CN102897750A - PrPrearation method for graphene film - Google Patents
PrPrearation method for graphene film Download PDFInfo
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- CN102897750A CN102897750A CN2011102158567A CN201110215856A CN102897750A CN 102897750 A CN102897750 A CN 102897750A CN 2011102158567 A CN2011102158567 A CN 2011102158567A CN 201110215856 A CN201110215856 A CN 201110215856A CN 102897750 A CN102897750 A CN 102897750A
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Abstract
The invention discloses a preparation method for a graphene film. The method comprises the steps of putting small sheets of the in advance synthetic graphene film on a substrate, and growing the graphene film on the substrate by using the small sheets of the in advance synthetic graphene film as induced points for the growth of s large-area graphene film and adopting carbon atoms released by carbon atom-containing gas carbon source, solid carbon source, liquid carbon source or composite carbon source materials thereof. The graphene film can directly grow on the substrate of practical application graphene film, so that the graphene film needs not to be transferred when being used. The number of layers, the structure and the size of the prepared graphene film are easy to control; the temperature for growing the graphene film can be 0 DEG C-2000 DEG C; the prepared graphene film has excellent photoelectric characteristics and is suitable for large-scale manufacture of optoelectronic devices.
Description
Technical field
The present invention relates to graphene film, relate in particular to a kind of preparation method of graphene film.
Background technology
Graphene is that mono-layer graphite is otherwise known as by the former molecular two-dirnentional structure material of cellular monolayer carbon; On physical property, it has been generally acknowledged that the material that Graphene is piled up more than ten layers is exactly the graphite of three-dimensional structure, carbon nanotube is the monodimension nanometer material that is rolled into tubbiness by Graphene.Graphene has remarkable two-dimentional electricity, optics, calorifics, mechanical property and chemical stability, the crystallography quality of its unique two-dirnentional structure and excellence is so that it is at supper-fast micro-nano opto-electronic device, radio-frequency devices, the fields such as clear energy sources and various kinds of sensors have important practical value.Such as, electronics is followed relativistic quantum mechanics in Graphene, there is not rest mass, ultraspeed operation with 1/300 light velocity, show unusual room temperature quantum hall effect and ballistic transport phenomenon, can prepare room temperature ballistic transport transistor, be regarded as the important foundation novel material of Future Information nano-device; Graphene electric transmission speed is 150 times of silicon, is expected to supper-fast computer and radio-frequency devices that the speed of preparing reaches megahertz; The susceptibility of the unit molecule degree of Graphene is expected to be used widely such as fields such as gas sensor and biosensors at various sensors; Graphene has the optical characteristics of 2.3% photoabsorption, make it can be for the preparation of supper-fast photo-detector and mode locked laser, on the other hand, because extremely low optical absorption characteristics, so that Graphene both can be used for preparing opto-electronic device, such as the transparency electrode of photodiode and solar cell etc., thereby replace cost costliness, resource scarcity, the not collapsible ITO nesa coating take indium as main component, also can be used for preparing ultracapacitor and lithium ion battery; Effciency of energy transfer based on the solar battery of Graphene is expected to reach 24%.
The preparation method of graphene film comprise the mechanically peel method [K. S. Novoselov,
Et al. Science 306,666 (2004) .], solution stripping method [X. L. Li, et al. Science 319,1229 (2008) .], chemistry redox method [D. A. Dikin, et al. Nature 448,457 (2007). Z. S. Wu, et al. Carbon 47,493 (2009) .], silicon carbide thermal decomposition method [C. Berger
Et al. Science 312,1191 (2006); A. Tzalenchuk, et al. Nature Nanotechnol 5,186 (2010) .], chemical Vapor deposition process (CVD) [C. A. Di, et al. Adv. Mater. 20,3289 (2008); A. Reina, et al. Nano Lett. 9,30 (2009); K. S. Kim, et al. Nature 457,706 (2009) .], carbon segregation method (segregation) etc.Wherein the shape of the graphene film prepared of mechanically peel method, solution stripping method and chemistry redox method all is random basically, and the number of plies of graphene film and size are difficult to control; Although the mechanically peel method can produce the Graphene of perfect lattice, only be adapted to fundamental research, be not suitable for large-scale application.The silicon carbide thermal decomposition method is a kind of method of solid carbon source growing graphene film, its basic step is included under the ultrahigh vacuum(HHV), pyroprocessing silicon carbide with about 1400 ℃, Siliciumatom is evaporated and allow carbon atom form graphene film at silicon carbide, this method requires very high, very harsh to preparation condition, and is difficult to obtain the single uniform graphene film of the number of plies.Chemical Vapor deposition process (CVD) is to use gaseous carbon source growing graphene film on metal catalytic layer, except utilizing gaseous carbon source, also utilize the solid carbon source [J. M. Tour,
Et al.Nature 468,549 (2010)] and liquid carbon source [F. Muller,
Et al.Small 5,2291 (2009); Y. Miyata,
Et al.Applied Physics Letters 96,263105 (2010)] adopt and to be similar to chemical Vapor deposition process synthesizing graphite alkene film on the substrate of metal catalytic is being arranged.Carbon segregation method (segregation) is at first carbon atom to be doped in the metal catalytic layer, then through Overheating Treatment carbon atom is disengaged from metal catalytic layer, thereby forms graphene film in the metallic surface.
