CN109013250A - A method of improving electrically conductive ink uniformity and adhesive force - Google Patents

A method of improving electrically conductive ink uniformity and adhesive force Download PDF

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Publication number
CN109013250A
CN109013250A CN201810522453.9A CN201810522453A CN109013250A CN 109013250 A CN109013250 A CN 109013250A CN 201810522453 A CN201810522453 A CN 201810522453A CN 109013250 A CN109013250 A CN 109013250A
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Prior art keywords
electrically conductive
conductive ink
adhesive force
pedot
surfactant
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Chinese (zh)
Inventor
孙宽
奚佳磊
陈瑞
李猛
臧志刚
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Chongqing University
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Chongqing University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/12Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • B05D3/0254After-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50Multilayers
    • B05D7/52Two layers
    • B05D7/54No clear coat specified
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2201/00Polymeric substrate or laminate
    • B05D2201/02Polymeric substrate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2203/00Other substrates
    • B05D2203/30Other inorganic substrates, e.g. ceramics, silicon
    • B05D2203/35Glass
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2508/00Polyesters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2518/00Other type of polymers

Abstract

The invention discloses a kind of raising electrically conductive ink uniformity and the methods of adhesive force, it is characterised in that: surfactant is added in electrically conductive ink;One layer of organic solvent is applied on the electrically conductive;The conductive layer for being coated with organic solvent is made annealing treatment.By adding nonionic surfactant in electrically conductive ink, the surface free energy of ink is reduced, so that ink can avoid the occurrence of in coating procedure that liquid level is shunk, form a film incomplete phenomenon with uniform fold in substrate surface in film forming procedure.Meanwhile one layer of uniform organic solvent is coated on the electrically conductive, and make annealing treatment to the transparency conducting layer for being coated with organic solvent, the excellent transparent conductive film of available adhesive force.

Description

A method of improving electrically conductive ink uniformity and adhesive force
Technical field
The present invention relates to organic optoelectronic technologic material field, specifically a kind of raising electrically conductive ink uniformity and adhesive force Method.
Background technique
Photoelectric device such as light emitting diode, solar battery, Trackpad etc. has extensive and important answer in many fields With.Photoelectric device requires at least one transparent electrode that can absorb or emit light to meet photoelectric device.Tin indium oxide is mesh Preceding most common transparent electrode material, however the high request and tin indium oxide of the preparation of the scarcity of indium, indium tin oxide films are solid Some brittleness has all greatly affected its following application.Therefore it needs to seek new transparent conductive material at present to replace aoxidizing Indium tin.
Poly- (3,4~ethylenedioxy thiophene) (PEDOT) is synthesized for the first time in the laboratory A G Bayer of Germany, is The Typical Representative of thiophene-based conductive polymer, it is conductive by introducing what ethylene two oxy obtained at 3 of thiphene ring and 4 Dopant states it is highly stable.And the absorption peak of the conjugated bonds of PEDOT does not occur in visible absorption range, absorbs wave wave Length is about in 300nm or so, the property with light transmission.
Therefore, PEDOT possesses excellent electromagnetic property, machining property as most conductive polymer material, Stable chemical property, good transparency, higher photoelectric efficiency, excellent mechanical flexibility and bio-compatibility etc. are special Point.This just imparts PEDOT as protein and other is immobilized, prepares biosensor, electrochromism device, electrochemistry The ideal material of capacitor, solar battery, strain gauge and touch screen etc..
However there are easy to fall off, poor with substrate adhesion for the transparent conductive film prepared by PEDOT:PSS electrically conductive ink The problem of, this just seriously limits the application of PEDOT conductive film in the industry, it is desirable to realize the big rule of PEDOT conductive film Mould production, improving adhesive force between film and substrate is the technical barrier that not can bypass.
Therefore to improve PEDOT conductive film adhesive force method carry out further investigation have extremely strong realistic meaning and Commercial value.
Summary of the invention
Present invention aim to address problems of the prior art, a kind of raising electrically conductive ink uniformity and attached is provided The method puted forth effort.
