CN104498892A - Method for preparing graphene film through low-temperature fixed-point nucleating - Google Patents

Method for preparing graphene film through low-temperature fixed-point nucleating Download PDF

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Publication number
CN104498892A
CN104498892A CN201410768777.2A CN201410768777A CN104498892A CN 104498892 A CN104498892 A CN 104498892A CN 201410768777 A CN201410768777 A CN 201410768777A CN 104498892 A CN104498892 A CN 104498892A
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carbon source
graphene film
metal base
fixed point
solid
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Inventor
高翾
黄德萍
李占成
张永娜
朱鹏
姜浩
史浩飞
杜春雷
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Chongqing Institute of Green and Intelligent Technology of CAS
Chongqing Graphene Technology Co Ltd
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Chongqing Institute of Green and Intelligent Technology of CAS
Chongqing Graphene Technology Co Ltd
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Priority to CN201410768777.2A priority Critical patent/CN104498892A/en
Publication of CN104498892A publication Critical patent/CN104498892A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/186Preparation by chemical vapour deposition [CVD]
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0272Deposition of sub-layers, e.g. to promote the adhesion of the main coating

Abstract

The invention relates to a technical field of preparation of a graphene film, in particular to a method for preparing a graphene film through low-temperature fixed-point nucleating. The method for preparing a graphene film through low-temperature fixed-point nucleating is characterized by comprising the following steps: coating a layer of carbon source solution on a metal substrate and stoving till the carbon source solution is cured; patterning the cured carbon source solution on the surface of the metal substrate to form a plurality of solid-state carbon sources; putting the whole metal substrate into a CVD reaction cavity and carrying out graphene nucleating so that the carbon atoms of the solid-state carbon sources are recombined and subjected to fixed-point nucleating; after carbon atom fixed-point nucleating, diffusing the carbon atoms to the whole metal substrate to form a graphene film; and cooling the formed graphene film, thus finishing the preparation of the graphene film.

