CN114220909A - PEDOT (Polytetrafluoroethylene)/PSS (Poly (styrene sulfonate) self-supporting thermoelectric film and preparation method thereof - Google Patents
PEDOT (Polytetrafluoroethylene)/PSS (Poly (styrene sulfonate) self-supporting thermoelectric film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a PEDOT PSS self-supporting thermoelectric film and a preparation method thereof, wherein the method comprises the steps of coating a water solution of PEDOT PSS on a substrate, drying, and forming a PEDOT PSS layer on the substrate to obtain a compound A; soaking the compound A in an organic polar solvent, removing the PSS insulated on the outer wall of the PSS, forming a film of the PSS on the substrate, removing the organic polar solvent, and drying to obtain a compound B; and dripping an L-ascorbic acid solution on the compound B to enable the L-ascorbic acid solution to cover the upper surface layer of the compound B, then removing the L-ascorbic acid solution, drying, and removing the substrate to obtain the PEDOT/PSS self-supporting film. And (3) adjusting the oxidation level of PEDOT molecules by using L-ascorbic acid treatment, and tuning the coupling relation between the conductivity of the PEDOT, namely PSS and the Seebeck coefficient so as to obtain a higher power factor.
Description
Technical Field
The invention belongs to the field of preparation of flexible thermoelectric materials, and particularly relates to a PEDOT (Poly ethylene glycol Ether-styrene) PSS (Poly styrene) self-supporting thermoelectric film and a preparation method thereof.
Background
The conductive polymer has the advantages of high electrical conductivity, low thermal conductivity, low price, simple preparation method and the like, so that the conductive polymer becomes a thermoelectric material with high value. Poly (3, 4-ethylenedioxythiophene) (PEDOT for short) is one of the most promising conductive polymers. PEDOT is an insoluble polymer per se, which limits its practical application, and a water-soluble, uniformly dispersed aqueous dispersion, i.e., an aqueous solution of PEDOT: PSS, can be obtained by doping with a water-soluble polyelectrolyte, polystyrene sulfonic acid (PSS). The PEDOT and PSS are hot spots in the field of organic thermoelectric materials due to the advantages of low intrinsic thermal conductivity, easy regulation and control of electrical properties, excellent environmental stability, good film-forming property and the like. PSS, which has excellent performance, has high conductivity and high Seebeck coefficient, but the two parameters are not isolated and are coupled with each other. Therefore, how to realize the decoupling between the conductivity of PEDOT, PSS and the Seebeck coefficient and obtain a high power factor is the current key point.
At present, some methods for improving thermoelectric performance of the PEDOT PSS film are reported in documents, for example, post-treatment is carried out by using strong acid (sulfuric acid, nitric acid and the like), strong base (sodium hydroxide and the like) and strong reducing agent (hydrazine hydrate, sodium borohydride and the like), but the reagents have strong stimulation and corrosion effects and have certain harm to human bodies and the environment, so that loss of service life of devices can be caused when flexible thermoelectric devices are subsequently designed, and the conductivity of the PEDOT PSS film can be greatly reduced by using the strong reducing agent for treatment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the PEDOT/PSS self-supporting thermoelectric film and the preparation method thereof, wherein the oxidation level of PEDOT molecules is adjusted by using the treatment of a non-toxic and mild organic reducing agent L-ascorbic acid, and the coupling relation between the conductivity and the Seebeck coefficient of the PEDOT/PSS is tuned to enable the PEDOT and the PSS to reach a balanced state so as to obtain a higher power factor.
The invention is realized by the following technical scheme:
a preparation method of a PEDOT/PSS self-supporting thermoelectric film comprises the following steps:
coating a PEDOT PSS aqueous solution on a substrate, and then drying to form a PEDOT PSS layer on the substrate to obtain a compound A;
soaking the compound A in an organic polar solvent, removing the PSS insulated on the outer wall of the PEDOT PSS, forming a PEDOT PSS film on the substrate, removing the organic polar solvent in the PEDOT PSS film, and drying to obtain a compound B;
and dripping an L-ascorbic acid solution on the compound B to enable the L-ascorbic acid solution to cover the upper surface layer of the compound B, removing the L-ascorbic acid solution, drying, and removing the substrate to obtain the PEDOT/PSS self-supporting thermoelectric film.
