CN114230898B - Graphene transparent conductive film and preparation method and application thereof - Google Patents
Graphene transparent conductive film and preparation method and application thereof Download PDFInfo
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- CN114230898B CN114230898B CN202111674620.XA CN202111674620A CN114230898B CN 114230898 B CN114230898 B CN 114230898B CN 202111674620 A CN202111674620 A CN 202111674620A CN 114230898 B CN114230898 B CN 114230898B
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- graphene
- transparent conductive
- conductive film
- graphene transparent
- vapor deposition
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 229920001684 low density polyethylene Polymers 0.000 claims abstract description 19
- 239000004702 low-density polyethylene Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 230000001681 protective effect Effects 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 5
- -1 polyethylene Polymers 0.000 abstract description 5
- 229920000573 polyethylene Polymers 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000007740 vapor deposition Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram 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
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The invention relates to the technical field of material synthesis, and particularly discloses a graphene transparent conductive film, and a preparation method and application thereof. The preparation method of the graphene transparent conductive film comprises the following steps: a. methane is used as a carbon source to be mixed with a protective gas, and then chemical vapor deposition reaction is carried out to form a graphene film on a substrate; b. melt blending the graphene film and low-density polyethylene according to a mass ratio of 100:1-1.5 under a vacuum condition of 280-300 ℃ to obtain a blend; c. and under the vacuum condition, preparing the graphene transparent conductive film from the blend by a physical vapor deposition method. The preparation method of the graphene transparent conductive film solves the problems that the surface of the graphene film prepared by the vapor deposition method has some folds and discontinuities, and the special composite film formed by graphene and polyethylene has high transparency and high conductivity.
Description
Technical Field
The invention relates to the technical field of material synthesis, in particular to a graphene transparent conductive film, and a preparation method and application thereof.
Background
With the increasing innovation of technology, people have increasingly higher requirements on electronic intelligent devices. The touch screen is an extremely important part of the flexible OLED display screen, and the basic principle is that when a finger or other objects touch the touch screen arranged at the front end of the display, the touched position (in the form of coordinates) is detected by a touch screen controller and sent to a CPU (central processing unit) through an interface, so that input information is determined. The main technologies of touch screens are resistive touch screens and capacitive touch screens, and the core of the touch screens is an ITO (indium tin oxide) conductive layer. The conductive layer has high light transmittance and high conductivity, but the main components of the conductive layer are indium oxide and tin oxide, wherein indium is a rare metal, so that the preparation cost of the ITO material is extremely high.
Compared with the traditional indium tin oxide film, the graphene transparent conductive film has the characteristics of strong conductivity, high transparency, high flexibility, abundant resources and lower cost. And the graphene has a stable, thin and hard structure, and is a conductor with excellent performance. The graphene is mainly prepared by a chemical vapor deposition method, but the graphene prepared by the method has some folds and discontinuities on the surface. When a graphene sample is transferred onto a flexible substrate, stress is applied, and the defects are more remarkable in touch screen application, so that the electrochemical performance of the graphene sample is affected, and the ideal electrochemical performance effect is not achieved. At present, a graphene transparent conductive film is prepared by adding an auxiliary agent, an organic polymer material and the like to form a composite material with graphene so as to overcome the defects of the graphene film, but the preparation method is complex, the period is long, and the conductivity of the graphene conductive film prepared by a chemical vapor deposition method is seriously influenced due to the high insulativity of the organic polymer material.
Disclosure of Invention
Aiming at the problems of the graphene transparent conductive film prepared by the conventional chemical vapor deposition method, the invention provides the graphene transparent conductive film, and the preparation method and application thereof.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
the preparation method of the graphene transparent conductive film comprises the following steps:
a. methane is used as a carbon source to be mixed with a protective gas, and then chemical vapor deposition reaction is carried out to form a graphene film on a substrate;
b. melt blending the graphene film and low-density polyethylene according to a mass ratio of 100:1-1.5 under a vacuum condition of 280-300 ℃ to obtain a blend;
c. and under the vacuum condition, preparing the graphene transparent conductive film from the blend by a physical vapor deposition method.
Compared with the prior art, the graphene transparent conductive film provided by the invention takes graphene and low-density polyethylene as raw materials, and firstly, the graphene film is precipitated on a substrate by a chemical vapor deposition method; then carrying out melt blending on the graphene film and the low-density polyethylene according to a specific proportion under the vacuum condition of 280-300 ℃; and finally, generating a composite film by adopting a physical vapor deposition method. The composite film not only solves the problem that the surface of the graphene film prepared by vapor deposition has some folds and discontinuities, but also realizes the alternate coexistence of graphene and polyethylene in a specific form on a nanometer scale, effectively avoids the phenomenon of reduced conductivity caused by the introduction of insulating materials, and ensures that the special composite film formed by the graphene and the polyethylene has high transparency and high conductivity, and can obviously increase the smoothness of the touch screen when being used for manufacturing the touch screen.
