CN105609216B - A kind of preparation method of the flexible transparent electrode based on ink print technique - Google Patents
A kind of preparation method of the flexible transparent electrode based on ink print technique Download PDFInfo
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- CN105609216B CN105609216B CN201610036699.6A CN201610036699A CN105609216B CN 105609216 B CN105609216 B CN 105609216B CN 201610036699 A CN201610036699 A CN 201610036699A CN 105609216 B CN105609216 B CN 105609216B
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Abstract
The invention discloses a kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprises the following steps 1) doping PEDOT:The preparation configuration of PSS dispersion liquids is doped with poly- (3,4 Ethylenedioxy Thiophene) poly- (styrene sulfonic acid) dispersion liquid of 0.001~0.1mol/L complex acids, as PEDOT:PSS dispersion liquids, stirring, obtain sample dispersion liquid；2) rejection film of dispersion liquid is by step 1) in obtained sample dispersion liquid and glass or plastic substrate after removing residual processing through over cleaning, handled by sol evenning machine, obtain the PEDOT of the complexing acid doping of uniform fold substrate:PSS solid films；3) transparency electrode heat treatment is by step 2) in the solid membrane sample made, after being handled by heated at constant temperature, naturally cool to room temperature, obtain transparency electrode.
Description
Technical field
The present invention relates to organic optoelectronic technologic material field, specifically a kind of flexible and transparent based on ink print technique
The preparation method of electrode.
Background technology
Photoelectric device such as light emitting diode, solar cell, Trackpad etc. many fields it is extensive and important should
With.Photoelectric device requires that at least one transparency electrode can absorb or launch light to meet photoelectric device.Tin indium oxide is mesh
Preceding the most frequently used transparent electrode material, but the high request and tin indium oxide of the preparation of the scarcity of indium, indium tin oxide films are solid
Some fragility all greatly have impact on its following application.Therefore need badly at present and seek new transparent conductive material to replace oxidation
Indium tin.
Poly- in recent years (3,4- Ethylenedioxy Thiophenes)-poly- (styrene sulfonic acid) (PEDOT:PSS) in field of photoelectric devices
PEDOT of great interest, preparing:The characteristics of PSS transparency electrodes have the high grade of transparency and high mechanical flexibility, but its
Square resistance is generally greater than 100k Ω-1, this is substantially inferior to tin indium oxide.But to PEDOT:PSS carries out the acid after film forming
Square resistance can be made less than 100 Ω in post processing-1Transparency electrode, its splendid photoelectric characteristic made PEDOT:PSS
Research frontier as conducting polymer.
But to PEDOT:The step of PSS sour last handling process adds industrial production, time and complexity, so as to increase
Preparation cost is added.Therefore PEDOT is passed through:The regulation and control of PSS ink are directly obtained with stronger optical property and electric property
Transparency electrode there is extremely strong realistic meaning and commercial value.
The content of the invention
Present invention aim to address the PEDOT in the prior art, prepared:PSS transparency electrode steps are numerous and diverse, institute's used time
Between it is long, the problems such as prepare cost high and big complexity.
To realize that the technical scheme that the object of the invention is used is as described below, a kind of flexibility based on ink print technique is thoroughly
The preparation method of prescribed electrode, it is characterised in that comprise the following steps：
1) adulterate PEDOT:The preparation of PSS dispersion liquids
Configure poly- (3,4- Ethylenedioxy Thiophenes)-poly- (styrene sulphur doped with 0.001~0.1mol/L complex acids
Acid) dispersion liquid, as PEDOT:PSS dispersion liquids, stirring, obtain sample dispersion liquid；
2) rejection film of dispersion liquid
By step 1) in obtained sample dispersion liquid and the glass substrate after removing residual processing through over cleaning, at sol evenning machine
Reason, obtains the glass substrate of uniform fold sample dispersion liquid；
3) transparency electrode is heat-treated
By step 2) in the glass substrate made, after being handled by heated at constant temperature, naturally cool to room temperature, obtain transparent
Electrode.
