CN107833698A - A kind of method for preparing transparent graphene conductive film - Google Patents
A kind of method for preparing transparent graphene conductive film Download PDFInfo
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- CN107833698A CN107833698A CN201711026158.6A CN201711026158A CN107833698A CN 107833698 A CN107833698 A CN 107833698A CN 201711026158 A CN201711026158 A CN 201711026158A CN 107833698 A CN107833698 A CN 107833698A
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- 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
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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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- 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 kind of method for preparing transparent graphene conductive film, belong to conductive film production technical field.The method comprising the steps of, and 5~10 parts of graphene platelets, 5~10 parts of graphene oxide thin slices, 30~40 parts of styrene-acrylic emulsions, 10~15 parts of Nano Silver powder, 55~65 parts of water are placed in centrifuge tube by the preparation of A. coating solutions, standby after 15~25min of sonic oscillation；B. coat, dry：By coating solution made from step A, coated on dry glass plate, coating thickness is 100~200 μm, is dried after coating, standby；C, reduction and reparation：The obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 500 800 DEG C, turned on the power, and adjusts power, plasma is produced in stove；Produced after being subsequently passed carbon source reaction.The present invention has production cost low, conducts electricity very well, the advantages of being adapted to mass produce.
Description
Technical field
The present invention relates to a kind of preparation method of transparent graphene conductive film, belong to conductive film production technical field.
Background technology
With the development of science and technology, society is also more and more to the demand of new material.Material is human civilization progress
With the material base of development in science and technology, the renewal of material makes the life of people, and also there occurs great variety.At present, it is booming new
The transparent and conductive thin-film material of type is in liquid crystal display, touch-screen, smart window, solar cell, microelectronics, information sensing
The device even field such as military project, which is obtained for, to be widely applied, and is being penetrated into other sciemtifec and technical spheres.Due to thin film technique
It is closely related with multiple technologies, thus the scientists of every field are excited to film preparation and its interest of performance.
Conductive film is that a kind of energy is conductive, realizes the film of some specific electric functions, is widely used in display, touches
Touch in the electronic devices such as screen and solar cell.At present, as a kind of transparent and conducting semiconductor material tin indium oxide
(ITO）, it is widely used in film applications always.Transparent lead is prepared by using magnetron sputtering that ITO is deposited over the transparent substrate
Conductive film, transparent base include such as glass and polyethylene terephthalate（PET）Film etc..Because tin indium oxide has height
Electrical conductivity, high thang-kng rate, so as one of main material for preparing conductive film.But tin indium oxide conductive film makes
There is also some shortcomings during, including:(1) indium resource is less, causes price continuous rise so that ITO turns into increasingly high
Expensive material, such as spraying, pulsed laser deposition, plating.And indium oxide has certain toxicity, unreasonable easily cause is recycled
Environmental pollution.（2）Characteristic crisp ITO prevents it from meeting some new opplications (such as 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
Crystal structure is tieed up, imparts its unique performance, research finds that graphene has excellent mechanical performance and excellent electrical property
Matter, the electron mobility of graphene is up to 15000cm2v under normal temperature-1s-1, and resistivity is only 10-6Ωcm.Graphene is being permitted
It is many-sided that there is more potential advantages, such as quality, robustness, pliability, chemical stability, infrared light transmission than tin indium oxide
Property and price etc..Therefore graphene is expected to replace tin indium oxide very much, for developing thinner, the conductive 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 (camphor) for presoma,
Graphene film is obtained on nickel foil, scientists achieve much obtains grinding for thickness controllable grapheme lamella in different matrix
Study carefully progress.By carrying out chemical etching on metallic matrix, graphene sheet layer is separated and is transferred on another matrix, and this is just
Eliminate complicated machinery or chemical treatment method and obtain the graphene sheet layer of high quality.The state such as South Korea and Japan adopts one after another
Big size graphene transparent conductive film has been prepared in this way, and desired main application fields are in flat-panel screens
On, serve as anode.Such as in new OLED（OLED）On exploitation, OLED has cost low, all solid state, main
Dynamic luminous, brightness height, contrast is high, visual angle is wide, fast response time, thickness of thin, low-voltage direct-current drive, are low in energy consumption, work temperature
Degree scope is wide, the features such as soft screen display can be achieved, and turns into the developing direction of future display technology.
