CN106397799A - PEDOT-PSS nanometer film with high conductivity and preparation and transfer methods thereof - Google Patents
PEDOT-PSS nanometer film with high conductivity and preparation and transfer methods thereof Download PDFInfo
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- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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Abstract
The invention discloses a PEDOT-PSS nanometer film with high conductivity and preparation and transfer methods thereof, belonging to the field of organic photoelectricity. A mass ratio of PEDOT to PSS in the PEDOT-PSS nanometer film is 1: 2.5; and the nanometer film has a thickness of 0.15 to 0.35 [mu]m and conductivity of 1300 to 1610 S/cm. The preparation method is simple and short in process flow; and the prepared nanometer film has a smooth and complete surface, high conductivity and stable performance.
Description
Technical field
The present invention relates to organic photoelectric field, particularly relate to a kind of high connductivity PEDOT:PSS nano thin-film and its preparation and
Transfer method.
Background technology
In recent years, increasingly increasing with energy crisis, the opto-electronic device such as energy conversion and energy stores is increasingly subject to
Concern to people.In terms of energy conversion device, organic solar batteries are with its cleaning, cheap, renewable, flexible etc. superior
Property, favored by scientist.In terms of energy stores, the charging interval is short, power density is high, storehouse due to having for ultracapacitor
The advantages of logical sequence efficiency high and long service life, becomes current research focus.And it is related to gold during current Fabrication of Optoelectronic Devices
Belong to the air stability of electrode, high cost of non-flexible and vacuum process etc., therefore there is preferable air stability, high conductivity
The exploitation of flexible electrode is extremely urgent.
Conducting polymer, due to having the advantages that higher electrical conductivity, preferable air stability and flexibility, is recognized by people
For being the ideal chose replacing ITO conductive glass electrode.Wherein, the conducting polymer PEDOT of commercialization:The solid phase of PSS solution
Content is the mass ratio of 0.6%～5.0%, PEDOT and PSS is 5:8～1:20, wherein, PEDOT is EDOT (3,4- ethylene two
Oxygen thiophene monomer) polymer, PSS is poly styrene sulfonate, adds in the solution for improving the dissolubility of PEDOT.
PEDOT:PSS solution has higher electrical conductivity, solution processable performance, high transmission rate and heat stability, and formula is various, can
Meet the requirement of dissimilar device, thus gain great popularity.
Now, conventional preparation PEDOT:The method of PSS thin film is drop coating, spin coating etc., but the thin film mistake of drop-coating preparation
Thick it is impossible to meet actual demand, spin-coated thin film is difficult to control to accurate respective thickness, and cannot realize large-scale production, using taking out
The PEDOT that the method for filter obtains:PSS thin film is smooth and has higher electrical conductivity, such as discloses in patent No. CN105405977A
Method using sucking filtration obtains nano thin-film, but needs first by PEDOT:PSS is added drop-wise in acid solution to improve the conductance of thin film
Rate, gained PEDOT:In PSS thin film, mass ratio is 3:7～15:2 PEDOT and PSS, described PEDOT:The thickness of PSS thin film
For 1 μm～50 μm, square resistance is 0.10 Ω/sq～120 Ω/sq, and electrical conductivity is 210S/cm～1827S/cm.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of low cost, smooth surface, the high connductivity that complete, electrical conductivity is high
PEDOT:PSS nano thin-film and its preparation and transfer method.
For solving above-mentioned technical problem, the present invention provides technical scheme as follows：
A kind of high connductivity PEDOT:PSS nano thin-film, described PEDOT:PEDOT in PSS nano thin-film:PSS mass ratio is
1:2.5, the thickness of described nano thin-film is 0.15 μm～0.35 μm, and electrical conductivity is 1300S/cm～1610S/cm.PEDOT with
PSS mixes in certain proportion, can form homogeneous scattered PEDOT:PSS aqueous solution, due to dissolubility in water for the PSS relatively
High it is possible to larger raising PEDOT:The dissolubility of PSS, obtains the preferable solution of dispersibility, and has stable electrical conductivity,
Good transparency.
Further, described PEDOT:PEDOT in PSS nano thin-film:PSS mass ratio is 1:1.2～1:1.7.
A kind of high connductivity PEDOT:The preparation method of PSS nano thin-film, comprises the following steps：
Step 1：With organic solvent by PEDOT:PSS solution dilutes, ultrasonic disperse；
Step 2:Above-mentioned solution is laid on microporous filter membrane；
Step 3：Described nano thin-film is obtained by vacuum filtration.
Wherein：In described step 1, organic solvent is ethanol, methanol, dimethyl sulfoxide, dimethylformamide dimethyl amide, ethylene glycol
One or more of.