To realize the present invention purpose and the technical solution adopted is that such, a kind of raising electrically conductive ink uniformity and attachment The method of power, which comprises the following steps:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, after standing 5~30min, is adulterated There is the electrically conductive ink of nonionic surfactant;
The electrically conductive ink includes PEDOT:PSS dispersion liquid;
The weight ratio range of the surfactant and PEDOT:PSS dispersion liquid is 0.01%~1%;
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in doped with nonionic surfactant Electrically conductive ink, obtain uniform transparency conducting layer wet film;
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature range is 90~140 DEG C, and time range is 5~60min;
2.3) organic solvent will be coated on transparency conducting layer obtained in step 2.2);
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with organic solvent obtained in step 2.3) is placed in heated at constant temperature environment, annealing solidification is carried out After processing, cooled to room temperature obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 90~160 DEG C, and the time is 5~60min.
Further, the electrically conductive ink in the step 1) is a kind of conductive polymer polymer, and the electrically conductive ink removes It further include one of polyaniline, polypyrrole and polythiophene or a variety of outside PEDOT:PSS;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid, and wherein the quality of PEDOT and PSS compares range For 1 ︰, 1~1 ︰ 6.
Further, the surfactant in the step 1) is a kind of nonionic surfactant, the surfactant Including octyl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, high-carbon fatty alcohol polyoxyethylene ether, aliphatic acid polyethenoxy ether, Fatty acid methyl ester ethoxylate, sucrose fatty ester, fatty acid methyl ester APEO, polyethenoxy sorbitan list oil Acid esters, polyoxyethylene 20 sorbitan monolaurate, octanol polyoxyethylene ether, ethoxylated dodecyl alcohol, octyl phenyl are poly- One or more of ethylene oxide ether or lauryl sodium sulfate.
Further, the organic solvent includes toluene, dimethylbenzene, hexamethylene, cyclohexanone, chlorobenzene, dichloro-benzenes, acetic acid second Ester, butyl acetate, methanol, ethyl alcohol, propyl alcohol, isopropanol, n-butanol, isobutanol, methylisobutylketone, acetone, butanone, propylene glycol first Ether, dipropylene glycol methyl ether, ether, propylene oxide, glycol monoethyl ether, ethylene glycol monoethyl ether, methylene chloride, styrene, perchloro- One or more of ethylene, trichloro ethylene or ethylene glycol ether.
Further, in the whipping process in the step 1): stirring rate range is 100~1500rpm, mixing time model It encloses for 5~60min.
Further, the preprocessing process of the base material in the step 2.1) are as follows:
Base material is cut into square base, it is successively clear with dish washing liquid, deionized water, acetone and each ultrasound of isopropanol After washing 20min, base material is carried out with high pure nitrogen to remove residual processing;The size of the square base include 20mm × 20mm。
Further, the coating method in the step 2.1) includes sol evenning machine spin coating, inkjet printing, bar coating, slit One or more of squash type coating and scraper method
Coating method in the step 2.3) includes sol evenning machine spin coating, inkjet printing, bar coating, slot die painting One or more of cloth, Best-Effort request plated film and scraper method.
Further, the base material in the step 2.1) includes polyethylene terephthalate, poly- naphthalenedicarboxylic acid second two Alcohol ester, polyimides and nonbreakable glass.
It is a kind of to be obtained by the method according to any one of claims 1 to 8 for improving electrically conductive ink uniformity and adhesive force The transparent electrode obtained.
The solution have the advantages that unquestionable, the invention has the following advantages that
1) the present invention provides a kind of raising electrically conductive ink uniformity and the methods of adhesive force, by adding in electrically conductive ink Add nonionic surfactant, reduce the surface free energy of ink, so that ink can be existed in film forming procedure with uniform fold Substrate surface, avoids the occurrence of in coating procedure that liquid level is shunk, form a film incomplete phenomenon;
2) present invention coats one layer of uniform organic solvent on the electrically conductive, and to the transparency conducting layer for being coated with organic solvent It is made annealing treatment, the excellent transparent conductive film of available adhesive force;Because organic polymer conductive film exists and substrate Between poor adhesive force, it is easy to fall off the problems such as, it is good in industrialized production that this has just seriously affected organic polymer conductive film Rate, the present invention effectively improve the adhesive force between film and substrate by carrying out secondary treatment to organic polymer conductive layer;
3) present invention has the characteristics of simple processing step, low production cost, the extensive life suitable for electrically conductive ink It produces;
4) it using the invention enables the processes of industrialization of organic polymer conductive film further to be promoted, is effectively improved The antistrip performance of conductive film.
