CN104934540B - The highly conductive PEDOT of one kind modeling base:PSS membrane electrodes and preparation method and application - Google Patents
The highly conductive PEDOT of one kind modeling base:PSS membrane electrodes and preparation method and application Download PDFInfo
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Abstract
The present invention is a kind of highly conductive PEDOT of modeling base:A kind of PSS membrane electrodes and preparation method and application, it is proposed that highly conductive, flexible, transparent PEDOT:The preparation of PSS membrane electrodes preparation method and flexible organic solar batteries.Its step is：PET substrate is cleaned, prepares the PEDOT containing fluorine surfactant and methanol mixing：PSS spin coating liquid, spin coating, pyrovinic acid solution acid treatment, then through 120 DEG C of thermal annealings, so as to form highly conductive PEDOT：PSS films.With highly conductive PEDOT：PSS films can assemble flexible organic solar batteries.Due to mixing PEDOT：Fluorine surfactant is added in PSS spin coating liquid, solves PEDOT:The PSS aqueous solution difficult point that wellability is poor on the plastic substrate and conductance is poor.Conductance is prepared at 130 DEG C and is up to 3560S cm‑1PEDOT:PSS films.Preparation process is simple to operate, and securely and reliably, while environmental pollution is few.
Description
【Technical field】
The present invention relates to highly conductive, flexible and transparent poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid (PEDOT:
PSS) film and its application on flexible organic solar batteries, are generated more particularly, to a kind of alkyd coprocessing
The polymeric transparent film PEDOT of highly conductive, strong mechanical tenacity:PSS, and using this film as flexible and transparent conductive electrode
Organic solar batteries development.
【Background technology】
It is a kind of cheap, solution-processible, transparent and conducting polymer thin film, poly- (3,4-ethylene dioxythiophene)：Poly- (benzene
Ethene) (abbreviation PEDOT：PSS) film, battery, luminous and display device boundary layer and electrode have been widely used in
Material [1-4].PEDOT：PSS films have the high grade of transparency, high mechanical tenacity and excellent heat endurance in visible-range
And environmental stability.However, PSS is a kind of insulator, cause untreated PEDOT：The conductance of PSS films is very low (low
In 1.0S cm-1)[4].Further, since PEDOT crystallinity is not high, the efficiency of transmission and collection efficiency in hole are hindered.It is and good
Good polymer electrode material requirements PEDOT：PSS has higher electric conductivity.
At present, document report is on highly conductive PEDOT:The preparation method of PSS films mainly has：(1) alcohol is handled, including
Methanol, ethanol, ethylene glycol etc.；(2) acid treatment, including sulfuric acid, pyrovinic acid, oxalic acid etc..The PEDOT of alcohol processing:PSS films
Conductance is not general high, no more than 2000S cm-1[4-6].And sulfuric acid or pyrovinic acid acidification PEDOT:PSS can be formed
High conductivity thin polymer film, conductance are respectively 4380S cm-1[5] and 3065S cm-1[2], then, prepared by the above method
Film prepared in clear glass substrate, preparation temperature be 140~160 DEG C, making substrate with plastics can also form
PEDOT:PSS high conductivity thin polymer films, and plastic-substrates have extremely strong hydrophobicity, PEDOT:The PSS aqueous solution is difficult to
Spread out in plastic-substrates；Meanwhile (140-160 DEG C) easily chemically react these strong acid with plastic-substrates at high temperature, cause
The transparency variation of film.
【Bibliography】
[1]Y.H.Kim,C.Sachse,M.L.Machala,C.May,L.M.-Meskamp and K.Leo,
Adv.Funct.Mater.,2011,21,1076.
[2]Y.J.Xia,K.Sun and J.Ouyang,Adv.Mater.2012,24,2436.
[3]D.Alemu,H.-Yu Wei,K.-C.Hod and C.-W.Chu,Energy Environ.Sci.,2012,
5,9662.
[4]W.F Zhang,B.F.Zhao,Z.C.He,X.M.Zhao,H.T.Wang,S.F.Yang,H.B Wu and
Y.Cao,Energy Environ.Sci.,2013,6,19566.
[5]N.Kim,S.Kee,S.H.Lee,B.H.Lee,Y.H.Kahng,Y.-R.Jo,B.-J.Kim and K.Lee,
Adv.Mater.,2014,26,2268.
【The content of the invention】
Based on above-mentioned technical background, highly conductive PEDOT is prepared as substrate using plastics it is an object of the invention to provide a kind of:
The preparation method of PSS films.It this method solve PEDOT:PSS wellability differences and the problem of poorly conductive on the plastic substrate.
