CN112185608B - Novel flexible transparent electrode with double-layer conductive network structure and preparation method thereof - Google Patents
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Abstract
The invention discloses a novel flexible transparent electrode with a double-layer conductive network structure and a preparation method thereof, wherein the novel double-layer network conductive structure is formed by compounding tannic acid functionalized carbon nano tubes and silver nano wires, the functionalized carbon nano tube conductive network at the bottom layer provides a conductive path for the silver nano wires and can be used as a conductive adhesive to increase the conductive stability of a composite film and the adhesion between the silver nano wires and a substrate, a polyethylene glycol terephthalate (PET) substrate film is ultrasonically cleaned by distilled water and ethanol and then dried, and the prepared tannic acid modified carbon nano tube solution (TCNT) is prepared. According to the novel flexible transparent electrode with the double-layer conductive network structure and the preparation method thereof, the conductive film is subjected to post-treatment by mechanically pressing and spraying the poly 3, 4-ethylenedioxythiophene (PEDOT) solution, so that the transparent electrode with good adhesion, low surface roughness and high conductivity is obtained.
Description
Technical Field
The invention relates to the technical field of electrode preparation, in particular to a novel flexible transparent electrode with a double-layer conductive network structure and a preparation method thereof.
Background
Electronic devices refer to devices made by utilizing and controlling the laws of motion of electrons in vacuum, gas, or solid. Divided into electro-vacuum devices, gas-filled tube devices and solid-state electronic devices. In the analog circuit, the functions of rectification, amplification, modulation, oscillation, frequency conversion, phase locking, control, correlation and the like are performed; the digital circuit is used for sampling, amplitude limiting, logic, storage, counting, delaying and the like, and the gas tube device is mainly used for rectifying, stabilizing voltage and displaying. In the past few years, optoelectronic devices, including Organic Light Emitting Diodes (OLEDs), Organic Solar Cells (OSCs) and Field Effect Transistors (FETs), have been developed sufficiently, and the demand for transparent conductive thin films (TCFs) has become more and more urgent, and the existing transparent flexible electrodes have low surface roughness, low adhesion and poor electrical conductivity.
Disclosure of Invention
The invention aims to provide a novel flexible transparent electrode with a double-layer conductive network structure and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a novel flexible transparent electrode with a double-layer conductive network structure comprises a novel double-layer network conductive structure, wherein the novel double-layer network conductive structure is formed by compounding tannic acid functionalized carbon nanotubes and silver nanowires, the functionalized carbon nanotube conductive network at the bottom layer provides a conductive path for the silver nanowires and can be used as a conductive adhesive to increase the conductive stability of a composite film and the adhesion between the silver nanowires and a substrate, a polyethylene glycol terephthalate (PET) substrate film is ultrasonically cleaned and dried by distilled water and ethanol, prepared tannic acid modified carbon nanotube solution (TCNT) and silver nanowires (AgNW) are respectively coated on the PET film substrate layer by adopting a spraying method and a spin coating method to obtain the flexible transparent electrode with the double-layer conductive network structure, and then the conductive film is subjected to post-treatment by adopting mechanical pressing and spraying poly 3, 4-ethylenedioxythiophene (PEDOT) solution, the single-walled carbon nanotube (TCNT) functionalized by Tannic Acid (TA) is used as a bonding layer of the silver nanowire and the substrate, and a TCNT/AgNW double-layer conductive network structure is constructed. The TA molecules rich in phenolic hydroxyl are adsorbed on the wall of the carbon nano tube through pi-pi interaction, so that the functionalized carbon nano tube (TCNT) shows hydrophilicity and effectively improves the adhesion with AgNWs. In addition, the fine conductive carbon nanotube network fills the openings of the AgNW network, increases the transmission path of carriers, and effectively improves the conductivity and the electrical stability of the hybrid film. PSS post-treatment process of mechanical pressing and PEDOT spraying enables the roughness of the film to be greatly reduced, meanwhile, the conductivity, the mechanical property and the corrosion resistance of the film are further improved, when the light transmittance is 80% -90%, the surface resistance is 10-100 omega/sq, and the surface roughness is less than 10 nm.
