CN104860307A - Nondestructive transferring method of graphene film - Google Patents
Nondestructive transferring method of graphene film Download PDFInfo
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- CN104860307A CN104860307A CN201510237214.5A CN201510237214A CN104860307A CN 104860307 A CN104860307 A CN 104860307A CN 201510237214 A CN201510237214 A CN 201510237214A CN 104860307 A CN104860307 A CN 104860307A
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- graphene film
- adhesive tape
- target substrate
- graphene
- nondestructive
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000758 substrate Substances 0.000 claims abstract description 53
- 239000002390 adhesive tape Substances 0.000 claims abstract description 50
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000011888 foil Substances 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 4
- 238000012546 transfer Methods 0.000 claims description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 239000011889 copper foil Substances 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 54
- 239000000243 solution Substances 0.000 description 7
- 239000003292 glue Substances 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000013404 process transfer Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- -1 and in figure Chemical compound 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the technical field of materials science, and relates to an environment-friendly, efficient and convenient nondestructive transferring method of a graphene film. The nondestructive transferring method comprises the following steps: a metal foil on which the graphene film grows is put on a glass slide flatwise, and an adhesive tape is affixed to the graphene film; the metal foil of which the surface is attached with the adhesive tape is put into a corrosion solution, is corroded for 2-10 hours, and is removed to obtain an adhesive tape/graphene film structure; the adhesive tape/graphene film structure is picked up, is affixed to a target substrate after hydrophilic treatment by using a 10-50W plasma cleaning machine, and is naturally placed at room temperature for 3-6 hours to obtain an adhesive tape/graphene film/target substrate structure; finally, the adhesive tape on the surface of the adhesive tape/graphene film/target substrate structure is slowly torn in the parallel direction to realize the nondestructive transferring. The nondestructive transferring method is novel in design, scientific in principle, simple in process, easy to operate, and relatively good in transferring effect.
Description
Technical field:
The invention belongs to materials science field, relate to a kind of environmental protection, efficiently, easily graphene film can't harm transfer method, the Graphene utilizing chemical Vapor deposition process to prepare can be carried out high-quality transfer.
Background technology:
Graphene (Graphene) is a kind of Two-dimensional Carbon material, is the general designation of single-layer graphene, bilayer graphene and few layer graphene.Graphene is considered to hypothetical structure always, cannot stable existence separately, until 2004, Univ Manchester UK physicist An Deliehaimu and Constantine Nuo Woxiaoluofu, successfully from graphite, isolate Graphene in an experiment---by the former molecular honeycomb two-dirnentional structure of monolayer carbon, and confirm that it can Individual existence.Graphene is thin, the hardest nano material in known at present world, and it is almost completely transparent, and thermal conductivity is up to 5300W/mK, and under normal temperature, its electronic mobility is more than 15000cm2/Vs, and resistivity only has an appointment 10
-8Ω m, because its resistivity is extremely low, electron transfer rate is exceedingly fast, and is therefore expected to can be used to develop thinner, conduction speed electronic component of new generation or transistor faster, and is applicable to for manufacturing transparent touch screen, liquid-crystal display, tabula rasa and solar cell etc.
In practice, because chemical Vapor deposition process can prepare few layer graphene film of big area, continuous print, transparent, high conductivity, thus the comparatively effective preparation method of Graphene is become, but the Graphene prepared by the method is attached to metal foil surface usually, therefore how graphene film be can't harm, efficient, easy, transfer on suitable substrate and become a problem demanding prompt solution to environmental protection, also become the key that can realize graphene film industrialization.Transfer method conventional at present needs whirl coating and colloidal sol process usually, but these methods have colloid residual many, and process is complicated, in a large number with an organic solvent, needs heating, the shortcomings such as technique is unstable, the method of such as a kind of Graphene disclosed in Chinese patent 201210587780.5 or graphene oxide transfer, it processes rear recycling extrusion machine to target substrate and the Graphene on flexible substrate or graphene oxide film and target substrate is pressed together, film is fully contacted with target substrate, then flexible substrate is slowly taken off, transfer to target substrate by film by flexible substrate, a kind of transfer method of graphene film disclosed in Chinese patent 201310143181.9, it prepares the defective Graphene of band on metal film surfaces, then the metal thin film structure with Graphene is put in acidic solution, the Graphene realizing the upper and lower surface of metallic film is separated with metallic film simultaneously, again Graphene is picked up from solution and be placed in deionized water, directly dry and be transferred on various substrate after cleaning, a kind of transfer method of graphene film disclosed in Chinese patent 201410111360.9, first will the metal substrate of graphene film be had to fit together from the process transfer substrate of glue is smooth with hot soarfing by chemical vapor deposition, etch away described metal substrate, obtain process transfer substrate/hot soarfing from glue/graphene film work in-process, high temperature high pressure process is carried out after being fitted in this work in-process graphene film face and target substrate again, make the two laminating evenly and make described hot soarfing lose viscosity from glue, tear described process transfer substrate off, obtain target substrate/graphene film product, the equal program of aforesaid method is loaded down with trivial details, conditional request is high, and be difficult to operation and realize, therefore the present invention works out a kind of graphene film simple, easy and simple to handle and can't harm transfer method, the transfer realizing graphene film that can be light, easy, harmless, has good using value.