Further, the step 1) in complex acid be selected from chloroplatinic acid (H2PtCl6·6H2O), gold chloride (HAuCl4·
4H2) or chlorine palladium acid (H O2PdCl4) in one or more.
Further, the step 1) in the cleaning of glass substrate be except residual processing procedure：By the glass base cleaned up
After piece is dried up with high pure nitrogen, it is placed in ozone processing instrument, is taken out after 15~60min of processing.
Further, the step 2) in sol evenning machine rotary speed be 1000~8000rpm, rotational time be 1~3min.
Further, the step 3) in heated at constant temperature temperature range be 100~180 DEG C, the heat time be 5~
120min。
Further, to the step 1) in the PEDOT that stirs:In PSS dispersion liquids, polar solvent is added, is stirred again
Mix, obtain sample dispersion liquid and carry out step 2) and step 3), obtain transparency electrode.The mixing time is 10~1440min, institute
State step 3) in mixing time be 10~1440min；The PEDOT:The volume hundred of the polar solvent added in PSS dispersion liquids
It is 0~15% to divide content.After polar solvent is added, transparency electrode performance can be lifted further
Further, the polar solvent is selected from one in ethylene glycol (EG), dimethyl sulfoxide (DMSO) (DMSO) or isopropanol (IPA)
Plant or several.
Further, the material of the flexible transparent electrode is in addition to rigid glass substrate, in addition to flexible plastic, transparent
Substrate；The plastic, transparent substrate is selected from polyethylene terephthalate substrate, PEN substrate or poly-
Acid imide substrate.
Further, the ink print preparation technology is except the step 2) in spin coating spin-coating method in addition to, in addition to slit type
Extrusion pressing type coating, inkjet printing or volume to volume typography and scraper preparation technology；The slit type extrusion pressing type coating, ink-jet are beaten
Print or volume to volume typography, are directly produced under the cryogenic conditions of room temperature~200 DEG C, without carrying out transparency electrode heat treatment step
Suddenly.
What deserves to be explained is, in PEDOT:A certain proportion of complex acid is added in PSS aqueous dispersion liquid, or is added
A certain proportion of polar solvent is added after a certain proportion of complex acid, so as to form brand-new transparency electrode ink.The ink system
It is standby go out electrode performance be greatly improved, and the ink can be by multiple inks printing technology direct high-volume in a short time
Ground is prepared with the low-resistance flexible transparency electrode of high transmission rate, without being post-processed or expensive vacuum or high temperature
Preparation method.
The PEDOT:The each component polar solvent volumn concentration added in PSS dispersion liquids is：0~15%.In detail
Volume proportion scheme have multiple combinations mode.Such as 0~15%EG, 0~15%DMSO and 0~15%IPA, each polar solvent can
Individually addition also combinable addition.
The solution have the advantages that unquestionable, the present invention has the following effects that：
The invention has the advantages that devising a kind of brand-new based on PEDOT:PSS ink formulations, can pass through ink print
Preparation technology, such as spin coating spin-coating method (spin coating), slit type extrusion pressing type coating (slot die coating), ink-jet are beaten
(inkjet printing) or volume to volume typography (roll-to-roll printing) etc. are printed, in room temperature or less than 200
Degree Celsius low temperature, the transparent electrode thin film with excellent photoelectric properties and mechanical flexibility is directly prepared in substrates of different, and
It need not further post-process, so as to reduce production stage and complexity, reduce production cost and reduce energy damage
Consumption, is that extensive preparation flexible transparent electrode and wearable photoelectric device provide reliable method.Importantly, utilizing this
Invent the transparency electrode performance prepared and obtain great lifting.
Brief description of the drawings
Fig. 1 is a kind of doping PEDOT:PSS transparent electrode structure schematic diagrames；
Fig. 2 is the light transmittance curve of the transparency electrode for preparing in 350~800nm wave-length coverages in embodiment 1~7；
Fig. 3 is the transparency electrode displaying figure for preparing in case study on implementation 3.
Embodiment
With reference to embodiment, the invention will be further described, but should not be construed above-mentioned subject area of the 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, all should be included within the scope of the present invention.
