CN108089366B - Color film substrate and preparation method thereof - Google Patents
Color film substrate and preparation method thereof Download PDFInfo
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- CN108089366B CN108089366B CN201711275653.0A CN201711275653A CN108089366B CN 108089366 B CN108089366 B CN 108089366B CN 201711275653 A CN201711275653 A CN 201711275653A CN 108089366 B CN108089366 B CN 108089366B
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- ethylenedioxythiophene
- polystyrene sulfonate
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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
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133509—Filters, e.g. light shielding masks
- G02F1/133514—Colour filters
- G02F1/133516—Methods for their manufacture, e.g. printing, electro-deposition or photolithography
Abstract
The invention provides a color film substrate and a preparation method thereof, wherein the method comprises the following steps: firstly, providing a substrate, preparing a color film color resistance layer on the substrate, and coating a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material subjected to high-resistance low-viscosity treatment on the color film color resistance layer to form a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate film; then, performing preset treatment on the surface of the substrate coated with the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material to convert the membrane surface structure of the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate membrane into a low-resistance state, and performing curing treatment; finally, the poly 3, 4-ethylenedioxythiophene-sodium polystyrene sulfonate film is patterned to form a transparent electrode.
Description
Technical Field
The invention relates to the technical field of liquid crystal display, in particular to a color film substrate and a preparation method thereof.
Background
The transparent electrode is a transparent and conductive material, and is widely used in solar cells, panel displays, touch screens, PDP displays, OLED displays, and other related technologies. Transparent electrodes generally require as low a resistance as possible, as high a transmittance, and a simple fabrication process to ensure as low a cost as possible. Indium tin oxide ITO is widely used as an electrode in the above devices, and although the devices have good light transmittance and conductivity, the sputtering film formation equipment thereof has high cost and high patterning difficulty. In terms of flexibility, the ITO material is brittle, which limits its application to emerging flexible electronic devices due to the hardness of the thin film. In addition, the lack of indium raw material makes the application of ITO thin film in common electronic products increasingly limited.
And the organic polymer material PEDOT, namely PSS, has higher transmittance and lower resistance after film formation, has good stability in air, and also has excellent expression in the aspect of flexible electrodes. However, due to the presence of the conformational isomerism structure, PEDOT: PSS has a relatively high viscosity while having a low electrical resistance. However, high viscosity is an important factor that restricts the coating characteristics of the mainstream large-area coating apparatus IJP and Slit Coater. Currently, PEDOT: the PSS is mainly applied to small size by a spin coating mode, but the existing spin coating mode can not carry out large-area film formation, which greatly restricts the application and development of large-area and patterning of the novel conductive material with great potential.
In summary, the conventional organic polymer material PEDOT: PSS has a relatively high viscosity, and is greatly restricted in large-area film formation and application in large-size display panels.
Disclosure of Invention
The invention provides a color film substrate and a preparation method thereof, which can enable organic polymer material PEDOT (PSS) to be uniformly formed into a film on a large-size display panel, thereby forming a transparent electrode with high transmittance and low resistance.
In order to solve the above problems, the technical scheme provided by the invention is as follows:
the invention provides a preparation method of a color film substrate, which comprises the following steps:
step S1, providing a substrate, preparing a color film color resistance layer on the substrate, and coating the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material which are subjected to high-resistance low-viscosity treatment on the color film color resistance layer to form a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate film;
step S2, performing preset treatment on the surface of the substrate coated with the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate materials to convert the membrane surface structure of the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate membrane into a low-resistance state, and performing curing treatment;
and step S3, patterning the poly 3, 4-ethylenedioxythiophene-sodium polystyrene sulfonate film to form a transparent electrode.
