WO2022202170A1 - ガスバリアフィルム及びガスバリアフィルムの製造方法 - Google Patents
ガスバリアフィルム及びガスバリアフィルムの製造方法 Download PDFInfo
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- WO2022202170A1 WO2022202170A1 PCT/JP2022/008955 JP2022008955W WO2022202170A1 WO 2022202170 A1 WO2022202170 A1 WO 2022202170A1 JP 2022008955 W JP2022008955 W JP 2022008955W WO 2022202170 A1 WO2022202170 A1 WO 2022202170A1
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- Prior art keywords
- gas barrier
- barrier layer
- inorganic transparent
- barrier film
- gas
- Prior art date
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- 230000004888 barrier function Effects 0.000 title claims abstract description 243
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000000463 material Substances 0.000 claims abstract description 64
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 229910052743 krypton Inorganic materials 0.000 claims description 24
- 229910052724 xenon Inorganic materials 0.000 claims description 23
- 150000007530 organic bases Chemical class 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 229910052718 tin Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 description 127
- 239000010410 layer Substances 0.000 description 107
- 238000004544 sputter deposition Methods 0.000 description 15
- 229910052760 oxygen Inorganic materials 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 230000005540 biological transmission Effects 0.000 description 12
- 239000011701 zinc Substances 0.000 description 12
- 239000011135 tin Substances 0.000 description 10
- -1 etc. Substances 0.000 description 9
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 239000000356 contaminant Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000002346 layers by function Substances 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
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- 238000001514 detection method Methods 0.000 description 4
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- 238000002834 transmittance Methods 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
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- 229910045601 alloy Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229920001225 polyester resin Polymers 0.000 description 3
- 239000004645 polyester resin Substances 0.000 description 3
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- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
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- 238000009434 installation Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 229920001748 polybutylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- 229920001577 copolymer Polymers 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical group [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920001485 poly(butyl acrylate) polymer Polymers 0.000 description 1
- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
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- 229920002530 polyetherether ketone Polymers 0.000 description 1
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- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/048—Forming gas barrier coatings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- 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
- C23C14/08—Oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- 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
- C23C14/34—Sputtering
Definitions
- the present invention relates to a gas barrier film and a method for producing a gas barrier film.
- gas barrier films are used for packaging of foods, industrial goods, pharmaceuticals, etc., liquid crystal display elements, OLED (Organic Light Emitting Diode), organic EL (organic Electro-Luminescence), substrates for solar cells, etc. Widely used.
- a gas barrier sheet with suppressed warpage for example, a gas barrier sheet having, on a substrate, an anchor layer containing a polysiloxane polymer and a gas barrier layer containing silicon oxide and a conductive material has been disclosed (for example, see Patent Document 1).
- the gas barrier sheet of Patent Document 1 needs to have two layers, an anchor layer and a gas barrier layer, in order to make it difficult to warp.
- the materials to be used are limited to materials containing Si.
- a gas barrier layer containing a compound such as Si, Zn, Sn, or Al is generally used for a gas barrier film. It is desirable to be able to select as appropriate. Therefore, in order to utilize the gas barrier film, there is a demand for a method of suppressing the warpage of the gas barrier film without being restricted by the materials constituting the gas barrier layer, such as the compounds described above.
- An object of one aspect of the present invention is to provide a gas barrier film capable of suppressing warping without limiting the material constituting the gas barrier layer.
- One aspect of the gas barrier film according to the present invention comprises an organic base material and an inorganic transparent barrier layer provided on one side of the organic base material, and the inorganic transparent barrier layer contains a barrier material as a main component. , and at least one of Kr and Xe.
- Another aspect of the method for producing a gas barrier film according to the present invention is the above-described method for producing a gas barrier film, wherein a target containing Zn is used in a gas atmosphere containing at least one of Kr and Xe to produce a Then, the inorganic transparent barrier layer is formed by sputtering a barrier material containing at least one of Kr and Xe.
- One aspect of the gas barrier film according to the present invention can suppress warpage without limiting the material that constitutes the gas barrier layer.
- FIG. 1 is a schematic cross-sectional view showing the structure of the gas barrier film according to this embodiment.
