CN104451592A - Method for nondestructively transferring graphene from metal surface to surface of target substrate - Google Patents
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- CN104451592A CN104451592A CN201410779092.8A CN201410779092A CN104451592A CN 104451592 A CN104451592 A CN 104451592A CN 201410779092 A CN201410779092 A CN 201410779092A CN 104451592 A CN104451592 A CN 104451592A
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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Abstract
The invention discloses a method for nondestructively transferring graphene from a metal surface to the surface of a target substrate. The method comprises the steps of enabling graphene to grow on the surface of metal copper; coating the surface of graphene with a PMMA film, floating a copper substrate in an etching agent solution to corrode and remove the copper to obtain a PMMA/graphene composite film; enabling a PET film with static electricity in a friction manner to approach the PMMA/graphene composite film which is floated on the liquid surface, and adsorbing the graphene/PMMA composite film on the surface of the PET film by utilizing the electrostatic effect, contacting the graphene/PMMA composite film with the deionized water, meanwhile, releasing static electricity on the surface of the PET film, separating the PMMA/graphene composite film from the PET film, and floating the PMMA/graphene composite film on the water surface; repeating the steps, washing graphene, and completely removing the copper etching agent attached to the surface of the graphene; and finally transferring the PMMA/graphene composite film to the surface of the target substrate, and dissolving and removing the PMMA on the surface. By utilizing the method, not only can the location transfer of the large-sized graphene be realized, but also the damage rate of the graphene can be greatly reduced.
Description
Technical field
The invention belongs to field of material technology, particularly relate to a kind of by Graphene from metallic surface to target substrate surface nondestructive transfer method.
Background technology
2004, Univ Manchester UK professor Geim prepared Graphene [K.S.Novoselov, A.K.Geim, S.V.Morozov first, D.Jiang, Y.Zhang, S.V.Dubonos, I.V.Grigorieva, A.A.Firsov, Science 2004,306,666.].Graphene is by the former molecular six side's honeycomb two-dirnentional structures of monolayer carbon.Under graphene film room temperature, native electronic mobility can reach 200000cm
2/ Vs, has excellent electrical properties [K.I.Bolotin, K.J.Sikes, Z.Jiang, M.Klima, G.Fudenberg, J.Hone, P.Kim, H.L.Stormer, Solid StateCommunications 2008,146,351.].In addition, Graphene all has high transmittance in whole visible region, and research finds that the transmittance of single-layer graphene is close to 97%[R.R.Nair, P.Blake, A.N.Grigorenko, K.S.Novoselov, T.J.Booth, T.Stauber, N.M.R.Peres, A.K.Geim, Science 2008,320,1308.], therefore Graphene has huge application prospect in person in electronics, opto-electronics and conductive film etc.
Realize the large-scale application of Graphene, primary prerequisite is the growth preparation of large-area graphene film.There are some researches show and utilized chemical vapour deposition (CVD) method can realize growth [X.S.Li, W.W.Cai, the J.H.An of individual layer, High-performance graphene film in copper substrate, S.Kim, J.Nah, D.X.Yang, R.Piner, A.Velamakanni, I.Jung, E.Tutuc, S.K.Banerjee, L.Colombo, R.S.Ruoff, Science 2009,324,1312.].
Up to the present, the growth of Graphene in metallic surface after deliberation more deep, restriction Graphene large-scale application mainly how to realize Graphene harmless transfer to target substrate surface from metallic surface.Have direct contact type and non-direct contact type clean Graphene and shift in existing transfer method, but these two kinds of methods can cause the defect of the damaged or a large amount of consumption of natural resource of Graphene.
Therefore, the harmless transfer how realizing Graphene is efficiently the precondition realizing Graphene large-scale application.
Summary of the invention
(1) technical problem that will solve
In view of this, main purpose of the present invention be to provide a kind of by Graphene from metallic surface the method to the transfer of target substrate surface nondestructive, to save the resource consumption in transfer process, Graphene in transfer process is avoided to contact with transfer the direct of apparatus, reduce the damaged degree of Graphene, improve the quality of graphene film.
