CN105220214B - A kind of preparation method of graphene film - Google Patents
A kind of preparation method of graphene film Download PDFInfo
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- CN105220214B CN105220214B CN201510778938.0A CN201510778938A CN105220214B CN 105220214 B CN105220214 B CN 105220214B CN 201510778938 A CN201510778938 A CN 201510778938A CN 105220214 B CN105220214 B CN 105220214B
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Abstract
The present invention provides a kind of preparation method of graphene film, comprises the following steps：S1：One copper foil is provided；S2：Electrochemical etching is carried out to the copper foil surface；S3：Graphene film is grown in the copper foil surface using chemical vapour deposition technique.The preparation method of the graphene film of the present invention is improved for existing method, by carrying out electrochemical etching on metal copper foil surface, the nucleation core of multi-layer graphene is formed, then 2 ~ 3 layers of graphene film is grown in copper foil surface with chemical vapour deposition technique can.The present invention can be with the controllable multi-layer graphene film of the large area deposition number of plies, to the practical significant of graphene.
Description
Technical field
The invention belongs to material to prepare manufacture field, is related to a kind of preparation method of graphene film.
Background technology
The crystal film material that graphene film is made up of single layer of carbon atom, there is high light transmittance, good electric conductivity
And pliability, suffer from being widely applied prospect in Flexible Displays, solar cell, lithium ion battery and sensor.Graphite
Alkene can be as transparent conductive electrode and the raw material of field-effect transistor in various flexible photoelectric devices.These applications will
Ask the graphene prepared that there is the performance that area is big, square resistance is low and transmitance is high.
Preparation large area is best suitable at present, the technique of high-quality graphene film is in metallic copper with chemical vapour deposition technique
Graphene is grown on paper tinsel.Its detailed process is：The surface of metal copper foil is cleaned with deionized water, alcohol and acetone equal solvent and done
Only, it is put into after drying in high temperature process furnances；Discharge inner air tube is simultaneously passed through hydrogen, by diamond heating to 1000 DEG C or so, then
The methane of certain flow is passed through as carbon source for growth graphene film；After the completion of growth, methane is closed, tube furnace is down to room temperature
And take out copper foil；The graphene film of copper foil surface is thus obtained being grown in.
This growing method utilizes metal copper foil as the catalyst to growth graphene film, the pattern of copper foil surface is to stone
The property of black alkene film has a major impact.Bilayer graphene can be formed at the defects of copper foil surface, and other regions cover with list
After layer graphene, catalyst is obstructed by graphene, can not just be further continued for playing a role.So graphene film finally prepared
Most of region is individual layer, but is wherein mingled with bilayer graphene scattered on a small quantity.In actual applications, single-layer graphene
Square resistance is too high, it is impossible to meets needs.And the square resistance of continuous bilayer or multi-layer graphene is lower, band structure also can
Change, more application potentials can have been given play to.Therefore, the controllable multi-layer graphene film of the large area deposition number of plies is to graphene
It is practical significant.
Therefore, how a kind of preparation method of graphene film is provided, it is thin with the graphene that the large area deposition number of plies is controllable
Film, turn into those skilled in the art's important technological problems urgently to be resolved hurrily.
The content of the invention
In view of the above the shortcomings that prior art, it is an object of the invention to provide a kind of preparation side of graphene film
Method, multi-layer graphene can not be grown on copper foil for solving existing growing method, realizes the large area of multi-layer graphene film
The problem of preparation.
In order to achieve the above objects and other related objects, the present invention provides a kind of preparation method of graphene film, including
Following steps：
S1：One copper foil is provided；
S2：Electrochemical etching is carried out to the copper foil surface；
S3：Graphene film is grown in the copper foil surface using chemical vapour deposition technique.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, in the step S1, the copper
The thickness range of paper tinsel is 10 μm~1mm.
