CN105329884B - Method for rapidly peeling and transferring graphene oxide leaching film to substrate - Google Patents
Method for rapidly peeling and transferring graphene oxide leaching film to substrate Download PDFInfo
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- CN105329884B CN105329884B CN201510828612.4A CN201510828612A CN105329884B CN 105329884 B CN105329884 B CN 105329884B CN 201510828612 A CN201510828612 A CN 201510828612A CN 105329884 B CN105329884 B CN 105329884B
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- graphene oxide
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Abstract
The invention discloses a method for rapidly peeling and transferring a graphene oxide leaching film to a substrate. The method specifically comprises the steps of firstly adding graphene oxide in water, forming graphene oxide dispersion liquid in an ultrasonic dispersion way, arranging the substrate on a sand core of a leaching flask, installing a leaching device, then pouring the prepared graphene oxide dispersion liquid into the leaching device, and starting leaching; then taking out the substrate which is attached with a leached graphene oxide film, and putting the substrate into an organic solvent, enabling the graphene oxide film to be rapidly formed through dewatering, and enabling the graphene oxide film to fall off the substrate; enabling the smooth substrate to be in direct contact with the floated graphene oxide film in the organic solvent, and enabling the graphene oxide film to transfer to be attached onto the substrate. Through the method disclosed by the invention, the drying time is not needed at all, and the time for peeling a thick film is greatly shortened; meanwhile, a thin film can also be peeled, a smooth graphene oxide film can be obtained, and the shape can be well maintained.
Description
Technical field
The present invention relates to a kind of quick stripping graphene oxide suction filtration film and the method that is transferred to substrate.Belong to graphite oxide
The technical field that alkene suction filtration film is quickly peeled off and shifted.
Background technology
With the discovery of Graphene, its excellent electrical properties, mechanical property, thermal property and magnetic property cause people
Extensive concern.Used as the important derivatives of Graphene, graphene oxide is also more and more paid attention to.Graphene oxide
As a kind of new carbon of excellent performance, with cellular two-dimensional structure, due to special physics, chemical property,
Such as specific surface area higher, higher porosity, containing abundant oxygen-containing functional group, the features such as asepsis environment-protecting.Graphene oxide with
And its reduzate Graphene is in many fields, such as absorption (Yubing Sun, Shubin Yang, Yue Chen, Congcong
Ding, Wencai Cheng, Xiangke Wang, Environ.Sci.Technol.2015,49,4255-4262), sewage it is net
Change (Yi Han, Zhen Xu, and Chao Gao, Adv.Funct.Mater.2013,23,3693), ultracapacitor (Li,
Meng；Tang, Zhe, Leng, Mei, et al.Adv.Funct.Mater.2014,24,7495-7502), fuel cell catalyst
Agent (Jia, Lingpu, Sun, Xiao, Jiang, Yimin, et al.Adv.Funct.Mater.2015,25,1814-1820) etc.
Multiple fields receive extensive research.How to prepare smooth two dimensional oxidation graphene film is asking for the continuous exploration of present people
Topic.The method of preparation graphene oxide membrane also emerges in an endless stream and has LB methods (Laura J.Cote, Franklin Kim, and
Jiaxing Huang.J.AM.Chem.Soc.2009,131,1043-1049), spin-coating method (Kymakis, Emmanuel；
Savva, Kyriak, Stylianakis, Minas M, et al.Adv.Funct.Mater.2013,23,2742-2749), spray
Coating (Parviz, Dorsa, Metzler, ShaneD., Das, Sriya, et al.small2015,11, No.22,2661-
2668) etc..Vacuum filtration is easy to operate due to its, and obtained film enjoys people compared with other liquid membrane formation process uniform grounds the most
Pay close attention to.But the greatest problem that suction method faces is how to peel off graphene oxide membrane from substrate.If oxidation stone
Black alkene film is too thin, then complete film cannot be peeled off from substrate；And if film is sufficiently thick, is completely dried graphene oxide and is also required to
Plenty of time.Substrate is dissolved with corrosive liquids such as acetone in some experiments, and so obtained film pattern cannot keep smooth.
