CN104851522A - Preparation method of large-area PEDOT/PSS transparent conductive film - Google Patents
Preparation method of large-area PEDOT/PSS transparent conductive film Download PDFInfo
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- CN104851522A CN104851522A CN201510262126.0A CN201510262126A CN104851522A CN 104851522 A CN104851522 A CN 104851522A CN 201510262126 A CN201510262126 A CN 201510262126A CN 104851522 A CN104851522 A CN 104851522A
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Abstract
The invention discloses a preparation method of a large-area PEDOT/PSS transparent conductive film, i.e., a wire rod coating method, and belongs to the field of a transparent conductive film. The preparation method of the transparent conductive film involves preparing a PEDOT/PSS coating liquid doped with glycol (EG) and a surfactant (Capstone FS-30), employing a wire rod coating film and performing thermal processing. The large-area PEDOT/PSS transparent conductive film prepared by use of the method has good conductivity, high transparency and high uniformity. Compared to a conventional spin coating method frequently used for preparing a film, the method provided by the invention prevents enormous waste of the coating liquid, more importantly, can be manufactured in a large scale, and accordingly realizes roll-to-roll large-scale production.
Description
Technical field
The invention belongs to transparent conductive film field, be specifically related to use line rod rubbing method to prepare the method for PEDOT/PSS film on flexible pet substrate, particularly at ambient pressure, large area preparation has the method for the PEDOT/PSS film of the transparency and conductivity concurrently.
Background technology
Along with IT electronic product, developing rapidly of intelligent appliance industry, transparent conductive film achieves extensive use in fields such as flat-panel monitor, electrical control panel, solar cells.Wherein, tin indium oxide (ITO) is generally acknowledge at present the most ripe and most widely used transparent conductive material.But indium resource scarcity, expensive, in the last few years, the transparent conductive material developing alternative ITO had become a new research field, and conducting polymer composite is in occupation of critical role.
In conducting polymer field, PEDOT/PSS good film-forming property, the advantages such as the conducting film formed after coating has conductivity high (through suitably adulterating), excellent, the easy solution of environmental stability processes process, light transmission is good, achieving application in fields such as Organic Light Emitting Diode, antistatic, ultracapacitors, is a kind of conducting polymer that Recent study is maximum.
The method that what current utilization was maximum are used for studies conducting polymer transparent membrane is spin-coating method.But spin-coating method is due to self intrinsic deficiency, and the film of preparation exists non-uniform phenomenon in conductivity and light transmission, and can cause the significant wastage of dispersion liquid, again cannot large area preparation.Line rod rubbing method is the one of print process, operation is simple, normal temperature and pressure conditions operates, speed is controlled, various thickness can be prepared and the good film of uniformity to meet test request, efficiency is high, but wants to obtain superior in quality PEDOT/PSS film, meet large area preparation, also need to carry out exploratory development to its parameter index.
Summary of the invention
For the present Research of electrically conducting transparent film preparation, the present invention aims to provide and a kind ofly large area can prepare the method for transparent conductive film, meets industrial production demand.
For realizing this goal of the invention, the present invention carries out exploratory development to technical parameter index in described large area PEDOT/PSS transparent conductive film preparation process, and concrete preparation method is realized by following steps:
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning, dry up with hair-dryer for subsequent use;
(2) the PEDOT/PSS dispersion liquid of preparation doping ethylene glycol and surfactant Capstone FS-30, stirs under normal temperature, makes to mix;
(3) under normal temperature clean pet substrate reach the standard grade rod coating above-mentioned dispersion liquid;
(4) heat treatment under normal pressure, naturally cools to room temperature.
Prepare in the method for PEDOT/PSS transparent conductive film in above-mentioned large area, the doping ratio of the ethylene glycol described in step (2) is the 4%-7% of PEDOT/PSS dispersion liquid total weight.
Prepare in the method for PEDOT/PSS transparent conductive film in above-mentioned large area, the doping ratio of the surfactant Capstone FS-30 described in step (2) is the 0.5%-7% of PEDOT/PSS dispersion liquid total weight.
Prepare in the method for PEDOT/PSS transparent conductive film in above-mentioned large area, the coating speed described in step (3) is 24.2 rpm-199.6 rpm.
Prepare in the method for PEDOT/PSS transparent conductive film in above-mentioned large area, the line rod type described in step (3) number is No.3, No.5, No.7, No.9.
