WO2022107939A1 - 내구성이 강화된 투명필름 - Google Patents
내구성이 강화된 투명필름 Download PDFInfo
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- WO2022107939A1 WO2022107939A1 PCT/KR2020/016536 KR2020016536W WO2022107939A1 WO 2022107939 A1 WO2022107939 A1 WO 2022107939A1 KR 2020016536 W KR2020016536 W KR 2020016536W WO 2022107939 A1 WO2022107939 A1 WO 2022107939A1
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- Prior art keywords
- layer
- inorganic material
- transparent film
- refractive index
- passivation layer
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Images
Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2400/24—Thermosetting resins
Definitions
- the present invention relates to a transparent film with enhanced durability.
- LED TV generates a lot of heat not only from TFT but also from the LED itself, which generates more heat and electromagnetic waves than LCD/OLED, and the need to block heat and electromagnetic waves at the same time is increasing.
- the conventional ITO electrode it is widely used as an electrode material having excellent electrical conductivity and high light transmittance.
- the thermal barrier properties and electromagnetic wave shielding performance are remarkably deteriorated to a level that cannot be used.
- silver nanowire (AgNW) has high transparency, it has a chronic problem in that it cannot overcome the problems of heat blocking ability and reliability.
- silver has superior electromagnetic and heat shielding and blocking properties than any other material, so research to secure the durability of silver is continuing.
- a plastic film used as a display substrate has inferior light transmission properties compared to a glass substrate. Therefore, it is not an easy task to improve optical properties with a plastic substrate, and it is important to increase the transmittance even as fine as possible.
- the anti-reflection effect must be applied to the film and the gas permeation barrier effect must be realized at the same time.
- the permeability to oxygen or moisture is sometimes explained by the pinhole model. For this reason, the multi-layer structure has a remarkable effect in preventing the penetration of oxygen, moisture, etc. due to separation in terms of the distance of the pinholes between layers.
- the technical problem to be solved by the present invention is to prevent oxidation of the silver thin film layer to secure durability, and to provide a transparent film with enhanced durability that can simultaneously implement heat blocking and electromagnetic blocking.
- a transparent film with enhanced durability includes a base layer; a first inorganic material layer laminated on one surface of the base layer; a metal layer laminated on one surface of the first inorganic material layer; a second inorganic material layer laminated on one surface of the metal layer; and a plurality of organic material layers stacked on one surface of the second inorganic material layer.
- a hard coating layer disposed on both sides of the base layer, respectively; may further include.
- a refractive index matching layer that is respectively disposed between the base layer and the first inorganic material layer and between the second inorganic material layer and the passivation layer to reinforce the refractive index; may further include.
- the passivation layer a first passivation layer comprising a first organic material; a second passivation layer including a second organic material different from the first organic material; a third passivation layer including a third organic material different from the first and second organic materials; and a fourth passivation layer including a fourth organic material different from the first, second, and third organic materials.
- the metal layer may include silver (Ag), and the first inorganic material layer and the second inorganic material layer may include copper oxide (CuOx).
- the metal layer may include silver (Ag), and the first inorganic material layer and the second inorganic material layer may include copper nitride (CuNx).
- the present invention has an effect of preventing oxidation of the silver thin film layer by compounding the organic and inorganic layers into multiple layers.
- the present invention has the effect of being able to provide a durable transparent film in which the durability of the silver thin film layer is strengthened and thus high heat blocking and electromagnetic blocking performance are realized.
- FIG. 1 shows a transparent film with enhanced durability according to an embodiment of the present invention.
- FIG. 5 is a photograph comparing before and after a reliability test of an embodiment of the present invention.
- FIG. 6 shows the measurement results of moisture permeability over time of the durable transparent film according to an embodiment of the present invention.
- FIG 7 shows the level of radio interference noise according to the frequency of the durable transparent film according to an embodiment of the present invention.
- FIG. 1 shows a transparent film 100 with enhanced durability according to an embodiment of the present invention.
- the transparent film 100 with enhanced durability has a first hard coating layer 110 , a base layer 120 , a second hard coating layer 130 , and a first refractive index matching.
- the first hard coating layer 110 and the second hard coating layer 130 are transparent films of high hardness and may be provided to secure transmittance and strength.
