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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- 238000007641 inkjet printing Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000009736 wetting Methods 0.000 title description 9
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 21
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 19
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 17
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Images
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Manufacturing Of Electric Cables (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Non-Insulated Conductors (AREA)
Abstract
本发明提供一种基于浸润性基底精细喷墨打印制备柔性透明导电膜的方法，其包括以下步骤：S1、制备导电高分子/碳材料复合墨水；S2、获取高精度半嵌入结构的粘弹性基底表面：通过热固化型的聚二甲基硅氧烷，均匀添加引发剂形成高精度的半嵌入结构；S3、完成基于粘弹性基底的柔性透明导电膜制备：将制备的导电高分子/碳材料复合墨水注入打印机墨盒，采用精细喷头在半嵌入结构的粘弹性基底表面进行喷墨打印得到柔性透明导电膜。本发明利用复合增强的功能性导电墨水，研究粘弹性基底的流动性对喷墨打印墨滴在挥发干燥沉积过程中的浸润挤压行为，得出墨滴可控沉积形成高精度半嵌入点、线结构的机理，实现精细打印高性能柔性透明导电膜。
The present invention provides a method for preparing a flexible transparent conductive film based on fine inkjet printing of a wettable substrate, which comprises the following steps: S1, preparing a conductive polymer/carbon material composite ink; S2, obtaining a viscoelastic substrate with a high-precision semi-embedded structure Surface: Heat-curable polydimethylsiloxane is used to uniformly add initiators to form a high-precision semi-embedded structure; S3. Complete the preparation of a flexible transparent conductive film based on a viscoelastic substrate: the prepared conductive polymer/carbon material The composite ink is injected into a printer cartridge, and a flexible transparent conductive film is obtained by inkjet printing on the surface of the semi-embedded viscoelastic substrate by using a fine nozzle. The invention utilizes the composite-enhanced functional conductive ink to study the infiltration and extrusion behavior of the ink-jet printing ink droplets by the fluidity of the viscoelastic substrate during the volatilization drying deposition process, and obtains the controllable deposition of the ink droplets to form high-precision semi-embedded dots, The mechanism of the wire structure realizes fine printing of high-performance flexible transparent conductive films.
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)
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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 |
| CN115893304B (en) * | 2022-11-10 | 2025-06-03 | 齐鲁工业大学(山东省科学院) | A preparation method and application of a flexible concave microstructure surface based on direct writing printing |
| CN116533549A (en) * | 2023-02-17 | 2023-08-04 | 郑州大学 | Preparation method of flexible strain sensor with braided grid |
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| CN101465409A (en) * | 2008-12-31 | 2009-06-24 | 电子科技大学 | Substrate for flexible organic optoelectronic device and preparation method thereof |
| CN102616033A (en) * | 2012-04-13 | 2012-08-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for quickly manufacturing high-light-transmission conductive patterns |
| CN104240798A (en) * | 2014-09-25 | 2014-12-24 | 上海交通大学 | Transparent conductive film and preparation method thereof |
| KR20180015860A (en) * | 2016-08-04 | 2018-02-14 | 연세대학교 산학협력단 | Method for manufacturing flexible transparent electrode substrate using polymer film and flexible transparent electrode substrate manufactured by the same |
| CN107093500A (en) * | 2017-03-30 | 2017-08-25 | 华南理工大学 | A kind of graphic method of nano silver wire flexible transparent conductive film |
| CN107770948A (en) * | 2017-09-28 | 2018-03-06 | 重庆秉为科技有限公司 | A kind of manufacture method of flexible PCB |
| CN107993747A (en) * | 2017-11-23 | 2018-05-04 | 清华大学深圳研究生院 | A kind of nesa coating, conductive structure and preparation method thereof |
| CN108063001A (en) * | 2017-12-07 | 2018-05-22 | 南京邮电大学 | A kind of membrane electrode and preparation method thereof and application |
| CN108337813A (en) * | 2018-01-08 | 2018-07-27 | 南京邮电大学 | A kind of method of high-precision ink jet printing flexible circuit |
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