CN112614627A - Flexible transparent electrode with high conductive coverage rate and preparation method thereof - Google Patents
Flexible transparent electrode with high conductive coverage rate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a flexible transparent electrode with high conductive coverage rate and low surface roughness, belonging to the technical field of flexible electronics. The flexible transparent electrode with high conductive coverage rate and low surface roughness comprises flexible transparent macromolecules and a composite conductive network embedded in the range of dozens of nanometers on the surface of the flexible transparent macromolecules. The flexible transparent electrode with high conductive coverage rate and low surface roughness disclosed by the invention has the advantages of high conductive coverage rate, low surface roughness, high conductivity, high light transmittance and high flexibility, the conductive coverage rate reaches 60%, the surface roughness is as low as 1.72nm, the light transmittance reaches 85%, the sheet resistance reaches 15.7 omega/sq, and the flexible transparent electrode can bear 500 times of bending deformation.
Description
Technical Field
The invention discloses a flexible transparent electrode with high conductive coverage rate and a preparation method thereof, belonging to the technical field of flexible electronics.
Background
Flexible electronics is an emerging cross-technology field that encompasses multiple areas of organic electronics, printed electronics, and printed electronics. Compared with the traditional electronic device, the flexible electronic device has the advantages of convenience in use, wide applicable scene, high flexibility and the like. The flexible transparent electrode is a very important component in a flexible electronic device, and plays a role of transporting carriers (electrons or holes). Currently, Indium Tin Oxide (ITO) materials are widely used to process non-flexible transparent electrodes. However, the ITO material is brittle and the price is continuously increased, making the ITO material unsuitable for processing flexible transparent electrodes. Therefore, the task of developing flexible transparent electrodes using new materials is still very difficult. Nowadays, metal nanowires, graphene, carbon nanotubes and conductive polymers have been used to process flexible transparent electrodes. Compared with the novel material, the metal nanowire has high conductivity, good light transmission, high flexibility and low price, and is the best material for processing the flexible transparent electrode.
The metal nanowire has extremely high conductivity but has no light transmittance by itself, and it is necessary to form a metal nanowire network to simultaneously achieve high conductivity and high light transmittance. The metal nanowire network can transmit carriers, and light can penetrate through gaps in the middle of the metal nanowire network. For a metal nanowire flexible transparent electrode with excellent photoelectric properties (light transmittance >90%, sheet resistance <100 ohm/sq), the conductive coverage is less than 10% (conductive coverage refers to the ratio of the area of the metal nanowire network to the area of the whole flexible transparent electrode). The flexible electronic device (such as a flexible solar cell and a flexible organic light emitting diode) is prepared on the surface of the flexible transparent electrode by the technologies of spin coating, evaporation and the like, and current carriers are injected into the flexible electronic device from the surface of the flexible transparent electrode. Because the conductive coverage rate of the flexible transparent electrode is low, the density distribution of carriers injected into the flexible electronic device is not uniform, even partial areas are free from carrier injection, and the performance of the flexible electronic device is reduced. Therefore, it is necessary to improve the conductive coverage of the flexible transparent electrode. Generally, covering the surface of the metal nanowire network with another layer of conductive material improves the conductive coverage. Although the conductive coverage rate of the flexible transparent electrode can be improved by the process method, the bonding force between the conductive medium and the substrate in the prepared flexible transparent electrode is weak, so that the flexibility is poor. In addition, the surface roughness of the flexible transparent electrode prepared by the process method is very large, and short circuit failure of the flexible electronic device can be caused.
Therefore, it is desired to develop a flexible transparent electrode having high conductive coverage, low surface roughness, high conductivity, high light transmittance, and high flexibility.
Disclosure of Invention
The invention provides a flexible transparent electrode with high conductive coverage rate and a preparation method thereof. The flexible transparent electrode with high conductive coverage rate has the advantages of high conductive coverage rate, low surface roughness, high conductivity, high light transmittance and high flexibility.
