CN105329884A - 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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- CN105329884A CN105329884A CN201510828612.4A CN201510828612A CN105329884A CN 105329884 A CN105329884 A CN 105329884A CN 201510828612 A CN201510828612 A CN 201510828612A CN 105329884 A CN105329884 A CN 105329884A
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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 transfer to the method for substrate.Belong to the technical field that graphene oxide suction filtration film is peeled off fast and shifted.
Background technology
Along with the discovery of Graphene, the electrical properties of its excellence, mechanical property, thermal property and magnetic property cause the extensive concern of people.As the important derivatives of Graphene, graphene oxide is also subject to increasing attention.Graphene oxide, as a kind of new carbon of excellent performance, has cellular two-dirnentional structure, owing to having special physics, chemical property, as higher specific surface area, and higher porosity, containing abundant oxygen-containing functional group, the features such as asepsis environment-protecting.Graphene oxide and its reduzate Graphene in a lot of field, as absorption (YubingSun, ShubinYang, YueChen, CongcongDing, WencaiCheng, XiangkeWang, Environ.Sci.Technol.2015,49,4255-4262), sewage purification (YiHan, ZhenXu, andChaoGao, Adv.Funct.Mater.2013,23,3693), ultracapacitor (Li, Meng; Tang, Zhe, Leng, Mei, etal.Adv.Funct.Mater.2014,24,7495 – 7502), fuel-cell catalyst (Jia, Lingpu, Sun, Xiao, Jiang, Yimin, etal.Adv.Funct.Mater.2015,25,1814 – 1820) etc. multiple field receive and study widely.How preparing smooth two dimensional oxidation graphene film is the problem that present people constantly explore.The method preparing graphene oxide membrane also emerges in an endless stream LB method (LauraJ.Cote, FranklinKim, andJiaxingHuang.J.AM.Chem.Soc.2009,131,1043 – 1049), spin-coating method (Kymakis, Emmanuel; Savva, Kyriak, Stylianakis, MinasM, etal.Adv.Funct.Mater.2013,23,2742 – 2749), spraying method (Parviz, Dorsa, Metzler, ShaneD., Das, Sriya, etal.small2015,11, No.22,2661 – 2668) etc.Vacuum filtration is easy to operate due to it, and obtained film is compared with other liquid membrane formation process uniform ground the most, enjoys people to pay close attention to.But the greatest problem that suction method faces is exactly how graphene oxide membrane to be peeled off from substrate.If graphene oxide membrane is too thin, then cannot peel off complete film from substrate; And if film is enough thick, complete drying graphene oxide also needs the plenty of time.Dissolve substrate with corrosive liquid such as acetone in some experiments, and film pattern obtained like this cannot keep smooth.So in order to utilize the advantage of suction filtration graphene oxide membrane completely, and can reduce further and obtain smooth graphene film, must can find a kind of method of quick stripping graphene oxide membrane, thus transfer to the operation that various substrate realizes further functionalization.
Summary of the invention
Technical problem: the invention provides a kind of quick stripping graphene oxide suction filtration film and transfer to the method for substrate, can realize graphene oxide membrane rapid dehydration complete for firm suction filtration is dry and peel off from substrate and shift.
Technical scheme: a kind of quick stripping graphene oxide suction filtration film of the present invention also transfers to the method for substrate, comprises the following steps:
First be added to the water by graphene oxide, ultrasonic disperse forms graphene oxide aqueous dispersions, is then placed on the core of filter flask by substrate, puts up Suction filtration device, then pour the graphene oxide dispersion prepared into Suction filtration device, starts suction filtration; Then the substrate of graphene oxide membrane good for attachment suction filtration is taken out, be put in organic solvent, graphene oxide membrane rapid dehydration be shaped, and split away off from substrate; Smooth substrate (as silicon chip, glass, tinsel etc.) is directly contacted with floating graphene oxide membrane in organic solvent, graphene oxide membrane just can be made to shift and be attached on substrate.
