CN104192833A - Transfer method of graphene film - Google Patents
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- CN104192833A CN104192833A CN201410410144.4A CN201410410144A CN104192833A CN 104192833 A CN104192833 A CN 104192833A CN 201410410144 A CN201410410144 A CN 201410410144A CN 104192833 A CN104192833 A CN 104192833A
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Abstract
The invention provides a transfer method of a graphene film, which at least comprises the following steps: providing a metal substrate, and sequentially forming a graphene film, an organic polymer protective layer and a polymer frame support layer on the metal substrate surface, wherein the organic polymer protective layer and polymer frame support layer respectively have surface energy or viscosity; peeling the graphene film from the metal substrate, and attaching the graphene film to a target substrate; and finally, sequentially peeling the polymer frame support layer and organic polymer protective layer. By utilizing the proper surface energy or proper viscosity of the organic polymer protective layer and polymer frame support layer, the organic polymer protective layer and polymer frame support layer can be directly attached without any adhesive, and can be peeled without damage after transfer, thereby simplifying and stabilizing the technique and ensuring the complete transfer of the graphene film and the reutilization of the metal substrate.
Description
Technical field
The present invention relates to material and prepare manufacture field, particularly relate to a kind of transfer method of graphene film.
Background technology
Graphene is the two-dimensional material with polynuclear plane that a kind of monolayer carbon atom is arranged and formed with hexagonal structure, since first passage micromechanics in 2004 is peeled off and is produced, because of its unique optics, electricity, calorifics and mechanical property, obtained the extensive concern from researchist all over the world.In the past ten years, several different methods and process quilt Application and Development, in the preparation of graphene film, are mainly chemical vapour deposition (CVD) method of micromechanics stripping method, oxidation reduction process, epitaxial growth method and metal catalytic.Because there is advantage aspect growing large-area continuous graphite alkene film in metal catalytic CVD method, so the method becomes the main growth pattern of present graphene film.It adopts metal base if copper, nickel etc. are as substrate and catalyzer, the decomposition of the carbon sources such as catalytic methane, acetylene and deposition, thus realize the continuous growth of graphene film, obtain and be attached to the graphene film in metal base.In actual applications, conventionally require graphene film to be positioned in the functional layer film of the substrates such as silica glass, silicon, polyethylene terephthalate or device, therefore, how the graphene film being grown in metal base is transferred in target substrate most important.
The transfer method that grows in the graphene film in metal base is a lot, and wherein using polymkeric substance is a kind of very important method as the method for protective layer dissolution of metals substrate.The method is at the Graphene surface spin coating one layer of polymeric supporting layer growing in metal base, by etchant solution, by dissolving metal, is obtained polymer/graphene film freely, then is transferred to target substrate.The method is current studied maximum method, has the advantages such as process stabilizing, transfer techniques is ripe, operating process is simpler, but the method also has the shortcomings such as the not reproducible usability of metal base and time loss length simultaneously.Thereby electrochemistry bubbling is this can be reduced time loss and can guarantee that the technology that metal base can reuse arises at the historic moment simultaneously.Electrochemistry bubbling technology is to form one layer of polymeric protective layer on the Graphene surface being grown in metal base; and be placed in electrolytic solution and be connected with power cathode; adopt the conductive electrodes such as graphite be placed in electrolytic solution and be connected with positive source; utilize in brine electrolysis process the bubble forming between metal base and Graphene to realize the separated of Graphene and metal substrate, then transferred in target substrate.In prior art, the method that only bubbling shifts after the spin on polymers protective layer of Graphene surface has the unsettled shortcoming of technique, easily causes the breaking of curling and graphene film of polymkeric substance protective membrane in transfer process.And Ce ' sar J.Lockhart de la Rosa proposes polymer protective layer outward more additional polyethylene terephthalate (PET) though the method for support frame can improve the technology stability of transfer process; but only can shift the Graphene of framework inside, and fail to realize the complete transfer of graphene film.Simultaneously; between PETYu lower floor polymer protective layer in the method, adopt gluing mode; need by dropping in liquid also the mode of the sticking polymkeric substance drop of tool (as polymetylmethacrylate) realize the laminating of PETYu lower floor polymer protective layer, technological process is more loaded down with trivial details.
Therefore, the present invention is directed to the problems referred to above, intend introducing novel material, utilize its suitable surface energy or viscosity own, can directly not need gluing with lower polymeric material laminating, and characteristic that can nondestructively peeling after transfer, to can meet simplification, stabilization process and guarantee the complete transfer of graphene film and the recycling of metal base simultaneously.