The content of the invention
It is an object of the invention to provide a kind of preparation method of new transparent graphene conductive film, production cost is low,
And conduct electricity very well, the transparent graphene conductive film of large area can be produced, disclosure satisfy that the demand of large-scale production.
In order to realize foregoing invention purpose, technical scheme is as follows：
A kind of method for preparing transparent graphene conductive film, comprises the following steps：
A. prepared by coating solution
By 5~10 parts of graphene platelets, 5~10 parts of graphene oxide thin slices, 30~40 parts of styrene-acrylic emulsions, 10~15 parts of Nano Silvers
Powder, 55~65 parts of water are placed in centrifuge tube, standby after 15~25min of sonic oscillation；
B. coat, dry
By coating solution made from step A, coated on dry glass plate, coating thickness is 100~200 μm, is done after coating
It is dry, it is standby；
C, reduction and reparation
The obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 500-800 DEG C, opened
Power supply, and power is adjusted, plasma is produced in stove；Graphene electrically conducting transparent is produced after being subsequently passed carbon source reaction
Film.
The styrene-acrylic emulsion is Nano latex prepared by semi-continuous emulsion polymerizing technique, and its particle diameter is 45~80nm.
In step B, the condition of the drying is that 35~50min is dried at 100~120 DEG C.
In step C, the flow of the gas is 5-30sccm；Stove heating rate is：5-15℃/min；The power supply
Including RF power supplys；Power is adjusted to 50-200W；The flow of carbon source is 3-10sccm；Reaction time is 5-30min.
In step C, the carbon source includes methane, ethene or difluoromethane；The gas includes hydrogen, argon gas or it is mixed
Compound.
The light transmittance of the transparent graphene conductive film is 82~85%.
The resistance of the transparent graphene conductive film is 0.9~1.1M Ω/sq.
Beneficial effects of the present invention：
The present invention adds a certain proportion of Nano Silver powder in the coating liquid of graphene, greatly improves the electric conductivity of graphene
Energy.Compared with prior art, the present invention breaches the limitation of original technology, realizes a transparent graphene conductive film and is testing
The leap that the large scale of indoor small size to industrial applications is applied, there is the advantages of production cost is low, and electric conductivity is high, especially
It is adapted to mass produce, and is expected to substitute traditional inorganic oxide electrode material ITO, promotes the hair of graphene conductive film industry
Exhibition, has preferable economic benefit and social benefit.
Embodiment
Embodiment 1
A kind of method for preparing transparent graphene conductive film, comprises the following steps：
A. prepared by coating solution
5 parts of graphene platelets, 5 parts of graphene oxide thin slices, 30 parts of styrene-acrylic emulsions, 10 parts of Nano Silver powder, 55 parts of water are placed in
It is standby after sonic oscillation 15min in centrifuge tube；
B. coat, dry
By coating solution made from step A, coated on dry glass plate, coating thickness is 100 μm, is dried after coating, standby
With；
C, reduction and reparation
The obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 500 DEG C, opens electricity
Source, and power is adjusted, plasma is produced in stove；It is subsequently passed after carbon source reaction that to produce graphene electrically conducting transparent thin
Film.
Embodiment 2
A kind of method for preparing transparent graphene conductive film, comprises the following steps：
10 parts of graphene platelets, 10 parts of graphene oxide thin slices, 40 parts of styrene-acrylic emulsions, 15 parts of Nano Silver powder, 65 parts of water are put
It is standby after sonic oscillation 25min in centrifuge tube；
B. coat, dry
By coating solution made from step A, coated on dry glass plate, coating thickness is 200 μm, is dried after coating, standby
With；
C, reduction and reparation
The obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 800 DEG C, opens electricity
Source, and power is adjusted, plasma is produced in stove；It is subsequently passed after carbon source reaction that to produce graphene electrically conducting transparent thin
Film.
The styrene-acrylic emulsion is Nano latex prepared by semi-continuous emulsion polymerizing technique, and its particle diameter is 45nm.
In step B, the condition of the drying is that 35min is dried at 100 DEG C.
In step C, the flow of the gas is 5sccm；Stove heating rate is：10℃/min；The power supply includes RF
Power supply；Power is adjusted to 50W；The flow of carbon source is 3sccm；Reaction time is 5min.
