CN112011079A - Flexible transparent electrode of reinforced concrete structure and preparation method thereof - Google Patents
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2365/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention discloses a flexible transparent electrode with a reinforced concrete structure and a preparation method thereof, which mainly comprises the steps of realizing reduction and functionalization of Graphene Oxide (GO) by adopting dopamine of biomimetic adhesive protein through an in-situ polymerization one-step method, and increasing the conductive capacity of a film and the adhesion between a coating and a substrate as a conductive adhesive; the preparation method comprises the steps of coating a Polydopamine Functionalized Graphene (PFG), a Carbon Nano Tube (CNT) and a poly 3, 4-ethylenedioxythiophene (PEDOT) solution on a polyethylene terephthalate (PET) film substrate layer by adopting a spraying method to prepare a transparent electrode with a reinforced concrete structure, and then treating a conductive coating by using an organic solvent and inorganic acid synergistic treatment method to obtain the transparent electrode with good adhesion, low roughness and high conductivity. The process is simple and has short period.
Description
Technical Field
The invention belongs to the technical field of preparation of flexible transparent electrodes based on graphene, carbon nanotubes and conductive polymers, and particularly relates to a preparation process for improving the conductivity of a film and the adhesion of the film to a substrate.
Background
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. At present, the transparent conductive film material in the photoelectric device is mainly Indium Tin Oxide (ITO). However, due to the shortage of indium element, the price of indium rises year by year, and due to the limitation of the preparation process conditions, the cost of ITO is relatively expensive, and especially the brittleness of ITO limits the application of ITO in flexible electronic devices. The nano conductive material Carbon Nano Tube (CNT) is considered as an ideal ITO (indium tin oxide) substitute material for the transparent conductive film in the flexible electronic device in the future due to excellent mechanical, optical, electrical and thermal properties. However, many problems must be overcome, such as poor interfacial adhesion of the CNT thin film to the substrate, and the large roughness of the thin film due to the mutual overlapping of the carbon nanotubes in the thin film is not good for improving the device performance. The dopamine of the biomimetic adhesive protein can realize reduction and modification of graphene oxide in the polymerization process, so that the poly-dopamine functionalized graphene is introduced into a CNT film to be used as a conductive adhesive to improve the adhesion of the film, and the poly-3, 4-ethylenedioxythiophene: sodium polystyrene sulfonate (PEDOT: PSS) has excellent conductivity, light transmittance and good film forming property and can be used for reducing the roughness of a film. A high-performance transparent conductive film is prepared by a simple and convenient process, and a polydopamine functionalized graphene/carbon nano tube/poly 3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) flexible transparent electrode with a reinforced concrete structure is prepared by a simple spraying method.
Disclosure of Invention
The invention aims to provide a preparation method of a polydopamine functionalized graphene/carbon nano tube/poly 3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) flexible transparent electrode with a reinforced concrete structure, so that the transparent electrode has excellent photoelectric performance, super-strong adhesion, extremely low roughness and a stable structure, and is widely applied to the fields of photoelectric devices, displays, touch screens and the like.
The technical scheme of the invention is as follows: the main steps are that firstly, the polyethylene terephthalate (PET) substrate is cleaned by ethanol ultrasonic wave and then dried. The preparation method comprises the steps of coating a poly-dopamine functional graphene, a carbon nano tube and a poly-3, 4-ethylenedioxythiophene solution on a PET substrate layer by adopting a simple spraying method to obtain a poly-dopamine functional graphene/carbon nano tube/poly-3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) flexible transparent electrode with a reinforced concrete structure. The dopamine of the biomimetic adhesive protein can realize reduction and functionalization of graphene oxide in the polymerization process, can improve the conductivity of the film and can be used as a conductive adhesive to improve the adhesion of a coating to a substrate; the PEDOT layer is post-treated by adopting an organic solvent and an inorganic acid, so that the conductivity of the film can be greatly improved, and the roughness of the film can be reduced. The preparation process is simple, short in period and excellent in film performance, when the light transmittance is 75-90%, the surface resistance is 25-200 omega/sq, and the surface roughness is less than 10 nm. The characterization result of a scanning electron microscope shows that the poly-dopamine functionalized graphene, the carbon nano tube and the poly-3, 4-ethylenedioxythiophene in the transparent electrode are not simply stacked, but are intersected with each other through pi-pi action to form a stable reinforced concrete structure, so that the film has more excellent photoelectric property and stability.