According to a preferred embodiment of the present invention, the coating of the sodium polystyrene sulfonate material of poly-3, 4-ethylenedioxythiophene and poly-4-ethylenedioxythiophene subjected to high resistance and low viscosity treatment on the color filter color resistance layer includes the following steps:
step S101, adding sodium polystyrene sulfonate, 3, 4-ethylenedioxythiophene, alcohol compounds and deionized water into a reaction bottle, and stirring until the sodium polystyrene sulfonate, the 3, 4-ethylenedioxythiophene, the alcohol compounds and the deionized water are completely dissolved;
step S102, adding an oxidant, a catalyst and glycerol to react to form an aqueous dispersion containing the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate;
s103, filtering and purifying the aqueous dispersion, finally diluting the precipitate with deionized water, and performing ultrasonic dispersion to obtain a dark blue aqueous dispersion containing the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate;
s104, filtering the poly 3, 4-ethylenedioxythiophene, namely sodium polystyrene sulfonate aqueous dispersion, adding an organic auxiliary agent at least containing isopropanol, and stirring until the organic auxiliary agent is dissolved to obtain a poly 3, 4-ethylenedioxythiophene, namely sodium polystyrene sulfonate material with a high-resistance low-viscosity structure;
and S105, coating the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material on the color film color resistance layer through coating equipment.
According to a preferred embodiment of the present invention, the stirring temperature in the steps S101 and S104 is 20 to 60 ℃.
According to a preferred embodiment of the present invention, the reaction time of step S102 is 8-24 hours.
According to a preferred embodiment of the present invention, in step S103, the filtering and purifying operation is performed by using anion-cation exchange resin, the water dispersion is centrifuged, the precipitate is diluted with distilled water and then dispersed and dissolved again, and the process is repeated for 3 to 5 times.
According to a preferred embodiment of the present invention, the amount of the isopropanol added is 3% to 60% of the volume of the solution of poly-3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate.
According to a preferred embodiment of the present invention, the viscosity of the poly 3, 4-ethylenedioxythiophene-sodium polystyrene sulfonate material with the high resistance and low viscosity structure is 8-30 cps.
According to a preferred embodiment of the present invention, the step S2 includes:
and spraying ethylene glycol on the poly 3, 4-ethylenedioxythiophene sodium polystyrene sulfonate film of the substrate for surface treatment to convert the film surface structure of the poly 3, 4-ethylenedioxythiophene sodium polystyrene sulfonate film into a low-resistance high-viscosity state, and then carrying out curing treatment.
According to a preferred embodiment of the present invention, after the curing treatment, the thickness of the poly 3, 4-ethylenedioxythiophene-sodium polystyrene sulfonate film is 50-2500 nm.
The invention also provides a color film substrate prepared by the preparation method.
The invention has the beneficial effects that: compared with the color film substrate in the prior art, the color film substrate and the preparation method thereof utilize the conformational isomerism principle of PEDOT: PSS (poly 3, 4-ethylenedioxythiophene: sodium polystyrene sulfonate), firstly, isopropanol is used for treating the PEDOT: PSS to reduce the viscosity of the PEDOT: PSS, so that the viscosity of the PEDOT: PSS can be well matched with equipment, the uniformity of large-area film formation is ensured, a solution with low viscosity after treatment is coated on the color film substrate or the glass substrate which is not subjected to the ITO process through an Ink Jet Printer (IJP) or quantitative spin coating equipment (Slit Coater), and then, the surface treatment is carried out through ethylene glycol, so that the PEDOT coated on the glass: PSS is converted into a structure with high viscosity and low resistance so as to meet the use requirement of the low-resistance transparent conductive film. Therefore, the difficult problem that large-area (2200 x 2500mm can be increased) film formation of PEDOT and PSS is difficult is solved, the air stability of the PEDOT and PSS is good, the requirements of the existing flexible transparent electrode can be completely met, the material cost is greatly saved, and the processing equipment and the flow are simplified.
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 flowchart illustrating a manufacturing process of a color filter substrate according to a first embodiment of the present invention;
fig. 2 is a flowchart of a process for preparing a PEDOT/PSS film of a color film substrate according to a first embodiment of the present invention;
fig. 3 is a flowchart of a manufacturing method of a color filter substrate according to a second 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 aims at the technical problem that PSS, an organic polymer material PEDOT, is greatly restricted in large-area film forming and application of large-size display panels due to relatively high viscosity in the existing color film substrate, and the embodiment can solve the defect.
The color film substrate and the method for manufacturing the color film substrate according to the embodiments of the present invention are described in detail below with reference to the accompanying drawings.