Preferably, the substrate is washed clean by deionized water, acetone and isopropanol in sequence, then dried, and then the obtained substrate is coated with PEDOT/PSS aqueous solution.
Preferably, the organic polar solvent is ethylene glycol, formamide, N-dimethylformamide, sorbitol, dimethyl sulfoxide, N-methylpyrrolidone or glycerol;
preferably, after the aqueous solution of PEDOT and PSS is coated on the substrate, the aqueous solution is dried for 8-12 h under the temperature of 50-100 ℃ in vacuum, and the compound A is obtained.
Preferably, the compound A is soaked in an organic polar solvent for 5-20 min, then taken out, and the organic polar solvent in the PEDOT, namely the PSS film is removed.
Preferably, the PEDOT PSS film is dried for 10-20 min at the temperature of 60-80 ℃ after being washed, so that the compound B is obtained.
Preferably, the concentration of the L-ascorbic acid solution dropped on the compound B is 0.5-1.5 mol/L.
Preferably, after the L-ascorbic acid solution is dripped on the compound B, the L-ascorbic acid solution is remained for 5-20 min and then removed.
Preferably, the upper surface layer of the compound B is dried at 60-80 ℃ after the L-ascorbic acid solution is removed.
A PEDOT PSS self-supporting thermoelectric film obtained by the preparation method of the PEDOT PSS self-supporting thermoelectric film.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a preparation method of a PEDOT/PSS self-supporting thermoelectric film, which comprises the steps of coating a PEDOT/PSS aqueous solution on a substrate, drying to form a PEDOT/PSS layer, sequentially and continuously treating a preliminarily formed PEDOT/PSS film by using an organic polar solvent and L-ascorbic acid, and improving the conductivity and Seebeck coefficient of the film step by step, wherein the high dielectric constant and the high polarity of the organic polar solvent can introduce a shielding effect between current carriers, reduce the coulomb force generated by charges between the PEDOT and the PSS, remove redundant insulating PSS, enable PEDOT molecules to gather, enable PEDOT molecular chains to gradually show a stretching state, promote the transmission of the current carriers, and further improve the conductivity of the PEDOT/PSS thermoelectric film. Because PEDOT molecular chains present a one-dimensional chain conformation, fitting is carried out through a carrier transport equation, and the organic polar solvent is further proved to promote the rearrangement of the PEDOT molecules, and the electron transmission also has three-dimensional steering one-dimensional transmission. According to the invention, a mild reducing agent L-ascorbic acid is used as a second-step treatment solvent, the L-ascorbic acid is a food antioxidant additive, is nontoxic and harmless to human bodies, and does not produce toxic substances or pollute the environment when the PEDOT is reduced by the L-ascorbic acid. The oxidation doping concentration of PEDOT molecules is effectively reduced through the treatment of an organic reducing agent L-ascorbic acid, and the balance of the conductivity and the Seebeck coefficient is tuned. The PEDOT/PSS flexible thermoelectric film with higher power factor is obtained by optimizing the concentration of the organic reducing agent and the processing time. The method for preparing the thermoelectric film by adopting the drop coating method is simple and has lower cost, the prepared thermoelectric film has excellent flexibility and mechanical property, the preparation process is mild and environment-friendly, and the design of a flexible thermoelectric device can be realized.
Drawings
FIG. 1 is a flat-sheet of a freestanding PEDOT: PSS film obtained in example 2 of the present invention.
FIG. 2 is a folded view of a freestanding PEDOT: PSS film obtained in example 3 of the present invention.
FIG. 3 is a double-folded view of a freestanding thermoelectric film of PEDOT: PSS obtained in example 4 of the present invention.
FIG. 4 is a folded view of a freestanding PEDOT: PSS film obtained in example 5 of the present invention.
FIG. 5 is a cross-sectional SEM of an untreated PEDOT PSS thermoelectric film of the present invention.
FIG. 6 is a SEM image of a cross section of a PEDOT PSS thermoelectric film of the present invention after a primary treatment.
FIG. 7 is a SEM image of a cross section of a PEDOT PSS thermoelectric film of the present invention after two treatments.
FIG. 8 is a graph of the power factor, Seebeck coefficient and electrical conductivity as a function of temperature for example 4PEDOT PSS thermoelectric films of the present invention.
