CN203451227U - Transfer device for graphene - Google Patents
Transfer device for graphene Download PDFInfo
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- CN203451227U CN203451227U CN201320412547.3U CN201320412547U CN203451227U CN 203451227 U CN203451227 U CN 203451227U CN 201320412547 U CN201320412547 U CN 201320412547U CN 203451227 U CN203451227 U CN 203451227U
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Abstract
The utility model provides a transfer device for graphene, and particularly relates to a device which transfers graphene to a substrate. The transfer device for graphene provided by the utility model is simple and feasible, and can simply transfer a graphene thin film in a large area to any substrate with less damage.
Description
Technical field
The utility model relates to a kind of transfer device of Graphene, especially a kind of Graphene is transferred to the device on substrate, belongs to conductive film field.
Background technology
Graphene is the cellular two dimensional crystal of six sides by monolayer carbon atomic building.Because Graphene has excellent electricity, mechanics, calorifics and optical characteristics, so it has a wide range of applications at Material Field, such as for the manufacture of transparency electrode and thinner, switching speed electronic component etc. faster.
At present, the preparation method of Graphene mainly comprises: mechanically peel method, chemical stripping method, epitaxial method, solvent stripping method, chemical Vapor deposition process (CVD).Wherein, chemical Vapor deposition process is one of method of preparing big size graphene film.But the graphene film of preparing by chemical Vapor deposition process is attached in metal foil substrate conventionally, thereby need to carry out follow-up transfer step, transfer them on other substrate.Described transfer step is generally: at Graphene surface spin coating one deck organism, polymethylmethacrylate (PMMA) for example, then in corrosive fluid, tinsel is eroded, thereby make the film floating being formed by organic thin film and graphene film on corrosive fluid surface.Then this layer film is repeatedly cleaned in deionized water, subsequently the graphene film being supported by organic thin film is transferred on other substrate, then removes organic thin film with solvent, thereby obtain the graphene film on other substrate.
Yet, when shifting large-area graphene film by above chemical Vapor deposition process, for example, due to organic thin film thinner thickness (hundreds of nanometer), and it does not support in transfer process, therefore not easy to operate, and easily cause graphene film damaged, thus generally when shifting larger area Graphene, there is limitation, easily damaged in transfer process.On the other hand, this layer of organic film can not be too thick, otherwise cannot on substrate, shakeout on transferring to substrate time, and while making to dissolve this layer of organism, Graphene can be damaged.In addition, corroding Copper Foil and from corrosive fluid, fishing in the process of organic film and graphene film, corrosive fluid is easy to flow to or drip to the film upper surface of organic thin film and graphene film formation, even after removing organic film, still can on graphene film, form the yellow spot that cannot remove, have a strong impact on light transmission and the outward appearance of graphene film.And this traditional method that allows organic film and graphene film swim on corrosive fluid needs the corrosion pond that floor space is very large.So according to above various reasons, this traditional graphene film rotor mode is difficult to be used to carry out heavy industrialization graphene film rotor technique.
Summary of the invention
An aspect of the present utility model provides a kind of transfer device of Graphene, and it comprises the transfer wall that at least one is ventilative, forms cavity together with other wall of described transfer wall and transfer device, and described cavity has the control device of at least one cavity internal gas pressure.
Transfer device of the present utility model and cavity thereof can be for being applicable to any shape of operation, such as square, rectangular parallelepiped, right cylinder etc.
According to an embodiment of the present utility model, transfer device of the present utility model can have one or more transfer walls, if suitable, it preferably has 1,2,3,4 or 5 transfer wall.The outside surface of described transfer wall can be flat or uneven.
According to an embodiment of the present utility model, in transfer device of the present utility model, described at least one ventilative transfer wall comprises the ventilative part consisting of at least one air-permeable layer.The number of plies for air-permeable layer in this ventilative part is not particularly limited, and for example, it can be one or more layers, is preferably 1,2,3,4,5,6,7,8,9,10 layer or more multi-layered, more preferably 1,2,3,4 or 5 layer.Ventilation part divides the size of the graphene film that outer surface area can shift with needs to adapt, and for example it can equal, be less than or greater than the area of graphene film, is preferably equal to or less than the area of graphene film.In addition, preferably, described ventilation part divides outside surface large as much as possible.Particularly preferably, the outside surface of described ventilative part is flat or substantially flat.If needed, described transfer wall can be whole all ventilative.
