CN104934540A - Plastic-based high-conductivity PEDOT: PSSS film electrode, preparation method and application thereof - Google Patents
Plastic-based high-conductivity PEDOT: PSSS film electrode, preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a plastic-based high-conductivity PEDOT: PSSS film electrode, a preparation method and an application thereof. The invention provides a preparation method for the high-conductivity, flexible, and transparent PEDOT: PSS film electrode and the preparation of a bendable organic solar cell. The method includes: cleaning a PET plastic substrate, preparing a PEDOT: PSS spin coating liquid containing a mixture of fluorinated surfactants and methanol, performing spin coating, performing acid treatment of a methanesulfonic acid solution, and performing thermal annealing at 120 DEG C to form the high-conductivity PEDOT: PSS film. The bendable organic solar cell can be assembled with the high-conductivity PEDOT: PSS film. The fluorinated surfactants are added into the mixed PEDOT: PSS spin coating liquid so that the difficulties of poor immersion and poor conductivity of the PEDOT: PSS water solution on the plastic substrate are solved; the PEDOT: PSS film with the conductivity of 3560S cm<-1> is prepared at 130 DEG C; the preparation process and operation are simple, safety and reliability are realized, and the environmental pollution is less.
Description
[technical field]
The present invention relates to high connductivity, flexible and transparent poly-(3,4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT:PSS) film and its application on flexible organic solar batteries, especially relate to a kind of alkyd coprocessing and generate high connductivity, the polymeric transparent film PEDOT:PSS of strong mechanical tenacity, and with the development of this film for the organic solar batteries of flexible and transparent conductive electrode.
[background technology]
A kind of cheapness, solution-processible, transparent and conducting polymer thin film, poly-(3,4-ethylenedioxy thiophene): poly-(styrene) (being called for short PEDOT:PSS) film, be widely used in battery, the boundary layer of luminescence and display device and electrode material [1-4].PEDOT:PSS film has the high grade of transparency in visible-range, high mechanical tenacity and excellent thermal stability and environmental stability.But PSS is a kind of insulator, cause the conductance of untreated PEDOT:PSS film very low (lower than 1.0S cm
-1) [4].In addition, because the degree of crystallinity of PEDOT is not high, efficiency of transmission and the collection efficiency in hole is hindered.And good polymer electrode material requirements PEDOT:PSS has higher conductivity.
At present, bibliographical information mainly contains about the preparation method of the PEDOT:PSS film of high connductivity: (1) alcohol process, comprises methyl alcohol, ethanol, ethylene glycol etc.; (2) acid treatment, comprises sulfuric acid, pyrovinic acid, oxalic acid etc.The conductance of the PEDOT:PSS film of alcohol process is general not high, is no more than 2000S cm
-1[4-6].And sulfuric acid or pyrovinic acid acidification PEDOT:PSS can form high conductivity thin polymer film, conductance is respectively 4380S cm
-1[5] and 3065S cm
-1[2], then, film prepared by said method is all prepared in clear glass substrate, preparation temperature is 140 ~ 160 DEG C, do substrate with plastics and also can form PEDOT:PSS high conductivity thin polymer film, and plastic-substrates has extremely strong hydrophobicity, the PEDOT:PSS aqueous solution is difficult to spread out on the plastic substrate; Meanwhile, these strong acid at high temperature (140 – 160 DEG C) easily and plastic-substrates generation chemical reaction, cause the transparency of film to be deteriorated.
[list of references]
[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.
[summary of the invention]
Based on above-mentioned technical background, the object of this invention is to provide a kind of preparation method taking plastics as substrate and prepare the PEDOT:PSS film of high connductivity.This method solve PEDOT:PSS wettability difference and the problem of poorly conductive on the plastic substrate.Its operating procedure is simple, and experimental cost is cheap, and experiment byproduct environmental pollution is few simultaneously; In addition, the overall structure of prepared PEDOT:PSS film is clear, and size distribution is even, effectively can be applied to flexible organic assembly, such as, develop flexible organic solar batteries, have a good application prospect.
For achieving the above object, the present invention adopts PETG (PET) plastics to be substrate, in the PEDOT:PSS aqueous solution, add the fluorine-containing surfactant Zonyl FS-300 of 0.5vol.%, successfully overcome a difficult problem for PEDOT:PSS wettability difference in plastic; By two-step method, i.e. pyrovinic acid process after first methyl alcohol process, and control reaction temperature and time, thus in PET, prepared the PEDOT:PSS film of high connductivity.Finally, using the PEDOT:PSS flexible transparent film of acid alcohol process as anode, assemble flexible and high efficiency organic solar batteries.