Chemical Vapor deposition process and carbon segregation method can big area synthesizing graphite alkene films, and can control preferably to a certain extent the number of plies of graphene film, be adapted to large-scale application, but must adopt metal catalytic layer and on this metal catalytic substrate the synthesizing graphite alkene film, synthesis temperature is generally more than 650 ℃.Like this, must just can use graphene film with transferring on other target substrate such as the insulating substrate at the synthetic big area graphene film of metal substrate during the practical application graphene film; Also there is very large challenge at present big area transfer graphene film, therefore, if there is technological method graphene film can be grown directly upon on the substrate such as isolator or semiconducter substrate that is fit to the graphene film particular application technology, to not need transfer step, also can avoid the variation of the graphene film texture quality that caused by transfer process; This will speed up Graphene technical development and practical application.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of simple preparation method who is suitable for the graphene film of large area deposition is provided, for this reason, the present invention is by the following technical solutions: choose a small pieces graphene film from pre-synthesis graphene film, described small pieces graphene film is transferred to conductor, as the starting point of inducing the graphene film growth, come from solid carbon source in described substrate employing on the substrate of semi-conductor or isolator, the liquid carbon source, the carbon atom that any two or more mixed carbon source discharges in gaseous carbon sources or the aforementioned carbon source is take the small pieces graphene film as starting point growing graphene film.
Described conduct induce the graphene film small pieces of graphene film large area deposition be selected from by micromechanics peel off, liquid phase is peeled off, chemical vapour deposition, carbon segregation, chemistry redox reaction, decompose solid-phase carbon source or decompose the method for phase carbon source and synthetic graphene film.
Conductor, semi-conductor or insulator substrates that described conduct is used for the large area deposition graphene film are inorganic materials, organic polymer material or its matrix material that is suitable for the graphene film particular application technology, such as: be metal or alloy; For preparing at present Si, Ge, Ge-Si, Se, GaN, GaAs, GaAsN, InP, ZnS, CdTe, HgTe, InAs-InP, GaAs-GaP, the ZnGeP of semiconducter device
2, ZnGeAs
2, CdGeAs
2, CdSnSe
2, CuGaSe
2, AgInTe
2, AgTlTe
2, CuInSe
2, CuAlS
2, Cu
3AsSe
4, Ag
3AsTe
4, Cu
3SbS
4, Ag
3SbSe
4, Cu
2FeSnS
4, the inorganic semiconductor material such as ZnO, CuO and pentacene, poly--3 alkylthrophenes of P3HT(), C
60, PCBM, PPV(be poly-to vinylbenzene), the organic semiconductor material such as naphthalene, anthracene, polyacrylonitrile, phthalocyanine; Be SiO
2, Al
2O
3, HfO
2, BN, SiN
x, the insulating material such as SiC, AlN, mica, glass, pottery, sapphire, polyvinyl alcohol, poly-(4-Vinyl phenol), divinyl tetramethyl disiloxane-two (benzocyclobutene), polyethylene terephthalate (PET), polymethylmethacrylate (PMMA), Derlin, chloroprene rubber, polyvinyl chloride, styrene-butadiene rubber(SBR), polymeric amide, trimeric cyanamide, polyethylene, tetrafluoroethylene, but be not limited to above material.
Described gaseous carbon source, solid-state carbon source, liquid carbon source material or mixed carbon source material refer to contain the material of the carbon atoms that discharges easily carbon atom, comprise alkane such as methane etc., alkene such as ethene etc., alkynes such as acetylene etc., aromatic hydrocarbon such as benzene, alcohol are such as ethanol etc., ketone such as acetone etc., graphite, the material of the carbon containings such as carbon pipe, but be not limited to above material.
