CN113504595A - Switchable color filter based on doped indium gallium zinc oxide and preparation method thereof - Google Patents
Switchable color filter based on doped indium gallium zinc oxide and preparation method thereof Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/12—Optical coatings produced by application to, or surface treatment of, optical elements by surface treatment, e.g. by irradiation
Abstract
The invention discloses a switchable color filter based on doped indium gallium zinc oxide, and relates to the technical field of color filters. The color-switchable filter is characterized in that a PMMA layer, a first Ag thin film layer, an IGZO layer and a second Ag thin film layer are sequentially connected from top to bottom, the IGZO layer with the thickness of 115-220 nm is obtained by combining a magnetron sputtering method with an annealing process, the first Ag thin film layer and the second Ag thin film layer with the thicknesses of 20nm are formed by electron beam evaporation deposition, the first Ag thin film layer is coated on the upper side of the IGZO layer, the second Ag thin film layer is coated on the lower side of the IGZO layer, the PMMA layer with the thickness of 84nm is coated on the first Ag thin film layer in a spinning mode, the filter is obtained, and hydrogen plasma enhanced chemical vapor deposition is carried out on the filter, so that the color-switchable filter is obtained. The switchable color filter of the invention enhances chemical vapor deposition through hydrogen plasma, realizes adjustable color output, and has the characteristics of high efficiency, high spatial resolution and high stability.
Description
Technical Field
The invention relates to the technical field of color filters, in particular to a switchable color filter based on doped indium gallium zinc oxide and a preparation method thereof.
Background
The structural color is widely applied, is ubiquitous in nature, such as rainbow and butterfly wings, has the advantages of high resolution, wide color gamut, stable chemical performance and the like, and is widely applied to the fields of display, imaging, color printing and the like. However, the structural colors based on interference, diffraction and plasmon effects all belong to static structural colors, the structural colors obtained after the structural parameters such as thickness, size and period are determined are fixed and unchanged, and the structural parameters are not changed any more after the structure is prepared, so that the practical application is limited. And the performance of conventional dye and pigment filters is susceptible to high intensity, long lasting light illumination and numerous chemical processes.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a switchable color filter based on doped indium gallium zinc oxide and a preparation method thereof, which realize adjustable color output by enhancing chemical vapor deposition through hydrogen plasma and have the characteristics of high efficiency, high spatial resolution and high stability.
In order to achieve the purpose, the invention adopts the following technical scheme: the switchable color filter is characterized in that a PMMA layer, a first Ag thin film layer, an IGZO layer and a second Ag thin film layer are sequentially connected from top to bottom, the IGZO layer with the thickness of 115-220 nm is obtained by combining a magnetron sputtering method and an annealing process, the first Ag thin film layer and the second Ag thin film with the thickness of 20nm are deposited by electron beam evaporation, the first Ag thin film layer is coated on the upper side of the IGZO layer, the second Ag thin film layer is coated on the lower side of the IGZO layer, the PMMA layer with the thickness of 84nm is coated on the first Ag thin film layer in a spinning mode and used for compensating color saturation, a filter is obtained, and hydrogen plasma enhanced chemical vapor deposition is carried out on the filter, so that the switchable color filter is obtained.
Further, the preparation process of the IGZO layer specifically comprises: an IGZO target is adopted, and the vacuum of the sputtering background is 3.8 multiplied by 10-3Pa, sputtering power of 60-100W, introducing mixed gas of argon and oxygen during sputtering, wherein the molar ratio of argon to oxygen is 80:20, sputtering pressure is 0.55-0.75 Pa, and sputtering time is 8-30 min to obtain an IGZO thin film which is sputtered completely, and placing the IGZO thin film on O2Annealing at 300 deg.c for 2 hr to form IGZO layer.
Further, the IGZO target is composed of In, Ga and Zn In a molar ratio of 1:1: 1.
Further, the first Ag thin film layer and the second Ag thin film layer are prepared by the following method: adjusting the current of 2mA, determining the beam spot of the electron beam in the silver crucible, adjusting the controller of the silver crucible to make the beam spot in the center of the crucible and make the area of the beam spot equal to the upper caliber of the crucible, maintaining the shape and size of the beam spot unchanged during evaporation, increasing the current slowly, and setting the vacuum degree to be 1.5 multiplied by 10 when the evaporation rate reaches 0.2 nm/s-3Pa, using electron beams of 2.5kV for evaporation, reducing the current to 0 when the film thickness is 20nm, turning off the electron beams, and obtaining the Ag film after 15 minutes.
