CN110317525A - A kind of conducting polymer aqueous slurry and its preparation method and application - Google Patents
A kind of conducting polymer aqueous slurry and its preparation method and application Download PDFInfo
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- CN110317525A CN110317525A CN201910647612.2A CN201910647612A CN110317525A CN 110317525 A CN110317525 A CN 110317525A CN 201910647612 A CN201910647612 A CN 201910647612A CN 110317525 A CN110317525 A CN 110317525A
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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
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- 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
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- 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
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- 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 present invention relates to a kind of conducting polymer aqueous slurries and its preparation method and application, and conducting polymer aqueous slurry comprises the following raw materials by weight percent: PEDOT/PSS conducting polymer aqueous solution: 16wt% to 89wt%；Conducting inorganic material modification strengthening agent: 0.2wt% to 5.0wt%；Conducting polymer activator: 0.05wt% to 4.5wt%；Binder: 0.2wt% to 3.0wt%；Surface tension modifier: 0.01wt% to 0.5wt%；Levelling agent: 0.01wt% to 15wt%；Defoaming agent: 0.01wt% to 20wt%；Thickener: 0.2wt% to 2.0wt%；Crosslinking agent: 0.01wt% to 2.0wt%；Volatility modifier: 0wt% to 20wt%；Moisturizer: 0wt% to 5.0wt%；Other functional additives: 0.01wt% to 1.0wt%；Water: surplus.While conductive layer prepared by conducting polymer aqueous slurry of the invention has excellent electric conductivity and crocking resistance, also there is good light transmission.
Description
Technical field
The present invention relates to conductive polymer material fields, and in particular to a kind of conducting polymer aqueous slurry and its preparation side
Method and technique for applying and case.
Background technique
Circuit electrode especially transparent conductive circuit and transparent electrode field in the application of existing large-scale commercial applications, oxidation
Yellow light wet etching used by indium tin (ITO), metal grill and nano-silver thread coated film, laser etch process, exist
Many and diverse process, waste of material, the problem of environmental pollution is serious manufacture enterprise and bring many puzzlements.And conducting polymer
Although electric conductivity is always its weakness by the development of many years, it is difficult to be used for high-end electronic component.For example, application number
A kind of method for manufacturing macromolecule transparent conductive film is disclosed for 201410215856.0 Chinese invention patent application, includes:
Conducting polymer aqueous solution is provided, wherein conducting polymer aqueous solution includes PEDOT:PSS；Conductive auxiliary agent is added to conductive polymer
Dispersion liquid is made in sub- aqueous solution；Dispersion liquid is configured to the surface of substrate, dispersion liquid film is made；And by dispersion liquid
Film is dried at a temperature of 140 DEG C or more, macromolecule transparent conductive film is made.But its transparent conducting coating obtained
Sheet resistance in 100 to 300 Ω/, light transmittance is 80 to 90%, due to needing to keep high transparency, the electric conductivity of conductive coating
It is bad.The component of existing macromolecule electrically conducting transparent route or transparent conductive electrode design, generally existing fever, high current are logical
Cross limitation, pressure drop cause photoelectric functional decline defect, and the hardness of conductive layer surface and crocking resistance etc. have it is to be strengthened.
Summary of the invention
In view of the deficiencies of the prior art, the first object of the present invention is to provide a kind of electric conductivity and crocking resistance is good
Conducting polymer aqueous slurry.The second object of the present invention is to provide the preparation method of the conducting polymer aqueous slurry.This hair
Bright third purpose is to provide the conducting polymer aqueous slurry and is preparing the application on conductive layer.
The first purpose to realize the present invention, the present invention provides a kind of conducting polymer aqueous slurries, by following weight
The raw material of percentage forms:
PEDOT/PSS conducting polymer aqueous solution: 16wt% to 89wt%；
Conducting inorganic material modification strengthening agent: 0.2wt% to 5.0wt%；
Conducting polymer activator: 0.05wt% to 4.5wt%；
Binder: 0.2wt% to 3.0wt%；
Surface tension modifier: 0.01wt% to 0.5wt%；
Levelling agent: 0.01wt% to 15wt%；
Defoaming agent: 0.01wt% to 20wt%；
Thickener: 0.2wt% to 2.0wt%；
Crosslinking agent: 0.01wt% to 2.0wt%；
Volatility modifier: 0wt% to 20wt%；
Moisturizer: 0wt% to 5.0wt%；
Other functional additives: 0.01wt% to 1.0wt%；
Water: surplus.
