CN110317525B - Conductive polymer aqueous slurry and preparation method and application thereof - Google Patents

Conductive polymer aqueous slurry and preparation method and application thereof Download PDF

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CN110317525B
CN110317525B CN201910647612.2A CN201910647612A CN110317525B CN 110317525 B CN110317525 B CN 110317525B CN 201910647612 A CN201910647612 A CN 201910647612A CN 110317525 B CN110317525 B CN 110317525B
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conductive polymer
water
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polymer aqueous
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CN110317525A (en
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周海涛
江百昌
胡婉洁
麦文清
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Zhou Haitao
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
    • C09D125/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D165/00—Coating compositions based on macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0806—Silver
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention relates to conductive polymer aqueous slurry and a preparation method and application thereof, wherein the conductive polymer aqueous slurry is prepared from the following raw materials in percentage by weight: PEDOT/PSS conductive polymer aqueous solution: 16 wt% to 89 wt%; conductive inorganic material modification reinforcing agent: 0.2 to 5.0 wt%; conductive polymer activator: 0.05wt% to 4.5 wt%; connecting materials: 0.2 to 3.0 wt%; surface tension adjusting agent: 0.01wt% to 0.5 wt%; leveling agent: 0.01wt% to 15 wt%; defoaming agent: 0.01wt% to 20 wt%; thickening agent: 0.2 to 2.0 wt%; a crosslinking agent: 0.01 to 2.0 wt%; volatile regulators: 0wt% to 20 wt%; humectant: 0wt% to 5.0 wt%; other functional additives: 0.01wt% to 1.0 wt%; water: and (4) the balance. The conductive layer prepared by the conductive polymer aqueous slurry has excellent conductivity and friction resistance, and also has good light transmittance.

Description

Conductive polymer aqueous slurry and preparation method and application thereof
Technical Field
The invention relates to the field of conductive polymer materials, in particular to conductive polymer aqueous slurry, a preparation method, an application process and a case thereof.
Background
In the field of the existing circuit electrodes for large-scale commercial application, particularly transparent conductive circuits and transparent electrodes, yellow wet etching and laser etching processes adopted by Indium Tin Oxide (ITO), metal grids and nano silver wire coating films have the problems of complicated procedures, material waste and serious environmental pollution, and bring about a lot of troubles to production and manufacturing of enterprises. Although the conductive polymer has been developed for many years, its conductivity has been a weak point, and it is difficult to apply to high-end electronic components. For example, chinese patent application No. 201410215856.0 discloses a method for manufacturing a transparent conductive polymer film, comprising: providing an aqueous conductive polymer solution, wherein the aqueous conductive polymer solution comprises PEDOT: PSS; adding a conductive additive into the conductive polymer aqueous solution to prepare a dispersion liquid; disposing the dispersion on the surface of the substrate to form a dispersion film; and drying the dispersion liquid film at a temperature of 140 ℃ or higher to obtain the polymer transparent conductive film. However, the sheet resistance of the transparent conductive coating prepared by the method is 100-300 omega/□, the light transmittance is 80-90%, and the conductivity of the conductive coating is poor due to the need of keeping high light transmittance. The existing components designed by the polymer transparent conductive circuit or the transparent conductive electrode generally have the defects of reduced photoelectric function caused by heating, large current passing limitation and voltage drop, and the hardness, the friction resistance and the like of the surface of the conductive layer need to be enhanced.
Disclosure of Invention
In view of the defects of the prior art, the first purpose of the invention is to provide conductive polymer aqueous slurry with good conductivity and friction resistance. The second purpose of the invention is to provide a preparation method of the conductive polymer aqueous slurry. The third purpose of the invention is to provide the application of the conductive polymer aqueous slurry in preparing a conductive layer.
In order to achieve the first purpose of the invention, the invention provides conductive polymer aqueous slurry which is prepared from the following raw materials in percentage by weight:
PEDOT/PSS conductive polymer aqueous solution: 16 wt% to 89 wt%;
conductive inorganic material modification reinforcing agent: 0.2 to 5.0 wt%;
conductive polymer activator: 0.05wt% to 4.5 wt%;
connecting materials: 0.2 to 3.0 wt%;
surface tension adjusting agent: 0.01wt% to 0.5 wt%;
leveling agent: 0.01wt% to 15 wt%;
defoaming agent: 0.01wt% to 20 wt%;
thickening agent: 0.2 to 2.0 wt%;
a crosslinking agent: 0.01 to 2.0 wt%;
volatile regulators: 0wt% to 20 wt%;
humectant: 0wt% to 5.0 wt%;
other functional additives: 0.01wt% to 1.0 wt%;
water: and (4) the balance.
