CN109080281B - Method for preparing flexible transparent conductive film based on wetting substrate fine ink-jet printing - Google Patents
Method for preparing flexible transparent conductive film based on wetting substrate fine ink-jet printing Download PDFInfo
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- CN109080281B CN109080281B CN201810911529.7A CN201810911529A CN109080281B CN 109080281 B CN109080281 B CN 109080281B CN 201810911529 A CN201810911529 A CN 201810911529A CN 109080281 B CN109080281 B CN 109080281B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/0041—Digital printing on surfaces other than ordinary paper
- B41M5/0047—Digital printing on surfaces other than ordinary paper by ink-jet printing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The invention provides a method for preparing a flexible transparent conductive film based on fine inkjet printing of a wetting substrate, which comprises the following steps: s1, preparing conductive polymer/carbon material composite ink; s2, obtaining the viscoelastic substrate surface of the high-precision semi-embedded structure: uniformly adding an initiator through thermosetting polydimethylsiloxane to form a high-precision semi-embedded structure; s3, completing preparation of the flexible transparent conductive film based on the viscoelastic substrate: and injecting the prepared conductive polymer/carbon material composite ink into an ink box of a printer, and performing ink-jet printing on the surface of the semi-embedded viscoelastic substrate by adopting a fine spray head to obtain the flexible transparent conductive film. The invention researches the wetting and extruding behavior of the fluidity of the viscoelastic substrate to the ink drop of the ink-jet printing in the volatilization, drying and deposition process by using the composite enhanced functional conductive ink to obtain the mechanism of forming a high-precision semi-embedded point and a line structure by controllable deposition of the ink drop, and realizes the fine printing of the high-performance flexible transparent conductive film.
Description
Technical Field
The invention relates to the field of ink-jet printing, in particular to a preparation method of a flexible transparent conductive film.
Background
With the development of portability of photoelectric devices, flexible electronic devices, such as flexible solar cells, flexible touch screens, wearable devices, and the like, have attracted wide attention. Transparent conductive films have good electrical conductivity and optical transparency, and have become an indispensable component in the manufacture of optoelectronic functional devices. Currently, Indium Tin Oxide (ITO), a widely used transparent conductive material, has excellent light transmittance and good conductivity, so that ITO has been used as a transparent conductive material in the fields of touch display and light-emitting illumination. However, with the rapid increase of the demand of touch panels, ITO faces the problems of world resource shortage, complex processing, high energy consumption, and the like. Meanwhile, as an oxide, the ITO has high brittleness and poor flexibility, and the requirements of the new generation of touch display technology on the flexibility, the bendability and the like of products are difficult to meet. Therefore, a new transparent conductive flexible material capable of replacing ITO is a hot spot in the current display field. In recent years, researchers begin to apply metals, carbon materials and the like to the preparation of flexible transparent conductive films, and flexible transparent films prepared by using chemical vapor deposition, suction filtration, coating and other methods based on materials such as metal nanowires, carbon nanotubes, graphene, conductive polymers and the like have been well applied to touch screens, intelligent glass, photovoltaic devices and the like. However, these methods often have problems such as post-treatment, introduction of defects, and unstable performance in order to improve light transmittance and conductivity during the preparation of the flexible transparent conductive film, and it is difficult to realize large-area preparation of a high-quality flexible transparent conductive film.
In the current research, the patterning of the conductive material to form a high-precision grid provides a new idea for the preparation of the transparent conductive film. However, the fine grid structure prepared by patterning the conductive material is often present on the surface of the patterned substrate, and the flexibility and adhesion between the conductive structure and the substrate are difficult to meet the application requirements of the flexible transparent conductive film. Meanwhile, the preparation of the high-precision grid structure needs methods such as template and photoetching, the process is complex, and the production cost is high.
In recent years, the research of the inkjet printing technology in the patterning of functional materials has received much attention. Compared with the traditional functional material patterning technology, the ink-jet printing technology is to directly deposit the ink in a specific area, does not need a mask and exposure etching, can realize rapid large-area preparation, saves the cost and greatly reduces the pollution. Currently, inkjet printing technology has made important progress in green plate making, transparent conductive films, organic semiconductors, light emitting diodes, photovoltaic devices, microchips, RFID antennas, sensors, and 3D microfabrication.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention utilizes the composite enhanced functional conductive ink and the viscoelastic substrate to solve the problems in the prior art and realize the method for finely printing the high-performance flexible transparent conductive film.
