CN103072976A - 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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- CN103072976A CN103072976A CN2012105877805A CN201210587780A CN103072976A CN 103072976 A CN103072976 A CN 103072976A CN 2012105877805 A CN2012105877805 A CN 2012105877805A CN 201210587780 A CN201210587780 A CN 201210587780A CN 103072976 A CN103072976 A CN 103072976A
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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 the 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 on the target substrate from the preparation substrate specifically.
Background technology
Badeker in 1907 etc. utilize sputtering method to prepare CdO transparent conductive film (Transparentconducting films, TCFs).The electrically conducting transparent multilayer film of the ITO that the sixties has been experienced in the research of TCFs (the In2O3 base film that Sn mixes), the seventies and the ZnO that mixes the eighties.Along with the progress of science and technology and the discovery of novel material, novel carbon nanotube TCFs, Graphene TCFs have appearred in recent years.After Graphene was successfully prepared in 2004, than present industrial widely used ITO, the FTO (SnO that F mixes
2Base film) and AZO (Al mix zno-based film) material, have transmittance height (theoretical value is 97.5%), the characteristics such as snappiness is good, weather resistance is high, aboundresources are incorporated into rapidly in the function film field.
The preparation method of graphene film mainly contains chemical Vapor deposition process, vacuum filtration method, spin-coating method, self-assembly etc.Owing to studies show that in single-layer graphene λ=300-2500nm spectral range in a large number, its interband absorbs and 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 increases by 2.3% opaqueness approximately.The mobility of room temperature download stream can reach 15000cm
2More than/the Vs, can be observed quantum hall effect under the normal temperature simultaneously.Because its unique photoelectric characteristic of Graphene has determined that graphene film can be applicable to electroluminescent device, plane liquid-crystal display, Organic Light Emitting Diode, dyes the fields such as sensitization solar battery, sensor, smart window.
At present both at home and abroad after using flexible substrate to carry out film forming, transfer to target substrate from the preparation substrate and generally adopt chemical method, its technological process is to exert pressure for some time first, then adopt the flexible substrate material that dissolves former graphene film, with organic solvent film is being carried out flushing for several times at last.Though the method can effectively realize the transfer of film, but its complex technical process is time-consuming, has introduced simultaneously the performance of organic impurity influence film, especially in the process of using a large amount of organic solvents, not only wasted resource, and can damage human body and environment.Be difficult to satisfy the demand of large-scale industrialization preparation.Simultaneously, also the someone adopts film was placed 45 ℃ of vacuum drying ovens dry 24 hours together with flexible substrate, then film is taken off from flexible base, board, is shifting.The method migration period is long, and higher to technical requirements in taking off the process of film.Be difficult to equally satisfy the demand of large-scale industrialization preparation.
Summary of the invention
Purpose of the present invention is exactly a kind of simple to operate, favorable reproducibility is provided in order to overcome the defective that above-mentioned prior art exists, does not introduce impurity, does not use the Graphene of organic substance or the transfer method of graphene oxide film.
Purpose of the present invention can be achieved through the following technical solutions:
Different in kind according to the reactive force that adsorbs molecule and solid surface can be divided into absorption physical adsorption and chemisorption.Do not have transfer transport in adsorption process, 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 the chemisorption, chemical reaction has occured in absorption molecule and solid surface, and its reactive force is similar with the reactive force between the compound Atom.The substrate surfaces such as the glass of processing through the vitriol oil and hydrogen peroxide, PET make on its surface band-OH, and the inadequate graphene oxide lamella of graphene oxide and reduction peripheral zone has-COOH, esterification can occur with-COOH in-OH, so that substrate and graphene film link by chemical bond, and be simple physical adsorption between graphene film and the preparation flexible substrate.Because chemical bonding force will be much larger than Van der Waals force, thereby realized effective transfer of graphene film.Simultaneously, silicate is during as target base plate, and graphene oxide is electronegative, and the easy positively charged of most of silicate surfaces.Molecular structure such as glass is more special, it is very weak to the constraint ability (magnetism) of electronics, when glass contacted with other materials and rubs, other attracted the molecule of the stronger material of electronic capability to seize the electronics of glass surface molecule, make it be with positive electricity.Heterocharge attracts each other and also is conducive to the transfer of graphene film.