Described air-permeable layer can be the air-permeable envelope consisting of gas permeable material, comprises the air-permeable envelope consisting of organic materials, inorganic materials or matrix material (such as polymkeric substance, leather, fabric, paper and/or pottery etc.).Described gas permeable material is preferably inert material.On described air-permeable envelope, can also there are one or more breather holes.
Described air-permeable layer can be also the porous-film consisting of non-gas permeable material, comprises that (porous-film forming such as metal, polymkeric substance (as plastics) and/or oxide compound etc., described material is preferably inert material by organic materials, inorganic materials or matrix material.Preferably, part or all of transfer device of the present utility model made by inert material.
Preferably, the thickness of air-permeable layer can regulate according to the jump condition of Graphene.When air-permeable layer is multilayer, the thickness between different air-permeable layer can be identical or different.Wherein, use elliptical polarization spectroscopy to measure, described thickness is preferably 50 μ m to 5mm independently of one another, more preferably 100 μ m, 125 μ m, 0.3mm, 0.36mm, 0.5mm, 0.9mm, 1mm, 2mm, 3mm or 4mm.
Preferably, the aperture of described porous-film can regulate according to the jump condition of Graphene.The aperture of same porous-film, and can be identical or different between the aperture of different porous-films when porous-film is multilayer, and be preferably independently of one another 20nm to 5mm, more preferably 50nm, 100nm, 150nm, 200nm, 220nm, 25 μ m, 50 μ m, 100 μ m, 0.1mm, 0.5mm, 0.6mm, 1mm, 2mm, 3mm or 4mm.Particularly preferably, the 0.1-10 that above-mentioned aperture is thickness times, for example 0.5,1,2,3,4 or 5 times.In one embodiment, the aperture of porous-film is 0.1-10 times of adjacent layers thickness, for example 0.5,1,2,3,4 or 5 times.
According to an embodiment of the present utility model, except shifting the ventilation part of wall divides, the other parts (that is, not only comprise other wall except shifting wall, also comprise the non-ventilative part that shifts wall) that form the wall of cavity in the utility model transfer device consist of non-ventilative material.Described non-ventilative material is also known in the art, such as organic materials, inorganic materials or matrix material etc., and the example is metal or polymkeric substance (for example plastics).Described non-ventilative material is preferably inert material.Preferably, between the adjacent wall of formation cavity, combine closely.More preferably, except shifting ventilation part on wall exceptionally, other any part of described cavity is non-ventilative.
In the utility model transfer device, cavity has the control device of at least one cavity internal gas pressure, thereby when needed the pressure in cavity is adjusted to negative pressure, malleation or environmental stress.
In one embodiment, the pipeline that this Pneumatic controller is hollow, inside cavity is stretched in its one end.The other end of described pipeline can be connected with air pump, thereby makes when needed inside cavity reach the pressure needing.
The installation site of the control device of described cavity internal gas pressure is not particularly limited, and it can be placed on any wall of cavity, for example, be placed in the non-ventilative part (if existence) or non-transfer wall that shifts wall.
Described Pneumatic controller can exist one or more, for example 1,2,3 or 4.When exist more than 2 control device time, they can work or alternation simultaneously.Or, they can be worked according to for example following mode: one of them (or a plurality of) control device is adjusted to cavity pressure negative pressure or environmental stress when needed, and another (or a plurality of) control device is adjusted to cavity pressure malleation or environmental stress when needed.For example, one of them control device is air extractor (as pipeline), and another control device is diffuser (as pipeline).Preferably, the inside cavity of the control device of cavity internal gas pressure is divided and can also be had one or more air outlets or shower nozzle.
Described transfer device can comprise that at least one is to the device that passes into fluid in cavity.Wherein, described fluid can, for the organic or inorganic solvent of water or other inertia, be preferably deionized water.This device can be can be to the device (as pipeline) that passes into water in cavity, i.e. water feed apparatus (pipeline).Preferably, when passing into fluid in cavity, the inside cavity of this device is divided can also have one or more water outlets or shower nozzle.