Prepare in the method for PEDOT/PSS transparent conductive film in above-mentioned large area, the heat treatment temperature described in step (4) is 50 DEG C-160 DEG C.
Through validation trial: the present invention is at doping 1 wt% surfactant Capstone FS-30,7 wt%EG, use No.3 line rod, uniformity has been prepared good under motor speed 100.8rpm and heat treatment temperature 120 DEG C of conditions, have both the film of satisfactory electrical conductivity and light transmission, see accompanying drawing 9 and table 1.
Prepare in the process of PEDOT/PSS transparent conductive film at this, the use of surfactant can strengthen adhesive force between dispersion liquid and pet substrate, improve dispersion liquid in on-chip spreading ability, is the step that large area prepares transparent conductive film key; The doping object of ethylene glycol (EG) improves the conductivity of film.
Innovative point of the present invention is: use excellent painting mode large area to prepare film, has probed into different model line rod and coating speed to the impact at made film rectangular resistance (Rs) and 550 nm places light transmittance (T), has seen accompanying drawing 3 and 4; In addition, probed into the impact of film thermal treatment temperature on photo electric, accompanying drawing 5 is shown in the impact electrical on film light of different heat treatment temperature; In addition, also inquired into the impact that the doping of different amount ethylene glycol is electrical on film light, seen accompanying drawing 6.
The invention has the advantages that; Adopt line rod rubbing method to prepare PEDOT/PSS film, can not only be had concurrently the film that light transmission is good and conductivity is good uniformly, and can large area preparation.Preparing compared with film with using now more spin-coating method, not only avoid a large amount of wastes of coating fluid, the more important thing is can large area manufacture, and then realizes volume to volume large-scale production.
Accompanying drawing explanation
Fig. 1 is the contact angle of PEDOT/PSS dispersion liquid on pet substrate and the relation of surfactant doping content.
Fig. 2 is the relation (EG7%, motor speed 100rpm, heat treatment temperature 50 DEG C) of Rs and T of PEDOT/PSS film and line rod type number.
Fig. 3 be coated with by No.3, No.5, No.7, No.9 tetra-line rod type number PEDOT/PSS film (5% Capstone FS-30,7%EG, motor speed 100.8rpm, heat treatment temperature 50 DEG C).
Fig. 4 is Rs and T of PEDOT/PSS film and the relation (1% Capstone FS-30,7% EG, No.3 line rod, heat treatment temperature 120 DEG C) of coating speed (motor speed).
Fig. 5 is the PEDOT/PSS film (1% Capstone FS-30,7% EG, No.3 line rod, heat treatment temperature 120 DEG C) prepared under motor speed 74.6rpm condition.
Fig. 6 is Rs and T of PEDOT/PSS film and the relation (1% Capstone FS-30,7% EG, No.3 line rod, motor speed 100rpm) of heat treatment temperature.
Fig. 7 is the PEDOT/PSS film (1% Capstone FS-30,7% EG, No.3 line rod, motor speed 100rpm) under 140 DEG C of heat-treat conditions.
Fig. 8 is Rs and T of PEDOT/PSS film and the relation (1% Capstone FS-30, No.3 line rod, motor speed 100rpm, heat treatment temperature 120 DEG C) of ethylene glycol doping content.
Fig. 9 is the PEDOT/PSS film (1% Capstone FS-30, No.3 line rod, motor speed 100rpm, heat treatment temperature 120 DEG C) of doping EG 7%.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment.
Embodiment 1
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 1.6465g in 10ml sample bottle, then add ethylene glycol 0.1239g and 0.0177g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fixed electrical machinery rotating speed 100.8 rpm, the pet substrate cleaned uses No.3 respectively, the above-mentioned coating fluid of No.5, No.7, No.9 line rod coating;
(4) under normal pressure in 50 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, see accompanying drawing 2.
Embodiment 2
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 1.5694g in 10ml sample bottle, then add ethylene glycol 0.1181g and 0.0095g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fixed electrical machinery rotating speed 100.8 rpm, the pet substrate cleaned uses No.3 respectively, the above-mentioned coating fluid of No.5, No.7, No.9 line rod coating;
(4) under normal pressure in 50 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, see accompanying drawing 3.