The technical solution of the invention is as follows: a flexible transparent electrode with high conductive coverage rate comprises a flexible transparent polymer and a composite conductive network embedded in the surface of the flexible transparent polymer within the range of 1-100 nm, wherein the flexible transparent electrode with high conductive coverage rate and low surface roughness comprises the flexible transparent polymer; the composite conductive network of the flexible transparent electrode with high conductive coverage rate comprises a carbon nano tube network and a metal nano tube network; the flexible transparent electrode with high conductive coverage rate has the conductive coverage rate of more than 50%, the surface roughness of less than 2nm, the light transmittance of more than 80%, the sheet resistance of less than 20ohm/sq, and can bear 500 times of bending deformation.
The preparation method comprises the following steps:
(1) forming a sacrificial layer on the surface of the substrate;
(2) forming a carbon nano tube network on the surface of the substrate/sacrificial layer;
(3) forming a metal nanowire network on the surface of the substrate/the sacrificial layer/the carbon nanotube network;
(4) coating a high-molecular precursor on the surface of the substrate/the sacrificial layer/the carbon nanotube network/the metal nanowire network;
(5) curing the polymer precursor to form a flexible transparent electrode with high conductive coverage rate;
(6) and dissolving the sacrificial layer, and completely stripping the flexible transparent electrode with high conductive coverage rate.
In the step (1), a sacrificial layer is formed on the surface of a substrate, wherein the substrate is one of glass, monocrystalline silicon and polycrystalline silicon.
In the step (1), a sacrificial layer is formed on the surface of the substrate, wherein the sacrificial layer is one of polystyrene sulfonate, poly 3, 4-ethylenedioxythiophene and polymethyl methacrylate; the preparation step of the sacrificial layer comprises the steps of coating a sacrificial layer solution and volatilizing a solvent; the concentration of the sacrificial layer solution is 1-100 mg/ml; the solvent of the sacrificial layer solution is one or a mixture of water, ethanol, propanol and chlorobenzene; the coating method of the sacrificial layer solution comprises a spin coating method, a blade coating method or a meyer rod method.
In the step (2), a carbon nanotube network is formed on the surface of the substrate/sacrificial layer, and the carbon nanotube network is prepared by coating a carbon nanotube solution and volatilizing a solvent; the carbon nano tube is one of a single-wall carbon nano tube and a multi-wall carbon nano tube or a mixture of the single-wall carbon nano tube and the multi-wall carbon nano tube; the diameter of the carbon nano tube is 1-100 nm, and the length of the carbon nano tube is 1-100 mu m; the concentration of the carbon nano tube solution is 0.1-10 mg/ml; the solvent of the carbon nano tube solution is one or a mixture of water, ethanol and glycerol; the coating method of the carbon nano tube solution comprises a spin coating method, a blade coating method, a Meyer rod method or a spray coating method.
In the step (3), a metal nanowire network is formed on the surface of the substrate/sacrificial layer/carbon nanotube network, and the metal nanowire network is prepared by coating a metal nanowire solution and volatilizing a solvent; the metal nano-wire is one or a mixture of silver nano-wires, copper nano-wires, gold nano-wires, silver-plated copper nano-wires, gold-plated copper nano-wires or gold-silver-plated nano-wires; the diameter of the metal nanowire is 10-1000 nm, and the length of the metal nanowire is 1-1000 mu m; the concentration of the metal nanowire solution is 1-100 mg/ml; the solvent of the metal nanowire solution is one or a mixture of water, ethanol and glycerol; the coating method of the metal nanowire solution comprises a spin coating method, a blade coating method, a meyer rod method or a spraying method.
In the step (4), coating a polymer precursor on the surface of the substrate/the sacrificial layer/the carbon nanotube network/the metal nanowire network, wherein the polymer precursor comprises a thermosetting polymer precursor and a photocuring polymer precursor, and the thermosetting polymer precursor is a polyimide precursor or a polydimethylsiloxane precursor; the photocuring polymer precursor is one or a mixture of a plurality of Sartomer monomers and oligomers; the coating method is spin coating, knife coating, meyer rod method or spray coating.
In the step (5) of curing the polymer precursor, the flexible transparent polymer is prepared by thermally curing or ultraviolet curing the polymer precursor.
Dissolving the sacrificial layer, completely stripping the flexible transparent electrode with high conductive coverage rate, and soaking the substrate/the sacrificial layer/the flexible transparent electrode with high conductive coverage rate in a sacrificial layer dissolving solution to realize; the sacrificial layer dissolving solution is one or a mixture of water and acetone.