The main innovation points of the invention are as follows:
1. the reduction and functionalization of graphene oxide are realized by the in-situ polymerization one-step method of dopamine, and the functionalized graphene can be used as a conductive adhesive to improve the conductive capability of a film and improve the adhesion of a coating to a substrate;
2. strong pi-pi effects exist among the poly-dopamine functionalized graphene, the carbon nano tube and the poly-3, 4-ethylenedioxythiophene, the strong pi-pi effects can improve the conductivity of the film, and a reinforced concrete structure formed by the poly-dopamine functionalized graphene, the carbon nano tube and the poly-3, 4-ethylenedioxythiophene is favorable for improving the stability of the film;
3. the conductivity of the transparent electrode can be greatly improved by a synergistic treatment method of an organic solvent (DMSO-EG) and an inorganic acid (H2 SO 4).
The method for preparing the poly-dopamine functionalized graphene comprises the following steps: firstly, weighing a certain amount of GO, adding the weighed GO into a certain amount of tris buffer solution, stirring and ultrasonically dispersing for a certain time to obtain a uniform GO dispersion liquid, and adjusting the pH value of the buffer solution to 8.5-9. And adding a certain amount of dopamine into the solution, stirring vigorously continuously, stirring at a constant temperature of 60 ℃ for 12-24 hours, keeping introducing oxygen, and centrifuging the solution for multiple times after stirring to obtain the PFG dispersion liquid with the concentration of 0.5-2 mg/ml. The method for preparing the carbon nanotube dispersion liquid is as follows: the method is characterized in that 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 is used as a raw material, sodium dodecyl benzene sulfonate is used as a dispersing agent, and distilled water is used as a solvent. The method comprises the following steps of (1): 5-1: 10, adding distilled water with a corresponding volume, performing water bath ultrasound for 30-80 min, performing ultrasound for 35 min by using an ultrasonic cell crusher, centrifuging for 15 min at a speed of 8000 r/min by using a centrifuge, and extracting supernatant to obtain carbon nanotube dispersion liquid with the concentration of 0.1-1 mg/ml. And coating the prepared solutions of the Polydopamine Functionalized Graphene (PFG), the Carbon Nano Tube (CNT) and the poly 3, 4-ethylenedioxythiophene (PEDOT) with different amounts on the PET film substrate layer by adopting a spraying method. And soaking the prepared transparent electrode in EG solution for 20-40 min, washing and drying the film by deionized water, soaking the film in 10M-12M H2SO4 again, and drying to obtain the transparent electrode with good adhesion, low roughness and high conductivity.
Reagents and materials used in the invention: dopamine, tris buffer solution, Graphene Oxide (GO), single-walled Carbon Nanotubes (CNT), poly-3, 4-ethylenedioxythiophene (PEDOT: PSS), polyethylene terephthalate (PET), sodium dodecylbenzene sulfonate, sulfuric acid (H2 SO 4), dimethyl sulfoxide (DMSO), distilled water, ethanol and the like.
The surface resistance and the light transmittance of the transparent conductive film are respectively measured by adopting a Gishili 2700 and an ultraviolet spectrophotometer. Scanning Electron Microscopy (SEM) was used to characterize the morphology of the prepared carbon nanotube/poly-3, 4-ethylenedioxythiophene/carbon nanotube (CNT/PEDOT/CNT) films.
Drawings
Fig. 1 is a schematic diagram of a poly-dopamine functionalized graphene/carbon nanotube/poly-3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) transparent conductive film.
Fig. 2 shows the sheet resistance and the light transmittance of the poly-dopamine functionalized graphene/carbon nanotube/poly-3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) transparent conductive film.
Fig. 3 shows the change of resistance of the poly-dopamine functionalized graphene/carbon nanotube/poly-3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) transparent conductive film exposed to air.