Concrete preparation flow of the present invention and technique as follows:
(1) substrate is cleaned
Choose PET substrate successively through cleaning agent, deionized water, acetone, the ultrasonic process of isopropyl alcohol, each 15 minutes, often kind of solvent process 2 times, the then process in 15 minutes through UV ozone room;
(2) preparation mixing PEDOT:PSS spin coating liquid
Be in the PEDOT:PSS aqueous solution of 6% (Clevios PH1000) at content, mix the fluorine-containing surfactant Zonyl FS-300 of 0.5% volume and the pure methyl alcohol of 6% volume, stir 24 hours;
(3) spin coating and methyl alcohol process
PEDOT:PSS film is prepared in rotating speed spin coating with 2500 revolutions per seconds in PET substrate.Spin-coating time is 60 seconds, then, is immersed in by film in pure methyl alcohol, rinsing three times, takes out sample, then, heat treatment 10 minutes on hot plate, temperature is 120 DEG C;
(4) pyrovinic acid solution acid process
The pyrovinic acid solution of proportioning 8M.Be placed on hot plate by PEDOT:PSS film, temperature is 130 DEG C.Drip the pyrovinic acid solution of 8M, be paved with the surface of whole film, heat treatment 5 minutes.Then, take out sample, spend deionized water three times, then 120 DEG C of thermal annealings 10 minutes, thus form the PEDOT:PSS film of high connductivity.
Flexible organic solar energy cell structure is PET base/PEDOT:PSS electrode/PEDOT:PSS (Clevios P VP 4083) resilient coating/P3HT:PCBM active layer/Ca/Al electrode layer.
The step preparing flexible organic solar batteries with the present invention is:
1, in PET substrate, high connductivity PEDOT:PSS film is formed.
(a) cleaning substrate
Choose PET substrate successively through cleaning agent, deionized water, acetone, the ultrasonic process of isopropyl alcohol, each 15 minutes, often kind of solvent process 2 times.Then the process in 15 minutes through UV ozone room.
(b) preparation mixing PEDOT:PSS spin coating liquid
Be in the PEDOT:PSS aqueous solution of 6% (Clevios PH1000) at content, mix the fluorine-containing surfactant Zonyl FS-300 of 0.5% volume and the methyl alcohol of 6% volume, stir 24 hours;
(c) spin coating and methyl alcohol process
PEDOT:PSS film is prepared in rotating speed spin coating with 2500 revolutions per seconds in PET substrate.Spin-coating time is 60 seconds, then, is immersed in by film in pure methyl alcohol, rinsing three times, takes out sample, then, heat treatment 10 minutes on hot plate, temperature is 120 DEG C;
The process of (d) pyrovinic acid solution acid
The pyrovinic acid solution of proportioning 8M.Be placed on hot plate by PEDOT:PSS film, temperature is 130 DEG C.Drip the pyrovinic acid solution of 8M, be paved with the surface of whole film, heat treatment 5 minutes.Then, take out sample, spend deionized water three times, then 120 DEG C of thermal annealings 10 minutes, thus form the PEDOT:PSS film of high connductivity.
2, on PEDOT:PSS film, PEDOT:PSS resilient coating is formed
With the rotating speed spin coating PEDOT:PSS of 5000 revolutions per seconds (Clevios P VP 4083) solution, rotational time is 60 seconds, prepares anode buffer layer, 120 DEG C of heat treatment 10 minutes.
3, then, the blend solution of spin coating P3HT and PCBM on anode buffer layer, solvent is o-dichlorohenzene, and rotating speed is 600 revolutions per seconds, and the time is 60 seconds.
4, then, solvent annealing and thermal annealing is carried out.Subsequently, evaporation negative electrode Ca and Al, thus have developed flexible organic solar batteries.Fig. 1 is the structural representation of this device.
Film characterization and device detection
Preparation-obtained PEDOT:PSS film transmission spectrum, X-ray diffraction, atomic force electron-microscopic analysis have been carried out.The instrument that X-ray diffraction (XRD) analysis uses is D8Advance, and condition determination is the scanning of 0.001 °/step.Atomic force electron microscope carries out under the voltage of 40KV and the electric current of 50mA.
The flexible organic solar batteries assembled is carried out photoelectric properties test.The measurement of the device of current density (J – V) carries out at a computer-controlled Keithley 236 source measuring unit.Device characterization carries out, with 100mW cm in the environment under illumination AM1.5G
-2xenon lamp based on solar simulator (from Newport Co., LTD.).The DSP lock-in amplifier SR830 of external quantum efficiency and Stamford Study system model adds WDG3 monochrome suit and 500W xenon lamp is measured.The intensity of the light of often kind of wavelength and the monocrystalline silicon photovoltaic cell of standard are calibrated.