Its operating procedure is simple, and experimental cost is cheap, while it is few to test byproduct environmental pollution；In addition, prepared PEDOT:PSS
The overall structure of film is clear, and size distribution is uniform, can be efficiently applied to the organic assembly of flexibility, such as develops flexible organic
Solar cell, have a good application prospect.
To achieve the above object, the present invention uses polyethylene terephthalate (PET) plastics as substrate, in PEDOT:
0.5vol.% fluorine-containing surfactant Zonyl FS-300 are added in the PSS aqueous solution, successfully overcome PEDOT:PSS is being moulded
Expect the problem of wellability difference on substrate；By two-step method, i.e., after first methyl alcohol process pyrovinic acid handle, and controlling reaction temperature and
Time, so as to be prepared for highly conductive PEDOT in PET:PSS films.Finally, by the PEDOT of acid alcohol processing:PSS is soft
Property transparent membrane as anode, assemble flexible and efficient organic solar batteries.
The specific preparation flow and technique of membrane electrode of the present invention are as follows：
(1) substrate is cleaned
Choose PET substrate and successively pass through cleaning agent, deionized water, acetone, isopropanol supersound process, 15 points every time
Clock, every kind of solvent are handled 2 times, then handled within 15 minutes through UV ozone room；
(2) mixing PEDOT is prepared：PSS spin coating liquid
In the PEDOT that content is 6%：In the PSS aqueous solution (Clevios PH1000), the fluorine-containing table of 0.5% volume is mixed
Face activating agent Zonyl FS-300 and 6% volume pure methanol, stir 24 hours；
(3) spin coating and methyl alcohol process
PEDOT is prepared with 2500 revolutions per seconds of rotating speed spin coating in PET substrate：PSS films.Spin-coating time is 60 seconds,
Then, film is immersed in pure methanol, rinsing three times, is taken out sample, then, is heat-treated 10 minutes on hot plate, temperature is
120℃；
(4) pyrovinic acid solution acid treatment
Match 8M pyrovinic acid solution.By PEDOT：PSS films are placed on hot plate, and temperature is 130 DEG C.It is added dropwise 8M's
Pyrovinic acid solution, the surface of whole film is paved with, be heat-treated 5 minutes.Then, sample is taken out, is washed with deionized three times,
120 DEG C of thermal annealings 10 minutes again, so as to form highly conductive PEDOT：PSS films.
It is PET base/PEDOT to prepare flexible organic solar energy cell structure with the present invention:PSS electrodes/PEDOT:
PSS (Clevios P VP 4083) cushion/P3HT:PCBM active layers/Ca/Al electrode layers.Wherein in PET substrate
PEDOT:PSS electrode film layers thickness is 65nm；
In PEDOT:PEDOT on PSS electrode film layers:PSS buffer thin film thickness degree is 30nm；
In PEDOT:P3HT on PSS buffer thin film layers:PCBM active layer thickness is 200nm；
In P3HT:Ca and Al electrodes on PCBM active layers, the thickness of Ca and Al electrodes is 20nm and 100nm respectively；
The thickness of PET substrate is 120 μm；
Described highly conductive PEDOT:PSS flexible electrodes are Clevios PH1000 types；
Described PEDOT:PSS buffer thin film layers are the types of Clevios P VP 4083.
Fig. 1 c are the structural representations of this device.
It is with the step of preparing flexible organic solar batteries of the invention：
1st, in PET substrate, highly conductive PEDOT is formed：PSS films.
(a) substrate is cleaned
Choose PET substrate and successively pass through cleaning agent, deionized water, acetone, isopropanol supersound process, 15 points every time
Clock, every kind of solvent are handled 2 times.Then handled within 15 minutes through UV ozone room.