Therefore, the conductive polymer aqueous slurry is modified and enhanced by adopting the conductive inorganic material modification enhancer. The conductive polymer aqueous solution of PEDOT/PSS is an aqueous solution of poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid), the weight percentage of the conductive polymer aqueous solution of PEDOT/PSS in the conductive polymer aqueous slurry is higher, the conductive polymer aqueous slurry has good film forming performance, the conductive layer has good tensile property after film forming, and the PEDOT/PSS forms a uniform conductive substrate after film forming, so that the conductive uniformity of the conductive layer can be effectively maintained. The conductive inorganic material modification reinforcing agent has the advantages that the mechanical strength of the conductive inorganic material modification reinforcing agent can endow the conductive layer with good friction resistance and improve the surface hardness, a non-uniform net-shaped structure is formed in the dried conductive layer, the electron moving speed in the conductive inorganic material modification reinforcing agent is high, the conductive inorganic material modification reinforcing agent and the PEDOT/PSS conductive polymer aqueous solution are compounded for use, and the conductive inorganic material modification reinforcing agent and the PEDOT/PSS conductive polymer aqueous solution have synergistic effect, so that the conductive performance can be effectively improved. The conductive polymer aqueous slurry can be directly patterned through the additive process designed by the circuit electrode, is used for manufacturing a transparent conductive electrode and a transparent conductive circuit to form a transparent conductive film layer with the thickness of 0.1-0.5 mu m, has high light transmittance and ultralow impedance, and also has the characteristic of high weather resistance. In addition, the slurry of the present invention is aqueous, environmentally friendly, and has good processability.
The further technical proposal is that the weight percentage of PEDOT/PSS conductive macromolecule aqueous solution is 35 wt% to 89 wt%; the solid content of the PEDOT/PSS conductive polymer aqueous solution is 0.5wt% to 2.0wt%, the conductivity is 150S/cm to 1100S/cm, and the solvent is deionized water.
As can be seen from the above, the invention further prefers the weight percentage, solid content and conductivity of the PEDOT/PSS conductive polymer aqueous solution, and when the parameters are within the above ranges, the conductive property, film forming property and tensile property can be further improved. The PEDOT/PSS conductive polymer aqueous solution can be an aqueous solution per se, has the solid content of 0.9 wt% to 1.5wt%, and can also be prepared by dissolving gel-state PEDOT/PSS in water.
The further technical proposal is that the conductive inorganic material modification reinforcing agent is at least one of carbon nano-tubes, graphene and silver nano-wires; the carbon nanotube has an average diameter of 10nm to 30nm, an average length of 10 μm to 30 μm, and a specific surface area of 50m2G to 150m2(ii)/g; the specific surface area of the graphene is 150m2G to 350m2(ii)/g, D50 is from 5 μm to 10 μm, the mean longitudinal dimension is 1nm and 3nm, and the mean transverse dimension is less than or equal to 5 μm; the diameter of the nano silver wire is 8nm to 40nm, the average length is 8 mu m to 40 mu m, and the length-diameter ratio is 500 to 1200.
Therefore, the conductive inorganic material modification reinforcing agent is one or a combination of carbon nanotubes, graphene and silver nanowires, the fillers can provide a conductive mesh structure after film formation, and the filler and PEDOT/PSS are cooperated to endow the conductive layer with excellent conductivity, so that when the minimum sheet resistance of the printed transparent conductive coating is reduced to 2 omega/□ -5 omega/□, the light transmittance of the conductive layer can still reach over 80 percent, and when the transparent conductive coating is designed into a transparent conductive circuit, the application problems caused by heating, large current and voltage drop are avoided, and the requirements of upper and lower process turnover and rear-end packaging on the hardness and the friction resistance of the coating in the manufacturing process are also met. The nano silver wire can be dispersed in water, prepared into a suspension with the mass fraction of 0.5-10.0% and then added, the nano silver wire has a strong conductive effect, and the prepared conductive layer has good light transmittance; the carbon nanotubes are black powder and are generally directly added for use, or the carbon nanotubes are dispersed in water to prepare turbid liquid to be added, so that the carbon nanotubes have high conductivity and can improve the strength and the wear resistance of the conductive layer; the graphene is black, fluffy and light powder and can be directly added for use, the graphene can also be dispersed in water to prepare paste dispersion liquid and then added, and the graphene can improve the conductivity of the slurry and endow the conductive layer with good performances such as heat conduction, corrosion resistance, wear resistance, toughness and the like.
The further technical scheme is that the conductive inorganic material modification reinforcing agent is at least two of carbon nano-tubes, graphene and silver nano-wires.
As can be seen from the above, the conductive inorganic material modification enhancer of the present invention is preferably a combination of at least two of the above to achieve a balance between the improvement of conductivity and friction resistance. When the combination contains graphene, the sheet structure of the graphene can play a role in reinforcing the joint between the carbon nanotube or silver nanowire and PEDOT/PSS.
The further technical scheme is that the nano silver wire is subjected to surface passivation treatment by inert metal, and the inert metal is at least one of gold, platinum and palladium.
Therefore, the silver nanowire can be coated by inert metal, and the resistance of the silver nanowire in the process of oxidation resistance, sulfuration resistance and the like is improved through the core-shell structure passivation treatment process.
The further technical proposal is that the conductive polymer activating agent is dimethyl sulfoxide and a pH value regulator; the pH value regulator is at least one of water-soluble organic acid, water-soluble organic amine and ammonia water; the water-soluble organic acid is at least one of acetic acid and lactic acid; the water-soluble organic amine is at least one of monoethanolamine, diethanolamine, triethanolamine and N, N-dimethylethanolamine.
