CN106024111A - Preparation method of conductive thin film - Google Patents
Preparation method of conductive thin film Download PDFInfo
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- CN106024111A CN106024111A CN201610464555.0A CN201610464555A CN106024111A CN 106024111 A CN106024111 A CN 106024111A CN 201610464555 A CN201610464555 A CN 201610464555A CN 106024111 A CN106024111 A CN 106024111A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000010409 thin film Substances 0.000 title abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 70
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 34
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000000151 deposition Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000011265 semifinished product Substances 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- -1 graphite alkene Chemical class 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 21
- 239000010439 graphite Substances 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 38
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 2
- 239000000463 material Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 5
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229940025250 camphora Drugs 0.000 description 1
- 239000010238 camphora Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004984 smart glass Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physical Vapour Deposition (AREA)
- Carbon And Carbon Compounds (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The invention discloses a preparation method of 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, namely depositing a nickel thin film layer with the thickness of 1-3 nickel atoms on a glass substrate; (B) depositing a graphene layer, namely depositing a graphene thin film layer by a CVD method, wherein the thickness of the graphene thin film layer is 50-100 microns; and (C) carrying out cleaning and drying, namely carrying out cooling treatment on a semi-finished product obtained in the step (B), after the temperature is reduced to a room temperature, cleaning the graphene thin film layer, removing the nickel thick film layer on the surface and then carrying out drying. The method has the advantages of low production cost and high efficiency.
Description
Technical field
The present invention relates to the preparation method of a kind of 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 conductive film, production cost is low, 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 preparation method of conductive film, it is characterised in that: comprise the following steps:
A. deposited nickel layer
The nickel thin layer that 1～3 nickle atom of deposition is thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50～100 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,
Remove surface nickel thin layer, be then dried.
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: 1 × 10-5～1 × 10-4Pa, sputtering pressure 1～3Pa, underlayer temperature 30～100 DEG C.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2Mixing with He
Gas；The temperature of deposition is 550～700 DEG C, and the pressure of deposition is 1 × 10-4～5 × 10-4Pa。
In step C, described cleaning refers to, with weak acid solution, the semi-finished product after cooling are soaked 2～3h.
In step C, described dry condition is to be dried 30～45min at 110～130 DEG C.
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 suitable for large-scale production, is expected to substitute tradition inorganic oxide electrode material
Material ITO, promotes the development of conductive film industry, has preferable economic benefit and social benefit.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of conductive film, comprises the following steps:
A. deposited nickel layer
The nickel thin layer that 1 nickle atom of deposition is thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50 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,
Remove surface nickel thin layer, be then dried.
Embodiment 2
The preparation method of a kind of conductive film, comprises the following steps:
A. deposited nickel layer
The nickel thin layer that 3 nickle atoms of deposition are thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 100 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,
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, background vacuum: 1 × 10-5Pa, spatters
Injection pressure 1Pa, underlayer temperature 30 DEG C.
Embodiment 3
The preparation method of a kind of conductive film, comprises the following steps:
A. deposited nickel layer
The nickel thin layer that 2 nickle atoms of deposition are thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 68 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,
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, background vacuum: 1 × 10-4Pa, spatters
Injection pressure 3Pa, underlayer temperature 100 DEG C.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2Mixing with He
Gas, mixed proportion is 2:1；The temperature of deposition is 550 DEG C, and the pressure of deposition is 1 × 10-4Pa。
Embodiment 4
The preparation method of a kind of conductive film, comprises the following steps:
A. deposited nickel layer
The nickel thin layer that 3 nickle atoms of deposition are thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 80 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,
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, background vacuum: 1 × 10-4Pa, spatters
Injection pressure 3Pa, underlayer temperature 100 DEG C.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2Mixing with He
Gas, mixed proportion is 10:1；The temperature of deposition is 700 DEG C, and the pressure of deposition is 5 × 10-4Pa。
In step C, described cleaning refers to, with weak acid solution, the semi-finished product after cooling are soaked 2h.In step C, described dry
Condition be at 110 DEG C be dried 30min.Embodiment 5
The preparation method of a kind of conductive film, comprises the following steps:
A. deposited nickel layer
The nickel thin layer that 1 nickle atom of deposition is thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 70 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,
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, background vacuum: 6 × 10-5Pa, spatters
Injection pressure 2Pa, underlayer temperature 60 DEG C.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2Mixing with He
Gas, mixed proportion is 45:1；The temperature of deposition is 600 DEG C, and the pressure of deposition is 3 × 10-4Pa。
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 be at 110 DEG C be dried 45min.