The invention has the beneficial effects that:
(1) the flexible transparent electrode has the advantages of high conductive coverage rate, low surface roughness, high conductivity, high light transmittance and high flexibility; the conductive coverage rate is high, the injection density and the injection area of current carriers are improved, and the performance of the flexible electronic device is improved.
(2) According to the flexible transparent electrode with high conductive coverage rate, the conductive medium is embedded on the surface of the flexible transparent polymer, so that extremely low surface roughness is realized, and short circuit failure of a flexible electronic device is avoided; in addition, the binding force between the conductive medium and the flexible transparent polymer is strong, and excellent flexibility is realized.
(3) The flexible transparent electrode with high conductive coverage rate and low surface roughness adopts a composite conductive network as a conductive medium. The composite conductive network comprises a carbon nanotube network and a metal nanotube network. The metal nanowire network has slightly poor light transmittance and good conductivity and is used as a main transmission channel of a current carrier; the carbon nanotube network has high light transmittance and slightly poor conductivity, and is used as a secondary transmission channel of a current carrier, so that the effects of uniform current carrier transmission area and improvement of conductive coverage rate are achieved. The composite conductive network structure is adopted to simultaneously realize high conductive coverage rate, high conductivity and high light transmittance.
(4) By adopting the sacrificial layer stripping technology, the composite conductive network is embedded in the range of 1-100 nm on the surface of the flexible transparent polymer, the surface roughness is ensured to be lower than 2nm, and meanwhile, efficient carrier transmission is carried out by means of a tunneling effect.
Drawings
FIG. 1 is an atomic force microscope image of a flexible transparent electrode with high conductive coverage;
FIG. 2 is a result of a bonding force test between a conductive medium and a flexible transparent polymer in a flexible transparent electrode with high conductive coverage;
fig. 3 is a flexibility test result of a flexible transparent electrode having a high conductive coverage.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of a flexible transparent electrode with high conductive coverage rate, which comprises the following specific implementation steps:
(1) coating a PSS sacrificial layer on the surface of a glass substrate:
first, PSS was dissolved in water, and the solubility of PSS in water was 5 mg/ml. And (3) dropwise adding the PSS aqueous solution on the surface of the glass substrate, and carrying out spin coating treatment at the speed of 1000rpm after the PSS aqueous solution is completely spread on the surface of the glass substrate. And (3) carrying out heat treatment at 120 ℃ for 20min to form a PSS sacrificial layer on the surface of the glass substrate.
(2) Coating a carbon nanotube network on the surface of the glass substrate/PSS sacrificial layer:
the carbon nano tube is dispersed in ethanol by using the dispersion effect of ultrasonic, and the concentration of the carbon nano tube in the ethanol is 0.5 mg/ml. And coating the carbon nanotube ethanol solution on the surface of the glass substrate/PSS sacrificial layer by a Meyer rod method, and forming a carbon nanotube network on the surface of the glass substrate/PSS sacrificial layer after the ethanol is volatilized.
(3) Coating a silver nanowire network on the surface of the glass substrate/the PSS sacrificial layer/the carbon nanotube network:
the silver nanowires are dispersed in ethanol by using the vortex force generated by a vortex mixer, and the concentration of the silver nanowires in the ethanol is 5 mg/ml. Coating the silver nanowire ethanol solution on the surface of the glass substrate/the PSS sacrificial layer/the carbon nanotube network by a Meyer rod method, and forming a silver nanowire network on the surface of the glass substrate/the PSS sacrificial layer/the carbon nanotube network after ethanol volatilizes.
(4) Coating a polymer precursor on the surface of the glass substrate/the PSS sacrificial layer/the carbon nanotube network/the silver nanowire network:
three monomers, namely, Ethylated (6) trimetylpropane triacrylate (SR 449), Ethylated (4) bisphenol A dimorphinate (SR 540) and 2, 2-dimethyl-2-phenylacetophenone (DMPA), are mixed according to the mass fraction of 200:100:1.5 to prepare a high molecular precursor. And coating a polymer precursor on the surface of the glass substrate/the PSS sacrificial layer/the carbon nanotube network/the silver nanowire network by a Meyer rod method. Since the polymer precursor has excellent fluidity, it can infiltrate into the voids between the carbon nanotube network and the silver nanotube network.