Therefore, dimethyl sulfoxide and a pH value regulator can be used as activators of the conductive polymer, and the dimethyl sulfoxide and the conductive polymer can form a conjugated system, so that the restriction of movement of electrons is reduced, and the conductivity of the conductive polymer is improved; the conductive polymer has stronger conductivity in a weak acidic system than an alkaline system, and the pH value regulator can regulate the acidity and alkalinity of the slurry so as to keep the slurry in weak acidity.
The further technical scheme is that the connecting material is at least one of water-soluble cellulose ether, polyvinyl alcohol, polyethylene glycol, water-dispersible acrylic emulsion and water-dispersible polyurethane emulsion, and the water-soluble cellulose ether is at least one of hydroxypropyl cellulose and hydroxypropyl methyl cellulose.
Therefore, the invention can adopt the high polymer materials as the connecting agent, and the high polymer materials endow the slurry with good film-forming property and mechanical property.
The further technical proposal is that the surface tension regulator is at least one of alkyl alcohol ether carboxylate, fluorocarbon surfactant, silicone surfactant, alkynol surfactant, alkyl glucoside, fatty glyceride, span and Tween.
Therefore, the surfactant can be used as a tension regulator in the invention, and the surface tension of the system can be effectively regulated.
The further technical scheme is that the flatting agent is at least one of an acrylic flatting agent, an acrylate flatting agent, a fluorine modified acrylate flatting agent, a silane wetting flatting agent, a fluorocarbon flatting agent, a higher alcohol and a dihydric alcohol polycondensate.
Therefore, the leveling agent can be used for improving the wetting and leveling performance of the slurry on a base material and preventing the defects of film formation such as shrinkage, needle eyes, orange peel and the like. Wherein the higher alcohol can be diacetone alcohol and primary alcohol and secondary alcohol containing more than five carbons, and the dihydric alcohol polycondensate can be polyethylene glycol and derivatives thereof.
The further technical scheme is that the defoaming agent is at least one of oxygen-containing solvents such as nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, organic silicon, polyether modified organic silicon, alcohols and the like, and acetylene glycol type defoaming agents.
As can be seen from the above, the present invention can eliminate the bubbles in the slurry and suppress the generation of bubbles by using the above-mentioned defoaming agent.
The further technical scheme is that the thickening agent is at least one of polyurethane thickening agent, acrylic thickening agent, polyoxyethylene ether, cellulose ether and fumed silica.
Therefore, the thickening agent can be used for endowing the paste with thixotropic property and adjusting the viscosity of the paste, so that the storage stability of the paste is enhanced, the printing process adaptability of the paste is improved, and the minimum pitch precision of paste printing can reach 0.06 mm.
The further technical scheme is that the cross-linking agent is more than one of a water-based blocked isocyanate curing agent, an aziridine cross-linking agent, an aziridine modified isocyanate cross-linking agent, a silane coupling agent, an organic titanium cross-linking agent and an organic zirconium cross-linking agent.
As can be seen from the above, the present invention can use the above-mentioned cross-linking agent to improve the cross-linking density between organic materials and inorganic materials, between organic materials and organic materials, and between slurry and a substrate, and to improve the adhesion fastness of a conductive layer to the substrate, and the mechanical strength and chemical resistance of the conductive layer.
The further technical scheme is that the volatility regulator is at least one of alcohol and alcohol ether, the alcohol is at least one of ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, tert-butanol, n-pentanol, isopentanol, sec-pentanol, n-hexanol, isohexanol, sec-hexanol, tert-hexanol, n-octanol, isooctanol, sec-octanol and diacetone alcohol, and the alcohol ether is at least one of ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, propylene glycol methyl ether and propylene glycol ethyl ether.
Therefore, the volatility regulator can be used for regulating the volatilization speed of the slurry to match different operation processes, so that a high-quality film layer is obtained.
The further technical scheme is that the humectant is at least one of dihydric alcohol and derivatives thereof, and trihydric alcohol and derivatives thereof.
Therefore, the invention can adopt the humectant to improve the moisture retention of the slurry and prevent the adverse effect caused by too fast volatilization of water in the operation process. The humectant can be one or more of ethylene glycol, propylene glycol, glycerol, and butanediol.
The further technical proposal is that the other functional additives are at least one of odor masking agent, dispersant and film forming auxiliary agent.
Therefore, the invention can also be added with an odor covering agent, a dispersing agent, a film forming additive and the like for further improving or enhancing the odor, the dispersibility, the film forming property and the like of the slurry.
The further technical proposal is that the water is deionized water, ultrapure water, distilled water and filtered tap water.
Therefore, the water with higher purity can be adopted in the water, and the influence of impurities on the performance of the conducting layer is reduced.
In order to achieve the second object of the present invention, the present invention provides a method for preparing the above conductive polymer aqueous slurry, comprising the steps of:
a first mixing step: sequentially adding the PEDOT/PSS conductive polymer aqueous solution, the conductive polymer activator and the conductive inorganic material modification reinforcing agent into a container for dispersion;
a second mixing step: adding the connecting material, the surface tension regulator, the leveling agent, the defoaming agent, the volatile regulator, the humectant and the other functional additives, and dispersing;
a third mixing step: adding the cross-linking agent, the thickening agent and the balance of water, and dispersing.