These analysis results are listed in accompanying drawing respectively.
Advantage of the present invention and characteristic part are:
(1) the present invention adopts the PEDOT:PSS aqueous solution of mixing fluorocarbon surfactant Zonyl FS-300, alkyd solution (methyl alcohol/pyrovinic acid) facture again after film forming, by controlling concentration, the temperature and time of reaction solution, PET substrate is prepared PEDOT:PSS Thin film conductive rate up to 3560S cm
-1.
(2) overcome the PEDOT:PSS aqueous solution and infiltrate poor difficult point on the plastic substrate.
(3) good mechanical property of PEDOT:PSS film that obtains of the present invention, and the clear in structure of PEDOT:PSS film, neat and orderly.Compared with the flexible organic solar batteries of traditional alcohol process, the energy conversion efficiency of the acid-treated flexible organic solar batteries of alcohol significantly improves 11.7%.And in an atmosphere after 100 times significantly bend, still can keep the performance of about 80%, have a extensive future.
(4) whole preparation process is simple to operate, safe and reliable, and environmental pollution is few simultaneously.
[accompanying drawing explanation]
The substrate of Fig. 1 PET;
The flexible organic solar batteries profile of Fig. 2;
The structural representation of the flexible organic solar batteries of Fig. 3.
The surface topography of the PEDOT:PSS film of Fig. 4 alkyd coprocessing.
Fig. 5 is untreated, alcohol process, the XRD of the PEDOT:PSS film of acid treatment and alkyd coprocessing.
J-V curve (a) of Fig. 6 plane and flexible device
The external quantum efficiency (b) of Fig. 7 plane and flexible device.
[embodiment]
The present invention can be understood better below by embodiment.
Embodiment 1
Preparation flow and the technique of PEDOT:PSS membrane electrode and device are as follows:
(1) preliminary treatment of PET substrate
It is the square structure that the commercial PET of 120 μm is cut into 1.5cm × 1.5cm by thickness.Use cleaning agent successively, deionized water, ethylene glycol carries out ultrasonic cleaning, is cleaned up by the impurity of PET substrate.Dry up for subsequent use in air with hair-dryer.In this experimental procedure, often walking sonication treatment time in cleaning process is 15 minutes, each solvent supersonic twice.
(2) alcohol process PEDOT:PSS film
In PEDOT:PSS solution, add the fluorine-containing surfactant Zonyl FS-300 of 0.5vol.% successively, the methyl alcohol of 6% volume, at least stir 24 hours, improve PEDOT:PSS aqueous solution wettability on the plastic substrate.Spin coating PEDOT:PSS solution in the PET substrate of 1.5cm × 1.5cm, rotating speed 5000 revolutions per seconds, the time is 60 seconds, preparation PEDOT:PSS film, 120 DEG C of heat treatment 10 minutes.
(3) acid treatment PEDOT:PSS film
The preparation of pyrovinic acid solution: the aqueous solution of the pyrovinic acid of configuration 8M, adds magnetic stir bar, stir 24 hours.
Be placed on hot plate by PEDOT:PSS film, temperature is 130 DEG C.Inhale the pyrovinic acid solution of 50ml with dropper, drop on PEDOT:PSS film, ensure that solution is paved with the surface of whole film, heat treatment 5 minutes.Hydrogen ion in acid and PSS anion are combined into neutral PSSH, cause the Coulomb force of PEDOT and PSS to disappear.Then, take out sample with tweezers, put into the beaker of deionized water, wash three times, remove a large amount of nonconducting PSS.Take out sample, then 120 DEG C of thermal annealings 10 minutes, thus define high connductivity, the PEDOT:PSS film of flexible and transparent.PEDOT nano thread structure can be seen clearly, high-sequential from atomic force microscope (Fig. 2).
Embodiment 2
Take PEDOT:PSS as the assembling of the flexible organic solar batteries of electrode
Flexible organic solar energy cell structure is plastic-substrates/PEDOT:PSS electrode/PEDOT:PSS (Clevios P VP 4083) resilient coating/P3HT:PCBM active layer/Ca/Al, and electrode area is 11.0mm
2.