Wherein：In described step 1, extension rate is 30～200 times.
Wherein：In described step 2, the aperture of microporous filter membrane is less than 0.5 μm.
Wherein：In described step 3, the thickness of described nano thin-film is 0.2 μm～0.25 μm.
PEDOT using organic solvent diluting：The self-supporting nano thin-film that PSS is obtained, conductivity is excellent.
Arbitrary described high connductivity PEDOT in above-mentioned:The transfer method of PSS nano thin-film is it is characterised in that include following
Step：
Step 1：The microporous filter membrane being loaded with nano thin-film is immersed in deionized water, carries out demoulding；
Step 2：The nano thin-film coming off is transferred on plastics or glass chip；
Step 3：Vacuum drying.
Wherein：In described step 3, vacuum drying temperature is 100 DEG C～120 DEG C.
Process as done demoulding after being completely dried the microporous filter membrane being loaded with nano thin-film obtaining after sucking filtration again, cannot be complete
Whole nano thin-film and operate very difficult, if the microporous filter membrane being loaded with nano thin-film not being completely dried is placed in water, enter
Row wet method shifts, and both can obtain complete nano thin-film and easy to operate.
The invention has the advantages that：
Compared with prior art, in such scheme, PEDOT:PEDOT in PSS nano thin-film:PSS mass ratio is 1:2.5,
More save PEDOT:The cost of raw material of PSS, and it is easier the thickness of thin film needed for control using the method for sucking filtration, make
Its application is convenient, and prepared nano film thickness uniformly, is 0.2 μm～0.25 μm, electrical conductivity be 1300S/cm～
1610S/cm, electric conductivity is excellent, preparation process is simple, and flow process is short, carries out wet method transfer, more before the film drying of sucking filtration
Be easy to get complete nano thin-film, and is suitable to large-scale production.
Brief description
Fig. 1 is PEDOT:The preparation of PSS nano thin-film and transfer flow figure；
The PEDOT of Fig. 2 difference piece group-transfer:PSS nano thin-film and elastic schematic diagram；
Clear PE DOT of Fig. 3 different solvents preparation:PSS nano thin-film schematic diagram；
The PEDOT of the different-thickness that Fig. 4 is prepared for solvent based on ethanol:PSS nano thin-film schematic diagram；
The PEDOT of Fig. 5 different solvents preparation:PSS nano film thickness block diagram；
The PEDOT of Fig. 6 different organic solvents preparation:PSS nano thin-film electrical conductivity block diagram；
Fig. 7 PEDOT:PSS nano film thickness and the relation curve of its consumption；
The PEDOT of the different-thickness that Fig. 8 is prepared for solvent based on ethanol:PSS nano thin-film electrical conductivity broken line graph.
Specific embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool
Body embodiment is described in detail.
Embodiment 1
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS adds in the ethanol (EtOH) of 6mL, and ultrasonic disperse is laid on
On microporous filter membrane；
(3) vacuum filtration film forming；
(4) microporous filter membrane being loaded with thin film is immersed in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
As seen in figs. 5-6, the thickness of prepared nano thin-film is 0.225 μm, and conductivity is 1400S/cm, thin film pliability
Well, good transparency (shown in Fig. 2) is all presented on plastic and glass chip base.
Embodiment 2
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS add 6mL methanol (MeOH) in, ultrasonic disperse, paving with
On microporous filter membrane；
(3) vacuum filtration film forming；
(4) it is immersed into being loaded with the microporous filter membrane of thin film in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
As seen in figs. 5-6, the thickness of prepared nano thin-film is 0.25 μm, and conductivity is 1590S/cm, thin film pliability
Well, good transparency is all presented on plastic and glass chip base.
Embodiment 3
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS adds in the dimethyl sulfoxide (DMSO) of 6mL, ultrasonic point
Dissipate, be laid on microporous filter membrane；
(3) vacuum filtration film forming；
(4) microporous filter membrane being loaded with thin film is immersed in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
As seen in figs. 5-6, the thickness of prepared nano thin-film is 0.227 μm, and conductivity is 1610S/cm, thin film pliability
Well, good transparency (shown in Fig. 2) is all presented on plastic and glass chip base.
Embodiment 4
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS adds in the dimethylformamide (DMF) of 6mL, ultrasonic point
Dissipate, be laid on microporous filter membrane；
(3) vacuum filtration film forming；
(4) microporous filter membrane being loaded with thin film is immersed in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
As seen in figs. 5-6, the thickness of prepared nano thin-film is 0.225 μm, and conductivity is 1400S/cm, thin film pliability
Well, good transparency (shown in Fig. 2) is all presented on plastic and glass chip base.
