CN103072976B - Transfer method of graphene or oxidized graphene thin film - Google Patents
Transfer method of graphene or oxidized graphene thin film Download PDFInfo
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- CN103072976B CN103072976B CN201210587780.5A CN201210587780A CN103072976B CN 103072976 B CN103072976 B CN 103072976B CN 201210587780 A CN201210587780 A CN 201210587780A CN 103072976 B CN103072976 B CN 103072976B
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Abstract
The invention relates to a transfer method of a graphene or oxidized graphene thin filma, which is used for transferring the graphene or oxidized graphene thin film from a flexible substrate to a target substrate and comprises the following steps: cleaning the target substrate, and performing drying treatment for later use; performing activation treatment to the target substrate to add hydroxy onto the surface of the target substrate; forming a thin film on one side of the flexible substrate in a vacuum suction filtration device; tiling the side of the flexible substrate with the thin film on the target substrate in 30 s in moist atmosphere; squeezing the side of the flexible substrate without the thin film by using a brush to preclude the vesicles between the thin film and the target substrate; fast squeezing the flexible substrate and the target substrate by using an extruder before the thin film is dried to enable the thin film and the target substrate to be in full contact; and slowly tearing off the flexible substrate to transfer the thin film from the flexible substrate to the target substrate. Compared with the prior art, the method is simple to operate, the repeatability is good, no impurity is introducedand no organic matter is used.
Description
Technical field
The invention belongs to function film technical field, relate to a kind of transfer method of graphene film, is that graphene film is transferred to a kind of method target substrate from preparing substrate specifically.
Background technology
Badeker in 1907 etc. utilize sputtering method to prepare CdO transparent conductive film (Transparentconducting films, TCFs).The research of TCFs experienced by the ITO (the In2O3 base film of Sn doping) of the sixties, the electrically conducting transparent multilayer film of the seventies and the ZnO of the doping eighties.In recent years along with the progress of science and technology and the discovery of novel material, novel carbon nanotube TCFs, Graphene TCFs are there is.After within 2004, Graphene is successfully prepared, compared to current industrial widely used ITO, FTO (SnO of F doping
2base film) and AZO (the zno-based film of Al doping) material, there is the feature such as transmittance high (theoretical value is 97.5%), snappiness is good, weather resistance is high, aboundresources and be incorporated into rapidly in function film field.
The preparation method of graphene film mainly contains chemical Vapor deposition process, vacuum filtration method, spin-coating method, self-assembly etc.Because large quantity research shows that in single-layer graphene λ=300-2500nm spectral range, its inter-band absorption only has 2.3%.The light tight rate of multi-layer graphene increases with the increase of its number of plies, and every one deck about increases by the opaqueness of 2.3%.The mobility of room temperature download stream can reach 15000cm
2/ more than Vs, can be observed quantum hall effect under normal temperature simultaneously.Photoelectric characteristic due to its uniqueness of Graphene determines graphene film and can be applicable to the fields such as electroluminescent device, flat liquid crystal display, Organic Light Emitting Diode, dye sensitization solar battery, sensor, smart window.
Domestic and international after utilization flexible substrate carries out film forming at present, transfer to target substrate generally adopt chemical method from preparing substrate, its technological process first applies pressure for some time, then adopt the flexible substrate material dissolving former graphene film, finally with organic solvent, flushing is for several times being carried out to film.Though the method effectively can realize the transfer of film, but its complex technical process is time-consuming, introduce the performance of organic impurity influence film, especially in the process using a large amount of organic solvents simultaneously, not only waste resource, and can to human body and environmental pollution.Be difficult to meet the demand that industrialization is prepared on a large scale.Meanwhile, also someone adopts and film is placed in 45 DEG C of vacuum drying ovens dry 24 hours together with flexible substrate, is then taken off from flexible base board by film, is shifting.The method migration period is long, and higher to technical requirements in the process of taking off film.Be difficult to meet the demand that industrialization is prepared on a large scale equally.
Summary of the invention
Object of the present invention is exactly providing a kind of simple to operate, favorable reproducibility to overcome defect that above-mentioned prior art exists, not introducing impurity, not using the Graphene of organic substance or the transfer method of graphene oxide film.