Preferably, the adopted raw materials are silver nanowire solution, the length of the silver nanowire solution is 40-60 mu m, the diameter of the silver nanowire solution is 40-70 nm, the purity of the single-walled carbon nanotube is more than 95 wt.%, the outer diameter of the single-walled carbon nanotube is 1-2 nm, the length of the single-walled carbon nanotube is 5-30 mu m, the tannin powder is AR grade, the pH value of the poly-3, 4-ethylenedioxythiophene solution is 1000, and the solid content of the poly-3, 4-ethylenedioxythiophene solution is 1-1.3%.
Preferably, the TCNT dispersion liquid is prepared by an ultrasonic dispersion machine under the conditions that the power is 100-200W and the time is 30-80min, the dispersing agent is sodium dodecyl benzene sulfonate, and the concentration of the prepared carbon nano tube solution is 0.1-0.5 mg/ml.
Preferably, the concentration of the prepared silver nanowire aqueous solution is 0.8-1.2 mg/ml.
Preferably, the poly 3, 4-ethylenedioxythiophene solution is diluted by 5-20 times, then 5 wt.% of dimethyl sulfoxide is added, and the mixture is stirred for more than 20 min.
Preferably, the transparency of the obtained transparent conductive film is 80% or more, the sheet resistance is 50 Ω/sq. or less, and the surface roughness is 10nm or less.
The invention also provides a preparation method of the novel flexible transparent electrode with the double-layer conductive network structure, which comprises the following steps:
a tannic acid functionalized carbon nanotube (TCNT) solution is prepared by dispersing SWCNT and tannic acid in deionized water in a ratio of 1: 1-4, stirring for 24 hours under a water bath heating condition at 60 ℃, centrifuging, filtering, freeze-drying to collect TCNT powder, dispersing a certain amount of TCNT in distilled water by using SDBS as a dispersing agent, performing water bath ultrasonic treatment for 30min, putting the solution into 120W probe ultrasonic treatment for continuous ultrasonic dispersion for 40min, centrifuging the mixed solution for 20min at 8000rmp, collecting 90% of supernatant to obtain TCNT suspension with corresponding concentration, spraying the prepared tannic acid modified carbon nanotube (TCNT) solutions with different amounts on a PET substrate by adopting a spraying method, drying after nitric acid soaking for 20min, spin-coating silver nanowire solutions with different concentrations on a TCNT layer at a rotating speed of 2000 rpm, and fully drying, and obtaining the film with the double-layer conductive network structure, wherein the final treatment process comprises mechanical pressing and surface PEDOT spraying: and a PSS solution, wherein the prepared double-layer conductive network film is placed on a tablet press and pressed for 10min under the pressure of 25MPa so as to weld silver nanowires with each other, and then 3ml of poly (3, 4-ethylenedioxythiophene) (PEDOT) solution is sprayed on the pressed film.
Compared with the prior art, the invention has the beneficial effects that:
firstly, post-processing the conductive film by mechanically pressing and spraying a poly 3, 4-ethylenedioxythiophene (PEDOT) solution to obtain a transparent electrode with good adhesion, low surface roughness and high conductivity.
The preparation process of the transparent electrode is simple, the period is short, the double-layer conductive network structure enables the structure of the film to be stable, the adhesion force to be strong, the conductivity of the electrode after high-efficiency post-treatment is greatly improved, and the roughness is sharply reduced.
And thirdly, the high-performance transparent electrode can be widely applied to the aspects of OLED organic light-emitting devices, displays, touch screens, thin film transistors, photovoltaic devices and the like.
Fourthly, spraying a solution of poly 3, 4-ethylenedioxythiophene (PEDOT) on the film after the pressing treatment, and drying to obtain the transparent electrode with good adhesion, low roughness and high conductivity.