As the present invention graphene film preparation method a kind of preferred scheme, in the step S1, in addition to
The step of being cleaned to the copper foil.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the side cleaned to the copper foil
Method includes：It is cleaned by ultrasonic copper foil surface with deionized water and organic solvent；After being cleaned by ultrasonic, using nitrogen by the copper foil table
Ground drying.
As the present invention graphene film preparation method a kind of preferred scheme, the organic solvent include ethanol,
One or more in isopropanol, acetone and acetic acid.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, in the step S2：To described
The method that copper foil surface carries out electrochemical etching includes：The copper foil is put into acid solution as anode, and a metal is provided
Negative electrode, apply voltage between the copper foil and the metallic cathode, electrochemical etching is carried out to the copper foil surface.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the acid solution includes sulfuric acid, salt
One or more in acid, nitric acid, orthophosphoric acid and acetic acid.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the material of the metallic cathode includes
One or more in gold, platinum, silver, copper, iron and aluminium.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the scope of the voltage is 1~
10V, the time range of electrochemical etching is 1~30min.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, in the step S3, first will
Cleaned by the copper foil of electrochemical etching, then again in its superficial growth graphene film.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the side cleaned to the copper foil
Method includes：Using copper foil surface described in deionized water rinsing at least once, then using nitrogen by the copper foil surface dry up.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, in the step S3, using change
Learn vapour deposition process includes in copper foil surface growth graphene film：The copper foil is put into firing equipment, discharges institute
The air in firing equipment is stated, and is passed through hydrogen, the firing equipment is then heated to preset temperature, then is passed through carbon source gas
Body, graphene film is grown in the copper foil surface.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, after the completion of growth, carbon source gas is closed
Body, the firing equipment is down to room temperature, and takes out the copper foil of superficial growth graphene film.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the firing equipment is tube furnace.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the preset temperature range is 900
~1060 DEG C.
As the present invention graphene film preparation method a kind of preferred scheme, the carbon-source gas include methane,
One or more in ethane, propane, acetylene, propine and ethanol.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, during the growth of the graphene film
Between be 5~120min.
As a kind of preferred scheme of the preparation method of the graphene film of the present invention, the graphene film includes bilayer
At least one of with three layer graphenes.
As described above, the preparation method of the graphene film of the present invention, has the advantages that：The present invention is with graphene
Preparation method be research object, be improved for existing method, by metal copper foil surface carry out electrochemical etching, shape
Into the nucleation core of multi-layer graphene, then grow in copper foil surface with chemical vapour deposition technique can 2~3 layers of graphene
Film.The present invention can have important meaning with the controllable multi-layer graphene film of the large area deposition number of plies to the practical of graphene
Justice.
Brief description of the drawings
Fig. 1 is shown as the process chart of the preparation method of the graphene film of the present invention.
The structural representation for the copper foil that the preparation method that Fig. 2 is shown as the graphene film of the present invention provides.
The preparation method that Fig. 3 is shown as the graphene film of the present invention is shown copper foil surface progress electrochemical etching
It is intended to.
Fig. 4 is shown as the structural representation of the copper foil by electrochemical etching in the preparation method of the graphene film of the present invention
Figure.
The preparation method that Fig. 5 is shown as the graphene film of the present invention is thin in copper foil surface growth graphene in tube furnace
The schematic diagram of film.
The copper foil that Fig. 6 is shown as superficial growth in the preparation method of the graphene film of the present invention and has graphene film is illustrated
Figure.
Component label instructions
S1~S3 steps
101 copper foils
102 acid solutions
103 metallic cathodes
104 be etched after copper foil surface
105 boiler tubes
106 air inlets
107 gas outlets
108 graphene films
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
Fig. 1 is referred to Fig. 6.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, the component relevant with the present invention is only shown in schema then rather than according to package count during actual implement
Mesh, shape and size are drawn, and kenel, quantity and the ratio of each component can be a kind of random change during its actual implementation, and its
Assembly layout kenel may also be increasingly complex.
