CN113284668A - Preparation method and application of metal grid transparent conductive film - Google Patents
Preparation method and application of metal grid transparent conductive film Download PDFInfo
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- CN113284668A CN113284668A CN202110345126.2A CN202110345126A CN113284668A CN 113284668 A CN113284668 A CN 113284668A CN 202110345126 A CN202110345126 A CN 202110345126A CN 113284668 A CN113284668 A CN 113284668A
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- copper
- aluminum
- conductive film
- nanoparticles
- ink
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 30
- 239000002184 metal Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002105 nanoparticle Substances 0.000 claims abstract description 59
- 229910052802 copper Inorganic materials 0.000 claims abstract description 53
- 239000010949 copper Substances 0.000 claims abstract description 53
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 49
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 239000004642 Polyimide Substances 0.000 claims abstract description 12
- 229920001721 polyimide Polymers 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000003848 UV Light-Curing Methods 0.000 claims abstract description 6
- 238000001723 curing Methods 0.000 claims abstract description 6
- 239000003292 glue Substances 0.000 claims abstract description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 17
- 229920000178 Acrylic resin Polymers 0.000 claims description 17
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 16
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 16
- 229940116411 terpineol Drugs 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 239000003223 protective agent Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000001856 Ethyl cellulose Substances 0.000 claims description 5
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 5
- 229920001249 ethyl cellulose Polymers 0.000 claims description 5
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 5
- -1 polyethylene Polymers 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 238000010297 mechanical methods and process Methods 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229920002457 flexible plastic Polymers 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 125000005462 imide group Chemical group 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002834 transmittance Methods 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
- 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
- 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
- H01B1/023—Alloys based on aluminium
-
- 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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
-
- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- 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
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Laminated Bodies (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a preparation method of a metal grid transparent conductive film, which comprises the following steps: (1) coating UV curing impression glue on the transparent polyimide substrate, and carrying out ultraviolet curing to obtain a transparent colloidal layer with a groove network; (2) filling copper/aluminum composite conductive ink in the groove network, and sintering; the copper/aluminum composite conductive ink comprises copper nanoparticles and aluminum nanoparticles, and the mass ratio of the copper nanoparticles to the aluminum nanoparticles is 3-5: 1. The metal grid transparent conductive film prepared by the invention ensures the conductivity, increases the adhesion between the metal grid and the substrate, and can be applied to transparent flexible display screens.
Description
Technical Field
The invention belongs to the technical field of photoelectron materials, and particularly relates to a preparation method and application of a metal grid transparent conductive film.
Background
In recent years, with the rapid development of flexible electronic and photoelectric devices, the traditional ITO film is increasingly unable to meet the application requirements, and new challenges are provided for novel flexible transparent conductive films. The metal grid transparent conductive film is produced under the background, has the advantages of high conductivity, high transmittance, low cost, flexibility, stretchability and the like, and has potential to become the best alternative material of ITO.
Polyimide refers to a polymer having an imide ring in the main chain, which has excellent properties such as excellent heat resistance, low temperature resistance, mechanical properties, and a low thermal expansion coefficient, and has the highest glass transition temperature among flexible plastics. The excellent performances enable the flexible transparent conductive film to have wide application prospects in the field of flexible electronics, and the flexible transparent conductive film serving as a substrate material is one of application directions of the flexible transparent conductive film.
However, the existing metal mesh transparent conductive film based on the transparent polyimide substrate has the problems of poor adhesion between the metal mesh and the transparent polyimide substrate, and the like, and further application of the metal mesh transparent conductive film is limited.
Disclosure of Invention
Based on the technical problems, the invention provides a preparation method of a metal grid transparent conductive film, which can increase the adhesiveness of a metal grid on a transparent polyimide substrate while ensuring the conductivity of the metal grid transparent conductive film.
The technical scheme of the invention is as follows:
the invention provides a preparation method of a metal grid transparent conductive film, which comprises the following steps: (1) coating UV curing impression glue on the transparent polyimide substrate, and carrying out ultraviolet curing to obtain a transparent colloidal layer with a groove network; (2) filling copper/aluminum composite conductive ink in the groove network, and sintering;
the copper/aluminum composite conductive ink comprises copper nanoparticles and aluminum nanoparticles, and the mass ratio of the copper nanoparticles to the aluminum nanoparticles is 3-5: 1.