Embodiment 5
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS adds in the ethylene glycol (EG) of 6mL, and ultrasonic disperse is laid on
On microporous filter membrane；
(3) vacuum filtration film forming；
(4) microporous filter membrane being loaded with thin film is immersed in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
As seen in figs. 5-6, the thickness of prepared nano thin-film is 0.225 μm, and recording conductivity is 1300S/cm, and thin film is soft
Toughness is good, all presents good transparency (shown in Fig. 2) in plastic and glass chip base.
Embodiment 6
Mass ratio is taken to be 1 respectively:2.5 PEDOT:PSS solution 30 μ L, 50 μ L, 100 μ L, 200 μ L add the ethanol of 6mL
(EtOH), in, to the thin film after transfer sucking filtration, electrical conductivity and the test of film thickness are carried out.
As shown in figure 4, the PEDOT of different taken amounts:Picture on plastics for the PSS aqueous solution, with PEDOOT:PSS consumption
Increase, the color of thin film gradually deepens.
As shown in fig. 7, film thickness is with PEDOT:The increase of PSS taken amount and thicken.
Additionally, as shown in figure 8, the electrical conductivity of nano thin-film is with PEDOT:The increase of PSS taken amount is in first increases and then decreases
Trend.
Embodiment 7
The PEDOT of EtOH, MeOH, DMF, DMSO, EG will be diluted in:The nano thin-film that PSS makes, condition of equivalent thickness condition
Under, as shown in figure 3, nano thin-film shows different transparencys on plastics.
Comparative example 1
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS adds in the water of 6mL, and ultrasonic disperse is laid on microporous filter membrane
On；
(3) vacuum filtration film forming；
(4) microporous filter membrane being loaded with thin film is immersed in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
The thickness of prepared nano thin-film is 0.24 μm, and conductivity is 1.5S/cm.
Comparative example 2
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS adds in the isopropanol of 6mL, and ultrasonic disperse is laid on micropore
On filter membrane；
(3) vacuum filtration film forming；
(4) microporous filter membrane being loaded with thin film is immersed in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
The thickness of prepared nano thin-film is 0.234 μm, and conductivity is 1100S/cm.
Comparative example 3
(1) plastics (glass) chip base is cleaned with OTG cleanout fluid, deionized water cleans, after ethanol purge is clean, dry standby
With；
(2) by 100 μ L mass ratioes be 1:2.5 PEDOT:PSS adds in the N-Methyl pyrrolidone (NMP) of 6mL, ultrasonic
Dispersion, is laid on microporous filter membrane；
(3) vacuum filtration film forming；
(4) microporous filter membrane being loaded with thin film is immersed in deionized water, demoulding；
(5) transfer process (shown in Fig. 1), the thin film coming off transfer is transferred on plastics or glass chip respectively；
(6) will be vacuum dried at 120 DEG C of the thin film taken off；
(7) electrical conductivity test is carried out using four probe method, using scanning electron microscope, the thickness of thin film is tested.
The thickness of prepared nano thin-film is 0.23 μm, and conductivity is 520S/cm.
Find, in comparative example 2, organic solvent uses isopropanol through overtesting, electrical conductivity is more than 1000S/cm, comparative example 3
In, organic solvent uses NMP, and electrical conductivity is less than 1000S/cm, and because length is limited, organic solvent can choose examination commonly used in the art
Agent, to form new embodiment, is not enumerated one by one, but it should be noted that organic solvent in addition to the foregoing, can also be adopted
With those skilled in the art's other organic solvents thinkable, these also should be regarded as protection scope of the present invention.
To sum up, PEDOT in the present invention:PSS nano thin-film more saves PEDOT:The cost of raw material of PSS, and make
, so as to application is convenient, prepared nano film thickness is uniform for the thickness of thin film needed for being easier to control with the method for sucking filtration,
Good transparency, compared with comparative example 1, the PEDOT that the present invention is obtained all are presented on plastic and glass chip base:PSS nanometer
Thin film conductive performance is excellent, and electrical conductivity is 1300S/cm～1610S/cm, preparation process is simple, and flow process is short, in the thin film of sucking filtration
Carry out wet method transfer before drying, be more easy to obtain complete nano thin-film, and be suitable to large-scale production.
The above is the preferred embodiment of the present invention it is noted that for those skilled in the art
For, on the premise of without departing from principle of the present invention, some improvements and modifications can also be made, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of high connductivity PEDOT:PSS nano thin-film is it is characterised in that described PEDOT:PEDOT in PSS nano thin-film:PSS
Mass ratio is 1：2.5, the thickness of described nano thin-film is 0.15 μm～0.35 μm, and electrical conductivity is 1300S/cm～1610S/cm.
