CN115394905A - Preparation method of flexible PVA/PEDOT/PSS composite thermoelectric film - Google Patents
Preparation method of flexible PVA/PEDOT/PSS composite thermoelectric film Download PDFInfo
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- CN115394905A CN115394905A CN202210924662.2A CN202210924662A CN115394905A CN 115394905 A CN115394905 A CN 115394905A CN 202210924662 A CN202210924662 A CN 202210924662A CN 115394905 A CN115394905 A CN 115394905A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/12—Stencil printing; Silk-screen printing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/26—Printing on other surfaces than ordinary paper
- B41M1/30—Printing on other surfaces than ordinary paper on organic plastics, horn or similar materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—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 alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2425/00—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
- C08J2425/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2465/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
Abstract
The invention relates to a thermoelectric material, in particular to a preparation method of a flexible PVA/PEDOT/PSS composite thermoelectric film, which comprises the following steps: s1: adding PVA into a PEDOT (PSS) solution, stirring and heating, and then naturally cooling to obtain a mixed solution; s2: printing the mixed solution on a substrate by a screen printing technology, and drying to obtain a flexible composite thermoelectric film crude product; s3: water bath treatment: immersing the crude product into deionized water, heating, washing by the deionized water and drying to obtain a flexible composite thermoelectric film subjected to water bath treatment; s4: and (3) DMSO (dimethylsulfoxide) post-treatment: and (3) soaking the composite thermoelectric film subjected to water bath treatment in DMSO, washing with deionized water and drying to obtain the flexible PVA/PEDOT/PSS composite thermoelectric film. Compared with the prior art, the invention further improves the thermoelectric property of the film while maintaining the flexibility of the composite film.
Description
Technical Field
The invention relates to a thermoelectric material, in particular to a preparation method of a flexible PVA/PEDOT/PSS composite thermoelectric film.
Background
With the gradual consumption of primary energy sources such as petroleum, coal, natural gas and the like and the gradual deepening of the problem of ecological environment pollution, the development and utilization of novel energy source materials are urgent. Meanwhile, the thermoelectric material can be suitable for the new theme of green environmental protection in the 21 st century, and the wide attention of material researchers is attracted. The thermoelectric material is a new functional material which realizes the interconversion of thermal energy and electric energy through the transmission of carriers (including electrons e and holes h) in the solid material.
The flexible thermoelectric power generation device has the advantages of small volume, no noise, environmental protection, easiness in carrying and the like, can convert the temperature difference between skin and the external environment into electric energy to supply power to intelligent wearable equipment, and therefore is widely concerned by researchers. However, the main reason for limiting the large-scale use of flexible thermoelectric power generation devices is the poor performance of the flexible polymer-based composite thermoelectric materials used for manufacturing the devices, so that research and development of high-performance flexible polymer-based composite thermoelectric materials are urgently needed.
Screen printing is a process of printing a paste to a substrate through a gap by a squeegee and a screen plate, and obtaining a coating after heat treatment. The film forming effect is usually controlled by parameters such as the mesh number, material, and screen printing distance of the screen printing plate. The PEDOT PSS is used as a high-molecular conductive polymer and has the following advantages compared with the traditional inorganic thermoelectric material (bismuth telluride and the like): (1) good film forming properties; (2) lower thermal conductivity; (3) good flexibility and (4) solution processability. Meanwhile, organic polar solvents (such as DMSO, methanol, ethanol, ethylene glycol and the like) are used for doping, so that the conductivity of the PEDOT/PSS can be obviously enhanced, but the PEDOT/PSS solution is low in viscosity and cannot be directly printed into a film, and further improvement is needed to prepare the thermoelectric film with excellent performance.
Disclosure of Invention
Polyvinyl alcohol (PVA) has the advantages of good film forming property, low price and the like, and is often used for aqueous slurry, but PVA is not conductive per se and has great influence on the thermoelectric property of the prepared composite film, so that the content of the PVA needs to be reduced as much as possible after the preparation of the composite film is finished, and the influence of the reduction of the content on the flexibility of the film needs to be considered. At present, no report related to the preparation of the flexible PVA/PEDOT/PSS composite thermoelectric material by a screen printing process is found.