The coating thickness of the UV curable imprinting paste in the present invention is not particularly limited, and may be adjusted based on the requirements conventionally used in the art. In the present invention, the depth of the trench is 1 μm to 10 μm.
Preferably, the diameter of the copper nanoparticles is 30-180 nm; the diameter of the aluminum nanoparticles is 30-180 nm.
Preferably, the copper/aluminum composite conductive ink is prepared by the following method:
s1, preparing copper nanoparticle ink: dispersing copper nanoparticles into terpineol solution containing a protective agent, adding an adhesive, and uniformly stirring to obtain copper nanoparticle ink;
s2, preparing aluminum nanoparticle ink: dispersing aluminum nano particles into terpineol solution containing a protective agent, adding an adhesive, and uniformly stirring to obtain aluminum nano particle ink;
s3, preparing copper/aluminum composite conductive ink: and mixing the copper nanoparticle ink and the aluminum nanoparticle ink by adopting a physical mechanical method to obtain the copper/aluminum composite conductive ink.
Preferably, the protective agent is acrylic resin or PVP; more preferably, an acryl resin.
The acrylic resin is an ethyl acrylate/methyl methacrylate copolymer, and the molecular weight of the acrylic resin is 10000-100000.
Preferably, the adhesive is ethyl cellulose or polyethylene.
Preferably, in the copper nanoparticle ink, the mass ratio of the copper nanoparticles to the protective agent to the terpineol to the adhesive is 10:1-2:5-8: 0.1-0.3; in the aluminum nanoparticle ink, the mass ratio of aluminum nanoparticles to a protective agent to terpineol to an adhesive is 10:2-4:8-10: 0.2-0.5.
Preferably, the physical mechanical process is a ball milling process; during ball milling, the rotating speed is 200-.
The invention also provides application of the metal grid transparent conductive film prepared by the method in a transparent flexible display screen.
Has the advantages that:
the invention provides a preparation method of a metal grid transparent conductive film, which is formed by filling copper/aluminum composite conductive ink into grooves of a transparent colloidal layer on a transparent polyimide substrate and then sintering.
The prepared metal grid transparent conductive film greatly improves the adhesion between the metal grid and the transparent polyimide as the substrate on the base material without influencing the conductivity. The metal grid transparent conductive film prepared by the preparation method can be used for transparent display screens such as curtain wall glass.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
The preparation method of the metal grid transparent conductive film comprises the following steps:
(1) coating UV curing impression glue with the thickness of 8 microns on a transparent polyimide substrate with the thickness of 80 microns, and performing ultraviolet curing to form a transparent colloidal layer with a deep groove of 5 microns; (2) and filling copper/aluminum composite conductive ink in the groove network, and performing flash sintering.
Preparing copper/aluminum composite conductive ink:
s1, preparing copper nanoparticle ink: dispersing 10 parts of copper nanoparticles (with the diameter of 80nm) into 6 parts of terpineol solution containing acrylic resin, adding 0.1 part of ethyl cellulose, and uniformly stirring to obtain copper nanoparticle ink;
s2, preparing aluminum nanoparticle ink: dispersing 2.5 parts of aluminum nanoparticles (with the diameter of 60nm) into 2 parts of terpineol solution containing acrylic resin, adding 0.05 part of ethyl cellulose, and uniformly stirring to obtain aluminum nanoparticle ink;
s3, preparing copper/aluminum composite conductive ink: ball-milling the copper nanoparticle ink and the aluminum nanoparticle ink at the rotating speed of 200r/min for 4 hours to obtain copper/aluminum nanoparticle ink; wherein the mass ratio of the acrylic resin to the terpineol is 1:5, and the molecular weight of the acrylic resin is 10000.