Embodiment 1：
PEDOT in embodiment:PSS is purchased from Heraeus companies of Germany, product type PH1000.Chloroplatinic acid (H2PtCl6·
6H2) and other solvents are purchased from Chemical Reagent Co., Ltd., Sinopharm Group O.
A kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) cleaning of glass substrate
1.1) size is numbered for 15mm × 15mm square glass substrate after splitting, by the glass base after numbering
Piece is placed on polyfluortetraethylecleaning cleaning support, is placed a stent into beaker, added into beaker 120ml deionized waters and 5%~
10% liquid detergent, the deionized water there was not glass substrate；
1.2) after beaker is sealed with masking foil, beaker is placed in the ultrasonic cleaner equipped with water and cleaned, institute
Ultrasonic time is stated for 10min, the supersonic frequency is 40kHz, the ultrasonic power is 80W；
1.3) after beaker is taken out, masking foil is opened, deionized water and the mixing liquid of liquid detergent is poured out, will be new
120ml deionized waters are placed in beaker, and beaker is covered to be placed in ultrasonic cleaner after masking foil and cleaned；The step
1.3) it is repeated 3 times；
1.4) after beaker is taken out, masking foil is opened, deionized water is poured out, 120ml acetone is placed in beaker, by beaker
It is placed in ultrasonic cleaner and is cleaned after covering masking foil, ultrasonic time is 10min；
1.5) after beaker is taken out, masking foil is opened, acetone is poured out, 150ml isopropanols is placed in beaker, beaker is covered
Lid masking foil, deposits cleaned glass substrate；
2) glass substrate remove residual processing
2.1) by the step 1.5) in after the glass substrate that is stored in isopropyl acetone takes out, dried up with high pure nitrogen；
2.2) dried glass substrate is placed in culture dish, culture dish is placed in UV ozone processing instrument, handled
Taken out after 15min；
3) adulterate PEDOT:The preparation of PSS dispersion liquids
3.1) a certain amount of chloroplatinic acid is weighed using electronic balance to be put into reagent bottle.
3.2) pipetted with pipettor respective amount PEDOT:PSS solution be put into reagent bottle make containing
The PEDOT of 0.035mol/L chloroplatinic acids:PSS solution.
3.3) magnetic stir bar is put into the platinum acid chloride solution reagent bottle prepared, and reagent bottle is placed on magnetic stirring apparatus
On, setting speed is 500~1000rpm, and timing 10-120min is stirred.
4) rejection film of dispersion liquid
By step 2.2) in the treated glass substrate of obtained ozone, be placed at the pivot of sol evenning machine, glass base
The μ L sample dispersion liquids of uniform fold 70~100 on piece, open sol evenning machine and carry out rejection film；The one-level rotating speed of sol evenning machine is set to
1500rpm, the time is 60s, and Second-Stage Rotating Speed is set to 4000rpm, and the time is 3s.
5) transparency electrode is heat-treated
By step 4) in the glass substrate made, be placed on constant temperature heating plate and toast 10min, the constant temperature heating plate
Temperature range is 120 DEG C；After glass substrate baking terminates, room temperature is naturally cooled to, transparency electrode is obtained.
Embodiment 2：
A kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) cleaning of glass substrate
1.1) size is numbered for 15mm × 15mm square glass substrate after splitting, by the glass base after numbering
Piece is placed on polyfluortetraethylecleaning cleaning support, is placed a stent into beaker, added into beaker 120ml deionized waters and 5%~
10% liquid detergent, the deionized water there was not glass substrate；
1.2) after beaker is sealed with masking foil, beaker is placed in the ultrasonic cleaner equipped with water and cleaned, institute
Ultrasonic time is stated for 10min, the supersonic frequency is 40kHz, the ultrasonic power is 80W；
1.3) after beaker is taken out, masking foil is opened, deionized water and the mixing liquid of liquid detergent is poured out, will be new
120ml deionized waters are placed in beaker, and beaker is covered to be placed in ultrasonic cleaner after masking foil and cleaned；The step
1.3) it is repeated 3 times；
1.4) after beaker is taken out, masking foil is opened, deionized water is poured out, 120ml acetone is placed in beaker, by beaker
It is placed in ultrasonic cleaner and is cleaned after covering masking foil, ultrasonic time is 10min；
1.5) after beaker is taken out, masking foil is opened, acetone is poured out, 150ml isopropanols is placed in beaker, beaker is covered
Lid masking foil, deposits cleaned glass substrate；
2) glass substrate remove residual processing
2.1) by the step 1.5) in after the glass substrate that is stored in isopropyl acetone takes out, dried up with high pure nitrogen；
2.2) dried glass substrate is placed in culture dish, culture dish is placed in UV ozone processing instrument, handled
Taken out after 15min；
3) adulterate PEDOT:The preparation of PSS dispersion liquids
3.1) a certain amount of chloroplatinic acid is weighed using electronic balance to be put into reagent bottle.