Fig. 4 is a schematic diagram of a transparent electrode lighting bulb made of a poly-dopamine functionalized graphene/carbon nanotube/poly-3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) transparent conductive film.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1:
1. adding 200 mg of GO into 400 mL of tris buffer solution, stirring and ultrasonically dispersing for 30 min to obtain a uniform GO dispersion solution, and adjusting the pH value of the buffer solution to 8.5. Then adding 100 mg of dopamine into the GO-dispersed tris buffer solution and stirring vigorously, stirring at a constant temperature of 60 ℃ for 24 hours while keeping oxygen introduced, and centrifuging the solution for multiple times after stirring to obtain PFG dispersion liquid with the concentration of 0.5 mg/mL;
2. taking 20 mg of single-walled carbon nanotube raw material and 200 mg of sodium dodecyl benzene sulfonate as a dispersing agent, adding 20 ml of distilled water, carrying out water bath ultrasound for 30 min, carrying out ultrasound for 70 min by adopting an ultrasonic cell crusher, centrifuging for 15 min at a speed of 8000 r/min by using a centrifuge, and extracting supernatant to obtain carbon nanotube dispersion liquid with the concentration of about 1 mg/ml;
3. diluting poly 3, 4-ethylenedioxythiophene solution with solid content of 1 wt.% by 5 times, adding 5 wt.% dimethyl sulfoxide, and stirring for more than 20 min;
4. and (3) placing the cleaned PET film on a heating plate, controlling the temperature on the heating plate to be 105 ℃, spraying the poly-dopamine functional graphene, the carbon nano tube and the poly-3, 4-ethylenedioxythiophene solution in sequence, and obtaining the poly-dopamine functional graphene/carbon nano tube/poly-3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) transparent electrodes with different transmittances through different spraying amounts. And soaking the prepared transparent electrode into EG solution for 40 min, washing and drying the film by deionized water, and soaking the film into 12M H2SO4 again to obtain the transparent electrode with the surface resistance of 25-80 omega/sq DEG and the surface roughness of less than 5 nm when the light transmittance is 75-90%.
Example 2:
1. adding 400 mg of GO into 400 mL of tris buffer solution, stirring and ultrasonically dispersing for 30 min to obtain a uniform GO dispersion solution, and adjusting the pH value of the buffer solution to 9. Then adding 200 mg of dopamine into the GO-dispersed trihydroxymethylaminomethane Tri buffer solution, stirring vigorously continuously, stirring at a constant temperature of 60 ℃ for 10 hours, keeping oxygen introduced during stirring, and centrifuging the solution for multiple times to obtain a PFG (poly-fluoro-ethylene) dispersion liquid with the concentration of 1 mg/mL after stirring;
2. taking 10 mg of single-walled carbon nanotube raw material and 100 mg of sodium dodecyl benzene sulfonate as a dispersing agent, adding 20 ml of distilled water, carrying out water bath ultrasound for 30 min, carrying out ultrasound for 70 min by adopting an ultrasonic cell crusher, centrifuging for 15 min at a speed of 8000 r/min by using a centrifuge, and extracting supernatant to obtain carbon nanotube dispersion liquid with the concentration of about 0.5 mg/ml;
3. diluting poly 3, 4-ethylenedioxythiophene solution with solid content of 1.3 wt.% by 10 times, adding 5 wt.% dimethyl sulfoxide, and stirring for more than 20 min;
4. and (3) placing the cleaned PET film on a heating plate, controlling the temperature on the heating plate to be 105 ℃, spraying the poly-dopamine functional graphene, the carbon nano tube and the poly-3, 4-ethylenedioxythiophene solution in sequence, and obtaining the poly-dopamine functional graphene/carbon nano tube/poly-3, 4-ethylenedioxythiophene (PFG/CNT/PEDOT) transparent electrodes with different transmittances through different spraying amounts. And soaking the prepared transparent electrode into EG solution for 20 min, washing and drying the film by deionized water, and soaking the film into 10M H2SO4 again to obtain the transparent electrode with the surface resistance of 25-200 omega/sq DEG and the surface roughness of less than 10 nm when the light transmittance is 75-90%.
