CN109666265B - Method for preparing PEDOT film in large area - Google Patents
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Abstract
The invention discloses a method for preparing a PEDOT film in a large area, which is characterized by comprising the following steps: 1) preparing a precursor solution; 2) preparing an EDOT monomer solution; 3) film forming of the precursor liquid; 4) film formation of PEDOT; 5) heat treatment of the transparent electrode; the invention designs a method for preparing a PEDOT film in a large area, which can directly prepare large-area transparent electrodes with excellent photoelectric property and mechanical flexibility on substrates with different areas at room temperature or a low temperature lower than 200 ℃ by an ink printing preparation process, has simple production steps and greatly reduces the production cost; the large-area transparent electrode prepared by the invention has good electrical properties.
Description
Technical Field
The invention relates to the field of organic photoelectron technical materials, in particular to a method for preparing a PEDOT film in a large area.
Background
Nowadays, photoelectric devices such as light emitting diodes and solar cells have been widely and importantly applied in many fields. All optoelectronic devices have at least one transparent electrode through which light can be absorbed or emitted from the device.
Poly (3, 4-ethylenedioxythiophene) (PEDOT) is one of the most interesting conducting polymers. The synthesized PEDOT film has a plurality of unique properties, such as excellent light transmission, high conductivity, good stability in air and the like, and has a great prospect as a transparent electrode in a photoelectric device.
At present, the technology for internationally synthesizing the PEDOT film is not mature enough, and the preparation technology of the large-area PEDOT film is complex, expensive and difficult to realize commercial production.
Therefore, the research on the preparation method of the large-area PEDOT film has strong practical significance and commercial value.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing a PEDOT film in a large area.
The technical scheme adopted for achieving the aim of the invention is that the method for preparing the PEDOT film in a large area is characterized by comprising the following steps:
1) preparation of precursor solution
1.1) mixing a transition metal oxide with an acid, stirring and standing to obtain a mixture A;
the mass and volume ratio (mmol: mL) of the transition metal oxide to the acid is (1-2): 5-10);
in the standing process: standing for 5-24 h;
1.2) diluting the mixture A obtained in the step 1.1) with an organic solvent A to obtain a mixture B;
the organic solvent A comprises one or more of methanol, ethanol, isopropanol or dimethyl sulfoxide;
the volume ratio of the mixture A to the organic solvent A is 1: 0.5-5;
1.3) adding a surfactant and resin into the mixture B obtained in the step 1.2) to obtain a precursor solution;
the volume ratio of the mixture B, the surfactant and the resin is 1: 0.005-0.05;
2) preparation of EDOT monomer solution
Mixing an EDOT monomer with an organic solvent B to obtain an EDOT monomer solution;
the organic solvent B comprises one or more of chloroform, dichloromethane, isopropanol, ethyl acetate or n-hexane;
the volume ratio of the EDOT monomer to the organic solvent B is 1: 0.5-30;
3) film formation from precursor solution
Uniformly coating the precursor solution obtained in the step 1.3) on a substrate to obtain the substrate uniformly covered with the precursor solution;
4) film formation of PEDOT
4.1) immersing the substrate obtained in the step 3) into the EDOT monomer solution obtained in the step 2) to obtain a substrate uniformly covering PEDOT;
4.2) immersing the substrate obtained in the step 4.1) into an organic solvent C to obtain a substrate with impurities removed;
the organic solvent C comprises one or more of methanol, ethanol or isopropanol;
the soaking time is 10 s-10 min;
5) heat treatment of PEDOT films
Carrying out constant-temperature heating treatment on the prepared substrate obtained in the step 4.2), and naturally cooling to room temperature to obtain a PEDOT film;
in the constant-temperature heating process: the temperature is 100-180 ℃ and the time is 5-120 min.
Further, the transition metal oxide in the step 1.1) comprises CuO and V2O5、Co3O4、MoO3Or MnO2One kind of (1).
Further, the acid in the step 1.1) comprises H2SO4、HCl、HNO3、CH4O3S、HOOCCH2COOH、HOOCCOOH、CH3COCOOH or CH3CH2CH2One kind of COOH.