As shown in fig. 1, a flow chart for manufacturing a color filter substrate according to a first embodiment of the present invention includes the following steps:
step S1, providing a substrate, preparing a color film color resistance layer on the substrate, and coating the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material which are subjected to high-resistance low-viscosity treatment on the color film color resistance layer to form a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate film;
step S2, performing preset treatment on the surface of the substrate coated with the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate materials to convert the membrane surface structure of the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate membrane into a low-resistance state, and performing curing treatment;
and step S3, patterning the poly 3, 4-ethylenedioxythiophene-sodium polystyrene sulfonate film to form a transparent electrode.
As shown in fig. 2, the step of coating the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material subjected to high resistance and low viscosity treatment on the color film color resistance layer specifically includes the following steps:
step S101, adding sodium polystyrene sulfonate, 3, 4-ethylenedioxythiophene, alcohol compounds and deionized water into a reaction bottle, and stirring until the sodium polystyrene sulfonate, the 3, 4-ethylenedioxythiophene, the alcohol compounds and the deionized water are completely dissolved;
step S102, adding an oxidant, a catalyst and glycerol to react to form an aqueous dispersion containing the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate;
s103, filtering and purifying the aqueous dispersion, finally diluting the precipitate with deionized water, and performing ultrasonic dispersion to obtain a dark blue aqueous dispersion containing the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate;
s104, filtering the poly 3, 4-ethylenedioxythiophene, namely sodium polystyrene sulfonate aqueous dispersion, adding an organic auxiliary agent at least containing isopropanol, and stirring until the organic auxiliary agent is dissolved to obtain a poly 3, 4-ethylenedioxythiophene, namely sodium polystyrene sulfonate material with a high-resistance low-viscosity structure;
and S105, coating the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material on the color film color resistance layer through coating equipment.
The preparation of the high-resistance low-viscosity poly 3, 4-ethylenedioxythiophene sodium polystyrene sulfonate (PEDOT: PSS) material mainly comprises the following two steps:
firstly, adding sodium polystyrene sulfonate (PSS), 3, 4-Ethylenedioxythiophene (EDOT), alcohol compounds and deionized water into a reaction bottle, stirring at 30-50 ℃, and completely dissolving; then adding an oxidant, a catalyst and glycerol, and reacting for 12-24 hours to form an aqueous dispersion containing the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate; and filtering and purifying the aqueous dispersion through anion and cation exchange resin, centrifuging the aqueous dispersion, removing supernatant, diluting the precipitate with distilled water, dispersing and dissolving again, repeating the centrifugation operation for 3-5 times, preferably 3 times, finally diluting the precipitate with deionized water, and performing ultrasonic dispersion for 1h to obtain the deep blue aqueous dispersion containing PEDOT and PSS.
And secondly, filtering the prepared PEDOT PSS solution, adding an organic auxiliary agent at least containing isopropanol and the like, stirring at 20-60 ℃ until the solution is completely dissolved, wherein the stirring temperature is preferably 30-50 ℃, the structure of the solution is changed from long-chain low-resistance high-viscosity structure to short-chain high-resistance low-viscosity structure, and the addition amount of the isopropanol is 3-60% of the volume of the PEDOT PSS, and is preferably 5-50%. Samples were taken during mixing to monitor and obtain the PEDOT: PSS material at a viscosity of 8-30cps, preferably 8-20cps, for IJP/Slit Coater coating.
