CN103922327A - Method for nondestructively transferring graphene thin film in large area - Google Patents
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Abstract
The invention relates to a method for nondestructively transferring a graphene thin film in a large area. The method comprises the following steps: (1) aligning and attaching the both surfaces of a metal substrate on which a graphene thin film grows to a transfer medium, and carrying out roll pressing by using a rolling press to obtain a transfer medium/graphene thin film/metal substrate/graphene thin film/transfer medium laminar material; (2) with the laminar material obtained in the step (1) as a positive electrode and a platinum electrode as a negative electrode, inserting into an electrolytic cell, applying a direct voltage, putting the transfer medium/graphene thin film into corrosive liquid after the transfer medium/graphene thin film is completely peeled from the metal substrate, etching the residual metal on the surface of the graphene thin film, then rinsing with distilled water, and drying by blowing; and (3) attaching the transfer medium/graphene thin film to a target substrate, and carrying out roll pressing on a thermal rolling press, thus transferring the graphene into the target substrate. According to the method, the residual metal on the graphene thin film is removed by using the corrosive liquid, and thus the defect of metal residual on the surface of the graphene thin film in an existing electrochemical peeling method is overcome.
Description
Technical field
The present invention relates to graphene film transfer method, the harmless method that shifts graphene film of especially a kind of big area.
Background technology
The transfer method of graphene film at present, according to shifting in the process of graphene film, to the difference of growth substrate processing mode, can be divided into " substrate etch " and " non-substrate etch "." substrate etch " is conventionally first Graphene surface coverage transfer medium (heat discharges glue etc. for PMMA, PDMS); Recycle suitable corrosive fluid (FeCl3 etc.) by metal base erosion removal, then transfer medium/graphene film is transferred in target substrate; Finally remove transfer medium, realize the transfer of Graphene." non-substrate etch " comprising: electrochemistry transfer method, dry method shifts and mechanically peel method, the people such as Gao adopt electrochemistry transfer method, utilize the chemical property difference between metal base and Graphene, form surface reaction, metal substrate surface produces microbubble and drives Graphene to peel off (specifically referring to Gao L, Ren W, Xu H, et al.Repeated growth and bubbling transfer of graphene with millimetre-size single-crystal grains using platinum[J] .Nature communications, 2012, 3:699.), the people such as Lock adopt dry method to shift, form covalent linkage by selecting between suitable linking agent and Graphene, adsorptive power between covalent linkage produces thus Graphene and polymkeric substance is than large many of the adsorptive power between Graphene and metal, for Graphene provides a kind of effectively approach (specifically referring to Lock E H with effective separation of metallic matrix, Baraket M, Laskoski M, et al.High-quality uniform dry transfer of graphene to polymers[J] .Nano letters, 2011,12 (1): 102-107.), the people such as Yoon adopt mechanically peel method, utilize reactive force strong between epoxy resin and Graphene, target substrate and Graphene are coupled together by epoxy cement technology, utilize certain mechanical force to strip down from the growth end complete Graphene, and can not destroy growth substrate, thereby realize nondestructive transfer (specifically referring to Yoon T, Shin W C, Kim T Y, et al.Direct measurement of adhesion energy of monolayer graphene as-grown on copper and its application to renewable transfer process[J] .Nano letters, 2012, 12 (3): 1448-1452.).
Wherein, " substrate etch " is a kind of transfer method the most extensively adopting, in this method, owing to having used transfer medium, although guaranteed the stability shifting, also increased the complexity of process simultaneously.Main, the method is that to sacrifice growth substrate be prerequisite, and cost is high, be unfavorable for quantizing to produce and application,, and ensureing that the structural integrity of big area Graphene, the aspect such as pollution-free still have deficiency.In addition, for accurate microelectronic, need to use precious metal single crystal substrates (as Pt, Ru etc.) to carry out the single crystal graphene film of growing large-size.Price and the strong erosion resistance of considering single crystal substrates costliness, therefore " substrate etch " is also inapplicable.In " non-substrate etch ": electrochemistry transfer method is incorporated into interfacial electrochemistry reaction process in Graphene transfer, this method has high efficiency, low consumption, the advantages such as recoverable metal substrate, but because its supporting layer is to be obtained by polymethyl methacrylate (PMMA) spin coating, PMMA supporting layer is very thin, easy breakage and fold in the process shifting, can not carry out large-area transfer, and in the process that uses electrochemical stripping graphene film, inevitably have the surface that some residual metals are attached to graphene film, in addition PMMA easy cull in the process of removing, affect optics and the conductivity of graphene film, and dry method shifts and mechanically peel rule is to utilize a kind of suitable binding agent, there are the metal base of Graphene and target substrate to fit together growth, then utilize the sticking power between adhesive power between Graphene and binding agent large and Graphene and Copper Foil that Graphene is transferred to target substrate, but the graphene film that this mode shifts is breakage and the gravitation due to binding agent easily, can cause the conductivity of graphene film and light transmission to decline.How efficient, low consumption, in not sacrificial metal substrate, keep, in the situation of graphene film self excellent properties, large-area graphene film being transferred to target substrate, be current urgent problem.