In step C, the carbon source includes methane, ethene or difluoromethane；The gas includes hydrogen, argon gas or it is mixed
Compound.
The light transmittance of the transparent graphene conductive film is 82~85%.
The resistance of the transparent graphene conductive film is 0.9~1.1M Ω/sq.
Embodiment 3
A kind of method for preparing transparent graphene conductive film, comprises the following steps：
A. prepared by coating solution
8 parts of graphene platelets, 8 parts of graphene oxide thin slices, 35 parts of styrene-acrylic emulsions, 12 parts of Nano Silver powder, 60 parts of water are placed in
It is standby after sonic oscillation 20min in centrifuge tube；
B. coat, dry
By coating solution made from step A, coated on dry glass plate, coating thickness is 150 μm, is dried after coating, standby
With；
C, reduction and reparation
The obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 600 DEG C, opens electricity
Source, and power is adjusted, plasma is produced in stove；It is subsequently passed after carbon source reaction that to produce graphene electrically conducting transparent thin
Film.
The styrene-acrylic emulsion is Nano latex prepared by semi-continuous emulsion polymerizing technique, and its particle diameter is 45nm.
In step B, the condition of the drying is that 35min is dried at 100 DEG C.
In step C, the flow of the gas is 30sccm；Stove heating rate is：15℃/min；The power supply includes
RF power supplys；Power is adjusted to 200W；The flow of carbon source is 10sccm；Reaction time is 30min.
In step C, the carbon source includes methane, ethene or difluoromethane；The gas includes hydrogen, argon gas or it is mixed
Compound.
The light transmittance of the transparent graphene conductive film is 85~88%.
The resistance of the transparent graphene conductive film is 0.9~1.1M Ω/sq.
Embodiment 4
A kind of method for preparing transparent graphene conductive film, comprises the following steps：
A. prepared by coating solution
9 parts of graphene platelets, 7 parts of graphene oxide thin slices, 38 parts of styrene-acrylic emulsions, 13 parts of Nano Silver powder, 58 parts of water are placed in
It is standby after sonic oscillation 25min in centrifuge tube；
B. coat, dry
By coating solution made from step A, coated on dry glass plate, coating thickness is 180 μm, is dried after coating, standby
With；
C, reduction and reparation
The obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 700 DEG C, opens electricity
Source, and power is adjusted, plasma is produced in stove；It is subsequently passed after carbon source reaction that to produce graphene electrically conducting transparent thin
Film.
The styrene-acrylic emulsion is Nano latex prepared by semi-continuous emulsion polymerizing technique, and its particle diameter is 45~80nm.
In step B, the condition of the drying is that 48min is dried at 120 DEG C.
In step C, the flow of the gas is 30sccm；Stove heating rate is：10℃/min；The power supply includes
RF power supplys；Power is adjusted to 120W；The flow of carbon source is 6sccm；Reaction time is 15min.
In step C, the carbon source includes methane, ethene or difluoromethane；The gas includes hydrogen, argon gas or it is mixed
Compound.
The light transmittance of the transparent graphene conductive film is 85~88%.
The resistance of the transparent graphene conductive film is 0.9~1.1M Ω/sq.
Embodiment 5
A kind of method for preparing transparent graphene conductive film, comprises the following steps：
A. prepared by coating solution
7 parts of graphene platelets, 9 parts of graphene oxide thin slices, 40 parts of styrene-acrylic emulsions, 15 parts of Nano Silver powder, 65 parts of water are placed in
It is standby after sonic oscillation 25min in centrifuge tube；
B. coat, dry
By coating solution made from step A, coated on dry glass plate, coating thickness is 130 μm, is dried after coating, standby
With；
C, reduction and reparation
The obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 650 DEG C, opens electricity
Source, and power is adjusted, plasma is produced in stove；It is subsequently passed after carbon source reaction that to produce graphene electrically conducting transparent thin
Film.
The styrene-acrylic emulsion is Nano latex prepared by semi-continuous emulsion polymerizing technique, and its particle diameter is 80nm.
In step B, the condition of the drying is that 35min is dried at 110 DEG C.