The method that described carbon source material from carbon atoms discharges carbon atom is through Overheating Treatment, sputtering method, laser treatment, Cement Composite Treated by Plasma or decomposition reaction.
It can be arbitrary shape that the shape of graphene film small pieces is a little induced in described conduct, such as square, rectangle, circle, ellipse or irregular type; Be 1 layer to 200 layers as the number of plies of inducing graphene film small pieces a little, be preferably 1 layer to 20 layers, optimum is 1 layer to 5 layers; Be 1nm as the area of inducing graphene film small pieces a little
2To 50000cm
2, optimum is 1nm
2To 1000cm
2, the most optimum is 1nm
2To 100um
2
The number of plies of described graphene film of growing in conductor, semi-conductor or insulator substrates is 1 layer to 200 layers, is preferably 1 layer to 20 layers, and optimum is 1 layer to 5 layers.
The temperature of growing graphene film is 0 ℃ to 2000 ℃, is preferably 50 ℃ to 1000 ℃, and optimum is 50 ℃ to 600 ℃.
The method for preparing graphene film of the present invention is to adopt pre-synthesis graphene film sheet and induce the graphene film large area deposition; Because the graphene film small pieces can be placed on conductor, semi-conductor or insulator substrates, thus can be on any target substrate the large area deposition graphene film, just do not need to shift again like this graphene film during using mineral carbon alkene film; The underlayer temperature of growing graphene film can be suitable for the low-temperature epitaxy graphene film between 50 ℃ to 600 ℃, be compatible with existing semi-conductor industry; The thickness of graphene film, structure, size are controlled easily; Prepare graphene film and have excellent photoelectric characteristic, be applicable to make on a large scale high performance opto-electronic device.
Description of drawings
Fig. 1 is the synoptic diagram that the present invention prepares graphene film: (a) extract small pieces and transfer on the substrate from pre-synthesis graphene film, (b) with the small pieces graphene film that shifts for inducing a little, utilization by the carbon atom of the gaseous carbon source that contains carbon atom, liquid carbon source, solid-state carbon source or its mixed carbon source material production at the Grown graphene film;
Fig. 2 for the single-layer graphene of mechanically peel method preparation as the small pieces Graphene that brings out the Graphene large area deposition, at SiO
2The optical microscope image of Grown single-layer graphene;
Fig. 3 for the double-layer graphite alkene of chemical gaseous phase depositing process preparation as the small pieces Graphene that brings out Graphene and grow, at the Raman collection of illustrative plates of polymer P ET Grown double-layer graphite alkene;
The small pieces Graphene of Fig. 4 for growing as bringing out Graphene take the single-layer graphene of mechanically peel method preparation is at the scanning electron microscope image of Au Grown single-layer graphene;
Fig. 5 for the minority layer graphene film of redox chemical process preparation as the small pieces graphene film that brings out Graphene and grow, at the Auger electron collection of illustrative plates of Si Grown graphene film.
Embodiment
As shown in Figure 1, the preparation method of graphene film adopts to select a small pieces graphene film 2 from pre-synthesis graphene film 1, the small pieces graphene film of choosing is positioned on the substrate 3 that is adapted to the graphene film particular application technology, utilize come from the carbon atom 4 that discharges in gaseous carbon source, liquid carbon source, solid-state carbon source or its mixed carbon source material that contains carbon atom and on substrate 3 growing graphene film 5.
Described graphene film sheet be select in peeled off by micromechanics, liquid phase is peeled off, chemical vapour deposition, carbon segregation, chemistry redox reaction, decompose solid-phase carbon source or decompose the method for phase carbon source and synthetic graphene film.Be shaped as square, rectangle, circle, ellipse or irregular type as the graphene film sheet that brings out graphene film growth; The number of plies as the graphene film sheet that brings out the graphene film growth is 1 layer to 200 layers, and optimum is 1 layer to 20 layers, and the most optimum is 1 layer to 5 layers; Area as the graphene film sheet that brings out the graphene film growth is 1nm
2To 50000 cm
2, optimum is 1nm
2To 1000 cm
2, the most optimum is 1nm
2To 100um
2Described substrate material is inorganic or organic conductor, semi-conductor, isolator or its matrix material that is applicable to the graphene film particular application technology.Described gaseous carbon source, solid-state carbon source, liquid carbon source material or its mixed carbon source refer to contain the material by carbon atom, and be optimum for discharging easily the material of carbon atom.The number of plies of described graphene film at Grown is 1 layer to 200 layers, and optimum is 1 layer to 20 layers, and the most optimum is 1 layer to 5 layers.
