CN106158145A - A kind of preparation method of graphene conductive film - Google Patents
A kind of preparation method of graphene conductive film Download PDFInfo
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- CN106158145A CN106158145A CN201610465005.0A CN201610465005A CN106158145A CN 106158145 A CN106158145 A CN 106158145A CN 201610465005 A CN201610465005 A CN 201610465005A CN 106158145 A CN106158145 A CN 106158145A
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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Abstract
The invention discloses the preparation method of a kind of graphene conductive film, belong to conductive film production technical field.Said method comprising the steps of A. and deposit nickel thin layer: deposit nickel thin layer on the glass substrate；B. deposited graphite alkene thin layer: using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50～90 μm；C. clean, be dried: semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are carried out by graphene film layer dust technology, remove surface nickel thin layer, be then dried.It is low that the present invention has production cost, the advantage that efficiency is high.
Description
Technical field
The present invention relates to the preparation method of a kind of graphene conductive film, belong to conductive film production technical field.
Background technology
Along with the development of science and technology, the demand of new material is also got more and more by society.Material is human civilization progress
With the material base of development in science and technology, the renewal of material makes the life of people also there occurs great variety.At present, flourish new
Type transparent and conduction thin-film material at liquid crystal display, touch screen, smart window, solaode, microelectronics, information sensing
The fields such as device even military project are obtained for and are widely applied, and are penetrating in other sciemtifec and technical sphere.Due to thin film technique
Closely related with multiple technologies, thus excite the scientists of every field to film preparation and the interest of performance thereof.
Conductive film is a kind of energy conduction, realizes the thin film of some specific electric functions, is widely used in display, touches
Touch in the electronic devices such as screen and solaode.At present, as a kind of transparent and conducting semiconductor material tin indium oxide
(ITO), it is widely used in film applications always.By using magnetron sputtering evaporation ITO to prepare transparent leading over the transparent substrate
Conductive film, transparent base includes such as glass and polyethylene terephthalate (PET) thin film etc..Because tin indium oxide has height
Electrical conductivity, high pass light rate, so becoming one of main material preparing conductive film.But, tin indium oxide conductive film makes
There is also some shortcomings during with, including: (1) indium resource is less, causes price continuous rise so that ITO becomes the most high
Expensive material, such as spraying, pulsed laser deposition, plating etc..And Indium sesquioxide. has certain toxicity, recycle unreasonable easily causing
Environmental pollution.(2) characteristic crisp for ITO makes it can not meet some new opplication (the most flexible flexible display, touch
Screen, organic solar batteries) performance requirement, be not suitable for the production of flexible electronic device of future generation.The two of Graphene uniqueness
Dimension crystal structure, imparts the performance of its uniqueness, and research finds, Graphene has the electrical property of excellent mechanical performance and excellence
Matter, under room temperature, the electron mobility of Graphene is up to 15000cm2v-1s-1, and resistivity is only 10-6Ωcm.Graphene is being permitted
Many-sided have more potential advantage than tin indium oxide, such as quality, robustness, pliability, chemical stability, infrared light transmission
Property and price etc..Therefore Graphene is expected to replace tin indium oxide very much, is used for developing thinner, the conduction faster flexible electronic of speed
Device.
At present, the preparation method of Graphene mainly has: micromechanics stripping method, oxidation-reduction method, chemical vapour deposition technique, have
Machine molecule intercalation method etc..Chemical vapour deposition technique is used by Somani etc. from 2006, with camphanone (Camphora) as presoma,
Obtaining graphene film on nickel foil, scientists achieves and much obtains grinding of thickness controllable grapheme lamella in different matrix
Study carefully progress.By carrying out chemical etching on metallic matrix, graphene sheet layer is separated and transfers on another matrix, and this is just
Eliminate complicated machinery or chemical treatment method and obtain high-quality graphene sheet layer.The states such as Korea S and Japan adopt one after another
Prepared big size graphene transparent conductive film in this way, it is desirable to main application fields be in flat-panel screens
On, serve as anode.The such as exploitation in new OLED (OLED), OLED has low cost, all solid state, main
Move luminescence, brightness height, contrast height, visual angle width, fast response time, thickness are thin, low-voltage direct-current drives, low in energy consumption, work temperature
Spend wide ranges, the features such as soft screen shows can be realized, become the developing direction of future display technology.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of new graphene conductive film, production cost is low, and energy
Produce large-area graphene conductive film, it is possible to meet the demand of large-scale production.