- the gas barrier film 1 according to this embodiment includes an organic substrate 10 and an inorganic transparent barrier layer 20 provided on the upper surface 10a side of the organic substrate 10.
- the inorganic transparent barrier layer 20 is It contains at least one of krypton (Kr) and xenon (Xe) as a mixed component while containing a barrier material as a main component.
- the gas barrier film 1 can suppress warping (curling) regardless of the material of the main component constituting the inorganic transparent barrier layer 20.
- the thickness direction (vertical direction) of the gas barrier film 1 is defined as the Z-axis direction
- the lateral direction (horizontal direction) orthogonal to the thickness direction is defined as the X-axis direction.
- the inorganic transparent barrier layer 20 side in the Z-axis direction is the +Z-axis direction
- the organic substrate 10 side is the -Z-axis direction.
- the +Z-axis direction is referred to as upward or upward
- the ⁇ Z-axis direction is referred to as downward or downward, but this does not represent a universal vertical relationship.
- the main component means that the content of the barrier material is 95 atm% or more, preferably 97 atm% or more, more preferably 99 atm% or more.
- the organic substrate 10 is a plate-like member or film having two opposing main surfaces, and is a substrate on which the inorganic transparent barrier layer 20 is installed.
- the organic substrate 10 is provided so that the lower surface of the inorganic transparent barrier layer 20 is in contact with the upper surface (principal surface) 10a.
- a polymer can be used as a material for forming the organic base material 10 .
- polymers examples include acrylic resins, polyester resins, polyolefin resins, cyclic polyolefins, triacetyl cellulose (TAC), polyether sulfide (PES), polyether ketones, polyether ether ketones, and polyimides. These may be used individually by 1 type, and may use 2 or more types together.
- acrylic resins examples include polycarbonate (PC), polymethyl methacrylate (PMMA), polyethyl methacrylate, and polybutyl acrylate.
- polyester resins examples include polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polybutylene terephthalate, and isophthalate copolymers.
- polyolefin resins examples include polyethylene (PE), polypropylene (PP), polybutylene (PB), polypentene, and cycloolefin polymers.
- polyester resins and polyolefin resins are preferable from the viewpoint of transparency.
- PET and cycloolefin polymer resins are more preferred.
- the thickness of the organic base material 10 is not particularly limited, and can be set to any desired thickness according to the use of the gas barrier film 1, the material of the organic base material 10, and the like.
- the thickness of the organic substrate 10 is, for example, preferably 10 ⁇ m to 400 ⁇ m, more preferably 20 ⁇ m to 200 ⁇ m.
- the thickness of the organic substrate 10 refers to the length of the organic substrate 10 in the direction perpendicular to the main surface.
- the thickness of the organic substrate 10 may be, for example, the thickness measured at an arbitrary location in the cross section of the organic substrate 10, or the thickness measured at several locations at arbitrary locations, and the average value of these measured values. good too.
- the definition of thickness is similarly defined for other members.
- the organic base material 10 preferably has an absorptance of, for example, 4% or less for light with a wavelength of 380 nm.
- absorptance of the organic base material 10 for example, catalog values are adopted. Absorption of light on the short wavelength side is due to the bandgap. If the bandgap is close to the short wavelength component of visible light, absorption in the short wavelength region may occur. On the other hand, when the bandgap is wide, the absorption edge on the short wavelength side shifts to the short wavelength side, so absorption of visible light can be reduced. That is, the transparency of the organic substrate 10 is improved. Therefore, in the present embodiment, regarding the absorptance of the organic base material 10, attention is paid to the absorptivity of light with a wavelength of 380 nm, which is located in the short wavelength region, among visible light.
- the organic substrate 10 may have, for example, an easy-adhesion layer (not shown) on its lower main surface.
- the inorganic transparent barrier layer 20 is provided on the upper surface 10a of the organic substrate 10, as shown in FIG.
- the inorganic transparent barrier layer 20 can contain a transparent oxide film, and is preferably made of a transparent oxide film.
- the transparent oxide film preferably contains a barrier material as a main component and at least one of Kr and Xe as an additive component, and has transparency (optical transparency) to visible light.
