CN108780684B - Method for preparing flexible transparent electrode in large scale - Google Patents
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Abstract
The invention discloses a method for preparing a flexible transparent electrode in a large scale, which is characterized by comprising the following steps: 1) preprocessing a substrate; taking out the cleaned substrate, drying the substrate by using high-purity nitrogen, and treating the substrate in an ultraviolet ozone treatment instrument; 2) preparing a conductive solution based on a doped PEDOT PSS dispersion; placing the PEDOT PSS dispersion liquid and the acid solution into a container for mixing to obtain a conductive solution based on the doped PEDOT PSS dispersion liquid; the concentration range of acid in the conductive solution based on the PEDOT-PSS-doped dispersion liquid is 0.2-0.6 mol/L; the concentration range of the acid solution is 0.8-2 mol/L; 3) spinning the dispersion liquid; depositing the conductive solution obtained in the step 2) on the substrate obtained in the step 1) through a coating process; 5) heat treatment of the transparent electrode; heating the substrate covered with the conductive solution prepared in the step 3) at a constant temperature, and naturally cooling to room temperature to obtain a transparent electrode; the constant-temperature heating temperature range is 100-170 ℃, and the heating time is 5-120 min.
Description
Technical Field
The invention relates to the field of organic photoelectron technical materials, in particular to a method for preparing a flexible transparent electrode in a large scale.
Background
Transparent conductive electrodes are important components of a variety of electronic devices, including touch screens, displays, thin film solar cells, and the like. Currently, a metal oxide, such as an Indium Tin Oxide (ITO) film, is generally used for the transparent conductive electrode. Because the reserves of indium metal elements are limited, and simultaneously, the metal oxide film needs vacuum coating equipment and technology, the cost of the electrode rises due to various factors; more critically, metal oxides cannot be used in flexible devices that are becoming increasingly popular today due to their intrinsic fragility.
Research shows that the transparent electrode prepared based on poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid) (PEDOT: PSS) has high light transmittance, and the performance in flexibility can meet the requirements of people.
However, the square resistance of the electrode prepared from PEDOT and PSS is large, so that the conductivity of the electrode is lower than 1S/cm, and the application range of the electrode is greatly limited.
The conductivity of PEDOT (PSS) can be remarkably improved by surface treatment of acid or polar organic solvent after film formation. However, surface treatment increases the steps, time and complexity of industrial production, thereby increasing the production cost.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing a flexible transparent electrode in a large scale.
The technical scheme adopted for achieving the aim of the invention is that the method for preparing the flexible transparent electrode in a large scale is characterized by comprising the following steps:
1) pretreatment of substrates
Taking out the cleaned substrate, drying the substrate by using high-purity nitrogen, and treating the substrate in an ultraviolet ozone treatment instrument;
2) preparation of conductive solutions based on doped PEDOT PSS dispersions
Placing the PEDOT PSS dispersion liquid and the acid solution into a container for mixing to obtain a conductive solution based on the doped PEDOT PSS dispersion liquid;
the concentration range of acid in the conductive solution based on the PEDOT-PSS-doped dispersion liquid is 0.01-0.9 mol/L;
the concentration range of the acid solution is 0.8-2 mol/L;
3) spinning film of dispersion liquid
Depositing the conductive solution obtained in the step 2) on the substrate obtained in the step 1) through a coating process;
5) heat treatment of transparent electrodes
Heating the substrate covered with the conductive solution prepared in the step 3) at a constant temperature, and naturally cooling to room temperature to obtain a transparent electrode;
the constant-temperature heating temperature range is 100-170 ℃, and the heating time is 5-120 min.
Further, the cleaning process of the glass substrate in the step 1) comprises the following steps: placing the cut square glass substrate on a polytetrafluoroethylene cleaning support, placing the support in a container, sequentially adding deionized water, detergent, deionized water and acetone into the container, placing the container in an ultrasonic cleaner filled with water for cleaning, and repeating the step of cleaning with deionized water for a plurality of times; and after the cleaning is finished, replacing the solution in the container with isopropanol, and storing the cleaned glass substrate.