The transfer method of a kind of Graphene or graphene oxide film is transferred to Graphene or graphene oxide film on the target substrate from flexible substrate, and the method may further comprise the steps:
(1) target substrate is carried out decontamination, drying treatment, for subsequent use;
(2) target substrate of processing through step (1) is carried out activation treatment, make hydroxyl on the surface band of target substrate;
(3) in the vacuum filtration device, form film in a side of flexible substrate;
(4) in the atmosphere of humidity, a side that flexible substrate is had film is tiled on the target substrate in 30s;
(5) push the side that flexible substrate does not have film with hairbrush, get rid of the bubble between film and the target substrate;
When (6) treating that film is not dried, push 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, be about to film and transferred on the target substrate by flexible substrate.
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 described drying treatment of step (1) is: dry 4～6min under 40～60 ℃ the temperature.
The concrete steps of the described activation treatment of step (2) are: under 70～90 ℃ condition, target substrate is boiled bubble 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.
Step (3) to the film described in the step (7) is graphene film or graphene oxide film.
Step (3) is described in the vacuum filtration device, film forming concrete grammar is on a side of flexible substrate: graphene solution or the graphene oxide solution of 0.05～1mg/ml were descended centrifugal 10～15 minutes at 10000～15000 rev/mins, under the voltage of 20v, reduced one hour subsequently, the solution of gained is allocated to PH=10 with ammoniacal liquor, carry out again ultra-sonic dispersion, then in the vacuum filtration device, be film forming on the flexible substrate of 0.2～0.5um in the aperture.
Compared with prior art, the present invention has the following advantages:
(1) compare with the complicated time-consuming method of tradition, the present invention adopts micromechanics to shift and can finish in tens seconds, has simple, timesaving characteristics.
(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 have to use the organic substance to environment and human body harmful.Not only reduce the injury to environment and human body, and reduced 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, has further reduced cost.
(5) not only cost of transfer is low for the method, and has processing ease, favorable reproducibility, and suitability is strong.
Description of drawings
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the structural representation of extrusion machine;
Fig. 3 is that graphene oxide film is transferred to scanning electron microscope image on the glass substrate among the embodiment 1;
Fig. 4 is that graphene film is transferred to scanning electron microscope image on the glass substrate among the embodiment 2.
Among the figure, 1 is support, and 2 is motor driven compressor, and 3 is extruding disk, and 4 is pole, and 5 is chute.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Graphene oxide film is transferred on the glass substrate
Shown in Fig. 1 schema, not air-dry film on the flexible substrate is tiled on the target substrate, then the bubble between extrusion film and the target substrate, then with extrusion machine extruding flexible substrate and target substrate, so that film and target substrate close contact, then film just is molded on the target substrate, and this moment, film was air-dry film, then take flexible substrate off, namely so that air-dry adhesion of film on target substrate.
The graphene oxide solution of 1mg/ml is turned lower centrifugal 10 minutes 14000, subsequently reduction one hour under the voltage of 20v, with the solution of gained allocate with ammoniacal liquor its PH=10 carry out ultrasonic from new dispersion.Be to be tiled in 0.25um polyvinylidene fluoride film film forming in the vacuum filtration device on the glass substrate at first rapidly with the one side of film take the aperture; When treating that film is not dried, then suitably push the eliminating bubble with brush first, be placed on subsequently in the extrusion machine as shown in Figure 2 and push, after to be extruded the finishing, throw off polyvinylidene fluoride film with hand or tweezers, can realize the transfer of oxidation graphene film.Forcing machine shown in Figure 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, the left and right sides 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 that graphene oxide film is transferred to the scanning electron microscope image on the glass substrate, and when using tranfer system of the present invention, resulting film is even, integrity is better as can be seen from Figure, and the shape characteristic of film can be found out clearly.
Graphene film is transferred on the glass substrate
Shown in Fig. 1 schema, be that 0.45um water system CN-CA is film forming in the vacuum filtration device of flexible substrate in the aperture with the graphene oxide solution of .1mg/ml at first; Then will there be rapidly film from the vacuum filtration device, to take off gently, will has the one side of film to be tiled in rapidly on the glass substrate; When treating that film is not dried, then suitably push the eliminating bubble with brush rapidly, be placed on subsequently in the extrusion machine such as Fig. 2 and push, after to be extruded the finishing, throw off CN-CA with hand or tweezers, can realize the transfer of graphene oxide film.Fig. 4 is that graphene film is transferred to the scanning electron microscope image on the glass substrate, and when using tranfer system of the present invention, resulting film is even, integrity is better as can be seen from Figure, and the shape characteristic of film can be found out clearly.
Graphene oxide film is transferred on the flexible base, board PET.