- the first hard coating layer 110 and the second hard coating layer 130 may be used for refractive index matching with other substrates while ensuring high hardness and wear resistance characteristics.
- the second hard coating layer 130 also improves interlayer adhesion when the inorganic layer is deposited thereon.
- the refractive index of the first hard coating layer 110 and the second hard coating layer 130 is preferably selected to be relatively low.
- the first hard coating layer 110 and the second hard coating layer 130 are a bar coating method, a knife coating method, a roll coating method, a blade coating method, a die coating method, a micro gravure coating method, a comma coating method, a slot die coating method, It may be manufactured by a lip coating method or a method for manufacturing a hard coating film performed by a solution casting method.
- a base layer 120 may be stacked on the first hard coating layer 110 , and a second hard coating layer 130 may be stacked on the base layer 120 again.
- the substrate layer 120 may include an inorganic material or an organic material.
- the inorganic material may be any one or a combination of glass, quartz, Al2O3, SiC, Si, GaAs, and InP, but is not limited thereto.
- Organic material is Kepton foil, polyimide (PI), polyethersulfone (PES), polyacrylate (PAR), polyetherimide (PEI), polyethylene naphthalate (PEN) , polyethyleneterephthalate (PET), polyphenylene sulfide (PPS), polyarylate (polyarylate), polycarbonate (PC), cellulose triacetate (CTA), cellulose acetate propio It may be selected from nate (cellulose acetate propionate, CAP), but is not limited thereto.
- the base layer 120 may be made of polyethylene terephthalate (PET) used for optics.
- PET polyethylene terephthalate
- the base layer 120 is prone to curvature due to the thickness of the passivation layers 192, 194, 196, and 198 to be composed of an organic material, it may be preferable to form a thickness of at least 100 ⁇ m.
- the second hard coating layer 130 may be laminated on the base layer 120 .
- the first refractive index matching layer 140 may be laminated on the second hard coating layer 130 .
- the first refractive index matching layer 140 may include an insulating material that is different from the refractive index of the layers stacked thereon.
- the first refractive index matching layer 140 it is preferable to use a material having a large refractive index of 2.0 or more.
- a ceramic material used for refractive index matching TiOx, Nb2Ox, or the like is used.
- the first refractive index matching layer 140 may include a metal oxide, and the metal oxide may include any type of metal oxide having an amphiphilic property.
- titanium sub-oxide TiOx and Titanium oxide, TiO2
- zinc oxide Zinc oxide, ZnO
- tungsten oxide Tungsten oxide, W2O3, WO2, WO3
- molybdenum oxide MoO2, MoO2
- MoOX Molybdenum sub-oxide
- the first refractive index matching layer 140 is preferably zinc oxide (Zinc oxide, ZnO) may be included.
- the first inorganic material layer 150 may be stacked on the first refractive index matching layer 140 .
- a metal layer 160 may be stacked on the first inorganic material layer 150
- the second inorganic material layer 170 may be stacked on the other surface of the metal layer 160 .
- the metal layer 160 may be surrounded by two inorganic material layers.
- the silver (Ag) element diffuses to the interface to self-generate a new diffusion barrier, or the specific resistance due to the remaining alloying elements in the silver (Ag) thin film increases. Measures were needed to prevent this.
- the first inorganic material layer 150 and the second inorganic material layer 170 are configured to function as a thermally or chemically stable diffusion barrier layer.
- the first inorganic material layer 150 and the second inorganic material layer 170 include transition metals such as Cu and Ti having low mutual solubility with silver (Ag). may be desirable.
- the first inorganic material layer 150 and the second inorganic material layer 170 may be formed of a CuNx or SiNx thin film deposited using sputtering.
- x is used to mean that there is no fixed or known amount of nitrogen. This is because even if nitrogen is supplied to the metal when manufacturing the metal nitride, the exact bonding ratio cannot be known.
- the passivation characteristics of the first inorganic material layer 150 and the second inorganic material layer 170 are improved as the deposition thickness thereof increases.
- the SiNx thin film formed by the dry oxidation method exhibited about 20 times or more excellent passivation characteristics because it had a denser interfacial structure than that formed by the wet oxidation method.