Summary of the invention
The shortcoming of prior art in view of the above; the object of the present invention is to provide a kind of transfer method of graphene film; be used for solving and between prior art support frame and polymer protective layer, need to drip viscous drop and strengthen laminating dynamics, and the follow-up problem such as can not completely shift of Graphene.
For achieving the above object and other relevant objects, the invention provides a kind of transfer method of graphene film, the transfer method of described graphene film at least comprises step:
1) provide a metal base, in described metal substrate surface, be formed with successively graphene film, organic polymer protective layer and polymer frame supporting layer, described organic polymer protective layer and polymer frame supporting layer all have surface energy or viscosity;
2) described graphene film and metal base are peeled off, then by described graphene film and target substrate laminating;
3) peel off successively described polymer frame supporting layer and organic polymer protective layer.
As a kind of preferred version of the transfer method of graphene film of the present invention, the material that described metal base is be in Au, Co, Pt, Pd, Ir, Ru, Ni, Cu one or more alloy material or be coated with the tinsel of above metallic substance.
As a kind of preferred version of the transfer method of graphene film of the present invention, described organic polymer protective layer is selected from a kind of in polymethylmethacrylate, epoxy resin, polyethylene terephthalate, transparent fluoro-resin, polydimethylsiloxane.
As a kind of preferred version of the transfer method of graphene film of the present invention, adopt that dipping lifts, a kind of technique in spin coating, scraper, spraying, wet coating, silk screen printing, roller coating or board-like coating prepares described organic polymer protective layer.
As a kind of preferred version of the transfer method of graphene film of the present invention, in described technique, adopt a kind of in methyl-phenoxide, chlorobenzene, chloroform, methylene dichloride or trichloromethane to form process slurry as organic polymer protective layer described in dissolution with solvents.
As a kind of preferred version of the transfer method of graphene film of the present invention, in described technique, need to heat-treat to realize solidifying of described organic polymer protective layer.
As a kind of preferred version of the transfer method of graphene film of the present invention, described organic polymer protective layer thickness is 300～800 nanometers.
As a kind of preferred version of the transfer method of graphene film of the present invention, described polymer frame supporting layer comprises hot stripping tape or polydimethylsiloxane.
As a kind of preferred version of the transfer method of graphene film of the present invention, described polymer frame supporting layer thickness is 0.1～5 millimeter.
As a kind of preferred version of the transfer method of graphene film of the present invention, adopt cutting technique to prepare described polymer frame supporting layer.
As a kind of preferred version of the transfer method of graphene film of the present invention, the frame shape of described polymer frame supporting layer is consistent with described metal base, frame outer and metal base justified margin, and leg of frame wide region is 1～10 millimeter.
As a kind of preferred version of the transfer method of graphene film of the present invention, described step 2) in adopt electrochemistry Bubbling method that described graphene film and metal base are peeled off.
As a kind of preferred version of the transfer method of graphene film of the present invention, described step 2) in the step of graphene film and target substrate laminating is specifically comprised:
2-1) by target substrate described in ultrasonic cleaning, and the one-piece construction that comprises graphene film of peeling off acquisition is placed in described target substrate, washed with de-ionized water, more naturally dry;
2-2) heat-treat, the bonding force between described graphene film and target substrate is strengthened.
As a kind of preferred version of the transfer method of graphene film of the present invention, described step 2-1) in the time range of naturally drying be 0.1～3 hour.
As step 2-2 described in a kind of preferred version of the transfer method of graphene film of the present invention) in Heating temperature be 90～180 ℃, be 5～30 minutes heat-up time.
As step 3 described in a kind of preferred version of the transfer method of graphene film of the present invention) in adopt the method for mechanically peel to peel off described polymer frame supporting layer, after heat-treating, while hot described polymer frame supporting layer is taken off.
As step 3 described in a kind of preferred version of the transfer method of graphene film of the present invention) in adopt the mode of annealing under organic solvent dissolution and/or reducing atmosphere to peel off described organic polymer protective layer.
As organic solvent described in a kind of preferred version of the transfer method of graphene film of the present invention, be selected from a kind of in acetone, acetic acid, toluene, chlorine benzene,toluene,xylene, methylene dichloride, trichloromethane, ethyl methyl ketone, butylacetate, dioxane, normal hexane, hexanaphthene, dimethyl formamide.