Preferably, when being mounted with the control device of at least one cavity internal gas pressure and at least one simultaneously passing into fluid means on described cavity wall, the control device of at least one cavity internal gas pressure and at least one can be passed into fluid means and merge.That is, use same device to realize two kinds of functions, for example, use (as the pipeline) air inlet of same device and/or influent stream body.
Preferably, on the transfer wall of Graphene transfer device of the present utility model, be also provided with tightness system.Described tightness system can prevent in transfer process that corrosive fluid from entering cavity.For tightness system, having no particular limits, can be flange, sealing-ring, seal gum and/or seal strip etc. such as it.Described tightness system can be combined with, for example, can use flange and sealing-ring simultaneously.Wherein, tightness system is preferably by inert material, and for example metal or polymkeric substance (as plastics, rubber) are made.And the shape of tightness system can be carried out any adjustment according to the shape at required sealing position, wherein flange is preferably annular.Particularly preferably, described tightness system can also have the fixedly effect of graphene film.
" inert material " herein refer to and Graphene be transferred in the process on other substrate, and this material is for contacted conditioned disjunction environment (for example, with Graphene and corrosive fluid) anergy or essentially no reactivity.Preferably, part or all of transfer device of the present utility model made by inert material, and for example the cladding material of transfer device and corrosive fluid contact part is inert material.In one embodiment, transfer device of the present utility model is all made by inert material.
" the organic or inorganic solvent of inertia " herein refers to the material anergy in cavity wall and cavity or essentially no reactive organic or inorganic solvent.
Also provide a kind of and used Graphene transfer device of the present utility model that Graphene is transferred to the method on substrate, comprised the following steps:
1) use chemical Vapor deposition process at the first substrate surface growing graphene film;
2) the graphene film surface-coated organism on the first substrate of gained is to form the graphene film of surface-coated organic thin film;
3) by step 2) in the graphene film of surface-coated organic thin film on the first substrate of obtaining be positioned on the transfer wall outside surface of Graphene transfer device of the present utility model, make graphene film one side that the first substrate top surface applies organic thin film to shifting wall;
4) by being positioned over the first substrate and the graphene film that shift on wall, immerse corrosive fluid so that the first substrate etching;
5) graphene film of surface-coated organic thin film is transferred on the second substrate.
Wherein, in step 3) or after step 3) and before step 4), make to form in cavity negative pressure.
Preferably, described the first and second substrates can be identical or different, and be selected from independently of one another metal (for example nickel, copper), nonmetal (for example glass, synthetic glass, silicon carbide, silicon, silicon-dioxide, polymkeric substance are as plastics) and/or semiconducter substrate.
Preferably, the graphene film in step 1) is continuous film.
Preferably, step 2) organism in can be for following polymkeric substance a kind of, two kinds or more of mixtures: polyethylene terephthalate (PET), polydimethylsiloxane (PDMS), polypropylene (PP), epoxy resin quasi-polyethylene (PE), polystyrene (PS), ABS plastic, polyvinyl chloride (PVC), polyoxymethylene (POM), polycarbonate (PC), phenoplast, urethane plastic, epoxy resin, unsaturated polyester plastic, furans plastics, silicone resin, the polymkeric substance such as allyl resin (such as polymethylmethacrylate (PMMA)) etc. and modified resin thereof.
Preferably, the coating step 2) can be used by methods such as spraying, roller coat, spin coating, blade coatings.
Preferably, in step 2) (for example, in step 2) afterwards and before step 3) afterwards) remove the Graphene that does not apply the another side of organic thin film on the first substrate.Wherein, the Graphene of removing the first substrate another side can adopt the method for etching or mechanical friction.Etching can be any lithographic method as known in the art, for example, can use oxygen plasma etch.
Preferably, in step 3), by step 2) in the first substrate top surface of obtaining graphene film of applying organic thin film be positioned on the transfer wall outside surface of Graphene transfer device of the present utility model, then by form negative pressure in cavity, the first substrate is fixed together with graphene film, if or needed, use tightness system sealing, then by sealing device with form negative pressure in cavity graphene film is fixed.