(b) mixing PEDOT is prepared：PSS spin coating liquid
In the PEDOT that content is 6%：In the PSS aqueous solution (Clevios PH1000), the fluorine-containing table of 0.5% volume is mixed
Face activating agent Zonyl FS-300 and 6% volume methanol, stir 24 hours；
(c) spin coating and methyl alcohol process
PEDOT is prepared with 2500 revolutions per seconds of rotating speed spin coating in PET substrate：PSS films.Spin-coating time is 60 seconds,
Then, film is immersed in pure methanol, rinsing three times, is taken out sample, then, is heat-treated 10 minutes on hot plate, temperature is
120℃；
(d) pyrovinic acid solution acid treatment
Match 8M pyrovinic acid solution.By PEDOT：PSS films are placed on hot plate, and temperature is 130 DEG C.It is added dropwise 8M's
Pyrovinic acid solution, the surface of whole film is paved with, be heat-treated 5 minutes.Then, sample is taken out, is washed with deionized three times,
120 DEG C of thermal annealings 10 minutes again, so as to form highly conductive PEDOT：PSS films.
2nd, in PEDOT：PEDOT is formed on PSS films：PSS cushions
With 5000 revolutions per seconds of rotating speed spin coating PEDOT：PSS (Clevios P VP 4083) solution, rotational time are 60 seconds,
Anode buffer layer is prepared, 120 DEG C are heat-treated 10 minutes.
3rd, then, on anode buffer layer spin coating P3HT and PCBM blend solution, solvent is o-dichlorohenzene, and rotating speed is
600 revolutions per seconds, the time is 60 seconds.
4th, then, solvent anneal and thermal annealing are carried out.Then, evaporation negative electrode Ca and Al, it is flexible so as to have developed
Organic solar batteries.
Film characterization and device detection
By preparation-obtained PEDOT：PSS films have carried out transmission spectrum, X-ray diffraction, atomic force electron microscope point
Analysis.The instrument that X-ray diffraction (XRD) analysis uses is D8Advance, and condition determination is the scanning of 0.001 °/step.Atomic force electronics
Microscope is carried out under 40KV voltage and 50mA electric current.
The flexible organic solar batteries assembled are subjected to photoelectric properties test.The device of current density (J-V)
Measurement is the source measuring unit progress of Keithley 236 in a computer control.Device characterization is to illuminate the ring under AM1.5G
Carried out in the atmosphere of border, with 100mW cm-2Xenon lamp based on solar simulator (coming from Newport Co., LTD.).
The DSP lock-in amplifiers SR830 of external quantum efficiency and Stamford research system model adds the monochromatic suits of WDG3 and 500W xenon lamps
Measurement.The intensity of the light of every kind of wavelength and the monocrystalline Silicon photrouics of standard are calibrated.
These analysis results are listed in accompanying drawing respectively.
It is in place of advantages of the present invention and characteristic：
(1) present invention is using the PEDOT for mixing fluorocarbon surfactant Zonyl FS-300:The PSS aqueous solution, after film forming again
Alkyd solution (methanol/pyrovinic acid) facture, by controlling concentration, the temperature and time of reaction solution, in PET substrate
On prepare PEDOT:PSS Thin film conductive rates are up to 3560S cm-1。
(2) PEDOT is overcome:The PSS aqueous solution infiltrates the difficult point of difference on the plastic substrate.
(3) PEDOT that the present invention obtains:The good mechanical property of PSS films, and PEDOT:PSS films it is clear in structure,
It is neat and orderly.With traditional alcohol processing flexible organic solar batteries compared with, alcohol acid treatment it is flexible organic
The energy conversion efficiency of solar cell has been obviously improved 11.7%.And remained in an atmosphere after 100 times significantly bend
About 80% performance is kept, is had a extensive future.
(4) whole preparation process is simple to operate, and securely and reliably, while environmental pollution is few.
【Brief description of the drawings】
Fig. 1 PET substrates；
The flexible organic solar batteries profiles of Fig. 2；
The structural representation of the flexible organic solar batteries of Fig. 3.
The PEDOT of Fig. 4 alkyd coprocessing:The surface topography of PSS films.
Fig. 5 is untreated, alcohol processing, the PEDOT of acid treatment and alkyd coprocessing:The XRD of PSS films.
The J-V curves (a) of Fig. 6 planes and flexible device
The external quantum efficiency (b) of Fig. 7 planes and flexible device.
【Embodiment】
Below by embodiment it will be better understood that the present invention.
Embodiment 1
PEDOT：The preparation flow and technique of PSS membrane electrodes and device are as follows：
(1) pretreatment of PET substrate
The commercial PET that thickness is 120 μm is cut into 1.5cm × 1.5cm square structure.Cleaning agent is used successively,
Deionized water, ethylene glycol are cleaned by ultrasonic, and the impurity of PET substrate is cleaned up.It is standby with hair-dryer drying in air
With.In this experimental procedure, it is 15 minutes often to walk sonication treatment time in cleaning process, and each solvent supersonic is twice.
