CN108010637B - Preparation method of flexible transparent electrode - Google Patents
Preparation method of flexible transparent electrode Download PDFInfo
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- CN108010637B CN108010637B CN201711202618.6A CN201711202618A CN108010637B CN 108010637 B CN108010637 B CN 108010637B CN 201711202618 A CN201711202618 A CN 201711202618A CN 108010637 B CN108010637 B CN 108010637B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1343—Electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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Abstract
The invention provides a preparation method of a flexible transparent electrode, which comprises the steps of firstly preparing a PEDOT/PSS mixed solution and a nano silver wire mixed solution, then mixing the PEDOT/PSS mixed solution and the nano silver wire mixed solution, adding a catalyst, an alcohol solvent and a stabilizer, stirring under the conditions of constant-temperature water bath and sealing to obtain a coating solution with proper viscosity, finally coating the coating solution on a substrate, and curing to obtain the flexible transparent electrode. Has the advantages that: the oxidation resistance of the nano silver wire is improved, and the excellent conductivity and mechanical property of the nano silver wire are also kept; the nano silver wire transparent conductive film can be used as a built-in substituted ITO transparent conductive film, the manufacturing process is simple, the requirements of new technologies such as touch control and flexible display can be met, the equipment and material costs of the traditional ITO transparent conductive material are reduced, and the product reliability is improved.
Description
Technical Field
The invention relates to the technical field of display, in particular to a preparation method of a flexible transparent electrode.
Background
LCD (Liquid crystal display) is a widely used flat panel display, and mainly uses Liquid crystal switches to modulate the light field intensity of a backlight source to realize image display. The LCD display device includes a TFT (thin film Transistor) device, and the TFT-LCD is a thin film Transistor liquid crystal display, each liquid crystal pixel on the display device is driven by a thin film Transistor integrated behind the liquid crystal pixel, so that the liquid crystal display device has the characteristics of high response speed, high brightness, high contrast, small volume, low power consumption, no radiation and the like, and occupies a dominant position in the current display market.
The transparent electrode in the LCD is a thin film material with high conductivity and high visible light transmittance, and is a core element of optoelectronic devices such as light emitting diodes, solar cells, liquid crystal displays, touch panels, and the like. Currently, the most widely used transparent electrode material is a metal oxide semiconductor, such as Indium Tin Oxide (ITO) and the like. Despite its high conductivity, high transmittance, ITO still suffers from some inherent material property problems. Firstly, indium element in ITO is a scarce material, which is expensive and costly, and the storage of indium on earth has been far from meeting the increasing demand of people for transparent electrodes. Secondly, most of metal oxide semiconductors are ceramic materials, which are brittle and easy to break, and the conductivity of the thin film is easy to reduce, so that the metal oxide semiconductors are not suitable for being applied to flexible optoelectronic devices. Compared with metal oxide semiconductors and emerging carbon-based conductive materials (including polymer semiconductors, carbon nanotubes, graphene and the like), metals show good electrical and optical properties, and particularly, the silver nanowires are most prominent.
In the field of the existing liquid crystal display panel, stability is an important factor affecting the display quality of the liquid crystal display and other electronic devices. In which, because the nano silver wire is very easy to be oxidized, the conductivity and transmittance of the oxidized nano silver wire are obviously reduced. The existing nano silver wire is mainly applied by coating a protective layer on the surface of a nano silver wire film to play a role in blocking air; the existence of the protective layer limits the application of the protective layer in certain fields, such as the application of replacing ITO in LCD as a liquid crystal display; in addition, because the protective layer typically requires several hundred nanometers, and the tendency of LCDs to be thinner has become more apparent in recent years, the presence of the protective layer can significantly increase the thickness of the LCD cell; moreover, the existence of the protective layer can also increase the distance of an electric field in the LCD and generate unnecessary influence on the rotation of the liquid crystal; finally, it is unknown whether the addition of the protective layer will react to the alignment layer and the liquid crystal. Therefore, the above reason is a main factor that restricts the application of the nano silver wire to the display device.
In addition, in the prior art, poly (3, 4-ethylenedioxythiophene) doped poly (4-styrenesulfonic acid) (PEDOT/PSS) is a colloid of gel particles formed by water dispersion, is the most successful conductive polymer developed at present, and the PEDOT/PSS colloid gel particles have very stable conductive doping state, excellent plasticity, electromagnetic performance, electrochemical stability and good light transmission. Therefore, the nano silver wire can be applied to printing organic electronics, flexible displays, transparent electrodes, touch screens, solar cells and the like, and at the present stage, PEDOT/PSS is generally selected to wrap the nano silver wire to replace ITO in LCDs.