Embodiment 1: utilize the single-layer graphene of mechanically peel method preparation as the Graphene small pieces of inducing the Graphene large area deposition, at SiO
2The Grown graphene film
Utilize the Scotch adhesive tape of 3M company to adopt the mechanically peel method from the standby single-layer graphene of Pintsch process graphite-made, and transfer to SiO
2The graphene film small pieces of Graphene growth are brought out in conduct on the substrate; The SiO that the graphene film small pieces will be arranged
2Substrate is positioned in the ultrahigh vacuum(HHV) (6.0 * 10
-9Torr) carry out 1000 oC thermal treatments 5 minutes; Subsequently, at the logical H of 800oC
2With C
2H
4Mixed gas, at SiO
2Graphene small pieces on the substrate are induced Graphene growth 5 minutes; Drop at last room temperature, thereby at SiO
2The substrate large area deposition single-layer graphene (Fig. 2).
Effect: SiO
2The important dielectric materials of contemporary silica-based electron device, numeral/logical circuit, directly at SiO
2Insulating substrate growing graphene film will speed up the integrated of Graphene technology and contemporary optoelectronics industry, reduces cost.
Embodiment 2: utilize the Graphene small pieces of being induced the Graphene large area deposition by the double-layer graphite alkene conduct of chemical gaseous phase depositing process preparation, prepare graphene film at polymer poly ethylene glycol terephthalate (PET) substrate
The thick Cu sheet of 25um after polishing and the surface treatment is positioned in the high vacuum (1.0 * 10
-8Torr) carry out 1000 oC thermal treatments 30 minutes; Subsequently, logical CH
4Gas and H
2Gas growth 2 minutes; With 15oC/ minute rate of temperature fall with the near room temperature of temperature, thereby obtain double-layer graphite alkene at the Cu film.Shift a fritter Graphene to polymer P ET from Cu: spin coating 500nm polymethylmethacrylate (PMMA) layer on synthetic Graphene surface, Graphene/the Cu that scribbles PMMA is positioned in the iron nitrate solution Cu erosion is fallen, thereby obtain the PMMA/ Graphene, then the PMMA/ Graphene is transferred on the PET, fall PMMA with acetone solution subsequently, small pieces double-layer graphite alkene has been transferred on the PET like this.
, will produce carbon atom by liquid ethanol and be incorporated into the PET substrate zone that is placed with a fritter graphene film that temperature is 100oC, thereby induce graphene film large area deposition (Fig. 3) on PET with these Graphene small pieces as carrier with Ar gas.
Effect: various flat pannel display, touch screen and solar cell etc. all need ELD, flexible device is more and more attracted attention, PET is transparent flexible materials, Graphene that directly will transparent conduction under lower temperature is grown on the PET, lays a good foundation for developing soft graphite alkene conductive, transparent membrane technique.
Embodiment 3: with the single-layer graphene of mechanically peel method preparation as the Graphene small pieces of inducing the Graphene large area deposition, at golden substrate growing graphene
Utilize the Scotch adhesive tape of 3M company to adopt the mechanically peel method from the standby single-layer graphene of Pintsch process graphite-made, and transfer on the Au substrate as the Graphene small pieces of inducing the Graphene large area deposition at Au.The Au substrate that is loaded with the Graphene small pieces is positioned over sputtering chamber, adopt sputtering method that carbon atom is splashed on the Au substrate from the agraphitic carbon target, thus the Graphene small pieces that shift brought out on the Au substrate under the underlayer temperature of 300 oC growing graphene (Fig. 4).
Effect: gold waits the resource-constrained of noble metal material, and Graphene has excellent physical strength and the transparency, and directly plating one layer graphene helps to protect the precious materials of gold on the surface of gold etc.
Embodiment 4: with the minority layer graphene film of redox chemical process preparation as the Graphene small pieces of inducing the Graphene large area deposition, at Si Grown graphene film
Adopt redox chemical process that graphite oxidation is become graphite oxide, graphite oxide is through supersound process and centrifugal and graphite oxide is split up into graphene oxide; Then graphene oxide being inserted pure hydrazine solution obtains as the Graphene small pieces of inducing the Graphene large area deposition through reduction reaction; The small pieces graphene film transferred on the Si substrate and bring out the graphene film growth.