Embodiment 3
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 2.2504g in 10ml sample bottle, then add ethylene glycol 0.1694g and 0.0244g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fix N is number line rod o.3, fixed electrical machinery rotating speed 199.6 rpm, clean pet substrate reach the standard grade rod coating above-mentioned coating fluid;
(4) under normal pressure in 50 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, be respectively 2.4 × 10
2Ω sq
-1with 84.4%.
Embodiment 4
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 4.7716g in 10ml sample bottle, then add ethylene glycol 0.3590g and 0.0518g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fix N is number line rod o.3, fixed electrical machinery rotating speed 24.4 rpm, clean pet substrate reach the standard grade rod coating above-mentioned coating fluid;
(4) under normal pressure in 50 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, be respectively 2.4 × 10
2Ω sq
-1with 84.1%.
Embodiment 5
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 6.9551g in 10ml sample bottle, then add ethylene glycol 0.5168g and 0.0756g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fix N is number line rod o.3, fixed electrical machinery rotating speed 100.8 rpm, clean pet substrate reach the standard grade rod coating above-mentioned coating fluid;
(4) under normal pressure in 80 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, be respectively 2.7 × 10
2Ω sq
-1with 84.3%.
Embodiment 6 (Best Applying Condition)
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 2.0712g in 10ml sample bottle, then add ethylene glycol 0.1559g and 0.0226g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fix N is number line rod o.3, fixed electrical machinery rotating speed 100.8 rpm, clean pet substrate reach the standard grade rod coating above-mentioned coating fluid;
(4) under normal pressure in 120 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, see accompanying drawing 9 and table 1.
Embodiment 7
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 2.4107g in 10ml sample bottle, then add ethylene glycol 0.1531g and 0.0261g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fix N is number line rod o.3, fixed electrical machinery rotating speed 100.8 rpm, clean pet substrate reach the standard grade rod coating above-mentioned coating fluid;
(4) under normal pressure in 120 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, be respectively 2.5 × 10
2Ω sq
-1with 84.4%.
Embodiment 8
(1) PET substrate is successively used liquid detergent water, absolute ethyl alcohol, deionized water ultrasonic cleaning 15min respectively, dry up with hair-dryer for subsequent use;
(2) under normal temperature, accurately take PH1000 dispersion liquid 2.3541g in 10ml sample bottle, then add ethylene glycol 0.1230g and 0.0254g surfactant Capstone FS-30, stir 5h under normal temperature, fully mix, be made into coating fluid;
(3) under normal temperature, fix N is number line rod o.3, fixed electrical machinery rotating speed 100.8 rpm, clean pet substrate reach the standard grade rod coating above-mentioned coating fluid;
(4) under normal pressure in 120 DEG C of heat treatment 20min, naturally cool to room temperature; Measure the square resistance (Rs) of film and the light transmittance (T) at 550nm place, be respectively 2.7 × 10
2Ω sq
-1with 84.8%.
Above embodiment agents useful for same is and directly uses after producer buys, without doing any process, PEDOT/PSS is poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid), Capstone FS-30 is fluorocarbon surfactant, PH1000 dispersion liquid is the trade name of poly-(3,4-ethylenedioxy thiophene)/poly-p styrene sulfonic acid dispersion liquid; PET sheet used is parylene's glycol ester, and original light transmittance is 85.0%; Key instrument equipment used and model: automatic film coating instrument (NO 542-AB, day intrinsic safety field essence mechanism does institute); UV, visible light near-infrared spectrophotometer (AU12320005, Agilent company of the U.S.); Low ESR tester (MCP-T610, Mitsubishi Chemical Co., Ltd.).
Table 1 adulterates 1% surfactant Capstone FS-30,7%EG, uses No.3 line rod, the square resistance of the film prepared under motor speed 100.8rpm and heat treatment temperature 120 DEG C of conditions and light transmittance
| Sample number | Square resistance/× 10 2 Ω sq -1 | Light transmittance (%, 550nm) |
| 1-1 | 2.3 | 84.8 |
| 1-2 | 2.8 | 84.8 |
| 1-3 | 2.0 | 83.6 |
| 1-4 | 2.1 | 84.7 |
| Mean value | 2.3 | 84.5 |
Note: each square resistance is 15 different local mean values measured on film.
From table 1 and Fig. 9, when surfactant Capstone FS-30 doping content is 1 wt%, EG doping is 7%, fix N o.3 number line rod and motor speed 100.8rpm time, film heat treatment 15min under 120 DEG C of conditions of preparation, not only large-area uniformity is good for the film of preparation, and has good light permeability and conductivity concurrently.