Claims (10)
1. A flexible transparent electrode with a reinforced concrete structure and a preparation method thereof mainly comprises the steps of realizing reduction and functionalization of Graphene Oxide (GO) by adopting dopamine of biomimetic adhesive protein through in-situ polymerization by a one-step method, and increasing the conductive capacity of a film and the adhesion between a coating and a substrate by using the dopamine as a conductive adhesive; ultrasonically cleaning a polyethylene terephthalate (PET) substrate film by using distilled water and ethanol, and then drying;
coating the prepared poly-dopamine functionalized graphene (PFG), carbon nano-tube (CNT) and poly-3, 4-ethylenedioxythiophene (PEDOT) solution on a PET film substrate layer by adopting a spraying method, wherein the PEDOT solution is diluted and then added with dimethyl sulfoxide (DMSO) to enable the solution to be easily sprayed, preparing a transparent electrode with a reinforced concrete structure from the PFG, the CNT and the PEDOT coated on the PET film substrate layer by layer, and then treating the conductive coating by using an organic solvent and inorganic acid synergistic treatment method to obtain the transparent electrode with good adhesion, low roughness and high conductivity; the transparent electrode is simple in preparation process and short in period, the reinforced concrete structure enables the structure of the film to be stable, the adhesion force to be strong and the roughness to be low, the conductivity of the electrode after high-efficiency post-treatment is greatly improved, when the light transmittance is 75-90%, the surface resistance is 25-200 omega/sq., and the surface roughness is less than 10 nm;
the high-performance transparent electrode can be widely applied to the aspects of organic light-emitting devices, displays, touch screens, thin film transistors, photovoltaic devices and the like.
2. The method according to claim 1, characterized in that the raw material used is graphene oxide powder; the single-walled carbon nanotube has the purity of more than 95 wt.%, the outer diameter of 1-2 nm and the length of 5-30 μm; the PH value of the poly 3, 4-ethylenedioxythiophene solution is 1000, and the solid content is 1-1.3%.
3. The method of claim 1, wherein the concentration of the prepared poly-dopamine functionalized graphene (PFG) solution is 0.1-2 mg/ml.
4. The method according to claim 1, wherein the conditions for preparing the carbon nanotube dispersion using the ultrasonic cell disruptor are as follows: the power is 100-.
5. The method according to claim 1, wherein the poly (3, 4-ethylenedioxythiophene) solution is diluted by 5 to 20 times, then 5 wt.% of dimethyl sulfoxide is added, and the mixture is stirred for more than 20 min.
6. The method of claim 1, wherein the PET film substrate is coated with the prepared solutions of Polydopamine Functionalized Graphene (PFG), Carbon Nanotube (CNT) and poly 3, 4-ethylenedioxythiophene (PEDOT) in different amounts layer by a spray coating method.
7. The method of claim 1, wherein the organic solvent is dimethyl sulfoxide (DMSO) and Ethylene Glycol (EG), the inorganic acid is sulfuric acid (H2 SO 4), the prepared transparent electrode is soaked in the EG solution for 20-40 min, the film is washed with deionized water and dried, and then is soaked in 10M-12M H2SO4 again, and the transparent electrode with good adhesion, low roughness and high conductivity is obtained after drying.
8. The method of claim 1, wherein the transparent electrode has a "reinforced concrete" structure with a carbon nanotube layer sandwiched between a poly-dopamine functionalized graphene layer and a poly-3, 4-ethylenedioxythiophene layer, and the electrode structure has excellent stability and adhesion.
9. The method according to claim 1, wherein the transparency of the obtained transparent conductive film is 75% or more, the sheet resistance is 200 Ω/sq. or less, and the surface roughness is 10 nm or less.
10. The method of claim 1, wherein the high performance transparent electrode is widely applicable to organic light emitting devices, displays, touch panels, thin film transistors, and photovoltaic devices.
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| DE102013223569A1 (en) * | 2013-11-19 | 2015-05-21 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | A method of making a homogeneous conductive carbon nanotube-containing coating on a substrate and substrate having a homogeneous conductive carbon nanotube-containing coating |
| CN105321592A (en) * | 2014-08-01 | 2016-02-10 | 广东阿格蕾雅光电材料有限公司 | CNT (carbon nanotube)-polymer laminated composite flexible transparent electrode and preparation method thereof |
| CN108470598A (en) * | 2018-04-06 | 2018-08-31 | 天津工业大学 | Flexible transparent conductive film and preparation method thereof |
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| DE102013223569A1 (en) * | 2013-11-19 | 2015-05-21 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | A method of making a homogeneous conductive carbon nanotube-containing coating on a substrate and substrate having a homogeneous conductive carbon nanotube-containing coating |
| CN105321592A (en) * | 2014-08-01 | 2016-02-10 | 广东阿格蕾雅光电材料有限公司 | CNT (carbon nanotube)-polymer laminated composite flexible transparent electrode and preparation method thereof |
| CN108470598A (en) * | 2018-04-06 | 2018-08-31 | 天津工业大学 | Flexible transparent conductive film and preparation method thereof |
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