Therefore conducting polymer aqueous slurry of the invention is modified using conducting inorganic material modification strengthening agent
Enhancing.Wherein, PEDOT/PSS conducting polymer aqueous solution refers to poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulphur
Acid) aqueous solution, PEDOT/PSS conducting polymer aqueous solution weight percent in conducting polymer aqueous slurry is higher, leads
Electric polymer waterborne slurry has good filming performance, and conductive layer has good tensile property after film forming, and after film forming
PEDOT/PSS forms homogeneous conducting base, can effectively keep the conductivity uniformity of conductive layer.Conducting inorganic material is modified to be increased
The mechanical strength of strong agent itself can assign the good crocking resistance of conductive layer and improve surface hardness, and conduction after the drying
The reticular structure of nonuniformity is formed in layer, the mobile fast speed of electronics, Conductive inorganic in conducting inorganic material modification strengthening agent
Material modification reinforcing agent is used in compounding with PEDOT/PSS conducting polymer aqueous solution, and the two synergistic effect can be effectively improved and be led
Electrical property.Moreover, the present invention is combined by the screening of auxiliary agent, solves conducting polymer aqueous slurry and scheme in addition process processing procedure
Shape chemical industry skill adaptive problem, the present invention in conducting polymer aqueous slurry can by circuit electrode design addition process processing procedure can
With directly graphical, for making transparent conductive electrode and electrically conducting transparent route, formed saturating with a thickness of 0.1 μm to 0.5 μm
Bright conductive film layer has high transparency and super-low impedance, while the characteristics of be also equipped with high weatherability.In addition, slurry of the invention
Be it is aqueous, it is environmentally friendly, and processing performance is good.
Further technical solution is, the weight percent of PEDOT/PSS conducting polymer aqueous solution be 35wt% extremely
89wt%；The water-soluble fluid solid content of PEDOT/PSS conducting polymer be 0.5wt% to 2.0wt%, conductivity be 150S/cm extremely
1100S/cm, solvent are deionized water.
Therefore weight percent, the solid content of the further preferred PEDOT/PSS conducting polymer aqueous solution of the present invention
And conductivity, these parameters help to further increase electric conductivity, filming performance and tensile property in above range.
PEDOT/PSS conducting polymer aqueous solution can itself be aqueous solution, and solid content is 0.9wt% to 1.5wt%, can also be by
The PEDOT/PSS of gel state is dissolved in water and is made.
Further technical solution is that conducting inorganic material modification strengthening agent is carbon nanotubes, in graphene, nano-silver thread
At least one；The average caliber of carbon nanotubes is 10nm to 30nm, and average length is 10 μm to 30 μm, and specific surface area is
50m2/ g to 150m2/g；The specific surface area of graphene is 150m2/ g to 350m2/ g, D50 are 5 μm to 10 μm, average longitudinal dimension
It is 3nm for 1nm, average transverse is less than or equal to 5 μm；The diameter of nano-silver thread is 8nm to 40nm, and average length is 8 μm
To 40 μm, draw ratio is 500 to 1200.
Therefore conducting inorganic material modification strengthening agent of the invention is carbon nanotubes, in graphene, nano-silver thread
One or more combinations, these fillers are capable of providing conductive mesh structure after film forming, and act synergistically with PEDOT/PSS, assign
The excellent electric conductivity of conductive layer is given, when so that the sheet resistance minimum of transparent conducting coating dropping to 2 Ω/ to 5 Ω/ after printing,
The light transmittance of conductive layer remains to reach 80% or more, this avoids fever, high current, pressure when being designed to electrically conducting transparent route
Bring application problem is dropped, process turnover and rear end above and below in manufacturing process is also met and encapsulates to coating hardness, rub resistance
The requirement of energy.Wherein, nano-silver thread can be dispersed in water, and be configured to the suspension that mass fraction is 0.5% to 10.0% again
It is added, nano-silver thread has strong electric action, and prepared conductive layer has good light permeability；Carbon nanotubes is black powder
Carbon nanotubes can also be dispersed in water and be configured to suspension and be added again by last, general directly addition use, carbon nanotubes
With high electrical conductivity, while it can be improved conductive layer intensity and wearability；Graphene is the fluffy slim and graceful powder of black, can be with
Directly addition uses, and graphene dispersion can also be configured to paste dispersion liquid in water and be added again, graphene can mention
The performances such as the good thermally conductive, anti-corrosion of conductive layer, wear-resisting, toughness are assigned while the electric conductivity of high slurry.
Further technical solution is that conducting inorganic material modification strengthening agent is carbon nanotubes, in graphene, nano-silver thread
At least two.
Therefore conducting inorganic material modification strengthening agent of the invention is preferably at least two combinations of the above, to reach
To the balance for improving the performances such as electric conductivity and rub resistance.When containing graphene in combination, the laminated structure of graphene can be
Play the role of reinforcement in junction between carbon nanotubes or nano-silver thread and PEDOT/PSS.
Further technical solution is, nano-silver thread passes through inert metal surface Passivation Treatment, inert metal be gold, platinum,
At least one of palladium.
Therefore inert metal cladding can be used in nano-silver thread of the invention, passes through core-shell structure Passivation Treatment work
Skill improves the patience such as anti-oxidant and sulfuration resistant of the nano-silver thread in manufacturing process.
Further technical solution is that conducting polymer activator is dimethyl sulfoxide and pH adjusting agent；PH value is adjusted
Agent is at least one of water-soluble organic acid, water-soluble organic amine and ammonium hydroxide；Water-soluble organic acid be acetic acid, in lactic acid extremely
Few one kind；Water-soluble organic amine is monoethanolamine, diethanol amine, triethanolamine, N, at least one in N- dimethylethanolamine
Kind.
Therefore the present invention can using dimethyl sulfoxide and pH adjusting agent as conducting polymer activator, two
Methyl sulfoxide and conducting polymer can form conjugated system, reduce the constraint of the movement of electronics, to improve conductive height
The electric conductivity of molecule；Electric conductivity of the conducting polymer in faintly acid system is better than alkaline system, and pH adjusting agent can be adjusted
The acid-base property of slurry is saved to make slurry keep faintly acid.