Detailed description of the invention
Fig. 1 is the preparation structure schematic diagram according to conductive polymer film in the embodiment of the present invention 1;
Fig. 2 is according to the conductive polymer film prepared in the embodiment of the present invention 1.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention only It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used With means, various replacements and change are made, should all include within the scope of the present invention.
Embodiment 1:
PEDOT:PSS is purchased from Heraeus company of Germany, product type PH1000 in embodiment.Other drugs and solvent are equal Purchased from Sinopharm Chemical Reagent Co., Ltd..
As depicted in figs. 1 and 2, a method of improving electrically conductive ink uniformity and adhesive force, which is characterized in that including with Lower step:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, stand 20min after, obtain doped with The electrically conductive ink of nonionic surfactant;
The surfactant is lauryl sodium sulfate;The weight percent of the lauryl sodium sulfate is 0.05%;
The electrically conductive ink is PEDOT:PSS dispersion liquid;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid;
The volume of the PEDOT:PSS dispersion liquid is 5mL;
The stirring rate is 500rpm, mixing time 10min.
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in doped with nonionic surfactant Electrically conductive ink, obtain uniform transparency conducting layer wet film;
The preprocessing process of the base material are as follows:
Glass substrate is cut into square base, it is successively clear with dish washing liquid, deionized water, acetone and each ultrasound of isopropanol After washing 20min, glass substrate is carried out with high pure nitrogen to remove residual processing;The size of the square base include 20mm × 20mm。
The coating procedure are as follows:
The glass substrate being dried with nitrogen is placed on sol evenning machine, if setting sol evenning machine level-one revolving speed 1000rpm, time are PEDOT electrically conductive ink is spun in glass substrate by 60s, Second-Stage Rotating Speed 3000rpm, time 3s.
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature is 120 DEG C, time 10min;
2.3) dichloro-benzenes will be coated on transparency conducting layer obtained in step 2.2);
It is described it is coated be known as: transparent electrode is placed on sol evenning machine, the revolving speed of 1500rpm is set, dichloro-benzenes is coated with Onto PEDOT transparent electrode;
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with dichloro-benzenes obtained in step 2.3) is placed in heated at constant temperature environment, is carried out at annealing solidification After reason, cooled to room temperature obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 120 DEG C, time 30min.
Embodiment 2:
A method of improving electrically conductive ink uniformity and adhesive force, which comprises the following steps:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, stand 20min after, obtain doped with The electrically conductive ink of nonionic surfactant;
The surfactant is lauryl sodium sulfate;The weight percent of the lauryl sodium sulfate is 0.05%;
The electrically conductive ink is PEDOT:PSS dispersion liquid;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid;
The volume of the PEDOT:PSS dispersion liquid is 5mL;
The stirring rate is 500rpm, mixing time 10min.
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in doped with nonionic surfactant Electrically conductive ink, obtain uniform transparency conducting layer wet film;
The preprocessing process of the base material are as follows:
Glass substrate is cut into square base, it is successively clear with dish washing liquid, deionized water, acetone and each ultrasound of isopropanol After washing 20min, glass substrate is carried out with high pure nitrogen to remove residual processing;The size of the square base include 20mm × 20mm。
The coating procedure are as follows:
The glass substrate being dried with nitrogen is placed on sol evenning machine, if setting sol evenning machine level-one revolving speed 1000rpm, time are PEDOT electrically conductive ink is spun in glass substrate by 60s, Second-Stage Rotating Speed 3000rpm, time 3s.