Embodiment 6
The preparation method of a kind of conductive film, comprises the following steps:
A. deposited nickel layer
The nickel thin layer that 1 nickle atom of deposition is thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 70 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,
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, background vacuum: 8 × 10-5Pa, spatters
Injection pressure 1.5Pa, underlayer temperature 55 DEG C.
In step B, during described CVD deposited graphite alkene thin layer, carbon source is methane, and gas is H2Mixing with He
Gas, mixed proportion is 1:1；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 weak acid solution, the semi-finished product after cooling are soaked 2.5h.In step C, described dry
Dry condition is to be dried 40min at 130 DEG C.
Claims (5)
1. the preparation method of a conductive film, it is characterised in that: comprise the following steps:
A. deposited nickel layer
The nickel thin layer that 1～3 nickle atom of deposition is thick on the glass substrate；
B. deposited graphite alkene layer
Using CVD deposited graphite alkene thin layer, the thickness of described graphene film layer is 50～100 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,
Remove surface nickel thin layer, be then dried.
The preparation method of a kind of conductive film the most as claimed in claim 1, it is characterised in that: in step A, described deposited nickel layer
Method be magnetron sputtering method, background vacuum: 1 × 10-5～1 × 10-4Pa, sputtering pressure 1～3Pa, underlayer temperature 30～
100℃。
The preparation method of a kind of conductive film the most as claimed in claim 1, it is characterised in that: in step B, described CVD is sunk
During long-pending Graphene thin layer, carbon source is methane, and gas is H2Mixed gas with He；The temperature of deposition is 550～700
DEG C, the pressure of deposition is 1 × 10-4～5 × 10-4Pa。
The preparation method of a kind of conductive film the most as claimed in claim 1, it is characterised in that: in step C, described cleaning refers to
With weak acid solution, the semi-finished product after cooling are soaked 2～3h.
5. the preparation method of a kind of 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 30～45min at 110～130 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464555.0A CN106024111A (en) | 2016-06-24 | 2016-06-24 | Preparation method of conductive thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464555.0A CN106024111A (en) | 2016-06-24 | 2016-06-24 | Preparation method of conductive thin film |
Publications (1)
| Publication Number | Publication Date |
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| CN106024111A true CN106024111A (en) | 2016-10-12 |
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ID=57086025
Family Applications (1)
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| CN201610464555.0A Pending CN106024111A (en) | 2016-06-24 | 2016-06-24 | Preparation method of conductive thin film |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101835609A (en) * | 2007-09-10 | 2010-09-15 | 三星电子株式会社 | Graphene sheet and process of preparing the same |
| CN102120574A (en) * | 2011-03-15 | 2011-07-13 | 东南大学 | Method for preparing large-scale two-dimensional nanomaterial graphite |
| CN102751043A (en) * | 2011-04-20 | 2012-10-24 | 日东电工株式会社 | Method of manufacturing conductive laminated film |
| CN102849961A (en) * | 2011-07-01 | 2013-01-02 | 中央研究院 | Method for growing carbon film or inorganic material film on substrate |
| CN104085887A (en) * | 2014-07-29 | 2014-10-08 | 苏州斯迪克新材料科技股份有限公司 | Chemical vapor deposition method for preparing graphene |
| 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 |
-
2016
- 2016-06-24 CN CN201610464555.0A patent/CN106024111A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101835609A (en) * | 2007-09-10 | 2010-09-15 | 三星电子株式会社 | Graphene sheet and process of preparing the same |
| CN102120574A (en) * | 2011-03-15 | 2011-07-13 | 东南大学 | Method for preparing large-scale two-dimensional nanomaterial graphite |
| CN102751043A (en) * | 2011-04-20 | 2012-10-24 | 日东电工株式会社 | Method of manufacturing conductive laminated film |
| CN102849961A (en) * | 2011-07-01 | 2013-01-02 | 中央研究院 | Method for growing carbon film or inorganic material film on substrate |
| CN104085887A (en) * | 2014-07-29 | 2014-10-08 | 苏州斯迪克新材料科技股份有限公司 | Chemical vapor deposition method for preparing graphene |
| 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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