Detailed Description
The invention will be described in detail with reference to the drawings, which are provided for the purpose of illustration and not for the purpose of limitation.
The invention relates to a preparation method of a high-performance PEDOT/PSS self-supporting thermoelectric film, which comprises the following steps:
the method comprises the following steps: cleaning a glass substrate with deionized water, acetone and isopropanol in sequence, and then drying;
step two: dripping 100-300 mu L of PEDOT (PSS) aqueous solution (Clevious PH1000) onto the glass substrate obtained in the step one, placing the glass substrate into a vacuum drying oven, and drying the glass substrate for 8-12 hours at 50-100 ℃ to obtain a film A;
the PEDOT and PSS aqueous solution is a commercial product with the specification of Clevious PH1000, and the specific information is as follows:
step three: soaking the film A obtained in the step two in an organic polar solvent for 5-20 min, then taking out, washing with deionized water for 2-3 times, and drying at 60-80 ℃ for 10-20 min to obtain a film B;
the organic polar solvent is ethylene glycol, formamide, N-dimethylformamide, sorbitol, dimethyl sulfoxide, N-methylpyrrolidone or glycerol.
Step four: and (3) dripping the L-ascorbic acid solution with the concentration range of 0.5-1.5 mol/L and the volume of 200 mu L on the surface of the film B obtained in the step three until the L-ascorbic acid solution completely covers the surface of the film B, standing for 5-20 min, then washing the film with deionized water, and drying at 60-80 ℃ to obtain the PEDOT/PSS self-supporting thermoelectric film C.
Example 1:
the method comprises the following steps: cleaning a glass substrate with deionized water, acetone and isopropanol in sequence, and then drying;
step two: dripping 100 mu L of PEDOT, namely PSS aqueous solution (Clevious PH1000) onto the glass substrate obtained in the step one, placing the glass substrate into a vacuum drying oven, and drying the glass substrate for 8 hours at 50 ℃ to obtain a film A;
step three: soaking the film A obtained in the step two in ethylene glycol for 5min, then taking out, washing with deionized water for 2 times, and drying at 60 ℃ for 20min to obtain a film B;
step four: and (3) dripping the L-ascorbic acid solution with the concentration of 0.5mol/L and the volume of 200 mu L on the surface of the film B obtained in the step three until the surface is completely covered, staying for 20min, then washing with deionized water, and drying at 60 ℃ to obtain the PEDOT/PSS self-supporting thermoelectric film C.
Example 2:
the method comprises the following steps: cleaning a glass substrate with deionized water, acetone and isopropanol in sequence, and then drying;
step two: dripping 200 mu L of PEDOT, namely PSS aqueous solution (Clevious PH1000) onto the glass substrate obtained in the step one, placing the glass substrate into a vacuum drying oven, and drying the glass substrate for 12 hours at the temperature of 60 ℃ to obtain a film A;
step three: soaking the film A obtained in the step two in formamide (analytically pure) for 15min, then taking out, washing with deionized water for 3 times, and drying at 80 ℃ for 15min to obtain a film B;
step four: and (3) dripping the L-ascorbic acid solution with the concentration of 1mol/L and the volume of 200 mu L on the surface of the film B obtained in the step three until the L-ascorbic acid solution completely covers the surface of the film B, staying for 5min, then washing the film with deionized water, and drying the film at 80 ℃ to obtain the PEDOT/PSS self-supporting thermoelectric film C.
Example 3:
the method comprises the following steps: cleaning a glass substrate with deionized water, acetone and isopropanol in sequence, and then drying;
step two: dripping 200 mu L of PEDOT, namely PSS aqueous solution (Clevious PH1000) onto the glass substrate obtained in the step one, placing the glass substrate into a vacuum drying oven, and drying the glass substrate for 12 hours at the temperature of 60 ℃ to obtain a film A;
step three: soaking the film A obtained in the step two in formamide (analytically pure) for 15min, then taking out, washing with deionized water for 2 times, and drying at 80 ℃ for 15min to obtain a film B;
step four: and (3) dripping the L-ascorbic acid solution with the concentration of 1.5mol/L and the volume of 200 mu L on the surface of the film B obtained in the step three until the surface is completely covered, staying for 5min, then washing with deionized water, and drying at 80 ℃ to obtain the PEDOT/PSS self-supporting thermoelectric film C.
