CN103922327B - A kind of big area can't harm the method for transfer graphene film - Google Patents
A kind of big area can't harm the method for transfer graphene film Download PDFInfo
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Abstract
A kind of big area can't harm the method for transfer graphene film, (1) have the metal base two sides of graphene film all to aim at transfer medium growth to fit, use roll squeezer to carry out roll-in, obtain transfer medium/graphene film/metal base/graphene film/transfer medium stratified material; (2) stratified material step (1) obtained is as negative pole, using platinum electrode as positive pole, insertion is equipped with in electrolyzer, pass to volts DS, after medium/graphene film to be transferred is peeled off from metal base completely, transfer medium/graphene film is put into corrosive fluid and etch graphene film surface residual metal, then dry up with distilled water rinsing; (3) transfer medium/graphene film is being fitted with target substrate, and carries out roll-in on hot calender, and namely Graphene is transferred in target substrate.Utilize the residual metal above corrosive fluid removal graphene film, overcome the defect that in existing electrochemical stripping method, graphene film surface metal is residual.
Description
Technical field
The present invention relates to graphene film transfer method, especially a kind of big area can't harm the method for transfer graphene film.
Background technology
The transfer method of current graphene film, according in the process of transfer graphene film, to the difference of growth substrate processing mode, can be divided into " substrate corrosion method " and " non-substrate corrosion method "." substrate corrosion method " first covers transfer medium (PMMA, PDMS, Thermal release glue etc.) at graphenic surface usually; 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 corrosion method " comprising: electrochemistry transfer method, dry method transfer 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 see GaoL, RenW, XuH, etal.Repeatedgrowthandbubblingtransferofgraphenewithmill imetre-sizesingle-crystalgrainsusingplatinum [J] .Naturecommunications, 2012,3:699.), the people such as Lock adopt dry method to shift, covalent linkage is formed by selecting between suitable linking agent and Graphene, much larger than the adsorptive power between Graphene and metal of adsorptive power thus between the Graphene that produces of covalent linkage and polymkeric substance, for Graphene provides a kind of effective approach (specifically see LockEH with being effectively separated of metallic matrix, BaraketM, LaskoskiM, etal.High-qualityuniformdrytransferofgraphenetopolymers [J] .Nanoletters, 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 complete for Graphene can be stripped down from the growth end, and can not destroy growth substrate, thus realize nondestructive transfer (specifically see YoonT, ShinWC, KimTY, etal.Directmeasurementofadhesionenergyofmonolayergraphen eas-grownoncopperanditsapplicationtorenewabletransferpro cess [J] .Nanoletters, 2012, 12 (3): 1448-1452.).
Wherein, " substrate corrosion method " is a kind of transfer method the most extensively adopted, owing to employing transfer medium in this method, although ensure that the stability of transfer, too increases the complexity of process simultaneously.More importantly, the method is that cost is high to sacrifice premised on growth substrate, is unfavorable for quantizing to produce and application, and ensure large-area graphene structural integrity, pollution-free etc. in 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.Consider the price of single crystal substrates costliness and strong erosion resistance, therefore " substrate corrosion method " inapplicable.In " non-substrate corrosion method ": interfacial electrochemistry reaction process is incorporated in Graphene transfer by electrochemistry transfer method, this method has high efficiency, low consumption, the advantages such as recoverable metal substrate, but because its supporting layer is obtained by polymethyl methacrylate (PMMA) spin coating, PMMA supporting layer is very thin, easy damaged and fold in the process of transfer, large-area transfer can not be carried out, and using the process of 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 removed, affect optics and the conductivity of graphene film, and dry method transfer and mechanically peel rule utilize a kind of suitable binding agent, the metal base of Graphene and target substrate is had to fit together growth, then utilize large and between Graphene and Copper Foil the sticking power of the adhesive power between Graphene and binding agent that Graphene is transferred to target substrate, but the graphene film that this mode shifts is easily damaged and due to the gravitation of binding agent, the conductivity of graphene film and light transmission can be caused to decline.How efficient, low consumption, in not sacrificial metal substrate, when keeping graphene film self excellent properties, large-area graphene film is transferred to target substrate, is current urgent problem.
Summary of the invention
The application overcomes that substrate corrosion method cost in prior art is high, electrochemistry transfer method has the deficiency that residual metal is attached to the surface of graphene film, provides a kind of big area to can't harm the method for transfer graphene film.