Summary of the invention
The surperficial deficiency that the application overcomes that substrate etch cost in prior art is high, electrochemistry transfer method has residual metal and be attached to graphene film, provides a kind of big area the harmless method that shifts graphene film.
The harmless method that shifts graphene film of big area, step is as follows:
(1) growth there is is the metal base two sides of graphene film all aim at laminating with transfer medium, re-use roll squeezer and carry out roll-in, obtain transfer medium/graphene film/metal base/graphene film/transfer medium stratified material;
(2) stratified material step (1) being obtained is as negative pole, using platinum electrode as positive pole, insertion is equipped with in electrolyzer, pass to volts DS, medium/graphene film to be transferred is completely from metal base is peeled off, transfer medium/graphene film is put into corrosive fluid etching graphene film surface residual metal, then with distilled water rinsing three times and dry up;
(3) transfer medium/graphene film step (2) being obtained is being fitted with target substrate, and on hot-rolling press, carries out roll-in, and Graphene is transferred in target substrate.
As preferably, the described metal base of step (1) is copper or nickel.
Further, the described transfer medium of step (1) is that heat discharges adhesive tape or Pressuresensitive Tape.
Further, the described roll squeezer roller bearing spacing of step (1) is 0～2mm, and roll-in speed is 50～300rpm.
As preferably, in the described electrolyzer of step (2), ionogen is the one in ammonium sulfate, Potassium Persulphate or sodium hydroxide, and wherein electrolyte concentration is 0.1～1mol/L.
Further, the described volts DS of step (2) is 8～30V, and electrolysis time is 1～20h.
As preferably, the described corrosive fluid of step (2) is rare nitric acid that hydrochloric acid and the hydrogen peroxide mass ratio mixing solutions that is 1:1 or massfraction are 5%, and described transfer medium/graphene film residence time in corrosive fluid is 10～60min.
Further, the described hot-rolling press roller bearing spacing of step (3) is 0～5mm, and roll-in speed is 50～300rpm, and wherein hot-rolling press roller bearing temperature is 120～150 DEG C.
Further, described target substrate is PET, glass or silicon chip.
The invention has the beneficial effects as follows: utilize the mode of electrochemical stripping to weaken the bonding force between Graphene and metal base, graphene film is transferred on transfer medium, and utilize corrosive fluid to remove the residual metal above graphene film, overcome the residual defect of graphene film surface metal in existing electrochemical stripping method, improve the performance of graphene film, overcome the shortcoming that existing electrochemical stripping method can only shift small area graphene film and easy cull simultaneously, by the mode that the method for electrochemistry up-stripping and the continuous transfer techniques of roller press type are combined, transfer efficiency is high, realize efficient recovery and the recycling of metallic growth substrate simultaneously.
Embodiment
Further illustrate technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is the restriction to technical scheme.