Wherein:
Described organic solvent is methyl alcohol, ethanol, acetone, tetrahydrofuran (THF), DMF, DMA, one in DMSO, HMPA, fourth sulfone, dioxane, hydroxy-propionic acid, ethamine, quadrol, ethylene glycol, glycerine, ethylene glycol list first/second/propyl ether, diglyme or 1,3-dioxolane.
Graphene oxide content in described graphene oxide aqueous dispersions is 0.1ug/mi ~ 100mg/ml.
Described substrate is the material do 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, tetrafluoroethylene, PDMS or metal.
If need further reduction to obtain graphene oxide membrane, can be reduced by high-temperature hot, the method for hydrazine reduction obtains.
In the present invention, 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, propylene be fine-the smooth flexibility of divinyl-styrene copolymerized compound film, Polystyrene Film, polyvinyl alcohol film or tinsel or plastic substrate.
The present invention utilizes organic solution and water well to dissolve each other, and by making the water molecules between film inner layer run off fast thus dry forming, and graphene oxide good dispersity and dispersed bad in organic solvent in water, therefore produces repulsion and departs from from substrate.Because the planeness of film is higher, by directly contacting the method depended on, film can be transferred on substrate smooth equally.
Beneficial effect: the present invention compared with prior art, has the following advantages:
In existing data, there is no a kind of method can peeling off the graphene oxide membrane after suction filtration fast.Because graphene oxide membrane is through excessive pressure suction filtration, often very strong with substrate combination degree, be not easy to peel off from substrate.Great majority all can connect substrate and use together, which greatly limits the use range of graphene oxide membrane.Existing stripping means has (1) by increasing the rear stripping to be dried of graphene oxide film thickness.This method can only obtain the very thick graphene oxide membrane of thickness, and owing to will wait until that film complete drying could be peeled off, increases thickness and be certain to time of drying is increased; Or (2) as acetone, substrate dissolved with severe corrosive solution and obtain simple graphene oxide membrane.The film that this method obtains has certain deformation fold, can not fully demonstrate the feature that suction filtration film is smooth, and more or less also can remain the vestige of substrate.And by method of the present invention, can not need time of drying completely, and the time stripping thick film is shortened greatly, simultaneously also can stripping film, obtain smooth graphene oxide membrane, form trait is very intact.And the substrate peeled off can recycle, and economizes on resources.And due to planeness high, easily can be attached on smooth substrate, contact very good.
Accompanying drawing explanation
Fig. 1 is graphene oxide content is 0.08mg, and ethanol is peptizer, and substrate is the film that polycarbonate membrane peels off.
Fig. 2 is that the film in Fig. 1 is transferred in PET flexible substrate.
Fig. 3 is the scanning electron microscope (SEM) photograph of Fig. 1 sample.
Fig. 4 graphene oxide content is 0.12mg, and ethanol is peptizer, and substrate is the scanning electron microscope (SEM) photograph of the film that polycarbonate membrane peels off.
Fig. 5 is graphene oxide content is 0.3mg, and ethanol is peptizer, and substrate is the scanning electron microscope (SEM) photograph of the film that polycarbonate membrane peels off.
Embodiment
Below by embodiment the present invention done and illustrate further.
Embodiment 1:
The first step, gets the graphene oxide aqueous dispersions 10ul of 1mg/ml, and adds in 100ml water.
Second step, is fixed on the polycarbonate substrate in 0.4um aperture in Suction filtration device.
3rd step, pours into graphene oxide dispersion in filter flask and starts suction filtration.
4th step, after suction filtration completes, puts into ethanolic soln rapidly by gained film, obtains the graphene oxide membrane of peeling off.
5th step, combines the graphene oxide membrane swum in ethanolic soln and silicon substrate.
Embodiment 2:
Regulate and control method is substantially with embodiment 1, and difference is: the graphene oxide aqueous dispersions 4ml getting 1mg/ml, and adds in 100ml water.
Embodiment 3:
Regulate and control method is substantially with embodiment 1, and difference is: the graphene oxide aqueous dispersions 10ml getting 1mg/ml, and adds in 100ml water.