Further technical solution is that binder is water-soluble cellulose ether, polyvinyl alcohol, polyethylene glycol, water dispersible
At least one of acrylic emulsion, water-dispersible polyurethane lotion, water-soluble cellulose ether are hydroxypropyl cellulose, hydroxypropyl
At least one of methylcellulose.
Therefore the present invention can be using above-mentioned high molecular material as bridging agent, these high molecular materials assign slurry
Expect good filming performance and mechanical performance.
Further technical solution is that surface tension modifier is alkyl alcohol ether carboxylate, fluorocarbon surfactant, silicone
At least one of class surfactant, alkynes alcohol surfactants, alkyl glucoside, fatty glyceride, sapn, tween.
Therefore the present invention can be using above-mentioned surfactant as tension regulator, it being capable of effective regulation system
Surface tension.
Further technical solution is, levelling agent be acrylic compounds levelling agent, esters of acrylic acid levelling agent, fluorine richness third
Olefin(e) acid esters levelling agent, silanes moistening flatting agent, fluorocarbons class levelling agent, higher alcohols, in dihydric alcohol condensation polymer
It is at least one.
Therefore the present invention can improve slurry to the wetting flow leveling of substrate using above-mentioned levelling agent, prevent from contracting
The film forming disadvantage such as hole, pinprick, orange peel.Wherein, higher alcohols can be diacetone alcohol and containing more than five carbon primary alconol and secondary
Alcohol, dihydric alcohol condensation polymer can be polyethylene glycol and its derivative etc..
Further technical solution is, defoaming agent be nonylphenol polyoxyethylene ether, octyl phenol polyoxyethylene ether, organosilicon,
At least one of the oxo solvent such as organic silicon modified by polyether, alcohols, acetylenic glycols type defoaming agent.
Therefore the present invention can eliminate the bubble in slurry using above-mentioned defoaming agent, restrain the generation of bubble.
Further technical solution is, thickener be polyurethanes thickener, acrylic thickener, polyoxyethylene ether,
At least one of cellulose ether, fumed silica.
Therefore the present invention can assign slurry thixotropic property using above-mentioned thickener and adjust the viscosity of slurry,
To strengthening slurry storage stability, the printing technology adaptability of slurry is improved, the spacing accuracy for printing slurry is minimum reachable
To 0.06mm.
Further technical solution is that crosslinking agent is watersoluble closed type isocyanate curing agent, aziridine crosslinker, nitrogen third
One or more of pyridine modified isocyanate crosslinking agent, silane coupling agent, organic titanium cross-linking agent, organic zirconium crosslinker.
Therefore the present invention can be improved using above-mentioned crosslinking agent organic material and inorganic material, organic material with
Crosslink density between organic material, slurry and substrate improves conductive layer to the attachment fastness of substrate and the machinery of conductive layer
Intensity and chemical resistance.
Further technical solution is that volatility modifier is at least one of alcohols, alcohol ether, and alcohol is ethyl alcohol, positive third
Alcohol, isopropanol, n-butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, n-amyl alcohol, isoamyl alcohol, sec-amyl alcohol, n-hexyl alcohol, isohexyl alcohol, it is secondary oneself
At least one of alcohol, tertiary hexanol, n-octyl alcohol, isooctanol, sec-octyl alcohol, diacetone alcohol, alcohol ether are ethylene glycol monomethyl ether, ethylene glycol ethyl ethers
At least one of ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether.
Therefore the present invention can adjust the evaporation rate of slurry using above-mentioned volatility modifier, to match not
Same operation technique, to obtain the film layer of high quality.
Further technical solution is, moisturizer be in dihydric alcohol and its derivative, trihydroxylic alcohol and its derivative at least
It is a kind of.
Therefore the present invention can improve the moisture retention of slurry using above-mentioned moisturizer, prevent in operation process because
Water volatilization is too fast to bring undesirable influence.Moisturizer can be one of ethylene glycol, propylene glycol, glycerine, butanediol or more
Kind combination.
Further technical solution is, other functional additives be odor-masking agent, dispersing agent, in coalescing agent extremely
Few one kind.
Therefore the present invention can also add odor-masking agent, dispersing agent, coalescing agent etc., for further improving
Or improve smell, dispersibility and the filming performance etc. of slurry.
Further technical solution is that water is deionized water, ultrapure water, distilled water, filtered tap water.
Therefore water of the invention can use the higher water of purity, reduce influence of the impurity to conductive layer performance.
The second purpose to realize the present invention, the present invention provides a kind of preparation sides of above-mentioned conducting polymer aqueous slurry
Method, including mixing step:
First mixing step: by the PEDOT/PSS conducting polymer aqueous solution, the conducting polymer activator, institute
It states conducting inorganic material modification strengthening agent to sequentially add in container, disperse；
Second mixing step: be added the binder, the surface tension modifier, the levelling agent, the defoaming agent,
The volatility modifier, the moisturizer and other functional additives, dispersion；
Third mixing step: being added the water of the crosslinking agent, the thickener and surplus, dispersion.
Therefore slurry of the invention mainly passes through three mixing steps and is made, it, can will be each by three mixing steps
Raw material are sufficiently mixed uniformly, and simple process, and high production efficiency is at low cost.