Therefore, the slurry is mainly prepared through three mixing steps, all raw materials can be fully and uniformly mixed through the three mixing steps, and the slurry is simple in process, high in production efficiency and low in cost.
The further technical scheme is that the temperature of the first mixing step, the second mixing step and the third mixing step is 15-35 ℃, and the stirring speed is 200-1000 r/min; the stirring time of the first mixing step is 5min to 15min, the stirring time of the second mixing step is 5min to 15min, and the stirring time of the third mixing step is 20min to 40 min.
Therefore, the invention further optimizes the process conditions of each mixing step and is beneficial to obtaining the aqueous conductive slurry with good dispersibility.
The further technical scheme is that the method also comprises a dispersion step before the mixing step: preparing PEDOT/PSS conductive polymer aqueous solution gel particles, a conductive inorganic material modification reinforcing agent and a connecting material into a dispersion liquid or suspension liquid.
Therefore, before mixing, the PEDOT/PSS conductive polymer aqueous solution gel particles, the conductive inorganic material modification reinforcing agent and the connecting material can be prepared into dispersion liquid or suspension liquid, so that subsequent mixing and uniform dispersion are facilitated. If fumed silica is used as the thickening agent, the fumed silica can also be formulated into a fumed silica paste dispersion prior to mixing.
The further technical scheme is that the method also comprises a filtering step after the mixing step: filtering with 100-200 mesh filter screen.
Therefore, the invention can also filter the slurry to remove large-particle insoluble substances and improve the uniformity of the slurry and the prepared conductive layer.
In order to achieve the third object of the present invention, the present invention provides an application of the above conductive polymer aqueous paste in preparing a conductive layer, wherein the conductive polymer aqueous paste is used for preparing the conductive layer through at least one of a liquid atomization 3D printing process, a screen printing process, a roll-to-roll gravure printing process, a flexographic printing process, and a mask spraying process.
Therefore, the conductive polymer aqueous slurry provided by the invention adopts a direct patterning process, is suitable for various mainstream patterning processes, can adopt liquid atomization 3D printing processes, screen printing processes, reel-to-reel gravure printing processes, flexographic printing processes, mask spraying processes and other additive process processes for preparing the transparent conductive circuit and the transparent conductive electrode, avoids the problems of complicated processes, material waste and serious environmental pollution caused by subtractive process processes, and also brings revolutionary promotion on the conductive layer manufacturing process. The prepared conducting layer can be widely applied to the fields of touch control based on capacitive design, electromagnetic radiation prevention based on transparent conducting coating design, electromagnetic shielding and the like, electroluminescence and electrochromism based on transparent electrode interlayer design, transparent advertising boards, signs, oversized LED screens based on transparent circuit design, solar cells and the like, photoelectric components can be thinned, the development trend of electronic components is met, and the target of market application requirements is met.
The further technical scheme is that the conducting layer is prepared on a substrate, the substrate is the surface of an organic material, an inorganic material or a functional coating, and the organic material is a film or a plate made of at least one of polyurethane, polyester, polycarbonate, polyimide, polyvinyl chloride and acrylic resin; the inorganic material is ceramic, glass or crystalline silicon material.
Therefore, different base materials can be selected according to the requirements of the base material of the conducting layer, the conducting layer can be firmly attached to the base material, the base material can be a film material or a special-shaped base material, and the conducting polymer aqueous slurry can be used for forming films on different base materials.
The further technical scheme is that the drying temperature of the conductive polymer aqueous slurry is 100-160 ℃, and the drying time is 1-60 min.
Therefore, when the conductive layer is prepared by the conductive polymer aqueous slurry, the temperature can be raised and the conductive layer can be dried, the process conditions are simple, and the aqueous solvent can be effectively removed.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
The embodiment provides a modified reinforced conductive polymer aqueous slurry, which is prepared from the following raw materials in percentage by weight:
PEDOT/PSS conductive polymer aqueous solution: 50wt% and a solid content of 1.2 wt%;
conductive inorganic material modification reinforcing agent: 1.5wt% of graphene and 0.5wt% of nano silver wire;
dimethyl sulfoxide: 2.5 wt%;
acetic acid: 0.02 wt%;
polyvinyl alcohol: 0.5 wt%;
fluorocarbon surfactant: 0.05 wt%;
diacetone alcohol (leveling agent): 6 wt%;
defoaming agent: 0.05 wt%;
polyurethane thickener: 0.50 wt%;
aqueous blocked isocyanate curing agent (crosslinking agent): 0.1 wt%;
ethylene glycol monobutyl ether (volatility regulator): 5 wt%;
ethylene glycol (humectant): 2 wt%;
2-hexanol (odor masking agent): 0.05 wt%;
water: and (4) the balance.