Embodiment 1
Growth there is is the Copper Foil of graphene film aim at laminating with heat release adhesive tape, re-use roll squeezer and carry out roll-in, heat release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 0.5mm, roll-in speed is 50rpm, obtains heat and discharges adhesive tape/graphene film/metal base/graphene film/heat release adhesive tape stratified material;
Above-mentioned stratified material is as negative pole, using platinum electrode as positive pole, be inserted in the tank that ammonium persulphate electrolytic solution is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 0.1mol/L, voltage 8V, time 1h, treat that heat discharges adhesive tape/graphene film and peels off from metal base completely, heat is discharged to the mixing solutions etching 10min that adhesive tape/graphene film is 1:1 at hydrochloric acid and hydrogen peroxide mass ratio.Re-use distilled water rinsing 10min, in triplicate, then use nitrogen to dry up, graphene film is transferred to heat and discharges on adhesive tape.Have the heat of graphene film to discharge adhesive tape and PET laminating transfer, carry out roll-in on roll squeezer, roll squeezer roller bearing spacing is 0.5mm, and roll-in speed is 50rpm, 120 DEG C of roller bearing temperature, and graphene film is transferred to PET substrate.
Embodiment 2
Growth there is is the Copper Foil of graphene film aim at laminating with heat release adhesive tape, re-use roll squeezer and carry out roll-in, heat release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 1mm, roll-in speed is 150rpm, obtains heat and discharges adhesive tape/graphene film/metal base/graphene film/heat release adhesive tape stratified material;
Using stratified material obtained above as negative pole, using platinum electrode as positive pole, be inserted in the tank that Potassium Persulphate electrolytic solution is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 5h, treat that heat discharges adhesive tape/graphene film and peels off from metal base completely, heat is discharged to the mixing solutions etching 30min that adhesive tape/graphene film is 1:1 at hydrochloric acid and hydrogen peroxide mass ratio.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred to heat and discharges on adhesive tape.With changing soft roller, there is the heat of graphene film to discharge adhesive tape and glass gluing transfer, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 1mm, roll-in speed is 150rpm, 130 DEG C of roller bearing temperature, graphene film is transferred to substrate of glass.
Embodiment 3
Growth there is is the Copper Foil of graphene film aim at laminating with heat release adhesive tape, re-use roll squeezer and carry out roll-in, heat release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 2mm, roll-in speed is 300rpm, obtains heat and discharges adhesive tape/graphene film/metal base/graphene film/heat release adhesive tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that electrolytic solution is housed, pass to volts DS, sodium hydroxide electrolyte concentration in electrolytic solution is 1mol/L, voltage 30V, time 20h, treat that heat discharges adhesive tape/graphene film and peels off from metal base completely, heat is discharged to the mixing solutions etching 60min that adhesive tape/graphene film is 1:1 at hydrochloric acid and hydrogen peroxide mass ratio.Re-use distilled water rinsing 60min, in triplicate, then use nitrogen to dry up, graphene film is transferred to heat and discharges on adhesive tape.With changing soft roller, there is the heat of graphene film to discharge adhesive tape and silicon chip laminating transfer, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 5mm, and roll-in speed is 300rpm, and 150 DEG C of roller bearing temperature, at the bottom of graphene film is transferred to silicon wafer-based.
Embodiment 4
Growth there is is the nickel foil of graphene film aim at laminating with heat release adhesive tape, re-use roll squeezer and carry out roll-in, heat release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 0.5mm, roll-in speed is 50rpm, obtains heat and discharges adhesive tape/graphene film/metal base/graphene film/heat release adhesive tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that ammonium persulphate electrolytic solution is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 0.1mol/L, voltage 8V, time 1h, treat that heat discharges adhesive tape/graphene film and peels off from metal base completely, heat is discharged to etching 10min in rare nitric acid that adhesive tape/graphene film is 5% at massfraction.Re-use distilled water rinsing 10min, in triplicate, then use nitrogen to dry up, graphene film is transferred to heat and discharges on adhesive tape.Have the heat of graphene film to discharge adhesive tape and PET laminating transfer, carry out roll-in on roll squeezer, roll squeezer roller bearing spacing is 0.5mm, and roll-in speed is 50rpm, 120 DEG C of roller bearing temperature, and graphene film is transferred to PET substrate.
Embodiment 5
Growth there is is the nickel foil of graphene film aim at laminating with heat release adhesive tape, re-use roll squeezer and carry out roll-in, heat release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 1mm, roll-in speed is 150rpm, obtains heat and discharges adhesive tape/graphene film/metal base/graphene film/heat release adhesive tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that electrolytic solution is housed, pass to volts DS, Potassium Persulphate electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 5h, treat that heat discharges adhesive tape/graphene film and peels off from metal base completely, heat is discharged to etching 30min in rare nitric acid that adhesive tape/graphene film is 5% at massfraction.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred to heat and discharges on adhesive tape.With changing soft roller, there is the heat of graphene film to discharge adhesive tape and glass gluing transfer, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 1mm, roll-in speed is 150rpm, 130 DEG C of roller bearing temperature, graphene film is transferred to substrate of glass.