Further, the stirring process in the step 1.1): the stirring speed range is 500-1000 rpm, and the time range is 10-120 min;
further, the surfactant in step 1.3) includes one or more of polyoxyethylene octylphenol ether, polyoxyethylene nonylphenol ether, high-carbon polyoxyethylene fatty alcohol ether, polyoxyethylene fatty acid ether, fatty acid methyl ester ethoxylate, sucrose fatty acid ester, polyoxyethylene fatty acid methyl ester, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monolaurate, polyoxyethylene octanol, polyoxyethylene lauryl ether, polyoxyethylene octylphenyl ether, or sodium lauryl sulfate.
Further, the resin in step 1.3) includes one or more of phenolic resin, epoxy resin, unsaturated polyester resin, amino resin, silicon ether resin, melamine formaldehyde resin, furfural phenol resin, furfural acetone resin, furfuryl alcohol resin, polybutadiene resin, organic silicon resin, urea resin, polyethylene resin, polypropylene resin, polyurethane resin, poly-1-butylene resin, polyvinyl chloride resin, polystyrene resin, polytetrafluoroethylene resin, polycarbonate resin, polyether sulfone resin, melamine formaldehyde resin, polyamide resin, polyvinyl alcohol or acrylic resin.
Further, the coating process in the step 3) includes a bar coating method, a nip extrusion coating method, an inkjet printing method, a roll-to-roll printing process, or a doctor blade preparation process.
Further, the substrates in the step 3) include a PET substrate, a polyethylene naphthalate substrate, a polyimide substrate and a glass substrate.
The technical effects of the present invention are undoubted, and the present invention has the following advantages:
1) the invention designs a method for preparing a PEDOT film in a large area, which can directly prepare large-area transparent electrodes with excellent photoelectric properties and mechanical flexibility on substrates with different areas at room temperature or a low temperature lower than 200 ℃ by a bar coating method, a slit type extrusion coating method, an ink-jet printing process, a roll-to-roll printing process, a scraper preparation process and the like, and has simple production steps and greatly reduced production cost;
2) the method disclosed by the invention can be used for directly preparing large-area low-resistance flexible transparent electrodes in a short time in a large scale without expensive vacuum or high-temperature preparation methods, so that the production cost is greatly reduced.
Drawings
FIG. 1 is a schematic diagram of a large-area PEDOT flexible transparent electrode structure;
fig. 2 is a display view of a transparent electrode prepared in embodiment 1.
Detailed Description
The present invention is further illustrated by the following examples, but it should not be construed that the scope of the above-described subject matter is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.
Example 1:
v in the examples2O5Purchased from western reagent, and EDOT monomer purchased from western reagent.
As shown in fig. 1, a method for preparing a PEDOT film in a large area includes the following steps:
1) preparation of precursor solution
1.1) preparation of transition Metal oxide V2O5Mixing with methanesulfonic acid, stirring and standing to obtain a mixture A;
the V is2O5The concentration of (A) is 0.03 mol/L;
in the stirring process: the stirring speed is 500-1000 rpm, and the time is 10-120 min;
in the standing process: standing for 5-24 h;
1.2) diluting the mixture A obtained in the step 1.1) with isopropanol to obtain a mixture B with a volume fraction of 1%;
1.3) adding a surfactant and resin into the mixture B obtained in the step 1.2) to obtain a precursor solution;
the surfactant is octyl phenyl polyoxyethylene ether (Triton X-100);
the resin is polyvinyl alcohol resin;
the volume sum of the surfactant and the resin accounts for 1 percent of the volume of the mixture B;
2) preparation of EDOT monomer solution
Mixing an EDOT monomer with an organic solvent B to obtain an EDOT monomer solution;
the organic solvent B comprises chloroform and n-hexane;
the volume ratio of the chloroform to the normal hexane is 1: 1;
the volume ratio of the organic solvent B to the EDOT monomer is 9: 1;
3) film formation from precursor solution
Uniformly coating the precursor solution obtained in the step 1.3) on a PET substrate by using a coating rod to obtain a substrate uniformly covering the precursor solution;
4) film formation of PEDOT
4.1) immersing the substrate obtained in the step 3) into the EDOT monomer solution obtained in the step 2) to obtain a substrate uniformly covering PEDOT;
4.2) immersing the substrate obtained in the step 4.1) into an organic solvent C to obtain a substrate with impurities removed;
the organic solvent C comprises methanol;
the soaking time is 30 s;
5) heat treatment of PEDOT films
Carrying out constant-temperature heating treatment on the prepared substrate obtained in the step 4.2), and naturally cooling to room temperature to obtain a PEDOT film shown in figure 2;
in the constant-temperature heating process: the temperature is 120 deg.C, and the time is 10 min.