In step C, the flow of the gas is 20sccm；Stove heating rate is：12℃/min；The power supply includes
RF power supplys；Power is adjusted to 50-200W；The flow of carbon source is 10sccm；Reaction time is 20min.
In step C, the carbon source includes methane, ethene or difluoromethane；The gas includes hydrogen, argon gas or it is mixed
Compound.
The light transmittance of the transparent graphene conductive film is 85~88%.
The resistance of the transparent graphene conductive film is 0.9~1.1M Ω/sq.
Claims (7)
- A kind of 1. method for preparing transparent graphene conductive film, it is characterised in that：Comprise the following steps：A. prepared by coating solutionBy 5~10 parts of graphene platelets, 5~10 parts of graphene oxide thin slices, 30~40 parts of styrene-acrylic emulsions, 10~15 parts of Nano Silvers Powder, 55~65 parts of water are placed in centrifuge tube, standby after 15~25min of sonic oscillation；B. coat, dryBy coating solution made from step A, coated on dry glass plate, coating thickness is 100~200 μm, is done after coating It is dry, it is standby；C, reduction and reparationThe obtained semi-finished product of step B are placed in stove, gas is passed through and opens vavuum pump；Stove is warming up to 500-800 DEG C, opened Power supply, and power is adjusted, plasma is produced in stove；Graphene electrically conducting transparent is produced after being subsequently passed carbon source reaction Film.
- A kind of 2. method for preparing transparent graphene conductive film as claimed in claim 1, it is characterised in that：The phenylpropyl alcohol breast Liquid is Nano latex prepared by semi-continuous emulsion polymerizing technique, and its particle diameter is 45~80nm.
- A kind of 3. method for preparing transparent graphene conductive film as claimed in claim 1, it is characterised in that：In step B, institute It is that 35~50min is dried at 100~120 DEG C to state dry condition.
- A kind of 4. method for preparing transparent graphene conductive film as claimed in claim 1, it is characterised in that：In step C, The flow of the gas is 5-30sccm；Stove heating rate is：5-15℃/min；The power supply includes RF power supplys；Power supply work( Rate is adjusted to 50-200W；The flow of carbon source is 3-10sccm；Reaction time is 5-30min.
- A kind of 5. method for preparing transparent graphene conductive film as claimed in claim 1, it is characterised in that：In step C, The carbon source includes methane, ethene or difluoromethane；The gas includes hydrogen, argon gas or its mixture.
- A kind of 6. preparation method of transparent graphene conductive film as described in any one of Claims 1 to 5, it is characterised in that： The light transmittance of the transparent graphene conductive film is 82~85%.
- A kind of 7. preparation method of transparent graphene conductive film as described in any one of Claims 1 to 5, it is characterised in that： The resistance of the transparent graphene conductive film is 0.9~1.1M Ω/sq.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220566A (en) * | 2011-06-09 | 2011-10-19 | 无锡第六元素高科技发展有限公司 | Method for preparing single-layer or multi-layer graphene through chemical vapor deposition |
| WO2012102561A2 (en) * | 2011-01-26 | 2012-08-02 | 성균관대학교산학협력단 | Method for preparing a conductive thin film comprising reduced graphene oxide and carbon nanotube, and transparent electrode including the conductive thin film prepared thereby |
| CN106082693A (en) * | 2016-06-24 | 2016-11-09 | 成都天航智虹企业管理咨询有限公司 | A kind of method preparing transparent graphene conductive film |
| CN106882926A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院上海硅酸盐研究所 | The method for preparing transparent graphene conductive film |
-
2017
- 2017-10-27 CN CN201711026158.6A patent/CN107833698A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012102561A2 (en) * | 2011-01-26 | 2012-08-02 | 성균관대학교산학협력단 | Method for preparing a conductive thin film comprising reduced graphene oxide and carbon nanotube, and transparent electrode including the conductive thin film prepared thereby |
| CN102220566A (en) * | 2011-06-09 | 2011-10-19 | 无锡第六元素高科技发展有限公司 | Method for preparing single-layer or multi-layer graphene through chemical vapor deposition |
| CN106882926A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院上海硅酸盐研究所 | The method for preparing transparent graphene conductive film |
| CN106082693A (en) * | 2016-06-24 | 2016-11-09 | 成都天航智虹企业管理咨询有限公司 | A kind of method preparing transparent graphene conductive film |
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