3.2) pipetted with pipettor respective amount PEDOT:PSS solution be put into reagent bottle make containing
The PEDOT of 0.035mol/L chloroplatinic acids:PSS solution.
3.3) magnetic stir bar is put into the platinum acid chloride solution reagent bottle prepared, and reagent bottle is placed on magnetic stirring apparatus
On, setting speed is 500~1000rpm, and timing 10-120min is stirred.
3.4) in step 3.3) to add percentage in obtained solution be 3% ethylene glycol (EG), 10~120min of timing enters
Row stirring, speed of agitator is 500~1000rpm.
4) rejection film of dispersion liquid
By step 2.2) in the treated glass substrate of obtained ozone, be placed at the pivot of sol evenning machine, glass base
The μ L sample dispersion liquids of uniform fold 70~100 on piece, open sol evenning machine and carry out rejection film；The one-level rotating speed of sol evenning machine is set to
1500rpm, the time is 60s, and Second-Stage Rotating Speed is set to 4000rpm, and the time is 3s.
5) transparency electrode is heat-treated
By step 4) in the glass substrate made, be placed on constant temperature heating plate and toast 10min, the constant temperature heating plate
Temperature range is 120 DEG C；After glass substrate baking terminates, room temperature is naturally cooled to, transparency electrode is obtained.
Embodiment 3：
A kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) cleaning of glass substrate
1.1) size is numbered for 15mm × 15mm square glass substrate after splitting, by the glass base after numbering
Piece is placed on polyfluortetraethylecleaning cleaning support, is placed a stent into beaker, added into beaker 120ml deionized waters and 5%~
10% liquid detergent, the deionized water there was not glass substrate；
1.2) after beaker is sealed with masking foil, beaker is placed in the ultrasonic cleaner equipped with water and cleaned, institute
Ultrasonic time is stated for 10min, the supersonic frequency is 40kHz, the ultrasonic power is 80W；
1.3) after beaker is taken out, masking foil is opened, deionized water and the mixing liquid of liquid detergent is poured out, will be new
120ml deionized waters are placed in beaker, and beaker is covered to be placed in ultrasonic cleaner after masking foil and cleaned；The step
1.3) it is repeated 3 times；
1.4) after beaker is taken out, masking foil is opened, deionized water is poured out, 120ml acetone is placed in beaker, by beaker
It is placed in ultrasonic cleaner and is cleaned after covering masking foil, ultrasonic time is 10min；
1.5) after beaker is taken out, masking foil is opened, acetone is poured out, 150ml isopropanols is placed in beaker, beaker is covered
Lid masking foil, deposits cleaned glass substrate；
2) glass substrate remove residual processing
2.1) by the step 1.5) in after the glass substrate that is stored in isopropyl acetone takes out, dried up with high pure nitrogen；
2.2) dried glass substrate is placed in culture dish, culture dish is placed in UV ozone processing instrument, handled
Taken out after 15min；
3) adulterate PEDOT:The preparation of PSS dispersion liquids
3.1) a certain amount of chloroplatinic acid is weighed using electronic balance to be put into reagent bottle.
3.2) pipetted with pipettor respective amount PEDOT:PSS solution be put into reagent bottle make containing
The PEDOT of 0.035mol/L chloroplatinic acids:PSS solution.