- [Table 1] compares the performances according to the materials of the first inorganic material layer 150 and the second inorganic material layer 170 .
- a* and b* are coordinates defined in CIE (International Commission on Illumination) LAB color space, a* is the degree of red and green, b* is yellow and Indicates the degree of blue. Y represents luminance, L* represents brightness, and transmittance was measured at 550 nm.
- CIE International Commission on Illumination
- copper oxide and copper nitride were compared and analyzed.
- copper oxide was advantageous in terms of increase in transmittance, but it was found that nitride was excellent in passivation characteristics.
- the first inorganic material layer 150 and the second inorganic material layer 170 may be formed in a range of 5 nm to 10 nm in consideration of transmittance.
- the metal layer 160 may include a conductive material such as APC, Cu, Cu alloy, Ag, Ag alloy, Mo/Ag, or Mo/APC.
- the metal layer 160 may include silver (Ag).
- the transmittance of the metal layer 160 decreases due to absorption or scattering when the multilayer thin film is formed.
- the second refractive index matching layer 180 may be stacked on the second inorganic material layer 170 .
- the material for the second refractive index matching layer 180 may be a material having a refractive index different from that of the first refractive index matching layer 140 .
- the second refractive index matching layer 180 is preferably made of a material having a large refractive index of 2.0 or more.
- a ceramic material used for the second refractive index matching layer 180 TiOx, Nb2Ox, or the like is used.
- the second refractive index matching layer 180 may include a metal oxide, and the metal oxide may include any type of metal oxide having an amphiphilic property.
- titanium sub-oxide TiOx and Titanium oxide, TiO2
- zinc oxide Zinc oxide, ZnO
- tungsten oxide Tungsten oxide, W2O3, WO2, WO3
- molybdenum oxide MoO2, MoO2
- MoOX Molybdenum sub-oxide
- the second refractive index matching layer 180 is zinc oxide (Zinc oxide, ZnO) may be included.
- the first passivation layer 192 may be stacked on the second refractive index matching layer 180 .
- the first passivation layer 192 may include a first organic material.
- the first passivation layer 192 may complement the other laminated thin films to prevent oxidation of the metal layer 160 , that is, the silver thin film, thereby strengthening the durability of the transparent heat shielding film.
- the first passivation layer 192 may be formed of a material having an adhesive force with the second refractive index matching layer 180 and having a different refractive index.
- the first passivation layer 192 may be formed of a polymer having a lower refractive index than that of the second refractive index matching layer 180 , and may be formed of a material having a refractive index of 1.5.
- the first passivation layer 192 is, polyvinylpyrrolidone (Polyvinylpyrrolidone, PVP), polycarbonate (Polycarbonate, PC), polymethyl methacrylate (Poly (methyl methacrylate), PMMA), polystyrene (Polystyrene, PS), poly It may be formed of any one selected from among vinyl alcohol (Polyvinyl alcohol, PVA) and cellulose (Cellulose).
- the first passivation layer 192 may be formed to a thickness of 30 nm to 300 nm using a solution process. If the first passivation layer 192 is formed to be less than 30 nm, there may be difficulties during solution coating, and if it is formed to be more than 300 nm, it may be difficult to attach to the refractive index matching layer. In addition, when it is out of the corresponding range, the transmittance may be lowered.
- the second passivation layer 194 may be stacked on the first passivation layer 192 .
- the second passivation layer 194 may include a second organic material.
- the second passivation layer 194 may complement the other laminated thin films to prevent oxidation of the metal layer 160 , that is, the silver thin film, thereby enhancing the durability of the transparent heat shielding film.
- the second passivation layer 194 may be formed of a material having an adhesive force and a refractive index different from that of the first passivation layer 192 .
- the second passivation layer 194 may be formed of a material having a refractive index of 1.55.
- the second passivation layer 194 may be formed by including a polymer selected from any one group of urethane acrylate-based, silicone acrylate-based, and epoxy acrylate-based polymers.
- the second passivation layer 194 is preferably a polymer that can be cured.
- the second passivation layer 194 may also be formed by applying an additive such as a resin additive or an inorganic filler to improve performance. These additives may serve to increase the spreadability or to adjust the refractive index to a desired degree.