Further, the PMMA layer is obtained by the following method: adding anisole into PMMA powder to prepare PMMA solution with the mass concentration of 8%, uniformly stirring, dripping the PMMA solution onto a first Ag film layer on a rotating table, firstly controlling the rotating speed of a spin coater to be 1000 rpm/min, and spin-coating for 10 s; and controlling the rotating speed of the spin coater to be 5000rpm/min, spin-coating for 50s, and drying the first Ag film layer at 80 ℃ to obtain the PMMA film.
Further, the method for hydrogen plasma enhanced chemical vapor deposition specifically comprises the following steps: putting the filter into a hydrogen plasma enhanced chemical vapor deposition chamber, and introducing H with the flow rate of 10 sccm2Controlling the pressure in the plasma enhanced chemical vapor deposition chamber to be 3.2 PaPerforming H at 120 ℃ with RF power of 200W2Plasma treatment was carried out for 5 minutes to obtain a switchable color filter.
Compared with the prior art, the invention has the following beneficial effects: the thickness of the filter prepared by the method is 115-220 nm, RGB three primary colors with high transmission and high purity can be obtained, and the thickness of the filter is set in the range, so that the color of the filter can be switched to any color in a visible light range; the IGZO layer is provided with the PMMA layer, so that the color saturation of the IGZO layer is improved; the filter provided by the invention adjusts the carrier concentration in the IGZO layer through hydrogen plasma enhanced chemical vapor deposition, so that the conductivity in the IGZO layer is changed, the dynamic adjustment of the structural color is realized, and the color switching can be realized under the condition that the structural parameters of the filter are not changed any more. The switchable color filter can be widely applied to thin film transistors, thin film circuits, sensors and the like of flat panel displays.
Drawings
FIG. 1 is a schematic diagram of a switchable color filter based on doped InGaZn oxide according to the present invention;
FIG. 2 is a graph of the transmission spectra of the IGZO layer in the switchable color filter of the present invention at 180nm, 220nm and 115nm thicknesses, respectively;
fig. 3 is a transmission spectrum corresponding to the adjustment of the thicknesses of the first Ag thin film layer and the second Ag thin film layer when the IGZO layer in the filter of the present invention has thicknesses of 180nm, 220nm, and 115nm, respectively: fig. 3 (a) shows transmission spectra corresponding to the adjustment of the thicknesses of the first Ag thin film layer and the second Ag thin film layer when the IGZO layer thickness is 180nm, fig. 3 (b) shows transmission spectra corresponding to the adjustment of the thicknesses of the first Ag thin film layer and the second Ag thin film layer when the IGZO layer thickness is 220nm, and fig. 3 (c) shows transmission spectra corresponding to the adjustment of the thicknesses of the first Ag thin film layer and the second Ag thin film layer when the IGZO layer thickness is 115 nm;
FIG. 4 is a transmission spectrum corresponding to the adjustment of the incident light angle when the thicknesses of the IGZO layers of the filter of the present invention are 180nm, 220nm and 115nm, respectively: fig. 4 (a) is a transmission spectrum corresponding to an angle of incident light adjusted when the IGZO layer has a thickness of 180nm, fig. 4 (b) is a transmission spectrum corresponding to an angle of incident light adjusted when the IGZO layer has a thickness of 220nm, and fig. 4 (c) is a transmission spectrum corresponding to an angle of incident light adjusted when the IGZO layer has a thickness of 115 nm;
fig. 5 is a transmission spectrum of the filter of the present invention before and after hydrogen plasma treatment: fig. 5 (a) shows a transmission spectrum before the hydrogen plasma treatment, and fig. 5 (b) shows a transmission spectrum after the hydrogen plasma treatment.
Detailed Description
The technical solution of the present invention is further explained with reference to the drawings and the embodiments.