Disclosure of Invention
The invention provides a preparation method of a flexible transparent electrode, which is used for replacing the traditional transparent electrode material and reducing the adverse effect brought by a protective layer when the traditional nano silver wire material is applied.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the invention provides a preparation method of a flexible transparent electrode, which comprises the following steps:
step S10, preparing PEDOT/PSS mixed solution and nano silver wire mixed solution;
step S20, mixing the PEDOT/PSS mixed solution and the nano silver wire mixed solution, adding a catalyst, an alcohol solvent and a stabilizer to obtain a mixed solution A, and stirring for 3-120 min in a constant-temperature water bath at 50-100 ℃ and under a sealed condition;
and step S30, uniformly coating the mixed solution A on a substrate base plate to obtain the flexible transparent electrode.
According to a preferred embodiment of the present invention, the step of preparing the PEDOT/PSS mixed solution and the nano silver wire mixed solution comprises:
preparing a PEDOT/PSS mixed solution, wherein the PEDOT/PSS mixed solution comprises 3, 4-ethylenedioxythiophene and polystyrene sulfonic acid, the mass fraction of the 3, 4-ethylenedioxythiophene is 0.5% -5%, and the mass fraction of the polystyrene sulfonic acid is 0.5% -5%;
preparing a mixed solution of the carboxylated nano silver wires with the mass fraction of 0.5-3%.
According to a preferred embodiment of the present invention, the step of preparing the PEDOT/PSS mixing solution and the nano silver wire mixing solution comprises:
preparing a PEDOT/PSS mixed solution with the mass fraction of 1% -10%, wherein the PEDOT/PSS in the mixed solution is one or two of long-chain PEDOT/PSS and granular PEDOT/PSS;
preparing a nano silver wire mixed solution with the mass fraction of 0.3-5%.
According to a preferred embodiment of the present invention, the mixed solution of the nano silver wire is subjected to pre-soaking or ultraviolet irradiation treatment.
According to a preferred embodiment of the present invention, the mass fraction of the catalyst is 1% to 3%, the mass fraction of the alcohol solvent is 90% to 95%, and the mass fraction of the stabilizer is 1% to 5%.
According to a preferred embodiment of the present invention, the catalyst is a high molecular compound containing an imidazole group or a phenol group;
the alcohol solvent is one of methanol, ethanol, isopropanol and glycerol;
the stabilizer is one of benzophenones, benzotriazoles, octyloxyphenols and phosphites.
According to a preferred embodiment of the present invention, the length of the silver nanowire in the silver nanowire mixed solution is 5 to 30 um.
According to a preferred embodiment of the present invention, the step of uniformly coating the mixed solution a on a substrate base to obtain the flexible transparent electrode comprises:
uniformly coating the mixed solution A on a substrate by a spin coater, wherein the coating time is T1;
increasing the rotation speed of a spin coater to enable the mixed solution A to be uniformly distributed on the substrate, wherein the duration is T2;
and curing to obtain the flexible transparent electrode.
According to a preferred embodiment of the present invention, the spin coater has a set rotation speed of 400 to 2500r/min, the T1 is 2 to 10s, and the T2 is 2 to 10 s.
According to a preferred embodiment of the present invention, the substrate is selected from one of silicon wafer, glass, gold sheet, silver sheet, polyester film, polyimide film, polyethylene film, polypropylene film, silicon rubber or polytetrafluoroethylene.
The invention has the beneficial effects that: compared with the prior art, the PEDOT/PSS mixed solution and the nano silver wire mixed solution are fully mixed, so that the PEDOT-coated nano silver wire in the PEDOT/PSS mixed solution is used for forming a film, the contact between the nano silver wire and air is blocked, the oxidation resistance of the nano silver wire is improved, and the excellent conductivity and mechanical property of the nano silver wire are retained; in addition, the PEDOT-coated silver nanowire has a simpler preparation and storage process, can achieve a better coating effect during coating, and provides more guarantee and support for the application of the PEDOT-coated silver nanowire on ITO substituted materials and flexible displays; finally, the nano silver wire transparent conductive film can be used as a built-in substituted ITO transparent conductive film, the manufacturing process is simple, the requirements of new technologies such as touch control and flexible display can be met, the equipment and material costs of the traditional ITO transparent conductive material are reduced, and the product reliability is improved.
Drawings
In order to illustrate the embodiments or the technical solutions in the prior art more clearly, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the invention, and it is obvious for a person skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for manufacturing a flexible transparent electrode according to a preferred embodiment of the present invention.
Detailed Description
The following description of the various embodiments refers to the accompanying drawings that illustrate specific embodiments in which the invention may be practiced. The directional terms mentioned in the present invention, such as [ upper ], [ lower ], [ front ], [ rear ], [ left ], [ right ], [ inner ], [ outer ], [ side ], are only referring to the directions of the attached drawings. Accordingly, the directional terms used are used for explanation and understanding of the present invention, and are not used for limiting the present invention. In the drawings, elements having similar structures are denoted by the same reference numerals.