Example 2:
v in the examples2O5Purchased from western reagent, and EDOT monomer purchased from western reagent.
A method for preparing a PEDOT film in a large area is characterized by comprising the following steps:
1) preparation of precursor solution
1.1) preparation of transition Metal oxide V2O5Mixing with methanesulfonic acid, stirring and standing to obtain a mixture A;
the V is2O5The concentration of (A) is 0.03 mol/L;
in the stirring process: the stirring speed is 500-1000 rpm, and the time is 10-120 min;
in the standing process: standing for 5-24 h;
1.2) diluting the mixture A obtained in the step 1.1) with an organic solvent methanol to obtain a mixture B;
1.3) adding a surfactant and resin into the mixture B obtained in the step 1.2) to obtain a precursor solution;
the surfactant is octyl phenyl polyoxyethylene ether (Triton X-100);
the resin is polyvinyl alcohol resin;
the volume sum of the surfactant and the resin accounts for 1 percent of the volume of the mixture B;
2) preparation of EDOT monomer solution
Mixing an EDOT monomer with an organic solvent B to obtain an EDOT monomer solution;
the organic solvent B comprises chloroform;
the volume ratio of the organic solvent B to the EDOT monomer is 9: 1;
3) film formation from precursor solution
Uniformly coating the precursor solution obtained in the step 1.3) on a PET substrate by using a coating rod to obtain a substrate uniformly covering the precursor solution;
4) film formation of PEDOT
4.1) immersing the substrate obtained in the step 3) into the EDOT monomer solution obtained in the step 2) to obtain a substrate uniformly covering PEDOT;
4.2) immersing the substrate obtained in the step 4.1) into an organic solvent C to obtain a substrate with impurities removed;
the organic solvent C comprises methanol;
the soaking time is 30 s;
5) heat treatment of PEDOT films
Carrying out constant-temperature heating treatment on the prepared substrate obtained in the step 4.2), and naturally cooling to room temperature to obtain a PEDOT film;
in the constant-temperature heating process: the temperature is 120 deg.C, and the time is 10 min.
As shown in table 1, the data of the transparent electrodes prepared in examples 1 and 2 are shown. From the data, the large-area transparent electrode prepared by the method has good electrical properties.
TABLE 1
| Square resistance omega sq-1 | |
| Example 1 | 90.6 |
| Example 2 | 101.4 |
Claims (9)
1. A method for preparing a PEDOT film in a large area is characterized by comprising the following steps:
1) preparation of precursor solution
1.1) mixing a transition metal oxide with an acid, stirring and standing to obtain a mixture A;
the mass and volume ratio of the transition metal oxide to the acid is (1-2): 5-10, wherein the unit of the mass is expressed in mmol, and the unit of the volume is expressed in mL;
in the standing process: standing for 5-24 h;
1.2) diluting the mixture A obtained in the step 1.1) with an organic solvent A to obtain a mixture B;
the organic solvent A comprises one or more of methanol, ethanol, isopropanol or dimethyl sulfoxide;
the volume ratio of the mixture A to the organic solvent A is 1: 0.5-5;
1.3) adding a surfactant and resin into the mixture B obtained in the step 1.2) to obtain a precursor solution;
the volume ratio of the mixture B, the surfactant and the resin is 1: 0.005-0.05;
2) preparation of EDOT monomer solution
Mixing an EDOT monomer with an organic solvent B to obtain an EDOT monomer solution;
the organic solvent B comprises one or more of chloroform, dichloromethane, isopropanol, ethyl acetate or n-hexane;
the volume ratio of the EDOT monomer to the organic solvent B is 1: 0.5-30;
3) film formation from precursor solution
Uniformly coating the precursor solution obtained in the step 1.3) on a substrate to obtain the substrate uniformly covered with the precursor solution;
4) film formation of PEDOT
4.1) immersing the substrate obtained in the step 3) into the EDOT monomer solution obtained in the step 2) to obtain a substrate uniformly covering PEDOT;
4.2) immersing the substrate obtained in the step 4.1) into an organic solvent C to obtain a substrate with impurities removed;
the organic solvent C comprises one or more of methanol, ethanol or isopropanol;
the soaking time is 10 s-10 min;
5) heat treatment of PEDOT films
Carrying out constant-temperature heating treatment on the prepared substrate obtained in the step 4.2), and naturally cooling to room temperature to obtain a PEDOT film;
in the constant-temperature heating process: the temperature is 100-180 ℃ and the time is 5-120 min.