On the plastics of 1.5cm × 1.5cm, alcohol acid treatment forms high connductivity PEDOT PSS film (see embodiment 1).Half PEDOT:PSS film is removed with moistening tweezers and blade, then, the aqueous solution of spin coating PEDOT:PSS (Clevios P VP 4083), the PEDOT:PSS anode buffer layer of preparation 30nm, 120 DEG C of heat treatment 10 minutes.Then, o-dichlorohenzene blend solution (1:1 weight ratio, the 34mg mL of spin coating P3HT and PCBM on PEDOT PSS anode buffer layer
-1p3HT:PCBM), rotating speed is 600 revolutions per seconds, and the time is 60 seconds.Wet P3HT:PCBM blend film is placed in semi-enclosed little glass culture dish the solvent annealing carrying out one hour, and the color of active layer becomes peony from light yellow.Then, in glove box, 150 DEG C of thermal annealings 10 minutes.Finally, 10
-4under the vacuum of Pa, the Al (encapsulation) of Ca and 120nm of thermal evaporation 20nm, thus complete the assembling of flexible organic solar batteries.
Claims (3)
1. mould a preparation method for base high connductivity PEDOT:PSS film, it is characterized in that step is:
(1) substrate is cleaned
Choose PET substrate successively through cleaning agent, deionized water, acetone, the ultrasonic process of isopropyl alcohol, each 15 minutes, often kind of solvent process 2 times, the then process in 15 minutes through UV ozone room;
(2) preparation mixing PEDOT:PSS spin coating liquid
Be in the PEDOT:PSS aqueous solution of 6% at content, mix the fluorine-containing surfactant ZonylFS-300 of 0.5% volume and the pure methyl alcohol of 6% volume, stir 24 hours; The described PEDOT:PSS aqueous solution is CleviosPH1000 type;
(3) spin coating and methyl alcohol process
PEDOT:PSS film is prepared in rotating speed spin coating with 2500 revolutions per seconds in PET substrate.Spin-coating time is 60 seconds, then, is immersed in by film in pure methyl alcohol, rinsing three times, takes out sample, then, heat treatment 10 minutes on hot plate, temperature is 120 DEG C;
(4) pyrovinic acid solution acid process
The pyrovinic acid solution of proportioning 8M.Be placed on hot plate by PEDOT:PSS film, temperature is 130 DEG C.Drip the pyrovinic acid solution of 8M, be paved with the surface of whole film, heat treatment 5 minutes.Then, take out sample, spend deionized water three times, then 120 DEG C of thermal annealings 10 minutes, thus form the PEDOT:PSS film of high connductivity.
2. a flexible organic solar batteries, this device is made up of PEDOT:PSS (Clevios PH1000) flexible electrode of PETG (PET) plastic-substrates, high connductivity, PEDOT:PSS (CleviosP VP 4083) buffer thin film layer, Ca and Al electrode; It is characterized in that at PET suprabasil PEDOT:PSS electrode film layer thickness be 65nm;
PEDOT:PSS buffer thin film layer thickness on PEDOT:PSS electrode film layer is 30nm;
P3HT:PCBM active layer thickness on PEDOT:PSS buffer thin film layer is 200nm;
Ca and Al electrode on P3HT:PCBM active layer, the thickness of Ca and Al electrode is 20nm and 100nm respectively;
The thickness of PET substrate is 120 μm;
The PEDOT:PSS flexible electrode of described high connductivity is Clevios PH1000 type;
Described PEDOT:PSS buffer thin film layer is Clevios P VP 4083 type.
3. the flexible organic solar batteries of one according to claim 1, is characterized in that the PEDOT:PSS flexible electrode of described high connductivity utilizes the method described in claim 1 to prepare.
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| 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 |
| CN106299134A (en) * | 2016-10-21 | 2017-01-04 | 华中科技大学 | The combined solar battery of a kind of patterning and colored solar battery module thereof |
| WO2018010935A1 (en) | 2016-07-11 | 2018-01-18 | Institutt For Energiteknikk | Organic-inorganic hybrid material and method for silicon surface passivation |
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| 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 |
| CN112635671A (en) * | 2020-12-19 | 2021-04-09 | 南京理工大学 | Femtosecond laser modification-based resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) |
| CN113643855A (en) * | 2021-06-18 | 2021-11-12 | 南京邮电大学 | Preparation method and application of flexible transparent electrode |
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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 |
| WO2018010935A1 (en) | 2016-07-11 | 2018-01-18 | Institutt For Energiteknikk | 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 |
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| CN112635671A (en) * | 2020-12-19 | 2021-04-09 | 南京理工大学 | Femtosecond laser modification-based resistance reduction method for conductive polymer PEDOT (PEDOT-PSS) |
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