(2) alcohol processing PEDOT:PSS films
In PEDOT:0.5vol.% fluorine-containing surfactant Zonyl FS-300,6% body are added in PSS solution successively
Long-pending methanol, at least stir 24 hours, improve PEDOT:The wellability of the PSS aqueous solution on the plastic substrate.1.5cm ×
Spin coating PEDOT in 1.5cm PET substrate:PSS solution, 5000 revolutions per seconds of rotating speed, time are 60 seconds, prepare PEDOT:PSS
Film, 120 DEG C are heat-treated 10 minutes.
(3) acid treatment PEDOT:PSS films
The preparation of pyrovinic acid solution：The aqueous solution of 8M pyrovinic acid is configured, adds magnetic stir bar, stirring 24 is small
When.
By PEDOT：PSS films are placed on hot plate, and temperature is 130 DEG C.50ml pyrovinic acid solution, drop are inhaled with dropper
In PEDOT：On PSS films, ensure that solution is paved with the surface of whole film, be heat-treated 5 minutes.Hydrogen ion in acid is born with PSS
Ions binding causes PEDOT and PSS Coulomb force to disappear into the PSSH of neutrality.Then, with tweezers take out sample, be put into from
In beaker in sub- water, washing three times, removes substantial amounts of nonconducting PSS.Take out sample, then 120 DEG C of thermal annealings 10 minutes, from
And form highly conductive, flexible and transparent PEDOT：PSS films.It is clear that from AFM (Fig. 2)
PEDOT nano thread structures, high-sequential.
Embodiment 2
With PEDOT:PSS is the assembling of the flexible organic solar batteries of electrode
Flexible organic solar energy cell structure is plastic-substrates/PEDOT:PSS electrodes/PEDOT:PSS(Clevios
P VP 4083) cushion/P3HT:PCBM active layers/Ca/Al, electrode area 11.0mm2。
On 1.5cm × 1.5cm plastics, alcohol acid treatment forms highly conductive PEDOT PSS films (referring to embodiment 1).
Remove half PEDOT with the tweezers and blade of moistening:PSS films, then, spin coating PEDOT：PSS(Clevios P VP 4083)
The aqueous solution, prepare 30nm PEDOT：PSS anode buffer layers, 120 DEG C are heat-treated 10 minutes.Then, in PEDOT PSS anodes
Spin coating P3HT and PCBM o-dichlorohenzene blend solution (1 on cushion:1 weight ratio, 34mg mL-1P3HT：PCBM), rotating speed
For 600 revolutions per seconds, the time is 60 seconds.Wet P3HT：PCBM blend films are placed in semi-enclosed small glass culture dish and carry out one
The solvent anneal of individual hour, the color of active layer is from light yellow change laking.Then, in glove box, 150 DEG C of thermal annealings 10
Minute.Finally, 10-4Under Pa vacuum, thermal evaporation 20nm Ca and 120nm Al (unencapsulated) are flexible so as to complete
The assembling of organic solar batteries.
Claims (2)
1. the highly conductive PEDOT of one kind modeling base:The preparation method of PSS films, it is characterised in that step is：
（1）Clean substrate
Choose PET substrate and successively pass through cleaning agent, deionized water, acetone, isopropanol supersound process, 15 minutes every time, often
Kind solvent is handled 2 times, is then handled within 15 minutes through UV ozone room；
（2）Prepare mixing PEDOT：PSS spin coating liquid
In the PEDOT that content is 6%：In the PSS aqueous solution, mix 0.5% volume fluorine-containing surfactant Zonyl FS-300 and
The pure methanol of 6% volume, stir 24 hours；Described PEDOT：The PSS aqueous solution is Clevios PH1000 types;
（3）Spin coating and methyl alcohol process
PEDOT is prepared with 2500 revolutions per seconds of rotating speed spin coating in PET substrate：PSS films, spin-coating time are 60 seconds, so
Afterwards, film is immersed in pure methanol, rinsing three times, is taken out sample, then, is heat-treated 10 minutes on hot plate, temperature 120
℃；
（4）Pyrovinic acid solution acid treatment
8M pyrovinic acid solution is matched, by PEDOT：PSS films are placed on hot plate, and temperature is 130 DEG C, and 8M methyl is added dropwise
Sulfonic acid solutions, the surface of whole film is paved with, is heat-treated 5 minutes, then, takes out sample, be washed with deionized three times, then
