CN112614627B - Flexible transparent electrode with high conductive coverage rate and preparation method thereof - Google Patents
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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, and belongs to the technical field of flexible electronics. The flexible transparent electrode with high conductive coverage and low surface roughness comprises a flexible transparent polymer and a composite conductive network embedded on the surface of the flexible transparent polymer within a range of tens of nanometers. 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 15.7ohm/sq, and the flexible transparent electrode can bear 500 times of bending deformation.
Description
Technical Field
The invention relates to 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 includes multiple fields of organic electronics, printing electronics, and printing electronics. Compared with the traditional electronic device, the flexible electronic device has the advantages of convenient use, wide application scene, high flexibility and the like. Flexible transparent electrodes are very important components in flexible electronic devices, which are responsible for transporting carriers (electrons or holes). Currently, indium Tin Oxide (ITO) materials are widely used for processing inflexible transparent electrodes. However, ITO materials are brittle and continue to increase in price, making ITO materials unsuitable for processing flexible transparent electrodes. Thus, the task of developing flexible transparent electrodes using new materials remains 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 transmittance, high flexibility and low price, and is the optimal material for processing the flexible transparent electrode.
The metal nanowire has extremely high conductivity but is not light-transmitting by itself, and it is necessary to form a metal nanowire network to achieve both high conductivity and high light-transmitting properties. The metal nanowire network can transmit carriers, and light can penetrate through gaps in the middle of the metal nanowire network. For a metallic nanowire flexible transparent electrode with excellent optoelectronic properties (light transmittance >90%, sheet resistance <100 ohm/sq), its conductive coverage is less than 10% (conductive coverage refers to the ratio between the area of the metallic nanowire network and the area of the entire flexible transparent electrode). And preparing a flexible electronic device (such as a flexible solar cell and a flexible organic light-emitting diode) on the surface of the flexible transparent electrode by spin coating, vapor deposition and other technologies, and injecting carriers into the flexible electronic device from the surface of the flexible transparent electrode. Because the conductive coverage of the flexible transparent electrode is low, the density distribution of the injected carriers into the flexible electronic device is uneven, and even no carrier is injected into partial areas, which can reduce the performance of the flexible electronic device. Therefore, it is necessary to improve the conductive coverage of the flexible transparent electrode. Typically, a further layer of conductive material is applied to the surface of the metal nanowire network to enhance the conductive coverage. Although the process method can improve the conductive coverage rate of the flexible transparent electrode, 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, there is a need 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: the flexible transparent electrode with high conductive coverage rate and low surface roughness comprises a flexible transparent polymer and a composite conductive network embedded on the surface of the flexible transparent polymer within the range of 1-100 nm; the composite conductive network of the flexible transparent electrode with high conductive coverage comprises a carbon nanotube network and a metal nanowire network; the flexible transparent electrode with high conductive coverage rate has the conductive coverage rate exceeding 50%, the surface roughness being lower than 2nm, the light transmittance exceeding 80%, the sheet resistance being lower 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 nanotube network on the surface of the substrate/the sacrificial layer;
(3) Forming a metal nanowire network on the surface of the substrate/the sacrificial layer/the carbon nanotube network;
(4) Coating a macromolecule precursor on the surface of the substrate/the sacrificial layer/the carbon nano tube network/the metal nano tube 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.
And (2) forming a sacrificial layer on the surface of the substrate in the step (1), wherein the substrate is one of glass, monocrystalline silicon and polycrystalline silicon.
The step (1) is to form a sacrificial layer on the surface of a substrate, wherein the sacrificial layer is one of polystyrene sulfonate, poly 3, 4-ethylenedioxythiophene and polymethyl methacrylate; the sacrificial layer preparation step 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 mixed solution of more than one of water, ethanol, propanol and chlorobenzene; the method of coating the sacrificial layer solution includes spin coating, knife coating, or meyer rod method.
In the step (2), a carbon nano tube network is formed on the surface of the substrate/the sacrificial layer, wherein the carbon nano tube network preparation step comprises the steps of coating a carbon nano tube solution and volatilizing a solvent; the carbon nano tube is one or a mixture of single-wall carbon nano tube and 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 nanotube solution is one or a mixture of more of water, ethanol and glycerol; the coating method of the carbon nanotube solution includes spin coating, knife coating, meyer rod method or spray coating method.