To have the Si substrate of graphene film small pieces to place sputtering chamber, and adopt the laser pulse method that carbon atom is splashed on the Si substrate from the agraphitic carbon target, thus take the graphene film small pieces as starting point at Si Grown graphene film (Fig. 5).
Effect: Si is the core material of contemporary silica-based electron device, numeral/logical circuit, directly at semiconducter substrate growing graphene films such as Si, will speed up the integrated of Graphene technology and contemporary optoelectronics industry, reduces cost.
Above-described embodiment only is not used in for explanation the present invention and limits the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (9)
1. the preparation method of a graphene film, it is characterized in that from pre-synthesis graphene film (1), choosing a small pieces graphene film (2), described small pieces graphene film (2) is transferred to conductor, the upper starting point as inducing the graphene film growth of the substrate of semi-conductor or isolator (3) comes from solid carbon source in described substrate (3) employing, the liquid carbon source, the carbon atom (4) that any two or more mixed carbon source discharges in gaseous carbon sources or the aforementioned carbon source is take small pieces graphene film (2) as starting point growing graphene film (5).
2. the preparation method of graphene film according to claim 1, it is characterized in that described pre-synthesis graphene film (1) be by micromechanics peel off, liquid phase is peeled off, chemical vapour deposition, carbon segregation, chemistry redox reaction, decompose solid-phase carbon source or decompose the method for phase carbon source and synthetic graphene film.
3. the preparation method of graphene film according to claim 1, what it is characterized in that described small pieces graphene film (2) is shaped as square, rectangle, circle, ellipse or irregular type.
4. the preparation method of graphene film according to claim 1, the number of plies that it is characterized in that described small pieces graphene film (2) is 1 layer to 200 layers, is preferably 1 layer to 20 layers, optimum is 1 layer to 5 layers.
5. the preparation method of graphene film according to claim 1 is characterized in that described small pieces graphene film (2) area is 1nm
2To 50000cm
2, be preferably 1nm
2To 1000cm
2, optimum is 1nm
2To 100um
2
6. the preparation method of graphene film according to claim 1 is characterized in that take small pieces graphene film (2) as inducing the required carbon atom (4) of some large area deposition graphene films (5) to come from any two or more mixed carbon source material in the gaseous carbon source that contains carbon atom of easy generation carbon atom, solid-state carbon source, liquid carbon source material or the aforementioned carbon source.
7. the preparation method of graphene film according to claim 1 is characterized in that from solid carbon source, liquid carbon source, gaseous carbon sources or aforementioned carbon source method that any two or more mixed carbon source discharges carbon atom comprises thermal treatment, sputtering method, laser treatment, Cement Composite Treated by Plasma or the decomposition reaction through the metal catalytic material; The carbon atom of described release is at the Grown graphene film that pre-synthesis small pieces graphene film is arranged.
8. the preparation method of graphene film according to claim 1 is characterized in that the number of plies of the graphene film (5) that becomes at Grown is 1 layer to 200 layers, is preferably 1 layer to 20 layers, and optimum is 1 layer to 5 layers.
9. the preparation method of graphene film according to claim 1, the temperature that it is characterized in that growing graphene film (5) is 0 ℃ to 2000 ℃, is preferably 50 ℃ to 1000 ℃, optimum is 50 ℃ to 600 ℃.
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| CN109411331A (en) * | 2018-10-23 | 2019-03-01 | 东北林业大学 | Two-dimensional superlattice indium selenide and preparation method thereof with preparing the application in photodetector |
| CN109368622A (en) * | 2018-11-27 | 2019-02-22 | 西安理工大学 | A method of preparing graphene in dielectric material substrate |
| CN110828550A (en) * | 2019-10-21 | 2020-02-21 | 浙江大学 | Boron nitride/graphene heterojunction device |
| CN111276295A (en) * | 2020-02-20 | 2020-06-12 | 上海超碳石墨烯产业技术有限公司 | Preparation method of graphene primary coated copper wire |
| CN113299801A (en) * | 2021-04-22 | 2021-08-24 | 江苏度微光学科技有限公司 | Method for preparing bulk graphene film based on polymer necking process and application of bulk graphene film in blue light LED device |
| CN113299801B (en) * | 2021-04-22 | 2022-06-10 | 江苏度微光学科技有限公司 | Method for preparing bulk graphene film based on polymer necking process and application of bulk graphene film in blue light LED device |
| CN115074694A (en) * | 2022-07-01 | 2022-09-20 | 常州第六元素半导体有限公司 | Graphene film preparation method |
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