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature is 120 DEG C, time 10min;
2.3) methanol will be coated on transparency conducting layer obtained in step 2.2);
It is described it is coated be known as: transparent electrode is placed on sol evenning machine, the revolving speed of 1500rpm is set, methanol is coated with In PEDOT transparent electrode;
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with methanol obtained in step 2.3) is placed in heated at constant temperature environment, annealing curing process is carried out Afterwards, cooled to room temperature, obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 120 DEG C, time 30min.
Embodiment 3:
A method of improving electrically conductive ink uniformity and adhesive force, which comprises the following steps:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, stand 20min after, obtain doped with The electrically conductive ink of nonionic surfactant;
The surfactant is polyoxyethylene sorbitan monooleate;The polyethenoxy sorbitan list oil The weight percent of acid esters is 0.05%;
The electrically conductive ink is PEDOT:PSS dispersion liquid;
The volume of the PEDOT:PSS dispersion liquid is 5mL;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid;
The stirring rate is 500rpm, mixing time 10min.
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in doped with nonionic surfactant Electrically conductive ink, obtain uniform transparency conducting layer wet film;
The preprocessing process of the base material are as follows:
Glass substrate is cut into square base, it is successively clear with dish washing liquid, deionized water, acetone and each ultrasound of isopropanol After washing 20min, glass substrate is carried out with high pure nitrogen to remove residual processing;The size of the square base include 20mm × 20mm。
The coating procedure are as follows:
The glass substrate being dried with nitrogen is placed on sol evenning machine, if setting sol evenning machine level-one revolving speed 1000rpm, time are PEDOT electrically conductive ink is spun in glass substrate by 60s, Second-Stage Rotating Speed 3000rpm, time 3s.
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature is 120 DEG C, time 10min;
2.3) dichloro-benzenes will be coated on transparency conducting layer obtained in step 2.2);
It is described it is coated be known as: transparent electrode is placed on sol evenning machine, the revolving speed of 1500rpm is set, dichloro-benzenes is coated with Onto PEDOT transparent electrode;
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with dichloro-benzenes obtained in step 2.3) is placed in heated at constant temperature environment, is carried out at annealing solidification After reason, cooled to room temperature obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 120 DEG C, time 30min.
Embodiment 4:
A method of improving electrically conductive ink uniformity and adhesive force, which comprises the following steps:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, stand 20min after, obtain doped with The electrically conductive ink of nonionic surfactant;
The surfactant is polyoxyethylene sorbitan monooleate;The polyethenoxy sorbitan list oil The weight percent of acid esters is 0.2%;
The electrically conductive ink is PEDOT:PSS dispersion liquid;
The volume of the PEDOT:PSS dispersion liquid is 5mL;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid;
The stirring rate is 500rpm, mixing time 10min.
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in doped with nonionic surfactant Electrically conductive ink, obtain uniform transparency conducting layer wet film;
The preprocessing process of the base material are as follows:
Glass substrate is cut into square base, it is successively clear with dish washing liquid, deionized water, acetone and each ultrasound of isopropanol After washing 20min, glass substrate is carried out with high pure nitrogen to remove residual processing;The size of the square base include 20mm × 20mm。
The coating procedure are as follows:
The glass substrate being dried with nitrogen is placed on sol evenning machine, if setting sol evenning machine level-one revolving speed 1000rpm, time are PEDOT electrically conductive ink is spun in glass substrate by 60s, Second-Stage Rotating Speed 3000rpm, time 3s.
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature is 120 DEG C, time 10min;
2.3) dichloro-benzenes will be coated on transparency conducting layer obtained in step 2.2);
It is described it is coated be known as: transparent electrode is placed on sol evenning machine, the revolving speed of 1500rpm is set, dichloro-benzenes is coated with Onto PEDOT transparent electrode;
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with dichloro-benzenes obtained in step 2.3) is placed in heated at constant temperature environment, is carried out at annealing solidification After reason, cooled to room temperature obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 120 DEG C, time 30min.