Example 4:
the method comprises the following steps: cleaning a glass substrate with deionized water, acetone and isopropanol in sequence, and then drying;
step two: dripping 200 mu LPEDOT PSS aqueous solution (Clevious PH1000) on the glass substrate obtained in the step one, placing the glass substrate in a vacuum drying oven, and drying for 12h at 60 ℃ to obtain a film A;
step three: soaking the film A obtained in the step two in formamide (analytically pure) for 15min, then taking out, washing with deionized water for 3 times, and drying at 80 ℃ for 15min to obtain a film B;
step four: and (3) dripping the L-ascorbic acid solution with the concentration of 0.5mol/L and the volume of 200 mu L on the surface of the film B obtained in the step three until the surface is completely covered, staying for 10min, then washing with deionized water, and drying at 80 ℃ to obtain the PEDOT/PSS self-supporting thermoelectric film C.
Example 5:
the method comprises the following steps: cleaning a glass substrate with deionized water, acetone and isopropanol in sequence, and then drying;
step two: dripping 200 mu L of PEDOT, namely PSS aqueous solution (Clevious PH1000) onto the glass substrate obtained in the step one, placing the glass substrate into a vacuum drying oven, and drying the glass substrate for 12 hours at the temperature of 60 ℃ to obtain a film A;
step three: soaking the film A obtained in the step two in formamide (analytically pure) for 15min, then taking out, washing with deionized water for 2 times, and drying at 80 ℃ for 15min to obtain a film B;
step four: and (3) dripping the L-ascorbic acid solution with the concentration of 0.5mol/L and the volume of 200 mu L on the surface of the film B obtained in the step three until the surface is completely covered, staying for 15min, then washing with deionized water, and drying at 80 ℃ to obtain the PEDOT/PSS self-supporting thermoelectric film C.
Example 6:
the method comprises the following steps: cleaning a glass substrate with deionized water, acetone and isopropanol in sequence, and then drying;
step two: dripping 300 mu L of PEDOT, namely PSS aqueous solution (Clevious PH1000) onto the glass substrate obtained in the step one, placing the glass substrate into a vacuum drying oven, and drying the glass substrate for 8 hours at the temperature of 100 ℃ to obtain a film A;
step three: soaking the film A obtained in the step two in formamide (analytically pure) for 15min, then taking out, washing with deionized water for 3 times, and drying at 70 ℃ for 20min to obtain a film B;
step four: and (3) dripping the L-ascorbic acid solution with the concentration of 1mol/L and the volume of 200 mu L on the surface of the film B obtained in the step three until the L-ascorbic acid solution completely covers the surface of the film B, staying for 20min, then washing the film with deionized water, and drying the film at 70 ℃ to obtain the PEDOT/PSS self-supporting thermoelectric film C.
As shown in fig. 1, 2, 3 and 4, the dark blue square image is the PEDOT: PSS self-supporting thermoelectric film, which can be independently formed, shows excellent flexibility, and can be arbitrarily bent and folded in half.
As shown in FIGS. 5 to 7, the parts indicated by arrows are the cross sections of the PEDOT/PSS thermoelectric thin film, and the other parts are impurity parts which cannot be avoided during detection, the PEDOT/PSS thin film is treated by formamide, the coulomb force between the PEDOT and the PSS is weakened due to the shielding effect generated by the high polarity and the high dielectric constant of the formamide, the content of the insulating PSS is reduced, the thickness of the thermoelectric thin film is reduced from 6 mu m (shown in FIG. 5) to 4 mu m (shown in FIG. 6), and the thickness of the thermoelectric thin film is still 4 mu m (shown in FIG. 7) and is not obviously changed after the treatment by the L-ascorbic acid, which indicates that the reducing agent has no influence on the content ratio of the PEDOT and the PSS.