(5) Ultraviolet curing the polymer precursor to form the flexible transparent electrode with high conductive coverage rate:
under the irradiation of ultraviolet rays, the polymer precursor is crosslinked and cured to form flexible transparent polymers, and the carbon nanotube network and the silver nanowire network are embedded on the surface of the flexible transparent polymers to form the flexible transparent electrode with high conductive coverage rate.
(6) Dissolving the sacrificial layer to completely strip the flexible transparent electrode with high conductive coverage rate from the surface of the glass substrate:
the glass substrate/PSS sacrificial layer/flexible transparent electrode with high conductive coverage was soaked in water for 2 h. Since the PSS sacrificial layer can be dissolved in water, the flexible transparent electrode having high conductive coverage can be easily and completely peeled off from the glass substrate surface. Fig. 1 is an atomic force microscope picture of a flexible transparent electrode with high conductive coverage prepared. As can be seen from the figure, the surface roughness is only 1.72nm, and the carbon nanotube network and the silver nanowire network are completely embedded on the surface of the flexible transparent polymer. When no PSS sacrificial layer is arranged on the surface of the glass substrate, most of the carbon nanotube network and the silver nanowire network cannot be transferred to the surface of the flexible transparent polymer from the glass substrate due to the strong adsorption force between the carbon nanotube network and the glass substrate and the silver nanowire network, so that the surface roughness is improved, and the improvement of the conductive coverage rate of the flexible transparent electrode cannot be realized.
(7) Performance analysis of flexible transparent electrodes with high conductive coverage:
the sheet resistance of the flexible transparent electrode having high conductive coverage prepared in example 1 was 15.7ohm/sq, and the light transmittance was 85%. And (3) adhering the surface of the flexible transparent electrode with high conductive coverage rate by using a 3M adhesive tape, and testing the binding force between the carbon nanotube network and the substrate and between the silver nanotube network and the substrate. As shown in fig. 2, after 100 cycles of the 3M adhesive tape adhesion test, the relative resistance (the relative resistance is the ratio of the resistance to the initial resistance) of the flexible transparent electrode with high conductive coverage rate is substantially maintained at 1, which indicates that the bonding force between the carbon nanotube network and the silver nanotube network of the flexible transparent electrode with high conductive coverage rate of the invention and the flexible transparent polymer is strong. As shown in fig. 3, the relative resistance of the flexible transparent electrode having high conductive coverage after 500 times of bending at a radius of curvature of 2.5mm increases to only 1.2, illustrating that the inventive flexible transparent electrode having high conductive coverage has high flexibility.
Example 2:
the embodiment provides a preparation method of a flexible transparent electrode with high conductive coverage rate, which comprises the following specific implementation steps:
(1) coating a PMMA sacrificial layer on the surface of a glass substrate:
first, PMMA was dissolved in chlorobenzene, the solubility of PMMA being 5mg/ml in chlorobenzene. And dropwise adding a PMMA chlorobenzene solution on the surface of the glass substrate, and performing spin coating treatment at the speed of 1000rpm after the PMMA chlorobenzene solution is completely spread on the surface of the glass substrate. And (3) carrying out heat treatment at 120 ℃ for 20min to form a PMMA sacrificial layer on the surface of the glass substrate.
(2) Coating a carbon nanotube network on the surface of the glass substrate/PMMA sacrificial layer:
the carbon nano tube is dispersed in ethanol by using the dispersion effect of ultrasonic, and the concentration of the carbon nano tube in the ethanol is 0.5 mg/ml. Coating the carbon nanotube ethanol solution on the surface of the glass substrate/PMMA sacrificial layer by a Meyer rod method, and forming a carbon nanotube network on the surface of the glass substrate/PMMA sacrificial layer after ethanol is volatilized.