Description

A kind of low temperature fixed point nucleation prepares the method for graphene film
Technical field
The present invention relates to the preparing technical field of graphene film, particularly relate to the method that a kind of low temperature fixed point nucleation prepares graphene film.
Background technology
Graphene is the hexagonal honey comb structure that carbon atom forms based on sp2 hydridization, the only two dimensional crystal of an atomic layers thick.2004, the people such as Andre Geim and Konstantin Novoselov found the single-layer graphene of stable existence, also obtained Nobel Prize in physics in 2010 because of its initiative work in Graphene.In recent years, Graphene all shows many stem-winding performances and potential application prospect in fields such as microelectronics, quantum physics, material, chemistry, has attracted the extensive concern of scientific circles and industry member.Graphene has excellent power, heat, the character such as optical, electrical.Electronic mobility under Graphene normal temperature, more than 15000cm2/Vs, exceedes carbon nanotube and silicon crystal, and resistivity only about 10 -6Ω cm, lower than copper or silver is the material that resistivity is minimum in the world at present.And its up to 97.7% all wave band transmittance be that other electro-conductive materials are difficult to be equal to.
The industrial chemical Vapor deposition process (also referred to as CVD, CVD is the abbreviation of Chemical Vapor Deposition to chemical Vapor deposition process) that generally adopts is as the method preparing large-area graphene at present.But for the single-chip size of composition graphene film, nucleation site and nucleation density, the number of plies of graphene film, is all difficult to control, thus causes the electric property of graphene film entirety well below theoretical value.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of low temperature spot jamming nuclear graphite alkene film, overcome conventional graphite alkene method for manufacturing thin film nucleation site, nucleation density and thin film layer numerical control system difficulty, the defect of the Graphene electric property difference produced.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of low temperature fixed point nucleation prepares the method for graphene film, it is characterized in that, comprises the following steps:
1) be coated with one deck carbon source solution (so-called carbon source solution refers to the polymeric carbon source of carbon containing hydrogen-oxygen) on the metallic substrate, and dry carbon source solution to solidification;
2) the carbon source solution after metal substrate surface being solidified graphically forms multiple solid-state carbon source;
3) whole metal base is put into CVD reaction chamber, carry out Graphene nucleation, make the carbon atom restructuring fixed point nucleation of solid-state carbon source;
4) after carbon atom restructuring fixed point nucleation, carbon atom diffuses in whole metal base, forms graphene film;
5) graphene film generated is cooled, complete the preparation of graphene film.
The invention has the beneficial effects as follows: step is simple, easy to operate, decrease energy consumption, improves production efficiency, the amount by coating carbon source solution controls graphene film production quantity, simple and convenient.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in described step 1) in, described carbon source solution can be any one in the multipolymer of polyacrylic ester, polymethacrylate, polyacrylic ester and polymethacrylate, polyethers, polyester, polyolefine.
The beneficial effect of above-mentioned further scheme is adopted to be: to adopt above-mentioned carbon source solution to be conducive to preparing high-quality graphene film.
Further, in described step 1) in, the metal base of employing is any one in the metals such as annealed Cu, Ru, Ni, Ir, Pt.
The beneficial effect of above-mentioned further scheme is adopted to be: to adopt the metal after above-mentioned annealing as metal base, be conducive to the growth of graphene film.
Further, in described step 1) in, first smooth for metal base is laid on silicon chip, then is coated with the described carbon source solution that one deck concentration is 10% on the metallic substrate, and carried out the whirl coating of 50s with 3000r/m whirl coating rotating speed by photoresist spinner, carbon source dissolution homogeneity is coated with.
Adopt the beneficial effect of above-mentioned further scheme to be: simple to operation, carbon source dissolution homogeneity is coated with, the production number of plies of graphene film can be controlled by the amount of the carbon source solution of coating.
Further, in described step 1) in, by the oven dry of carbon source solution to the concrete operations in solidification process be: the silicon chip being placed with the metal base scribbling carbon source solution being put into temperature is dry carbon source solution in the stoving oven of 110 DEG C to solidification, and drying time is 20 minutes.
Adopt the beneficial effect of above-mentioned further scheme to be: bake out temperature is lower, adopt cold operation, reduce energy loss.
Further, in described step 2) in, the carbon source solution that metal substrate surface is solidified by using plasma lithographic method carries out graphically forming multiple solid-state carbon source, and an area that every square millimeter of metal base distributes is 0.25mm 2solid-state carbon source, the thickness of described solid-state carbon source is 40 ~ 80nm.
The beneficial effect of above-mentioned further scheme is adopted to be: by controlling nucleation site and the nucleation density of Graphene, and to control carbon source amount, thus control growth quality and the number of plies of graphene film, improve the quality of graphene film.
Further, in described step 3) in, whole metal base is put into CVD reaction chamber, pass into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, and the temperature of reaction in CVD reaction chamber is 400 ~ 500 DEG C, reaction pressure is normal pressure, makes the carbon atom restructuring fixed point nucleation of solid-state carbon source.