Wherein the molecular formula of the PSS is as follows: (C)8H7NO3S)XThe PSS is a light yellow solid and is easy to dissolve in water, and is applied to reactive emulsifiers, water-soluble polymers (coagulants, dispersants and the like), water treatment agents (dispersants, flocculants), sulfur exchange resins (membranes) and the like, and the structural formula of the PSS is listed as follows:
the molecular formula of EDOT is C6H6O2The method is mainly used for synthesizing a conductive polymer, namely poly 3, 4-ethylenedioxythiophene (PEDOT), wherein the PEDOT has the advantages of low energy gap, low electrochemical doping potential, short response time, high color change contrast, good stability and the like, and can generate reversible color change between sky blue and transparency under the action of an external electric field. The structural formula of PEDOT is listed below:
after the raw materials containing the PSS and the EDOT are reacted, the PEDOT PSS with a long-chain structure is generated, the characteristics of low resistance and high viscosity are achieved, however, the high viscosity is an important factor for restricting the coating characteristics of mainstream large-area coating equipment IJP and Slit Coater, and the PEDOT PSS material cannot be applied to large-size substrates. In the process of preparing the PEDOT/PSS material, the isopropanol organic auxiliary agent is added, so that the structure of the PEDOT/PSS is changed from a long-chain structure with low resistance and high viscosity to a short-chain structure with high resistance and low viscosity, namely the original conformation of the PEDOT/PSS is changed by utilizing the conformational isomerization principle of the PEDOT/PSS. PSS, wherein the organic auxiliary agent can also be other organic auxiliary agents, and the structural formula of the PEDOT which presents short chain after the conformation is changed is listed as follows:
the high resistance low viscosity PEDOT: PSS material obtained from the above procedure can be used to coat large size substrates (up to 2200 x 2500 mm). PSS material can be coated in one of the following two ways: firstly, the PEDOT PSS material with high resistance and low viscosity is sprayed on a substrate processed in advance by an IJP device to obtain a uniform PEDOT PSS film which can be patterned. Secondly, coating the PEDOT PSS material with high resistance and low viscosity on a substrate processed in advance by using Slit Coater equipment to obtain the PEDOT PSS film with uniform film surface. Wherein the film surface with good uniformity of different film thickness can be obtained by controlling the sample discharge amount of the IJP device and the spray rate change of the Slit Coater device. The PEDOT PSS material can be coated by other devices and corresponding modes.
And spraying ethylene glycol on the PEDOT/PSS film of the substrate in a small droplet mode for surface treatment to convert the surface structure of the PEDOT/PSS film into a low-resistance and high-viscosity state, then performing curing treatment to obtain the uniform PEDOT/PSS film with the thickness of 50-2000nm, wherein the film thickness is preferably 100-2000nm, and patterning the PEDOT/PSS film to form a transparent electrode. The spraying mode of the ethylene glycol may also include other conventional modes, which are not described herein. Wherein the PEDOT/PSS film treated by the ethylene glycol is converted into a low-resistance state equivalent to that of a PEDOT/PSS material which is not treated by the invention, and the structural formula of the PEDOT/PSS material treated by the ethylene glycol is listed as follows:
the PEDOT PSS material processed by the embodiment is used as a transparent electrode, has high transmittance and low resistance, has good stability in air, and is suitable for being applied to large-size substrates.
The second embodiment of the present invention further provides a method for manufacturing a color film substrate, as shown in fig. 3, the method includes the following steps:
step S11, providing a substrate, preparing a color film color resistance layer on the substrate, and treating the substrate by adopting a glycol spraying or UV irradiation mode to ensure that the surface of the substrate has a large amount of hydroxyl ions (-OH);
step S22, coating a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material with high resistance and low viscosity on the color film color resistance layer to form a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate film with low resistance;
and step S33, curing, namely imaging the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate film to form the transparent electrode.
Specifically, the preparation method of the PEDOT/PSS material with high resistance and low viscosity is the same as that of the first embodiment, and is not described herein; processing the substrate with the color film color resistance layer by means of ethylene glycol spraying or UV irradiation to enable the surface of the substrate to have a large amount of-OH, and then coating the PEDOT (PSS) material on the substrate in the same manner as in the first embodiment, which is not described herein again; and a large amount of-OH and the coated PEDOT/PSS material are subjected to chemical reaction to generate two or more polar groups, so that the PEDOT/PSS material is converted into a low-resistance material, and the conductivity of the PEDOT/PSS material is enhanced. And then curing the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate film, and forming a transparent electrode after patterning.