Further, the acid solution in the step 2) includes phosphoric acid (H)3PO4) Sulfuric acid (H)2SO4) Nitric acid (HNO)3) Pyrophosphoric acid (H)4P2O7) Perchloric acid (HClO)4) Methanesulfonic acid (CH)4SO3) Benzenesulfonic acid (C)6H6O3S), camphorsulfonic acid (C)10H16O4S), hydroxybenzenesulfonic acid (C)6H6O4S), 4-Chlorobenzenesulfonic acid (C)6H5ClO3S), p-toluenesulfonic acid (C)7H8O3S), 4-methoxybenzenesulfonic acid (C)7H8O4S), 4-Ethylbenzenesulfonic acid (C)8H10O3S), B-Naphthalenesulfonic acid (C)10H8O3S), dodecylbenzenesulfonic acid (C)18H30O3S), phosphorous acid (H)3PO3) Hexafluorophosphoric acid (HPF)6) Polyphosphoric acid (HO (HPO)3) H) and one or more of inorganic acids or organic acids having phosphate, sulfate, nitrate, chlorate and sulfonate.
Further, the mixing process in the step 2) is stirring or ultrasonic treatment; the stirring speed range is 500 rpm-1500 rpm, and the stirring time range is 5 min-12 hr.
Further, the substrate in the step 1) comprises a flexible plastic transparent substrate besides the rigid glass or quartz substrate material; the plastic transparent substrate includes a polyethylene terephthalate (PET), polyethylene naphthalate (PEN), or polyimide substrate (PI).
Further, the coating process in the step 3) includes a doctor blade preparation process, a rod coating process, a screen printing process, a slit extrusion coating process, an inkjet printing process or a printing process suitable for large-scale preparation besides the spin coating process.
It is worth mentioning that: by directly mixing a proper amount of acid solution with PEDOT PSS stock solution, the film formed has good optical property and electrical property, is simple to operate, can be used for large-scale preparation of flexible transparent electrodes, and has strong practical significance and commercial value.
The technical effects of the invention are undoubtedly, and the invention has the following advantages:
1) the invention designs a brand new solution formula based on PEDOT/PSS, and acid solution with a certain proportion is added into aqueous solution dispersion of the PEDOT/PSS, so that a brand new transparent electrode solution is formed. The electrode prepared by the solution can greatly reduce the square resistance, improve the conductivity of the electrode and simultaneously keep the original light transmittance and flexibility unchanged;
2) the preparation process of the electrode is simple and easy to operate, the electrode does not need to be subjected to post-treatment, a large amount of the electrode can be prepared in a short time, the production period is effectively shortened, the production cost is reduced, and large-scale commercial production is realized;
3) the invention can directly prepare transparent electrode films with excellent photoelectric property and mechanical flexibility on different substrates at room temperature or low temperature lower than 200 ℃ through ink printing preparation processes, such as spin coating, scraper preparation, rod coating, slot extrusion coating, ink-jet printing or roll-to-roll printing (roll-to-roll printing) and the like, and does not need surface treatment after film forming, thereby reducing preparation processes and production periods, lowering production cost and energy loss, and providing a feasible scheme for manufacturing flexible transparent electrodes on a large scale.
4) The performance of the flexible transparent electrode prepared by the invention is greatly improved, and a new method is provided for the application of the photoelectric device in the flexible direction in the later period.
Drawings
FIG. 1 is a schematic diagram of a doped PEDOT PSS transparent electrode;
FIG. 2 is a graph showing transmittance curves of the transparent electrodes prepared in examples 1 to 5 at a wavelength of 350 to 800 nm.
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:
in the examples, PEDOT: PSS was obtained from Heraeus, Germany under the product number PH 1000. Phosphoric acid and other chemicals were purchased from Adamas.