- the second passivation layer 194 may be formed to a thickness of 50 nm to 300 nm using a solution process. In addition, when it is out of the corresponding range, the transmittance may be lowered.
- the third passivation layer 196 may be stacked on the second passivation layer 194 .
- the third passivation layer 196 may include a third organic material.
- the third passivation layer 196 may complement the other laminated thin films to prevent oxidation of the metal layer 160 , that is, the silver thin film, thereby strengthening the durability of the transparent heat shielding film.
- the third passivation layer 196 may be formed of a material having an adhesive force and a refractive index different from that of the second passivation layer 194 .
- the third passivation layer 196 may be formed of a polymer having a lower refractive index than that of the second passivation layer 194 , and may be formed of a material having a refractive index of 1.5.
- the third passivation layer 196 is, polyvinylpyrrolidone (Polyvinylpyrrolidone, PVP), polycarbonate (Polycarbonate, PC), polymethyl methacrylate (Poly (methyl methacrylate), PMMA), polystyrene (Polystyrene, PS), poly It may be formed of any one selected from among vinyl alcohol (Polyvinyl alcohol, PVA) and cellulose (Cellulose).
- the third passivation layer 196 may be formed to a thickness of 30 nm to 300 nm using a solution process.
- the fourth passivation layer 198 may be stacked on the third passivation layer 196 .
- the fourth passivation layer 198 may include a fourth organic material.
- the fourth passivation layer 198 may complement the other laminated thin films to prevent oxidation of the metal layer 160 , that is, the silver thin film, thereby strengthening the durability of the transparent heat shielding film.
- the fourth passivation layer 198 may be formed of a material having an adhesive force and a refractive index different from that of the third passivation layer 196 .
- the fourth passivation layer 198 may be formed of a material having a refractive index of 1.55.
- the fourth passivation layer 198 may be formed by including a polymer selected from any one group of urethane acrylate-based, silicone acrylate-based, and epoxy acrylate-based polymers.
- the fourth passivation layer 198 is preferably a polymer that can be cured.
- the fourth passivation layer 198 may also be formed by applying an additive such as a resin additive or an inorganic filler to improve performance.
- the fourth passivation layer 198 may be formed to a thickness of 500 nm to 4 ⁇ m using a solution process.
- the transparent film includes a first hard coating layer 110 , a base layer 120 , a second hard coating layer 130 , a first refractive index matching layer 140 , a first inorganic material layer 150 , and a metal layer. (160), the second inorganic material layer 170, the second refractive index matching layer 180, the first passivation layer 192, the second passivation layer 194, the third passivation layer 196 and the fourth passivation layer ( 198) is composed.
- the first hard coating layer 110 and the second hard coating layer 130 were formed to a thickness of 3 ⁇ m, and the base layer 120 was formed to a thickness of 100 ⁇ m using PET.
- the first refractive index matching layer 140 was formed of Nb2O5 to a thickness of 35 nm, the first inorganic material layer 150 and the second inorganic material layer 170 were formed to a thickness of 5 nm with CuNx, and the metal layer 160 was formed of silver (Ag). was formed to a thickness of 10 nm.
- the second refractive index matching layer 180 was formed of Nb2O5 to a thickness of 35 nm
- the first passivation layer 192 was formed to a thickness of 100 nm with PMMA
- the second passivation layer 194 was formed to a thickness of 180 nm with epoxy acrylate
- the third passivation layer 196 was formed of PMMA with a thickness of 80 nm
- the fourth passivation layer 198 was formed with a thickness of 1.5 ⁇ m with urethane acrylate.
- the transparent film was composed of a first hard coating layer, a base layer, a second hard coating layer, a refractive index matching layer, and a metal layer.
- the first hard coating layer and the second hard coating layer were formed to a thickness of 3 ⁇ m, and the base layer was formed to a thickness of 100 ⁇ m using PET.
- the first refractive index matching layer was formed of Nb2O5 to a thickness of 35 nm, and the metal layer was formed of silver (Ag) to a thickness of 10 nm.
- the transparent film consists of a first hard coating layer, a base layer, a second hard coating layer, a refractive index matching layer, a first inorganic material layer, a metal layer, a second inorganic material layer, and a second refractive index matching layer.