The invention aims to solve at least one of the problems and provides a preparation method of a flexible PVA/PEDOT: PSS composite thermoelectric film, which can further improve the thermoelectric performance of the film while maintaining the flexibility of the composite film. The method has the advantages of simple preparation process, suitability for mass production and the like, and provides a brand new idea for the preparation of the high-performance flexible polymer-based composite thermoelectric material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a flexible PVA/PEDOT/PSS composite thermoelectric film comprises the following steps:
s1: preparation of PVA/PEDOT PSS Mixed solution: adding PVA to a PEDOT: PSS solution containing 5wt% DMSO, sealing and stirring for 5min, heating, stirring at room temperature for 2h to allow the mixed solution to cool naturally to obtain a mixed solution of PVA/PEDOT: PSS;
s2: PSS composite thermoelectric film rough product preparation: printing the PVA/PEDOT/PSS mixed solution obtained in the step S1 on a substrate by a screen printing technology, and performing vacuum drying at 80 ℃ for 12 hours to obtain a flexible PVA/PEDOT/PSS composite thermoelectric film rough finished product;
s3: water bath treatment: soaking the flexible PVA/PEDOT/PSS composite thermoelectric film crude product obtained in the step S2 into deionized water, sealing and heating, washing with the deionized water, and drying at 80 ℃ for 12 hours to obtain the water-bath-treated flexible PVA/PEDOT/PSS composite thermoelectric film;
s4: and (3) DMSO post-treatment: and (4) placing the water-bath-treated flexible PVA/PEDOT/PSS composite thermoelectric film obtained in the step (S3) in DMSO for soaking for 0.5h, then washing for 3 times by deionized water and carrying out vacuum drying at 80 ℃ for 12h to obtain the flexible PVA/PEDOT/PSS composite thermoelectric film.
Preferably, in step S1, the mass ratio of PVA to PEDOT: PSS solution is 1:1-1:50.
preferably, in step S1, the heating temperature is 40-95 ℃ and the time is 10-60min.
Complete dissolution of PVA in PEDOT: PSS solution was facilitated by means of stirring and heating.
Preferably, in step S2, the substrate is one of a nylon filter membrane, a polyvinylidene fluoride filter membrane, or a polytetrafluoroethylene membrane.
Preferably, in step S3, the heating temperature is 40-95 ℃ and the time is 0.1-24h.
The insulating phase PVA in the system can be effectively reduced through the water bath treatment in the step S3.
The DMSO treatment is adopted, so that the content of PSS in the insulating phase of PEDOT and PSS can be effectively regulated, the flexibility of the composite film is kept, and the thermoelectric property of the composite film is further improved.
Compared with the prior art, the invention has the following beneficial effects:
1. based on the current research situation, the flexible PVA/PEDOT/PSS composite thermoelectric material is prepared by a screen printing technology for the first time, the insulating phase PVA in the system can be effectively reduced through water bath treatment, the content of the insulating phase PSS in the PEDOT/PSS can be effectively regulated and controlled through DMSO treatment, the flexibility of the composite film is kept, the thermoelectric property of the composite film is further improved, and a new thought is provided for research and development of the flexible thermoelectric material.
2. The preparation process provided by the invention is simple and can be used for mass production, and the prepared flexible PVA/PEDOT/PSS composite film has excellent thermoelectric property and has wide application prospect in the fields of thermoelectric power generation and refrigeration devices.
Drawings
FIG. 1 is a schematic process flow diagram of the preparation method of the present invention;
FIG. 2 is a schematic representation of an untreated PVA/PEDOT PSS composite thermoelectric film of example 1;
FIG. 3 is a schematic diagram of a PVA/PEDOT/PSS composite thermoelectric film finally obtained in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
A preparation method of a flexible PVA/PEDOT/PSS composite thermoelectric film is shown in figure 1 and comprises the following steps:
s1: preparation of PVA/PEDOT PSS Mixed solution: according to the following steps: 1-1:50 to a mixed solution of PVA/PEDOT: PSS (containing 5wt% DMSO), stirring for 5min and heating in an oven at 40-95 ℃ for 10-60min to dissolve the PVA sufficiently, followed by stirring at room temperature for 2h to cool the mixed solution naturally to obtain a mixed solution of PVA/PEDOT: PSS;
s2: PSS composite thermoelectric film rough product preparation: printing the PVA/PEDOT/PSS mixed solution obtained in the step S1 on a substrate by a screen printing technology, and performing vacuum drying at 80 ℃ for 12 hours to obtain a flexible PVA/PEDOT/PSS composite thermoelectric film rough product;
s3: water bath treatment: the flexible PVA/PEDOT, PSS composite thermoelectric film crude product obtained in the step S2 is immersed in deionized water and heated for 0.1-24h at 40-95 ℃, and then washed by the deionized water and dried in vacuum for 12h at 80 ℃ to obtain the flexible PVA/PEDOT, PSS composite thermoelectric film processed by water bath;
s4: and (3) DMSO (dimethylsulfoxide) post-treatment: and (4) placing the water-bath-treated flexible PVA/PEDOT/PSS composite thermoelectric film obtained in the step (S3) in DMSO for soaking for 0.5h, then washing for multiple times by deionized water and drying in vacuum at 80 ℃ for 12h to obtain the flexible PVA/PEDOT/PSS composite thermoelectric film.
