CN105931757A - Method for preparing conductive thin film - Google Patents
Method for preparing conductive thin film Download PDFInfo
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- CN105931757A CN105931757A CN201610464549.5A CN201610464549A CN105931757A CN 105931757 A CN105931757 A CN 105931757A CN 201610464549 A CN201610464549 A CN 201610464549A CN 105931757 A CN105931757 A CN 105931757A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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 a method for preparing a conductive thin film, and belongs to the technical field of conductive thin film production. The method comprises the following steps of A, depositing a nickel layer: depositing a nickel thin film layer with a thickness which is equal to that of 1-2 nickel atoms on a glass substrate; B, depositing a graphene layer: depositing a graphene thin film layer by a CVD method, wherein the graphene thin film layer is 40-60[mu]m in thickness; in the CVD method deposition process, methane is used as the carbon source; the gas is a mixed gas of H<2> and He at a volume ratio of 2-5 to 1; and the volume ratio of methane to the mixed gas is 8-10 to 1; and C, cleaning and drying: reducing the temperature of the semifinished product obtained in the step B, then cleaning the graphene thin film layer after the temperature is reduced to the room temperature, next, removing the nickel thin film layer from the surface, and drying. Detection proves that the light transmittance of the conductive thin film prepared by the invention is greater than or equal to 85%. Compared with the prior art, the conductive thin film prepared by the invention has the advantages of low production cost, simple preparation method and high light transmittance.
Description
Technical field
The present invention relates to a kind of method preparing 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 a kind of new method preparing conductive film, production cost is low, and method is simple, thoroughly
Light rate is high, and can 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 method preparing conductive film, it is characterised in that: comprise the following steps:
A. deposited nickel layer
Substrate of glass clean, that be dried deposits the nickel thin layer that 1～2 nickle atom is thick；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 40～60 μm；Described CVD deposits
During, carbon source is methane, gas be volume ratio be the H of 2～5:12Mixed gas with He；Described methane and mixed gas
Volume ratio is 8～10:1；
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,
Remove surface nickel thin layer, be then dried；
Light transmittance >=85% of described conductive film.
In order to the present invention is better achieved, further, in step A, the method for described deposited nickel layer is magnetron sputtering method,
Background vacuum: 5 × 10-5～2 × 10-4Pa, sputtering pressure 3～5Pa, underlayer temperature 30～70 DEG C.
In step B, in step B, during described CVD deposited graphite alkene thin layer, the temperature of deposition is 750～850
DEG C, the pressure of deposition is 1 × 10-4～2 × 10-4Pa。
In step C, described cleaning refers to, with weak acid solution, the semi-finished product after cooling are soaked 1～3h.
In step C, described dry condition is to be dried 5～10min at 110～130 DEG C.
Beneficial effects of the present invention:
The present invention breaches the restriction of original technology, it is achieved that graphene conductive film small size in laboratory to industry
Changing the leap of the large scale application of application, compared with prior art, have production cost low, preparation method is simple, advantage, and this
Invent by further parameter optimization, furthermore achieved that prepared conductive film visible light transmittance rate is high, after testing, this
Light transmittance >=85% of bright prepared graphene conductive film, and surface cleaning is pollution-free, pliability is good, and image shows clearly
Effect, is suitable for large-scale production, has preferable economic benefit and social benefit.
Detailed description of the invention
Embodiment 1
A kind of method preparing conductive film, comprises the following steps:
A. deposited nickel layer
Substrate of glass clean, that be dried deposits the nickel thin layer that 1～2 nickle atom is thick；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 40 μm；Described CVD deposition process
In, carbon source is methane, gas be volume ratio be the H of 2:12Mixed gas with He；Described methane and the volume ratio of mixed gas
For 8:1；
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,
Remove surface nickel thin layer, be then dried；
After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.7%.
Embodiment 2
A kind of method preparing conductive film, comprises the following steps:
A. deposited nickel layer
Substrate of glass clean, that be dried deposits the nickel thin layer that 1～2 nickle atom is thick；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 60 μm；Described CVD deposition process
In, carbon source is methane, gas be volume ratio be the H of 5:12Mixed gas with He；Described methane and the volume ratio of mixed gas
For 10:1；
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,
Remove surface nickel thin layer, be then dried；
After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.2%.
Embodiment 3
A kind of method preparing conductive film, comprises the following steps:
A. deposited nickel layer
Substrate of glass clean, that be dried deposits the nickel thin layer that 1～2 nickle atom is thick；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 55 μm；Described CVD deposition process
In, carbon source is methane, gas be volume ratio be the H of 3:12Mixed gas with He；Described methane and the volume ratio of mixed gas
For 9:1；
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,
Remove surface nickel thin layer, be then dried；
After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.1%.
In the present embodiment step A, the method for described deposited nickel layer is magnetron sputtering method, background vacuum: 5 × 10-5Pa, spatters
Injection pressure 3Pa, underlayer temperature 30 DEG C.After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.4%.
Embodiment 4
The present embodiment is with the difference of embodiment 3: in step A, and the method for described deposited nickel layer is magnetron sputtering method, and background is true
Reciprocal of duty cycle is 2 × 10-4Pa, sputtering pressure 5Pa, underlayer temperature 70 DEG C.
After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.3%.