Drawings
FIG. 1 is a schematic diagram of a tannin-modified carbon nanotube/silver nanowire/poly-3, 4-ethylenedioxythiophene (TCNT/AgNW/PEDOT) transparent conductive film according to the present invention;
FIG. 2 is a scanning electron microscope image of a tannin modified carbon nanotube/silver nanowire (TCNT/AgNW) film of the present invention;
FIG. 3 is a scanning electron microscope image of a transparent conductive thin film of tannic acid modified carbon nanotube/silver nanowire/poly-3, 4-ethylenedioxythiophene (TCNT/AgNW/PEDOT) of the present invention;
FIG. 4 is a graph showing the sheet resistance and transmittance of the tannic acid modified carbon nanotube/silver nanowire/poly 3, 4-ethylenedioxythiophene (TCNT/AgNW/PEDOT) transparent conductive film of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1-4, an embodiment of the present invention is shown: the utility model provides a novel flexible transparent electrode of double-deck electrically conductive network structure, includes a novel double-deck network electrically conductive structure, its characterized in that: the novel double-layer network conductive structure is formed by compounding tannic acid functionalized carbon nanotubes and silver nanowires, the functionalized carbon nanotube conductive network at the bottom layer provides a conductive path for the silver nanowires and can be used as a conductive adhesive to increase the conductive stability of a composite film and the adhesion between the silver nanowires and a substrate, a polyethylene terephthalate (PET) substrate film is ultrasonically cleaned by distilled water and ethanol and then dried, a prepared tannic acid modified carbon nanotube solution (TCNT) and silver nanowires (AgNW) are respectively coated on the PET film substrate by adopting a spraying method and a spin-coating layer-by-layer coating method to obtain a flexible transparent electrode of the double-layer conductive network structure, and then the conductive film is subjected to post-treatment by adopting mechanical pressing and spraying of a poly 3, 4-ethylenedioxythiophene (PEDOT) solution.
Further, the adopted raw materials are silver nanowire solution, the length of the silver nanowire solution is 40-60 mu m, the diameter of the silver nanowire solution is 40-70 nm, the purity of the single-walled carbon nanotube is more than 95 wt.%, the outer diameter of the single-walled carbon nanotube is 1-2 nm, the length of the single-walled carbon nanotube is 5-30 mu m, the tannin powder is AR grade, the pH value of the poly-3, 4-ethylenedioxythiophene solution is 1000, and the solid content of the poly-3, 4-ethylenedioxythiophene solution is 1-1.3%.
Further, the TCNT dispersion liquid is prepared by an ultrasonic dispersion machine under the conditions that the power is 100-200W and the time is 30-80min, the dispersing agent is sodium dodecyl benzene sulfonate, and the concentration of the prepared carbon nano tube solution is 0.1-0.5 mg/ml.
Furthermore, the concentration of the prepared silver nanowire aqueous solution is 0.8-1.2 mg/ml.
Further, diluting the poly 3, 4-ethylenedioxythiophene solution by 5-20 times, adding 5 wt.% of dimethyl sulfoxide, and stirring for more than 20 min.
Further, the transparency of the obtained transparent conductive film is 80% or more, the surface resistance can be 50 Ω/sq. or less, and the surface roughness is 10nm or less.
The invention also provides a preparation method of the novel flexible transparent electrode with the double-layer conductive network structure, which comprises the following steps:
a tannic acid functionalized carbon nanotube (TCNT) solution is prepared by dispersing SWCNT and tannic acid in deionized water in a ratio of 1: 1-4, stirring for 24 hours under a water bath heating condition at 60 ℃, centrifuging, filtering, freeze-drying to collect TCNT powder, dispersing a certain amount of TCNT in distilled water by using SDBS as a dispersing agent, performing water bath ultrasonic treatment for 30min, putting the solution into 120W probe ultrasonic treatment for continuous ultrasonic dispersion for 40min, centrifuging the mixed solution for 20min at 8000rmp, collecting 90% of supernatant to obtain TCNT suspension with corresponding concentration, spraying the prepared tannic acid modified carbon nanotube (TCNT) solutions with different amounts on a PET substrate by adopting a spraying method, drying after nitric acid soaking for 20min, spin-coating silver nanowire solutions with different concentrations on a TCNT layer at a rotating speed of 2000 rpm, and fully drying, and obtaining the film with the double-layer conductive network structure, wherein the final treatment process comprises mechanical pressing and surface PEDOT spraying: and a PSS solution, wherein the prepared double-layer conductive network film is placed on a tablet press and pressed for 10min under the pressure of 25MPa so as to weld silver nanowires with each other, and then 3ml of poly (3, 4-ethylenedioxythiophene) (PEDOT) solution is sprayed on the pressed film.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (7)
1. The utility model provides a novel flexible transparent electrode of double-deck electrically conductive network structure, includes a novel double-deck network electrically conductive structure, its characterized in that: the novel double-layer network conductive structure is formed by compounding tannic acid functionalized carbon nanotubes and silver nanowires, the functionalized carbon nanotube conductive network at the bottom layer provides a conductive path for the silver nanowires and can be used as a conductive adhesive to increase the conductive stability of a composite film and the adhesion between the silver nanowires and a substrate, a polyethylene terephthalate (PET) substrate film is ultrasonically cleaned by distilled water and ethanol and then dried, a prepared tannic acid modified carbon nanotube solution (TCNT) and silver nanowires (AgNW) are respectively coated on the PET film substrate by adopting a spraying method and a spin-coating layer-by-layer coating method to obtain a flexible transparent electrode of the double-layer conductive network structure, and then the conductive film is subjected to post-treatment by adopting mechanical pressing and spraying of a poly 3, 4-ethylenedioxythiophene (PEDOT) solution.