The modified reinforced conductive polymer aqueous slurry of the embodiment is prepared according to the following method:
preparing materials: preparing raw materials according to a formula ratio; preparing graphene dispersion liquid from the graphene with the formula amount, preparing a nano silver wire suspension from the nano silver wire with the formula amount, and preparing a polyvinyl alcohol aqueous solution from the polyvinyl alcohol with the formula amount;
dispersing: at the temperature of 15-35 ℃, sequentially adding PEDOT/PSS conductive polymer aqueous solution with the solid content of 1.2wt%, dimethyl sulfoxide, acetic acid and a conductive inorganic material modification reinforcing agent into a stainless steel stirring barrel under the stirring state of 200 r/min-1000 r/min, and dispersing for 10 min; then adding polyvinyl alcohol aqueous solution, fluorocarbon surfactant, diacetone alcohol, defoaming agent, ethylene glycol monobutyl ether, ethylene glycol and 2-hexanol, and dispersing for 10 min; then sequentially adding the water-based closed isocyanate curing agent, the polyurethane thickener and the balance of water, and dispersing for 30 min;
and (3) filtering: filtering with 100-200 mesh filter screen to obtain modified reinforced conductive polymer aqueous slurry.
The process and application of the modified reinforced conductive polymer aqueous slurry for preparing the electrode of the embodiment are as follows:
step 1: preparing a graphical transparent conductive pattern on a transparent Polycarbonate (PC) film by using the prepared modified reinforced conductive polymer aqueous slurry through an additive mask spraying process, and baking the graphical transparent conductive pattern in a drying oven at 100 ℃ for 30min to obtain a graphical conductive coating;
step 2: coating a layer of electrochromic material on the surface of the conductive coating based on the PC film by using a spraying process to form an electrochromic coating;
and step 3: preparing a layer of transparent conductive electrode coating on the surface of the electrochromic coating formed in the step 2 by using the prepared modified reinforced conductive polymer aqueous slurry through a spraying process, and then packaging;
and 4, step 4: and (3) connecting the conductive coatings formed in the steps 1 and 3 with a power supply and driving, so that the electro-chromic areas with the same graphical patterns as the steps 1 can be formed.
Example 2
The embodiment provides a modified reinforced conductive polymer aqueous slurry, which is prepared from the following raw materials in percentage by weight:
PEDOT/PSS conductive polymer aqueous solution: 50wt% and a solid content of 1.2 wt%;
conductive inorganic material modification reinforcing agent nano silver wire: 0.5 wt%;
dimethyl sulfoxide: 2.5 wt%;
acetic acid: 0.02 wt%;
polyvinyl alcohol: 0.5wt%
Fluorocarbon surfactant: 0.05 wt%;
diacetone alcohol (leveling agent): 6 wt%;
defoaming agent: 0.05 wt%;
polyurethane thickener: 0.50 wt%;
aqueous blocked isocyanate curing agent (crosslinking agent): 0.1 wt%;
ethylene glycol monobutyl ether (volatility regulator): 5 wt%;
ethylene glycol (humectant): 2 wt%;
2-hexanol (odor masking agent): 0.05 wt%;
water: and (4) the balance.
The modified reinforced conductive polymer aqueous slurry of this example was prepared in the same manner as in example 1, except that it did not include the steps of preparing and adding the graphene dispersion liquid.
The process and application of the modified reinforced conductive polymer aqueous slurry for preparing the electrode are the same as those of the embodiment 1.
Example 3
The embodiment provides a modified reinforced conductive polymer aqueous slurry, which is prepared from the following raw materials in percentage by weight:
PEDOT/PSS conductive polymer aqueous solution: 35 wt%, its solid content is 1.0 wt%;
conductive inorganic material modification reinforcing agent: 4.8 wt% of carbon nanotubes and 3.8 wt% of silver nanowires;
dimethyl sulfoxide: 1.7 wt%;
diethanolamine: 0.01 wt%;
hydroxypropyl methylcellulose ether: 0.8 wt%;
tween 80: 0.08 wt%;
polyethylene glycol 600: 0.5 wt%;
and (3) organic silicon defoaming agent: 0.08 wt%;
isopropyl alcohol (alcohol defoamer): 6.0 wt%;
acrylic thickener: 1.8 wt%;
aqueous blocked isocyanate curing agent (crosslinking agent): 0.8 wt%;
titanate coupling agent (crosslinking agent): 0.2 wt%;
propylene glycol methyl ether (volatility regulator): 8.8 wt%;
ethylene glycol monobutyl ether (volatility regulator): 1.2 wt%;
glycerin (humectant): 0.8 wt%;
2-hexanol (odor masking agent): 0.05 wt%;
water: and (4) the balance.
The modified reinforced conductive polymer aqueous slurry of the embodiment is prepared according to the following method:
preparing materials: preparing raw materials according to a formula ratio; preparing carbon nanotube suspension from carbon nanotubes in formula amount, and preparing silver nanowire suspension from silver nanowires in formula amount; preparing hydroxypropyl methyl cellulose ether with the formula amount into a hydroxypropyl methyl cellulose ether aqueous solution;
dispersing: at the temperature of 15-35 ℃, sequentially adding PEDOT/PSS conductive polymer aqueous solution with solid content of 1.0wt%, dimethyl sulfoxide, diethanolamine and conductive inorganic material modification reinforcing agent into a stainless steel stirring barrel under the stirring state of 200 r/min-1000 r/min, and dispersing for 10 min; then adding hydroxypropyl methyl cellulose ether water solution, Tween 80 surfactant, polyethylene glycol 600, organic silicon defoamer, isopropanol, propylene glycol methyl ether, ethylene glycol monobutyl ether, glycerol and 2-hexanol, and dispersing for 10 min; then sequentially adding the waterborne closed isocyanate curing agent, the titanate coupling agent, the acrylic acid thickening agent and the balance of water, and dispersing for 30 min;
and (3) filtering: filtering with 100-200 mesh filter screen to obtain modified reinforced conductive polymer aqueous slurry.