Embodiment 5:
A method of improving electrically conductive ink uniformity and adhesive force, which comprises the following steps:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, stand 20min after, obtain doped with The electrically conductive ink of nonionic surfactant;
The surfactant is lauryl sodium sulfate;The weight percent of the lauryl sodium sulfate is 0.05%;
The electrically conductive ink is PEDOT:PSS dispersion liquid;
The volume of the PEDOT:PSS dispersion liquid is 5mL;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid;
The stirring rate is 500rpm, mixing time 10min.
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in doped with nonionic surfactant Electrically conductive ink, obtain uniform transparency conducting layer wet film;
The preprocessing process of the base material are as follows:
The optics PET substrate of 50 μ m-thicks is cut into A4 paper size, successively uses dish washing liquid, deionized water, acetone and isopropyl After alcohol is respectively cleaned by ultrasonic 20min, glass substrate is carried out with high pure nitrogen to remove residual processing.
The coating procedure are as follows:
Under room temperature, PET is fixed on smooth glass table, with No. 12 bar applying conductive ink on PET, is obtained To the PET containing PEDOT wet film.
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature is 120 DEG C, time 10min;
2.3) dichloro-benzenes will be coated on transparency conducting layer obtained in step 2.2);
The coating procedure is to be coated with dichloro-benzenes over transparent conductive layer with No. 12 bars;
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with dichloro-benzenes obtained in step 2.3) is placed in heated at constant temperature environment, is carried out at annealing solidification After reason, cooled to room temperature obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 120 DEG C, time 30min.
Embodiment 6:
A method of improving electrically conductive ink uniformity and adhesive force, which comprises the following steps:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, stand 20min after, obtain doped with The electrically conductive ink of nonionic surfactant;
The surfactant is lauryl sodium sulfate;The weight percent of the lauryl sodium sulfate is 0.05%;
The electrically conductive ink is PEDOT:PSS dispersion liquid;
The volume of the PEDOT:PSS dispersion liquid is 5mL;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid;
The stirring rate is 500rpm, mixing time 10min.
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in doped with nonionic surfactant Electrically conductive ink, obtain uniform transparency conducting layer wet film;
The preprocessing process of the base material are as follows:
The optics PET substrate of 50 μ m-thicks is cut into A4 paper size, successively uses dish washing liquid, deionized water, acetone and isopropyl After alcohol is respectively cleaned by ultrasonic 20min, glass substrate is carried out with high pure nitrogen to remove residual processing.
The coating procedure are as follows:
Under room temperature, PET is fixed on smooth glass table, with No. 12 bar applying conductive ink on PET, is obtained To the PET containing PEDOT wet film.
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature is 120 DEG C, time 10min;
2.3) dichloro-benzenes will be coated on transparency conducting layer obtained in step 2.2);
The coating procedure is to be coated with dichloro-benzenes over transparent conductive layer with No. 12 bars;
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with dichloro-benzenes obtained in step 2.3) is placed in heated at constant temperature environment, is carried out at annealing solidification After reason, cooled to room temperature obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 120 DEG C, time 30min.
Experimental example:
PEDOT conductive film obtained in Examples 1 to 6 is subjected to performance characterization test, test result is as shown in table 1:
Table 1

Claims (9)

1. a kind of method for improving electrically conductive ink uniformity and adhesive force, which comprises the following steps:
1) surfactant is added in electrically conductive ink
Electrically conductive ink and surfactant are added in container, are stirred until homogeneous, after standing 5~30min, is obtained doped with non- The electrically conductive ink of ionic surface active agent;
The electrically conductive ink includes PEDOT:PSS dispersion liquid;
The weight ratio range of the surfactant and PEDOT:PSS dispersion liquid is 0.01%~1%;
2) one layer of organic solvent is applied on the electrically conductive
2.1) coating step 1 on the base material after will be pretreated) obtained in leading doped with nonionic surfactant Electric ink obtains uniform transparency conducting layer wet film;
2.2) transparency conducting layer wet film obtained in step 2.1) is dried, obtains transparency conducting layer;
In the drying course: temperature range is 90~140 DEG C, and time range is 5~60min;
2.3) organic solvent will be coated on transparency conducting layer obtained in step 2.2);
3) conductive layer for being coated with organic solvent is made annealing treatment
The conduction for being coated with organic solvent obtained in step 2.3) is placed in heated at constant temperature environment, annealing curing process is carried out Afterwards, cooled to room temperature, obtains that adhesive force is excellent, transparent electrode of anti-strip;
The temperature of the annealing curing process is 90~160 DEG C, and the time is 5~60min.
