CN113362991A - Transparent conductive film and preparation method and application thereof - Google Patents
Transparent conductive film and preparation method and application thereof Download PDFInfo
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- CN113362991A CN113362991A CN202110626144.8A CN202110626144A CN113362991A CN 113362991 A CN113362991 A CN 113362991A CN 202110626144 A CN202110626144 A CN 202110626144A CN 113362991 A CN113362991 A CN 113362991A
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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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- 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
Abstract
The invention discloses a transparent conductive film and a preparation method and application thereof, in particular to a preparation method of a silver nanowire transparent conductive film, which comprises the following steps of firstly coating a silver nanowire dispersion liquid on the surface of a transparent substrate, and volatilizing a solvent; then, coating a silane coupling agent on the surface of the silver nanowire network, soaking the silver nanowire network in an alkaline aqueous solution, preserving the temperature for 1-60min at 30-100 ℃, and carrying out in-situ hydrolysis and polycondensation on the silane coupling agent to form a compact silicon dioxide coating layer on the surface of the nanowire; and finally, drying to obtain the silver nanowire transparent conductive film. The method has the advantages of simple process and low cost, and the prepared silver nanowire transparent conductive film has excellent sulfuration resistance, silver ion migration resistance, acid and alkali resistance and high-temperature stability.
Description
Technical Field
The invention relates to the field of conductive films, in particular to a transparent conductive film and a preparation method thereof.
Background
Modern electronic products are rapidly developing in the direction of miniaturization, light weight, thinness, intellectualization and flexible wearability. The transparent electrode is used as a key component of a flexible optoelectronic device and is widely applied to the fields of touch screens, displays, LEDs, solar cells, electromagnetic shielding, even energy sources and the like. At present, the mainstream transparent electrode material indium-doped tin oxide (ITO) has the defects of brittle quality, complex process, limited indium storage capacity, high energy consumption, high cost and the like, and is increasingly difficult to meet the requirements of the currently popular flexible wearable electronic products. In recent years, researchers have developed several new transparent electrode materials to replace ITO, such as: the transparent conductive film is prepared from graphene, carbon nano tubes, conductive polymers, silver grids, silver nanowires and the like. In comprehensive comparison, silver nanowires, typically transparent conductive films such as silver nanowires, have the advantages of excellent electrical, optical and mechanical properties, simple process, low cost and the like, and are considered to be the most potential alternative materials for ITO. However, sulfidation and silver ion migration have become key issues affecting the stability of silver nanowire transparent conductive films. It is common in the industry to add polymers or some additives to the silver nanowire dispersion and to coat the surface of the silver nanowire conductive network with a surface coating to inhibit or retard silver nanowire sulfidation and silver ion migration. However, these methods increase components of the silver nanowire ink formulation, thereby increasing costs, may cause environmental pollution, and have no significant effect on the inhibition of silver nanowire sulfidation and silver ion migration.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a silver nanowire transparent conductive film. The method has simple process and low cost, and the prepared silver nanowire transparent conductive film has excellent sulfuration resistance, ion migration resistance, acid and alkali resistance and high temperature resistance.
One aspect of the present invention provides a method for preparing a transparent conductive film, comprising the steps of:
1) coating the silver nanowire dispersion liquid on the surface of a transparent substrate, and volatilizing a solvent;
2) coating a silane coupling agent on the surface of the silver nanowire;
3) soaking in alkaline aqueous solution, and keeping the temperature at 30-100 deg.C;
4) and drying to obtain the silver nanowire transparent conductive film.
Further, in step 1), the solvent in the silver nanowire dispersion is at least one selected from deionized water, methanol, absolute ethyl alcohol, isopropanol, n-butanol, n-methylpyrrolidone, n-N-dimethylformamide, acetone, butanone, ethyl acetate or butyl acetate, preferably isopropanol.
Further, in step 1) or 2), the coating process is selected from one of wire bar coating, doctor blade coating, spin coating, spray coating, curtain coating, dip coating, micro gravure printing, slit extrusion, or screen printing.
Further, in step 1), the transparent substrate is selected from one of polyethylene terephthalate (PET), cycloolefin polymer (COP), polyethylene naphthalate (PEN), transparent polyimide (CPI), polymethyl methacrylate (PMMA), Polycarbonate (PC), or a glass plate.