(2) technical scheme
For achieving the above object, the invention provides a kind of by Graphene from metallic surface to target substrate surface nondestructive transfer method, the method comprises:
Step 1: at copper foil surface growing graphene;
Step 2: have copper foil surface coating polymethylmethacrylate (PMMA) of Graphene as supporting layer in growth, then swims in ferric chloride aqueous solutions surface corrosion removal copper and obtains PMMA/ graphene composite film by Copper Foil;
Step 3: the organic film utilizing a surface band electrostatic, is adsorbed in this organic film surface by PMMA/ graphene composite film by electrostatic interaction;
Step 4: wash PMMA/ graphene composite film with deionized water, to remove the liquor ferri trichloridi of graphenic surface attachment;
Step 5: the organic film again utilizing a surface band electrostatic, PMMA/ graphene composite film is adsorbed in this organic film surface by electrostatic interaction, then by PMMA/ graphene composite film and target substrate surface contact, eliminate this organic film surface institute static electrification simultaneously, realize the transfer of PMMA/ graphene composite film to target substrate surface;
Step 6: utilize the PMMA in dissolution with solvents removal PMMA/ graphene composite film, realize Graphene harmless transfer to target substrate surface from metallic surface.
In such scheme, at copper foil surface growing graphene described in step 1, comprising: Copper Foil is put into CVD stove, pass into the H of 10SCCM
2with the CH of 2SCCM
4, at copper foil surface growing graphene at 1000 DEG C.
In such scheme, organic film described in step 3 is can generate static electricity by the rubbing action and have polyethylene terephthalate (PET) film or the polytetrafluoroethylene film of certain physical strength.
In such scheme, organic film described in step 3 adopts PET film, described in step 3, PMMA/ graphene composite film is adsorbed in organic film surface by electrostatic interaction, comprise: utilize a surface of silk friction PET film to make its static electrification, then PET film is not rubbed a surface of not static electrification close to the PMMA/ graphene composite film swimming in ferric chloride aqueous solutions surface, by electrostatic interaction, PMMA/ graphene composite film is adsorbed in PET film surface.
In such scheme, with deionized water, PMMA/ graphene composite film is washed described in step 4, to remove the liquor ferri trichloridi of graphenic surface attachment, comprise: will the PMMA/ graphene composite film contact deionized water on PET film surface be adsorbed in, simultaneously by wet non-woven fabrics wiping PET film through the rubbed surface of silk to eliminate PET film surface electrostatic, PMMA/ graphene composite film is transferred to the water surface of deionized water; And then utilize a surface of silk friction PET film to make its static electrification, by electrostatic interaction, PMMA/ graphene composite film is adsorbed in PET film surface; Successively repeatedly, the liquor ferri trichloridi removing graphenic surface attachment is washed to PMMA/ graphene composite film.
In such scheme, eliminating organic film surface institute static electrification described in step 5, is use wet non-woven fabrics wiping PET film through the rubbed surface of silk, to eliminate organic film surface institute static electrification.
In such scheme, described target substrate comprises glass substrate, quartz substrate and PET film substrate.
(3) beneficial effect
As can be seen from technique scheme, the present invention has following beneficial effect:
1, provided by the invention by Graphene from metallic surface to target substrate surface nondestructive transfer method, utilize organic film with electrostatic to the adsorption of PMMA dexterously, not only achieve the efficient transfer of Graphene, and avoid Graphene and contact with the direct of organic film, thus reduce the breakage of Graphene, improve the quality of the rear graphene film of transfer.
2, provided by the invention by Graphene from metallic surface to target substrate surface nondestructive transfer method, not only achieve the efficient transfer of Graphene, save the resource consumption in transfer process, and to avoid in transfer process Graphene and contact with transfer the direct of apparatus, effectively reduce the damaged degree of Graphene, improve the quality of graphene film.
3, provided by the invention by Graphene from metallic surface to target substrate surface nondestructive transfer method, achieve the harmless transfer of copper substrate surfaces CVD Graphene on target substrate surface, not only reduce the resource consumption in transfer process, and improve the integrity of graphene film.
Accompanying drawing explanation
Fig. 1 be according to the embodiment of the present invention by Graphene from metallic surface to target substrate surface nondestructive transfer method flow diagram.
Fig. 2 be according to the embodiment of the present invention by Graphene from metallic surface to target substrate surface nondestructive transfer process flow sheet.