The present invention provides a kind of preparation method of graphene film, referring to Fig. 1, being shown as the technological process of this method
Figure, comprises the following steps：
S1：One copper foil is provided；
S2：Electrochemical etching is carried out to the copper foil surface；
S3：Graphene film is grown in the copper foil surface using chemical vapour deposition technique.
Referring initially to Fig. 2, step S1 is performed：One copper foil 101 is provided.
Specifically, substrate and catalyst of the copper foil 101 as graphene growth.In the present embodiment, the copper foil 101
Thickness range be 10 μm~1mm, it is preferred to use 25 microns of thick copper foils.
Specifically, before graphene film is grown, in addition to the step of cleaned to the copper foil, to remove copper foil
The impurity on surface, the surface of cleaning is provided for graphene film growth, improve the quality of graphene film.
As an example, the method cleaned to the copper foil includes：It is cleaned by ultrasonic copper with deionized water and organic solvent
Paper tinsel surface；After being cleaned by ultrasonic, the copper foil surface is dried up using nitrogen.
Specifically, the organic solvent includes the one or more in ethanol, isopropanol, acetone and acetic acid.The ultrasound
The time of cleaning is 5~30 minutes.In the present embodiment, divided using ethanol and acetone as organic solvent, each ultrasonic time 5
Clock.
Referring next to Fig. 3 and Fig. 4, step S2 is performed：Electrochemical etching is carried out to the surface of copper foil 101.
Electrochemical etching refers to the method being etched using the electrochemical reaction of anodic solution to metal material surface.This
In step, the purpose that electrochemical etching is carried out to the surface of copper foil 101 is that the nucleation of multi-layer graphene is formed in copper foil surface
Core.
As an example, the method for electrochemical etching is carried out to the copper foil surface includes following process：
As shown in figure 3, the copper foil 101 is put into acid solution 102 as anode, and a metallic cathode 103 is provided,
Apply voltage between the copper foil 101 and the metallic cathode 103, electrochemical etching is carried out to the surface of copper foil 101.
Specifically, the acid solution includes the one or more in sulfuric acid, hydrochloric acid, nitric acid, orthophosphoric acid and acetic acid.The gold
Belonging to the material of negative electrode includes the one or more in gold, platinum, silver, copper, iron and aluminium.The scope of the voltage is 1~10V, electrification
The time range for learning etching is 1~30min.
In the present embodiment, using the orthophosphoric acid of 85% volume fraction, using material of the copper as metallic cathode, in the copper
Apply 5V voltage between paper tinsel 101 and the metallic cathode 103, the electrochemical etching time is 5 minutes.
As shown in figure 4, the copper foil being shown as in the preparation method of the graphene film of the present invention by electrochemical etching
Structural representation, it illustrated therein is the copper foil surface after being etched 104.
Fig. 5 and Fig. 6 is referred to again, performs step S3：Using chemical vapour deposition technique in the superficial growth stone of copper foil 101
Black alkene film 108.
In the present embodiment, it will be cleaned first by the copper foil of electrochemical etching, then again in its superficial growth
Graphene film.
As an example, the method cleaned to the copper foil includes：Using copper foil surface described in deionized water rinsing extremely
Lack once, such as 3~5 times, then dried up the copper foil surface using nitrogen.The cleaning step can remove the copper foil surface
The electrolyte of residual.
In the present embodiment, included using chemical vapour deposition technique in copper foil surface growth graphene film：By described in
Copper foil is put into firing equipment, discharges the air in the firing equipment, and is passed through hydrogen, then heats the firing equipment
To preset temperature, then carbon-source gas are passed through, graphene film is grown in the copper foil surface.Wherein, the preset temperature model
It is 900~1060 DEG C to enclose, and the carbon-source gas include the one or more in methane, ethane, propane, acetylene, propine and ethanol,
The growth time of the graphene film is 5~120min.