A method for preparing a flexible transparent electrode in a large scale is characterized by comprising the following steps:
1) pretreatment of substrates
1.1) cleaning of glass substrates
Placing the cut square glass substrate on a polytetrafluoroethylene cleaning support, placing the support in a beaker, sequentially adding deionized water, detergent, deionized water and acetone into the beaker, placing the beaker in an ultrasonic cleaner filled with water for cleaning, and repeating the step of cleaning with deionized water for multiple times; after cleaning, replacing the solution in the beaker with isopropanol, and storing the cleaned glass substrate;
1.2) Defect removal treatment of glass substrates
Taking out the glass substrate stored in the isopropyl ketone in the step 1.1), drying the glass substrate by using high-purity nitrogen, and taking out the glass substrate after the glass substrate is properly treated in an ultraviolet ozone treatment instrument;
2) preparation of conductive solutions based on doped PEDOT PSS dispersions
Putting the PEDOT PSS dispersion liquid and the phosphoric acid solution into a container for mixing, and putting the container on a magnetic stirrer for stirring to obtain a conductive solution based on the doped PEDOT PSS dispersion liquid;
the concentration of phosphoric acid in the conductive solution based on the PEDOT-PSS-doped dispersion liquid is 0.6 mol/L;
the concentration range of the phosphoric acid solution is 1-2 mol/L;
3) spinning film of dispersion liquid
Placing the glass substrate treated by ozone at the rotating center of a spin coater, uniformly covering a sample dispersion liquid, and starting the spin coater to spin a film;
4) heat treatment of transparent electrodes
Heating the substrate covered with the conductive solution prepared in the step 3) at constant temperature, and naturally cooling to room temperature to obtain the transparent electrode shown in the figure 1;
the constant temperature heating temperature range is 150 ℃, and the heating time is 15 min.
The transparent electrodes prepared in this example were tested to obtain the results shown in table 1. As shown in fig. 2, the transmittance curve of the transparent electrode prepared in this embodiment is within a wavelength range of 350 to 800 nm.
TABLE 1
Example 2:
in the examples, PEDOT: PSS was obtained from Heraeus, Germany under the product number PH 1000. Sulfuric acid and other chemicals were purchased from Adamas.
A method for preparing a flexible transparent electrode in a large scale is characterized by comprising the following steps:
1) pretreatment of substrates
1.1) cleaning of glass substrates
Placing the cut square glass substrate on a polytetrafluoroethylene cleaning support, placing the support in a beaker, sequentially adding deionized water, detergent, deionized water and acetone into the beaker, placing the beaker in an ultrasonic cleaner filled with water for cleaning, and repeating the step of cleaning with deionized water for multiple times; after cleaning, replacing the solution in the beaker with isopropanol, and storing the cleaned glass substrate;
1.2) Defect removal treatment of glass substrates
Taking out the glass substrate stored in the isopropyl ketone in the step 1.1), drying the glass substrate by using high-purity nitrogen, and taking out the glass substrate after the glass substrate is properly treated in an ultraviolet ozone treatment instrument;
2) preparation of conductive solutions based on doped PEDOT PSS dispersions
Putting the PEDOT PSS dispersion liquid and the sulfuric acid solution into a container for mixing, and putting the container on a magnetic stirrer for stirring to obtain a conductive solution based on the doped PEDOT PSS dispersion liquid;
the concentration of sulfuric acid in the conductive solution based on the doped PEDOT and PSS dispersion liquid is 0.1 mol/L;
the concentration range of the sulfuric acid solution is 0.8-1 mol/L;
3) spinning film of dispersion liquid
Placing the glass substrate treated by ozone at the rotating center of a spin coater, uniformly covering a sample dispersion liquid, and starting the spin coater to spin a film;
4) heat treatment of transparent electrodes
Heating the substrate covered with the conductive solution prepared in the step 3) at a constant temperature, and naturally cooling to room temperature to obtain a transparent electrode;
the constant temperature heating temperature range is 150 ℃, and the heating time is 15 min.