Fig. 3 is the schematic diagram of the use electrostatic transfer according to the embodiment of the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Shown in 1, Fig. 1 be according to the embodiment of the present invention by Graphene from metallic surface to target substrate surface nondestructive transfer method flow diagram, the method comprises the following steps:
Step 1: at copper foil surface growing graphene;
In this step, at copper foil surface growing graphene, be that Copper Foil is put into CVD stove, pass into the H of 10SCCM
2with the CH of 2SCCM
4, at copper foil surface growing graphene at 1000 DEG C.
Step 2: have copper foil surface coating polymethylmethacrylate (PMMA) of Graphene as supporting layer in growth, then swims in ferric chloride aqueous solutions surface corrosion removal copper and obtains PMMA/ graphene composite film by Copper Foil.
Step 3: the organic film utilizing a surface band electrostatic, is adsorbed in this organic film surface by PMMA/ graphene composite film by electrostatic interaction;
In this step, organic film is can generate static electricity by the rubbing action and have polyethylene terephthalate (PET) film or the polytetrafluoroethylene film of certain physical strength; For PET film, PMMA/ graphene composite film is adsorbed in organic film surface by electrostatic interaction, utilize a surface of silk friction PET film to make its static electrification, then PET film is not rubbed a surface of not static electrification close to the PMMA/ graphene composite film swimming in ferric chloride aqueous solutions surface, by electrostatic interaction, PMMA/ graphene composite film is adsorbed in PET film surface.
Step 4: wash PMMA/ graphene composite film with deionized water, to remove the liquor ferri trichloridi of graphenic surface attachment;
In this step, for PET film, with deionized water, PMMA/ graphene composite film is washed, to remove the liquor ferri trichloridi of graphenic surface attachment, to be adsorbed in the PMMA/ graphene composite film contact deionized water on PET film surface, simultaneously by wet non-woven fabrics wiping PET film through the rubbed surface of silk to eliminate PET film surface electrostatic, realize being separated and making the former float on the water surface of deionized water of PMMA/ graphene composite film and PET film, and then PMMA/ graphene composite film is transferred to the water surface of deionized water; And then utilize a surface of silk friction PET film to make its static electrification, by electrostatic interaction, PMMA/ graphene composite film is adsorbed in PET film surface; Successively repeatedly, the liquor ferri trichloridi removing graphenic surface attachment is washed to PMMA/ graphene composite film.
Make the Electro-static Driven Comb on PET film surface simultaneously, realize being separated and making the former float on the water surface of PMMA/ graphene composite film and PET film
Step 5: the organic film again utilizing a surface band electrostatic, PMMA/ graphene composite film is adsorbed in this organic film surface by electrostatic interaction, then by PMMA/ graphene composite film and target substrate surface contact, eliminate this organic film surface institute static electrification simultaneously, realize the transfer of PMMA/ graphene composite film to target substrate surface;
In this step, eliminating organic film surface institute static electrification, is use wet non-woven fabrics wiping PET film through the rubbed surface of silk, to eliminate organic film surface institute static electrification.
Step 6: utilize the PMMA in dissolution with solvents removal PMMA/ graphene composite film, realize Graphene harmless transfer to target substrate surface from metallic surface;
Wherein, target substrate comprises glass substrate, quartz substrate or PET film substrate.
Embodiment 1: utilize electrostatic interaction to realize the transfer of copper foil surface CVD Graphene to glass surface.
Copper Foil is put into CVD stove, in 10sccm hydrogen and 2sccm methane blended atmosphere, under 1000 DEG C of hot conditionss, utilize chemical vapour deposition at copper surface growth Graphene; Grown the copper foil surface coating PMMA of Graphene; Copper Foil is swum in ferric chloride aqueous solutions surface corrosion removing metallic copper and obtain PMMA/ graphene composite film; A surface of silk friction polyethylene terephthalate (PET) film is utilized to make its static electrification, then another surface PET film do not rubbed, close to the PMMA/ graphene composite film swum on liquor ferri trichloridi, makes it be adsorbed on PET film surface by electrostatic interaction; To the PMMA/ graphene composite film contact deionized water on PET film surface be adsorbed on, and eliminate institute's static electrification with wet non-woven fabrics wiping PET through the surface that silk is rubbed simultaneously, PMMA/ graphene composite film is transferred to the water surface; Successively repeatedly, the liquor ferri trichloridi removing graphenic surface attachment is washed to PMMA/ graphene composite film; Again utilize the PET film of a surface band electrostatic, PMMA/ graphene composite film is made to be adsorbed on PET film surface, it is contacted with glass surface, eliminate institute's static electrification by wet non-woven fabrics wiping PET film through the surface that silk is rubbed simultaneously, realize the transfer of PMMA/ graphene composite film at glass surface; The PMMA film utilizing acetone solution to remove graphenic surface finally realizes the transfer of Graphene at glass surface.