The invention provides a preparation method of a flexible transparent electrode, because the traditional transparent electrode material needs to be coated with a protective layer to isolate the contact of oxygen and nano silver wires, the existence of the protective layer limits the application of the nano silver wires in certain fields, such as the application of replacing ITO in LCD as a liquid crystal display; in addition, because the protective layer typically requires several hundred nanometers, and the tendency of LCDs to be thinner has become more apparent in recent years, the presence of the protective layer can significantly increase the thickness of the LCD cell; moreover, the existence of the protective layer can also increase the distance of the electric field in the LCD, and generate unnecessary influence on the rotation of the liquid crystal, and the technical problem can be solved by the embodiment.
Fig. 1 is a schematic flow chart of a method for manufacturing a flexible transparent electrode according to a preferred embodiment of the present invention, including:
step S10, preparing PEDOT/PSS mixed solution and nano silver wire mixed solution;
in a preferred embodiment of the present invention, a PEDOT/PSS mixed solution and a silver nanowire mixed solution are first prepared, and the preparation method of the mixed solution includes:
(1) preparing a mixed solution of 0.5-5% of 3, 4-ethylenedioxythiophene and 0.5-5% of polystyrene sulfonic acid by mass fraction and preparing a mixed solution of 0.5-3% of carboxylated nano-silver wires by mass fraction,
wherein the 3, 4-ethylenedioxythiophene belongs to PEDOT class, and the polystyrene sulfonic acid belongs to PSS class;
(2) preparing a PEDOT/PSS mixed solution with the mass fraction of 1-10%, wherein the PEDOT/PSS in the mixed solution is one or a mixture of two of long-chain PEDOT/PSS and granular PEDOT/PSS, and preparing a nano-silver wire mixed solution with the mass fraction of 0.3-5%,
the PEDOT/PSS in the mixed solution can also comprise PEDOT/PSS after heating treatment;
in addition, in the mixed solution PEDOT/PSS, a large number of-H groups are arranged on the surface of the PEDOT/PSS; therefore, the nano silver wire solution mixed with the mixed solution needs to be soaked in advance or irradiated by ultraviolet rays, so that the surface of the nano silver wire solution is rich in a large amount of-OH, the PEDOT/PSS can be more tightly coated on the surface of the nano silver wire, and the density is as high as more than 99%;
specifically, in a preferred embodiment of the present invention, the length of the silver nanowire in the silver nanowire mixed solution is 5 to 30um, wherein the preferred length is 15 um; the solvent selected may be a common solvent, among which alcohol solvents are preferred.
Step S20, mixing the PEDOT/PSS mixed solution and the nano silver wire mixed solution, adding a catalyst, an alcohol solvent and a stabilizer to obtain a mixed solution A, and stirring for 3-120 min in a constant-temperature water bath at 50-100 ℃ and under a sealed condition;
in a preferred embodiment of the invention, firstly, the PEDOT/PSS mixed solution and the nano-silver wire mixed solution are mixed, and a catalyst, an alcohol solvent and a stabilizer are added into the mixed solution to obtain a mixed solution A, wherein the mass fraction of the catalyst is 1-3%, the mass fraction of the alcohol solvent is 90-95%, and the mass fraction of the stabilizer is 1-5%;
preferably, the catalyst is a macromolecular compound containing an imidazolyl group or a phenol group; the alcohol solvent is one of methanol, ethanol, isopropanol and glycerol; the stabilizer is one of benzophenones, benzotriazoles, octyloxyphenols and phosphites;
secondly, placing the mixed solution A in a constant-temperature water bath at 50-100 ℃ and sealing, and stirring the mixed solution A for 3-120 min; specifically, the temperature of the thermostatic water bath is preferably 70 ℃, and the stirring time is preferably 60 min.
And step S30, uniformly coating the mixed solution A on a substrate base plate to obtain the flexible transparent electrode.
In a preferred embodiment of the present invention, a regulator is added to the mixed solution a to obtain a coating mixed solution a with a suitable viscosity and a solid content, wherein the regulating solvent is generally selected from alcohol solvents such as isopropyl alcohol.