Object of the present invention can be achieved through the following technical solutions:
According to the different in kind of the reactive force of binding molecule and solid surface, absorption can be divided into physical adsorption and chemisorption.In adsorption process, do not have transfer transport, do not have generation and the destruction of chemical bond, the absorption of generation is Van der Waals force, is called physical adsorption.And in chemisorption, binding molecule and solid surface there occurs chemical reaction, the reactive force between its reactive force with compound Atom is similar.-OH on its surface band is made through the vitriol oil and the water-treated substrate surface such as glass, PET of dioxygen, and graphene oxide and the insufficient graphene oxide lamella peripheral zone of reduction have-COOH, esterification can be there is in-OH with-COOH, substrate and graphene film are connected by chemical bond, and graphene film and to prepare between flexible substrate just simple physical adsorption.Because chemical bond force much larger than Van der Waals force, thus will achieve effective transfer of graphene film.Meanwhile, when silicate is as target base plate, graphene oxide is electronegative, and the easy positively charged of most of silicate surfaces.Molecular structure as glass is more special, it is very weak to the constraint ability (magnetism) of electronics, when glass contacts with other materials and rubs, other attract the molecule of electronic capability stronger material the electronics of glass surface molecule will be seized, the positive electricity that made it bring.Heterocharge attracts each other and is also conducive to the transfer of graphene film.
A transfer method for Graphene or graphene oxide film, transfer to target substrate by Graphene or graphene oxide film from flexible substrate, the method comprises the following steps:
(1) decontamination, drying treatment are carried out to target substrate, for subsequent use;
(2) activation treatment is carried out to the target substrate processed through step (1), hydroxyl on the surface band making target substrate;
(3) in Vacuum filtration device, the side of flexible substrate forms film;
(4) in the atmosphere of humidity, side flexible substrate with film is laid on target substrate in 30s;
(5) there is no the side of film with hairbrush extruding flexible substrate, get rid of the bubble between film and target substrate;
(6) when film is not dry, extrude rapidly flexible substrate and target substrate with extrusion machine, film is fully contacted with target substrate;
(7) with hand or tweezers, flexible substrate is slowly taken off, transferred on target substrate by flexible substrate by film.
Described target substrate is glass substrate or PET substrate.
Described flexible substrate is polyvinylidene fluoride film or water system CN-CA.
The condition of the drying treatment described in step (1) is: dry 4 ~ 6min at the temperature of 40 ~ 60 DEG C.
The concrete steps of the activation treatment described in step (2) are: under the condition of 70 ~ 90 DEG C, by target substrate brew 40min ~ 50min in the mixed solution of concentrated acid and hydrogen peroxide.
Described concentrated acid is the vitriol oil, and the volume ratio of concentrated acid and hydrogen peroxide is 7: 3.
Film described in step (3) to step (7) is graphene film or graphene oxide film.
Described in step (3) in Vacuum filtration device, on the side of flexible substrate, film forming concrete grammar was: by the graphene solution of 0.05 ~ 1mg/ml or graphene oxide solution under 10000 ~ 15000 revs/min centrifugal 10 ~ 15 minutes, reduce one hour under the voltage of 20v subsequently, the solution of gained ammoniacal liquor is allocated to PH=10, carry out ultrasonic disperse again, then in Vacuum filtration device, in aperture be 0.2 ~ 0.5um flexible substrate on film forming.
Compared with prior art, the present invention has the following advantages:
(1), compared with time-consuming method complicated with tradition, the present invention adopts micromechanics to shift and can complete in tens seconds, has simple, timesaving feature.
(2) do not have by other material in the whole transfer process of film, do not introduce impurity on the surface of film, the film of gained has better properties.
(3) compare the substrate material that traditional chemical method dissolves former graphene/graphene oxide film, the present invention does not use the organic substance be harmful to environment and human body.Not only reduce the injury to environment and human body, and reduce cost of transfer.
(4) the present invention does not dissolve the substrate material of former graphene/graphene oxide film in transfer process, and its substrate material is reusable, reduce further cost.
(5) not only cost of transfer is low for the method, and has processing ease, favorable reproducibility, and suitability is strong.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the structural representation of extrusion machine;
Fig. 3 is that in embodiment 1, graphene oxide film transfers to the scanning electron microscope image on glass substrate;
Fig. 4 is that in embodiment 2, graphene film transfers to the scanning electron microscope image on glass substrate.
In figure, 1 is support, and 2 is motor driven compressor, and 3 is extruding disk, and 4 is pole, and 5 is chute.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Graphene oxide film is transferred on glass substrate
As shown in Fig. 1 schema, not air-dry film on flexible substrate is laid on target substrate, then the bubble between extrusion film and target substrate, then with extrusion machine extruding flexible substrate and target substrate, make film and target substrate close contact, then film is just molded on target substrate, and now film is air-dry film, then take flexible substrate off, namely make air-dry adhesion of film on target substrate.