120 DEG C of thermal annealings 10 minutes, so as to form highly conductive PEDOT：PSS films.
A kind of 2. highly conductive PEDOT of modeling base prepared by method with described in claim 1:PSS film preparations it is flexible it is organic too
The preparation method of positive energy battery, the flexible organic solar energy cell structure is by polyethylene terephthalate (PET)
Plastic-substrates, thickness are 120 μm;, highly conductive Clevios PH1000 PEDOT:PSS flexible electrodes, thickness 65nm,
Clevios P VP 4083 PEDOT:PSS buffer thin film layers, thickness are 30nm, and P3HT is provided with buffer thin film layer:PCBM
Active layer, its thickness are 200nm, are provided with Ca and Al electrodes on active layer, the thickness of Ca and Al electrodes be respectively 20nm and
100nm, it is characterised in that preparation process is as follows：
1）, in PET substrate, form highly conductive PEDOT：PSS films
（a）Clean substrate
Choose PET substrate and successively pass through cleaning agent, deionized water, acetone, isopropanol supersound process, 15 minutes every time, often
Kind solvent is handled 2 times, is then handled within 15 minutes through UV ozone room；
（b）Prepare mixing PEDOT：PSS spin coating liquid
In the PEDOT for the Clevios PH1000 that content is 6%：In the PSS aqueous solution, the fluorine-containing surfactants of 0.5% volume are mixed
Agent Zonyl FS-300 and 6% volume methanol, stir 24 hours；
（c）Spin coating and methyl alcohol process
PEDOT is prepared with 2500 revolutions per seconds of rotating speed spin coating in PET substrate：PSS films, spin-coating time are 60 seconds, so
Afterwards, film is immersed in pure methanol, rinsing three times, is taken out sample, then, is heat-treated 10 minutes on hot plate, temperature 120
℃；
（d）Pyrovinic acid solution acid treatment
8 M pyrovinic acid solution is matched, by PEDOT：PSS films are placed on hot plate, and temperature is 130 DEG C.8M first is added dropwise
Base sulfonic acid solutions, the surface of whole film is paved with, is heat-treated 5 minutes, then, takes out sample, be washed with deionized three times, then
120 DEG C of thermal annealings 10 minutes, so as to form highly conductive PEDOT：PSS films；
2）, in PEDOT：PEDOT is formed on PSS films：PSS cushions
With 5000 revolutions per seconds of rotating speed spin coating Clevios P VP 4083 PEDOT：PSS solution, rotational time are 60 seconds, are prepared
Anode buffer layer, 120 DEG C are heat-treated 10 minutes；
3）, then, spin coating P3HT and PCBM blend solution on anode buffer layer, solvent is o-dichlorohenzene, rotating speed 600
Revolutions per second, the time is 60 seconds；
4）, then, carry out solvent anneal and thermal annealing, then, evaporation negative electrode Ca and Al is flexible organic so as to have developed
Solar cell.
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| CN105914047B (en) * | 2016-04-14 | 2018-06-22 | 南京邮电大学 | A kind of flexible transparent film electrode and preparation method thereof |
| NO20161150A1 (en) | 2016-07-11 | 2018-01-12 | Inst Energiteknik | Organic-inorganic hybrid material and method for silicon surface passivation |
| CN106159109A (en) * | 2016-09-13 | 2016-11-23 | Tcl集团股份有限公司 | A kind of QLED and preparation method thereof |
| CN106299134B (en) * | 2016-10-21 | 2018-09-07 | 华中科技大学 | A kind of patterned combined solar battery and its colored solar battery module |
| CN109013250A (en) * | 2018-05-28 | 2018-12-18 | 重庆大学 | A method of improving electrically conductive ink uniformity and adhesive force |
| CN109360885A (en) * | 2018-08-16 | 2019-02-19 | 江西科技师范大学 | PEDOT:PSS/ce-MoS2The preparation method of film |
| CN110660912A (en) * | 2019-09-19 | 2020-01-07 | 深圳第三代半导体研究院 | Preparation method of flexible resistive random access memory device based on perovskite |
| CN112635671B (en) * | 2020-12-19 | 2022-09-06 | 南京理工大学 | Resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) based on femtosecond laser modification |
| CN113643855A (en) * | 2021-06-18 | 2021-11-12 | 南京邮电大学 | Preparation method and application of flexible transparent electrode |
| CN114320133B (en) * | 2022-01-27 | 2023-09-22 | 兰州大学 | Smart window and preparation method thereof |
| CN118366722A (en) * | 2024-04-03 | 2024-07-19 | 启东桢材新材料科技有限公司 | Method for preparing large-area flexible transparent conductive film by solution shearing method and application thereof |
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