Corrosive fluid in step 4) has corrosive nature to the first substrate, is preferably ferric chloride in aqueous solution, iron nitrate aqueous solution, hydrofluoric acid aqueous solution, aqueous nitric acid, aqueous sulfuric acid, copper sulfate solution or hydrochloric acid.Above-mentioned corrosive fluid can independent or several mixing uses.
Preferably, in step 5), thereby by malleation and/or by the surface that fluid is sprayed onto organic thin film, the graphene film of surface-coated organic thin film is released on substrate.
Optionally, after step 5), with solvent, the organic thin film of coating is removed.The preferred organic solvent of described solvent, for example acetone, methyl alcohol, ethanol and/or Virahol.
Except as otherwise noted, technical scheme mentioned herein, embodiment, example, and between preferred, preferred, particularly preferred technical characterictic or numerical range, can carry out combination arbitrarily or combination, the technical scheme of gained is encompassed in scope of the present utility model equally like this.
Graphene transfer device of the present utility model is simple, can simply big area graphene film be transferred on any substrate and damage less.Relatively traditional floating corrosion transferring device; Graphene transfer device of the present utility model has the protection of the wall of transfer; can effectively avoid corrosive fluid to stain organic film upper surface, so the film of absorption can be immersed in corrosion pond and corrodes, make full use of the space in corrosion pond.The utility model can be applicable to the graphene film rotor technique of large-scale industrialization, has commercial application prospect widely.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of an embodiment of Graphene transfer device of the present utility model, and in figure, each numerical markings represents with lower component:
101: metal or plastics flange;
102,103: rubber seal;
104: metal or plastic wall;
105: bleeding point, it extend into inside cavity and has a plurality of shower nozzles;
106: air inlet or water-in;
107,108,109 and 110: metal or plastics porous membrane, they have formed transfer wall, and have formed cavity together with 104;
111: organic thin film;
112: graphene film;
113: metallic membrane.
Fig. 2 is in an embodiment of the present utility model, the schematic diagram of corroding metal film in corrosive fluid.
Fig. 3 is in an embodiment of the present utility model, after corroding metal film, graphene film is transferred to the schematic diagram on substrate.
Figure 4 and 5 are to be transferred to the graphene film in glass substrate according to the utility model embodiment 1.
Embodiment
Below in conjunction with accompanying drawing, principle of the present utility model and feature are described, following example is only for the technical solution of the utility model is explained and illustrated, and is not intended to scope of the present utility model to limit.
Fig. 1 is the schematic diagram of an embodiment of Graphene transfer device of the present utility model, and wherein, this device comprises the wall 104 that metal or plastics are manufactured, and the material used corrosion that is not corroded.107,108,109 and 110 be metal or plastics porous membrane, wherein 110 aperture is 0.1 to 10 times of organic thin film 111 thickness, 109 aperture is 0.1 to 10 times of 110 thickness, and 108 aperture is 0.1 to 10 times of 109 thickness, and 107 aperture is 0.1 to 10 times of 108 thickness.The 105th, be used to form the bleeding point of negative pressure in chamber, the 106th, air inlet or water-in, water is sprayed onto porous film surface by a plurality of shower nozzles, is then penetrated into organic thin film surface, thereby separated with porous-film with the organic thin film of Graphene.101 is endless metal or plastics flange, and 102 and 103 is rubber seal.By the metal membrane-coating corrosive fluids of 101,102 and 103 protections, do not corroded, and the edge of metallic membrane is due to 101,102 and 103 protection and the corrosion that can not be corroded.
Fig. 2 is in an embodiment of the present utility model, at corrosive fluid, is the schematic diagram of corroding metal film in ferric chloride in aqueous solution.Wherein, by 105 bleeding points, bleed and make to form in cavity negative pressure, thereby 111,112 and 113 trilamellar membranes are adsorbed on multilayer porous film, then the transfer device that sample is housed is immersed in corrosive fluid completely.