Embodiment 6
Growth there is is the nickel foil of graphene film aim at laminating with heat release adhesive tape, re-use roll squeezer and carry out roll-in, heat release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 2mm, roll-in speed is 300rpm, obtains heat and discharges adhesive tape/graphene film/metal base/graphene film/heat release adhesive tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that NaOH electrolyte is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 1mol/L, voltage 30V, time 20h, treat that heat discharges adhesive tape/graphene film and peels off from metal base completely, heat is discharged to etching 60min in rare nitric acid that adhesive tape/graphene film is 5% at massfraction.Re-use distilled water rinsing 60min, in triplicate, then use nitrogen to dry up, graphene film is transferred to heat and discharges on adhesive tape.With changing soft roller, there is the heat of graphene film to discharge adhesive tape and silicon chip laminating transfer, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 5mm, and roll-in speed is 300rpm, and 150 DEG C of roller bearing temperature, at the bottom of graphene film is transferred to silicon wafer-based.
Embodiment 7
Growth there is is the Copper Foil of graphene film aim at laminating with Pressuresensitive Tape, re-use roll squeezer and carry out roll-in, Pressuresensitive Tape and metal base are fully fitted, roll squeezer roller bearing spacing is 2mm, roll-in speed is 300rpm, obtains Pressuresensitive Tape/graphene film/metal base/graphene film/Pressuresensitive Tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that Potassium Persulphate electrolytic solution is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 5h, treat that Pressuresensitive Tape/graphene film peels off from metal base completely, the mixing solutions etching 30min that is 1:1 at hydrochloric acid and hydrogen peroxide mass ratio by Pressuresensitive Tape/graphene film.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Pressuresensitive Tape.With changing hard roller, transfer is had to Pressuresensitive Tape and the PET laminating of graphene film, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 2.5mm, roll-in speed is 150rpm, 130 DEG C of roller bearing temperature, graphene film is transferred to PET substrate.
Embodiment 8
Growth there is is the nickel foil of graphene film aim at laminating with Pressuresensitive Tape, re-use roll squeezer and carry out roll-in, Pressuresensitive Tape and metal base are fully fitted, roll squeezer roller bearing spacing is 2mm, roll-in speed is 300rpm, obtains Pressuresensitive Tape/graphene film/metal base/graphene film/Pressuresensitive Tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that Potassium Persulphate electrolytic solution is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 5h, treat that Pressuresensitive Tape/graphene film peels off from metal base completely, etching 30min in the rare nitric acid that is 5% at massfraction by Pressuresensitive Tape/graphene film.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Pressuresensitive Tape.With changing hard roller, transfer is had to Pressuresensitive Tape and the PET laminating of graphene film, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 2.5mm, roll-in speed is 150rpm, 130 DEG C of roller bearing temperature, graphene film is transferred to substrate of glass.
Embodiment 9
Growth there is is the Copper Foil of graphene film aim at laminating with Pressuresensitive Tape, re-use roll squeezer and carry out roll-in, Pressuresensitive Tape and metal base are fully fitted, roll squeezer roller bearing spacing is 0.5mm, roll-in speed is 50rpm, obtains Pressuresensitive Tape/graphene film/metal base/graphene film/Pressuresensitive Tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that NaOH electrolyte is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 8h, treat that Pressuresensitive Tape/graphene film peels off from metal base completely, the mixing solutions etching 30min that is 1:1 at hydrochloric acid and hydrogen peroxide mass ratio by Pressuresensitive Tape/graphene film.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Pressuresensitive Tape.With changing hard roller, transfer is had to Pressuresensitive Tape and the PET laminating of graphene film, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 2.5mm, roll-in speed is 150rpm, 140 DEG C of roller bearing temperature, graphene film is transferred to PET substrate.