As an example, the firing equipment uses tube furnace.As shown in figure 5, discharged by gas outlet 107 in boiler tube 105
Air after, the hydrogen that flow is 50sccm is passed through by air inlet 106, by diamond heating to after 1000 DEG C, then is passed through stream
The methane for 10sccm is measured, grows graphene film.Certainly, in other embodiments, can also be set as needed using other
Standby and reaction condition, should not too it limit the scope of the invention herein.
After the completion of growth, carbon-source gas are closed, the firing equipment are down to room temperature, and take out superficial growth graphene
The copper foil of film.As shown in fig. 6, the superficial growth for being shown as the copper foil 101 has the schematic diagram of graphene film 108.This reality
Apply in example, the graphene film is bilayer graphene.
In other embodiments, gas flow and growth time when can also be grown by adjusting so that the graphene
Film 108 is three layer graphenes, or the subregion of the graphene film 108 is bilayer graphene, subregion is three layers
Graphene.Wherein, carbon source concentration is higher during growth, growth time is longer, is more readily obtained three layers of graphene.Laser microscope
The number of plies for the graphene film that test with Raman spectrum shows to obtain can regulate and control in 2~3 layers.
In summary, the preparation method of graphene film of the invention is improved for existing method, by metal
Copper foil surface carries out electrochemical etching, forms the nucleation core of multi-layer graphene, then with chemical vapour deposition technique can in copper
Paper tinsel superficial growth goes out 2~3 layers of graphene film.The present invention can with the controllable multi-layer graphene film of the large area deposition number of plies,
To the practical significant of graphene.So the present invention effectively overcomes various shortcoming of the prior art and has height
Spend industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (18)
1. a kind of preparation method of graphene film, it is characterised in that comprise the following steps：
S1：One copper foil is provided；
S2：Electrochemical etching is carried out to the copper foil surface, forms the nucleation core of multi-layer graphene；
S3：Multi-layer graphene film is grown in the copper foil surface using chemical vapour deposition technique.
2. the preparation method of graphene film according to claim 1, it is characterised in that：It is described in the step S1
The thickness range of copper foil is 10 μm~1mm.
3. the preparation method of graphene film according to claim 1, it is characterised in that：In the step S1, also wrap
Include the step of being cleaned to the copper foil.
4. the preparation method of graphene film according to claim 3, it is characterised in that：The copper foil is cleaned
Method includes：It is cleaned by ultrasonic copper foil surface with deionized water and organic solvent；After being cleaned by ultrasonic, using nitrogen by the copper foil
Surface dries up.
5. the preparation method of graphene film according to claim 4, it is characterised in that：The organic solvent includes second
One or more in alcohol, isopropanol, acetone and acetic acid.
6. the preparation method of graphene film according to claim 1, it is characterised in that：In the step S2：To institute
Stating the method for copper foil surface progress electrochemical etching includes：The copper foil is put into acid solution as anode, and a gold medal is provided
Belong to negative electrode, apply voltage between the copper foil and the metallic cathode, electrochemical etching is carried out to the copper foil surface.
7. the preparation method of graphene film according to claim 6, it is characterised in that：The acid solution include sulfuric acid,
One or more in hydrochloric acid, nitric acid, orthophosphoric acid and acetic acid.
8. the preparation method of graphene film according to claim 6, it is characterised in that：The material bag of the metallic cathode
Include the one or more in gold, platinum, silver, copper, iron and aluminium.
9. the preparation method of graphene film according to claim 6, it is characterised in that：The scope of the voltage is 1~
10V, the time range of electrochemical etching is 1~30min.
10. the preparation method of graphene film according to claim 1, it is characterised in that：In the step S3, first
It will be cleaned by the copper foil of electrochemical etching, then again in its superficial growth graphene film.
11. the preparation method of graphene film according to claim 10, it is characterised in that：The copper foil is cleaned
Method include：Using copper foil surface described in deionized water rinsing at least once, then using nitrogen by the copper foil surface dry up.