Fig. 3 is in an embodiment of the present utility model, after corroding metal film, graphene film is transferred to the schematic diagram on substrate.Wherein, after metal level 113 corrodes, transfer device is placed as Fig. 3.Unclamp 101 flanges, take 102 and 103 sealing-rings away, then pass into gas or water spray from 106, make 111 separated from transfer device with 112 layers.
111 and 112 layers be transferred on substrate after, in air, dry, then with solvent, 111 layers of organism are dissolved, just can obtain being transferred to the Graphene on substrate.
Embodiment 1
By normal atmosphere vapor deposition method, at the thick copper foil surface of 25 μ m, generate continuous graphene film.Then at the thick PMMA film of its surface spraying one deck 200nm.Follow the 2 minutes Graphenes with the removal back side of oxygen plasma etch with 300 watts.Film through oxygen plasma etch is fixed on transfer device.
Transfer device is comprised of following part: 101 and 104 is No. 304 stainless steels.107 is 304 stainless steel porous plates, and aperture is 4mm, and thickness is 0.9mm.108 is 304 stainless steel porous plates, and aperture is 0.6mm, and thickness is 0.5mm.109 is the porous membrane of Teflon, and aperture is 25 μ m, and thickness is 0.36mm.110 is the porous membrane of Teflon, and aperture is 220nm, and thickness is 125 μ m.Then vacuumize, making the pressure in cavity is 10KPa.Then transfer device as being immersed in the ferric chloride Solution of 1mol/L, Fig. 2 is corroded 4 hours.After Copper Foil has been corroded, with deionized water scouring stone China ink alkene surface, then transfer device is tipped upside down on to glass substrate surface as Fig. 3.Remove after flange and sealing-ring from 106 mouthfuls and spray into deionized water, Graphene and PMMA film are just transferred to glass substrate surface.Then in air, dry sample, then sheet glass is dried at 110 ℃ 3 minutes on warm table.Then in acetone, remove PMMA, then in Virahol and deionized water, clean sample.After drying, just obtain being transferred to the big area graphene film (as Fig. 4) in glass substrate.The transmittance that records graphene film is 95.1% under 550nm wavelength, and square resistance is 450 ohm/.
Embodiment 2
By low pressure gas phase deposition method, at the thick copper foil surface of 25 μ m, generate continuous graphene film.Then at the thick PMMA film of its surface spraying one deck 200nm.Follow the 1 minute Graphene with the removal back side of oxygen plasma etch with 300 watts.Film through oxygen plasma etch is fixed on transfer device.
Transfer device is comprised of following part: 101 and 104 is No. 304 stainless steels.107 is 304 stainless steel porous plates, and aperture is 2mm, and thickness is 0.8mm.108 is 304 stainless steel porous plates, and aperture is 0.2mm, and thickness is 0.3mm.109 is the porous membrane of Teflon, and aperture is 50 μ m, and thickness is 0.4mm.110 is the porous membrane of Teflon, and aperture is 100nm, and thickness is 100 μ m.Then vacuumize, making the pressure in cavity is 10KPa.Then transfer device as being immersed in the iron nitrate solution of 1mol/L, Fig. 2 is corroded 4 hours.After Copper Foil has been corroded, with deionized water scouring stone China ink alkene surface, then transfer device is tipped upside down on to glass substrate surface as Fig. 3.Remove after flange and sealing-ring from 106 and pass into nitrogen, make cavity pressure than the high 10KPa of normal atmosphere, Graphene and PMMA film are just transferred to glass substrate surface.Then in air, dry sample, then sheet glass is dried at 110 ℃ 3 minutes on warm table.Then in acetone, remove PMMA, then in Virahol and deionized water, clean sample.After drying, just obtain being transferred to the big area graphene film in glass substrate.The transmittance that records graphene film is 97.1% under 550nm wavelength, and square resistance is 850 ohm/.
Claims (29)
1. a transfer device for Graphene, it comprises the transfer wall that at least one is ventilative, forms cavity together with other wall of described transfer wall and transfer device, described cavity has the control device of at least one cavity internal gas pressure.
2. transfer device as claimed in claim 1, part or all of wherein said transfer device made by inert material.
3. transfer device as claimed in claim 1 or 2, wherein said at least one ventilative transfer wall comprises the ventilative part consisting of at least one air-permeable layer.