Embodiment 5
A kind of method preparing conductive film, comprises the following steps:
A. deposited nickel layer
Substrate of glass clean, that be dried deposits the nickel thin layer that 1～2 nickle atom is thick；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 45 μm；Described CVD deposition process
In, carbon source is methane, gas be volume ratio be the H of 4:12Mixed gas with He；Described methane and the volume ratio of mixed gas
For 10:1；
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,
Remove surface nickel thin layer, be then dried；
In the present embodiment step A, the method for described deposited nickel layer is magnetron sputtering method, and background vacuum is 1 × 10-4Pa, sputtering
Pressure 4Pa, underlayer temperature 55 DEG C.
In step B, during described CVD deposited graphite alkene thin layer, the temperature of deposition is 750 DEG C, the pressure of deposition
It is 1 × 10-4Pa。
After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.3%.
Embodiment 6
A kind of method preparing conductive film, comprises the following steps:
A. deposited nickel layer
Substrate of glass clean, that be dried deposits the nickel thin layer that 1～2 nickle atom is thick；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 45 μm；Described CVD deposition process
In, carbon source is methane, gas be volume ratio be the H of 2:12Mixed gas with He；Described methane and the volume ratio of mixed gas
For 9:1；
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,
Remove surface nickel thin layer, be then dried；
In the present embodiment step A, the method for described deposited nickel layer is magnetron sputtering method, and background vacuum is 1 × 10-4Pa, sputtering
Pressure 4Pa, underlayer temperature 70 DEG C.
In step B, during described CVD deposited graphite alkene thin layer, the temperature of deposition is 850 DEG C, the pressure of deposition
It is 2 × 10-4Pa。
In step C, described cleaning refers to, with weak acid solution, the semi-finished product after cooling are soaked 1h.
In step C, described dry condition is to be dried 5min at 130 DEG C.
After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.5%.
Embodiment 7
The present embodiment has the difference of embodiment 8 to be:
In step C, described cleaning refers to, with weak acid solution, the semi-finished product after cooling are soaked 3h.
In step C, described dry condition is to be dried 10min at 110 DEG C.
After testing, the light transmittance of the conductive film that the present embodiment prepares is 85.7%.
Claims (5)
1. the method preparing conductive film, it is characterised in that: comprise the following steps:
A. deposited nickel layer
Substrate of glass clean, that be dried deposits the nickel thin layer that 1～2 nickle atom is thick；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 40～60 μm；Described CVD deposits
During, carbon source is methane, gas be volume ratio be the H of 2～5:12Mixed gas with He；Described methane and mixed gas
Volume ratio is 8～10:1；
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,
Remove surface nickel thin layer, be then dried；
Light transmittance >=85% of described conductive film.
A kind of method preparing conductive film, it is characterised in that: in step A, described deposited nickel layer
Method be magnetron sputtering method, background vacuum: 5 × 10-5～2 × 10-4Pa, sputtering pressure 3～5Pa, underlayer temperature 30～70
℃。
A kind of method preparing conductive film, it is characterised in that: in step B, described CVD is sunk
During long-pending Graphene thin layer, the temperature of deposition is 750～850 DEG C, and the pressure of deposition is 1 × 10-4～2 × 10-4Pa。
A kind of method preparing conductive film, it is characterised in that: in step C, described cleaning refers to
With weak acid solution, the semi-finished product after cooling are soaked 1～3h.
5. a kind of method preparing conductive film as described in any one of Claims 1 to 4, it is characterised in that: in step C, institute
Stating dry condition is to be dried 5～10min at 110～130 DEG C.
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| CN201610464549.5A CN105931757A (en) | 2016-06-24 | 2016-06-24 | Method for preparing conductive thin film |
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| CN201610464549.5A CN105931757A (en) | 2016-06-24 | 2016-06-24 | Method for preparing conductive thin film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107732013A (en) * | 2017-10-27 | 2018-02-23 | 成都天航智虹知识产权运营管理有限公司 | A kind of preparation method of conductive film |
| CN107799233A (en) * | 2017-10-27 | 2018-03-13 | 成都天航智虹知识产权运营管理有限公司 | A kind of method for preparing conductive film |
| CN107863200A (en) * | 2017-10-27 | 2018-03-30 | 成都天航智虹知识产权运营管理有限公司 | The method for preparing conductive film |
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|---|---|---|---|---|
| JP2012234796A (en) * | 2011-04-20 | 2012-11-29 | Nitto Denko Corp | Method of producing conductive laminated film |
| CN104779015A (en) * | 2015-05-06 | 2015-07-15 | 南京汉能薄膜太阳能有限公司 | Preparation method for graphene transparent conducting thin film |
| CN104900497A (en) * | 2015-06-15 | 2015-09-09 | 北京工业大学 | Method for directly growing graphene on nonmetallic substrate |
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2016
- 2016-06-24 CN CN201610464549.5A patent/CN105931757A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012234796A (en) * | 2011-04-20 | 2012-11-29 | Nitto Denko Corp | Method of producing conductive laminated film |
| CN104779015A (en) * | 2015-05-06 | 2015-07-15 | 南京汉能薄膜太阳能有限公司 | Preparation method for graphene transparent conducting thin film |
| CN104900497A (en) * | 2015-06-15 | 2015-09-09 | 北京工业大学 | Method for directly growing graphene on nonmetallic substrate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107732013A (en) * | 2017-10-27 | 2018-02-23 | 成都天航智虹知识产权运营管理有限公司 | A kind of preparation method of conductive film |
| CN107799233A (en) * | 2017-10-27 | 2018-03-13 | 成都天航智虹知识产权运营管理有限公司 | A kind of method for preparing conductive film |
| CN107863200A (en) * | 2017-10-27 | 2018-03-30 | 成都天航智虹知识产权运营管理有限公司 | The method for preparing conductive film |
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Application publication date: 20160907 |