Embodiment 10
Growth there is is the nickel foil of graphene film aim at laminating with Pressuresensitive Tape, re-use roll squeezer and carry out roll-in, Pressuresensitive Tape and metal base are fully fitted, roll squeezer roller bearing spacing is 0.5mm, roll-in speed is 50rpm, obtains Pressuresensitive Tape/graphene film/metal base/graphene film/Pressuresensitive Tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted in the tank that NaOH electrolyte is housed, pass to volts DS, electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 8h, treat that Pressuresensitive Tape/graphene film peels off from metal base completely, etching 30min in the rare nitric acid that is 5% at massfraction by Pressuresensitive Tape/graphene film.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Pressuresensitive Tape.With changing soft roller, transfer is had to Pressuresensitive Tape and the glass gluing of graphene film, on roll squeezer, carry out roll-in, roll squeezer roller bearing spacing is 2.5mm, roll-in speed is 150rpm, 140 DEG C of roller bearing temperature, graphene film is transferred to substrate of glass.
Comparative example 1
By " heat being discharged to the mixing solutions etching 10min that adhesive tape/graphene film hydrochloric acid and hydrogen peroxide mass ratio are 1:1 " in embodiment 1, step is removed, and other steps, condition are with embodiment 1.
The performance test of the graphene film that embodiment 1 and comparative example 1 make is as follows:
Record sheet resistance 1437 Ω/sq, the transmittance after single-layer graphene shifts is 95.7%; Be 872 Ω/sq and record sheet resistance after processing by corrosive fluid, transmittance is 97.6%, quite close to the transmittance of single-layer graphene, has greatly improved the performance of graphene film.
Transmittance is to record (using the PET that does not turn graphene film as reference) by Shanghai Shun's space 721 type spectrophotometers; Sheet resistance is to record with MCP-T370 four point probe tester.
Claims (9)
1. the harmless method that shifts graphene film of big area, is characterized in that: step is as follows:
(1) growth there is is the metal base two sides of graphene film all aim at laminating with transfer medium, re-use roll squeezer and carry out roll-in, obtain transfer medium/graphene film/metal base/graphene film/transfer medium stratified material;
(2) stratified material step (1) being obtained is as negative pole, using platinum electrode as positive pole, insertion is equipped with in electrolyzer, pass to volts DS, medium/graphene film to be transferred is completely from metal base is peeled off, transfer medium/graphene film is put into corrosive fluid etching graphene film surface residual metal, then with distilled water rinsing three times and dry up;
(3) transfer medium/graphene film step (2) being obtained is being fitted with target substrate, and on hot-rolling press, carries out roll-in, and Graphene is transferred in target substrate.
2. the harmless method that shifts graphene film of big area according to claim 1, is characterized in that: the described metal base of step (1) is copper or nickel.
3. the harmless method that shifts graphene film of big area according to claim 1, is characterized in that: the described transfer medium of step (1) is hot adhesive tape or the Pressuresensitive Tape of discharging.
4. the harmless method that shifts graphene film of big area according to claim 1, is characterized in that: the described roll squeezer roller bearing spacing of step (1) is 0.5～2mm, and roll-in speed is 50～300rpm.
5. the harmless method that shifts graphene film of big area according to claim 1, is characterized in that: in the electrolyzer described in step (2), ionogen is the one in ammonium sulfate, Potassium Persulphate or sodium hydroxide, and wherein electrolyte concentration is 0.1～1mol/L.
6. the harmless method that shifts graphene film of big area according to claim 1, is characterized in that: the described volts DS of step (2) is 8～30V, and electrolysis time is 1～20h.
7. the harmless method that shifts graphene film of big area according to claim 1, it is characterized in that: the described corrosive fluid of step (2) is rare nitric acid that hydrochloric acid and the hydrogen peroxide mass ratio mixing solutions that is 1:1 or massfraction are 5%, and described transfer medium/graphene film residence time in corrosive fluid is 10～60min.
8. the harmless method that shifts graphene film of big area according to claim 1, it is characterized in that: the described hot-rolling press roller bearing spacing of step (3) is 0.5～5mm, roll-in speed is 50～300rpm, and wherein hot-rolling press roller bearing temperature is 120～150 DEG C.
9. the harmless method that shifts graphene film of big area according to claim 1, is characterized in that: described target substrate is PET, glass or silicon chip.
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