(3) Coating a silver nanowire network on the surface of the glass substrate/PMMA sacrificial layer/carbon nanotube network:
the silver nanowires are dispersed in ethanol by using the vortex force generated by a vortex mixer, and the concentration of the silver nanowires in the ethanol is 5 mg/ml. Coating the silver nanowire ethanol solution on the surface of the glass substrate/PMMA sacrificial layer/carbon nanotube network by a Meyer rod method, and forming a silver nanowire network on the surface of the glass substrate/PMMA sacrificial layer/carbon nanotube network after ethanol is volatilized.
(4) Coating a polymer precursor on the surface of the glass substrate/PMMA sacrificial layer/carbon nanotube network/silver nanowire network:
three monomers, namely, Ethylated (6) trimetylpropane triacrylate (SR 449), Ethylated (4) bisphenol A dimorphinate (SR 540) and 2, 2-dimethyl-2-phenylacetophenone (DMPA), are mixed according to the mass fraction of 200:100:1.5 to prepare a high molecular precursor. And coating a polymer precursor on the surface of the glass substrate/PMMA sacrificial layer/carbon nanotube network/silver nanowire network by a Meyer rod method. Since the polymer precursor has excellent fluidity, it can infiltrate into the voids between the carbon nanotube network and the silver nanotube network.
(5) Ultraviolet curing the polymer precursor to form the flexible transparent electrode with high conductive coverage rate:
under the irradiation of ultraviolet rays, the polymer precursor is crosslinked and cured to form flexible transparent polymers, and the carbon nanotube network and the silver nanowire network are embedded on the surface of the flexible transparent polymers to form the flexible transparent electrode with high conductive coverage rate.
(6) Dissolving the sacrificial layer to completely strip the flexible transparent electrode with high conductive coverage rate from the surface of the glass substrate:
the glass substrate/PMMA sacrificial layer/flexible transparent electrode with high conductive coverage was soaked in acetone for 12 h. Since the PMMA sacrificial layer can be dissolved in acetone, the flexible transparent electrode having a high conductive coverage can be easily and completely peeled off from the surface of the glass substrate.
Claims (9)
1. A flexible transparent electrode with high conductive coverage rate is characterized in that a conductive medium of the flexible transparent electrode is a carbon nano tube network and a metal nano wire network, a substrate is a flexible transparent polymer, the structure of the flexible transparent polymer is that the carbon nano tube network and the metal nano wire network are embedded on the surface of the flexible transparent polymer, and the carbon nano tube network and the metal nano wire network form a composite conductive network which is embedded in the range of 1-100 nm on the surface of the flexible transparent polymer.
2. The method for preparing a flexible transparent electrode with high conductive coverage according to claim 1, comprising the steps of:
(1) forming a sacrificial layer on the surface of the substrate;
(2) forming a carbon nano tube network on the surface of the substrate/sacrificial layer;
(3) forming a metal nanowire network on the surface of the substrate/the sacrificial layer/the carbon nanotube network;
(4) coating a high-molecular precursor on the surface of the substrate/the sacrificial layer/the carbon nanotube network/the metal nanowire network;
(5) curing the polymer precursor to form a flexible transparent electrode with high conductive coverage rate;
(6) and dissolving the sacrificial layer, and completely stripping the flexible transparent electrode with high conductive coverage rate.
3. The method as claimed in claim 2, wherein the step (1) is performed by forming a sacrificial layer on a surface of a substrate, wherein the substrate is one of glass, single crystal silicon and polysilicon.
4. The method as claimed in claim 2, wherein the step (1) is a step of forming a sacrificial layer on the surface of the substrate, wherein the sacrificial layer is one of polystyrene sulfonate, poly 3, 4-ethylenedioxythiophene and polymethyl methacrylate; the preparation step of the sacrificial layer comprises the steps of coating a sacrificial layer solution and volatilizing a solvent; the concentration of the sacrificial layer solution is 1-100 mg/ml; the solvent of the sacrificial layer solution is one or a mixture of water, ethanol, propanol and chlorobenzene; the coating method of the sacrificial layer solution comprises a spin coating method, a blade coating method or a meyer rod method.