Further, in the step 2), the silane coupling agent is selected from at least one of vinyl silane, epoxy silane, amino silane, mercapto silane, methacryloxy silane, methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
Further, in the step 3), the alkaline aqueous solution is selected from at least one of aqueous ammonia, aqueous sodium hydroxide, aqueous potassium hydroxide or aqueous sodium carbonate, and the pH of the alkaline aqueous solution is 8-12. For example, pH values of 8, 9, 10, 11, 12.
Further, in step 3), the temperature range is 30-100 ℃, preferably 50-80 ℃, for example 55 ℃, 60 ℃, 65 ℃, 70 ℃ and 75 ℃.
Further, in the step 4), the heat preservation time at 30-100 ℃ is 1-120min, preferably 20-60min, such as 10min, 20min, 30min, 40min, 50min, 60 min.
In another aspect of the invention, the transparent conductive film prepared by the above method of the invention is provided.
Further, the transparent conductive film is subjected to vulcanization treatment for 500 hours, wherein the sheet resistance change of the conductive film is less than or equal to 5%, preferably less than or equal to 1%; treating with 30V DC voltage for 500h to make the sheet resistance of the conductive film have a variation of 6% or less, preferably 1% or less; treating with 10% hydrochloric acid solution for 1000h to obtain conductive film with sheet resistance variation of 8% or less, preferably 1% or less; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with sheet resistance variation of 9% or less, preferably 1% or less; the sheet resistance change of the conductive film is less than 10%, preferably less than 4% by treating at 300 ℃ for 30 min.
In still another aspect, the present invention provides a use of the above transparent conductive film as an electrode material.
The invention also provides a method for improving the acid and alkali resistance, high temperature resistance and sulfuration resistance of the transparent electrode material, which comprises the steps of coating a silane coupling agent on the surface with silver nanowires, soaking the silver nanowires in an alkaline aqueous solution, and keeping the temperature at 30-100 ℃; and finally, drying to obtain the silver nanowire transparent conductive film.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1) according to the invention, the surface of the silver nanowire conductive network is coated with the silane coupling agent, and the silane coupling agent is subjected to in-situ hydrolysis and polycondensation in an alkaline aqueous solution, so that a compact silicon dioxide coating layer is formed on the surface of the silver nanowire, and the silicon dioxide shell layer can effectively block sulfide in the air and simultaneously hinder the transportation of silver ions, thereby remarkably improving the sulfuration resistance, silver ion migration resistance, high temperature and high pressure resistance of the silver nanowire transparent conductive film, and blocking the corrosion of acid and alkali to the silver nanowire to enhance the acid and alkali resistance.
2) The invention selects a special arrangement sequence, firstly arranges the silver nanowires and dries, then arranges the silane coupling agent, forms a film and then soaks in alkaline liquid, and the operation can minimally affect the distribution of the silver nanowires. And because the space of the silver nanowire is limited by the silicon dioxide shell layer, the silver nanowire is molten but is difficult to deform to form a granular shape or a rod shape with a larger diameter at high temperature, so that the original one-dimensional shape can be well kept, and the high-temperature stability of the silver nanowire is enhanced.
3) The transparent conductive film is vulcanized for 500 hours, the sheet resistance variation of the conductive film is less than 5%, and part of schemes can achieve less than 1%; 30V direct current voltage is processed for 500h, the sheet resistance variation of the conductive film is below 6%, and part of schemes can achieve below 1%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is below 8%, and part of the scheme can realize below 1%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with sheet resistance variation of 9% or less, and part of the scheme can achieve 1% or less; the sheet resistance change of the conductive film is less than 10% after the treatment at 300 ℃ for 30min, and part of the scheme can realize less than 4%.
Drawings
Fig. 1 is an SEM picture of a silver nanowire network on the surface of the transparent conductive film prepared in example 1.
Fig. 2 is an SEM picture of the silver nanowire network on the surface of the transparent conductive film prepared in example 2.
Fig. 3 is an SEM picture of the silver nanowire network on the surface of the transparent conductive film prepared in example 3.
Fig. 4 is an SEM picture of the silver nanowire network on the surface of the transparent conductive film prepared in example 4.
Fig. 5 is an SEM picture of the silver nanowire network on the surface of the transparent conductive film prepared in example 5.
Fig. 6 is an SEM picture of the silver nanowire network on the surface of the transparent conductive film prepared in example 6.