Big area can't harm a method for transfer graphene film, and step is as follows:
(1) have the metal base two sides of graphene film all to aim at transfer medium growth to fit, 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) obtained is as negative pole, using platinum electrode as positive pole, insertion is equipped with in electrolyzer, pass to volts DS, after medium/graphene film to be transferred is peeled off from metal base completely, transfer medium/graphene film is put into corrosive fluid and etch graphene film surface residual metal, then dry up with distilled water rinsing three times;
(3) transfer medium/graphene film step (2) obtained is being fitted with target substrate, and carries out roll-in on hot calender, and namely Graphene is transferred in target substrate.
As preferably, the metal base described in step (1) is copper or nickel.
Further, the transfer medium described in step (1) is Thermal release adhesive tape or Pressuresensitive Tape.
Further, the roll squeezer roller bearing spacing described in step (1) is 0 ~ 2mm, and roll-in speed is 50 ~ 300rpm.
As preferably, 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.
Further, the volts DS described in step (2) is 8 ~ 30V, and electrolysis time is 1 ~ 20h.
As preferably, mixing solutions or the massfraction of to be hydrochloric acid and hydrogen peroxide mass ratio the be 1:1 of the corrosive fluid described in step (2) are the dust technology of 5%, and described transfer medium/graphene film residence time in corrosive fluid is 10 ~ 60min.
Further, the hot calender roller bearing spacing described in step (3) is 0 ~ 5mm, and roll-in speed is 50 ~ 300rpm, and wherein hot calender 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 bonding force between Graphene and metal base, graphene film is transferred on transfer medium, and utilize the residual metal above corrosive fluid removal graphene film, overcome the defect that in existing electrochemical stripping method, graphene film surface metal is residual, improve the performance of graphene film, overcome existing electrochemical stripping method simultaneously and can only shift small area graphene film and the shortcoming of easy cull, 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 embodiments can not be interpreted as it is restriction to technical scheme.
Embodiment 1
Growth had the Copper Foil of graphene film to aim at Thermal release adhesive tape to fit, re-use roll squeezer and carry out roll-in, Thermal release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 0.5mm, roll-in speed is 50rpm, obtains Thermal release adhesive tape/graphene film/metal base/graphene film/Thermal 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 Thermal release adhesive tape/graphene film is peeled off from metal base completely, Thermal release adhesive tape/graphene film is etched 10min at the mixing solutions that hydrochloric acid and hydrogen peroxide mass ratio are 1:1.Re-use distilled water rinsing 10min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Thermal release adhesive tape.Have the Thermal release adhesive tape of graphene film and PET to fit transfer, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 0.5mm, and roll-in speed is 50rpm, and roller bearing temperature 120 DEG C, graphene film is transferred to PET base.
Embodiment 2
Growth had the Copper Foil of graphene film to aim at Thermal release adhesive tape to fit, re-use roll squeezer and carry out roll-in, Thermal release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 1mm, roll-in speed is 150rpm, obtains Thermal release adhesive tape/graphene film/metal base/graphene film/Thermal 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 Thermal release adhesive tape/graphene film is peeled off from metal base completely, Thermal release adhesive tape/graphene film is etched 30min at the mixing solutions that hydrochloric acid and hydrogen peroxide mass ratio are 1:1.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Thermal release adhesive tape.With changing soft roller, transfer is had Thermal release adhesive tape and the glass gluing of graphene film, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 1mm, and roll-in speed is 150rpm, and roller bearing temperature 130 DEG C, graphene film is transferred to substrate of glass.
Embodiment 3
Growth had the Copper Foil of graphene film to aim at Thermal release adhesive tape to fit, re-use roll squeezer and carry out roll-in, Thermal release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 2mm, roll-in speed is 300rpm, obtains Thermal release adhesive tape/graphene film/metal base/graphene film/Thermal release adhesive tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted into and be equipped with in the tank of electrolytic solution, pass to volts DS, sodium hydroxide electrolyte concentration in electrolytic solution is 1mol/L, voltage 30V, time 20h, treat that Thermal release adhesive tape/graphene film is peeled off from metal base completely, Thermal release adhesive tape/graphene film is etched 60min at the mixing solutions that hydrochloric acid and hydrogen peroxide mass ratio are 1:1.Re-use distilled water rinsing 60min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Thermal release adhesive tape.With changing soft roller, have the Thermal release adhesive tape of graphene film and silicon chip to fit transfer, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 5mm, and roll-in speed is 300rpm, and roller bearing temperature 150 DEG C, graphene film is transferred at the bottom of silicon wafer-based.