3.3) magnetic stir bar is put into the platinum acid chloride solution reagent bottle prepared, and reagent bottle is placed on magnetic stirring apparatus
On, 10~120min of timing is stirred, and setting speed is 500~1000rpm.
3.4) in step 3.3) percentage is added in obtained solution is 3% dimethyl sulfoxide (DMSO) (DMSO), timing 10~
120min is stirred, and rotating speed is 500~1000rpm.
4) rejection film of dispersion liquid
By step 2.2) in the treated glass substrate of obtained ozone, be placed at the pivot of sol evenning machine, glass base
The μ L sample dispersion liquids of uniform fold 70~100 on piece, open sol evenning machine and carry out rejection film；The one-level rotating speed of sol evenning machine is set to
1500rpm, the time is 60s, and Second-Stage Rotating Speed is set to 4000rpm, and the time is 3s.
5) transparency electrode is heat-treated
By step 4) in the glass substrate made, be placed on constant temperature heating plate and toast 10min, the constant temperature heating plate
Temperature range is 120 DEG C；After glass substrate baking terminates, room temperature is naturally cooled to, transparency electrode is obtained.
Embodiment 4：
A kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) cleaning of glass substrate
1.1) size is numbered for 15mm × 15mm square glass substrate after splitting, by the glass base after numbering
Piece is placed on polyfluortetraethylecleaning cleaning support, is placed a stent into beaker, added into beaker 120ml deionized waters and 5%~
10% liquid detergent, the deionized water there was not glass substrate；
1.2) after beaker is sealed with masking foil, beaker is placed in the ultrasonic cleaner equipped with water and cleaned, institute
Ultrasonic time is stated for 10min, the supersonic frequency is 40kHz, the ultrasonic power is 80W；
1.3) after beaker is taken out, masking foil is opened, deionized water and the mixing liquid of liquid detergent is poured out, will be new
120ml deionized waters are placed in beaker, and beaker is covered to be placed in ultrasonic cleaner after masking foil and cleaned；The step
1.3) it is repeated 3 times；
1.4) after beaker is taken out, masking foil is opened, deionized water is poured out, 120ml acetone is placed in beaker, by beaker
It is placed in ultrasonic cleaner and is cleaned after covering masking foil, ultrasonic time is 10min；
1.5) after beaker is taken out, masking foil is opened, acetone is poured out, 150ml isopropanols is placed in beaker, beaker is covered
Lid masking foil, deposits cleaned glass substrate；
2) glass substrate remove residual processing
2.1) by the step 1.5) in after the glass substrate that is stored in isopropyl acetone takes out, dried up with high pure nitrogen；
2.2) dried glass substrate is placed in culture dish, culture dish is placed in UV ozone processing instrument, handled
Taken out after 15min；
3) adulterate PEDOT:The preparation of PSS dispersion liquids
3.1) a certain amount of chloroplatinic acid is weighed using electronic balance to be put into reagent bottle.
3.2) pipetted with pipettor respective amount PEDOT:PSS solution be put into reagent bottle make containing
The PEDOT of 0.035mol/L chloroplatinic acids:PSS solution.
3.3) magnetic stir bar is put into the platinum acid chloride solution reagent bottle prepared, and reagent bottle is placed on magnetic stirring apparatus
On, 10~120min of timing is stirred, and setting speed is 500~1000rpm.
3.4) in step 3.3) to add percentage in obtained solution be 3%IPA, 10~120min of timing is stirred,
Rotating speed is 500~1000rpm.
4) rejection film of dispersion liquid
By step 2.2) in the treated glass substrate of obtained ozone, be placed at the pivot of sol evenning machine, glass base
The μ L sample dispersion liquids of uniform fold 70~100 on piece, open sol evenning machine and carry out rejection film；The one-level rotating speed of sol evenning machine is set to
1500rpm, the time is 60s, and Second-Stage Rotating Speed is set to 4000rpm, and the time is 3s.
5) transparency electrode is heat-treated
By step 4) in the glass substrate made, be placed on constant temperature heating plate and toast 10min, the constant temperature heating plate
Temperature range is 120 DEG C；After glass substrate baking terminates, room temperature is naturally cooled to, transparency electrode is obtained.