Shown in Fig. 1 schema, be that 0.25um water system CN-CA is film forming in the vacuum filtration device of flexible substrate in the aperture with the graphene oxide solution of 0.05mg/ml at first; Then will there be rapidly film from the vacuum filtration device, to take off gently, will has the one side of film to be tiled in rapidly on the pet substrate; When treating that film is not dried, then suitably push the eliminating bubble with brush rapidly, be placed on subsequently in the extrusion machine such as Fig. 2 and push, after to be extruded the finishing, throw off CN-CA with hand or tweezers, can realize the transfer of graphene oxide film.
A kind of transfer method of graphene film, graphene film is transferred on the target substrate from flexible substrate, its technical process as shown in Figure 1, not air-dry film on the flexible substrate is tiled on the target substrate, then the bubble between extrusion film and the target substrate, then with extrusion machine extruding flexible substrate and target substrate, so that film and target substrate close contact, then film just is molded on the target substrate, this moment, film was air-dry film, then take flexible substrate off, namely so that air-dry adhesion of film on target substrate.The method may further comprise the steps:
(1) target substrate is carried out decontamination, drying treatment, for subsequent use;
(2) target substrate of processing through step (1) is carried out activation treatment, make hydroxyl on the surface band of target substrate;
(3) in the vacuum filtration device, form film in a side of flexible substrate;
(4) in the atmosphere of humidity, a side that flexible substrate is had film is tiled on the target substrate in 30s;
(5) push the side that flexible substrate does not have film with hairbrush, get rid of the bubble between film and the target substrate;
When (6) treating that film is not dried, push 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, be about to film and transferred on the target substrate by flexible substrate.
Wherein, target substrate is glass substrate.Flexible substrate is polyvinylidene fluoride film.The condition of step (1) drying treatment is: dry 6min under 40 ℃ the temperature.The concrete steps of step (2) activation treatment are: under 70 ℃ condition, target substrate (volume ratio of concentrated acid and hydrogen peroxide is 7: 3) in the mixed solution of the vitriol oil and hydrogen peroxide is boiled bubble 50min.Step (3) to the middle film of step (7) is graphene film.Step (3) is in the vacuum filtration device, film forming concrete grammar is on a side of flexible substrate: graphene solution or the graphene oxide solution of 0.05mg/ml were descended centrifugal 15 minutes at 10000 rev/mins, under the voltage of 20v, reduced one hour subsequently, the solution of gained is allocated to PH=10 with ammoniacal liquor, carry out again ultra-sonic dispersion, then in the vacuum filtration device, be film forming on the flexible substrate of 0.2um in the aperture.
A kind of transfer method of graphene oxide film, graphene oxide film is transferred on the target substrate from flexible substrate, its technical process as shown in Figure 1, not air-dry film on the flexible substrate is tiled on the target substrate, then the bubble between extrusion film and the target substrate, then with extrusion machine extruding flexible substrate and target substrate, so that film and target substrate close contact, then film just is molded on the target substrate, this moment, film was air-dry film, then take flexible substrate off, namely so that air-dry adhesion of film on target substrate.The method may further comprise the steps:
(1) target substrate is carried out decontamination, drying treatment, for subsequent use;
(2) target substrate of processing through step (1) is carried out activation treatment, make hydroxyl on the surface band of target substrate;
(3) in the vacuum filtration device, form film in a side of flexible substrate;
(4) in the atmosphere of humidity, a side that flexible substrate is had film is tiled on the target substrate in 30s;
(5) push the side that flexible substrate does not have film with hairbrush, get rid of the bubble between film and the target substrate;
When (6) treating that film is not dried, push 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, be about to film and transferred on the target substrate by flexible substrate.
Wherein, target substrate is the PET substrate.Flexible substrate is the water system CN-CA.The condition of step (1) drying treatment is: dry 4min under 60 ℃ the temperature.The concrete steps of step (2) activation treatment are: under 90 ℃ condition, target substrate (volume ratio of concentrated acid and hydrogen peroxide is 7: 3) in the mixed solution of the vitriol oil and hydrogen peroxide is boiled bubble 40min.Step (3) to the middle film of step (7) is graphene oxide film.Step (3) is in the vacuum filtration device, film forming concrete grammar is on a side of flexible substrate: graphene solution or the graphene oxide solution of 1mg/ml were descended centrifugal 10 minutes at 15000 rev/mins, under the voltage of 20v, reduced one hour subsequently, the solution of gained is allocated to PH=10 with ammoniacal liquor, carry out again ultra-sonic dispersion, then in the vacuum filtration device, be film forming on the flexible substrate of 0.5um in the aperture.