Embodiment 2: utilize electrostatic interaction to realize the transfer of copper foil surface CVD Graphene to pet sheet face.
Concrete steps are similar to Example 1, but the last target substrate used is PET film.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. by Graphene from metallic surface to target substrate surface nondestructive transfer a method, it is characterized in that, the method comprises:
Step 1: at copper foil surface growing graphene;
Step 2: have the copper foil surface coating polymetylmethacrylate of Graphene as supporting layer in growth, then Copper Foil is swum in ferric chloride aqueous solutions surface corrosion removal copper and obtain PMMA/ graphene composite film;
Step 3: the organic film utilizing a surface band electrostatic, is adsorbed in this organic film surface by PMMA/ graphene composite film by electrostatic interaction;
Step 4: wash PMMA/ graphene composite film with deionized water, to remove the liquor ferri trichloridi of graphenic surface attachment;
Step 5: the organic film again utilizing a surface band electrostatic, PMMA/ graphene composite film is adsorbed in this organic film surface by electrostatic interaction, then by PMMA/ graphene composite film and target substrate surface contact, eliminate this organic film surface institute static electrification simultaneously, realize the transfer of PMMA/ graphene composite film to target substrate surface;
Step 6: utilize the PMMA in dissolution with solvents removal PMMA/ graphene composite film, realize Graphene harmless transfer to target substrate surface from metallic surface.
2. according to claim 1 by Graphene from metallic surface to target substrate surface nondestructive transfer method, it is characterized in that, at copper foil surface growing graphene described in step 1, comprising:
Copper Foil is put into chemical vapor deposition stove, passes into the H of 10SCCM
2with the CH of 2SCCM
4, at copper foil surface growing graphene at 1000 DEG C.
3. according to claim 1 by Graphene from metallic surface to target substrate surface nondestructive transfer method, it is characterized in that, organic film described in step 3 is can generate static electricity by the rubbing action and have polyethylene terephtalate film or the polytetrafluoroethylene film of certain physical strength.
4. according to claim 3 by Graphene from metallic surface to target substrate surface nondestructive transfer method, it is characterized in that, organic film described in step 3 adopts PET film, described in step 3, PMMA/ graphene composite film is adsorbed in organic film surface by electrostatic interaction, comprises:
A surface of silk friction PET film is utilized to make its static electrification, then PET film is not rubbed a surface of not static electrification close to the PMMA/ graphene composite film swimming in ferric chloride aqueous solutions surface, by electrostatic interaction, PMMA/ graphene composite film is adsorbed in PET film surface.
5. according to claim 4 by Graphene from metallic surface to target substrate surface nondestructive transfer method, it is characterized in that, with deionized water, PMMA/ graphene composite film is washed described in step 4, to remove the liquor ferri trichloridi of graphenic surface attachment, comprising:
The PMMA/ graphene composite film contact deionized water on PET film surface will be adsorbed in, simultaneously by wet non-woven fabrics wiping PET film through the rubbed surface of silk to eliminate PET film surface electrostatic, PMMA/ graphene composite film is transferred to the water surface of deionized water;
And then utilize a surface of silk friction PET film to make its static electrification, by electrostatic interaction, PMMA/ graphene composite film is adsorbed in PET film surface;
Successively repeatedly, the liquor ferri trichloridi removing graphenic surface attachment is washed to PMMA/ graphene composite film.
6. according to claim 5 by Graphene from metallic surface to target substrate surface nondestructive transfer method, it is characterized in that, organic film surface institute static electrification is eliminated described in step 5, use wet non-woven fabrics wiping PET film through the rubbed surface of silk, to eliminate organic film surface institute static electrification.
7. according to claim 1 by Graphene from metallic surface to target substrate surface nondestructive transfer method, it is characterized in that, described target substrate comprises glass substrate, quartz substrate or PET film substrate.
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