Fig. 7 is an SEM picture of the silver nanowire network on the surface of the transparent conductive film prepared in example 7.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below, but the present invention is not to be construed as being limited to the implementable range thereof.
Example 1
Firstly, coating a silver nanowire isopropanol dispersion liquid on the surface of PET (polyethylene terephthalate) by using a wire bar, and drying at 80 ℃ for 5min to volatilize a solvent; then, scraping ethyl orthosilicate on the surface of the silver nanowire network, soaking the silver nanowire network in a sodium hydroxide aqueous solution with the pH value of 10 at the temperature of 60 ℃, and preserving heat for 30 min; and finally, drying to obtain the silver nanowire transparent conductive film. Through transmission electron microscope tests, as shown in fig. 1, a silicon dioxide shell layer can be formed on the surface of the silver nanowire. Hydrogen sulfide treatment is carried out for 500 hours, and the sheet resistance variation of the conductive film is 0.2%; processing for 500 hours by using 30V direct current voltage, wherein the sheet resistance variation of the conductive film is 0.5%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is 0.7%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with sheet resistance variation of 0.5%; the sheet resistance of the conductive film is changed by 2 percent after being processed for 30min at 300 ℃.
Example 2
A silver nanowire transparent conductive film was prepared in the same manner as in example 1, except that the pH of the aqueous solution of sodium hydroxide was 12. Through transmission electron microscope tests, as shown in fig. 2, a silicon dioxide shell layer can be formed on the surface of the silver nanowire. Hydrogen sulfide treatment is carried out for 500 hours, and the sheet resistance variation of the conductive film is 0.3%; processing for 500h by using 30V direct current voltage, wherein the sheet resistance variation of the conductive film is 0.6%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is 0.6%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with sheet resistance variation of 0.5%; and (3) treating at 300 ℃ for 30min, wherein the sheet resistance variation of the conductive film is 4%.
Example 3
A silver nanowire transparent conductive film was prepared in the same manner as in example 1, except that the pH of the aqueous solution of sodium hydroxide was 8. Through transmission electron microscope tests, as shown in fig. 3, a silicon dioxide shell layer can be formed on the surface of the silver nanowire. Hydrogen sulfide treatment is carried out for 500 hours, and the sheet resistance variation of the conductive film is 0.1%; processing for 500 hours by using 30V direct current voltage, wherein the sheet resistance variation of the conductive film is 0.5%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is 0.5%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with sheet resistance variation of 0.8%; the sheet resistance of the conductive film is changed by 3 percent after being processed for 30min at 300 ℃.
Example 4
A silver nanowire transparent conductive film was prepared in the same manner as in example 1, except that the film was immersed in an aqueous solution of sodium hydroxide having a pH of 10 at 40 ℃. Through transmission electron microscope tests, as shown in fig. 4, a silicon dioxide shell layer can be formed on the surface of the silver nanowire. Hydrogen sulfide treatment is carried out for 500 hours, and the sheet resistance variation of the conductive film is 3%; processing for 500h by using 30V direct current voltage, wherein the sheet resistance variation of the conductive film is 2%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is 4%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with a sheet resistance variable of 5%; the sheet resistance of the conductive film is changed by 7 percent after being processed for 30min at 300 ℃.
Example 5
A silver nanowire transparent conductive film was prepared in the same manner as in example 1, except that the film was immersed in an aqueous solution of sodium hydroxide having a pH of 10 at 100 ℃. Through transmission electron microscope tests, as shown in fig. 5, a silicon dioxide shell layer can be formed on the surface of the silver nanowire. Hydrogen sulfide treatment is carried out for 500 hours, and the sheet resistance variation of the conductive film is 0.3%; processing for 500h by using 30V direct current voltage, wherein the sheet resistance variation of the conductive film is 0.2%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is 0.4%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with sheet resistance variation of 0.5%; the sheet resistance of the conductive film is changed by 6 percent after being processed for 30min at 300 ℃.
Example 6
A silver nanowire transparent conductive film was prepared in the same manner as in example 1, except that the film was immersed in a 60 ℃ aqueous solution of sodium hydroxide having a pH of 10 and heat-preserved for 5 min. Through transmission electron microscope tests, as shown in fig. 6, a silicon dioxide shell layer can be formed on the surface of the silver nanowire. Hydrogen sulfide treatment is carried out for 500 hours, and the sheet resistance variation of the conductive film is 5%; processing for 500h by using 30V direct current voltage, wherein the sheet resistance variation of the conductive film is 6%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is 8%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with a sheet resistance variable of 9%; the sheet resistance of the conductive film is changed by 10 percent after being processed for 30min at 300 ℃.