Adopt the beneficial effect of above-mentioned further scheme to be: suitable reaction environment is conducive to the carbon atom restructuring of carbon source, carbon atom is fixed a point nucleation, for next step technique is laid the groundwork.
Further, in described step 4) in, after solid-state carbon source advanced person has gone carbon atom restructuring fixed point nucleation, whole metal base is in CVD reaction chamber, growth 20 ~ 40 minutes is kept with growing environment, the pressure of growing environment is normal pressure, temperature is 400 ~ 500 DEG C and pass into argon gas and the hydrogen that flow is respectively 200sccm and 50sccm, makes carbon atom diffuse in whole metal base, forms graphene film.
Adopt the beneficial effect of above-mentioned further scheme to be: temperature of reaction is lower, save time and the energy consumption of the cooling that heats up, meanwhile, be conducive to graphene film and be shaped.
Further, described step 5) in, graphene film, in the process of cooling, passes into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, till graphene film is cooled to room temperature, completes the preparation of graphene film.
Adopt the beneficial effect of above-mentioned further scheme to be: graphene film to be lowered the temperature rapidly, continues to pass into gas and graphene film forming quality is stablized, improve the quality of graphene film.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that a kind of low temperature fixed point of the present invention nucleation prepares the method for graphene film;
Fig. 2 is the side-view of method when being coated with carbon source solution that a kind of low temperature fixed point of the present invention nucleation prepares graphene film;
Fig. 3 is the patterned solid-state carbon source side-view on the metallic substrate that a kind of low temperature of the present invention fixed point nucleation prepares the method for graphene film;
Fig. 4 is the patterned solid-state carbon source vertical view on the metallic substrate that a kind of low temperature of the present invention fixed point nucleation prepares the method for graphene film;
Fig. 5 is the graphene film side-view on the metallic substrate that preparation that a kind of low temperature of the present invention fixed point nucleation prepares the method for graphene film completes.
In accompanying drawing, the list of parts representated by each label is as follows:
1, metal base, 2, carbon source solution, 3, solid-state carbon source, 4, graphene film.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
As shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 4, Fig. 5, a kind of low temperature fixed point of the present invention nucleation prepares the method for graphene film 4, comprise the following steps: 1) be coated with carbon source solution 2, namely in metal base 1, be coated with one deck carbon source solution 2, and dry 2 to the solidification of carbon source solution; 2) graphically form solid-state carbon source 3, the carbon source solution 2 by metal base 1 surface cure graphically forms multiple solid-state carbon source 3; 3) fixed point nucleation, puts into CVD reaction chamber by whole metal base 1, carries out Graphene fixed point nucleation, makes the carbon atom restructuring fixed point nucleation of solid-state carbon source 3; 4) grow into film, namely after carbon atom restructuring fixed point nucleation, carbon atom diffuses in whole metal base 1, forms graphene film 4; 5) cool, namely the graphene film 4 generated is cooled, complete the preparation of graphene film 4.
Wherein, in described step 1) in, described carbon source solution 2 can be any one in the multipolymer, polyethers, polyester, polyolefine etc. of polyacrylic ester, polymethacrylate, polyacrylic ester and polymethacrylate.The metal base 1 adopted can be any one in the annealed metal such as Cu, Ru, Ni, Ir, Pt, Copper Foil.Above-mentioned carbon source solution and metal base is adopted to be conducive to preparing graphene film.
For aforesaid method step, there is operation specific as follows in corresponding step:
As shown in Figure 2, in described step 1) in, first smooth for metal base 1 is laid on silicon chip, then in metal base 1, is coated with the described carbon source solution 2 that one deck concentration is 10%, and carried out the whirl coating of 50s with 3000r/m whirl coating rotating speed by photoresist spinner, make carbon source solution 2 even spread.Carbon source solution 2 is dried to the concrete operations in solidification process and be: the silicon chip being placed with the metal base 1 scribbling carbon source solution 2 being put into temperature is dry 2 to the solidification of carbon source solution in the stoving oven of 110 DEG C, and drying time is 20 minutes.Carbon source solution 2, for providing solid-state carbon source 3, is controlled the amount of the carbon source after solidifying, thus controls the glue spread of solid-state carbon source 3, control the production quantity of graphene film 4 simply and easily by the amount of the carbon source solution 2 controlling coating.
As shown in Figure 3, Figure 4, in described step 2) in, the carbon source solution 2 of metal base 1 surface cure carries out graphically forming multiple solid-state carbon source 3 by using plasma lithographic method, and an area that every square millimeter of metal base 1 distributes is 0.25mm 2solid-state carbon source 3, the thickness of described solid-state carbon source 3 is 40 ~ 80nm, and this solid-state carbon source 3 amount is for generating single-layer graphene film 4, and to generate multi-layer graphene film 4, the corresponding amount increasing solid-state carbon source 3, the amount of solid-state carbon source 3 controls simple and convenient.In described step 3) in, whole metal base 1 is put into CVD reaction chamber, pass into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, and the temperature of reaction in CVD reaction chamber is 400 ~ 500 DEG C, reaction pressure is normal pressure, carbon atom is binned in patterned solid-state carbon source 3 fixes a point nucleation.