- having light transmittance refers to the transparency of transmitting visible light (light with a wavelength of 380 nm to 780 nm) through the inside of the transparent oxide film when it is irradiated from one main surface side of the transparent oxide film. It means that you have The visible light transmittance of the transparent oxide film is preferably 60% or more, more preferably 75% or more, and still more preferably 90% or more. Visible light transmittance can be specified as the average value of transmittance at each wavelength when measured using a spectrophotometer at wavelengths from 380 nm to 780 nm.
- the barrier material contains at least one component selected from the group consisting of zinc (Zn), silicon (Si), tin (Sn), magnesium (Mg) and aluminum (Al), and at least one of oxygen and nitrogen. is preferred. That is, the barrier material preferably contains an oxide containing at least one component selected from the group consisting of Zn, Si, Sn, Mg and Al.
- the barrier material consists essentially of the oxide containing the above components, and more preferably consists of only the oxide containing the above components.
- the term "substantially” means that in addition to oxides containing the above components and contaminant components, unavoidable impurities that may be unavoidably included during the manufacturing process may be included.
- the content of unavoidable impurities is, for example, 0.02 atomic % or less, more preferably 0.01 atomic % or less.
- barrier materials include oxides mainly composed of Si, composite oxides containing Zn, Al, Si and oxygen, composite oxides containing Zn, Sn and oxygen, Zn, Sn, Mg and oxygen. can be used.
- the barrier material is a Zn-based material containing at least one of Zn and Si as an essential element and a At least one of Si-based materials is preferable.
- the content of Zn contained in the barrier material is preferably 0 at % to 90 at %, more preferably 10 at % to 80 at %, even more preferably 20 at % to 70 at %.
- the Si content is preferably 0 at % to 90 at %, more preferably 10 at % to 80 at %, even more preferably 20 at % to 70 at %.
- the Sn content is preferably 0 at % to 90 at %, more preferably 10 at % to 80 at %, even more preferably 20 at % to 70 at %.
- the content of Mg is preferably 0 at % to 40 at %, more preferably 3 at % to 30 at %, even more preferably 5 at % to 25 at %.
- the content of Al is preferably 0 at % to 40 at %, more preferably 3 at % to 30 at %, even more preferably 5 at % to 25 at %.
- the content of the barrier material contained in the transparent oxide film is not particularly limited as long as the absorption rate and water vapor transmission rate for light (light with a wavelength of 380 nm) can be lowered, and can be determined arbitrarily.
- the identification and quantification of the main components contained in the transparent oxide film can be obtained, for example, using a fluorescent X-ray spectrometer.
- the content of the mixed component contained in the transparent oxide film is preferably more than 0 at % and 0.2 at % or less, more preferably 0.02 at % to 0.15 at %, and more preferably 0.04 at % to 0.10 at %. % is more preferred. If the content of the mixed component is within the preferred range described above, the amount of the component entering into the crystal lattice of the barrier material constituting the inorganic transparent barrier layer 20 can be suppressed. As a result, the inorganic transparent barrier layer 20 can be prevented from warping. In addition, since the content of the barrier material contained in the inorganic transparent barrier layer 20 can be kept high, the durability of the inorganic transparent barrier layer 20 can be enhanced and the adhesion to the organic substrate 10 can be improved.
- the content of contaminants can be measured, for example, by Rutherford backscattering analysis (RBS) using Pelletron 3SDH (manufactured by NEC Corporation) as a measuring device.
- RBS Rutherford backscattering analysis
- Pelletron 3SDH manufactured by NEC Corporation
- the thickness of the inorganic transparent barrier layer 20 is preferably 10 nm to 500 nm, more preferably 15 nm to 450 nm, even more preferably 30 nm to 400 nm. If the thickness of the inorganic transparent barrier layer 20 is within the above preferred range, the function of the inorganic transparent barrier layer 20 can be exhibited. In addition, even if the inorganic transparent barrier layer 20 contains a mixed component, the occurrence of cracks or the like in the inorganic transparent barrier layer 20 can be reduced, the deterioration of the barrier function can be suppressed, and the inorganic transparent barrier layer 20 can be prevented from warping. You can prevent it from happening.