Embodiment 4: regulate and control method is substantially with embodiment 1, and difference is: the graphene oxide aqueous dispersions 100ml getting 1mg/ml, and add in 100ml water.
Embodiment 5:
Regulate and control method is substantially with embodiment 2, and difference is: substrate changes polyvinylidene fluoride film into, and aperture is 0.22um.
Embodiment 6: regulate and control method is substantially with embodiment 3, and difference is: substrate changes tetrafluoroethylene into, aperture is 0.22um.
Embodiment 7: regulate and control method is substantially with embodiment 3, and difference is: tetrafluoroethylene aperture is 045um.
Embodiment 8:
Regulate and control method is substantially with embodiment 1, and difference is: organic solution is methyl alcohol.
Embodiment 9: regulate and control method is substantially with embodiment 1, and difference is: the graphene oxide aqueous dispersions 6ml getting 1mg/ml, organic solution is ethylene glycol.
Embodiment 10: regulate and control method is substantially with embodiment 9, and difference is: organic solution is Virahol.
Embodiment 11: regulate and control method is substantially with embodiment 9, and difference is: the graphene oxide aqueous dispersions 12ml getting 1mg/ml, organic solution is glycerine.
Embodiment 12: regulate and control method is substantially with embodiment 11, and difference is: organic solution is quadrol.
Embodiment 13: regulate and control method is substantially with embodiment 12, and difference is: difference is: the graphene oxide aqueous dispersions 15ml getting 1mg/ml, organic solution is tetrahydrofuran (THF).
Embodiment 14: regulate and control method is substantially with embodiment 13, and difference is: the graphene oxide aqueous dispersions 20ml getting 1mg/ml, suction filtration substrate is polyvinylidene fluoride film, aperture 0.45um, and organic solution is propyl ether.
Embodiment 15: regulate and control method is substantially with embodiment 14, and difference is: organic solution is Virahol.
Embodiment 16: regulate and control method is substantially with embodiment 15, and difference is: the graphene oxide aqueous dispersions 30ml getting 1mg/ml, organic solution is dimethyl formamide.
Embodiment 17: regulate and control method is substantially with embodiment 16, and difference is: suction filtration substrate is poly tetrafluoroethylene, aperture 0.45um, organic solution is DMA.
Embodiment 18: regulate and control method is substantially with embodiment 17, and difference is: organic solution is dimethyl sulfoxide (DMSO).
Embodiment 19: regulate and control method is substantially with embodiment 18, and difference is: the graphene oxide aqueous dispersions 35ml getting 1mg/ml, organic solution is HMPA.
Embodiment 20: regulate and control method is substantially with embodiment 19, and difference is: organic solution is fourth sulfone.
Embodiment 21: regulate and control method is substantially with embodiment 20, and difference is: the graphene oxide aqueous dispersions 40ml getting 1mg/ml, organic solution is dioxane.
Embodiment 22: regulate and control method is substantially with embodiment 21, and difference is: suction filtration substrate is Anodisk filter, aperture 0.22um organic solution is hydroxy-propionic acid.
Embodiment 23: regulate and control method is substantially with embodiment 22, and difference is: organic solution is ethamine.
Embodiment 24: regulate and control method is substantially with embodiment 23, and difference is: the graphene oxide aqueous dispersions 45ml getting 1mg/ml, organic solution is diglyme.
Embodiment 25: regulate and control method is substantially with embodiment 24, and difference is: the graphene oxide aqueous dispersions 50ml getting 1mg/ml, organic solution is 1,3-dioxolane.
Embodiment 26: regulate and control method is substantially with embodiment 25, and difference is: translate substrate is PET.
Embodiment 27: regulate and control method is substantially with embodiment 26, and difference is: the graphene oxide aqueous dispersions 55ml getting 1mg/ml, translate substrate is copper sheet.
Embodiment 28: regulate and control method is substantially with embodiment 27, and difference is: translate substrate is aluminium flake.