Summary of the invention:
Goal of the invention of the present invention is the shortcoming overcoming prior art existence, seek to design a kind of graphene film and can't harm transfer method, by attaching adhesive tape at graphenic surface, then corrosion dissolution falls tinsel matrix, realizes transferring to loss-free for graphene film in target substrate.
To achieve these goals, the graphene film that the present invention relates to can't harm transfer method and specifically comprises following processing step:
(1) have the tinsel of graphene film to lie on slide glass growth, adhesive tape being close to growth has in the metal foil surface of graphene film;
(2) tinsel above-mentioned surface being posted adhesive tape is put into corrosive fluid and is corroded 2-10h, obtains adhesive tape/graphene film structure after removing tinsel;
(3) adhesive tape/graphene film structure is put into the culture dish rinsing 10-30min that deionized water is housed after picking up gently, repeat this rinse cycle 3-5 time; With the plasma washing machine of 10-50W, target substrate surface is carried out to the hydrophilic treatment of 3-5min, then gently adhesive tape/graphene film structure is picked up, naturally place 3-6h under normal temperature after being attached at the processed surface of target substrate, obtain adhesive tape/graphene film/target substrate structure;
(4) adhesive tape of adhesive tape/graphene film/target substrate body structure surface is torn with parallel direction slowly, obtain the graphene film transferred in target substrate, realize the harmless transfer of graphene film.
Further, described tinsel can select Copper Foil or nickel foil; Described corrosive fluid selects iron nitrate solution or salpeter solution; Described target substrate selects PET, Si or SiO
2deng flexibility or rigidity substrate; Described adhesive tape is the high adhesive tape of commercially available think of or glue power is suitable with it other conventional adhesive tapes.
The present invention compared with prior art, by attaching adhesive tape at graphenic surface, corrosion dissolution tinsel matrix, the method for tearing adhesive tape realize harmless for graphene film to transfer in target substrate, whole process does not relate to spin coating and heat treated, easy, efficient, environmental protection, for the application of Graphene in transparent electrical conducting electrode is had laid a good foundation; The method is novel in design, scientific in principle, and process is simple, and operate simple and easy, transfer effect is better.
Accompanying drawing illustrates:
Fig. 1 is the technical process schematic block diagram that the graphene film that the present invention relates to can't harm transfer method.
Fig. 2 is each stage product structural representation in graphene film transfer process in the embodiment 1 that the present invention relates to, and 1 be graphene film, 2 is wherein Copper Foil, 3 is adhesive tape, 4 is iron nitrate corrosive fluid, 5 is deionized water, 6 is target substrate.
Fig. 3 is that in the embodiment 1 that the present invention relates to, graphene film is transferred to the transmittance curve figure in target substrate from Copper Foil, and in figure, Graphene absorbancy is about 2.3%, illustrates in the present embodiment that the Graphene transferred in target substrate is individual layer.
Fig. 4 is that in the embodiment 1 that the present invention relates to, graphene film is transferred to the Raman spectrogram in target substrate from Copper Foil, illustrates that the present embodiment Han Graphene always transferred in target substrate is high-quality single-layer graphene (ID/IG >=2 and ID/IG≤0.1).