In order to realize foregoing invention purpose, technical scheme is as follows:
A kind of preparation method of graphene conductive film, it is characterised in that: comprise the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum: 5
×10-5～2 × 10-4Pa, underlayer temperature 50～80 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50～90 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
In order to the present invention is better achieved, further, in step A, the pressure of described sputtering is 2Pa.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2；The temperature of deposition
Degree is 580～650 DEG C, and the pressure of deposition is 1 × 10-4～2 × 10-4Pa。
In step C, described cleaning refers to, with dilute nitric acid solution, the semi-finished product after cooling are soaked 1～3h, described dust technology
Mass concentration be 35～45%.
In step C, described dry condition is to be dried 20～40min at 110～130 DEG C.
The light transmittance of the graphene conductive film that the present invention prepares is 79～83%, assay method: use U-3010 type purple
Outward-visible spectrophotometer, with blank slide as reference, measures the saturating of graphene film in 400-900nm wave-length coverage
Light rate, and using the light transmittance at wavelength X=550nm as the light transmittance of graphene film.
The resistance of the graphene conductive film that the present invention prepares is 1.0～1.5M Ω/sq, assay method: use SB100A/
The film resistor of graphene film on 2 type four-point probe test slide base materials, the distance between probe is 3mm.
Beneficial effects of the present invention:
Compared with prior art, the present invention breaches the restriction of original technology, it is achieved that transparent graphene conductive film in reality
Test the leap to the large scale application of industrial applications of the indoor small size, there is production cost low, the advantage that efficiency is high, and this
Invent by further parameter optimization, furthermore achieved that prepared conductive film visible light transmittance rate is high, surface cleaning without
Polluting, pliability is good, and image shows effect clearly, is especially suitable for large-scale production, is expected to substitute tradition inorganic oxide electricity
Pole material ITO, promotes the development of graphene conductive film industry, has preferable economic benefit and social benefit.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of graphene conductive film, comprises the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum: 5
×10-5Pa, underlayer temperature 50 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
Embodiment 2
The preparation method of a kind of graphene conductive film, comprises the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum: 2
×10-4Pa, underlayer temperature 80 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 90 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
Embodiment 3
The preparation method of a kind of graphene conductive film, comprises the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum:
1.5×10-4Pa, underlayer temperature 60 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 60 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
In the present embodiment, in step A, the pressure of described sputtering is 2Pa.
Embodiment 4
The present embodiment is on the basis of embodiment 3, and in step B, during described CVD deposited graphite alkene thin layer, carbon source is
Methane, gas is H2；The temperature of deposition is 580 DEG C, and the pressure of deposition is 1 × 10-4Pa。
Embodiment 5
The preparation method of a kind of graphene conductive film, comprises the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum: 8
×10-5Pa, underlayer temperature 50 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 90 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
In the present embodiment, in step A, the pressure of described sputtering is 2Pa.
The present embodiment is on the basis of embodiment 3, in step B, during described CVD deposited graphite alkene thin layer, and carbon
Source is methane, and gas is H2；The temperature of deposition is 650 DEG C, and the pressure of deposition is 2 × 10-4Pa。
In step C, described cleaning refers to, with dilute nitric acid solution, the semi-finished product after cooling are soaked 1h, the matter of described dust technology
Amount concentration is 35%.
Embodiment 6
The preparation method of a kind of graphene conductive film, comprises the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum: 2
×10-4Pa, underlayer temperature 50 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
In the present embodiment step A, the pressure of described sputtering is 2Pa.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2；The temperature of deposition
Degree is 600 DEG C, and the pressure of deposition is 1.5 × 10-4Pa。
In step C, described cleaning refers to, with dilute nitric acid solution, the semi-finished product after cooling are soaked 3h, the matter of described dust technology
Amount concentration is 45%.
In step C, described dry condition is to be dried 20min at 130 DEG C.Embodiment 7
The preparation method of a kind of graphene conductive film, comprises the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum 8 ×
10-5Pa, underlayer temperature 78 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 60 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
In the present embodiment step A, the pressure of described sputtering is 2Pa.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2；The temperature of deposition
Degree is 620 DEG C, and the pressure of deposition is 1.2 × 10-4Pa。
In step C, described cleaning refers to, with dilute nitric acid solution, the semi-finished product after cooling are soaked 3h, the matter of described dust technology
Amount concentration is 40%.