By the graphene oxide solution of 1mg/ml under 14000 turns centrifugal 10 minutes, reduce one hour under the voltage of 20v subsequently, by the solution of gained allocate with ammoniacal liquor its PH=10 carry out ultrasonic from new dispersion.Take aperture as 0.25um polyvinylidene fluoride film film forming in Vacuum filtration device, first rapid by with film one side tiling on the glass substrate; When film is not dry, then first suitably extrude eliminating bubble with brush, be placed on subsequently in extrusion machine as shown in Figure 2 and extrude, to be extruded complete after, throw off polyvinylidene fluoride film with hand or tweezers, the transfer of oxidation graphene film can be realized.Forcing machine shown in Fig. 2 comprises support 1, motor driven compressor 2, extruding disk 3, pole 4 and chute 5, wherein, chute 5 is located at the two ends, left and right of support 1, and pole 4 is located at the centre of support 1, the two ends of pole 4 are connected with chute 5, and motor driven compressor 2 and extruding disk 3 are located at the both sides of pole 4.Fig. 3 is the scanning electron microscope image that graphene oxide film transfers on glass substrate, and as can be seen from Figure when using tranfer system of the present invention, the film obtained is comparatively even, integrity is better, and the shape characteristic of film can be found out clearly.
Embodiment 2
Graphene film is transferred on glass substrate
As shown in Fig. 1 schema, be first 0.45um water system CN-CA in aperture by the graphene oxide solution of .1mg/ml be film forming in the Vacuum filtration device of flexible substrate; Then film being had to take off gently from Vacuum filtration device rapidly, tiling there being the one side of film rapidly on the glass substrate; When film is not dry, then rapid brush suitably extrudes eliminating bubble, is placed on subsequently in the extrusion machine as Fig. 2 and extrudes, to be extruded complete after, throw off CN-CA with hand or tweezers, the transfer of graphene oxide film can be realized.Fig. 4 is the scanning electron microscope image that graphene film transfers on glass substrate, and as can be seen from Figure when using tranfer system of the present invention, the film obtained is comparatively even, integrity is better, and the shape characteristic of film can be found out clearly.
Embodiment 3
Graphene oxide film is transferred on flexible base board PET.
As shown in Fig. 1 schema, be first 0.25um water system CN-CA in aperture by the graphene oxide solution of 0.05mg/ml be film forming in the Vacuum filtration device of flexible substrate; Then film being had to take off gently from Vacuum filtration device rapidly, being laid in there being the one side of film rapidly on pet substrate; When film is not dry, then rapid brush suitably extrudes eliminating bubble, is placed on subsequently in the extrusion machine as Fig. 2 and extrudes, to be extruded complete after, throw off CN-CA with hand or tweezers, the transfer of graphene oxide film can be realized.
Embodiment 4
A kind of transfer method of graphene film, graphene film is transferred to target substrate from flexible substrate, its technical process as shown in Figure 1, not air-dry film on flexible substrate is laid on target substrate, then the bubble between extrusion film and target substrate, then with extrusion machine extruding flexible substrate and target substrate, make film and target substrate close contact, then film is just molded on target substrate, now film is air-dry film, then take flexible substrate off, namely make air-dry adhesion of film on target substrate.The method comprises the following steps:
(1) decontamination, drying treatment are carried out to target substrate, for subsequent use;
(2) activation treatment is carried out to the target substrate processed through step (1), hydroxyl on the surface band making target substrate;
(3) in Vacuum filtration device, the side of flexible substrate forms film;
(4) in the atmosphere of humidity, side flexible substrate with film is laid on target substrate in 30s;
(5) there is no the side of film with hairbrush extruding flexible substrate, get rid of the bubble between film and target substrate;
(6) when film is not dry, extrude rapidly flexible substrate and target substrate with extrusion machine, film is fully contacted with target substrate;
(7) with hand or tweezers, flexible substrate is slowly taken off, transferred on target substrate by flexible substrate by film.