Further technical solution is that the temperature of the first mixing step, the second mixing step and third mixing step is 15
DEG C to 35 DEG C, mixing speed 200r/min to 1000r/min；The mixing time of first mixing step be 5min to 15min, second
The mixing time of mixing step is 5min to 15min, and the mixing time of third mixing step is 20min to 40min.
Therefore the present invention has advanced optimized the process conditions of each mixing step, helps to obtain favorable dispersibility
Waterborne conductive slurry.
Further technical solution be further include dispersion steps before mixing step: by PEDOT/PSS conducting polymer
Aqueous gel grain, conducting inorganic material modification strengthening agent and binder are configured to dispersion liquid or suspension.
Therefore the present invention is before mixing, it can be first by PEDOT/PSS conducting polymer aqueous gel grain, conduction
Inorganic material-modified reinforcing agent and binder are configured to dispersion liquid or suspension, are uniformly dispersed convenient for subsequent mixing.If using
Fumed silica can also be configured to the dispersion of fumed silica paste before mixing as thickener by fumed silica
Liquid.
Further technical solution be after the mixing step further include filtration step: the filter using 100 mesh to 200 mesh
Net is filtered.
Therefore the present invention can also be filtered slurry, remove bulky grain insoluble matter, improve slurry and made
The uniformity of the conductive layer obtained.
Third purpose to realize the present invention, the present invention provides a kind of above-mentioned conducting polymer aqueous slurries to lead in preparation
Application in electric layer, conducting polymer aqueous slurry is recessed by liquid atomization 3D printing technique, silk-screen printing technique, reel-to-reel
At least one of version printing technique, flexography process, exposure mask spraying process prepare conductive layer.
Therefore the conducting polymer aqueous slurry in the present invention takes the processing procedure of direct patterning process, is suitble to more
The patterning process of kind mainstream can be atomized 3D printing technique, silk-screen printing technique, reel-to-reel intaglio process dataller using liquid
The addition processes processing procedures such as skill, flexography process, exposure mask spraying process are used to prepare transparent conductive circuit and transparent conductive electrode, keep away
Exempt from many and diverse process of subtractive process processing procedure bring, waste of material, the problem of environmental pollution is serious, the also band in conductive layer manufacturing process
Revolutionary promotion is carried out.Obtained conductive layer can be widely used for the touch-control field designed based on condenser type, be led based on transparent
The fields such as anti-electromagnetic radiation, the electromagnetic shielding of electrocoat design, electroluminescent, electrochromism based on transparent electrode sandwich design
Field, based on the fields such as advertisement transparent board, direction board, extra-large LED screen field and solar battery of transparent circuitry design,
Photoelectric component can be made lightening, meet the trend of electronic component development, meet the target of market application demand.
Further technical solution is that conductive layer is prepared on substrate, and substrate is that organic material, inorganic material or function apply
The surface of layer, organic material be polyurethane, polyester, polycarbonate, polyimides, polyvinyl chloride, in acrylic resin at least
Film made of a kind of or plate；Inorganic material is ceramics, glass or crystalline silicon material.
Therefore the substrate of conductive layer of the present invention can according to need and select different substrates, conductive layer is to substrate
Adhesion-tight, substrate can be membrane material or special-shaped substrate, and conducting polymer aqueous slurry of the invention can be on different substrate materials
Film forming.
Further technical solution is that the drying temperature of conducting polymer aqueous slurry is 100 DEG C to 160 DEG C, when dry
Between be 1min to 60min.
Therefore conducting polymer aqueous slurry of the invention can heat up when preparing conductive layer drying, process conditions
Simply, aqueous solvent can be effectively removed.
Specific embodiment
The present invention is described further combined with specific embodiments below.