As shown in Figure 5, in described step 4) in, after solid-state carbon source 3 has first carried out carbon atom restructuring fixed point nucleation, whole metal base 1 is in CVD reaction chamber, growth 20 ~ 40 minutes is kept with growing environment, the pressure of growing environment is normal pressure, temperature is 400 ~ 500 DEG C and pass into argon gas and the hydrogen that flow is respectively 200sccm and 50sccm, makes carbon atom diffuse in the whole metal base 1 of metal base 1, forms graphene film 4.Described step 5) in, graphene film 4, in the process of cooling, passes into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, till graphene film 4 is cooled to room temperature, completes the preparation of graphene film 4.
Now adopt Copper Foil to be illustrated as carbon source solution as metal base, PMMA solution (PMMA solution is polymethyl methacrylate solution) by aforesaid method the present invention, can following examples be adopted, but be not limited to following examples.
Embodiment one:
Be placed on silicon chip by smooth for the Copper Foil after the annealing of 5cm × 5cm, on even spread, concentration is the PMMA solution of 10%, then rotates 50 seconds by the speed that photoresist spinner take rotating speed as 3000r/m, completes the even spread of PMMA solution.Then silicon chip, Copper Foil are put in stoving oven and be heated to 110 DEG C, carry out heating in 20 minutes, make PMMA solution baking and curing.Then the method for using plasma etching, the PMMA that copper foil surface is solidified is patterned into as solid-state carbon source 3, solid-state carbon source 3 after graphical distributes with a solid-state carbon source 3 that every square millimeter of copper foil surface distributes, the size of each solid-state carbon source 3 is 0.25 square millimeter, the thickness of each solid-state carbon source 3 is 40nm, and the distributed number completing solid-state carbon source 3 is arranged.Then Copper Foil is put into CVD reaction chamber, pass into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, the pressure of adjustment reaction chamber is normal pressure, temperature of reaction is 400 DEG C, keep growth 40 minutes, carbon atom is binned in patterned solid-state carbon source 3 fixes a point nucleation, after fixed point nucleation, carbon atom diffuses in whole Copper Foil substrate, forms graphene film 4.Finally, stop heating, and continue to keep passing into argon gas and the hydrogen that flow is respectively 200sccm and 50sccm, cooling graphene film 4 to room temperature, completes the preparation of graphene film 4.
Embodiment two:
Be placed on silicon chip by smooth for the Copper Foil after the annealing of 5cm × 5cm, on even spread, concentration is the PMMA solution of 10%, then rotates 50 seconds by the speed that photoresist spinner take rotating speed as 3000r/m, completes the even spread of PMMA solution.Then silicon chip, Copper Foil are put in stoving oven and be heated to 110 DEG C, carry out heating in 20 minutes, make PMMA solution baking and curing.Then the method for using plasma etching, the PMMA that copper foil surface is solidified is patterned into as solid-state carbon source 3, solid-state carbon source 3 after graphical distributes with a solid-state carbon source 3 that every square millimeter of copper foil surface distributes, the size of each solid-state carbon source 3 is 0.25 square millimeter, the thickness of each solid-state carbon source 3 is 60nm, and the distributed number completing solid-state carbon source 3 is arranged.Then Copper Foil is put into CVD reaction chamber, pass into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, the pressure of adjustment reaction chamber is normal pressure, temperature of reaction is 450 DEG C, keep growth 30 minutes, carbon atom is binned in patterned solid-state carbon source 3 fixes a point nucleation, after fixed point nucleation, carbon atom diffuses in whole Copper Foil substrate, forms graphene film 4.Finally, stop heating, and continue to keep passing into argon gas and the hydrogen that flow is respectively 200sccm and 50sccm, cooling graphene film 4 to room temperature, completes the preparation of graphene film 4.
Embodiment three:
Be placed on silicon chip by smooth for the Copper Foil after the annealing of 5cm × 5cm, on even spread, concentration is the PMMA solution of 10%, then rotates 50 seconds by the speed that photoresist spinner take rotating speed as 3000r/m, completes the even spread of PMMA solution.Then silicon chip, Copper Foil are put in stoving oven and be heated to 110 DEG C, carry out heating in 20 minutes, make carbon source solution 2 baking and curing.Then the method for using plasma etching, the PMMA that copper foil surface is solidified is patterned into as solid-state carbon source 3, solid-state carbon source 3 after graphical distributes with a solid-state carbon source 3 that every square millimeter of copper foil surface distributes, the size of each solid-state carbon source 3 is 0.25 square millimeter, the thickness of each solid-state carbon source 3 is 80nm, and the distributed number completing solid-state carbon source 3 is arranged.Then Copper Foil is put into CVD reaction chamber, pass into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, the pressure of adjustment reaction chamber is normal pressure, temperature of reaction is 500 DEG C, keep growth 20 minutes, carbon atom is binned in patterned solid-state carbon source 3 fixes a point nucleation, after fixed point nucleation, carbon atom diffuses in whole Copper Foil substrate, forms graphene film 4.Finally, stop heating, and continue to keep passing into argon gas and the hydrogen that flow is respectively 200sccm and 50sccm, cooling graphene film 4 to room temperature, completes the preparation of graphene film 4.
The advantage of method of the present invention is: 1) growing graphene at low temperatures, decreases heating and cooling time and energy loss, is applicable to industrialization; 2) in process of growth, eliminate existing CVD method need the carbon source of gas and the cost of hydrogen, namely need cost carbon source being converted to gaseous state; 3) environment remaining on normal pressure carries out, and has saved energy loss; 4) controlled to the nucleation site precision of Graphene, form big area single-chip; 5) number of plies of graphene film is controlled by the glue spread of carbon source glue spread and carbon source solution 2, simple to operation.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (9)