Preferably, in the step a, the shielding gas is argon.
Preferably, in the step a, the volume ratio of the methane to the shielding gas is 1:3-2:5.
Preferably, in the step a, the temperature of the chemical vapor deposition reaction is 900-950 ℃ and the time is 10-15 min.
Preferably, in the step a, the substrate is a monocrystalline silicon substrate.
Preferably, in step b, the low density polyethylene has a density of 0.90g/cm 3 -0.95g/cm 3 。
The addition of the low-density polyethylene can further ensure the flatness and the continuity of the prepared graphene transparent conductive film.
Preferably, in the step b, the time of melt blending is 2min-6min.
Preferably, in the step c, the physical vapor deposition method adopts a sputtering coating method.
Preferably, in the step c, the thickness of the graphene transparent conductive film is 18 μm-22 μm.
The invention also provides the graphene transparent conductive film prepared by the preparation method of the graphene transparent conductive film.
The graphene transparent conductive film prepared by the preparation method provided by the invention has the advantages of no wrinkling and discontinuity, and higher conductivity.
The invention also provides application of the graphene transparent conductive film in preparation of an electronic touch screen.
The electronic touch screen prepared from the graphene transparent conductive film provided by the invention has smooth refreshing effect and excellent usability.
Drawings
Fig. 1 is a flow chart of a preparation process of a graphene transparent conductive film in embodiment 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The preparation method of the graphene transparent conductive film comprises the following steps:
a. opening a vacuum valve of the reaction furnace, vacuumizing the reaction furnace, heating the reaction furnace to 900 ℃, then introducing methane and argon (the volume ratio of the methane to the argon is 1:3), adjusting the ventilation valve to uniformly enter the reaction furnace, performing chemical vapor deposition reaction for 10min, and depositing carbon atoms on a monocrystalline silicon substrate under the carrying of an argon medium to form a graphene film;
b. the reaction furnace was evacuated, the temperature in the reaction furnace was adjusted to 280℃and low-density polyethylene was introduced to give a low-density polyethylene (density: 0.90 g/cm) 3 ) Carrying out fusion reaction with the graphene film in a reaction furnace for 2min (the mass ratio of the graphene film to the low-density polyethylene is 100:1), thereby realizing the following stepsMelt blending to obtain a blend;
c. the blend is subjected to a sputtering coating method under a vacuum condition to prepare a film with the thickness of 18 mu m on a monocrystalline silicon substrate, namely the graphene transparent conductive film.
A flow diagram of the above process steps is shown in fig. 1.
Example 2
The preparation method of the graphene transparent conductive film comprises the following steps:
a. opening a vacuum valve of the reaction furnace, vacuumizing the reaction furnace, heating the reaction furnace to 920 ℃, then introducing methane and argon (the volume ratio of the methane to the argon is 2:3), adjusting the ventilation valve to uniformly enter the reaction furnace, performing chemical vapor deposition reaction for 12min, and depositing carbon atoms on a monocrystalline silicon substrate under the carrying of an argon medium to form a graphene film;
b. the reaction furnace was evacuated, the temperature in the reaction furnace was adjusted to 290℃and low-density polyethylene was introduced to give a low-density polyethylene (density: 0.93 g/cm) 3 ) Carrying out fusion reaction for 3min (the mass ratio of the graphene film to the low-density polyethylene is 100:1.2) with the graphene film in a reaction furnace to realize melt blending and obtain a blend;
c. the blend is subjected to a sputtering coating method under a vacuum condition to prepare a film with the thickness of 20 mu m on a monocrystalline silicon substrate, namely the graphene transparent conductive film.
Example 3
The preparation method of the graphene transparent conductive film comprises the following steps:
a. opening a vacuum valve of the reaction furnace, vacuumizing the reaction furnace, heating the reaction furnace to 950 ℃, then introducing methane and argon (the volume ratio of the methane to the argon is 2:5), adjusting the ventilation valve to uniformly enter the reaction furnace, performing chemical vapor deposition reaction for 15min, and depositing carbon atoms on a monocrystalline silicon substrate under the carrying of an argon medium to form a graphene film;
b. vacuumizing the reaction furnace, regulating the temperature in the reaction furnace to 300 ℃, and introducing low-density polymerEthylene, low density polyethylene (density of 0.95g/cm 3 ) Carrying out fusion reaction with the graphene film in a reaction furnace for 6min (the mass ratio of the graphene film to the low-density polyethylene is 100:1.5), and realizing melt blending to obtain a blend;
c. the blend is subjected to a sputtering coating method under a vacuum condition to prepare a film with the thickness of 18-22 mu m on a monocrystalline silicon substrate, namely the graphene transparent conductive film.