The invention also provides a color film substrate manufactured by the manufacturing method, and the color film substrate comprises: a substrate; the color film color resistance layer is prepared on the substrate; the transparent electrode is prepared on the color film color resistance layer; the transparent electrode is made of PEDOT PSS materials and the method. Assembling the capacitive touch screen by adopting the color film substrate; and assembling the color film substrate and the array substrate, and performing module processing and the like to obtain the LCD panel. In addition, the transparent electrode is not limited to the pixel electrode, but also comprises a public electrode, and the transparent electrode prepared by the method has wide application prospect in the fields of flexible display and wearable equipment.
Compared with the color film substrate in the prior art, the color film substrate and the preparation method thereof utilize the conformational isomerism principle of PEDOT: PSS (poly 3, 4-ethylenedioxythiophene: sodium polystyrene sulfonate), firstly, isopropanol is used for treating the PEDOT: PSS to reduce the viscosity of the PEDOT: PSS, so that the viscosity of the PEDOT: PSS can be well matched with equipment, the uniformity of large-area film formation is ensured, a solution with low viscosity after treatment is coated on the color film substrate or the glass substrate which is not subjected to the ITO process through an Ink Jet Printer (IJP) or quantitative spin coating equipment (Slit Coater), and then, the surface treatment is carried out through ethylene glycol, so that the PEDOT coated on the glass: PSS is converted into a structure with high viscosity and low resistance so as to meet the use requirement of the low-resistance transparent conductive film. Therefore, the difficult problem that large-area (2200 x 2500mm can be increased) film formation of PEDOT and PSS is difficult is solved, the air stability of the PEDOT and PSS is good, the requirements of the existing flexible transparent electrode can be completely met, the material cost is greatly saved, and the processing equipment and the flow are simplified.
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 (8)
1. A preparation method of a color film substrate is characterized by comprising the following steps:
step S1, providing a substrate, preparing a color film color resistance layer on the substrate, adding sodium polystyrene sulfonate, 3, 4-ethylenedioxythiophene, alcohol compounds and deionized water into a reaction bottle, and stirring until the sodium polystyrene sulfonate, the 3, 4-ethylenedioxythiophene, the alcohol compounds and the deionized water are completely dissolved;
adding an oxidant, a catalyst and glycerol to react to form an aqueous dispersion containing 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate;
filtering and purifying the aqueous dispersion, finally diluting the precipitate with deionized water, and performing ultrasonic dispersion to obtain a dark blue aqueous dispersion containing 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate;
filtering the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate aqueous dispersion, adding an organic auxiliary agent at least containing isopropanol, and stirring until the organic auxiliary agent is dissolved to obtain a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material with a high resistance and a low viscosity structure;
coating the poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate material on a color film color resistance layer to form a poly 3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate film;
step S2, spraying glycol on the surface of the substrate coated with the poly-3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate materials for surface treatment, so that the membrane surface structure of the poly-3, 4-ethylenedioxythiophene and sodium polystyrene sulfonate membrane is converted into a low-resistance and high-viscosity state, and curing treatment is carried out;
and step S3, patterning the poly 3, 4-ethylenedioxythiophene-sodium polystyrene sulfonate film to form a transparent electrode.
2. The method according to claim 1, wherein the stirring temperature in step S1 is 20-60 ℃.
3. The preparation method according to claim 1, wherein the reaction time of adding the oxidant, the catalyst and the glycerol for the reaction is 8-24 hours.
4. The method according to claim 1, wherein the filtration and purification process is performed using anion and cation exchange resin in step S1, and the aqueous dispersion is centrifuged, and the precipitate is diluted with distilled water and then redispersed and dissolved, and the process is repeated 3 to 5 times.
5. The preparation method according to claim 1, wherein the isopropanol is added in an amount of 3-60% by volume of the solution of poly (3, 4-ethylenedioxythiophene) and sodium polystyrene sulfonate.
6. The method as claimed in claim 1, wherein the poly 3, 4-ethylenedioxythiophene sodium polystyrene sulfonate material with high resistance and low viscosity has a viscosity of 8-30 cps.
7. The preparation method according to claim 1, wherein after the curing treatment, the thickness of the poly (3, 4-ethylenedioxythiophene) -sodium polystyrene sulfonate film is 50-2500 nm.
8. A color film substrate prepared by the preparation method according to any one of claims 1 to 7.
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