1. low temperature fixed point nucleation prepares a method for graphene film, it is characterized in that, comprises the following steps:
1) in metal base (1) upper coating one deck carbon source solution (2), and carbon source solution (2) is dried to solidification;
2) the carbon source solution (2) after metal base (1) surface cure is graphically formed multiple solid-state carbon source (3);
3) whole metal base (1) is put into CVD reaction chamber, carry out Graphene nucleation, make the carbon atom restructuring fixed point nucleation of solid-state carbon source (3);
4) after carbon atom restructuring fixed point nucleation, carbon atom diffuses in whole metal base (1), forms graphene film (4);
5) graphene film (4) generated is cooled, complete the preparation of graphene film (4).
2. a kind of low temperature fixed point nucleation according to claim 1 prepares the method for graphene film, it is characterized in that, in described step 1) in, described carbon source solution (2) can be any one in the multipolymer of polyacrylic ester, polymethacrylate, polyacrylic ester and polymethacrylate, polyethers, polyester, polyolefine.
3. a kind of low temperature fixed point nucleation according to claim 2 prepares the method for graphene film, it is characterized in that, in described step 1) in, the metal base (1) of employing is any one in the metals such as annealed Cu, Ru, Ni, Ir, Pt.
4. a kind of low temperature fixed point nucleation according to claim 3 prepares the method for graphene film, it is characterized in that, in described step 1) in, first smooth for metal base (1) is laid on silicon chip, be the described carbon source solution (2) of 10% again in metal base (1) upper coating one deck concentration, and carried out the whirl coating of 50s with 3000r/m whirl coating rotating speed by photoresist spinner, make carbon source solution (2) even spread.
5. a kind of low temperature fixed point nucleation according to claim 3 prepares the method for graphene film, it is characterized in that, in described step 1) in, by carbon source solution (2) oven dry to the concrete operations in solidification process be: the silicon chip being placed with the metal base (1) scribbling carbon source solution (2) being put into temperature is dry carbon source solution (2) in the stoving oven of 110 DEG C to solidification, and drying time is 20 minutes.
6. a kind of low temperature fixed point nucleation according to claim 3 prepares the method for graphene film, it is characterized in that, in described step 2) in, the carbon source solution (2) of metal base (1) surface cure carries out graphically forming multiple solid-state carbon source (3) by using plasma lithographic method, and every square millimeter of upper distribution area of metal base (1) is 0.25mm 2solid-state carbon source (3), the thickness of described solid-state carbon source (3) is 40 ~ 80nm.
7. a kind of low temperature fixed point nucleation according to claim 3 prepares the method for graphene film, it is characterized in that, in described step 3) in, whole metal base (1) is put into CVD reaction chamber, pass into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, and the temperature of reaction in CVD reaction chamber is 400 ~ 500 DEG C, reaction pressure is normal pressure, makes the carbon atom restructuring fixed point nucleation of solid-state carbon source (3).
8. a kind of low temperature fixed point nucleation according to claim 7 prepares the method for graphene film, it is characterized in that, in described step 4) in, after solid-state carbon source (3) has first carried out carbon atom restructuring fixed point nucleation, whole metal base (1) is in CVD reaction chamber, growth 20 ~ 40 minutes is kept with growing environment, the pressure of growing environment is normal pressure, temperature is 400 ~ 500 DEG C and pass into argon gas and the hydrogen that flow is respectively 200sccm and 50sccm, make carbon atom diffuse in whole metal base (1), form graphene film (4).
9. a kind of low temperature fixed point nucleation according to any one of claim 1 to 8 prepares the method for graphene film, it is characterized in that, described step 5) in, graphene film (4) is in the process of cooling, pass into argon gas and hydrogen that flow is respectively 200sccm and 50sccm, till graphene film (4) is cooled to room temperature, complete the preparation of graphene film (4).
CN201410768777.2A 2014-12-12 2014-12-12 Method for preparing graphene film through low-temperature fixed-point nucleating Pending CN104498892A (en)

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CN108190864A (en) * 2018-01-16 2018-06-22 电子科技大学 A kind of graphene preparation method
CN108610501A (en) * 2018-03-30 2018-10-02 广州理文能源科技有限公司 A method of realizing super heated rubber conduction using vapor deposition graphene
CN108610501B (en) * 2018-03-30 2021-01-29 广州理文能源科技有限公司 Method for realizing high-temperature rubber conduction by using vapor deposition graphene
CN110359088A (en) * 2019-08-07 2019-10-22 中国电子科技集团公司第四十六研究所 A kind of large area single crystal graphene growing method
CN111072022A (en) * 2019-12-11 2020-04-28 中国科学院上海微系统与信息技术研究所 Preparation method of graphite film
CN114433631A (en) * 2022-01-26 2022-05-06 重庆墨希科技有限公司 Preparation method of high-conductivity graphene metal composite material based on solid carbon source

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Application publication date: 20150408