument ultrasonic 30 minutes, obtains glucose and oxidation that concentration is 3g/L
The mixed solution of Graphene；
(2) mixed solution is filtered, after the filtering residue obtained is dried 18 hours at 70 DEG C, takes out and be placed in stone
On Ying Zhou, and quartz boat is moved in reacting furnace；
(3) heating reaction furnace is to 450 DEG C, is incubated and reacts for 30 minutes, after question response terminates, the coldest
But to room temperature, collecting solid product, this solid product is the Graphene with loose structure.
The aperture of the Graphene of the present embodiment gained loose structure is 50～500nm, Graphene thickness be 1～
5nm。
Embodiment three
The preparation method of a kind of Graphene, comprises the following steps:
(1) fructose and graphite oxide being mixed during 0.01:1 joins beaker in mass ratio, addition is gone
Ionized water, is placed in beaker in Ultrasound Instrument ultrasonic 50 minutes, obtains fructose and oxidation stone that concentration is 0.1g/L
The mixed solution of ink alkene；
(2) mixed solution is filtered, after the filtering residue obtained is dried 12 hours at 80 DEG C, takes out and be placed in stone
On Ying Zhou, and quartz boat is moved in reacting furnace；
(3) heating reaction furnace is to 500 DEG C, is incubated and reacts for 20 minutes, after question response terminates, the coldest
But to room temperature, collecting solid product, this solid product is the Graphene with loose structure.
The aperture of the Graphene of the present embodiment gained loose structure is 50～200nm, Graphene thickness be 1～
5nm。
Embodiment four
The preparation method of a kind of Graphene, comprises the following steps:
(1) maltose and graphite oxide are mixed during 0.05:1 joins beaker in mass ratio, add
Deionized water, is placed in beaker in Ultrasound Instrument ultrasonic 40 minutes, obtains maltose and oxygen that concentration is 0.5g/L
The mixed solution of functionalized graphene；
(2) mixed solution is filtered, after the filtering residue obtained is dried 24 hours at 60 DEG C, takes out and be placed in stone
On Ying Zhou, and quartz boat is moved in reacting furnace；
(3) heating reaction furnace is to 600 DEG C, is incubated and reacts for 10 minutes, after question response terminates, the coldest
But to room temperature, collecting solid product, this solid product is the Graphene with loose structure.
The aperture of the Graphene of the present embodiment gained loose structure is 50～300nm, Graphene thickness be 1～
5nm。
Embodiment five
The preparation method of a kind of Graphene, comprises the following steps:
(1) starch and graphite oxide are mixed during 0.1:1 joins beaker in mass ratio, add go from
Sub-water, is placed in beaker in Ultrasound Instrument ultrasonic 30 minutes, obtains starch and graphite oxide that concentration is 7g/L
The mixed solution of alkene；
(2) mixed solution is filtered, after the filtering residue obtained is dried 24 hours at 60 DEG C, takes out and be placed in stone
On Ying Zhou, and quartz boat is moved in reacting furnace；
(3) heating reaction furnace is to 500 DEG C, is incubated and reacts for 20 minutes, after question response terminates, the coldest
But to room temperature, collecting solid product, this solid product is the Graphene with loose structure.
The aperture of the Graphene of the present embodiment gained loose structure is 50～300nm, Graphene thickness be 1～
5nm。
Using the electrical conductivity of the Graphene of four probe instrument testing example 1～5 preparations, it tests knot
Fruit is as shown in table 1:
The electrical conductivity of the Graphene of table 1 embodiment 1～5 preparation
| Embodiment | 1 | 2 | 3 | 4 | 5 |
| Electrical conductivity 104S/m | 4.6 | 0.8 | 3.3 | 1.9 | 1.2 |
The Graphene prepared by preparation method of the present invention has loose structure, and crystal structure is complete, and hole enriches
Uniformly, can be applicable to quieter material, gas adsorption material etc..
The above is the preferred embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, this
A little improvements and modifications are also considered as protection scope of the present invention.
Claims (6)
1. the preparation method of a Graphene, it is characterised in that comprise the following steps:
(1) glucide is mixed with graphite oxide in mass ratio 0.01～0.2:1, adds deionized water,
Ultrasonic 30～60 minutes, obtain the mixed solution of described glucide and graphene oxide；
(2) described mixed solution is filtered, after the filtering residue obtained is dried 12 ~ 24 hours at 60 ~ 80 DEG C,
It is placed in reacting furnace；
(3) heat described reacting furnace to 300～600 DEG C, be incubated and react for 10～30 minutes, question response
After end, being cooled to room temperature, open described reacting furnace, collect solid product, this solid product is graphite
Alkene.
2. the preparation method of Graphene as claimed in claim 1, it is characterised in that described glucide is
Sucrose, glucose, fructose, maltose or starch.
3. the preparation method of Graphene as claimed in claim 1, it is characterised in that described mixed solution
Concentration is 0.1 ~ 10g/L.
4. the preparation method of Graphene as claimed in claim 1, it is characterised in that after described filter residue and drying
Being placed on quartz boat, described quartz boat is placed in described reacting furnace.
5. the preparation method of Graphene as claimed in claim 1, it is characterised in that described Graphene has
Loose structure, aperture is 50～500nm.
6. the preparation method of Graphene as claimed in claim 1, it is characterised in that the thickness of described Graphene
Degree is 1～5nm.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103794204A (en) * | 2014-02-17 | 2014-05-14 | 东南大学 | Application method of graphene macroscopic materials |
| CN104118866A (en) * | 2014-06-25 | 2014-10-29 | 苏州世优佳电子科技有限公司 | Method for preparing graphene on basis of biological reduction process |
| CN105565304B (en) * | 2015-12-28 | 2017-09-05 | 成都新柯力化工科技有限公司 | A kind of method that utilization starch prepares graphene |
| CN105668562A (en) * | 2016-04-13 | 2016-06-15 | 北京晶晶星科技有限公司 | Preparation method of graphene |
| CN105883786B (en) * | 2016-04-13 | 2018-05-22 | 北京晶晶星科技有限公司 | A kind of graphene oxide solid phase dispersion system, its preparation method and its application |
| CN108314421A (en) * | 2018-01-03 | 2018-07-24 | 广东净雨环保科技有限公司 | One type graphene enhances the preparation method of architectural pottery |
| CN108101035B (en) * | 2018-03-06 | 2020-03-13 | 绍兴文理学院 | Green preparation method of high-quality graphene |
| CN108806662B (en) * | 2018-04-27 | 2022-12-09 | 北京石墨烯技术研究院有限公司 | Preparation method of graphene porous material for sound insulation and noise reduction |
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| CN101993056B (en) * | 2010-12-01 | 2012-05-30 | 天津大学 | Graphene-based porous macroscopic carbon material and preparation method thereof |
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