The transparent electrodes prepared in this example were tested to obtain the results shown in table 2. As shown in fig. 2, the transmittance curve of the transparent electrode prepared in this embodiment is within a wavelength range of 350 to 800 nm.
TABLE 2
Example 3:
in the examples, PEDOT: PSS was obtained from Heraeus, Germany under the product number PH 1000. Nitric acid and other chemicals were purchased from Adamas.
A method for preparing a flexible transparent electrode in a large scale is characterized by comprising the following steps:
1) pretreatment of substrates
1.1) cleaning of glass substrates
Placing the cut square glass substrate on a polytetrafluoroethylene cleaning support, placing the support in a beaker, sequentially adding deionized water, detergent, deionized water and acetone into the beaker, placing the beaker in an ultrasonic cleaner filled with water for cleaning, and repeating the step of cleaning with deionized water for multiple times; after the cleaning is finished, replacing the solution in the beaker with isopropanol, and storing the cleaned glass substrate;
1.2) Defect removal treatment of glass substrates
Taking out the glass substrate stored in the isopropyl alcohol in the step 1.1), drying by using high-purity nitrogen, putting the glass substrate into an ultraviolet ozone treatment instrument, and taking out the glass substrate after proper treatment;
2) preparation of conductive solutions based on doped PEDOT PSS dispersions
Putting the PEDOT PSS dispersion liquid and a nitric acid solution into a container for mixing, and putting the container on a magnetic stirrer for stirring to obtain a conductive solution based on the doped PEDOT PSS dispersion liquid;
the concentration of nitric acid in the conductive solution based on the doped PEDOT and PSS dispersion liquid is 0.6 mol/L;
the concentration range of the nitric acid solution is 1-2 mol/L;
3) spinning film of dispersion liquid
Placing the glass substrate treated by ozone at the rotating center of a spin coater, uniformly covering a sample dispersion liquid, and starting the spin coater to spin a film;
4) heat treatment of transparent electrodes
Heating the substrate covered with the conductive solution prepared in the step 3) at a constant temperature, and naturally cooling to room temperature to obtain a transparent electrode;
the constant temperature heating temperature range is 120 ℃, and the heating time is 10 min.
The transparent electrodes prepared in this example were tested to obtain the results shown in table 3. As shown in fig. 2, the transmittance curve of the transparent electrode prepared in this embodiment is within a wavelength range of 350 to 800 nm.
TABLE 3
Example 4:
in the examples, PEDOT: PSS was obtained from Heraeus, Germany under the product number PH 1000. Pyrophosphoric acid and other chemicals were purchased from Adamas.
A method for preparing a flexible transparent electrode in a large scale is characterized by comprising the following steps:
1) pretreatment of substrates
1.1) cleaning of glass substrates
Placing the cut square glass substrate on a polytetrafluoroethylene cleaning support, placing the support in a beaker, sequentially adding deionized water, detergent, deionized water and acetone into the beaker, placing the beaker in an ultrasonic cleaner filled with water for cleaning, and repeating the step of cleaning with deionized water for multiple times; after cleaning, replacing the solution in the beaker with isopropanol, and storing the cleaned glass substrate;
1.2) Defect removal treatment of glass substrates
Taking out the glass substrate stored in the isopropyl ketone in the step 1.1), drying the glass substrate by using high-purity nitrogen, and taking out the glass substrate after the glass substrate is properly treated in an ultraviolet ozone treatment instrument;
2) preparation of conductive solutions based on doped PEDOT PSS dispersions
Placing the PEDOT PSS dispersion liquid and the pyrophosphate solution into a container for mixing, placing the container on a magnetic stirrer for stirring, and obtaining a conductive solution based on the doped PEDOT PSS dispersion liquid;
the concentration of pyrophosphoric acid in the conductive solution based on the PEDOT-PSS-doped dispersion liquid is 0.2 mol/L;
the concentration range of the pyrophosphate solution is 0.8-1 mol/L;
3) spinning film of dispersion liquid
Placing the glass substrate treated by ozone at the rotating center of a spin coater, uniformly covering a sample dispersion liquid, and starting the spin coater to spin a film;
4) heat treatment of transparent electrodes
Heating the substrate covered with the conductive solution prepared in the step 3) at a constant temperature, and naturally cooling to room temperature to obtain a transparent electrode;
the constant temperature heating temperature range is 120 ℃, and the heating time is 10 min.