- the first hard coating layer and the second hard coating layer were formed to a thickness of 3 ⁇ m, and the base layer was formed to a thickness of 100 ⁇ m using PET.
- the first refractive index matching layer was formed of Nb2O5 to a thickness of 35 nm
- the first inorganic material layer and the second inorganic material layer were formed to a thickness of 5 nm with CuNx
- the metal layer was formed of silver (Ag) to a thickness of 10 nm
- the second refractive index matching layer Silver was formed with Nb2O5 to a thickness of 35 nm.
- Comparative Example 1 compared to the embodiment of the present invention, the condition that neither the inorganic layer nor the organic layer for protecting the metal layer exists, and the conditions (material and thickness) of other components are the same.
- Comparative Example 2 constitutes only an inorganic layer for protecting the metal layer and does not constitute an organic layer, and the conditions (material and thickness) of other components are the same as compared to an embodiment of the present invention.
- Table 2 shows the luminance Y and transmittance at a wavelength of 550 nm.
- Comparative Example 1 Comparative Example 2 embodiment of the present invention transmittance Y 65.4 77.3 88.1 @ 550 nm 76.9 77.6 88.4
- Y is the average transmittance
- @ 550 nm means transmittance at a wavelength of 550 nm.
- the transmittance according to wavelength in the visible ray region is the same as in FIG. 2 .
- the transmittance was lower as the wavelength increased, and in Comparative Example 2, the transmittance was relatively high as it approached the infrared ray.
- the Examples of the present invention showed high transmittance over the entire visible ray region, which was superior to those of Comparative Examples in terms of transmittance.
- Table 3 compares the before and after performances of Examples of the present invention and Comparative Examples 1 and 2 under high temperature and high humidity conditions, respectively.
- the experiment was conducted to measure the optical properties before and after 3,000 hours had elapsed under a temperature of 60 °C and a humidity of 90% (R.H).
- Comparative Example 1 Comparative Example 2 embodiment of the present invention I'm after I'm after I'm after transmittance Y 65.4 72.7 77.6 78.6 88.1 88.4 @ 550 nm 65.6 73.2 77.6 79.5 87.2 89.4
- FIG. 3A is a photograph before the experiment of Comparative Example 1
- FIG. 3B is a photograph after the experiment of Comparative Example 1.
- FIG. 4A is a photograph before the experiment of Comparative Example 2
- FIG. 4B is a photograph after the experiment of Comparative Example 2.
- FIG. 5A is a photograph before the experiment of the embodiment of the present invention
- FIG. 5B is a photograph after the experiment of the embodiment of the present invention.
- Figures 4b and 5b are taken after applying a blackboard to the back in order to more clearly confirm the change in appearance.
- the water vapor transmission rate of the transparent film according to the embodiment of the present invention was measured, and the water vapor transmission rate (WVTR, Water Vapor Transmission Rate) with the transparent film of Comparative Example 1 was compared. Moisture has the greatest influence on the oxidation of the metal layer. Comparing the difference in the degree of passing of water vapor can be a measure of reliability.
- the moisture permeability in Comparative Example 1 was 5200 mg/m2 ⁇ day, and the water vapor transmission rate in the Example of the present invention was measured to be 210 mg/m2 ⁇ day, so that the Example of the present invention had a higher water vapor transmission rate compared to Comparative Example 1. It was found that it was reduced to 1/25 level.
- the transparent film of the embodiment of the present invention there is an effect of lowering the moisture permeability, thereby improving the reliability under high temperature and high humidity conditions.
- the measurement result of the moisture permeability according to time is shown in FIG. 6 .
- the test measured the shielding performance in dB in the frequency range of 30 MHz - 1000 MHz.
- the electromagnetic wave was reduced by about 30 dB in the embodiment of the present invention. This is about 10dB lower than the ITO film.
- the level of jamming noise according to frequency is shown in FIG. 7 .
- the heat shielding performance of the transparent film according to the embodiment of the present invention was evaluated.
- Examples of the present invention were compared with ITO (Indium Tin Oxide) film and silver nanowire (AgNWs) film, respectively.
- the transparent film was composed of a first hard coating layer, a base layer, a second hard coating layer, a refractive index matching layer, and an ITO layer.
- the transparent film was composed of a first hard coating layer, a base layer, a second hard coating layer, a refractive index matching layer, and a silver nanowire layer.