Fig. 5 is the atomic force microscope figure being transferred to the graphene film at the bottom of target in the embodiment 1 that the present invention relates to, as shown in the figure: the graphenic surface after transfer is smooth, roughness is only 0.257nm//and surface is glue-free residual, illustrates that transfer effect is good.
Fig. 6 is the scanning electron microscope (SEM) photograph being transferred to the graphene film in target substrate in the embodiment 1 that the present invention relates to, as shown in the figure: the Graphene after transfer is complete, defect is few (stain may be seen indistinctly in figure represents defect) and surface is glue-free residual, illustrates that transfer effect is good.
Embodiment:
The present invention is described in further detail by embodiment below in conjunction with accompanying drawing, but the present invention is not limited to following embodiment.
Embodiment 1:
The graphene film related in the present embodiment can't harm transfer method concrete steps:
(1) have the Copper Foil of graphene film to lie on slide glass the growth of 1cm × 1cm or 2cm × 2cm, adhesive tape being close to growth has on the copper foil surface of graphene film;
(2) Copper Foil above-mentioned surface being posted adhesive tape is put into iron nitrate (Fe (NO3) 3) corrosive fluid that concentration is 0.1-0.5g/ml and is corroded 2-10h, obtain adhesive tape/graphene film structure after removing Copper Foil matrix, the sticking power between adhesive tape and Graphene is enough to the supporter making adhesive tape as graphene film;
(3) adhesive tape/graphene film structure is put into the culture dish rinsing 10-30min that deionized water is housed after picking up gently, repeat this rinse cycle 3-5 time; With the plasma washing machine of 10-50W, target substrate surface is carried out to the hydrophilic treatment of 3-5min, then gently adhesive tape/graphene film structure is picked up, naturally place 3-6h under normal temperature after being attached at the processed surface of target substrate, obtain adhesive tape/graphene film/target substrate structure;
(4) adhesive tape of adhesive tape/graphene film/target substrate body structure surface is torn with parallel direction slowly, namely obtain the graphene film transferred in target substrate; Because the sticking power between adhesive tape and Graphene is less than the adsorptive power between Graphene and target substrate, can realize shifting without the graphene film of spin coating so tear adhesive tape off.
Adhesive tape in the present embodiment involved by step (1) is the high adhesive tape of commercially available think of or glue power is suitable with it other conventional adhesive tapes, and described Copper Foil can be replaced with nickel foil, and described iron nitrate solution available quality mark is that the salpeter solution of 5-20% is replaced; Target substrate involved by step (3) comprises PET, Si and SiO
2deng flexibility or rigidity substrate.
Realize in the present embodiment utilizing adhesive tape the principle be transferred in target substrate being by the graphene film in tinsel: tinsel is corroded after corrosion falls, only remaining adhesive tape adhesion graphene film, because corrosion and rinsing are all carry out in the solution making water molecules enter between adhesive tape and graphene film, thus weaken the sticking power of adhesive tape to Graphene, make it the sticking power (because target substrate is through hydrophilic treatment) be less than between Graphene and target substrate to be transferred, therefore, it is possible to be easily easy to graphene film to transfer in target substrate from adhesive tape.
The foregoing is only better embodiment of the present invention; protection scope of the present invention is not limited with above-mentioned embodiment; in every case the equivalence that those skilled in the art do according to content of the present invention changes, and all should include in the protection domain recorded in claims.
Claims (2)
1. graphene film can't harm a transfer method, it is characterized in that specifically comprising following processing step:
(1) have the tinsel of graphene film to lie on slide glass growth, adhesive tape being close to growth has in the metal foil surface of graphene film;
(2) tinsel above-mentioned surface being posted adhesive tape is put into corrosive fluid and is corroded 2-10h, obtains adhesive tape/graphene film structure after removing tinsel;
(3) adhesive tape/graphene film structure is put into the culture dish rinsing 10-30min that deionized water is housed after picking up gently, repeat this rinse cycle 3-5 time; With the plasma washing machine of 10-50W, target substrate surface is carried out to the hydrophilic treatment of 3-5min, then gently adhesive tape/graphene film structure is picked up, naturally place 3-6h under normal temperature after being attached at the processed surface of target substrate, obtain adhesive tape/graphene film/target substrate structure;
(4) adhesive tape of adhesive tape/graphene film/target substrate body structure surface is torn with parallel direction slowly, obtain the graphene film transferred in target substrate, realize the harmless transfer of graphene film.