The transparent electrodes prepared in this example were tested to obtain the results shown in table 4. As shown in fig. 2, the transmittance curve of the transparent electrode prepared in this embodiment is within a wavelength range of 350 to 800 nm.
TABLE 4
Example 5:
in the examples, PEDOT: PSS was obtained from Heraeus, Germany under the product number PH 1000. Perchloric acid and other chemicals were purchased from Adamas.
A method for preparing a flexible transparent electrode in a large scale is characterized by comprising the following steps:
1) pretreatment of substrates
1.1) cleaning of glass substrates
Placing the cut square glass substrate on a polytetrafluoroethylene cleaning support, placing the support in a beaker, sequentially adding deionized water, detergent, deionized water and acetone into the beaker, placing the beaker in an ultrasonic cleaner filled with water for cleaning, and repeating the step of cleaning with deionized water for multiple times; after the cleaning is finished, replacing the solution in the beaker with isopropanol, and storing the cleaned glass substrate;
1.2) Defect removal treatment of glass substrates
Taking out the glass substrate stored in the isopropyl ketone in the step 1.1), drying the glass substrate by using high-purity nitrogen, and taking out the glass substrate after the glass substrate is properly treated in an ultraviolet ozone treatment instrument;
2) preparation of conductive solutions based on doped PEDOT PSS dispersions
Putting the PEDOT PSS dispersion liquid and a perchloric acid solution into a container for mixing, and putting the container on a magnetic stirrer for stirring to obtain a conductive solution based on the doped PEDOT PSS dispersion liquid;
the concentration of perchloric acid in the conductive solution based on the PEDOT-PSS-doped dispersion liquid is 0.2 mol/L;
the concentration range of the perchloric acid solution is 0.8-1 mol/L;
3) spinning film of dispersion liquid
Placing the glass substrate treated by ozone at the rotating center of a spin coater, uniformly covering a sample dispersion liquid, and starting the spin coater to spin a film;
4) heat treatment of transparent electrodes
Heating the substrate covered with the conductive solution prepared in the step 3) at a constant temperature, and naturally cooling to room temperature to obtain a transparent electrode;
the constant temperature heating temperature range is 120 ℃, and the heating time is 10 min.
The transparent electrodes prepared in this example were subjected to a test to obtain the results shown in table 5. As shown in fig. 2, the transmittance curve of the transparent electrode prepared in this embodiment is within a wavelength range of 350 to 800 nm.