- the method for measuring the thickness of the inorganic transparent barrier layer 20 can be the same as the method for measuring the thickness of the organic substrate 10 .
- the film density of the inorganic transparent barrier layer 20 can be set as appropriate, and is not particularly limited as long as it is within a range in which high gas barrier properties can be exhibited.
- the gas barrier properties of the inorganic transparent barrier layer 20 can be evaluated by measuring the water vapor transmission rate.
- the water vapor transmission rate can be measured at 25 ⁇ 0.5° C. and 90 ⁇ 2% RH based on JIS K 7129-1992.
- the water vapor transmission rate is, for example, preferably 5.0 ⁇ 10 ⁇ 2 (g/m 2 /day) or less, more preferably 4.0 ⁇ 10 ⁇ 2 (g/m 2 /day) or less, and 3.5 ⁇ 10 ⁇ 2 (g/m 2 /day) or less is more preferable. If the water vapor transmission rate of the gas barrier film 1 is equal to or less than the above preferable upper limit, the gas barrier film 1 is excellent in barrier properties, particularly water vapor barrier properties. In addition, the lower limit of the water vapor transmission rate of the gas barrier film 1 is not particularly limited.
- the transparency of the gas barrier film 1 can be evaluated by measuring the absorption rate for light with a wavelength of 380 nm.
- the absorbance of the gas barrier film 1 for light with a wavelength of 380 nm is, for example, preferably 12% or less, more preferably 10% or less, and even more preferably 7% or less. If the absorptance of the gas barrier film 1 for light with a wavelength of 380 nm is equal to or less than the above preferable upper limit, the gas barrier film 1 can have excellent transparency.
- the lower limit of the absorptance of the gas barrier film 1 for light with a wavelength of 380 nm is not particularly limited. Incidentally, the method for measuring the absorptivity is not particularly limited, and any suitable measuring method can be used.
- the atmosphere in which the organic base material 10 is placed is a gas atmosphere containing at least one of Kr and Xe. Then, in a gas atmosphere containing at least one of Kr and Xe, at least one of Kr and Xe is sputtered onto the upper surface 10a of the organic substrate 10 with a barrier material that constitutes the main component of the inorganic transparent barrier layer 20. as a mixed component and the inorganic transparent barrier layer 20 containing the barrier material as a main component is formed.
- the gas barrier film 1 is obtained by laminating the inorganic transparent barrier layer 20 on the upper surface 10 a of the organic substrate 10 .
- Examples of methods for forming the inorganic transparent barrier layer 20 include dry processes such as sputtering and vapor deposition, and wet processes such as plating.
- a thin inorganic transparent barrier layer 20 can be easily formed by using a dry process as a method for forming the inorganic transparent barrier layer 20 .
- a method for forming the inorganic transparent barrier layer 20 by using sputtering among dry processes, a barrier material is used as a main component and at least one of Kr and Xe is included as a mixed component in the main component, and an inorganic transparent barrier layer 20 with a high density is formed.
- a barrier layer 20 can be formed.
- the inside of the film forming chamber of the sputtering apparatus is an inert gas atmosphere.
- the inert gas contains at least one of Kr and Xe
- at least one of Kr atoms and Xe atoms enters into the crystal lattice of the barrier material contained in the inorganic transparent barrier layer 20, but other inert gases.
- Ar atoms are less likely to enter into the crystal lattice of the barrier material contained in the inorganic transparent barrier layer 20 than Ar atoms. Therefore, the film stress generated in the inorganic transparent barrier layer 20 is suppressed, and the warp of the inorganic transparent barrier layer 20 caused by the film stress can be suppressed. Therefore, by forming the inorganic transparent barrier layer 20 by sputtering in a gas atmosphere containing at least one of Kr and Xe, the inorganic transparent barrier layer 20 can be formed while suppressing warping.
- the organic base material 10 is placed on a film forming plate that serves as an anode in a film forming chamber of a sputtering device.
- the deposition plate may be rotatable, for example.