The process and application of the modified reinforced conductive polymer aqueous slurry for preparing the electrode of the embodiment are as follows:
step 1: manufacturing a screen printing plate: manufacturing a screen printing plate with a graphical pattern by adopting a 500-mesh stainless steel screen;
step 2: printing the prepared modified enhanced conductive polymer aqueous slurry on a double-sided hardened PET (polyethylene terephthalate) film by using an additive screen printing process to prepare a transparent conductive circuit, and baking the transparent conductive circuit on a drying oven at 155 ℃ for 30min to obtain a patterned transparent conductive circuit coating;
and step 3: and (3) applying the transparent conductive circuit prepared in the step (2) to the fields of touch control based on capacitive design, transparent advertising boards, signboards, oversized LED screens, solar cells and the like based on transparent circuit design.
Example 4
The embodiment provides a modified reinforced conductive polymer aqueous slurry, which is prepared from the following raw materials in percentage by weight:
PEDOT/PSS conductive polymer aqueous solution: 83wt%, its solid content is 1.3 wt%;
conductive inorganic material modification reinforcing agent: 2.0wt% of carbon nanotubes, 1.0wt% of graphene and 0.3 wt% of silver nanowires;
dimethyl sulfoxide: 3.5 wt%;
acetic acid: 0.03 wt%;
water-dispersible acrylic emulsion: 1.0 wt%;
silicone-based surfactant: 0.2 wt%;
an acrylate leveling agent: 0.2 wt%;
polyether modified silicone defoamer: 0.12 wt%;
fumed silica (thickener): 1.0 wt%;
aqueous blocked isocyanate curing agent (crosslinking agent): 0.3 wt%;
silane coupling agent (crosslinking agent): 0.3 wt%;
ethylene glycol methyl ether (volatility regulator): 2.0 wt%;
ethylene glycol monobutyl ether (volatility regulator): 0.5 wt%;
ethylene glycol (humectant): 0.5 wt%;
methyl isobutyl carbinol (odor masking agent): 0.03 wt%;
water: and (4) the balance.
The modified reinforced conductive polymer aqueous slurry of the embodiment is prepared according to the following method:
preparing materials: preparing raw materials according to a formula ratio; preparing carbon nano-tubes with formula amount into carbon nano-tube turbid liquid, preparing graphene with formula amount into graphene dispersion liquid, preparing nano-silver wires with formula amount into nano-silver wire turbid liquid, and preparing fumed silica with formula amount into fumed silica paste dispersion liquid;
dispersing: at the temperature of 15-35 ℃, sequentially adding PEDOT/PSS conductive polymer aqueous solution with the solid content of 1.3wt%, dimethyl sulfoxide, acetic acid and a conductive inorganic material modification reinforcing agent into a stainless steel stirring barrel under the stirring state of 200 r/min-1000 r/min, and dispersing for 10 min; then adding a water-dispersible acrylic emulsion, a silicone surfactant, an acrylate flatting agent, a polyether modified organic silicon defoaming agent, ethylene glycol methyl ether, ethylene glycol monobutyl ether, ethylene glycol and methyl isobutyl carbinol, and dispersing for 10 min; then sequentially adding the water-based closed isocyanate curing agent, the silane coupling agent, the fumed silica paste dispersion liquid and the balance of water, and dispersing for 30 min;
and (3) filtering: filtering with 100-200 mesh filter screen to obtain modified reinforced conductive polymer aqueous slurry.
The process and application of the modified reinforced conductive polymer aqueous slurry for preparing the electrode of the embodiment are as follows:
step 1: printing the prepared modified reinforced conductive polymer aqueous slurry on a special-shaped ceramic substrate by using an additive liquid atomization 3D printing process to prepare a transparent conductive electrode, and baking the transparent conductive electrode on a drying oven at 125 ℃ for 40min to obtain a patterned transparent conductive electrode coating;
step 2: the transparent conductive electrode prepared in the step 1 is used in the fields of electroluminescence, electrochromism and the like based on transparent electrode interlayer design.
Example 5
A modified reinforced conductive polymer aqueous slurry is composed of the following raw materials in percentage by weight:
PEDOT/PSS conductive polymer aqueous solution: 39% by weight, its solid content being 1.0% by weight;
conductive inorganic material modification reinforcing agent: 0.75 wt% of graphene and 0.25 wt% of nano silver wire;
dimethyl sulfoxide: 2.0 wt%;
concentrated ammonia water: 0.01wt%, with an ammonia content of 25 wt%;
water-dispersible polyurethane emulsion: 1.5 wt%;
fluorocarbon surfactant: 0.1 wt%;
polyethylene glycol 400: 0.2 wt%;
acetylene glycol type defoaming agent: 0.2 wt%;
polyurethane thickener: 0.8 wt%;
aqueous blocked isocyanate curing agent (crosslinking agent): 0.5 wt%;
organic zirconium crosslinking agent: 0.08 wt%;
isopropyl alcohol (volatility regulator): 9.0 wt%;
sec-butanol (volatility regulator): 3.0 wt%;
ethylene glycol (humectant): 0.2 wt%;
2-hexanol (odor masking agent): 0.02 wt%;
water: and (4) the balance.