Embodiment 5：
A kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) cleaning of PET substrates
1.1) size is carried out for 15mm × 15mm square polyethylene terephthalate (PET) substrate after splitting
Numbering, the PET substrates after numbering are placed on polyfluortetraethylecleaning cleaning support, placed a stent into beaker, are added into beaker
120ml deionized waters and 5%~10% liquid detergent, the deionized water there were not PET substrates；
1.2) after beaker is sealed with masking foil, beaker is placed in the ultrasonic cleaner equipped with water and cleaned, institute
Ultrasonic time is stated for 10min, the supersonic frequency is 40kHz, the ultrasonic power is 80W；
1.3) after beaker is taken out, masking foil is opened, deionized water and the mixing liquid of liquid detergent is poured out, will be new
120ml deionized waters are placed in beaker, and beaker is covered to be placed in ultrasonic cleaner after masking foil and cleaned；The step
1.3) it is repeated 3 times；
1.4) after beaker is taken out, masking foil is opened, deionized water is poured out, 120ml acetone is placed in beaker, by beaker
It is placed in ultrasonic cleaner and is cleaned after covering masking foil, ultrasonic time is 10min；
1.5) after beaker is taken out, masking foil is opened, acetone is poured out, 150ml isopropanols is placed in beaker, beaker is covered
Lid masking foil, deposits cleaned PET substrates；
2) PET substrates remove residual processing
2.1) by the step 1.5) in be stored in after PET substrates in isopropyl acetone take out, dried up with high pure nitrogen；
2.2) dried PET substrates are placed in culture dish, culture dish is placed in UV ozone processing instrument, handled
Taken out after 3min；
3) adulterate PEDOT:The preparation of PSS dispersion liquids
3.1) a certain amount of chloroplatinic acid is weighed using electronic balance to be put into reagent bottle.
3.2) pipetted with pipettor respective amount PEDOT:PSS solution be put into reagent bottle make containing
The PEDOT of 0.035mol/L chloroplatinic acids:PSS solution.
3.3) magnetic stir bar is put into the platinum acid chloride solution reagent bottle prepared, and reagent bottle is placed on magnetic stirring apparatus
On, setting speed is 500~1000rpm, and 10-120min of timing are stirred.
4) rejection film of dispersion liquid
By step 2.2) in the treated PET substrates of obtained ozone, be placed at the pivot of sol evenning machine, PET substrates
The upper μ L sample dispersion liquids of uniform fold 70~100, open sol evenning machine and carry out rejection film；The one-level rotating speed of sol evenning machine is set to
1500rpm, the time is 60s, and Second-Stage Rotating Speed is set to 4000rpm, and the time is 3s.
5) transparency electrode is heat-treated
By step 4) in the PET substrates made, be placed on constant temperature heating plate and toast 10min, the constant temperature heating plate
Temperature range is 120 DEG C；After the baking of PET substrates terminates, room temperature is naturally cooled to, the transparency electrode of flexibility is obtained.
Embodiment 6：
A kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) cleaning of glass substrate
1.1) size is numbered for 15mm × 15mm square glass substrate after splitting, by the glass base after numbering
Piece is placed on polyfluortetraethylecleaning cleaning support, is placed a stent into beaker, added into beaker 120ml deionized waters and 5%~
10% liquid detergent, the deionized water there was not glass substrate；
1.2) after beaker is sealed with masking foil, beaker is placed in the ultrasonic cleaner equipped with water and cleaned, institute
Ultrasonic time is stated for 10min, the supersonic frequency is 40kHz, the ultrasonic power is 80W；
1.3) after beaker is taken out, masking foil is opened, deionized water and the mixing liquid of liquid detergent is poured out, will be new
120ml deionized waters are placed in beaker, and beaker is covered to be placed in ultrasonic cleaner after masking foil and cleaned；The step
1.3) it is repeated 3 times；
1.4) after beaker is taken out, masking foil is opened, deionized water is poured out, 120ml acetone is placed in beaker, by beaker
It is placed in ultrasonic cleaner and is cleaned after covering masking foil, ultrasonic time is 10min；
1.5) after beaker is taken out, masking foil is opened, acetone is poured out, 150ml isopropanols is placed in beaker, beaker is covered
Lid masking foil, deposits cleaned glass substrate；
2) glass substrate remove residual processing
2.1) by the step 1.5) in after the glass substrate that is stored in isopropyl acetone takes out, dried up with high pure nitrogen；
2.2) dried glass substrate is placed in culture dish, culture dish is placed in UV ozone processing instrument, handled
Taken out after 15min；
3) adulterate PEDOT:The preparation of PSS dispersion liquids
3.1) gold chloride for weighing 20mg using electronic balance is put into reagent bottle.