So the advantage in order to utilize suction filtration graphene oxide membrane completely, it is possible to which further reduction obtains smooth graphene film,
Allow for finding a kind of method of quick stripping graphene oxide membrane, further functionalization is realized so as to be transferred to various substrates
Operation.
The content of the invention
Technical problem：The present invention provides a kind of quick stripping graphene oxide suction filtration film and the method for being transferred to substrate, can
Peel off and shift to realize by the complete graphene oxide membrane rapid dehydration drying of firm suction filtration and from substrate.
Technical scheme：A kind of quick stripping graphene oxide suction filtration film of the present invention and the method for being transferred to substrate, including with
Lower step：
Add graphene oxide into first in water, ultrasonic disperse forms graphene oxide aqueous dispersions, then puts substrate
In on the core of bottle,suction, Suction filtration device is put up, the graphene oxide dispersion that will then prepare pours into Suction filtration device, start to take out
Filter；Then the substrate that the good graphene oxide membrane of suction filtration will be adhered to takes out, and is put in organic solvent so that graphene oxide membrane is fast
Fast drainage and formation, and split away off from substrate；By smooth substrate (such as silicon chip, glass, sheet metal etc.) directly organic molten
Graphene oxide membrane in agent with floating is contacted, it is possible to so that graphene oxide film transfer is attached on substrate.
Wherein：
Described organic solvent is methyl alcohol, ethanol, acetone, tetrahydrofuran, DMF, DMA, DMSO, HMPA, fourth sulfone, dioxy six
Ring, hydracrylic acid, ethamine, ethylenediamine, ethylene glycol, glycerine, ethylene glycol list first/second/propyl ether, diethylene glycol dimethyl ether or 1,3- dioxy
One kind in heterocycle pentane.
Graphene oxide content in the graphene oxide aqueous dispersions is 0.1ug/mi~100mg/ml.
Described substrate is the material not reacted with described organic solvent.
The material of described substrate is polycarbonate membrane, pellumina or polyvinylidene fluoride film.
The substrate of transfer is PET, PP, silicon chip, glass, polytetrafluoroethylene (PTFE), PDMS or metal.
Graphene oxide membrane is obtained if necessary to further reduction, the method that can be reduced by high temperature thermal reduction, hydrazine is obtained
Arrive.
In the present invention, the substrate of transfer is silicon chip, and glass, polyethylene terephthalate film, polypropylene resin film gathers
Vinyl chloride film, poly tetrafluoroethylene, polyurethane film, poly- carbonic acid resin film, propylene be fine-and butadiene-styrene is common
Polymer film, polystyrene film, polyvinyl alcohol film or the smooth flexibility of sheet metal or plastic substrate.
The present invention is dissolved each other well using organic solution and water energy, by making film inner layer between hydrone quickly be lost in from
And dry forming, and graphene oxide good dispersion and poor dispersion in organic solvent in water, therefore produce repulsion from lining
Depart from bottom.Because the flatness of film is higher, the method that can be depended on by directly contact is by film transfer to same smooth lining
On bottom.