Embodiment 6
A kind of transfer method of graphene film, graphene film is transferred on the target substrate from flexible substrate, its technical process as shown in Figure 1, not air-dry film on the flexible substrate is tiled on the target substrate, then the bubble between extrusion film and the target substrate, then with extrusion machine extruding flexible substrate and target substrate, so that film and target substrate close contact, then film just is molded on the target substrate, this moment, film was air-dry film, then take flexible substrate off, namely so that air-dry adhesion of film on target substrate.The method may further comprise the steps:
(1) target substrate is carried out decontamination, drying treatment, for subsequent use;
(2) target substrate of processing through step (1) is carried out activation treatment, make hydroxyl on the surface band of target substrate;
(3) in the vacuum filtration device, form film in a side of flexible substrate;
(4) in the atmosphere of humidity, a side that flexible substrate is had film is tiled on the target substrate in 30s;
(5) push the side that flexible substrate does not have film with hairbrush, get rid of the bubble between film and the target substrate;
When (6) treating that film is not dried, push 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, be about to film and transferred on the target substrate by flexible substrate.
Wherein, target substrate is glass substrate.Flexible substrate is the water system CN-CA.The condition of step (1) drying treatment is: dry 5min under 50 ℃ the temperature.The concrete steps of step (2) activation treatment are: under 80 ℃ condition, target substrate (volume ratio of concentrated acid and hydrogen peroxide is 7: 3) in the mixed solution of the vitriol oil and hydrogen peroxide is boiled bubble 45min.Step (3) to the middle film of step (7) is graphene film.Step (3) is in the vacuum filtration device, film forming concrete grammar is on a side of flexible substrate: graphene solution or the graphene oxide solution of 0.5mg/ml were descended centrifugal 13 minutes at 12000 rev/mins, under the voltage of 20v, reduced one hour subsequently, the solution of gained is allocated to PH=10 with ammoniacal liquor, carry out again ultra-sonic dispersion, then in the vacuum filtration device, be film forming on the flexible substrate of 0.3um in the aperture.
Claims (8)
1. the transfer method of a Graphene or graphene oxide film is transferred to Graphene or graphene oxide film on the target substrate from flexible substrate, it is characterized in that the method may further comprise the steps:
(1) target substrate is carried out decontamination, drying treatment, for subsequent use;
(2) target substrate of processing through step (1) is carried out activation treatment, make hydroxyl on the surface band of target substrate;
(3) in the vacuum filtration device, form film in a side of flexible substrate;
(4) in the atmosphere of humidity, a side that flexible substrate is had film is tiled on the target substrate in 30s;
(5) push the side that flexible substrate does not have film with hairbrush, get rid of the bubble between film and the target substrate;
When (6) treating that film is not dried, push rapidly flexible substrate and target substrate with extrusion machine, film is fully contacted with target substrate;
(7) flexible substrate is slowly taken off, be about to film and transferred on the target substrate by flexible substrate.
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 described drying treatment of step (1) is: dry 4～6min under 40～60 ℃ the temperature.
5. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film, it is characterized in that, the concrete steps of the described activation treatment of step (2) are: under 70～90 ℃ condition, target substrate is boiled bubble 40min～50min in the mixed solution of concentrated acid and hydrogen peroxide.
6. the transfer method of a kind of Graphene according to claim 5 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.
7. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film is characterized in that, step (3) to the film described in the step (7) is graphene film or graphene oxide film.
8. the transfer method of a kind of Graphene according to claim 1 or graphene oxide film, it is characterized in that, step (3) is described in the vacuum filtration device, film forming concrete grammar is on a side of flexible substrate: graphene solution or the graphene oxide solution of 0.05～1mg/ml were descended centrifugal 10～15 minutes at 10000～15000 rev/mins, under the voltage of 20v, reduced one hour subsequently, the solution of gained is allocated to PH=10 with ammoniacal liquor, carry out again ultra-sonic dispersion, then in the vacuum filtration device, be film forming on the flexible substrate of 0.2～0.5um in the aperture.
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| CN108821273A (en) * | 2018-09-21 | 2018-11-16 | 北京石墨烯研究院 | Vacuum graphite alkene transfer device and vacuum graphite alkene 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 |
| CN109437182A (en) * | 2018-12-25 | 2019-03-08 | 吉林大学 | A method of enhancing graphene oxide shines |
| CN109437182B (en) * | 2018-12-25 | 2021-09-28 | 吉林大学 | Method for enhancing graphene oxide luminescence |
| CN110436449A (en) * | 2019-09-11 | 2019-11-12 | 西安交通大学 | A kind of two-dimensional material transfer method based on electricity auxiliary liquid bridge |
| 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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