Example 7
A silver nanowire transparent conductive film was prepared in the same manner as in example 1, except that the film was immersed in a 60 ℃ aqueous solution of sodium hydroxide having a pH of 10 and heat-preserved for 60 min. Through transmission electron microscope tests, as shown in fig. 7, a silicon dioxide shell layer can be formed on the surface of the silver nanowire. Hydrogen sulfide treatment is carried out for 500 hours, and the sheet resistance variation of the conductive film is 0.1%; processing for 500h by using 30V direct current voltage, wherein the sheet resistance variation of the conductive film is 0.3%; treating with 10% hydrochloric acid solution for 1000h, wherein the sheet resistance variation of the conductive film is 0.4%; treating with 10% sodium hydroxide solution for 1000h to obtain a conductive film with sheet resistance variation of 0.7%; the sheet resistance of the conductive film is changed by 3 percent after being processed for 30min at 300 ℃.
The method disclosed by the invention is simple in preparation method and pollution-free in material, and can obviously reduce the preparation cost of the transparent conductive film and improve the preparation efficiency from the aspect of the sheet resistance change conditions of high temperature, vulcanization, acid-base treatment and high-pressure treatment, and the prepared conductive film has excellent electrical properties and corrosion resistance.
Claims (10)
1. A method for preparing a transparent conductive film is characterized by comprising the following steps:
1) coating the silver nanowire dispersion liquid on the surface of a transparent substrate, and volatilizing a solvent;
2) coating a silane coupling agent on the surface of the silver nanowire;
3) soaking in alkaline aqueous solution, and keeping the temperature at 30-100 deg.C;
4) and drying to obtain the silver nanowire transparent conductive film.
2. The method of claim 1, wherein in the step 1), the solvent in the silver nanowire dispersion is at least one selected from deionized water, methanol, absolute ethanol, isopropanol, n-butanol, N-methylpyrrolidone, N-dimethylformamide, acetone, butanone, ethyl acetate, and butyl acetate, preferably isopropanol.
3. The method according to claim 1), wherein in step 1) or 2), the coating process is selected from one of wire bar coating, blade coating, spin coating, spray coating, curtain coating, dip coating, micro gravure, slit extrusion, or screen printing.
4. The method of claim 1, wherein in the step 1), the transparent substrate is selected from one of polyethylene terephthalate (PET), cycloolefin polymer (COP), polyethylene naphthalate (PEN), transparent polyimide (CPI), polymethyl methacrylate (PMMA), Polycarbonate (PC), or a glass plate.
5. The method according to claim 1, wherein in the step 3), the basic aqueous solution is at least one selected from the group consisting of aqueous ammonia, aqueous sodium hydroxide, aqueous potassium hydroxide and aqueous sodium carbonate, and further the basic aqueous solution has a pH of 8 to 12.
6. The method according to claim 1, wherein in step 3), the temperature range is 30-100 ℃, preferably 50-80 ℃.
7. The method according to claim 1, wherein in step 4), the holding time at 30-100 ℃ is 1-120min, preferably 20-60min, such as 10min, 20min, 30min, 40min, 50min, 60 min.
8. The transparent conductive film obtained by the production method according to any one of claims 1 to 7.
9. Use of the transparent conductive film according to claim 8 as an electrode material.
10. A method for improving the acid and alkali resistance, high temperature resistance and sulfuration resistance of a transparent electrode material comprises the steps of coating a silane coupling agent on the surface with silver nanowires, soaking the silver nanowires in an alkaline aqueous solution, and preserving heat at 30-100 ℃; and finally, drying to obtain the silver nanowire transparent conductive film.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114038623A (en) * | 2021-10-25 | 2022-02-11 | 南京邮电大学 | Silver nanowire-biological material composite transparent conductive film and preparation method and application thereof |
CN114613546A (en) * | 2022-02-28 | 2022-06-10 | 浙江大华技术股份有限公司 | Special-shaped base transparent conductive film and preparation method and application thereof |
CN114749587A (en) * | 2022-04-18 | 2022-07-15 | 安徽工业大学 | Silver nanowire welding interconnection method |
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