Beneficial effect：The present invention compared with prior art, with advantages below：
In existing data, there is no a kind of method that can quickly peel off the graphene oxide membrane after suction filtration.Due to oxidation
Graphene film is often very strong with substrate combination degree through excessive pressure suction filtration, it is not easy to peeled off from substrate.It is most of all to connect
Substrate is used together, which greatly limits the use scope of graphene oxide membrane.Existing stripping means has (1) by increasing oxygen
Peeled off after graphite alkene film thickness is to be dried.This method can only obtain the very thick graphene oxide membrane of thickness, and due to wanting
Could be peeled off when film is completely dried, increase thickness and be certain to so that drying time increases；Or (2) use severe corrosive solution such as
Substrate is dissolved and obtains simple graphene oxide membrane by acetone.Film obtained in this method has certain deformation fold,
Can not fully demonstrate suction filtration film it is smooth the characteristics of, and more or less can also residual substrate vestige.And pass through the method for the present invention,
Can be completely without drying time, the time greatly shortens for peeling off thick film, while can also stripping film, put down
Whole graphene oxide membrane, shape keeps very intact.And the substrate for peeling off can be recycled, and be economized on resources.And due to flat
Whole degree is high, can easily be attached on smooth substrate, contacts very good.
Brief description of the drawings
Fig. 1 is that graphene oxide content is 0.08mg, and ethanol is coagulator, and substrate is the film that polycarbonate membrane is peeled off.
Fig. 2 is film transfer in Fig. 1 in PET flexible substrates.
Fig. 3 is the scanning electron microscope (SEM) photograph of Fig. 1 samples.
Fig. 4 graphene oxides content is 0.12mg, and ethanol is coagulator, and substrate is the scanning of the film that polycarbonate membrane is peeled off
Electron microscope.
Fig. 5 is that graphene oxide content is 0.3mg, and ethanol is coagulator, and substrate is sweeping for the film that polycarbonate membrane is peeled off
Retouch electron microscope.
Specific embodiment
The present invention is further elaborated with below by embodiment.
Embodiment 1：
The first step, takes the graphene oxide aqueous dispersions 10ul of 1mg/ml, and adds 100ml water.
Second step, the polycarbonate substrate in 0.4um apertures is fixed in Suction filtration device.
3rd step, graphene oxide dispersion is poured into and starts suction filtration in bottle,suction.
4th step, after the completion of suction filtration, gained film is put into ethanol solution rapidly, the graphene oxide for being peeled off
Film.
5th step, the graphene oxide membrane and silicon substrate that will be swum in ethanol solution is combined.
Embodiment 2：
Regulation and control method is basic with embodiment 1, and difference is：The graphene oxide aqueous dispersions 4ml of 1mg/ml is taken, and is added
In entering 100ml water.
Embodiment 3：
Regulation and control method is basic with embodiment 1, and difference is：The graphene oxide aqueous dispersions 10ml of 1mg/ml is taken, and
In addition 100ml water.
Embodiment 4：Regulation and control method is basic with embodiment 1, and difference is：Take the graphene oxide aqueous dispersions of 1mg/ml
100ml, and add 100ml water.
Embodiment 5：
Regulation and control method is basic with embodiment 2, and difference is：Substrate is changed to polyvinylidene fluoride film, and aperture is 0.22um.
Embodiment 6：Regulation and control method is basic with embodiment 3, and difference is：Substrate is changed to polytetrafluoroethylene (PTFE), and aperture is
0.22um。
Embodiment 7：Regulation and control method is basic with embodiment 3, and difference is：Polytetrafluoroethylene (PTFE) aperture is 045um.
Embodiment 8：
Regulation and control method is basic with embodiment 1, and difference is：Organic solution is methyl alcohol.
Embodiment 9：Regulation and control method is basic with embodiment 1, and difference is：Take the graphene oxide aqueous dispersions of 1mg/ml
6ml, organic solution is ethylene glycol.
Embodiment 10：Regulation and control method is basic with embodiment 9, and difference is：Organic solution is isopropanol.
Embodiment 11：Regulation and control method is basic with embodiment 9, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 12ml, organic solution is glycerine.
Embodiment 12：Regulation and control method is basic with embodiment 11, and difference is：Organic solution is ethylenediamine.
Embodiment 13：Regulation and control method is basic with embodiment 12, and difference is：Difference is：Take the oxidation of 1mg/ml
Graphene aqueous dispersions 15ml, organic solution is tetrahydrofuran.