As mentioned above; the transfer method of graphene film of the present invention; there is following beneficial effect: it is research object that the transfer of graphene film in metal base is take in the present invention; for prior art, improve; on the basis of existing electrochemistry Bubbling method, introduce the peelable polymer frame supporting layer that self there is viscosity and do not damage organic polymer protective layer, thereby thereby improving electrochemistry Bubbling method technology stability and reducing the utilization ratio that the complete transfer that realizes graphene film on the basis of the loaded down with trivial details degree of prior art processes guarantees Graphene.The method not only retained electrochemistry Bubbling method with respect to tradition dissolve the saving time of substrate method, the advantage such as metal base can reuse, and also solved simultaneously the technique existing in existing Bubbling method technology unstable with Graphene cannot complete transfer problem.The improvement of this technical scheme, has very important realistic meaning to the transfer of graphene film and application.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the transfer method of graphene film of the present invention.
Fig. 2～Fig. 4 is shown as the transfer method step 1 of graphene film of the present invention) structural representation that presents.
Fig. 5～Fig. 6 is shown as the transfer method step 2 of graphene film of the present invention) structural representation that presents.
Fig. 7～Fig. 8 is shown as the transfer method step 3 of graphene film of the present invention) structural representation that presents.
Element numbers explanation
101 metal base
102 graphene films
103 organic polymer protective layers
104 polymer frame supporting layers
105 target substrate
Embodiment
Below, by specific specific examples explanation embodiments of the present invention, those skilled in the art can understand other advantages of the present invention and effect easily by the disclosed content of this specification sheets.The present invention can also be implemented or be applied by other different embodiment, and the every details in this specification sheets also can be based on different viewpoints and application, carries out various modifications or change not deviating under spirit of the present invention.
Refer to accompanying drawing 1 to Fig. 8.It should be noted that, the diagram providing in the present embodiment only illustrates basic conception of the present invention in a schematic way, satisfy and only show with assembly relevant in the present invention in graphic but not component count, shape and size drafting while implementing according to reality, during its actual enforcement, kenel, quantity and the ratio of each assembly can be a kind of random change, and its assembly layout kenel also may be more complicated.
As shown in Figure 1, the invention provides a kind of transfer method of graphene film, shown in the transfer method of graphene film at least comprise the following steps:
S1, provides a metal base, in described metal substrate surface, is formed with successively graphene film, organic polymer protective layer and polymer frame supporting layer, and described organic polymer protective layer and polymer frame supporting layer all have surface energy or viscosity;
S2, peels off described graphene film and metal base, then by described graphene film and target substrate laminating;
S3, peels off described polymer frame supporting layer and organic polymer protective layer successively.
Below in conjunction with concrete accompanying drawing, the transfer method of graphene film of the present invention is done to detailed introduction.
First perform step S1; as shown in Figure 2 to 3; one metal base 101 is provided; on described metal base 101 surfaces, be formed with successively graphene film 102, organic polymer protective layer 103 and polymer frame supporting layer 104, described organic polymer protective layer 103 and polymer frame supporting layer 104 all have surface energy or viscosity.
The material that described metal base 101 can be in Au, Co, Pt, Pt, Pd, Ir, Ru, Ni, Cu one or more alloy material or be coated with other tinsels of above metallic substance.Certainly, can be also other suitable catalytic substrate, at this, do not limit.In the present embodiment, adopt Copper Foil as metal catalytic substrate.
Can adopt chemical vapour deposition (CVD) method to prepare graphene film 102, detailed process is: Copper Foil is put into beaker, use successively deionized water, acetone, ethanol ultrasonic cleaning; Copper Foil after having cleaned is put into acetic acid and soak, after taking out, use washed with de-ionized water, N
2dry up; Subsequently Copper Foil is put in the silica tube on tube furnace, vacuumized; Pass into H
2, flow is chosen for 30～100sccm, is warming up to 900～1100 degree simultaneously; After equitemperature is stable, pass into CH
4, flow is chosen for 0.1～5sccm, time 0.5～10min; After cooling, take out the Copper Foil that covers with Graphene, as shown in Figure 2.Can see, the upper and lower surface growth of Copper Foil has graphene film 102, and we only need to choose one of them lip-deep graphene film 102 as research object.
In the present embodiment, can adopt the mode of spin coating to prepare described organic polymer protective layer 103, certainly, also can adopt in other embodiments the suitable techniques such as dipping lifts, spraying, silk screen printing to prepare described organic polymer protective layer 103.The detailed process that adopts the method for spin coating to be prepared with organic polymer protective layer 103 is: first polymethylmethacrylate (PMMA) is dissolved in solvent (in methyl-phenoxide, chlorobenzene, chloroform, methylene dichloride or trichloromethane a kind of), form slurry, afterwards at the surperficial spin coating one deck of described graphene film 102 PMMA slurry, PMMA concentration is 10～90mg/ml, spin coating rotating speed is 3000～9000rmp, and the spin coating time is 10～150s; The complete Copper Foil of spin coating is put in baking oven and toasted to solidify PMMA, and as shown in Figure 3, PMMA organic polymer protective layer 103 thickness of acquisition are in 300～800 nanometer range.In other embodiments, described organic polymer protective layer 103 can also be a kind of of epoxy resin, polyethylene terephthalate, transparent fluoro-resin, polydimethylsiloxane etc.