Comparative example 1
The mass ratio of the graphene film to the low-density polyethylene in the embodiment 1 is replaced by 100:0.5, and other preparation methods are the same as the embodiment, so that the graphene transparent conductive film is obtained.
Comparative example 2
The mass ratio of the graphene film to the low-density polyethylene in the embodiment 1 is replaced by 100:2, and other preparation methods are the same as the embodiment, so that the graphene transparent conductive film is obtained.
The electrochemical properties of the graphene transparent conductive films prepared in the above examples 1-3 and comparative examples 1-2 were tested, and the test results are shown in table 1.
TABLE 1 electrochemical Properties of graphene transparent conductive films
According to the data in table 1, the graphene transparent conductive film prepared by doping a certain amount of low-density polyethylene into the graphene, carrying out melt blending at a specific temperature and combining a sputtering coating process realizes the alternate coexistence of the graphene and the polyethylene at the nanometer scale, and plays the advantages of the graphene and the polyethylene in the transparent conductive film.
The graphene transparent conductive film prepared in the above embodiments 1-3 is cut and prepared into a touch screen, and the touch screen has smooth refreshing effect and excellent usability. The touch screen manufactured by using the graphene transparent conductive film obtained in comparative example 2 had a stuck refreshing effect and was poor in usability.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (9)
1. A preparation method of a graphene transparent conductive film is characterized by comprising the following steps: the method comprises the following steps:
a. methane is used as a carbon source to be mixed with a protective gas, and then chemical vapor deposition reaction is carried out to form a graphene film on a substrate;
b. melt blending the graphene film and low-density polyethylene according to a mass ratio of 100:1-1.5 under a vacuum condition of 280-300 ℃ to obtain a blend;
c. preparing the blend into the graphene transparent conductive film by a physical vapor deposition method under a vacuum condition;
in step b, the low density polyethylene has a density of 0.90g/cm 3 -0.95g/cm 3 ；
In the step c, the physical vapor deposition method is a sputtering coating method.
2. The method for preparing the graphene transparent conductive film according to claim 1, wherein: in the step a, the shielding gas is argon.
3. The method for preparing the graphene transparent conductive film according to claim 1, wherein: in the step a, the volume ratio of the methane to the shielding gas is 1:3-2:5.
4. The method for preparing the graphene transparent conductive film according to claim 1, wherein: in the step a, the temperature of the chemical vapor deposition reaction is 900-950 ℃ and the time is 10-15 min.
5. The method for preparing the graphene transparent conductive film according to claim 1, wherein: in the step a, the substrate is a monocrystalline silicon substrate.
6. The method for preparing the graphene transparent conductive film according to claim 1, wherein: in the step b, the time of melt blending is 2min-6min.
7. The method for preparing the graphene transparent conductive film according to claim 1, wherein: in the step c, the thickness of the graphene transparent conductive film is 18-22 mu m.
8. The transparent conductive graphene film according to any one of claims 1 to 7.
9. The application of the graphene transparent conductive film in preparing an electronic touch screen.
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| CN114230898B true CN114230898B (en) | 2024-01-12 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011081473A2 (en) * | 2009-12-31 | 2011-07-07 | 성균관대학교산학협력단 | Transparent graphene electrode, and flexible silicon thin film semiconductor device containing same |
| WO2015109684A1 (en) * | 2014-01-22 | 2015-07-30 | 武汉理工大学 | Methods for preparing composite graphene conductive oxide target and transparent conductive film thereof |
| CN105261778A (en) * | 2014-07-15 | 2016-01-20 | 廖伟豪 | Graphene battery and manufacturing method of electrode plate for graphene battery |
| CN107541709A (en) * | 2017-08-20 | 2018-01-05 | 长沙小新新能源科技有限公司 | The preparation method and graphene film of a kind of graphene film |
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- 2021-12-31 CN CN202111674620.XA patent/CN114230898B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011081473A2 (en) * | 2009-12-31 | 2011-07-07 | 성균관대학교산학협력단 | Transparent graphene electrode, and flexible silicon thin film semiconductor device containing same |
| WO2015109684A1 (en) * | 2014-01-22 | 2015-07-30 | 武汉理工大学 | Methods for preparing composite graphene conductive oxide target and transparent conductive film thereof |
| CN105261778A (en) * | 2014-07-15 | 2016-01-20 | 廖伟豪 | Graphene battery and manufacturing method of electrode plate for graphene battery |
| CN107541709A (en) * | 2017-08-20 | 2018-01-05 | 长沙小新新能源科技有限公司 | The preparation method and graphene film of a kind of graphene film |
Non-Patent Citations (1)
| Title |
|---|
| 李爱农、刘钰如主编.《工程材料及应用》.华中科技大学出版社,2019,第131-132页. * |
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