2. graphene film according to claim 1 can't harm transfer method, it is characterized in that described tinsel is Copper Foil or nickel foil; Described corrosive fluid is iron nitrate solution or salpeter solution; Described target substrate is PET, Si or SiO
2substrate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510237214.5A CN104860307B (en) | 2015-05-12 | 2015-05-12 | A kind of lossless transfer method of graphene film |
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| CN201510237214.5A CN104860307B (en) | 2015-05-12 | 2015-05-12 | A kind of lossless transfer method of graphene film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052382A (en) * | 2018-10-17 | 2018-12-21 | 北京镭硼科技有限责任公司 | A kind of method of wet process transfer graphene |
| CN109133046A (en) * | 2018-10-17 | 2019-01-04 | 东南大学 | A method of graphene is shifted using fullerene |
| CN109727706A (en) * | 2019-03-08 | 2019-05-07 | 华南协同创新研究院 | A kind of flexible transparent conductive film and preparation method thereof |
| WO2019100674A1 (en) * | 2017-11-24 | 2019-05-31 | 深圳大学 | Graphene material and sensor for detecting gas component |
| CN112263255A (en) * | 2020-09-28 | 2021-01-26 | 北京师范大学 | Graphene skin electrode based on conductive polymer transfer and preparation method thereof |
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| CN102592964A (en) * | 2011-01-07 | 2012-07-18 | 中国科学院微电子研究所 | Substrate transfer method of graphene film |
| CN103387230A (en) * | 2013-07-23 | 2013-11-13 | 中国科学院微电子研究所 | Preparation method of graphene conductive film |
| CN103922327A (en) * | 2014-04-17 | 2014-07-16 | 江南石墨烯研究院 | Method for nondestructively transferring graphene thin film in large area |
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2015
- 2015-05-12 CN CN201510237214.5A patent/CN104860307B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102592964A (en) * | 2011-01-07 | 2012-07-18 | 中国科学院微电子研究所 | Substrate transfer method of graphene film |
| CN103387230A (en) * | 2013-07-23 | 2013-11-13 | 中国科学院微电子研究所 | Preparation method of graphene conductive film |
| CN103922327A (en) * | 2014-04-17 | 2014-07-16 | 江南石墨烯研究院 | Method for nondestructively transferring graphene thin film in large area |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019100674A1 (en) * | 2017-11-24 | 2019-05-31 | 深圳大学 | Graphene material and sensor for detecting gas component |
| CN109052382A (en) * | 2018-10-17 | 2018-12-21 | 北京镭硼科技有限责任公司 | A kind of method of wet process transfer graphene |
| CN109133046A (en) * | 2018-10-17 | 2019-01-04 | 东南大学 | A method of graphene is shifted using fullerene |
| CN109133046B (en) * | 2018-10-17 | 2021-08-10 | 东南大学 | Method for transferring graphene by utilizing fullerene |
| CN109727706A (en) * | 2019-03-08 | 2019-05-07 | 华南协同创新研究院 | A kind of flexible transparent conductive film and preparation method thereof |
| CN112263255A (en) * | 2020-09-28 | 2021-01-26 | 北京师范大学 | Graphene skin electrode based on conductive polymer transfer and preparation method thereof |
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| CN104860307B (en) | 2017-06-09 |
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Address after: 266109 1st floor, C2 building, LANWAN Venture Park, No.1, Jinhui Road, high tech Zone, Qingdao, Shandong Province Patentee after: QINGDAO HUAGAO GRAPHENE TECHNOLOGY Corp.,Ltd. Address before: 266111 Shandong city of Qingdao province Songyuan Qingdao high tech Industrial Development Zone, No. 17 Qingdao Road, Industrial Technology Research Institute C C1 District 4 floor -1 Patentee before: QINGDAO HUAGAO ENERGY TECHNOLOGY Co.,Ltd. |
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Denomination of invention: A non-destructive transfer method for graphene thin films Granted publication date: 20170609 Pledgee: Huagao Holding Group Co.,Ltd. Pledgor: QINGDAO HUAGAO GRAPHENE TECHNOLOGY Corp.,Ltd. Registration number: Y2024980039404 |