2. The novel flexible transparent electrode with a double-layer conductive network structure as claimed in claim 1, wherein: the method comprises the following steps of using a silver nanowire solution as a raw material, wherein the length of the silver nanowire solution is 40-60 mu m, the diameter of the silver nanowire solution is 40-70 nm, using a single-walled carbon nanotube with the purity of 95 wt.%, the outer diameter of 1-2 nm and the length of 5-30 mu m, using tannic acid powder, using AR-grade, using a poly-3, 4-ethylenedioxythiophene solution with the pH of 1000 and the solid content of 1-1.3%.
3. The novel flexible transparent electrode with a double-layer conductive network structure as claimed in claim 1, wherein: the TCNT dispersion liquid is prepared by an ultrasonic dispersion machine under the conditions that the power is 100-200W and the time is 30-80min, the dispersing agent is sodium dodecyl benzene sulfonate, and the concentration of the prepared carbon nano tube solution is 0.1-0.5 mg/ml.
4. The novel flexible transparent electrode with a double-layer conductive network structure as claimed in claim 1, wherein: the concentration of the prepared silver nanowire aqueous solution is 0.8-1.2 mg/ml.
5. The novel flexible transparent electrode with a double-layer conductive network structure as claimed in claim 1, wherein: diluting the poly 3, 4-ethylenedioxythiophene solution by 5-20 times, adding 5 wt.% of dimethyl sulfoxide, and stirring for more than 20 min.
6. The novel flexible transparent electrode with a double-layer conductive network structure as claimed in claim 1, wherein: the obtained transparent conductive film has transmittance of 80% or more, surface resistance of 50 Ω/sq. or less, and surface roughness of 10nm or less.
7. The novel flexible transparent electrode with a double-layer conductive network structure as claimed in claim 1, further comprising a preparation method, which comprises the following steps:
a tannic acid functionalized carbon nanotube (TCNT) solution is prepared by dispersing SWCNT and tannic acid in deionized water in a ratio of 1: 1-4, stirring for 24 hours under a water bath heating condition at 60 ℃, centrifuging, filtering, freeze-drying to collect TCNT powder, dispersing a certain amount of TCNT in distilled water by using SDBS as a dispersing agent, performing water bath ultrasonic treatment for 30min, putting the solution into 120W probe ultrasonic treatment for continuous ultrasonic dispersion for 40min, centrifuging the mixed solution for 20min at 8000rmp, collecting 90% of supernatant to obtain TCNT suspension with corresponding concentration, spraying the prepared tannic acid modified carbon nanotube (TCNT) solutions with different amounts on a PET substrate by adopting a spraying method, drying after nitric acid soaking for 20min, spin-coating silver nanowire solutions with different concentrations on a TCNT layer at a rotating speed of 2000 rpm, and fully drying, and obtaining the film with the double-layer conductive network structure, wherein the final treatment process comprises mechanical pressing and surface PEDOT spraying: and a PSS solution, wherein the prepared double-layer conductive network film is placed on a tablet press and pressed for 10min under the pressure of 25MPa so as to weld silver nanowires with each other, and then 3ml of poly (3, 4-ethylenedioxythiophene) (PEDOT) solution is sprayed on the pressed film.
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| CN115910432A (en) * | 2022-11-26 | 2023-04-04 | 宁波碳源新材料科技有限公司 | Non-covalent modified carbon nano tube flexible transparent conductive film and preparation method 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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