Specifically, the invention provides a method for preparing a flexible transparent conductive film based on the fine inkjet printing of a wettable substrate, which comprises the following steps:
s1, preparing the conductive polymer/carbon material composite ink: carbon nanotubes are prepared in a volume ratio of 1: 1, carrying out ultrasonic treatment in concentrated nitric acid and concentrated hydrochloric acid to remove catalyst and metal impurity particles, partially oxidizing carbon nano tubes, then grafting carboxyl and hydroxyl groups, carrying out subsequent treatment to obtain sulfonated carbon nano tubes, dispersing the sulfonated carbon nano tubes in a polar solvent dimethyl sulfoxide, introducing the sulfonated carbon nano tubes into polyethylene dioxythiophene-polystyrene sulfonate in a solution blending mode, and further carrying out ultrasonic treatment to form uniform dispersion liquid so as to obtain conductive polymer/carbon material composite ink;
s2, obtaining the viscoelastic substrate surface of the high-precision semi-embedded structure: uniformly adding an initiator into thermosetting polydimethylsiloxane, spin-coating or extruding the mixture to prepare a liquid elastic prepolymer oily substrate, precuring for a certain time to obtain a fluid substrate with proper viscoelasticity, and forming a high-precision semi-embedded structure by utilizing the wetting and extruding behavior of the viscoelastic polydimethylsiloxane substrate on ink-jet printing ink drops, wherein the semi-embedded structure extrudes a conductive material subjected to ink-jet printing to form a semi-wrapped circuit existing in the surface layer of the polydimethylsiloxane;
s3, completing preparation of the flexible transparent conductive film based on the viscoelastic substrate: and injecting the prepared conductive polymer/carbon material composite ink into an ink box of a printer, and performing ink-jet printing on the surface of the semi-embedded viscoelastic substrate by adopting a fine spray head to obtain the flexible transparent conductive film.
Preferably, the initiator added in step S2 is a prepolymer with vinyl side chains.
Preferably, the mass ratio of the polydimethylsiloxane to the initiator is 15:1-10: 1.
Preferably, the subsequent processing in step S1 includes heating, dilution, washing, and cool drying.
Preferably, the time of the ultrasonic treatment in step S1 is 1 hour.
Preferably, the time for pre-curing in step S2 is 8-10 minutes.
Preferably, the temperature of the pre-curing in step S2 is 80-100 degrees celsius.
Compared with the prior art, the invention has the following beneficial effects:
the invention researches the wetting and extruding behavior of the fluidity of the viscoelastic substrate to the ink drop of the ink-jet printing in the volatilization, drying and deposition process by using the composite enhanced functional conductive ink to obtain the mechanism of forming a high-precision semi-embedded point and a line structure by controllable deposition of the ink drop, and realizes the fine printing of the high-performance flexible transparent conductive film. The conductive polymer/carbon material composite ink, the flexible transparent substrate and the fine ink-jet printing patterning technology are organically combined, so that the large-area preparation method of the flexible transparent conductive film with low cost and high efficiency is realized. The defects that the traditional method has poor bending resistance, complex process, difficulty in realizing large-area preparation and the like in the preparation of the flexible transparent conductive film are overcome.
Drawings
FIG. 1 is a schematic diagram of the structure of PEDOT: PSS in accordance with the present invention;
FIG. 2 is a schematic diagram of preparing a PEDOT PSS/CNT composite conductive ink according to the present invention;
FIG. 3 is a schematic diagram of an inkjet printing high precision semi-embedded structure according to the present invention;
FIG. 4 is a schematic flow chart of the present invention.
Detailed Description
Exemplary embodiments, features and aspects of the present invention will be described in detail below with reference to the accompanying drawings. In the drawings, like reference numbers can indicate functionally identical or similar elements. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The invention provides a method for preparing a flexible transparent conductive film based on fine inkjet printing of a wetting substrate, which comprises the following steps as shown in FIG. 4:
s1, preparing the conductive polymer/carbon material composite ink: the implementation content is to prepare PEDOT-PSS/CNT composite ink, the conductive polymer can conduct electricity, and the graph shown in the attached figure 1 is that a large amount of p-pi conjugated structures or pi-pi conjugated structures exist on the polymer chain. These conjugated structures delocalize the electrons together, and when a directed electric field is applied, the carriers can move freely throughout the polymer chains.