In the step (3), a metal nanowire network is formed on the surface of a substrate/a sacrificial layer/a carbon nanotube network, wherein the metal nanowire network is prepared by coating a metal nanowire solution and volatilizing a solvent; the metal nanowire is one or a mixture of a plurality of silver nanowires, copper nanowires, gold nanowires, silver-plated copper nanowires, gold-plated copper nanowires or gold-plated silver nanowires; 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 more of water, ethanol and glycerol; the coating method of the metal nanowire solution comprises a spin coating method, a knife coating method, a Meyer rod method or a spraying method.
The step (4) is to coat a macromolecule precursor on the surface of the substrate/the sacrifice layer/the carbon nano tube network/the metal nano tube network, wherein the macromolecule precursor comprises a thermosetting macromolecule precursor and a photo-curing macromolecule precursor, and the thermosetting macromolecule precursor is a polyimide precursor or a polydimethylsiloxane precursor; the photocuring polymer precursor is one or a mixture of more than one of Sartomer monomers and oligomers; the coating method is spin coating, knife coating, meyer rod or spray coating.
And (3) preparing the flexible transparent polymer by thermally curing or ultraviolet curing the polymer precursor in the step (5).
The sacrificial layer is dissolved in the step (6), the flexible transparent electrode with high conductive coverage rate is completely peeled off, and the substrate/the sacrificial layer/the flexible transparent electrode with high conductive coverage rate are soaked in the sacrificial layer dissolving solution; the sacrificial layer dissolving liquid is one or a mixture of water and acetone.
The invention has the beneficial effects that:
(1) The flexible transparent electrode has 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 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 nanowire network. The metal nanowire network has slightly poor light transmittance and good conductivity, and is used as a main transmission channel of carriers; the carbon nanotube network has high light transmittance and poor conductivity, and serves as a secondary transmission channel of carriers to achieve the effects of uniform carrier transmission area and improved conductive coverage rate. The composite conductive network structure is adopted to realize high conductive coverage rate, high conductivity and high light transmittance.
(4) The sacrificial layer stripping technology is adopted, 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, the efficient carrier transmission is carried out by means of the tunneling effect.
Drawings
FIG. 1 is an atomic force microscope image of a flexible transparent electrode with high electrical conductivity coverage;
FIG. 2 is a graph showing the results of a test of the binding force between a conductive medium and a flexible transparent polymer in a flexible transparent electrode with high conductive coverage;
fig. 3 is a flexible test result of a flexible transparent electrode with high conductive coverage.
Detailed Description
The following description of the present invention is provided with reference to the accompanying drawings, but is not limited to the following description, and any modifications or equivalent substitutions of the present invention should be included in the scope of the present invention without departing from the spirit and 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 5mg/ml. And (3) dripping the PSS aqueous solution on the surface of the glass substrate, and spin-coating at a speed of 1000rpm after the PSS aqueous solution is completely spread on the surface of the glass substrate. And performing heat treatment at 120 ℃ for 20min, and forming a PSS sacrificial layer on the surface of the glass substrate.
(2) Coating a carbon nano tube network on the surface of the glass substrate/PSS sacrificial layer:
the carbon nanotubes were dispersed in ethanol with a concentration of 0.5mg/ml in ethanol by using the dispersion effect of ultrasound. 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 ethanol volatilizes.
(3) Coating silver nanowire networks on the surfaces of the glass substrate/the PSS sacrificial layer/the carbon nanotube network:
silver nanowires were dispersed in ethanol at a concentration of 5mg/ml using a vortex force generated by a vortex mixer. And coating the silver nanowire ethanol solution on the surfaces of the glass substrate/the PSS sacrificial layer/the carbon nano tube network by a Meyer rod method, and forming the silver nano tube network on the surfaces of the glass substrate/the PSS sacrificial layer/the carbon nano tube network after ethanol volatilizes.
(4) Coating a high polymer precursor on the surface of the glass substrate/PSS sacrificial layer/carbon nano tube network/silver nano tube network:
ethoxylated (6) trimethylolpropane triacrylate (SR 449), ethoxylated (4) bisphenol A dimethacrylate (SR 540) and 2,2-Dimethoxy-2-phenylacetophenone (DMPA) are mixed according to the mass fraction of 200:100:1.5 to prepare the macromolecule precursor. And coating a polymer precursor on the surfaces of the glass substrate/the PSS sacrificial layer/the carbon nano tube network/the silver nano wire network by a Meyer rod method. Since the polymer precursor has excellent fluidity, it can infiltrate into the gaps between the carbon nanotube network and the silver nanowire network.