Wherein, target substrate is glass substrate.Flexible substrate is polyvinylidene fluoride film.The condition of step (1) drying treatment is: dry 6min at the temperature of 40 DEG C.The concrete steps of step (2) activation treatment are: under the condition of 70 DEG C, by target substrate (volume ratio of concentrated acid and hydrogen peroxide is 7: 3) brew 50min in the mixed solution of the vitriol oil and hydrogen peroxide.In step (3) to step (7), film is graphene film.Step (3) is in Vacuum filtration device, on the side of flexible substrate, film forming concrete grammar was: by the graphene solution of 0.05mg/ml or graphene oxide solution under 10000 revs/min centrifugal 15 minutes, reduce one hour under the voltage of 20v subsequently, the solution of gained ammoniacal liquor is allocated to PH=10, carry out ultrasonic disperse again, then in Vacuum filtration device, in aperture be 0.2um flexible substrate on film forming.
Embodiment 5
A kind of transfer method of graphene oxide film, graphene oxide film is transferred to target substrate from flexible substrate, its technical process as shown in Figure 1, not air-dry film on flexible substrate is laid on target substrate, then the bubble between extrusion film and target substrate, then with extrusion machine extruding flexible substrate and target substrate, make film and target substrate close contact, then film is just molded on target substrate, now film is air-dry film, then take flexible substrate off, namely make air-dry adhesion of film on target substrate.The method comprises the following steps:
(1) decontamination, drying treatment are carried out to target substrate, for subsequent use;
(2) activation treatment is carried out to the target substrate processed through step (1), hydroxyl on the surface band making target substrate;
(3) in Vacuum filtration device, the side of flexible substrate forms film;
(4) in the atmosphere of humidity, side flexible substrate with film is laid on target substrate in 30s;
(5) there is no the side of film with hairbrush extruding flexible substrate, get rid of the bubble between film and target substrate;
(6) when film is not dry, extrude rapidly flexible substrate and target substrate with extrusion machine, film is fully contacted with target substrate;
(7) with hand or tweezers, flexible substrate is slowly taken off, transferred on target substrate by flexible substrate by film.
Wherein, target substrate is PET substrate.Flexible substrate is water system CN-CA.The condition of step (1) drying treatment is: dry 4min at the temperature of 60 DEG C.The concrete steps of step (2) activation treatment are: under the condition of 90 DEG C, by target substrate (volume ratio of concentrated acid and hydrogen peroxide is 7: 3) brew 40min in the mixed solution of the vitriol oil and hydrogen peroxide.In step (3) to step (7), film is graphene oxide film.Step (3) is in Vacuum filtration device, on the side of flexible substrate, film forming concrete grammar was: by the graphene solution of 1mg/ml or graphene oxide solution under 15000 revs/min centrifugal 10 minutes, reduce one hour under the voltage of 20v subsequently, the solution of gained ammoniacal liquor is allocated to PH=10, carry out ultrasonic disperse again, then in Vacuum filtration device, in aperture be 0.5um flexible substrate on film forming.
Embodiment 6
A kind of transfer method of graphene film, graphene film is transferred to target substrate from flexible substrate, its technical process as shown in Figure 1, not air-dry film on flexible substrate is laid on target substrate, then the bubble between extrusion film and target substrate, then with extrusion machine extruding flexible substrate and target substrate, make film and target substrate close contact, then film is just molded on target substrate, now film is air-dry film, then take flexible substrate off, namely make air-dry adhesion of film on target substrate.The method comprises the following steps:
(1) decontamination, drying treatment are carried out to target substrate, for subsequent use;
(2) activation treatment is carried out to the target substrate processed through step (1), hydroxyl on the surface band making target substrate;
(3) in Vacuum filtration device, the side of flexible substrate forms film;
(4) in the atmosphere of humidity, side flexible substrate with film is laid on target substrate in 30s;
(5) there is no the side of film with hairbrush extruding flexible substrate, get rid of the bubble between film and target substrate;
(6) when film is not dry, extrude rapidly flexible substrate and target substrate with extrusion machine, film is fully contacted with target substrate;
(7) with hand or tweezers, flexible substrate is slowly taken off, transferred on target substrate by flexible substrate by film.
Wherein, target substrate is glass substrate.Flexible substrate is water system CN-CA.The condition of step (1) drying treatment is: dry 5min at the temperature of 50 DEG C.The concrete steps of step (2) activation treatment are: under the condition of 80 DEG C, by target substrate (volume ratio of concentrated acid and hydrogen peroxide is 7: 3) brew 45min in the mixed solution of the vitriol oil and hydrogen peroxide.In step (3) to step (7), film is graphene film.Step (3) is in Vacuum filtration device, on the side of flexible substrate, film forming concrete grammar was: by the graphene solution of 0.5mg/ml or graphene oxide solution under 12000 revs/min centrifugal 13 minutes, reduce one hour under the voltage of 20v subsequently, the solution of gained ammoniacal liquor is allocated to PH=10, carry out ultrasonic disperse again, then in Vacuum filtration device, in aperture be 0.3um flexible substrate on film forming.