Method that can cutting forms described polymer frame supporting layer 104, its detailed process is: first selecting thickness is polydimethylsiloxane (PDMS) film of 0.1～5 millimeter, be cut into and the similar shape of Copper Foil, and middle portion is removed, form square frame, the outer of square frame and the justified margin of Copper Foil, 1～10 millimeter of framework hem width; Square frame is fitted on Copper Foil, and applying light, guarantees laminating, and as shown in Figure 4, the thickness of the polymer frame supporting layer 104 obtaining is within the scope of 0.1～5 millimeter.
It should be noted that; the material requirements of selected organic polymer protective layer 103 and polymer frame supporting layer 104 has suitable surface can and itself will have certain viscosity; so that both can have good adhesivity when laminating, and require both when follow-up peeling off, can easily separate.In addition, organic polymer protective layer 103 and polymer frame supporting layer 104 can not be selected commaterial simultaneously.
Then perform step S2, as shown in Figure 5 and Figure 6, described graphene film 102 is peeled off with metal base 101, then by described graphene film 102 and target substrate 105 laminatings.
Can adopt electrochemistry Bubbling method to peel off graphene film 102 and metal base 101; detailed process is: the structure that step S1 is made is connected with power cathode; choosing Pt is connected with positive source; integral body is placed in 0.5～5M NaOH electrolytic solution; form loop line; regulating voltage and electric current, make produced bubble that the graphene film one-piece construction being attached to by the organic polymer protective membrane of frame supported is separated with Copper Foil, as shown in Figure 5.
Described graphene film 102 specifically comprises with the step of target substrate 105 laminatings: choose silicon chip that top layer is silicon-dioxide or silica glass etc. as target substrate 105, by target substrate described in ultrasonic cleaning 105, and the one-piece construction that comprises graphene film 102 of peeling off acquisition is picked up gently and is placed in the described target substrate 105 cleaning up from electrolytic solution, use again washed with de-ionized water, one-piece construction after cleaning is pulled out, be placed in 0.1～3h under room temperature, until water all volatilizees, naturally dry; Afterwards this structure is placed in to 90～180 degree baking ovens and toasts 5～30 minutes, the bonding force between described graphene film 102 and target substrate 101 is strengthened.The structure obtaining as shown in Figure 6.
Finally perform step S3, as shown in Figure 7 and Figure 8, peel off successively described polymer frame supporting layer 104 and organic polymer protective layer 103.
Adopt the method for mechanically peel to peel off described polymer frame supporting layer 104, after the thermal treatment of carrying out step S2, while hot described polymer frame supporting layer 104 is directly taken off, as shown in Figure 7.
After polymer-stripping frame supported layer 104, Jiang Qipao enters in acetone to remove organic polymer protective layer 103PMMA, obtains and is positioned at the graphene film 102 in target substrate 105 subsequently, as shown in Figure 8.Also can remove organic polymer protective layer 103 by the mode of annealing under reducing atmosphere.Certainly; can also adopt the method for the two kinds of mode combinations of annealing under organic solvent dissolution and reducing atmosphere to remove organic polymer protective layer 103, first steeped in acetone, remove organic polymer protective layer 103PMMA then under reducing atmosphere annealing to remove the resistates of organic polymer protective layer 103.
Described organic solvent be except selecting acetone, can also be selected from a kind of in acetic acid, toluene, chlorine benzene,toluene,xylene, methylene dichloride, trichloromethane, ethyl methyl ketone, butylacetate, dioxane, normal hexane, hexanaphthene, dimethyl formamide.
In sum, the invention provides a kind of transfer method of graphene film, described method comprises: first a metal base is provided, in described metal substrate surface, be formed with successively graphene film, organic polymer protective layer and polymer frame supporting layer, described organic polymer protective layer and polymer frame supporting layer all have surface energy or viscosity; Afterwards described graphene film and metal base are peeled off, then by described graphene film and target substrate laminating; Finally peel off successively described polymer frame supporting layer and organic polymer protective layer.Suitable surface energy or viscosity own that the present invention utilizes organic polymer protective layer and polymer frame supporting layer to have; both can directly fit and do not need gluing, and after transfer, have can nondestructively peeling characteristic meet simplification, stabilization process simultaneously and guarantee the complete transfer of graphene film and the recycling of metal base.