Fig. 1 is a schematic structural diagram of a switchable color filter based on indium gallium zinc oxide doped, according to the invention, a PMMA layer, a first Ag thin film layer, an IGZO layer, and a second Ag thin film layer are sequentially connected from top to bottom, the IGZO layer with a thickness of 115-220 nm is obtained by a magnetron sputtering method in combination with an annealing process, the thickness of the IGZO layer is set within the range, and the filter can realize resonance of visible light with any wavelength, so as to obtain a structural color with high transmission and high purity. Depositing a first Ag thin film layer and a second Ag thin film, both of which have a thickness of 20nm, by electron beam evaporation, coating the first Ag thin film layer on the upper side of the IGZO layer, and coating the second Ag thin film layer on the lower side of the IGZO layer, as a metal mirror, since Ag has the highest reflectance and the lowest absorptance in the visible light region; and a PMMA layer with the thickness of 84nm is spin-coated on the first Ag film layer, wherein PMMA is organic glass, has the advantages of better transparency, chemical stability, higher light transmittance and the like, can be used for improving the transmission efficiency of the filter to obtain the filter, and is subjected to hydrogen plasma enhanced chemical vapor deposition to obtain the color-switchable filter.
The preparation process of the IGZO layer in the invention specifically comprises the following steps: an IGZO target is adopted, the IGZO target consists of In, Ga and Zn with the molar ratio of 1:1:1, and the vacuum of the sputtering background is 3.8 multiplied by 10-3Pa, sputtering power of 60-100W, introducing mixed gas of argon and oxygen during sputtering, wherein the molar ratio of argon to oxygen is 80:20, sputtering pressure is 0.55-0.75 Pa, and sputtering time is 8-30 min to obtain an IGZO thin film which is sputtered completely, and placing the IGZO thin film on O2Annealing at 300 deg.c for 2 hr to form IGZO layer. The preparation method of the IGZO film by the magnetron sputtering method has the characteristics of simple process, high sputtering rate, low film forming temperature, uniform film and stable device performance, and is suitable for large-area batch production. In addition, the magnetron sputtering method of the present invention can easily control the thickness and properties of the IGZO layer by adjusting sputtering power, substrate temperature, gas pressure, and the like.
The first Ag film layer and the second Ag film layer are prepared by the following method: adjusting the current of 2mA, determining the beam spot of the electron beam in the silver crucible, adjusting the controller of the silver crucible to make the beam spot in the center of the crucible and make the area of the beam spot equal to the upper caliber of the crucible, maintaining the shape and size of the beam spot unchanged during evaporation, increasing the current slowly, and setting the vacuum degree to be 1.5 multiplied by 10 when the evaporation rate reaches 0.2 nm/s-3Pa, using electron beams of 2.5kV for evaporation, reducing the current to 0 when the film thickness is 20nm, turning off the electron beams, and obtaining the Ag film after 15 minutes. The first Ag film and the second Ag film are both obtained by an electron beam evaporation method, have the characteristics of economy, environmental protection, simple method and realization of large-scale production, and are widely applied to the preparation of various film materials in industry.
The PMMA layer in the present invention is obtained by the following method: adding anisole into PMMA powder to prepare PMMA solution with the mass concentration of 8%, uniformly stirring, dripping the PMMA solution onto a first Ag film layer on a rotating table, firstly controlling the rotating speed of a spin coater to be 1000 rpm/min, and spin-coating for 10 s; and controlling the rotating speed of the spin coater to be 5000rpm/min, spin-coating for 50s, and drying the first Ag film layer at 80 ℃ to obtain the PMMA film. The spin coating method adopts low-rotation-speed spin coating, so that the spin-coated film is more uniform.
The method for the hydrogen plasma enhanced chemical vapor deposition comprises the following steps: putting the filter into a hydrogen plasma enhanced chemical vapor deposition chamber, and introducing H with the flow rate of 10 sccm2Controlling the pressure in the plasma enhanced chemical vapor deposition chamber to be 3.2 Pa, and performing H at 120 ℃ and 200W of radio frequency power2Plasma treatment for 5 minutesA switchable color filter is obtained. The filter provided by the invention can be used for enhancing chemical vapor deposition through hydrogen plasma and adjusting the carrier concentration in the IGZO layer, so that the conductivity in the IGZO layer is changed, and the dynamic adjustment of the structural color is realized.
Examples
The invention provides a switchable color filter based on doped indium gallium zinc oxide, which is prepared by the following steps:
(1) an IGZO target is adopted, the IGZO target consists of In, Ga and Zn with the molar ratio of 1:1:1, and the vacuum of the sputtering background is 3.8 multiplied by 10-3Pa, setting the sputtering power to be 60-100W, introducing a mixed gas of argon and oxygen during sputtering, setting the molar ratio of argon to oxygen to be 80:20, sputtering the gas pressure to be 0.55-0.75 Pa, respectively sputtering for 8min, 18min and 30 min to obtain an IGZO film to be sputtered, and placing the IGZO film to O2Carrying out annealing treatment at the annealing temperature of 300 ℃ for 2h to form an IGZO layer; the thickness of the IGZO layer is 115nm, 180nm and 220nm respectively.