5. The method as claimed in claim 2, wherein the step (2) forms a carbon nanotube network on the surface of the substrate/sacrificial layer, the carbon nanotube network is prepared by coating a carbon nanotube solution and volatilizing a solvent; the carbon nano tube is one of a single-wall carbon nano tube and a multi-wall carbon nano tube or a mixture of the single-wall carbon nano tube and the multi-wall carbon nano tube; the diameter of the carbon nano tube is 1-100 nm, and the length of the carbon nano tube is 1-100 mu m; the concentration of the carbon nano tube solution is 0.1-10 mg/ml; the solvent of the carbon nano tube solution is one or a mixture of water, ethanol and glycerol; the coating method of the carbon nano tube solution comprises a spin coating method, a blade coating method, a Meyer rod method or a spray coating method.
6. The method as claimed in claim 2, wherein the step (3) is a step of forming a metal nanowire network on the surface of the substrate/sacrificial layer/carbon nanotube network, and the metal nanowire network is prepared by coating a metal nanowire solution and volatilizing a solvent; the metal nano-wire is one or a mixture of silver nano-wires, copper nano-wires, gold nano-wires, silver-plated copper nano-wires, gold-plated copper nano-wires or gold-silver-plated nano-wires; the diameter of the metal nanowire is 10-1000 nm, and the length of the metal nanowire is 1-1000 mu m; the concentration of the metal nanowire solution is 1-100 mg/ml; the solvent of the metal nanowire solution is one or a mixture of water, ethanol and glycerol; the coating method of the metal nanowire solution comprises a spin coating method, a blade coating method, a meyer rod method or a spraying method.
7. The method according to claim 2, wherein the step (4) comprises coating a polymer precursor on the surface of the substrate/sacrificial layer/carbon nanotube network/metal nanowire network, wherein the polymer precursor comprises a thermosetting polymer precursor and a photo-curing polymer precursor, and the thermosetting polymer precursor is a polyimide precursor or a polydimethylsiloxane precursor; the photocuring polymer precursor is one or a mixture of a plurality of Sartomer monomers and oligomers; the coating method is spin coating, knife coating, meyer rod method or spray coating.
8. The method as claimed in claim 2, wherein the step (5) of curing the polymer precursor comprises preparing the flexible transparent polymer by thermally curing or ultraviolet curing the polymer precursor.
9. The method according to claim 2, wherein the step (6) of dissolving the sacrificial layer, completely stripping the flexible transparent electrode with high conductive coverage, and immersing the substrate/sacrificial layer/flexible transparent electrode with high conductive coverage in the sacrificial layer dissolving solution; the sacrificial layer dissolving solution is one or a mixture of water and acetone.
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| CN113113188A (en) * | 2021-04-09 | 2021-07-13 | 中国科学院化学研究所 | Preparation method of flexible transparent electrode based on semi-embedded conductive grid, product and application thereof |
| CN113881229A (en) * | 2021-10-27 | 2022-01-04 | 华中科技大学 | Stretchable conductive composite material and preparation method and application thereof |
| CN117497229A (en) * | 2023-12-29 | 2024-02-02 | 北京航空航天大学 | Super-flexible transparent electrode, preparation method and application thereof |
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| CN104662619A (en) * | 2013-07-30 | 2015-05-27 | Lg化学株式会社 | Manufacturing method of flexible buried electrode film using thermal lamination transfer |
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| US20200401042A1 (en) * | 2019-05-09 | 2020-12-24 | The Board Of Trustees Of The Leland Stanford Junior University | Directly photo-patternable, stretchable, electrically conductive polymer |
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| CN104662619A (en) * | 2013-07-30 | 2015-05-27 | Lg化学株式会社 | Manufacturing method of flexible buried electrode film using thermal lamination transfer |
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| CN113113188A (en) * | 2021-04-09 | 2021-07-13 | 中国科学院化学研究所 | Preparation method of flexible transparent electrode based on semi-embedded conductive grid, product and application thereof |
| CN113881229A (en) * | 2021-10-27 | 2022-01-04 | 华中科技大学 | Stretchable conductive composite material and preparation method and application thereof |
| CN117497229A (en) * | 2023-12-29 | 2024-02-02 | 北京航空航天大学 | Super-flexible transparent electrode, preparation method and application thereof |
| CN117497229B (en) * | 2023-12-29 | 2024-04-16 | 北京航空航天大学 | Super-flexible transparent electrode, preparation method and application thereof |
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