(5) Ultraviolet curing the polymer precursor to form the flexible transparent electrode with high conductive coverage rate:
under ultraviolet irradiation, the polymer precursor is crosslinked and solidified to form a flexible transparent polymer, and the carbon nanotube network and the silver nanowire network are inlaid on the surface of the flexible transparent polymer to form the flexible transparent electrode with high conductive coverage rate.
(6) Dissolving the sacrificial layer allows the flexible transparent electrode with high conductive coverage to be completely peeled off from the surface of the glass substrate:
the glass substrate/PSS sacrificial layer/flexible transparent electrode with high conductive coverage were immersed in water for 2h. Since the PSS sacrifice layer can be dissolved in water, the flexible transparent electrode having high conductive coverage can be easily and completely peeled off from the surface of the glass substrate. Fig. 1 is an atomic force microscope picture of a prepared flexible transparent electrode with high conductive coverage. The figure shows that the surface roughness is only 1.72nm, and the carbon nano tube network and the silver nano tube network are completely embedded on the surface of the flexible transparent polymer. When the PSS sacrificial layer is not arranged on the surface of the glass substrate, most of carbon nanotube networks and silver nanowire networks cannot be transferred from the glass substrate to the surface of the flexible transparent polymer due to strong adsorption force between the carbon nanotube networks and the silver nanowire networks and the glass substrate, so that the surface roughness is improved, and the conductive coverage rate of the flexible transparent electrode is not improved.
(7) Performance analysis of flexible transparent electrode with high conductive coverage:
the sheet resistance of the flexible transparent electrode with high conductive coverage prepared in example 1 was 15.7ohm/sq and the light transmittance was 85%. The binding force between the carbon nanotube network and the silver nanowire network and the substrate was tested by adhering the surface of the flexible transparent electrode with high conductive coverage through a 3M tape. 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 basically kept to be 1, which indicates that the bonding force between the carbon nanotube network and the silver nanowire network of the flexible transparent electrode with high conductive coverage rate and the flexible transparent polymer is very strong. As shown in fig. 3, after 500 bends with a radius of curvature of 2.5mm, the relative resistance of the flexible transparent electrode with high conductive coverage increases to only 1.2, indicating that the inventive flexible transparent electrode with 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:
firstly, PMMA was dissolved in chlorobenzene to a solubility of 5mg/ml in chlorobenzene. And (3) dropwise adding a PMMA chlorobenzene solution on the surface of the glass substrate, and spin-coating at a speed of 1000rpm after the PMMA chlorobenzene solution is completely spread on the surface of the glass substrate. And (5) performing heat treatment at 120 ℃ for 20min, and forming a PMMA sacrificial layer on the surface of the glass substrate.
(2) Coating a carbon nano tube network on the surface of the glass substrate/PMMA sacrificial layer:
the carbon nanotubes were dispersed in ethanol with a concentration of 0.5mg/ml in ethanol by using the dispersion effect of ultrasound. And 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 volatilizes.
(3) Coating silver nanowire networks on the surfaces of the glass substrate/PMMA sacrificial layer/carbon nanotube network:
silver nanowires were dispersed in ethanol at a concentration of 5mg/ml using a vortex force generated by a vortex mixer. And coating the silver nanowire ethanol solution on the surface of the glass substrate/PMMA sacrificial layer/carbon nano tube network by a Meyer rod method, and forming a silver nanowire network on the surface of the glass substrate/PMMA sacrificial layer/carbon nano tube network after ethanol volatilizes.
(4) Coating a high polymer precursor on the surface of the glass substrate/PMMA sacrificial layer/carbon nano tube network/silver nano tube network:
ethoxylated (6) trimethylolpropane triacrylate (SR 449), ethoxylated (4) bisphenol A dimethacrylate (SR 540) and 2,2-Dimethoxy-2-phenylacetophenone (DMPA) are mixed according to the mass fraction of 200:100:1.5 to prepare the macromolecule precursor. And coating a polymer precursor on the surfaces of the glass substrate/the PMMA sacrificial layer/the carbon nano tube network/the silver nano tube network by a Meyer rod method. Since the polymer precursor has excellent fluidity, it can infiltrate into the gaps between the carbon nanotube network and the silver nanowire network.