Embodiment 4
Growth had the nickel foil of graphene film to aim at Thermal release adhesive tape to fit, re-use roll squeezer and carry out roll-in, Thermal release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 0.5mm, roll-in speed is 50rpm, obtains Thermal release adhesive tape/graphene film/metal base/graphene film/Thermal 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, treating that Thermal release adhesive tape/graphene film is peeled off from metal base completely, is etch 10min in the dust technology of 5% at massfraction by Thermal release adhesive tape/graphene film.Re-use distilled water rinsing 10min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Thermal release adhesive tape.Have the Thermal release adhesive tape of graphene film and PET to fit transfer, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 0.5mm, and roll-in speed is 50rpm, and roller bearing temperature 120 DEG C, graphene film is transferred to PET base.
Embodiment 5
Growth had the nickel foil of graphene film to aim at Thermal release adhesive tape to fit, re-use roll squeezer and carry out roll-in, Thermal release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 1mm, roll-in speed is 150rpm, obtains Thermal release adhesive tape/graphene film/metal base/graphene film/Thermal release adhesive tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted into and be equipped with in the tank of electrolytic solution, pass to volts DS, Potassium Persulphate electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 5h, treating that Thermal release adhesive tape/graphene film is peeled off from metal base completely, is etch 30min in the dust technology of 5% at massfraction by Thermal release adhesive tape/graphene film.Re-use distilled water rinsing 30min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Thermal release adhesive tape.With changing soft roller, transfer is had Thermal release adhesive tape and the glass gluing of graphene film, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 1mm, and roll-in speed is 150rpm, and roller bearing temperature 130 DEG C, graphene film is transferred to substrate of glass.
Embodiment 6
Growth had the nickel foil of graphene film to aim at Thermal release adhesive tape to fit, re-use roll squeezer and carry out roll-in, Thermal release adhesive tape and metal base are fully fitted, roll squeezer roller bearing spacing is 2mm, roll-in speed is 300rpm, obtains Thermal release adhesive tape/graphene film/metal base/graphene film/Thermal release adhesive tape stratified material;
Using above-mentioned stratified material as negative pole, using platinum electrode as positive pole, be inserted into and be equipped with in the tank of NaOH electrolyte, pass to volts DS, electrolyte concentration in electrolytic solution is 1mol/L, voltage 30V, time 20h, treating that Thermal release adhesive tape/graphene film is peeled off from metal base completely, is etch 60min in the dust technology of 5% at massfraction by Thermal release adhesive tape/graphene film.Re-use distilled water rinsing 60min, in triplicate, then use nitrogen to dry up, graphene film is transferred on Thermal release adhesive tape.With changing soft roller, have the Thermal release adhesive tape of graphene film and silicon chip to fit transfer, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 5mm, and roll-in speed is 300rpm, and roller bearing temperature 150 DEG C, graphene film is transferred at the bottom of silicon wafer-based.
Embodiment 7
Growth had the Copper Foil of graphene film to aim at Pressuresensitive Tape to fit, 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 is peeled off from metal base completely, Pressuresensitive Tape/graphene film is etched 30min at the mixing solutions that hydrochloric acid and hydrogen peroxide mass ratio are 1:1.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, have the Pressuresensitive Tape of graphene film and PET to fit transfer, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 2.5mm, and roll-in speed is 150rpm, and roller bearing temperature 130 DEG C, graphene film is transferred to PET base.
Embodiment 8
Growth had the nickel foil of graphene film to aim at Pressuresensitive Tape to fit, 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, treating that Pressuresensitive Tape/graphene film is peeled off from metal base completely, is etch 30min in the dust technology of 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, have the Pressuresensitive Tape of graphene film and PET to fit transfer, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 2.5mm, and roll-in speed is 150rpm, and roller bearing temperature 130 DEG C, graphene film is transferred to substrate of glass.
Embodiment 9
Growth had the Copper Foil of graphene film to aim at Pressuresensitive Tape to fit, 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 into and be equipped with in the tank of NaOH electrolyte, pass to volts DS, electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 8h, treat that Pressuresensitive Tape/graphene film is peeled off from metal base completely, Pressuresensitive Tape/graphene film is etched 30min at the mixing solutions that hydrochloric acid and hydrogen peroxide mass ratio are 1:1.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, have the Pressuresensitive Tape of graphene film and PET to fit transfer, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 2.5mm, and roll-in speed is 150rpm, and roller bearing temperature 140 DEG C, graphene film is transferred to PET base.