The modified reinforced conductive polymer aqueous slurry of the embodiment is prepared according to the following method:
preparing materials: preparing raw materials according to a formula ratio; preparing graphene into a graphene paste dispersion liquid according to the formula amount, and preparing a nano silver wire suspension liquid according to the formula amount;
dispersing: at the temperature of 15-35 ℃, sequentially adding a PEDOT/PSS conductive polymer aqueous solution with the solid content of 1.0wt%, dimethyl sulfoxide, 25% concentrated ammonia water and a conductive inorganic material modification reinforcing agent into a stainless steel stirring barrel under the stirring state of 1000r/min at 200r/min, and dispersing for 10 min; then adding water-dispersible polyurethane emulsion, fluorocarbon surfactant, polyethylene glycol 400, acetylene glycol type defoaming agent, isopropanol, sec-butyl alcohol, ethylene glycol and 2-hexanol, and dispersing for 10 min; then sequentially adding the waterborne closed isocyanate curing agent, the organic zirconium crosslinking agent, the polyurethane thickening agent and the balance of water, and dispersing for 30 min;
and (3) filtering: filtering with 100-200 mesh filter screen to obtain modified reinforced conductive polymer aqueous slurry.
The process and application of the modified reinforced conductive polymer aqueous slurry for preparing the electrode of the embodiment are as follows:
step 1: printing the prepared modified reinforced conductive polymer aqueous slurry on a PET (polyethylene terephthalate) film by using an additive gravure printing process to prepare a transparent conductive electrode, and baking the transparent conductive electrode in a drying oven at 145 ℃ for 1min to obtain a patterned transparent conductive electrode coating;
step 2: and (3) applying the transparent conductive electrode prepared in the step (1) to the touch control field based on capacitive design.
The electrode patterns obtained in examples 1 to 5 were tested for light transmittance using a photoelectric haze meter, for sheet resistance of the conductive coating using a four-probe tester, for thickness of the transparent conductive layer using a laser microscope using a dicing method, for adhesion using a 3M610 tape, and for hardness using a pencil hardness tester. The results of the performance tests are shown in table 1 below.
Table 1 results of performance testing
Figure BDA0002134037500000131
As can be seen from table 1, the transparent conductive layers prepared from the modified reinforced conductive polymer aqueous slurries of examples 1 to 5 have high light transmittance, low impedance, excellent adhesion and high hardness. In examples 1 to 5, the content of the PEDOT/PSS conductive polymer aqueous solution was high, and the conductive layer had good uniformity of conductivity. Meanwhile, as can be seen from the comparison of the formula and the performance in the embodiment 1 and the embodiment 2, the conductive performance of the conductive coating in the embodiment 1 and the embodiment 2 is basically consistent, and the graphene is not added as a conductive inorganic material reinforcing agent in the embodiment 2, so that the hardness is relatively low, and the conductive coating is easily scratched due to friction in the turnover process of spraying operation and the coating packaging process, which indicates that when the conductive inorganic material is used for reinforcing the modified conductive polymer, the modification reinforcing effect of the graphene and the nano silver wire in the combined addition use is superior to the modification reinforcing effect of the single nano silver wire in the improvement of the balance of the performance such as the conductivity and the friction resistance.
Finally, it should be emphasized that the above-described embodiments are merely preferred examples of the invention, which is not intended to limit the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. The conductive polymer aqueous slurry is characterized by comprising the following raw materials in percentage by weight:
PEDOT/PSS conductive polymer aqueous solution: 50 to 83 wt%;
conductive inorganic material modification reinforcing agent: 1.5 to 2.0 wt%;
conductive polymer activator: 2.52 to 3.53 wt%;
connecting materials: 0.5wt% to 1 wt%;
surface tension adjusting agent: 0.05wt% to 0.2 wt%;
leveling agent: 0.2 to 6 wt%;
defoaming agent: 0.05wt% to 0.2 wt%;
thickening agent: 0.5wt% to 1.0 wt%;
a crosslinking agent: 0.1 to 0.6 wt%;
volatile regulators: 2.5 to 5 wt%;
humectant: 0.5wt% to 2 wt%;
other functional additives: 0.01wt% to 1.0 wt%;
water: the balance;
the solid content of the PEDOT/PSS conductive polymer aqueous solution is 1.2wt% to 1.3wt%, the conductivity is 150S/cm to 1100S/cm, and the solvent is deionized water;
the conductive inorganic material modification reinforcing agent is a mixture of a nano silver wire and graphene or a mixture of a nano silver wire, graphene and a carbon nanotube;
the carbon nanotube has an average diameter of 10-30 nm, an average length of 10-30 μm, and a specific surface area of 50m2G to 150m2/g；
The specific surface area of the graphene is 150m2G to 350m2(ii)/g, D50 is from 5 μm to 10 μm, the mean longitudinal dimension is 1nm and 3nm, and the mean transverse dimension is less than or equal to 5 μm;
the diameter of the nano silver wire is 8nm to 40nm, the average length is 8 mu m to 40 mu m, the length-diameter ratio is 500 to 1200, the nano silver wire is subjected to surface passivation treatment by inert metal, and the inert metal is at least one of gold, platinum and palladium;
the conductive polymer activating agent is dimethyl sulfoxide and a pH value regulator, and the weight percentage of the dimethyl sulfoxide in the conductive polymer aqueous slurry is 2.5wt% to 3.5 wt%.