3.2) pipetted with pipettor respective amount PEDOT:PSS solution, which is put into reagent bottle, makes 0.01mol/L's
PEDOT containing gold chloride:PSS solution.
3.3) magnetic stir bar is put into the platinum acid chloride solution reagent bottle prepared, and reagent bottle is placed on magnetic stirring apparatus
On, setting speed is 500~1000rpm, and 10~120min of timing is stirred.
4) rejection film of dispersion liquid
By step 2.2) in the treated glass substrate of obtained ozone, be placed at the pivot of sol evenning machine, glass base
The μ L sample dispersion liquids of uniform fold 70~100 on piece, open sol evenning machine and carry out rejection film；The one-level rotating speed of sol evenning machine is set to
1500rpm, the time is 60s, and Second-Stage Rotating Speed is set to 4000rpm, and the time is 3s.
5) transparency electrode is heat-treated
By step 4) in the glass substrate made, be placed on constant temperature heating plate and toast 10min, the constant temperature heating plate
Temperature range is 120 DEG C；After glass substrate baking terminates, room temperature is naturally cooled to, transparency electrode is obtained.
Embodiment 7：
A kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) cleaning of glass substrate
1.1) size is numbered for 15mm × 15mm square glass substrate after splitting, by the glass base after numbering
Piece is placed on polyfluortetraethylecleaning cleaning support, is placed a stent into beaker, added into beaker 120ml deionized waters and 5%~
10% liquid detergent, the deionized water there was not glass substrate；
1.2) after beaker is sealed with masking foil, beaker is placed in the ultrasonic cleaner equipped with water and cleaned, institute
Ultrasonic time is stated for 10min, the supersonic frequency is 40kHz, the ultrasonic power is 80W；
1.3) after beaker is taken out, masking foil is opened, deionized water and the mixing liquid of liquid detergent is poured out, will be new
120ml deionized waters are placed in beaker, and beaker is covered to be placed in ultrasonic cleaner after masking foil and cleaned；The step
1.3) it is repeated 3 times；
1.4) after beaker is taken out, masking foil is opened, deionized water is poured out, 120ml acetone is placed in beaker, by beaker
It is placed in ultrasonic cleaner and is cleaned after covering masking foil, ultrasonic time is 10min；
1.5) after beaker is taken out, masking foil is opened, acetone is poured out, 150ml isopropanols is placed in beaker, beaker is covered
Lid masking foil, deposits cleaned glass substrate；
2) glass substrate remove residual processing
2.1) by the step 1.5) in after the glass substrate that is stored in isopropyl acetone takes out, dried up with high pure nitrogen；
2.2) dried glass substrate is placed in culture dish, culture dish is placed in UV ozone processing instrument, handled
Taken out after 15min；
3) adulterate PEDOT:The preparation of PSS dispersion liquids
3.1) chloroplatinic acid for the gold chloride and 50mg for weighing 20mg using electronic balance is put into reagent bottle.
3.2) pipetted with pipettor respective amount PEDOT:PSS solution, which is put into reagent bottle, to be made containing 0.01mol/
The PEDOT of L gold chlorides and 0.02mol/L chloroplatinic acids:PSS solution.
3.3) magnetic stir bar is put into the platinum acid chloride solution reagent bottle prepared, and reagent bottle is placed on magnetic stirring apparatus
On, setting speed is 500~1000rpm, and 10~120min of timing is stirred.