12. the preparation method of graphene film according to claim 1, it is characterised in that：In the step S3, use
Chemical vapour deposition technique includes in copper foil surface growth graphene film：The copper foil is put into firing equipment, discharged
Air in the firing equipment, and hydrogen is passed through, the firing equipment is then heated to preset temperature, then be passed through carbon source gas
Body, graphene film is grown in the copper foil surface.
13. the preparation method of graphene film according to claim 12, it is characterised in that：After the completion of growth, carbon is closed
Source gas, the firing equipment is down to room temperature, and takes out the copper foil of superficial growth graphene film.
14. the preparation method of graphene film according to claim 12, it is characterised in that：The firing equipment is tubular type
Stove.
15. the preparation method of graphene film according to claim 12, it is characterised in that：The preset temperature range is
900~1060 DEG C.
16. the preparation method of graphene film according to claim 12, it is characterised in that：The carbon-source gas include first
One or more in alkane, ethane, propane, acetylene, propine and ethanol.
17. the preparation method of graphene film according to claim 12, it is characterised in that：The life of the graphene film
It is for a long time 5~120min.
18. the preparation method of graphene film according to claim 1, it is characterised in that：The graphene film includes
At least one of double-deck and three layer graphenes.
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| CN107037933A (en) * | 2016-02-04 | 2017-08-11 | 中国科学院金属研究所 | A kind of preparation method of the grapheme capacitive touch screen of three layers of transparent electrode structure |
| CN105836735A (en) * | 2016-03-25 | 2016-08-10 | 西安电子科技大学 | Preparation method for ultra-three-dimension graphene |
| CN106698408B (en) * | 2016-12-30 | 2019-09-10 | 武汉理工大学 | A kind of concave structure single crystal graphene and preparation method thereof |
| CN108539581B (en) * | 2018-05-23 | 2020-06-26 | 西北核技术研究所 | Metal-based graphene film cathode gas spark switch |
| CN109440226A (en) * | 2018-06-29 | 2019-03-08 | 同济大学 | A kind of preparation method of high-strength light conductive graphene fiber |
| CN111741607B (en) * | 2020-06-19 | 2021-05-18 | 辽宁格莱菲尔健康科技有限公司 | Method for compositely integrating reduced graphene oxide high-sensitivity sensing circuit and latex |
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| JPH0878817A (en) * | 1994-08-31 | 1996-03-22 | Tsurumi Soda Co Ltd | Etching method |
| JP3709221B2 (en) * | 1994-10-06 | 2005-10-26 | 古河サーキットフォイル株式会社 | Copper foil surface roughening treatment method |
| CN102134067B (en) * | 2011-04-18 | 2013-02-06 | 北京大学 | Method for preparing single-layer graphene |
| CN102794945B (en) * | 2011-05-27 | 2014-08-20 | 清华大学 | Method for preparing graphene carbon nano tube composite membrane structure |
| CN102400109A (en) * | 2011-11-11 | 2012-04-04 | 南京航空航天大学 | Method for growing large area of layer-number-controllable graphene at low temperature through chemical vapor deposition (CVD) method by using polystyrene solid state carbon source |
| CN103466609B (en) * | 2013-09-25 | 2015-02-18 | 电子科技大学 | Preparation method of double-layer graphene films |
| US10072355B2 (en) * | 2014-04-15 | 2018-09-11 | Board Of Regents, The University Of Texas System | Methods of forming graphene single crystal domains on a low nucleation site density substrate |
| CN104694939A (en) * | 2015-04-07 | 2015-06-10 | 河南红日铜箔科技有限公司 | Surface treatment technology for ultralow-surface-roughness copper foil |
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Effective date of registration: 20221017 Address after: 201203 Pudong New Area, Shanghai, China (Shanghai) free trade trial area, 887 Lane 73, Chong Chong Road. Patentee after: PYLON TECHNOLOGIES Co.,Ltd. Address before: No. 99, Pudong New Area Road, Shanghai, Shanghai Patentee before: SHANGHAI ADVANCED Research Institute CHINESE ACADEMY OF SCIENCES |