(2) Adjusting the current of 2mA, determining the beam spot of the electron beam in the silver crucible, adjusting the controller of the silver crucible to make the beam spot in the center of the crucible and make the area of the beam spot equal to the upper caliber of the crucible, maintaining the shape and size of the beam spot unchanged during evaporation, increasing the current slowly, and setting the vacuum degree to be 1.5 multiplied by 10 when the evaporation rate reaches 0.2 nm/s-3Pa, performing evaporation by using an electron beam of 2.5kV, reducing the current to 0 when the thickness of the film is 20nm, closing the electron beam, and obtaining a first Ag film after 15 minutes, wherein a second Ag film is also prepared by the method; the first Ag thin film is provided on the upper side of the IGZO layer, and the second Ag thin film is provided on the lower side of the IGZO layer. In the invention, the influence of the thicknesses of the first Ag film and the second Ag film on the light transmittance of the filter is also detected, as shown in (a) - (c) in FIG. 3, the transmission spectra are respectively under blue, green and red, and the light intensity entering the IGZO layer is reduced along with the increase of the thickness of the Ag film, so that the transmittance is very low; when the thickness of the Ag film is too thin, the transmission wavelength is obviously red-shifted, the full width at half maximum is increased, and the color is deviated from the original color, so that the Ag filmThe thickness was set at 20 nm.
(3) Adding anisole into PMMA powder to prepare PMMA solution with the mass concentration of 8%, uniformly stirring, dripping the PMMA solution onto a first Ag film layer on a rotating table, firstly controlling the rotating speed of a spin coater to be 1000 rpm/min, and spin-coating for 10 s; and controlling the rotating speed of the spin coater to be 5000rpm/min, spin-coating for 50s, and drying the first Ag thin film layer at 80 ℃ to obtain the filter.
As shown in fig. 2, when the thickness of the IGZO layer in the filter is 115nm, the resonance wavelength is 671nm with a transmittance of 63.6% using vertical light incidence, corresponding to RGB being red; when the thickness of the IGZO layer in the filter is 180nm, vertical light incidence is used, the resonance wavelength is 462nm, the transmittance is 73.9%, and blue is corresponding to RGB; when the thickness of the IGZO layer in the filter is 220nm, vertical light incidence is used, the resonance wavelength is 535nm, the transmittance is 71.4%, and green is corresponding to RGB; the color change of the filter can be achieved by varying the thickness of the IGZO layer. As shown in fig. 4, when the incident light angles are adjusted to be 0 °, 20 °, 40 ° and 60 °, the transmission spectrograms of IGZO layers in the filter at thicknesses of 115nm, 180nm and 220nm are (a) - (c) in fig. 4, and when the incident light angles are changed from 0 ° to 60 °, the formants of each filter are only slightly blue-shifted, and the color change of the filter is not large, that is, the incident light angles have no influence on the color change of the filter.
(4) Putting the filter into a hydrogen plasma enhanced chemical vapor deposition chamber, and introducing H with the flow rate of 10 sccm2Controlling the pressure in the plasma enhanced chemical vapor deposition chamber to be 3.2 Pa, and performing H at 120 ℃ and 200W of radio frequency power2Performing plasma treatment for 5 minutes to obtain a switchable color filter, wherein specifically, when the thickness of an IGZO layer in the filter is 115nm, the color of the filter is changed from red to green; when the thickness of the IGZO layer in the filter is 180nm, the color of the filter is changed from blue to magenta; when the thickness of the IGZO layer in the filter was 220nm, the color of the filter changed from green to violet.