Embodiment 29: regulate and control method is substantially with embodiment 28, and difference is: the graphene oxide aqueous dispersions 60ml getting 1mg/ml, translate substrate is polyfluortetraethylene plate.
Embodiment 30: regulate and control method is substantially with embodiment 29, and difference is: translate substrate is polyfluortetraethylene plate.
Embodiment 31: regulate and control method is substantially with embodiment 30, and difference is: the graphene oxide aqueous dispersions 65ml getting 1mg/ml, translate substrate is quartz glass plate.
Embodiment 32: regulate and control method is substantially with embodiment 31, and difference is: translate substrate is polyfluortetraethylene plate.
Embodiment 33: regulate and control method is substantially with embodiment 32, and difference is: the graphene oxide aqueous dispersions 65ml getting 1mg/ml, translate substrate is polyethylene terephthalate film.
Embodiment 34: regulate and control method is substantially with embodiment 33, and difference is: translate substrate is polypropylene resin film.
Embodiment 35: regulate and control method is substantially with embodiment 34, and difference is: the graphene oxide aqueous dispersions 70ml getting 1mg/ml, translate substrate is polychloroethylene film.
Embodiment 36: regulate and control method is substantially with embodiment 35, and difference is: translate substrate is polyurethane film.
Embodiment 37: regulate and control method is substantially with implementing 36, and difference is: the graphene oxide aqueous dispersions 75ml getting 1mg/ml, translate substrate is poly-carbonic acid resin film.
Embodiment 38: regulate and control method is substantially with embodiment 37, and difference is: the graphene oxide aqueous dispersions 80ml getting 1mg/ml, translate substrate be propylene fine-divinyl-styrene copolymerized compound film.
Embodiment 39: regulate and control method is substantially with embodiment 38, and difference is: the graphene oxide aqueous dispersions 85ml getting 1mg/ml, translate substrate is Polystyrene Film.
Embodiment 40: regulate and control method is substantially with embodiment 39, and difference is: the graphene oxide aqueous dispersions 90ml getting 1mg/ml, translate substrate is polyvinyl alcohol film.
Claims (6)
1. fast peel off graphene oxide suction filtration film and transfer to the method for substrate, it is characterized in that, the method comprises the following steps:
First be added to the water by graphene oxide, ultrasonic disperse forms graphene oxide aqueous dispersions, is then placed on the core of filter flask by substrate, puts up Suction filtration device, then pour the graphene oxide dispersion prepared into Suction filtration device, starts suction filtration; Then the substrate of graphene oxide membrane good for attachment suction filtration is taken out, be put in organic solvent, graphene oxide membrane rapid dehydration be shaped, and split away off from substrate; Smooth substrate is directly contacted with floating graphene oxide membrane in organic solvent, graphene oxide membrane just can be made to shift and be attached on substrate.
2. a kind of quick stripping graphene oxide suction filtration film according to claim 1 transfer to the method for substrate, it is characterized in that, described organic solvent is methyl alcohol, ethanol, acetone, tetrahydrofuran (THF), DMF, DMA, one in DMSO, HMPA, fourth sulfone, dioxane, hydroxy-propionic acid, ethamine, quadrol, ethylene glycol, glycerine, ethylene glycol list first/second/propyl ether, diglyme or 1,3-dioxolane.
3. a kind of quick stripping graphene oxide suction filtration film according to claim 1 transfer to the method for substrate, it is characterized in that, the graphene oxide concentration in described 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 transfer to the method for substrate, it is characterized in that, described substrate is the material do not reacted with described organic solvent.
5. a kind of quick stripping graphene oxide suction filtration film according to claim 1 or 4 also transfers to the method for substrate, and it is characterized in that, the material of described substrate is polycarbonate membrane, pellumina or polyvinylidene fluoride film.
6. a kind of quick stripping graphene oxide suction filtration film according to claim 1 transfer to the method for substrate, it is characterized in that, 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, propylene be fine-the smooth flexibility of divinyl-styrene copolymerized compound film, Polystyrene Film, polyvinyl alcohol film or tinsel or plastic substrate.