In step C, described dry condition is to be dried 40min at 110 DEG C.
The light transmittance of the graphene conductive film that the present embodiment prepares is 79%；Resistance is 1.0M Ω/sq.
The assay method of light transmittance: use U-3010 type ultraviolet-visible spectrophotometer, with blank slide as reference,
The light transmittance of graphene film is measured in 400-900nm wave-length coverage, and using the light transmittance at wavelength X=550nm as stone
The light transmittance of ink alkene thin film.
The assay method of resistance: use graphene film on SB100A/2 type four-point probe test slide base material
Film resistor, the distance between probe is 3mm.
Embodiment 8
The preparation method of a kind of graphene conductive film, comprises the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum: 8
×10-5Pa, underlayer temperature 50 DEG C.
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 90 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
In the present embodiment step A, the pressure of described sputtering is 2Pa.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2；The temperature of deposition
Degree is 600 DEG C, and the pressure of deposition is 1.4 × 10-4Pa。
In step C, described cleaning refers to, with dilute nitric acid solution, the semi-finished product after cooling are soaked 3h, the matter of described dust technology
Amount concentration is 43%.
In step C, described dry condition is to be dried 40min at 110 DEG C.
The light transmittance of the graphene conductive film that the present embodiment prepares is 83%；Resistance is 1.5M Ω/sq.
The assay method of light transmittance: use U-3010 type ultraviolet-visible spectrophotometer, with blank slide as reference,
The light transmittance of graphene film is measured in 400-900nm wave-length coverage, and using the light transmittance at wavelength X=550nm as stone
The light transmittance of ink alkene thin film.
The assay method of resistance: use graphene film on SB100A/2 type four-point probe test slide base material
Film resistor, the distance between probe is 3mm.
Claims (7)
1. the preparation method of a graphene conductive film, it is characterised in that: comprise the following steps:
A. deposition nickel thin layer
Deposition nickel thin layer on the glass substrate；The method of described deposition nickel thin layer is magnetron sputtering method, background vacuum: 5
×10-5～2 × 10-4Pa, underlayer temperature 50～80 DEG C；
B. deposited graphite alkene thin layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50～90 μm；
C. post processing
Semi-finished product step B obtained carry out cooling process, after temperature is down to room temperature, are entered by graphene film layer dust technology
Row cleans, and removes surface nickel thin layer, is then dried and i.e. obtains described graphene conductive film.
The preparation method of a kind of graphene conductive film the most as claimed in claim 1, it is characterised in that: in step A, described in spatter
The pressure penetrated is 2Pa.
The preparation method of a kind of graphene conductive film the most as claimed in claim 1, it is characterised in that: in step B, described
During CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2；The temperature of deposition is 580～650 DEG C, deposition
Pressure is 1 × 10-4～2 × 10-4Pa。
The preparation method of a kind of graphene conductive film the most as claimed in claim 1, it is characterised in that: in step C, described clearly
Washing and refer to, with dilute nitric acid solution, the semi-finished product after cooling are soaked 1～3h, the mass concentration of described dust technology is 35～45%.
The preparation method of a kind of graphene conductive film the most as claimed in claim 1, it is characterised in that: in step C, described dry
Dry condition is to be dried 20～40min at 110～130 DEG C.
6. the preparation method of a kind of graphene conductive film as described in any one of Claims 1 to 5, it is characterised in that: described
The light transmittance of graphene conductive film is 79～83%, assay method: use U-3010 type ultraviolet-visible spectrophotometer, with sky
White microscope slide is reference, measures the light transmittance of graphene film in 400-900nm wave-length coverage, and with at wavelength X=550nm
The light transmittance at place is as the light transmittance of graphene film.
7. the preparation method of a kind of graphene conductive film as described in any one of Claims 1 to 5, it is characterised in that: described
The resistance of graphene conductive film is 1.0～1.5M Ω/sq, assay method: use the test of SB100A/2 type four-point probe
The film resistor of graphene film on microscope slide base material, the distance between probe is 3mm.
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| CN107887076A (en) * | 2017-10-27 | 2018-04-06 | 成都天航智虹知识产权运营管理有限公司 | A kind of preparation method of graphene conductive film |
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| CN107887076A (en) * | 2017-10-27 | 2018-04-06 | 成都天航智虹知识产权运营管理有限公司 | A kind of preparation method of graphene conductive film |
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