Embodiment 14：Regulation and control method is basic with embodiment 13, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 20ml, suction filtration substrate is polyvinylidene fluoride film, and aperture 0.45um, organic solution is propyl ether.
Embodiment 15：Regulation and control method is basic with embodiment 14, and difference is：Organic solution is isopropanol.
Embodiment 16：Regulation and control method is basic with embodiment 15, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 30ml, organic solution is dimethylformamide.
Embodiment 17：Regulation and control method is basic with embodiment 16, and difference is：Suction filtration substrate is poly tetrafluoroethylene, hole
Footpath 0.45um, organic solution is DMA.
Embodiment 18：Regulation and control method is basic with embodiment 17, and difference is：Organic solution is dimethyl sulfoxide (DMSO).
Embodiment 19：Regulation and control method is basic with embodiment 18, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 35ml, organic solution is HMPA.
Embodiment 20：Regulation and control method is basic with embodiment 19, and difference is：Organic solution is fourth sulfone.
Embodiment 21：Regulation and control method is basic with embodiment 20, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 40ml, organic solution is dioxane.
Embodiment 22：Regulation and control method is basic with embodiment 21, and difference is：Suction filtration substrate is Anodisk filter, aperture
0.22um organic solutions are hydracrylic acid.
Embodiment 23：Regulation and control method is basic with embodiment 22, and difference is：Organic solution is ethamine.
Embodiment 24：Regulation and control method is basic with embodiment 23, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 45ml, organic solution is diethylene glycol dimethyl ether.
Embodiment 25：Regulation and control method is basic with embodiment 24, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 50ml, organic solution is 1,3- dioxolane.
Embodiment 26：Regulation and control method is basic with embodiment 25, and difference is：Transfer substrate is PET.
Embodiment 27：Regulation and control method is basic with embodiment 26, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 55ml, transfer substrate is copper sheet.
Embodiment 28：Regulation and control method is basic with embodiment 27, and difference is：Transfer substrate is aluminium flake.
Embodiment 29：Regulation and control method is basic with embodiment 28, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 60ml, transfer substrate is polyfluortetraethylene plate.
Embodiment 30：Regulation and control method is basic with embodiment 29, and difference is：Transfer substrate is polyfluortetraethylene plate.
Embodiment 31：Regulation and control method is basic with embodiment 30, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 65ml, transfer substrate is quartz glass plate.
Embodiment 32：Regulation and control method is basic with embodiment 31, and difference is：Transfer substrate is polyfluortetraethylene plate.
Embodiment 33：Regulation and control method is basic with embodiment 32, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 65ml, transfer substrate is polyethylene terephthalate film.
Embodiment 34：Regulation and control method is basic with embodiment 33, and difference is：Transfer substrate is polypropylene resin film.
Embodiment 35：Regulation and control method is basic with embodiment 34, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 70ml, transfer substrate is polychloroethylene film.
Embodiment 36：Regulation and control method is basic with embodiment 35, and difference is：Transfer substrate is polyurethane
Film.
Embodiment 37：Substantially with implementation 36, difference is regulation and control method：Take the graphene oxide aqueous dispersions of 1mg/ml
75ml, transfer substrate is poly- carbonic acid resin film.
Embodiment 38：Regulation and control method is basic with embodiment 37, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 80ml, transfer substrate is the propylene styrene copolymerized compound film of fine-butadiene-.
Embodiment 39：Regulation and control method is basic with embodiment 38, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 85ml, transfer substrate is polystyrene film.
Embodiment 40：Regulation and control method is basic with embodiment 39, and difference is：The graphene oxide moisture for taking 1mg/ml dissipates
Liquid 90ml, transfer substrate is polyvinyl alcohol film.