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Cited By (11)
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| CN106395802A (en) * | 2016-09-08 | 2017-02-15 | 山东理工大学 | Method for preparing graphene porous membrane |
| CN108394896A (en) * | 2018-05-09 | 2018-08-14 | 东南大学 | A kind of method that gas stripping auxiliary prepares graphene oxide membrane |
| 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 |
| CN108793124A (en) * | 2018-07-10 | 2018-11-13 | 杭州高烯科技有限公司 | A kind of preparation method of self-supporting graphene film |
| CN108840329A (en) * | 2018-07-10 | 2018-11-20 | 杭州高烯科技有限公司 | A kind of preparation method of the graphene-based ultrathin membrane of independent self-supporting |
| CN108862262A (en) * | 2018-07-10 | 2018-11-23 | 杭州高烯科技有限公司 | A kind of preparation method of graphene-based ultra-thin composite membrane |
| CN108892133A (en) * | 2018-07-10 | 2018-11-27 | 浙江大学 | A kind of nanoscale sound generating membranes and nanoscale sonic generator |
| CN108970952A (en) * | 2018-07-10 | 2018-12-11 | 杭州高烯科技有限公司 | A kind of adjustable nanoscale sonic generator of tone color |
| CN109036851A (en) * | 2018-07-10 | 2018-12-18 | 浙江大学 | A kind of graphene-based thin-film solar cells |
| CN110420567A (en) * | 2019-07-12 | 2019-11-08 | 中国工程物理研究院材料研究所 | A kind of preparation method of graphene hydrophobic membrane and the application method of membrane distillation |
| CN111341997A (en) * | 2017-10-13 | 2020-06-26 | 南京旭羽睿材料科技有限公司 | Novel graphene membrane electrode preparation method |
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| CN106395802A (en) * | 2016-09-08 | 2017-02-15 | 山东理工大学 | Method for preparing graphene porous membrane |
| CN106395802B (en) * | 2016-09-08 | 2020-08-11 | 山东理工大学 | Preparation method of graphene porous membrane |
| CN111341997A (en) * | 2017-10-13 | 2020-06-26 | 南京旭羽睿材料科技有限公司 | Novel graphene membrane electrode preparation method |
| 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 |
| CN108394896A (en) * | 2018-05-09 | 2018-08-14 | 东南大学 | A kind of method that gas stripping auxiliary prepares graphene oxide membrane |
| CN108394896B (en) * | 2018-05-09 | 2021-09-07 | 东南大学 | Method for preparing graphene oxide film with assistance of gas stripping |
| CN108840329A (en) * | 2018-07-10 | 2018-11-20 | 杭州高烯科技有限公司 | A kind of preparation method of the graphene-based ultrathin membrane of independent self-supporting |
| CN108970952A (en) * | 2018-07-10 | 2018-12-11 | 杭州高烯科技有限公司 | A kind of adjustable nanoscale sonic generator of tone color |
| CN109036851A (en) * | 2018-07-10 | 2018-12-18 | 浙江大学 | A kind of graphene-based thin-film solar cells |
| CN108892133A (en) * | 2018-07-10 | 2018-11-27 | 浙江大学 | A kind of nanoscale sound generating membranes and nanoscale sonic generator |
| 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 |
| CN108862262A (en) * | 2018-07-10 | 2018-11-23 | 杭州高烯科技有限公司 | A kind of preparation method of graphene-based ultra-thin composite membrane |
| CN108892133B (en) * | 2018-07-10 | 2020-08-14 | 浙江大学 | Nanoscale sound wave generating film and nanoscale sound wave generator |
| CN108793124A (en) * | 2018-07-10 | 2018-11-13 | 杭州高烯科技有限公司 | A kind of 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 |
| CN110420567A (en) * | 2019-07-12 | 2019-11-08 | 中国工程物理研究院材料研究所 | A kind of preparation method of graphene hydrophobic membrane and the application method of membrane distillation |
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