2. high connductivity PEDOT according to claim 1:PSS nano thin-film is it is characterised in that described PEDOT:PSS nanometer
PEDOT in thin film:PSS mass ratio is 1:1.2～1:1.7.
3. a kind of high connductivity PEDOT:The preparation method of PSS nano thin-film is it is characterised in that comprise the following steps：
Step 1：With organic solvent by PEDOT:PSS solution dilutes, ultrasonic disperse；
Step 2:Above-mentioned solution is laid on microporous filter membrane；
Step 3：Described nano thin-film is obtained by vacuum filtration.
4. high connductivity PEDOT according to claim 3:The preparation method of PSS nano thin-film is it is characterised in that described step
In rapid 1, organic solvent is one or more of ethanol, methanol, dimethyl sulfoxide, dimethylformamide dimethyl amide, ethylene glycol.
5. high connductivity PEDOT according to claim 3:The preparation method of PSS nano thin-film is it is characterised in that described step
In rapid 1, extension rate is 30～200 times.
6. high connductivity PEDOT according to claim 3:The preparation method of PSS nano thin-film is it is characterised in that described step
In rapid 2, the aperture of microporous filter membrane is less than 0.5 μm.
7. high connductivity PEDOT according to claim 3:The preparation method of PSS nano thin-film is it is characterised in that described step
In rapid 3, the thickness of described nano thin-film is 0.2 μm～0.25 μm.
8. arbitrary described high connductivity PEDOT in claim 1-7:The transfer method of PSS nano thin-film is it is characterised in that wrap
Include following steps：
Step 1：The microporous filter membrane being loaded with nano thin-film is immersed in deionized water, carries out demoulding；
Step 2：The nano thin-film coming off is transferred on plastics or glass chip；
Step 3：Vacuum drying.
9. high connductivity PEDOT according to claim 8:The transfer method of PSS nano thin-film is it is characterised in that described step
In rapid 3, vacuum drying temperature is 100 DEG C～120 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928480A (en) * | 2017-03-29 | 2017-07-07 | 重庆大学 | A kind of PEDOT based on molecular template principle:The preparation method of PSS solution and film |
| CN109824915A (en) * | 2019-02-02 | 2019-05-31 | 江西科技师范大学 | A kind of preparation method of high-performance conductive polyalcohol hydrogel |
| CN109870493A (en) * | 2019-03-20 | 2019-06-11 | 江西科技师范大学 | A kind of electrochemical sensor and preparation method thereof of flexible thin film type detection tert-butyl hydroquinone |
| CN110233061A (en) * | 2019-06-19 | 2019-09-13 | 江西科技师范大学 | A kind of preparation method of the highly conductive porous flexible film of PEDOT:PSS |
| CN110333619A (en) * | 2019-05-09 | 2019-10-15 | 烟台如水光电科技有限公司 | A kind of polymer dispersed liquid crystal film and its manufacturing method based on macromolecule transparent conductive substrate |
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| CN105405977A (en) * | 2015-10-29 | 2016-03-16 | 华中科技大学 | Self-supporting PEDOT-PSS film, manufacturing method thereof and applications |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928480A (en) * | 2017-03-29 | 2017-07-07 | 重庆大学 | A kind of PEDOT based on molecular template principle:The preparation method of PSS solution and film |
| CN106928480B (en) * | 2017-03-29 | 2019-10-01 | 重庆大学 | It is a kind of based on the PEDOT:PSS solution of molecular template principle and the preparation method of film |
| CN109824915A (en) * | 2019-02-02 | 2019-05-31 | 江西科技师范大学 | A kind of preparation method of high-performance conductive polyalcohol hydrogel |
| CN109824915B (en) * | 2019-02-02 | 2021-09-14 | 江西科技师范大学 | Preparation method of high-performance conductive polymer hydrogel |
| CN109870493A (en) * | 2019-03-20 | 2019-06-11 | 江西科技师范大学 | A kind of electrochemical sensor and preparation method thereof of flexible thin film type detection tert-butyl hydroquinone |
| CN110333619A (en) * | 2019-05-09 | 2019-10-15 | 烟台如水光电科技有限公司 | A kind of polymer dispersed liquid crystal film and its manufacturing method based on macromolecule transparent conductive substrate |
| CN110233061A (en) * | 2019-06-19 | 2019-09-13 | 江西科技师范大学 | A kind of preparation method of the highly conductive porous flexible film of PEDOT:PSS |
| CN112864324A (en) * | 2020-12-31 | 2021-05-28 | 江西科技师范大学 | Construction of organic gate electrochemical transistor biosensor |
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