Claims (6)
1. a transfer method for Graphene or graphene oxide film, transfer to target substrate by Graphene or graphene oxide film from flexible substrate, it is characterized in that, the method comprises the following steps:
(1) decontamination, drying treatment are carried out to target substrate, for subsequent use;
(2) activation treatment is carried out to the target substrate processed through step (1), hydroxyl on the surface band making target substrate;
(3) in Vacuum filtration device, the side of flexible substrate forms film;
(4) in the atmosphere of humidity, side flexible substrate with film is laid on target substrate in 30s;
(5) there is no the side of film with hairbrush extruding flexible substrate, get rid of the bubble between film and target substrate;
(6) when film is not dry, extrude rapidly flexible substrate and target substrate with extrusion machine, film is fully contacted with target substrate;
(7) flexible substrate is slowly taken off, transfer on target substrate by film by flexible substrate;
Film described in step (3) to step (7) is graphene film or graphene oxide film;
The concrete steps of the activation treatment described in step (2) are: under the condition of 70 ~ 90 DEG C, by target substrate brew 40min ~ 50min in the mixed solution of concentrated acid and hydrogen peroxide.
2. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film, is characterized in that, described target substrate is glass substrate or PET substrate.
3. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film, is characterized in that, described flexible substrate is polyvinylidene fluoride film or water system CN-CA.
4. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film, is characterized in that, the condition of the drying treatment described in step (1) is: dry 4 ~ 6min at the temperature of 40 ~ 60 DEG C.
5. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film, is characterized in that, described concentrated acid is the vitriol oil, and the volume ratio of concentrated acid and hydrogen peroxide is 7:3.
6. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film, it is characterized in that, described in step (3) in Vacuum filtration device, on the side of flexible substrate, film forming concrete grammar was: by the graphene solution of 0.05 ~ 1mg/ml or graphene oxide solution under 10000 ~ 15000 revs/min centrifugal 10 ~ 15 minutes, reduce one hour under the voltage of 20v subsequently, the solution of gained ammoniacal liquor is allocated to PH=10, carry out ultrasonic disperse again, then in Vacuum filtration device, in aperture be 0.2 ~ 0.5um flexible substrate on film forming.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104261402B (en) * | 2014-10-17 | 2016-03-02 | 中国科学院宁波材料技术与工程研究所 | A kind of transfer method of Graphene |
| CN104505148B (en) * | 2014-11-13 | 2017-09-29 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method of the three-dimensional coplanar shape graphene film of flexible base |
| CN104713761A (en) * | 2015-02-28 | 2015-06-17 | 安庆美晶新材料有限公司 | Method for obtaining single-layer or thin-layer two-dimensional material with high sample density through humidity control |
| CN105329884B (en) * | 2015-11-24 | 2017-05-24 | 东南大学 | Method for rapidly peeling and transferring graphene oxide leaching film to substrate |
| CN105609217B (en) * | 2016-02-22 | 2017-06-23 | 京东方科技集团股份有限公司 | A kind of graphene transparent electrode, its preparation method and display device |
| CN105948005B (en) * | 2016-05-19 | 2018-02-02 | 东南大学 | A kind of method using dimethyl silicone polymer fast transfer black phosphorus film |
| CN106006585B (en) * | 2016-05-19 | 2018-04-24 | 东南大学 | A kind of method using dimethyl silicone polymer fast transfer boron nitride pellicle |
| CN108821273B (en) * | 2018-09-21 | 2020-10-13 | 北京石墨烯研究院 | Vacuum graphene transfer device and vacuum graphene transfer method |
| CN109179396A (en) * | 2018-11-16 | 2019-01-11 | 福建闽烯科技有限公司 | The direct transfer device of graphene film and method |
| CN109437182B (en) * | 2018-12-25 | 2021-09-28 | 吉林大学 | Method for enhancing graphene oxide luminescence |
| CN110436449B (en) * | 2019-09-11 | 2020-11-17 | 西安交通大学 | Two-dimensional material transfer method based on electric auxiliary liquid bridge |
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