So the present invention has effectively overcome various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all can, under spirit of the present invention and category, modify or change above-described embodiment.Therefore, such as in affiliated technical field, have and conventionally know that the knowledgeable, not departing from all equivalence modifications that complete under disclosed spirit and technological thought or changing, must be contained by claim of the present invention.
Claims (18)
1. a transfer method for graphene film, is characterized in that, the transfer method of described graphene film at least comprises step:
1) provide a metal base, in described metal substrate surface, be formed with successively graphene film, organic polymer protective layer and polymer frame supporting layer, described organic polymer protective layer and polymer frame supporting layer all have surface energy or viscosity;
2) described graphene film and metal base are peeled off, then by described graphene film and target substrate laminating;
3) peel off successively described polymer frame supporting layer and organic polymer protective layer.
2. the transfer method of graphene film according to claim 1, is characterized in that: the material of described metal base be in Au, Co, Pt, Pd, Ir, Ru, Ni, Cu one or more alloy material or be coated with the tinsel of above metallic substance.
3. the transfer method of graphene film according to claim 1, is characterized in that: described organic polymer protective layer is selected from a kind of in polymethylmethacrylate, epoxy resin, polyethylene terephthalate, transparent fluoro-resin, polydimethylsiloxane.
4. the transfer method of graphene film according to claim 1, is characterized in that: adopt that dipping lifts, a kind of technique in spin coating, scraper, spraying, wet coating, silk screen printing, roller coating or board-like coating prepares described organic polymer protective layer.
5. the transfer method of graphene film according to claim 4; it is characterized in that: in described technique, adopt a kind of in methyl-phenoxide, chlorobenzene, chloroform, methylene dichloride or trichloromethane to form process slurry as organic polymer protective layer described in dissolution with solvents.
6. the transfer method of graphene film according to claim 4, is characterized in that: in described technique, need to heat-treat to realize solidifying of described organic polymer protective layer.
7. the transfer method of graphene film according to claim 1, is characterized in that: described organic polymer protective layer thickness is 300～800 nanometers.
8. the transfer method of graphene film according to claim 1, is characterized in that: described polymer frame supporting layer comprises hot stripping tape or polydimethylsiloxane.
9. the transfer method of graphene film according to claim 1, is characterized in that: described polymer frame supporting layer thickness is 0.1～5 millimeter.
10. the transfer method of graphene film according to claim 1, is characterized in that: adopt cutting technique to prepare described polymer frame supporting layer.
The transfer method of 11. graphene films according to claim 1, is characterized in that: the frame shape of described polymer frame supporting layer is consistent with described metal base, frame outer and metal base justified margin, and leg of frame wide region is 1～10 millimeter.
The transfer method of 12. graphene films according to claim 1, is characterized in that: described step 2), adopt electrochemistry Bubbling method that described graphene film and metal base are peeled off.
The transfer method of 13. graphene films according to claim 1, is characterized in that: described step 2), the step of graphene film and target substrate laminating is specifically comprised:
2-1) by target substrate described in ultrasonic cleaning, and the one-piece construction that comprises graphene film of peeling off acquisition is placed in described target substrate, washed with de-ionized water, more naturally dry;
2-2) heat-treat, the bonding force between described graphene film and target substrate is strengthened.
The transfer method of 14. graphene films according to claim 13, is characterized in that: the time range of naturally drying described step 2-1) is 0.1～3 hour.
The transfer method of 15. graphene films according to claim 13, is characterized in that: described step 2-2), Heating temperature is 90～180 ℃, and be 5～30 minutes heat-up time.
The transfer method of 16. graphene films according to claim 15, is characterized in that: described step 3), adopt the method for mechanically peel to peel off described polymer frame supporting layer, after heat-treating, while hot described polymer frame supporting layer is taken off.
The transfer method of 17. graphene films according to claim 1, is characterized in that: described step 3), adopt the mode of annealing under organic solvent dissolution and/or reducing atmosphere to peel off described organic polymer protective layer.
The transfer method of 18. graphene films according to claim 17, is characterized in that: described organic solvent is selected from a kind of in acetone, acetic acid, toluene, chlorine benzene,toluene,xylene, methylene dichloride, trichloromethane, ethyl methyl ketone, butylacetate, dioxane, normal hexane, hexanaphthene, dimethyl formamide.
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