Example 1
(1) Preparation of PVA/PEDOT PSS Mixed solution: mixing 0.1g of PVA and 4mL of a PEDOT;
(2) PSS composite thermoelectric film preparation: printing PVA/PEDOT and PSS slurry on a nylon filter membrane by utilizing a screen printing technology, and performing vacuum drying at 80 ℃ for 12 hours to prepare a flexible PVA/PEDOT and PSS composite thermoelectric film;
(3) Water bath treatment: putting the PVA/PEDOT/PSS composite thermoelectric film into a beaker containing 60mL deionized water, sealing the cup mouth by using a sealing film, heating at 95 ℃ for 12h, washing by using the deionized water, and then drying in vacuum at 80 ℃ for 12h to obtain the PVA/PEDOT/PSS composite thermoelectric film treated by water bath;
(4) And (3) DMSO post-treatment: after the PVA/PEDOT/PSS composite thermoelectric film treated by the water bath is placed into a DMSO solution to be soaked for 0.5h, the PVA/PEDOT/PSS composite thermoelectric film is washed for 3 times by deionized water and then is dried for 12h in vacuum at 80 ℃ to prepare the PVA/PEDOT/PSS composite thermoelectric film with excellent performance, and the PVA/PEDOT/PSS composite thermoelectric film is shown in figure 3.
FIGS. 2 and 3 are schematic diagrams of the PVA/PEDOT: PSS composite thermoelectric film before and after being treated by water bath and DMSO in example 1, respectively, and the composite thermoelectric film before and after being treated has good flexibility.
Example 2
(1) Preparation of PVA/PEDOT PSS Mixed solution: mixing 0.1g PVA and 0.1mL of a PEDOT;
(2) Preparation of flexible PVA/PEDOT PSS composite thermoelectric film: printing PVA/PEDOT and PSS slurry on a polyvinylidene fluoride filter membrane by utilizing a screen printing technology, and performing vacuum drying at 80 ℃ for 12 hours to prepare a flexible PVA/PEDOT and PSS composite thermoelectric film;
(3) Water bath treatment: putting the PVA/PEDOT/PSS composite thermoelectric film into a beaker containing 60mL of deionized water, sealing the cup opening by using a sealing film, heating at 40 ℃ for 0.1h, washing by using the deionized water, and then drying in vacuum at 80 ℃ for 12h to obtain the PVA/PEDOT/PSS composite thermoelectric film treated by water bath;
(4) And (3) DMSO post-treatment: and (3) putting the PVA/PEDOT: PSS composite thermoelectric film subjected to water bath treatment into a DMSO solution, soaking for 0.5h, washing for 3 times by using deionized water, and performing vacuum drying at 80 ℃ for 12h to prepare the PVA/PEDOT: PSS composite thermoelectric film with excellent performance.
Example 3
(1) Preparation of PVA/PEDOT PSS Mixed solution: mixing 0.1g of PVA and 5mL of a PEDOT;
(2) PSS composite thermoelectric film preparation: printing PVA/PEDOT (polyvinyl acetate/PEDOT: PSS) slurry on a polytetrafluoroethylene film by utilizing a screen printing technology, and performing vacuum drying for 12 hours at 80 ℃ to prepare a flexible PVA/PEDOT: PSS composite thermoelectric film;
(3) Water bath treatment: putting the PVA/PEDOT/PSS composite thermoelectric film into a beaker containing 60mL deionized water, sealing the cup mouth by using a sealing film, heating at 95 ℃ for 24h, washing by using the deionized water, and then drying in vacuum at 80 ℃ for 12h to obtain the PVA/PEDOT/PSS composite thermoelectric film treated by water bath;
(4) And (3) DMSO (dimethylsulfoxide) post-treatment: and (3) putting the PVA/PEDOT: PSS composite thermoelectric film subjected to water bath treatment into a DMSO solution, soaking for 0.5h, washing for 3 times by using deionized water, and performing vacuum drying at 80 ℃ for 12h to prepare the PVA/PEDOT: PSS composite thermoelectric film with excellent performance.