Firstly, uniformly coating the mixed solution A on a substrate by a spin coater to obtain a wet film, wherein the coating time is T1; then, increasing the rotation speed of the spin coater to uniformly distribute the mixed solution on the substrate or throwing out the redundant mixed solution A, so that the solution of the whole substrate is uniform, and the duration is T2; finally, curing to obtain the flexible transparent electrode;
in this embodiment, the substrate is selected from one of silicon wafer, glass, gold sheet, silver sheet, polyester film, polyimide film, polyethylene film, polypropylene film, silicon rubber or polytetrafluoroethylene;
in the embodiment, the set rotating speed of the spin coater is 400-2500 r/min, and specific numerical values are selected according to real conditions;
in the first stage, namely the coating stage, the T1 is 2-10 s; in the second stage, the T2 is 2-10 s;
in addition, the curing treatment is to pre-test and post-bake the wet film in an environment of 40-120 ℃ and cure the transparent electrode material; in the subsequent operation, the patterning process can be directly carried out on the basis of the above steps.
The invention provides a preparation method of a flexible transparent electrode, which comprises the steps of firstly preparing a PEDOT/PSS mixed solution and a nano silver wire mixed solution, then mixing the PEDOT/PSS mixed solution and the nano silver wire mixed solution, adding a catalyst, an alcohol solvent and a stabilizer, stirring under the conditions of constant-temperature water bath and sealing to obtain a coating solution with proper viscosity, finally coating the coating solution on a substrate, and curing to obtain the flexible transparent electrode; according to the invention, the PEDOT is used for coating the nano silver wire to form a film, so that the contact between the nano silver wire and the air is blocked, the oxidation resistance of the nano silver wire is improved, and the excellent conductivity and mechanical property of the nano silver wire are also kept; in addition, the PEDOT-coated silver nanowire has a simpler preparation and storage process, can achieve a better coating effect during coating, and provides more guarantee and support for the application of the PEDOT-coated silver nanowire on ITO substituted materials and flexible displays; finally, the nano silver wire transparent conductive film can be used as a built-in substituted ITO transparent conductive film, the manufacturing process is simple, the requirements of new technologies such as touch control and flexible display can be met, the equipment and material costs of the traditional ITO transparent conductive material are reduced, and the product reliability is improved.
In summary, although the present invention has been described with reference to the preferred embodiments, the above-described preferred embodiments are not intended to limit the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, therefore, the scope of the present invention shall be determined by the appended claims.
Claims (6)
1. A method for preparing a flexible transparent electrode is characterized by comprising the following steps:
step S10, preparing PEDOT/PSS mixed solution and nano silver wire mixed solution;
step S20, mixing the PEDOT/PSS mixed solution and the nano silver wire mixed solution, adding a catalyst, an alcohol solvent and a stabilizer to obtain a mixed solution A, and stirring for 3-120 min in a constant-temperature water bath at 50-100 ℃ and under a sealed condition;
step S30, uniformly coating the mixed solution A on a substrate to obtain the flexible transparent electrode;
wherein the mass fraction of the catalyst is 1-3%, the mass fraction of the alcohol solvent is 90-95%, and the mass fraction of the stabilizer is 1-5%;
the catalyst is a macromolecular compound containing imidazolyl or phenolic groups;
the alcohol solvent is one of methanol, ethanol, isopropanol and glycerol;
the stabilizer is one of benzophenones, benzotriazoles, octyloxyphenols and phosphites;
the preparation method of the PEDOT/PSS mixed solution and the nano silver wire mixed solution comprises the following steps:
preparing a PEDOT/PSS mixed solution, wherein the PEDOT/PSS mixed solution comprises 3, 4-ethylenedioxythiophene and polystyrene sulfonic acid, the mass fraction of the 3, 4-ethylenedioxythiophene is 0.5% -5%, and the mass fraction of the polystyrene sulfonic acid is 0.5% -5%;
preparing a mixed solution of the carboxylated nano silver wires with the mass fraction of 0.5-3%.
2. The method according to claim 1, wherein the mixed solution of the nano silver wire is subjected to pre-soaking or ultraviolet irradiation.
3. The method according to claim 1, wherein the length of the silver nanowires in the mixed solution of silver nanowires is 5 to 30 um.
4. The method according to claim 1, wherein the step of uniformly applying the mixed solution a on a substrate base to obtain the flexible transparent electrode comprises:
uniformly coating the mixed solution A on a substrate by a spin coater, wherein the coating time is T1;
increasing the rotation speed of a spin coater to enable the mixed solution A to be uniformly distributed on the substrate, wherein the duration is T2;
and curing to obtain the flexible transparent electrode.
5. The method according to claim 4, wherein the spin coater is set to rotate at a speed of 400 to 2500r/min, the T1 is set to 2 to 10s, and the T2 is set to 2 to 10 s.
6. The method according to claim 1, wherein the substrate base plate is one selected from a silicon wafer, glass, gold plate, silver plate, polyester film, polyimide film, polyethylene film, polypropylene film, silicone rubber, and polytetrafluoroethylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711202618.6A CN108010637B (en) | 2017-11-27 | 2017-11-27 | Preparation method of flexible transparent electrode |
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