Embodiment 1
The conducting polymer aqueous slurry for present embodiments providing a kind of modified enhancing, below by weight percentage
Raw material composition:
PEDOT/PSS conducting polymer aqueous solution: 50wt%, solid content 1.2wt%；
Conducting inorganic material modification strengthening agent: 1.5wt%, by the graphene of 1.0wt% and the nano-silver thread group of 0.5wt%
At；
Dimethyl sulfoxide: 2.5wt%；
Acetic acid: 0.02wt%；
Polyvinyl alcohol: 0.5wt%；
Fluorocarbon surfactant: 0.05wt%；
Diacetone alcohol (levelling agent): 6wt%；
Defoaming agent: 0.05wt%；
Polyurethane thickener: 0.50wt%；
Watersoluble closed type isocyanate curing agent (crosslinking agent): 0.1wt%；
Ethylene glycol monobutyl ether (volatility modifier): 5wt%；
Ethylene glycol (moisturizer): 2wt%；
2- hexanol (odor-masking agent): 0.05wt%；
Water: surplus.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment is prepared in accordance with the following methods:
Stock: each raw material is got out according to formulation ratio；The graphene of formula ratio is configured to graphene dispersing solution, will be matched
The nano-silver thread just measured is configured to nano-silver thread suspension, and the polyvinyl alcohol of formula ratio is configured to polyvinyl alcohol water solution；
Dispersion: first that solid content is water-soluble for the PEDOT/PSS conducting polymer of 1.2wt% under 15 DEG C to 35 DEG C environment
Liquid, dimethyl sulfoxide, acetic acid, conducting inorganic material modification strengthening agent at 200r/min to 1000r/min stirring successively
It is added in steeliness blender, disperses 10min；Then polyvinyl alcohol water solution, fluorocarbon surfactant, diacetone are added again
Alcohol, defoaming agent, ethylene glycol monobutyl ether, ethylene glycol and 2- hexanol disperse 10min；Sequentially add watersoluble closed type isocyanates
The water of curing agent, polyurethane thickener and surplus disperses 30min；
Filtering: being the conducting polymer aqueous slurry that can be made into modified enhancing with the strainer filtering of 100 mesh to 200 mesh.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment prepares the technique of electrode and using as follows:
Step 1: the conducting polymer aqueous slurry addition process exposure mask spraying process of the modified enhancing of above-mentioned preparation is existed
Patterned transparent conductive pattern is prepared in clear polycarbonate (PC) membrane material, 30min is toasted in 100 DEG C of drying boxes, can make
Obtain patterned conductive coating；
Step 2: with spraying process in one layer of electrochromic material of the above-mentioned conductive coating external coating based on PC film,
Form one layer of Electro-Discolor Coating；
Step 3: being applied with the conducting polymer aqueous slurry of the modified enhancing of above-mentioned preparation in the electrochromism that step 2 is formed
Layer surface prepares layer of transparent conductive electrode coating with spraying process, is then packaged；
Step 4: step 1 being connect and driven with power supply with the conductive coating that step 3 is formed, can be formed and step 1 phase
With the electric to color change interval of graphical pattern.
Embodiment 2
The conducting polymer aqueous slurry for present embodiments providing a kind of modified enhancing, below by weight percentage
Raw material composition:
PEDOT/PSS conducting polymer aqueous solution: 50wt%, solid content 1.2wt%；
Conducting inorganic material modification strengthening agent nano-silver thread: 0.5wt%；
Dimethyl sulfoxide: 2.5wt%；
Acetic acid: 0.02wt%；
Polyvinyl alcohol: 0.5wt%
Fluorocarbon surfactant: 0.05wt%；
Diacetone alcohol (levelling agent): 6wt%；
Defoaming agent: 0.05wt%；
Polyurethane thickener: 0.50wt%；
Watersoluble closed type isocyanate curing agent (crosslinking agent): 0.1wt%；
Ethylene glycol monobutyl ether (volatility modifier): 5wt%；
Ethylene glycol (moisturizer): 2wt%；
2- hexanol (odor-masking agent): 0.05wt%；
Water: surplus.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment, in addition to do not include graphene dispersing solution preparation and
Step is added, remaining preparation method is same as Example 1.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment prepares 1 phase of technique and applicating adn implementing example of electrode
Together.
Embodiment 3
The conducting polymer aqueous slurry for present embodiments providing a kind of modified enhancing, below by weight percentage
Raw material composition:
PEDOT/PSS conducting polymer aqueous solution: 35wt%, solid content 1.0wt%；
Conducting inorganic material modification strengthening agent: 4.8wt%, by 1.0wt% carbon nanotubes and 3.8wt% nano-silver thread group
At；
Dimethyl sulfoxide: 1.7wt%；
Diethanol amine: 0.01wt%；
Hydroxypropyl methyl cellulose ether: 0.8wt%；
Tween 80: 0.08wt%；
Macrogol 600: 0.5wt%；
Organic silicon defoamer: 0.08wt%；
Isopropanol (alcohol defoaming agent): 6.0wt%；
Acrylic thickener: 1.8wt%；
Watersoluble closed type isocyanate curing agent (crosslinking agent): 0.8wt%；
Titanate coupling agent (crosslinking agent): 0.2wt%；
Propylene glycol monomethyl ether (volatility modifier): 8.8wt%；
Ethylene glycol monobutyl ether (volatility modifier): 1.2wt%；
Glycerine (moisturizer): 0.8wt%；
2- hexanol (odor-masking agent): 0.05wt%；
Water: surplus.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment is prepared in accordance with the following methods:
Stock: each raw material is got out according to formulation ratio；Carbon nanotubes suspension is made in the carbon nanotubes of formula ratio, it will
The nano-silver thread of formula ratio is configured to nano-silver thread suspension；The hydroxypropyl methyl cellulose ether of formula ratio is configured to hydroxypropyl
Methyl cellulose ether aqueous solution；
Dispersion: first that solid content is water-soluble for the PEDOT/PSS conducting polymer of 1.0wt% under 15 DEG C to 35 DEG C environment
Liquid, dimethyl sulfoxide, diethanol amine, conducting inorganic material modification strengthening agent are at 200r/min to 1000r/min stirring
It sequentially adds in steeliness blender, disperses 10min；Then hydroxypropyl methyl cellulose ether aqueous solution, Tween 80 table are added again
Face activating agent, Macrogol 600, organic silicon defoamer, isopropanol, propylene glycol monomethyl ether, ethylene glycol monobutyl ether, glycerine and 2-
Hexanol disperses 10min；Sequentially add watersoluble closed type isocyanate curing agent, titanate coupling agent, acrylic thickener and
The water of surplus disperses 30min；
Filtering: being the conducting polymer aqueous slurry that can be made into modified enhancing with the strainer filtering of 100 mesh to 200 mesh.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment prepares the technique of electrode and using as follows:
Step 1: halftone production: there is the halftone of graphical pattern using the production of 500 mesh stainless steel grenadines；
Step 2: the conducting polymer aqueous slurry addition process silk-screen printing technique of the modified enhancing of above-mentioned preparation is existed
Printing prepares electrically conducting transparent route on two-sided hardening PET film material, toasts 30min in 155 DEG C of drying boxes, can be prepared by graphical
Electrically conducting transparent route coating；
Step 3: electrically conducting transparent route made from step 2 being used for the touch-control field based on condenser type design and is based on saturating
Advertisement transparent board, direction board, the extra-large LED screen of bright circuit design, the fields such as solar battery.