4. transfer device as claimed in claim 3, wherein said air-permeable layer is the air-permeable envelope consisting of gas permeable material or the porous-film consisting of non-gas permeable material.
5. transfer device as claimed in claim 4, the wherein said air-permeable envelope consisting of gas permeable material is porous-film.
6. the transfer device as described in claim 4 or 5, wherein said air-permeable layer can be one or more layers, when it is multilayer, the thickness between different air-permeable layer can be identical or different; The aperture of same porous-film, and can be identical or different between the aperture of different porous-films when porous-film is multilayer.
7. transfer device as claimed in claim 6, the thickness of wherein said air-permeable layer is 50 μ m to 5mm independently of one another.
8. transfer device as claimed in claim 6, the aperture of same porous-film wherein, and the aperture of different porous-films is 20nm to 5mm independently of one another when porous-film is multilayer.
9. the transfer device as described in any one in claim 1,2,4,5,7 and 8, wherein said transfer device comprises that at least one is to the device that passes into fluid in cavity.
10. transfer device as claimed in claim 3, wherein said transfer device comprises that at least one is to the device that passes into fluid in cavity.
11. transfer devices as claimed in claim 6, wherein said transfer device comprises that at least one is to the device that passes into fluid in cavity.
12. transfer devices as claimed in claim 9, wherein said fluid is the organic or inorganic solvent of water or other inertia.
13. transfer devices as described in any one in claim 10 or 11, wherein said fluid is the organic or inorganic solvent of water or other inertia.
14. transfer devices as claimed in claim 12, wherein said fluid is deionized water.
15. transfer devices as claimed in claim 13, wherein said fluid is deionized water.
16. transfer devices as described in any one in claim 1,2,4,5,7,8,10-12 and 14-15, are also provided with tightness system on the transfer wall of wherein said transfer device.
17. transfer devices as claimed in claim 3, are also provided with tightness system on the transfer wall of wherein said transfer device.
18. transfer devices as claimed in claim 6, are also provided with tightness system on the transfer wall of wherein said transfer device.
19. transfer devices as claimed in claim 9, are also provided with tightness system on the transfer wall of wherein said transfer device.
20. transfer devices as claimed in claim 13, are also provided with tightness system on the transfer wall of wherein said transfer device.
21. transfer devices as claimed in claim 16, wherein said tightness system is flange, sealing-ring, seal gum and/or seal strip.
22. transfer devices as described in any one in claim 17-20, wherein said tightness system is flange, sealing-ring, seal gum and/or seal strip.
23. transfer devices as claimed in claim 16, wherein said tightness system is made by inert material.
24. transfer devices as described in any one in claim 17-21, wherein said tightness system is made by inert material.
25. transfer devices as claimed in claim 22, wherein said tightness system is made by inert material.
26. transfer devices as described in claim 23 or 25, wherein said inert material is metal or polymkeric substance.
27. transfer devices as claimed in claim 24, wherein said inert material is metal or polymkeric substance.
28. transfer devices as claimed in claim 26, wherein said polymkeric substance is plastics, rubber.
29. transfer devices as claimed in claim 27, wherein said polymkeric substance is plastics, rubber.
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| CN201320412547.3U CN203451227U (en) | 2013-07-11 | 2013-07-11 | Transfer device for graphene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332685A (en) * | 2013-07-11 | 2013-10-02 | 常州二维碳素科技有限公司 | Transfer device and transfer method of graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332685A (en) * | 2013-07-11 | 2013-10-02 | 常州二维碳素科技有限公司 | Transfer device and transfer method of graphene |
| CN103332685B (en) * | 2013-07-11 | 2015-04-22 | 常州二维碳素科技有限公司 | Transfer device and transfer method of graphene |
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Address after: 213149 No. 6 Xiangyun Road, Wujin Economic Development Zone, Jiangsu, Changzhou Patentee after: 2D CARBON (CHANGZHOU) TECH Inc.,Ltd. Address before: 213149 No. 6 Xiangyun Road, Wujin Economic Development Zone, Jiangsu, Changzhou Patentee before: 2D CARBON (CHANGZHOU) TECH Co.,Ltd. |
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