As shown in fig. 2, the specific method is to mix carbon nanotubes in a volume ratio of 1: 1, carrying out ultrasonic treatment in concentrated nitric acid and concentrated hydrochloric acid to remove catalyst and metal impurity particles, partially oxidizing carbon nano tubes, then grafting carboxyl and hydroxyl groups, carrying out subsequent treatment to obtain sulfonated carbon nano tubes, dispersing the sulfonated carbon nano tubes in a polar solvent dimethyl sulfoxide (DMSO), introducing the sulfonated carbon nano tubes into polyethylene dioxythiophene-polystyrene sulfonate in a solution blending mode, and further carrying out ultrasonic treatment to form uniform dispersion liquid to obtain the conductive polymer/carbon material composite ink.
S2, obtaining the viscoelastic substrate surface of the high-precision semi-embedded structure: as shown in fig. 3, a liquid elastic prepolymer oily substrate is prepared by uniformly adding an initiator through thermosetting polydimethylsiloxane, spin-coating or extruding the mixture, precuring for a certain time to obtain a fluid substrate with appropriate viscoelasticity, and a high-precision semi-embedded structure is formed by utilizing the wetting and extruding behavior of the viscoelastic polydimethylsiloxane substrate on ink-jet printing ink drops, wherein the semi-embedded structure extrudes a conductive material subjected to ink-jet printing to form a semi-wrapped line in the surface layer of the polydimethylsiloxane.
In the specific embodiment, through thermosetting polydimethylsiloxane, initiators are uniformly added, precuring is carried out for a certain time, fluid substrates with different viscoelasticity are obtained, and the high-precision semi-embedded structure is formed by utilizing the wetting and extruding behavior of the viscoelastic polydimethylsiloxane substrate on ink-jet printing ink drops.
S3, completing preparation of the flexible transparent conductive film based on the viscoelastic substrate: and injecting the prepared conductive polymer/carbon material composite ink into an ink box of a printer, and performing ink-jet printing on the surface of the semi-embedded viscoelastic substrate by adopting a fine spray head to obtain the flexible transparent conductive film.
Ink-jet printing is used as a new molding technology, electronic ink is sprayed on a substrate by utilizing a piezoelectric principle, and then annealing and deposition are carried out to form a film, so that an organic thin film in an organic device is obtained. The production can be directly controlled by a digital system control driving mode, and the waste of materials is reduced by an ink-jet on demand mode.
Preferably, the initiator added in step S2 is a prepolymer with vinyl side chains.
Preferably, the mass ratio of the polydimethylsiloxane to the initiator is 15:1-10: 1.
Preferably, the subsequent processing in step S1 includes heating, dilution, washing, and cool drying.
Preferably, the time of the ultrasonic treatment in step S1 is 1 hour.
Preferably, the time for pre-curing in step S2 is 8-10 minutes.
Implementation example:
1. preparing conductive polymer/carbon material composite ink: the mass ratio of each substance is as follows:
DMSO:80％
PEDOT:PSS：10％
sulfonated carbon nanotubes: 10 percent of
Carbon nanotubes are prepared in a volume ratio of 1: 1, carrying out ultrasonic treatment in concentrated nitric acid and concentrated hydrochloric acid to remove catalyst and metal impurity particles, partially oxidizing carbon nano tubes, then grafting carboxyl and hydroxyl groups, carrying out subsequent treatment to obtain sulfonated carbon nano tubes, dispersing the sulfonated carbon nano tubes in a polar solvent dimethyl sulfoxide, introducing the sulfonated carbon nano tubes into polyethylene dioxythiophene-polystyrene sulfonate in a solution blending mode, and further carrying out ultrasonic treatment to form uniform dispersion liquid so as to obtain conductive polymer/carbon material composite ink;
2. obtaining a viscoelastic substrate surface of a high-precision semi-embedded structure: the mass ratio of each substance is as follows:
PDMS: curing agent 10:1
Obtaining a viscoelastic substrate surface of a high-precision semi-embedded structure: the preparation method comprises the steps of uniformly adding an initiator into thermosetting polydimethylsiloxane, spin-coating or extruding the mixture to prepare a liquid elastic prepolymer oily substrate, precuring for 8 minutes at a curing temperature of 80 ℃ to obtain a fluid substrate with proper viscoelasticity, and forming a high-precision semi-embedded structure by utilizing the wetting and extruding behavior of the viscoelastic polydimethylsiloxane substrate on ink-jet printing ink drops, wherein the semi-embedded structure extrudes a conductive material subjected to ink-jet printing to form a semi-wrapped circuit to be present in the surface layer of the polydimethylsiloxane.