Embodiment 4
The conducting polymer aqueous slurry for present embodiments providing a kind of modified enhancing, below by weight percentage
Raw material composition:
PEDOT/PSS conducting polymer aqueous solution: 83wt%, solid content 1.3wt%；
Conducting inorganic material modification strengthening agent: 2.0wt%, by 0.7wt% carbon nanotubes, 1.0wt% graphene and
0.3wt% nano-silver thread composition；
Dimethyl sulfoxide: 3.5wt%；
Acetic acid: 0.03wt%；
Water-dispersible acrylic's lotion: 1.0wt%；
Silicone surfactant: 0.2wt%；
Esters of acrylic acid levelling agent: 0.2wt%；
Polyether Modified Polysiloxanes Defoaming Agent: 0.12wt%；
Fumed silica (thickener): 1.0wt%；
Watersoluble closed type isocyanate curing agent (crosslinking agent): 0.3wt%；
Silane coupling agent (crosslinking agent): 0.3wt%；
Ethylene glycol monomethyl ether (volatility modifier): 2.0wt%；
Ethylene glycol monobutyl ether (volatility modifier): 0.5wt%；
Ethylene glycol (moisturizer): 0.5wt%；
Methyl isobutyl carbinol (odor-masking agent): 0.03wt%；
Water: surplus.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment is prepared in accordance with the following methods:
Stock: each raw material is got out according to formulation ratio；Carbon nanotubes suspension is made in the carbon nanotubes of formula ratio, it will
The graphene of formula ratio is configured to graphene dispersing solution, and the nano-silver thread of formula ratio is configured to nano-silver thread suspension, will be matched
The fumed silica just measured is configured to fumed silica paste dispersion liquid；
Dispersion: first that solid content is water-soluble for the PEDOT/PSS conducting polymer of 1.3wt% under 15 DEG C to 35 DEG C environment
Liquid, dimethyl sulfoxide, acetic acid, conducting inorganic material modification strengthening agent at 200r/min to 1000r/min stirring successively
It is added in steeliness blender, disperses 10min；Then water-dispersible acrylic's lotion, silicone surfactant, third are added again
Olefin(e) acid esters levelling agent, Polyether Modified Polysiloxanes Defoaming Agent, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, ethylene glycol and methyl tert-butyl
Base methanol disperses 10min；Sequentially add watersoluble closed type isocyanate curing agent, silane coupling agent, fumed silica cream
The water of shape dispersion liquid and surplus disperses 30min；
Filtering: being the conducting polymer aqueous slurry that can be made into modified enhancing with the strainer filtering of 100 mesh to 200 mesh.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment prepares the technique of electrode and using as follows:
Step 1: the conducting polymer aqueous slurry addition process liquid of the modified enhancing of above-mentioned preparation is atomized 3D printing
Technique prints preparation transparent conductive electrode on non-conventional type ceramic substrate, toasts 40min in 125 DEG C of drying boxes, can be prepared by figure
Shape transparent conductive electrode coating；
Step 2: transparent conductive electrode made from step 1 is used for electroluminescent based on transparent electrode sandwich design, electricity
The fields such as mutagens color.
Embodiment 5
A kind of conducting polymer aqueous slurry of modified enhancing, is made of following raw material by weight percentage:
PEDOT/PSS conducting polymer aqueous solution: 39wt%, solid content 1.0wt%；
Conducting inorganic material modification strengthening agent: 0.75wt%, by 0.5wt% graphene and 0.25wt% nano-silver thread group
At；
Dimethyl sulfoxide: 2.0wt%；
Concentrated ammonia liquor: 0.01wt%, ammonia content 25wt%；
Water-dispersible polyurethane lotion: 1.5wt%；
Fluorocarbon surfactant: 0.1wt%；
Polyethylene glycol 400: 0.2wt%；
Acetylenic glycols type defoaming agent: 0.2wt%；
Polyurethanes thickener: 0.8wt%；
Watersoluble closed type isocyanate curing agent (crosslinking agent): 0.5wt%；
Organic zirconium crosslinker: 0.08wt%；
Isopropanol (volatility modifier): 9.0wt%；
Sec-butyl alcohol (volatility modifier): 3.0wt%；
Ethylene glycol (moisturizer): 0.2wt%；
2- hexanol (odor-masking agent): 0.02wt%；
Water: surplus.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment is prepared in accordance with the following methods:
Stock: each raw material is got out according to formulation ratio；Graphene paste dispersion liquid is made in the graphene of formula ratio, it will
The nano-silver thread of formula ratio is configured to nano-silver thread suspension；
Dispersion: first that solid content is water-soluble for the PEDOT/PSS conducting polymer of 1.0wt% under 15 DEG C to 35 DEG C environment
Liquid, dimethyl sulfoxide, 25% concentrated ammonia liquor, conducting inorganic material modification strengthening agent stir shape in the 1000r/min of 200r/min
It is sequentially added in steeliness blender under state, disperses 10min；Then it is living that water-dispersible polyurethane lotion, fluorocarbon surface are added again
Property agent, polyethylene glycol 400, acetylenic glycols type defoaming agent, isopropanol, sec-butyl alcohol, ethylene glycol and 2- hexanol, disperse 10min；Again according to
The secondary water that watersoluble closed type isocyanate curing agent, organic zirconium crosslinker, polyurethanes thickener and surplus is added, dispersion
30min；
Filtering: being the conducting polymer aqueous slurry that can be made into modified enhancing with the strainer filtering of 100 mesh to 200 mesh.