Example 2
The preparation method of the metal grid transparent conductive film comprises the following steps:
(1) coating UV curing impression glue with the thickness of 5 microns on a transparent polyimide substrate with the thickness of 80 microns, and performing ultraviolet curing to form a transparent colloidal layer with a deep groove of 3 microns; (2) and filling copper/aluminum composite conductive ink in the groove network, and performing flash sintering.
Preparing copper/aluminum composite conductive ink:
s1, preparing copper nanoparticle ink: dispersing 10 parts of copper nanoparticles (with the diameter of 120nm) into 8 parts of terpineol solution containing acrylic resin, adding 0.2 part of polyethylene, and uniformly stirring to obtain copper nanoparticle ink;
s2, preparing aluminum nanoparticle ink: dispersing 2.5 parts of aluminum nano particles (with the diameter of 100nm) into 2.5 parts of terpineol solution containing acrylic resin, adding 0.1 part of polyethylene, and uniformly stirring to obtain aluminum nano particle ink;
s3, preparing copper/aluminum composite conductive ink: ball-milling the copper nanoparticle ink and the aluminum nanoparticle ink at the rotating speed of 300r/min for 3h to obtain copper/aluminum nanoparticle ink; wherein the mass ratio of the acrylic resin to the terpineol is 1:4, and the molecular weight of the acrylic resin is 50000.
Example 3
Same as in example 1, except that the protectant was replaced with "PVP" from "acrylic resin".
Comparative example 1
The preparation method of the metal grid transparent conductive film comprises the following steps:
(1) coating UV curing impression glue with the thickness of 8 microns on a transparent polyimide substrate with the thickness of 80 microns, and performing ultraviolet curing to form a transparent colloidal layer with a deep groove of 5 microns; (2) and filling nano copper conductive ink in the groove network, and performing flash sintering.
Preparing nano copper conductive ink: dispersing 10 parts of copper nanoparticles (with the diameter of 80nm) into 6 parts of terpineol solution containing acrylic resin, adding 0.1 part of ethyl cellulose, and uniformly stirring to obtain nano-copper conductive ink; wherein the mass ratio of the acrylic resin to the terpineol is 1:5, and the molecular weight of the acrylic resin is 10000.
And (3) performance testing:
1. square resistance: measuring by adopting a four-probe tester;
2. adhesion force: adhesion ratings were determined using the Baige test method according to ASTM D3359. The test results are shown in table 1 below.
TABLE 1 Square resistance and adhesion test results
| Square resistance (omega/□) | Adhesion force | |
| Example 1 | 5.18 | 5B |
| Example 2 | 5.33 | 5B |
| Example 3 | 5.86 | 3B |
| Comparative example 1 | 5.12 | 1B |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A preparation method of a metal grid transparent conductive film is characterized by comprising the following steps: (1) coating UV curing impression glue on the transparent polyimide substrate, and carrying out ultraviolet curing to obtain a transparent colloidal layer with a groove network; (2) filling copper/aluminum composite conductive ink in the groove network, and sintering;
the copper/aluminum composite conductive ink comprises copper nanoparticles and aluminum nanoparticles, and the mass ratio of the copper nanoparticles to the aluminum nanoparticles is 3-5: 1.
2. The method for preparing a metal mesh transparent conductive film according to claim 1, wherein the diameter of the copper nanoparticles is 30 to 180 nm; the diameter of the aluminum nanoparticles is 30-180 nm.
3. The method for preparing a metal grid transparent conductive film according to claim 1 or 2, wherein the copper/aluminum composite conductive ink is prepared by the following method:
s1, preparing copper nanoparticle ink: dispersing copper nanoparticles into terpineol solution containing a protective agent, adding an adhesive, and uniformly stirring to obtain copper nanoparticle ink;
s2, preparing aluminum nanoparticle ink: dispersing aluminum nano particles into terpineol solution containing a protective agent, adding an adhesive, and uniformly stirring to obtain aluminum nano particle ink;
s3, preparing copper/aluminum composite conductive ink: and mixing the copper nanoparticle ink and the aluminum nanoparticle ink by adopting a physical mechanical method to obtain the copper/aluminum composite conductive ink.