4) rejection film of dispersion liquid
By step 2.2) in the treated glass substrate of obtained ozone, be placed at the pivot of sol evenning machine, glass base
The μ L sample dispersion liquids of uniform fold 70~100 on piece, open sol evenning machine and carry out rejection film；The one-level rotating speed of sol evenning machine is set to
1500rpm, the time is 60s, and Second-Stage Rotating Speed is set to 4000rpm, and the time is 3s.
5) transparency electrode is heat-treated
By step 4) in the glass substrate made, be placed on constant temperature heating plate and toast 10min, the constant temperature heating plate
Temperature range is 120 DEG C；After glass substrate baking terminates, room temperature is naturally cooled to, transparency electrode is obtained.
Result of the test
The transparency electrode data summary table prepared in case study on implementation
Claims (8)
1. a kind of preparation method of the flexible transparent electrode based on ink print technique, it is characterised in that comprise the following steps：
1) adulterate PEDOT:The preparation of PSS dispersion liquids
Configure poly- (3,4- Ethylenedioxy Thiophenes)-poly- (styrene sulfonic acid) point doped with 0.001~0.1mol/L complex acids
Dispersion liquid, as PEDOT:PSS dispersion liquids, stirring, obtain sample dispersion liquid；
The complex acid is selected from chloroplatinic acid (H2PtCl6·6H2O), gold chloride (HAuCl4·4H2) or chlorine palladium acid (H O2PdCl4) in
One or more；
2) rejection film of dispersion liquid
By step 1) in obtained sample dispersion liquid and the glass substrate after removing residual processing through over cleaning, handled by sol evenning machine,
Obtain the glass substrate of uniform fold sample dispersion liquid；
3) transparency electrode is heat-treated
By step 2) in the glass substrate made, after being handled by heated at constant temperature, naturally cool to room temperature, obtain transparent electricity
Pole.
2. a kind of preparation method of flexible transparent electrode based on ink print technique according to claim 1, its feature
It is：The step 1) in the cleaning of glass substrate be except residual processing procedure：By the glass substrate High Purity Nitrogen cleaned up
After air-blowing is dry, it is placed in ozone processing instrument, is taken out after 15~60min of processing.
3. a kind of preparation method of flexible transparent electrode based on ink print technique according to claim 1, its feature
It is：The step 2) in sol evenning machine rotary speed be 1000~8000rpm, rotational time be 1~3min.
4. a kind of preparation method of flexible transparent electrode based on ink print technique according to claim 1, its feature
It is：The step 3) in heated at constant temperature temperature range be 100~180 DEG C, the heat time be 5~120min.
5. a kind of preparation method of flexible transparent electrode based on ink print technique according to claim 1, its feature
It is：To the step 1) in the PEDOT that stirs:In PSS dispersion liquids, polar solvent is added, is again stirring for, obtains sample
Dispersion liquid carries out step 2) and step 3), obtain transparency electrode；The PEDOT:The body of the polar solvent added in PSS dispersion liquids
Product percentage composition is 0~15%.
6. a kind of preparation method of flexible transparent electrode based on ink print technique according to claim 5, its feature
It is：The polar solvent is selected from the one or more in ethylene glycol (EG), dimethyl sulfoxide (DMSO) (DMSO) or isopropanol (IPA).
7. a kind of preparation method of flexible transparent electrode based on ink print technique according to claim 1, its feature
It is：The material of the flexible transparent electrode is in addition to rigid glass substrate, in addition to flexible plastic, transparent substrate；The modeling
Expect that transparent substrate is selected from polyethylene terephthalate substrate, PEN substrate or polyimide base film.
8. a kind of preparation method of flexible transparent electrode based on ink print technique according to claim 1, its feature
It is：The ink print preparation technology is except the step 2) in spin coating spin-coating method in addition to, in addition to slit type extrusion pressing type coating,
Inkjet printing or volume to volume typography and scraper preparation technology；The slit type extrusion pressing type coating, inkjet printing or volume to volume
Typography, is directly produced under the cryogenic conditions of room temperature~200 DEG C, without carrying out transparency electrode heat treatment step.
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