- the heat shielding experiment was conducted in such a way that one side of the transparent film and the heat source in each example were facing each other, and infrared (IR) was placed on the other side to measure the temperature.
- IR infrared
- the transparent film of the embodiment of the present invention had a temperature of 35.4° C. on the other side, so it was found that the heat shielding performance was very excellent.
- the transparent film in Comparative Example 3 had a temperature of 69.6° C. on the other side, and the change was insignificant, and the transparent film in Comparative Example 4 had a temperature of 65.5° C. It was found to be insignificant compared to the examples of the invention.
- Figure 8a is an infrared photograph for evaluating the heat shielding performance of the transparent film of the embodiment of the present invention.
- Figure 8b is an infrared photograph for evaluating the heat shielding performance of the transparent film of Comparative Example 3.
- Figure 8c is an infrared photograph for evaluating the heat shielding performance of the transparent film of Comparative Example 4.
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Abstract
Description
구조 | 측정모드 | L* | a* | b* | Y | 550nm | 면저항 (Ω/sq) |
CuOx/Ag/CuOx | 투과 | 93.98 | -0.84 | 1.36 | 85.22 | 85.24 | 10.94 |
반사 | 25.74 | -0.95 | -4.68 | 4.66 | 4.82 | ||
CuNx/Ag/CuNx | 투과 | 93.16 | -1.16 | 0.7 | 83.33 | 83.58 | 11.66 |
반사 | 24.6 | 1.68 | -2.3 | 4.29 | 4.34 |
평가 항목 | 비교실시예 1 | 비교실시예 2 | 본 발명의 실시예 | |
투과율 | Y | 65.4 | 77.3 | 88.1 |
@ 550 nm | 76.9 | 77.6 | 88.4 |
평가 항목 | 비교실시예 1 | 비교실시예 2 | 본 발명의 실시예 | ||||
전 | 후 | 전 | 후 | 전 | 후 | ||
투과율 | Y | 65.4 | 72.7 | 77.6 | 78.6 | 88.1 | 88.4 |
@ 550 nm | 65.6 | 73.2 | 77.6 | 79.5 | 87.2 | 89.4 |
비교실시예1 | 본 발명의 실시예 | |
투습도(mg/m2·day) | 5200 | 210 |
Claims (6)
- 기재층;상기 기재층 일면에 적층되는 제1 무기물층;상기 제1 무기물층 일면에 적층되는 금속층;상기 금속층 일면에 적층되는 제2 무기물층; 및상기 제2 무기물층 일면에 적층되는 복수의 유기물층을 포함하는 패시베이션층;을 포함하는 것을 특징으로 하는 내구성이 강화된 투명필름.
- 제1항에 있어서,상기 기재층의 양면에 각각 배치되는 하드코팅층;을 더 포함하는 것을 특징으로 하는 내구성이 강화된 투명필름.
- 제1항에 있어서,상기 기재층과상기 제1 무기물층 사이, 상기 제2 무기물층과 상기 패시베이션층 사이에 각각 배치되어 굴절률을 보강하는 굴절률 매칭층;을 더 포함하는 것을 특징으로 하는 내구성이 강화된 투명필름.
- 제1항에 있어서,상기 패시베이션층은,제1 유기물을 포함하는 제1 패시베이션층;제2 유기물을 포함하는 제2 패시베이션층;제3 유기물을 포함하는 제3 패시베이션층; 및제4 유기물을 포함하는 제4 패시베이션층;을 포함하는 것을 특징으로 하는 내구성이 강화된 투명필름.
- 제1항에 있어서,상기 금속층은 은(Ag)을 포함하고,상기 제1 무기물층 및 제2 무기물층은 구리산화물(CuOx)을 포함하는 것을 특징으로 하는 내구성이 강화된 투명필름.
- 제1항에 있어서,상기 금속층은 은(Ag)을 포함하고,상기 제1 무기물층 및 제2 무기물층은 구리질화물(CuNx)을 포함하는 것을 특징으로 하는 내구성이 강화된 투명필름.
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JP6584187B2 (ja) * | 2015-07-22 | 2019-10-02 | 日東電工株式会社 | 積層体及びその製造方法 |
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