4. The method for preparing a metal grid transparent conductive film according to claim 3, wherein the protective agent is acrylic resin or PVP; preferably, acrylic resin.
5. The method for preparing a metal grid transparent conductive film according to claim 3 or 4, wherein the adhesive is ethyl cellulose or polyethylene.
6. The method for preparing a metal grid transparent conductive film according to any one of claims 3 to 5, wherein in the copper nanoparticle ink, the mass ratio of the copper nanoparticles to the protective agent to the terpineol to the adhesive is 10:1-2:5-8: 0.1-0.3; in the aluminum nanoparticle ink, the mass ratio of aluminum nanoparticles to a protective agent to terpineol to an adhesive is 10:2-4:8-10: 0.2-0.5.
7. The method for preparing a metal mesh transparent conductive film according to any one of claims 3 to 6, wherein the physical mechanical method is a ball milling method; during ball milling, the rotating speed is 200-.
8. Use of the metal mesh transparent conductive film obtained by the preparation method according to any one of claims 1 to 7 in a transparent flexible display screen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110345126.2A CN113284668A (en) | 2021-03-31 | 2021-03-31 | Preparation method and application of metal grid transparent conductive film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110345126.2A CN113284668A (en) | 2021-03-31 | 2021-03-31 | Preparation method and application of metal grid transparent conductive film |
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| Publication Number | Publication Date |
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| CN113284668A true CN113284668A (en) | 2021-08-20 |
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| CN202110345126.2A Pending CN113284668A (en) | 2021-03-31 | 2021-03-31 | Preparation method and application of metal grid transparent conductive film |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146260A (en) * | 2013-03-20 | 2013-06-12 | 中国人民解放军国防科学技术大学 | Conductive printing ink composition, conductive film layer as well as preparation method of conductive film layer and application of conductive printing ink composition |
| US20150008014A1 (en) * | 2013-02-05 | 2015-01-08 | Nanchang O-Film Tech. Co., Ltd. | Conductive film and preparation method thereof |
| KR20170006249A (en) * | 2015-07-06 | 2017-01-17 | 한국전자통신연구원 | Method for manufacturing transparent electrode |
| JP2017078207A (en) * | 2015-10-20 | 2017-04-27 | 公立大学法人 滋賀県立大学 | Silver nanowire and manufacturing method thereof as well as fluid dispersion and ink |
| CN108417295A (en) * | 2018-01-17 | 2018-08-17 | 深圳市易快来科技股份有限公司 | A kind of transparent conductive film and preparation method thereof |
| JP2018180622A (en) * | 2017-04-04 | 2018-11-15 | 三菱製紙株式会社 | Conductive material laminate |
| CN110473655A (en) * | 2018-05-10 | 2019-11-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of transparent conductive film and preparation method thereof |
-
2021
- 2021-03-31 CN CN202110345126.2A patent/CN113284668A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150008014A1 (en) * | 2013-02-05 | 2015-01-08 | Nanchang O-Film Tech. Co., Ltd. | Conductive film and preparation method thereof |
| CN103146260A (en) * | 2013-03-20 | 2013-06-12 | 中国人民解放军国防科学技术大学 | Conductive printing ink composition, conductive film layer as well as preparation method of conductive film layer and application of conductive printing ink composition |
| KR20170006249A (en) * | 2015-07-06 | 2017-01-17 | 한국전자통신연구원 | Method for manufacturing transparent electrode |
| JP2017078207A (en) * | 2015-10-20 | 2017-04-27 | 公立大学法人 滋賀県立大学 | Silver nanowire and manufacturing method thereof as well as fluid dispersion and ink |
| JP2018180622A (en) * | 2017-04-04 | 2018-11-15 | 三菱製紙株式会社 | Conductive material laminate |
| CN108417295A (en) * | 2018-01-17 | 2018-08-17 | 深圳市易快来科技股份有限公司 | A kind of transparent conductive film and preparation method thereof |
| CN110473655A (en) * | 2018-05-10 | 2019-11-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of transparent conductive film and preparation method thereof |
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Application publication date: 20210820 |