2. a kind of method for improving electrically conductive ink uniformity and adhesive force according to claim 1, it is characterised in that: described Electrically conductive ink in step 1) is a kind of conductive polymer polymer, and the electrically conductive ink further includes polyphenyl in addition to PEDOT:PSS One of amine, polypyrrole and polythiophene are a variety of;
PEDOT:PSS concentration is 1.3% in the PEDOT:PSS dispersion liquid, and wherein the quality of PEDOT and PSS is 1 ︰ 1 than range ~1 ︰ 6.
3. a kind of method for improving electrically conductive ink uniformity and adhesive force according to claim 1, it is characterised in that: described Surfactant in step 1) is a kind of nonionic surfactant, and the surfactant includes octylphenol polyethylene ethylene oxide Ether, nonylphenol polyoxyethylene ether, high-carbon fatty alcohol polyoxyethylene ether, aliphatic acid polyethenoxy ether, fatty acid methyl ester ethoxylation Object, sucrose fatty ester, fatty acid methyl ester APEO, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan Sorbitan monolaurate, octanol polyoxyethylene ether, ethoxylated dodecyl alcohol, octyl phenyl polyoxyethylene ether or dodecyl One or more of sodium sulphate.
4. a kind of method for improving electrically conductive ink uniformity and adhesive force according to claim 1, it is characterised in that: described Organic solvent includes toluene, dimethylbenzene, hexamethylene, cyclohexanone, chlorobenzene, dichloro-benzenes, ethyl acetate, butyl acetate, methanol, second Alcohol, propyl alcohol, isopropanol, n-butanol, isobutanol, methylisobutylketone, acetone, butanone, propylene glycol monomethyl ether, dipropylene glycol methyl ether, second Ether, propylene oxide, glycol monoethyl ether, ethylene glycol monoethyl ether, methylene chloride, styrene, perchloroethylene, trichloro ethylene or ethylene One or more of glycol ether.
5. a kind of method for improving electrically conductive ink uniformity and adhesive force according to claim 1, it is characterised in that: described In whipping process in step 1): stirring rate range is 100~1500rpm, and mixing time range is 5~60min.
6. a kind of method for improving electrically conductive ink uniformity and adhesive force according to claim 1, it is characterised in that: described The preprocessing process of base material in step 2.1) are as follows:
Base material is cut into square base, is successively respectively cleaned by ultrasonic with dish washing liquid, deionized water, acetone and isopropanol After 20min, base material is carried out with high pure nitrogen to remove residual processing;The size of the square base includes 20mm × 20mm.
7. a kind of method for improving electrically conductive ink uniformity and adhesive force according to claim 1, it is characterised in that: described Coating method in step 2.1) includes in sol evenning machine spin coating, inkjet printing, bar coating, slot die coating and scraper method One or more
Coating method in the step 2.3) include sol evenning machine spin coating, inkjet printing, bar coating, slot die coating, One or more of Best-Effort request plated film and scraper method.
8. a kind of method for improving electrically conductive ink uniformity and adhesive force according to claim 1, it is characterised in that: described Base material in step 2.1) includes polyethylene terephthalate, polyethylene naphthalate, polyimides and rigidity Glass.
9. a kind of method by raising electrically conductive ink uniformity according to any one of claims 1 to 8 and adhesive force is obtained Transparent electrode.
CN201810522453.9A 2018-05-28 2018-05-28 A method of improving electrically conductive ink uniformity and adhesive force Pending CN109013250A (en)

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CN105609216A (en) * 2016-01-20 2016-05-25 重庆大学 Ink printing process-based preparation method of flexible transparent electrode
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