TABLE 5
Claims (5)
1. A method for preparing a flexible transparent electrode in a large scale is characterized by comprising the following steps:
1) pretreatment of substrates
Taking out the cleaned substrate, drying the substrate by using high-purity nitrogen, and treating the substrate in an ultraviolet ozone treatment instrument;
2) based on doped PEDOT: preparation of conductive solution of PSS dispersion PEDOT: the PSS dispersion and the acid solution were mixed in a vessel to give a mixture based on doped PEDOT: (ii) a conductive solution of a PSS dispersion;
the concentration range of the acid solution is 0.8-2 mol/L, and the acid solution comprises one or more of inorganic acids or organic acids with phosphate radicals, sulfate radicals, nitrate radicals, chlorate radicals and sulfonate radicals, such as phosphoric acid, sulfuric acid, nitric acid, perchloric acid, methanesulfonic acid, benzenesulfonic acid, camphorsulfonic acid, hydroxybenzenesulfonic acid, chlorobenzenesulfonic acid, p-toluenesulfonic acid, 4-methoxybenzenesulfonic acid, 4-ethylbenzenesulfonic acid, B-naphthalenesulfonic acid, dodecylbenzenesulfonic acid, pyrophosphoric acid, phosphorous acid, hexafluorophosphoric acid, polyphosphoric acid and the like;
the doped PEDOT-based: the concentration range of acid in the conductive solution of the PSS dispersion liquid is 0.01-0.9 mol/L;
3) spinning film of dispersion liquid
Depositing the conductive solution obtained in the step 2) on the substrate obtained in the step 1) through a coating process;
4) heat treatment of transparent electrodes
Heating the substrate covered with the conductive solution prepared in the step 3) at a constant temperature, and naturally cooling to room temperature to obtain a transparent electrode;
the constant-temperature heating temperature range is 100-170 ℃, and the heating time is 5-120 min.
2. The method for the scalable preparation of the flexible transparent electrode according to claim 1, wherein the method comprises the following steps: the cleaning process of the glass substrate in the step 1) comprises the following steps: placing the cut square glass substrate on a polytetrafluoroethylene cleaning support, placing the support in a container, sequentially adding deionized water, detergent, deionized water and acetone into the container, placing the container in an ultrasonic cleaner filled with water for cleaning, and repeating the step of cleaning with deionized water for a plurality of times; and after the cleaning is finished, replacing the solution in the container with isopropanol, and storing the cleaned glass substrate.
3. The method for the scalable preparation of the flexible transparent electrode according to claim 1, wherein the method comprises the following steps: the mixing process in the step 2) is stirring or ultrasonic treatment; the stirring speed ranges from 500rpm to 1500rpm, and the stirring time ranges from 5min to 12 hr.
4. The method for the scalable preparation of the flexible transparent electrode according to claim 1, wherein the method comprises the following steps: the substrate in the step 1) comprises a flexible plastic transparent substrate besides a rigid glass or quartz substrate material; the plastic transparent substrate comprises a polyethylene terephthalate, polyethylene naphthalate or polyimide substrate.
5. The method for the scalable preparation of the flexible transparent electrode according to claim 1, wherein the method comprises the following steps: the coating process in the step 3) comprises a scraper preparation process, a rod coating process, a screen printing process, a slit type extrusion coating process, an ink-jet printing process or a roll-to-roll printing process, and is suitable for large-scale preparation besides the spin coating process of the step of the spin coating process of the spin coating process of the dip coating process of the spin coating process of the dip coating process of the dip coating process of the step 3) of the coating process of the dip coating process of the dip coating process.
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| US20100282998A1 (en) * | 2007-11-28 | 2010-11-11 | Dias H V Rasika | Poly(3,4-ethylenedioxythiophene) |
| CN102604334B (en) * | 2012-02-07 | 2013-08-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Self-supporting transparent highly-conductive poly-3,4-ethylenedioxythiophene (PEDOT) film and preparation method of the film |
| CN104672786B (en) * | 2015-03-11 | 2017-05-17 | 中国科学院理化技术研究所 | Water-soluble PEDOT-PSS dispersion and homogeneous polymerization preparation method thereof |
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| CN104851522A (en) * | 2015-05-21 | 2015-08-19 | 郑州大学 | Preparation method of large-area PEDOT/PSS transparent conductive film |
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| CN105914047A (en) * | 2016-04-14 | 2016-08-31 | 南京邮电大学 | Flexible transparent thin-film electrode and manufacturing method thereof |
| CN106297946A (en) * | 2016-08-09 | 2017-01-04 | 重庆大学 | A kind of preparation method of carbon electrode based on ink print technique |
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