The conducting polymer aqueous slurry of the modified enhancing of the present embodiment prepares the technique of electrode and using as follows:
Step 1: the conducting polymer aqueous slurry addition process gravure printing technique of the modified enhancing of above-mentioned preparation is existed
Printing preparation transparent conductive electrode on PET film material toasts 1min in 145 DEG C of drying boxes, can be prepared by patterned transparent conduction
Electrode coating；
Step 2: transparent conductive electrode made from step 1 is used for the touch-control field designed based on condenser type.
By 1 to 5 the electrode obtained figure layer of embodiment using the light transmittance of photoelectricity haze meter test transparency conducting layer, visited using four
The sheet resistance of needle tester testing conductive coating, the thickness of transparency conducting layer is measured using microtomy using laser microscope,
Using 3M610 adhesive tape test adhesive force, using measuring pencil durometer hardness.The performance test results are as shown in table 1 below.
1 the performance test results of table
As shown in Table 1, the transparency conducting layer tool of the conducting polymer aqueous slurry production of the modified enhancing of embodiment 1 to 5
There are high transparency, Low ESR, excellent attachment fastness and higher hardness.PEDOT/PSS conducting polymer in embodiment 1 to 5
Water-soluble liquid hold-up is higher, and conductive layer has good conductivity uniformity.Meanwhile by embodiment 1 and embodiment 2 formula and
Performance compares it is found that embodiment 1 and the electric conductivity of 2 conductive coating of embodiment are almost the same, and embodiment 2 does not add graphene
As conducting inorganic material reinforcing agent, hardness is relatively low, in spraying operation circular flow and in coating encapsulation process because
Friction easily scratches conductive coating, when showing that conducting inorganic material enhances denatured conductive macromolecule, to raising electric conductivity and rub resistance
Etc. in the balance of performances, graphene combines modification reinforcing effect that addition uses with nano-silver thread better than individually addition nano-silver thread
Modification reinforcing effect.
Finally it is emphasized that the above description is only a preferred embodiment of the present invention, it is not intended to restrict the invention.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (10)
1. a kind of conducting polymer aqueous slurry, it is characterised in that comprise the following raw materials by weight percent:
PEDOT/PSS conducting polymer aqueous solution: 16wt% to 89wt%；
Conducting inorganic material modification strengthening agent: 0.2wt% to 5.0wt%；
Conducting polymer activator: 0.05wt% to 4.5wt%；
Binder: 0.2wt% to 3.0wt%；
Surface tension modifier: 0.01wt% to 0.5wt%；
Levelling agent: 0.01wt% to 15wt%；
Defoaming agent: 0.01wt% to 20wt%；
Thickener: 0.2wt% to 2.0wt%；
Crosslinking agent: 0.01wt% to 2.0wt%；
Volatility modifier: 0wt% to 20wt%；
Moisturizer: 0wt% to 5.0wt%；
Other functional additives: 0.01wt% to 1.0wt%；
Water: surplus.
2. conducting polymer aqueous slurry according to claim 1, it is characterised in that:
The weight percent of the PEDOT/PSS conducting polymer aqueous solution is 35wt% to 89wt%；
The water-soluble fluid solid content of PEDOT/PSS conducting polymer be 0.5wt% to 2.0wt%, conductivity be 150S/cm extremely
1100S/cm, solvent are deionized water.
3. conducting polymer aqueous slurry according to claim 1, it is characterised in that:
The conducting inorganic material modification strengthening agent is at least one of carbon nanotubes, graphene, nano-silver thread；
The average caliber of the carbon nanotubes is 10nm to 30nm, and average length is 10 μm to 30 μm, specific surface area 50m2/ g is extremely
150m2/g；
The specific surface area of the graphene is 150m2/ g to 350m2/ g, D50 are 5 μm to 10 μm, and average longitudinal dimension is that 1nm is
3nm, average transverse are less than or equal to 5 μm；
The diameter of the nano-silver thread is 8nm to 40nm, and average length is 8 μm to 40 μm, and draw ratio is 500 to 1200.
4. conducting polymer aqueous slurry according to claim 3, it is characterised in that:
The conducting inorganic material modification strengthening agent is carbon nanotubes, graphene, at least two in nano-silver thread；
The nano-silver thread passes through inert metal surface Passivation Treatment, and the inert metal is at least one of gold, platinum, palladium.