(5) Ultraviolet curing the polymer precursor to form the flexible transparent electrode with high conductive coverage rate:
under ultraviolet irradiation, the polymer precursor is crosslinked and solidified to form a flexible transparent polymer, and the carbon nanotube network and the silver nanowire network are inlaid on the surface of the flexible transparent polymer to form the flexible transparent electrode with high conductive coverage rate.
(6) Dissolving the sacrificial layer allows the flexible transparent electrode with high conductive coverage to be completely peeled off from the surface of the glass substrate:
the glass substrate/PMMA sacrificial layer/flexible transparent electrode with high conductive coverage was immersed in acetone for 12h. Since the PMMA sacrificial layer can be dissolved in acetone, the flexible transparent electrode having high conductive coverage can be easily and completely peeled off from the surface of the glass substrate.
Claims (1)
1. The 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 tube network, a substrate is a flexible transparent polymer, the structure is that the carbon nano tube network and the metal nano tube network are embedded on the surface of the flexible transparent polymer, the carbon nano tube network and the metal nano tube network form a composite conductive network, and the composite conductive network is embedded on the surface of the flexible transparent polymer within the range of 1-100 nm, and the preparation method comprises the following steps:
(1) Forming a sacrificial layer on the surface of the substrate;
the step (1) is to form a sacrificial layer on the surface of a substrate, wherein the substrate is one of glass, monocrystalline silicon and polycrystalline silicon;
the step (1) is to form a sacrificial layer on the surface of a substrate, wherein the sacrificial layer is one of polystyrene sulfonate, poly 3, 4-ethylenedioxythiophene and polymethyl methacrylate; the sacrificial layer preparation step 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 mixed solution of more than one 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;
(2) Forming a carbon nanotube network on the surface of the substrate/the sacrificial layer;
in the step (2), a carbon nano tube network is formed on the surface of the substrate/the sacrificial layer, wherein the carbon nano tube network preparation step comprises the steps of coating a carbon nano tube solution and volatilizing a solvent; the carbon nano tube is one or a mixture of single-wall carbon nano tube and 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 nanotube solution is one or a mixture of more of water, ethanol and glycerol; the coating method of the carbon nanotube solution comprises a spin coating method, a knife coating method, a Meyer rod method or a spraying method;
(3) Forming a metal nanowire network on the surface of the substrate/the sacrificial layer/the carbon nanotube network;
in the step (3), a metal nanowire network is formed on the surface of a substrate/a sacrificial layer/a carbon nanotube network, wherein the metal nanowire network is prepared by coating a metal nanowire solution and volatilizing a solvent; the metal nanowire is one or a mixture of a plurality of silver nanowires, copper nanowires, gold nanowires, silver-plated copper nanowires, gold-plated copper nanowires or gold-plated silver nanowires; 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 more of water, ethanol and glycerol; the coating method of the metal nanowire solution comprises a spin coating method, a knife coating method, a Meyer rod method or a spraying method;
(4) Coating a macromolecule precursor on the surface of the substrate/the sacrificial layer/the carbon nano tube network/the metal nano tube network;
the step (4) is to coat a macromolecule precursor on the surface of the substrate/the sacrifice layer/the carbon nano tube network/the metal nano tube network, wherein the macromolecule precursor comprises a thermosetting macromolecule precursor and a photo-curing macromolecule precursor, and the thermosetting macromolecule precursor is a polyimide precursor or a polydimethylsiloxane precursor; the photocuring polymer precursor is one or a mixture of more than one of Sartomer monomers and oligomers; the coating method is spin coating, knife coating, meyer rod or spraying;
(5) Curing the polymer precursor to form a flexible transparent electrode with high conductive coverage rate;
in the step (5), preparing a flexible transparent polymer by thermally curing or ultraviolet curing the polymer precursor;
(6) Dissolving the sacrificial layer, and completely stripping the flexible transparent electrode with high conductive coverage rate;
the sacrificial layer is dissolved in the step (6), the flexible transparent electrode with high conductive coverage rate is completely peeled off, and the substrate/the sacrificial layer/the flexible transparent electrode with high conductive coverage rate are soaked in the sacrificial layer dissolving solution; the sacrificial layer dissolving liquid is one or a mixture of water and acetone.
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