As shown in fig. 5, which is a transmission spectrum of the filter before and after the hydrogen plasma treatment, as can be seen from (a) of fig. 5, as the thickness of the IGZO layer varies before the hydrogen plasma treatment, when the thickness of IGZO is increased from 115nm to 220nm in 15nm steps, the resonance wavelengths are shifted to 670nm, 731nm, 791nm, 427nm, 453nm, 479nm, 508nm and 535nm, respectively, as can be seen from (b) of FIG. 5, after the filter is processed by the hydrogen plasma, the carrier concentration in the IGZO layer is changed, thereby changing the electrical conductivity in the IGZO layer, the resonance wavelengths are 539nm, 584nm, 630nm, 677nm, 725nm, 404nm, 423nm and 442nm respectively, when the thickness of the IGZO is determined, after passing through the hydrogen plasma processing filter, for IGZO layers with the same thickness, the resonance wavelength is obviously shifted, so that the dynamic adjustment of structural color is realized; by the method, the dynamic switching of the structural color of the filter is realized on the basis of not changing the structure of the conventional filter.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (6)
1. The switchable color filter based on the doped indium gallium zinc oxide is characterized in that a PMMA layer, a first Ag thin film layer, an IGZO layer and a second Ag thin film layer are sequentially connected from top to bottom, the IGZO layer with the thickness of 115-220 nm is obtained through a magnetron sputtering method and an annealing process, the first Ag thin film layer and the second Ag thin film with the thicknesses of 20nm are deposited through electron beam evaporation, the first Ag thin film layer is coated on the upper side of the IGZO layer, the second Ag thin film layer is coated on the lower side of the IGZO layer, the PMMA layer with the thickness of 84nm is coated on the first Ag thin film layer in a spinning mode to obtain the filter, and hydrogen plasma enhanced chemical vapor deposition is carried out on the filter to obtain the switchable color filter.
2. The indium gallium zinc oxide doped based switchable color filter of claim 1, which isIs characterized in that the preparation process of the IGZO layer specifically comprises the following steps: an IGZO target is adopted, and the vacuum of the sputtering background is 3.8 multiplied by 10-3Pa, sputtering power of 60-100W, introducing mixed gas of argon and oxygen during sputtering, wherein the molar ratio of argon to oxygen is 80:20, sputtering pressure is 0.55-0.75 Pa, and sputtering time is 8-30 min to obtain an IGZO thin film which is sputtered completely, and placing the IGZO thin film on O2Annealing at 300 deg.c for 2 hr to form IGZO layer.
3. The indium gallium zinc oxide doped switchable color filter according to claim 2, wherein the IGZO target consists of In, Ga, Zn In a molar ratio of 1:1: 1.
4. The switchable color filter based on indium gallium zinc oxide doped according to claim 1, wherein the first Ag thin film layer and the second Ag thin film layer are prepared by the following method: adjusting the current of 2mA, determining the beam spot of the electron beam in the silver crucible, adjusting the controller of the silver crucible to make the beam spot in the center of the crucible and make the area of the beam spot equal to the upper caliber of the crucible, maintaining the shape and size of the beam spot unchanged during evaporation, increasing the current slowly, and setting the vacuum degree to be 1.5 multiplied by 10 when the evaporation rate reaches 0.2 nm/s-3Pa, using electron beams of 2.5kV for evaporation, reducing the current to 0 when the film thickness is 20nm, turning off the electron beams, and obtaining the Ag film after 15 minutes.
5. Switchable colour filter based on doped indium gallium zinc oxide according to claim 1, characterized in that the PMMA layer is obtained by: adding anisole into PMMA powder to prepare PMMA solution with the mass concentration of 8%, uniformly stirring, dripping the PMMA solution onto a first Ag film layer on a rotating table, firstly controlling the rotating speed of a spin coater to be 1000 rpm/min, and spin-coating for 10 s; and controlling the rotating speed of the spin coater to be 5000rpm/min, spin-coating for 50s, and drying the first Ag film layer at 80 ℃ to obtain the PMMA film.
6. The switchable color filter based on doped indium gallium zinc oxide of claim 1, wherein the method of hydrogen plasma enhanced chemical vapor deposition specifically comprises: putting the filter into a hydrogen plasma enhanced chemical vapor deposition chamber, and introducing H with the flow rate of 10 sccm2Controlling the pressure in the plasma enhanced chemical vapor deposition chamber to be 3.2 Pa, and performing H at 120 ℃ and 200W of radio frequency power2Plasma treatment was carried out for 5 minutes to obtain a switchable color filter.
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KR102130320B1 (en) * | 2019-01-03 | 2020-07-08 | 청주대학교 산학협력단 | Multilayered color filter having an amorphous oxide layer |
CN112509974A (en) * | 2020-12-01 | 2021-03-16 | 绵阳惠科光电科技有限公司 | Preparation method of IGZO array substrate |
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