5. conducting polymer aqueous slurry according to any one of claims 1 to 4, it is characterised in that:
The conducting polymer activator is dimethyl sulfoxide and pH adjusting agent；
The pH adjusting agent is at least one of water-soluble organic acid, water-soluble organic amine and ammonium hydroxide；
The water-soluble organic acid is at least one of acetic acid, lactic acid；
The water-soluble organic amine is monoethanolamine, diethanol amine, triethanolamine, N, at least one in N- dimethylethanolamine
Kind.
6. conducting polymer aqueous slurry according to any one of claims 1 to 4, it is characterised in that:
The binder is water-soluble cellulose ether, polyvinyl alcohol, polyethylene glycol, water-dispersible acrylic's lotion, water dispersible
At least one of polyaminoester emulsion, the water-soluble cellulose ether are hydroxypropyl cellulose, in hydroxypropyl methyl cellulose
It is at least one；
The surface tension modifier is alkyl alcohol ether carboxylate, fluorocarbon surfactant, silicone surfactant, alkynol class
At least one of surfactant, alkyl glucoside, fatty glyceride, sapn, tween；
The levelling agent be acrylic compounds levelling agent, esters of acrylic acid levelling agent, fluorine richness esters of acrylic acid levelling agent, silane
At least one of class moistening flatting agent, fluorocarbons class levelling agent, higher alcohols, dihydric alcohol condensation polymer；
The defoaming agent is nonylphenol polyoxyethylene ether, octyl phenol polyoxyethylene ether, organosilicon, organic silicon modified by polyether, alcohols
At least one of equal oxo solvent, acetylenic glycols type defoaming agent；
The thickener is polyurethanes thickener, acrylic thickener, polyoxyethylene ether, cellulose ether, gas phase titanium dioxide
At least one of silicon；
The crosslinking agent is watersoluble closed type isocyanate curing agent, aziridine crosslinker, the crosslinking of aziridine modified isocyanate
One or more of agent, silane coupling agent, organic titanium cross-linking agent, organic zirconium crosslinker；
The volatility modifier is at least one of alcohols, alcohol ether, and the alcohol is ethyl alcohol, normal propyl alcohol, isopropanol, positive fourth
It is alcohol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, n-amyl alcohol, isoamyl alcohol, sec-amyl alcohol, n-hexyl alcohol, isohexyl alcohol, secondary hexyl alcohol, tertiary hexanol, just pungent
At least one of alcohol, isooctanol, sec-octyl alcohol, diacetone alcohol, the alcohol ether are ethylene glycol monomethyl ether, ethylene glycol ethyl ether, ethylene glycol
At least one of monobutyl ether, diethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether；
The moisturizer is at least one of dihydric alcohol and its derivative, trihydroxylic alcohol and its derivative；
Other functional additives are at least one of odor-masking agent, dispersing agent, coalescing agent；
The water of surplus is deionized water, ultrapure water, distilled water, filtered tap water.
7. a kind of preparation method of conducting polymer aqueous slurry according to any one of claims 1 to 6, it is characterised in that
Including mixing step:
First mixing step: it by the PEDOT/PSS conducting polymer aqueous solution, the conducting polymer activator, described leads
The inorganic material-modified reinforcing agent of electricity sequentially adds in container, disperses；
Second mixing step: the binder, surface tension modifier, the levelling agent, the defoaming agent, described is added
Volatility modifier, the moisturizer and other functional additives, dispersion；
Third mixing step: being added the water of the crosslinking agent, the thickener and surplus, dispersion.
8. preparation method according to claim 7, it is characterised in that:
The temperature of first mixing step, second mixing step and the third mixing step is 15 DEG C to 35 DEG C, is stirred
Mix speed 200r/min to 1000r/min；The mixing time of first mixing step is 5min to 15min, and described second is mixed
The mixing time for closing step is 5min to 15min, and the mixing time of the third mixing step is 20min to 40min；
It before the mixing step further include dispersion steps: by PEDOT/PSS conducting polymer aqueous gel grain and described
Conducting inorganic material modification strengthening agent, the binder are configured to dispersion liquid or suspension；
After the mixing step further include filtration step: being filtered using the strainer of 100 mesh to 200 mesh.
9. a kind of conducting polymer aqueous slurry is preparing the application on conductive layer, it is characterised in that:
By preparation method described in conducting polymer aqueous slurry as claimed in any one of claims 1 to 6 or claim 7 or 8
Resulting conducting polymer aqueous slurry is atomized 3D printing technique, silk-screen printing technique, reel-to-reel intaglio process dataller by liquid
At least one of skill, flexography process, exposure mask spraying process prepare conductive layer.
10. application according to claim 9, it is characterised in that:
The conductive layer is prepared on substrate, and the substrate is the surface of organic material, inorganic material or functional coating, described to have
Machine material is thin made of at least one of polyurethane, polyester, polycarbonate, polyimides, polyvinyl chloride, acrylic resin
Film or plate；The inorganic material is ceramics, glass or crystalline silicon material；
The drying temperature of the conducting polymer aqueous slurry is 100 DEG C to 160 DEG C, and drying time is 1min to 60min.
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