3. And injecting the prepared conductive polymer/carbon material composite ink into an ink box of a printer, and performing ink-jet printing on the surface of the semi-embedded viscoelastic substrate by adopting a fine spray head to obtain the flexible transparent conductive film. The dot pitch for ink jet printing was 20 microns and the diameter of the ink jet nozzle was 40 microns.
The invention researches the wetting and extruding behavior of the fluidity of the viscoelastic substrate to the ink drop of the ink-jet printing in the volatilization, drying and deposition process by using the composite enhanced functional conductive ink to obtain the mechanism of forming a high-precision semi-embedded point and a line structure by controllable deposition of the ink drop, and realizes the fine printing of the high-performance flexible transparent conductive film.
Finally, it should be noted that: the above-mentioned embodiments are only used for illustrating the technical solution of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. A method for preparing a flexible transparent conductive film based on the fine inkjet printing of a wettable substrate is characterized by comprising the following steps: which comprises the following steps:
s1, preparing the conductive polymer/carbon material composite ink: carbon nanotubes are prepared in a volume ratio of 1: 1, carrying out ultrasonic treatment in concentrated nitric acid and concentrated hydrochloric acid to remove catalyst and metal impurity particles, partially oxidizing carbon nano tubes, then grafting carboxyl and hydroxyl groups, carrying out subsequent treatment to obtain sulfonated carbon nano tubes, dispersing the sulfonated carbon nano tubes in a polar solvent dimethyl sulfoxide, introducing the sulfonated carbon nano tubes into polyethylene dioxythiophene-polystyrene sulfonate in a solution blending mode, and further carrying out ultrasonic treatment to form uniform dispersion liquid so as to obtain conductive polymer/carbon material composite ink;
s2, obtaining the viscoelastic substrate surface of the high-precision semi-embedded structure: uniformly adding an initiator into thermosetting polydimethylsiloxane, spin-coating or extruding the mixture to prepare a liquid elastic prepolymer oily substrate, precuring for a certain time to obtain a fluid substrate with proper viscoelasticity, and forming a high-precision semi-embedded structure by utilizing the wetting and extruding behavior of the viscoelastic polydimethylsiloxane substrate on ink-jet printing ink drops, wherein the semi-embedded structure extrudes a conductive material subjected to ink-jet printing to form a semi-wrapped circuit existing in the surface layer of the polydimethylsiloxane;
s3, completing preparation of the flexible transparent conductive film based on the viscoelastic substrate: and injecting the prepared conductive polymer/carbon material composite ink into an ink box of a printer, and performing ink-jet printing on the surface of the semi-embedded viscoelastic substrate by adopting a fine spray head to obtain the flexible transparent conductive film.
2. The method for preparing a flexible transparent conductive film based on the fine inkjet printing of the wettable substrate as claimed in claim 1, wherein: the initiator added in step S2 is a prepolymer with vinyl side chains.
3. The method for preparing a flexible transparent conductive film based on the fine inkjet printing of the wettable substrate as claimed in claim 2, wherein: the mass ratio of the polydimethylsiloxane to the initiator is 15:1-10: 1.
4. The method for preparing a flexible transparent conductive film based on the fine inkjet printing of the wettable substrate as claimed in claim 1, wherein: the subsequent processing in step S1 includes heating, dilution, washing, and cool drying.
5. The method for preparing a flexible transparent conductive film based on the fine inkjet printing of the wettable substrate as claimed in claim 1, wherein: the time of the ultrasonic treatment in step S1 was 1 hour.
6. The method for preparing a flexible transparent conductive film based on the fine inkjet printing of the wettable substrate as claimed in claim 1, wherein: the time for precuring in step S2 is 8 to 10 minutes.
7. The method for preparing a flexible transparent conductive film based on the fine inkjet printing of the wettable substrate as claimed in claim 1, wherein: the temperature of the pre-curing in the step S2 is 80-100 ℃.
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| CN107969066B (en) * | 2017-12-06 | 2019-10-29 | 齐鲁工业大学 | The method for preparing stretchable circuit using oil-water interfaces reaction inkjet printing |
| CN110014764B (en) * | 2018-01-09 | 2020-07-24 | 厦门大学 | Liquid-liquid printing method |
| CN111554833B (en) * | 2020-06-02 | 2023-11-07 | 齐鲁工业大学 | Preparation method of flexible transparent electroluminescent film and display |
| CN114158148A (en) * | 2021-11-16 | 2022-03-08 | 西湖大学 | Preparation method and application of 3D printing transparent electric heating electrode |
| CN114136506A (en) * | 2021-11-22 | 2022-03-04 | 武汉工程大学 | Preparation and recovery method of stress sensor |
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