Claims (2)
1. large area prepares a method for PEDOT/PSS nesa coating, it is characterized in that, is realized by following steps:
(1) PET substrate is successively used the ultrasonic cleaning respectively of liquid detergent water, absolute ethyl alcohol, deionized water, dry up with hair-dryer for subsequent use;
(2) the PEDOT/PSS dispersion liquid of preparation doping ethylene glycol and surfactant Capstone FS-30, stirs under normal temperature, makes to mix;
(3) under normal temperature clean pet substrate reach the standard grade rod coating above-mentioned dispersion liquid;
(4) heat treatment under normal pressure, naturally cools to room temperature;
The 0.5%-7% of to be the 4%-7% of PEDOT/PSS dispersion liquid total weight, surfactant Capstone FS-30 doping the be PEDOT/PSS dispersion liquid total weight of the ethylene glycol doping described in step (2);
When line rod described in step (3) is coated with, coating speed is 24.2 rpm-199.6 rpm; Line rod type used number is No.3, No.5, No.7, No.9;
Heat treatment temperature described in step (4) is 50 DEG C-160 DEG C.
2. large area as claimed in claim 1 prepares the method for PEDOT/PSS nesa coating, it is characterized in that, is preferably as follows experiment condition:
Surfactant Capstone FS-30 doping is 1 % of PEDOT/PSS dispersion liquid total weight, and ethylene glycol doping is 7 % of PEDOT/PSS dispersion liquid total weight; Use No.3 line rod, motor speed 100.8rpm and heat treatment temperature 120 DEG C.
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| CN105895197A (en) * | 2016-04-14 | 2016-08-24 | 南京邮电大学 | Flexible transparent silver grid composite electrode and production method thereof |
| CN108089366A (en) * | 2017-12-06 | 2018-05-29 | 深圳市华星光电技术有限公司 | A kind of color membrane substrates and preparation method thereof |
| CN108780684A (en) * | 2018-01-10 | 2018-11-09 | 重庆大学 | It is a kind of can prepare with scale flexible transparent electrode method |
| CN108854593A (en) * | 2018-06-13 | 2018-11-23 | 山西大学 | A kind of high-throughput double excellent type PVDF plate membrane preparation methods with high rejection |
| CN112442899A (en) * | 2020-11-13 | 2021-03-05 | 香港纺织及成衣研发中心有限公司 | Stretchable flexible composite fabric-based sensor and application thereof |
| CN112786789A (en) * | 2021-01-08 | 2021-05-11 | 江苏大学 | Vertical Stacking of PEDOT PSS/PbS/CsPbCl3Preparation method of flexible light detector with nano structure |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105895197A (en) * | 2016-04-14 | 2016-08-24 | 南京邮电大学 | Flexible transparent silver grid composite electrode and production method thereof |
| CN108089366A (en) * | 2017-12-06 | 2018-05-29 | 深圳市华星光电技术有限公司 | A kind of color membrane substrates and preparation method thereof |
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| CN108780684A (en) * | 2018-01-10 | 2018-11-09 | 重庆大学 | It is a kind of can prepare with scale flexible transparent electrode method |
| CN108780684B (en) * | 2018-01-10 | 2022-07-12 | 重庆大学 | Method for preparing flexible transparent electrode in large scale |
| CN108854593A (en) * | 2018-06-13 | 2018-11-23 | 山西大学 | A kind of high-throughput double excellent type PVDF plate membrane preparation methods with high rejection |
| CN112442899A (en) * | 2020-11-13 | 2021-03-05 | 香港纺织及成衣研发中心有限公司 | Stretchable flexible composite fabric-based sensor and application thereof |
| CN112442899B (en) * | 2020-11-13 | 2023-08-18 | 香港纺织及成衣研发中心有限公司 | Stretchable flexible composite fabric-based sensor and application thereof |
| CN112786789A (en) * | 2021-01-08 | 2021-05-11 | 江苏大学 | Vertical Stacking of PEDOT PSS/PbS/CsPbCl3Preparation method of flexible light detector with nano structure |
| CN112786789B (en) * | 2021-01-08 | 2024-03-22 | 江苏大学 | Vertically stacking PEDOT: PSS/PbS/CsPbCl 3 Method for preparing nanostructure flexible photodetector |
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Application publication date: 20150819 |