Embodiment 10
Growth had the nickel foil of graphene film to aim at Pressuresensitive Tape to fit, 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 into and be equipped with in the tank of NaOH electrolyte, pass to volts DS, electrolyte concentration in electrolytic solution is 0.5mol/L, voltage 15V, time 8h, treating that Pressuresensitive Tape/graphene film is peeled off from metal base completely, is etch 30min in the dust technology of 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 Pressuresensitive Tape and the glass gluing of graphene film, roll squeezer carries out roll-in, and roll squeezer roller bearing spacing is 2.5mm, and roll-in speed is 150rpm, and roller bearing temperature 140 DEG C, graphene film is transferred to substrate of glass.
Comparative example 1
" mixing solutions being 1:1 by Thermal release adhesive tape/graphene film hydrochloric acid and hydrogen peroxide mass ratio etches 10min " step in embodiment 1 removed, other steps, condition are with embodiment 1.
The performance test of the graphene film that embodiment 1 and comparative example 1 obtain is as follows:
Record sheet resistance 1437 Ω/sq, the transmittance after single-layer graphene transfer is 95.7%; And be 872 Ω/sq by recording sheet resistance after corrosive fluid process, transmittance is 97.6%, quite close to the transmittance of single-layer graphene, substantially increases the performance of graphene film.
Transmittance is recorded (using not turning the PET of graphene film as reference) by Shanghai Shun's space 721 type spectrophotometer; Sheet resistance records with MCP-T370 four-point probe.
Claims (7)
1. big area can't harm a method for transfer graphene film, it is characterized in that: step is as follows:
(1) have the metal base two sides of graphene film all to aim at transfer medium growth to fit, 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) obtained is as negative pole, using platinum electrode as positive pole, inserting is equipped with in the tank of electrolytic solution, pass to volts DS, after medium/graphene film to be transferred is peeled off from metal base completely, transfer medium/graphene film is put into corrosive fluid and etch graphene film surface residual metal, then dry up with distilled water rinsing three times;
(3) transfer medium/graphene film step (2) obtained and target substrate are fitted, and carry out roll-in on hot calender, and namely Graphene is transferred in target substrate,
Wherein, the transfer medium described in step (1) is Pressuresensitive Tape; Target substrate described in step (3) is PET, glass or silicon chip.
2. big area according to claim 1 can't harm the method for transfer graphene film, it is characterized in that: the metal base described in step (1) is copper or nickel.
3. big area according to claim 1 can't harm the method for transfer graphene film, it is characterized in that: the roll squeezer roller bearing spacing described in step (1) is 0.5 ~ 2mm, and roll-in speed is 50 ~ 300rpm.
4. big area according to claim 1 can't harm the method for transfer graphene film, it is characterized in that: in the tank 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.
5. big area according to claim 1 can't harm the method for transfer graphene film, and it is characterized in that: the volts DS described in step (2) is 8 ~ 30V, electrolysis time is 1 ~ 20h.
6. big area according to claim 1 can't harm the method for transfer graphene film, it is characterized in that: mixing solutions or the massfraction of to be hydrochloric acid and hydrogen peroxide mass ratio the be 1:1 of the corrosive fluid described in step (2) are the dust technology of 5%, and described transfer medium/graphene film residence time in corrosive fluid is 10 ~ 60min.
7. big area according to claim 1 can't harm the method for transfer graphene film, it is characterized in that: the hot calender roller bearing spacing described in step (3) is 0.5 ~ 5mm, roll-in speed is 50 ~ 300rpm, and wherein hot calender roller bearing temperature is 120 ~ 150 DEG C.
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| CN104495824B (en) * | 2014-12-16 | 2016-08-24 | 中国科学院重庆绿色智能技术研究院 | A kind of method and apparatus of monolayer continuous graphite alkene film production |
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| CN104860307B (en) * | 2015-05-12 | 2017-06-09 | 青岛华高能源科技有限公司 | A kind of lossless transfer method of graphene film |
| CN105609217B (en) * | 2016-02-22 | 2017-06-23 | 京东方科技集团股份有限公司 | A kind of graphene transparent electrode, its preparation method and display device |
| CN106222660B (en) * | 2016-06-23 | 2018-11-02 | 无锡格菲电子薄膜科技有限公司 | A kind of CVD method prepares the low-temperature substrate etching liquid and its Cryo-etching method of graphene |
| CN106315561B (en) * | 2016-08-19 | 2018-10-12 | 北京旭碳新材料科技有限公司 | A kind of complex of the large area of graphene film lossless transfer method and graphene-target substrate |
| CN106629692A (en) * | 2016-10-18 | 2017-05-10 | 东南大学 | Synchronous transfer method for upper and lower graphene films growing on copper foil surfaces in coated manner |
| CN107039245B (en) * | 2017-04-20 | 2020-01-21 | 中国科学院微电子研究所 | Method for improving thermal conductivity of gallium oxide material |
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