FIG. 8 is a graph showing the power factor of the PEDOT PSS thermoelectric film of example 4 of the present invention as a function of temperature, showing that the power factor of the formamide and L-ascorbic acid treated film is 41.309 μ W/m/K at room temperature2Compared with the power factor of 21.974 mu W/m/K only after formamide treatment2The improvement is nearly 1 time, and the Seebeck coefficient of the PEDOT/PSS film after the two treatments is continuously improved along with the temperature rise, and the power factor reaches 117.956 mu W/m/K at 120 DEG C2This value is already comparable to the power factor obtained when treating PEDOT: PSS films with the strong reducing agent sodium borohydride. In addition, the L-ascorbic acid can be seen to regulate the oxidation level of PEDOT molecules, and simultaneously harmonize the coupling relation between the conductivity and the Seebeck coefficient of PEDOT, namely PSS, so that the two reach an equilibrium state.
Claims (10)
1. A preparation method of a PEDOT/PSS self-supporting thermoelectric film is characterized by comprising the following steps:
coating a PEDOT PSS aqueous solution on a substrate, and then drying to form a PEDOT PSS layer on the substrate to obtain a compound A;
soaking the compound A in an organic polar solvent, removing the PSS insulated on the outer wall of the PEDOT PSS, forming a PEDOT PSS film on the substrate, removing the organic polar solvent in the PEDOT PSS film, and drying to obtain a compound B;
and dripping an L-ascorbic acid solution on the compound B to enable the L-ascorbic acid solution to cover the upper surface layer of the compound B, removing the L-ascorbic acid solution, drying, and removing the substrate to obtain the PEDOT/PSS self-supporting thermoelectric film.
2. The method for preparing the PEDOT PSS self-supporting thermoelectric film as claimed in claim 1, wherein the substrate is washed with deionized water, acetone and isopropanol in sequence, then dried, and then the obtained substrate is coated with the aqueous solution of PEDOT PSS.
3. The method of claim 1, wherein the organic polar solvent is selected from the group consisting of ethylene glycol, formamide, N-dimethylformamide, sorbitol, dimethyl sulfoxide, N-methylpyrrolidone, and glycerol.
4. The method for preparing the PEDOT PSS self-supporting thermoelectric film as claimed in claim 1, wherein the compound A is obtained by coating a substrate with an aqueous solution of PEDOT PSS and then drying the coated substrate in vacuum at 50-100 ℃ for 8-12 h.
5. The preparation method of the PEDOT PSS self-supporting thermoelectric film as claimed in claim 1, wherein the compound A is soaked in an organic polar solvent for 5-20 min, and then taken out, and the organic polar solvent in the PEDOT PSS film is removed.
6. The method for preparing the PEDOT PSS self-supporting thermoelectric film as claimed in claim 1, wherein the compound B is obtained by washing and drying the PEDOT PSS film at 60-80 ℃ for 10-20 min.
7. The method for preparing a PEDOT/PSS self-supporting thermoelectric film as claimed in claim 1, wherein the concentration of the L-ascorbic acid solution dropped on the compound B is 0.5-1.5 mol/L.
8. The method for preparing the PEDOT/PSS self-supporting thermoelectric film as claimed in claim 1, wherein the L-ascorbic acid solution is dropped on the compound B, and then the L-ascorbic acid solution is removed after staying for 5-20 min.
9. The method for preparing a PEDOT/PSS self-supporting thermoelectric film as claimed in claim 1, wherein the upper surface layer of the compound B is dried at 60-80 ℃ after removing the L-ascorbic acid solution.
10. A PEDOT/PSS self-supporting thermoelectric film obtained by the method for preparing a PEDOT/PSS self-supporting thermoelectric film according to any one of claims 1 to 9.
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| CN202111520107.5A CN114220909A (en) | 2021-12-13 | 2021-12-13 | PEDOT (Polytetrafluoroethylene)/PSS (Poly (styrene sulfonate) self-supporting thermoelectric film and preparation method thereof |
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| CN202111520107.5A CN114220909A (en) | 2021-12-13 | 2021-12-13 | PEDOT (Polytetrafluoroethylene)/PSS (Poly (styrene sulfonate) self-supporting thermoelectric film and preparation method thereof |
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| CN114813881A (en) * | 2022-05-09 | 2022-07-29 | 西安交通大学 | Biosensor based on organic electrochemical transistor and detection method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114813881A (en) * | 2022-05-09 | 2022-07-29 | 西安交通大学 | Biosensor based on organic electrochemical transistor and detection method |
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