Example 4
(1) Preparation of PVA/PEDOT PSS Mixed solution: mixing 0.1g of PVA and a 2mL of a PEDOT;
(2) Preparation of flexible PVA/PEDOT PSS composite thermoelectric film: printing PVA/PEDOT and PSS slurry on a nylon filter membrane by utilizing a screen printing technology, and performing vacuum drying at 80 ℃ for 12 hours to prepare a flexible PVA/PEDOT and PSS composite thermoelectric film;
(3) Water bath treatment: putting the PVA/PEDOT/PSS composite thermoelectric film into a beaker containing 60mL of deionized water, sealing the cup mouth by using a sealing film, heating at 80 ℃ for 6h, washing by using the deionized water, and then drying in vacuum at 80 ℃ for 12h to obtain the PVA/PEDOT/PSS composite thermoelectric film treated by water bath;
(4) And (3) DMSO (dimethylsulfoxide) post-treatment: and (3) putting the PVA/PEDOT: PSS composite thermoelectric film subjected to water bath treatment into a DMSO solution, soaking for 0.5h, washing for 3 times by using deionized water, and performing vacuum drying at 80 ℃ for 12h to prepare the PVA/PEDOT: PSS composite thermoelectric film with excellent performance.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (5)
1. A preparation method of a flexible PVA/PEDOT/PSS composite thermoelectric film is characterized by comprising the following steps:
s1: preparation of PVA/PEDOT PSS Mixed solution: adding PVA to a PEDOT: PSS solution containing 5wt% DMSO, sealing and stirring for 5min, heating, stirring at room temperature for 2h to allow the mixed solution to cool naturally to obtain a mixed solution of PVA/PEDOT: PSS;
s2: PSS composite thermoelectric film rough product preparation: printing the PVA/PEDOT/PSS mixed solution obtained in the step S1 on a substrate by a screen printing technology, and performing vacuum drying at 80 ℃ for 12 hours to obtain a flexible PVA/PEDOT/PSS composite thermoelectric film rough finished product;
s3: water bath treatment: soaking the flexible PVA/PEDOT PSS composite thermoelectric film crude product obtained in the step S2 into deionized water, sealing and heating, washing by using the deionized water, and drying at 80 ℃ for 12 hours to obtain a water-bath-treated flexible PVA/PEDOT PSS composite thermoelectric film;
s4: and (3) DMSO post-treatment: and (4) placing the flexible PVA/PEDOT: PSS composite thermoelectric film subjected to water bath treatment obtained in the step (S3) in DMSO for soaking for 0.5h, then washing for 3 times by using deionized water, and performing vacuum drying for 12h at 80 ℃ to obtain the flexible PVA/PEDOT: PSS composite thermoelectric film.
2. The method for preparing the flexible PVA/PEDOT: PSS composite thermoelectric film according to claim 1, wherein in the step S1, the mass ratio of the PVA to the PEDOT: PSS solution is 1:1-1:50.
3. the method for preparing the flexible PVA/PEDOT: PSS composite thermoelectric film according to claim 1, wherein in step S1, the heating temperature is 40-95 ℃ and the heating time is 10-60min.
4. The method for preparing the flexible PVA/PEDOT: PSS composite thermoelectric film according to claim 1, wherein in step S2, the substrate is one of a nylon filter membrane, a polyvinylidene fluoride filter membrane or a polytetrafluoroethylene film.
5. The method for preparing the flexible PVA/PEDOT: PSS composite thermoelectric film according to claim 1, wherein in the step S3, the heating temperature is 40-95 ℃ and the heating time is 0.1-24h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116478577A (en) * | 2023-04-28 | 2023-07-25 | 陕西科技大学 | Direct-writing conductive ink stabilized by polymer and preparation and application methods thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116478577A (en) * | 2023-04-28 | 2023-07-25 | 陕西科技大学 | Direct-writing conductive ink stabilized by polymer and preparation and application methods thereof |
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