2. The method for preparing the PEDOT film with the large area according to claim 1, wherein: the transition metal oxide in the step 1.1) comprises CuO and V2O5、Co3O4、MoO3Or MnO2One kind of (1).
3. The method for preparing the PEDOT film with the large area according to claim 1, wherein: said step 1The acid in 1) includes H2SO4、HCl、HNO3、CH4O3S、HOOCCH2COOH、HOOCCOOH、CH3COCOOH or CH3CH2CH2One kind of COOH.
4. The method for preparing the PEDOT film with the large area according to claim 1, wherein: the stirring process in the step 1.1): the stirring speed is 500-1000 rpm, and the time is 10-120 min.
5. The method for preparing the PEDOT film with the large area according to claim 1, wherein: the surfactant in the step 1.3) comprises one or more of octylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, high-carbon fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, sucrose fatty acid ester, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monolaurate or sodium dodecyl sulfate.
6. The method for preparing the PEDOT film with the large area according to claim 5, wherein: the higher fatty alcohol polyoxyethylene ether is octanol polyoxyethylene ether or lauryl alcohol polyoxyethylene ether.
7. The method for preparing the PEDOT film with the large area according to claim 1, wherein:
the resin in the step 1.3) comprises one or more of phenolic resin, epoxy resin, unsaturated polyester resin, amino resin, silicon ether resin, melamine formaldehyde resin, furfural phenol resin, furfural acetone resin, furfuryl alcohol resin, polybutadiene resin, organic silicon resin, urea resin, polyethylene resin, polypropylene resin, polyurethane resin, poly-1-butylene resin, polyvinyl chloride resin, polystyrene resin, polytetrafluoroethylene resin, polycarbonate resin, polyether sulfone resin, melamine formaldehyde resin, polyamide resin, polyvinyl alcohol or acrylic resin.
8. The method for preparing the PEDOT film with the large area according to claim 1, wherein: the coating process in the step 3) comprises a bar coating method, a slit type extrusion coating method, an ink-jet printing method, a roll-to-roll printing process or a scraper preparation process.
9. The method for preparing the PEDOT film with the large area according to claim 1, wherein: the substrate in the step 3) comprises a PET substrate, a polyethylene naphthalate substrate, a polyimide substrate and a glass substrate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103627255A (en) * | 2013-05-06 | 2014-03-12 | 苏州冷石纳米材料科技有限公司 | Nano-silver conductive ink and conductive film prepared by employing same |
| CN106992040A (en) * | 2017-04-10 | 2017-07-28 | 重庆大学 | A kind of novel processing step of PEDOT flexible transparent electrodes |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103627255A (en) * | 2013-05-06 | 2014-03-12 | 苏州冷石纳米材料科技有限公司 | Nano-silver conductive ink and conductive film prepared by employing same |
| CN106992040A (en) * | 2017-04-10 | 2017-07-28 | 重庆大学 | A kind of novel processing step of PEDOT flexible transparent electrodes |
Non-Patent Citations (1)
| Title |
|---|
| "高电导率聚(3,4-乙撑二氧噻吩)/木质素磺酸复合物的制备与结构表征";王婷;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20170215;第1.1.4节 * |
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