Claims (5)
1. a kind of quick stripping graphene oxide suction filtration film and the method for being transferred to substrate, it is characterised in that the method include with
Lower step：
Add graphene oxide into first in water, ultrasonic disperse forms graphene oxide aqueous dispersions, is then placed in substrate and takes out
On the core of filter flask, Suction filtration device is put up, the graphene oxide dispersion that will then prepare pours into Suction filtration device, start suction filtration；
Then the substrate that the good graphene oxide membrane of suction filtration will be adhered to takes out, and is put in organic solvent so that graphene oxide membrane is rapid
Drainage and formation, and split away off from substrate；By smooth substrate directly in organic solvent with floating graphene oxide membrane
Contact, it is possible to so that graphene oxide film transfer is attached on substrate；
Described substrate is the material not reacted with described organic solvent.
2. a kind of quick stripping graphene oxide suction filtration film according to claim 1 and the method for being transferred to substrate, it is special
Levy and be, described organic solvent is methyl alcohol, ethanol, acetone, tetrahydrofuran, DMF, DMA, DMSO, HMPA, fourth sulfone, dioxy six
Ring, hydracrylic acid, ethamine, ethylenediamine, ethylene glycol, glycerine, ethylene glycol list first/second/propyl ether, diethylene glycol dimethyl ether or 1,3- dioxy
One kind in heterocycle pentane.
3. a kind of quick stripping graphene oxide suction filtration film according to claim 1 and the method for being transferred to substrate, it is special
Levy and be, the graphene oxide concentration in the graphene oxide aqueous dispersions is 0.1ug/ml~100mg/ml.
4. a kind of quick stripping graphene oxide suction filtration film according to claim 1 and the method for being transferred to substrate, it is special
Levy and be, the material of described substrate is polycarbonate membrane, pellumina or polyvinylidene fluoride film.
5. a kind of quick stripping graphene oxide suction filtration film according to claim 1 and the method for being transferred to substrate, it is special
Levy and be, the substrate of transfer is silicon chip, glass, polyethylene terephthalate film, polypropylene resin film, polychloroethylene film,
Poly tetrafluoroethylene, polyurethane film, poly- carbonic acid resin film, acrylonitrile-butadiene-styrene copolymerized compound film,
The smooth flexibility or plastic substrate of polystyrene film, polyvinyl alcohol film or sheet metal.
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| CN106395802B (en) * | 2016-09-08 | 2020-08-11 | 山东理工大学 | Preparation method of graphene porous membrane |
| CN111341997B (en) * | 2017-10-13 | 2021-05-28 | 南京旭羽睿材料科技有限公司 | Preparation method of graphene membrane electrode |
| CN108394896B (en) * | 2018-05-09 | 2021-09-07 | 东南大学 | Method for preparing graphene oxide film with assistance of gas stripping |
| CN108840329B (en) * | 2018-07-10 | 2020-07-07 | 杭州高烯科技有限公司 | Preparation method of independent self-supporting graphene-based ultrathin film |
| CN108970952B (en) * | 2018-07-10 | 2020-09-04 | 杭州高烯科技有限公司 | Tone adjustable nano-scale sound wave generator |
| CN108862262B (en) * | 2018-07-10 | 2020-05-12 | 杭州高烯科技有限公司 | Preparation method of graphene-based ultrathin composite film |
| CN108793124B (en) * | 2018-07-10 | 2020-06-23 | 杭州高烯科技有限公司 | Preparation method of self-supporting graphene film |
| CN108640106A (en) * | 2018-07-10 | 2018-10-12 | 杭州高烯科技有限公司 | A kind of stripping means of graphene film |
| CN108892133B (en) * | 2018-07-10 | 2020-08-14 | 浙江大学 | Nanoscale sound wave generating film and nanoscale sound wave generator |
| CN109036851B (en) * | 2018-07-10 | 2020-02-21 | 浙江大学 | Graphene-based thin-film solar cell |
| CN110420567B (en) * | 2019-07-12 | 2022-04-22 | 中国工程物理研究院材料研究所 | Preparation method of graphene hydrophobic membrane and application method of membrane distillation |
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