2. The aqueous slurry of an electroconductive polymer according to claim 1, wherein:
the conductive polymer activating agent is dimethyl sulfoxide and a pH value regulator;
the pH value regulator is at least one of water-soluble organic acid, water-soluble organic amine and ammonia water;
the water-soluble organic acid is at least one of acetic acid and lactic acid;
the water-soluble organic amine is at least one of monoethanolamine, diethanolamine, triethanolamine and N, N-dimethylethanolamine.
3. The aqueous slurry of conductive polymer according to claim 1 or 2, wherein:
the connecting material is at least one of water-soluble cellulose ether, polyvinyl alcohol, polyethylene glycol, water-dispersible acrylic emulsion and water-dispersible polyurethane emulsion, and the water-soluble cellulose ether is at least one of hydroxypropyl cellulose and hydroxypropyl methyl cellulose;
the surface tension regulator is at least one of alkyl alcohol ether carboxylate, fluorocarbon surfactant, silicone surfactant, alkynol surfactant, alkyl glucoside, fatty glyceride, span and Tween;
the flatting agent is at least one of an acrylate flatting agent, a fluorine-modified acrylate flatting agent, a silane wetting flatting agent, a fluorocarbon flatting agent, a higher alcohol and a dihydric alcohol polycondensate;
the defoaming agent is at least one of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, organic silicon, polyether modified organic silicon and alcohol;
the thickening agent is at least one of polyurethane thickening agent, acrylic thickening agent, polyoxyethylene ether, cellulose ether and fumed silica;
the cross-linking agent is more than one of a water-based blocked isocyanate curing agent, an aziridine cross-linking agent, an aziridine modified isocyanate cross-linking agent, a silane coupling agent, an organic titanium cross-linking agent and an organic zirconium cross-linking agent;
the volatility regulator is at least one of alcohol and alcohol ether, the alcohol is at least one of ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, tert-butanol, n-pentanol, isopentanol, sec-pentanol, n-hexanol, isohexanol, sec-hexanol, tert-hexanol, n-octanol, isooctanol, sec-octanol and diacetone alcohol, and the alcohol ether is at least one of ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, propylene glycol methyl ether and propylene glycol ethyl ether;
the humectant is at least one of dihydric alcohol and derivatives thereof, and trihydric alcohol and derivatives thereof;
the other functional additive is at least one of an odor covering agent, a dispersing agent and a film forming auxiliary agent;
the balance of the water is deionized water, ultrapure water, distilled water and filtered tap water.
4. A method for producing the aqueous slurry of conductive polymer according to any one of claims 1 to 3, characterized by comprising a mixing step of:
a first mixing step: sequentially adding the PEDOT/PSS conductive polymer aqueous solution, the conductive polymer activator and the conductive inorganic material modification reinforcing agent into a container for dispersion;
a second mixing step: adding the connecting material, the surface tension regulator, the leveling agent, the defoaming agent, the volatile regulator, the humectant and the other functional additives, and dispersing;
a third mixing step: adding the cross-linking agent, the thickening agent and the balance of water, and dispersing.
5. The method of claim 4, wherein:
the temperature of the first mixing step, the second mixing step and the third mixing step is 15 ℃ to 35 ℃, and the stirring speed is 200r/min to 1000 r/min; the stirring time of the first mixing step is 5min to 15min, the stirring time of the second mixing step is 5min to 15min, and the stirring time of the third mixing step is 20min to 40 min;
before the mixing step, the method also comprises a dispersion step: preparing PEDOT/PSS conductive polymer aqueous solution gel particles, the conductive inorganic material modification reinforcing agent and the connecting material into dispersion liquid or suspension liquid;
a filtration step is also included after the mixing step: filtering with 100-200 mesh filter screen.
6. The application of the conductive polymer aqueous slurry in preparing the conductive layer is characterized in that:
preparing the conductive polymer aqueous paste according to any one of claims 1 to 3 or the conductive polymer aqueous paste obtained by the preparation method according to claim 4 or 5 into a conductive layer by at least one of a liquid atomization 3D printing process, a screen printing process, a roll-to-roll gravure printing process, a flexographic printing process, and a mask spraying process.
7. Use according to claim 6, characterized in that:
the conductive layer is prepared on a substrate, the substrate is the surface of an organic material, an inorganic material or a functional coating, and the organic material is a film or a plate made of at least one of polyurethane, polyester, polycarbonate, polyimide, polyvinyl chloride and acrylic resin; the inorganic material is ceramic, glass or crystalline silicon material;
the drying temperature of the conductive polymer water-based slurry is 100-160 ℃, and the drying time is 1-60 min.
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