- the inorganic transparent barrier layer 20 can be formed on the organic substrate 10 in batch mode.
- the organic substrate 10 may be wound around a drum roll, which is a film-forming roll, instead of the film-forming plate as an anode.
- a drum roll By arranging a drum roll in the film forming chamber, it is possible to continuously form the inorganic transparent barrier layer 20 on the organic substrate 10 while transporting the organic substrate 10 in a roll-to-roll manner. Become.
- the organic base material 10 includes, for example, an easy-adhesion layer
- the easy-adhesion layer is brought into contact with the anode.
- a plurality or a single target containing the barrier material contained as a main component in the inorganic transparent barrier layer 20 is used as a cathode.
- a plurality of targets or a single target are arranged so as to face the film forming plate with a gap therebetween.
- each target contains a different type of material that constitutes the barrier material contained in the inorganic transparent barrier layer 20 .
- a target containing Zn, a target containing Si or Sn, and a target containing Al or Mg can be used.
- each target may be a metal oxide target containing oxygen.
- a plurality of targets are preferably arranged in the deposition chamber at intervals. At the time of sputtering, the power applied to each target is adjusted according to the type of barrier material contained in the inorganic transparent barrier layer 20, and the atoms of the materials constituting the inorganic transparent barrier layer 20 are separated. Adjust proportions.
- the single target When a single target is used as a cathode, the single target contains the barrier material contained in the inorganic transparent barrier layer 20.
- an alloy target in which the atomic proportions of the barrier materials contained in the inorganic transparent barrier layer 20 are adjusted can be used.
- an alloy target containing Zn, Si or Sn, and Al or Mg can be used.
- the alloy target may be a metal oxide target containing barrier material and oxygen.
- At least one of Kr gas and Xe gas is supplied as a sputtering gas into the film forming chamber of the sputtering apparatus to create a gas atmosphere containing at least one of Kr and Xe in the film forming chamber.
- an oxygen gas may be supplied as a sputtering gas into the film forming chamber to create a gas atmosphere containing at least one of Kr and Xe and oxygen.
- At least one of Kr gas and Xe gas may be supplied into the deposition chamber, or a mixed gas containing at least one of Kr gas and Xe gas and oxygen gas may be supplied, or Kr gas and Xe gas may be supplied. At least one of the gases and the oxygen gas may be supplied separately.
- the degree of vacuum in the film forming chamber is preferably adjusted to 0.1 Pa to 2.0 Pa, more preferably 0.15 Pa to 0.8 Pa, and even more preferably 0.2 Pa to 0.6 Pa. If the degree of vacuum in the film forming chamber is within the above preferable range, the gas barrier properties of the inorganic transparent barrier layer 20 can be enhanced. In addition, since the amount of Kr atoms or Xe atoms entering the crystal lattice of the barrier material contained in the inorganic transparent barrier layer 20 can be suppressed, the film stress can be suppressed, and the resulting gas barrier film 1 can be prevented from warping. . At this time, the pressure in the mixed gas atmosphere during sputtering is preferably 0.10 Pa to 2.00 Pa, more preferably 0.15 Pa to 0.80 Pa, even more preferably 0.20 Pa to 0.60 Pa.
- the ratio of the flow rate of oxygen to the total flow rate of at least one of Kr and Xe and oxygen depends on the type of gas, the content of oxygen contained in the barrier material, and the like. For example, it is preferably 0.1% to 20%, more preferably 1% to 10%.
- the ratio of the flow rate of oxygen to the total flow rate of at least one of Kr and Xe and oxygen is within the above preferred range, by sputtering the organic substrate 10 using a plurality or single targets containing barrier materials
- the inorganic transparent barrier layer 20 even if Kr atoms or Xe atoms enter the crystal lattice of the barrier material contained in the inorganic transparent barrier layer 20, the amount of the atoms entering can be suppressed. Therefore, it is possible to prevent the inorganic transparent barrier layer 20 from being warped due to film stress.
- the gas barrier film 1 includes the organic substrate 10 and the inorganic transparent barrier layer 20.
- the inorganic transparent barrier layer 20 contains a barrier material as a main component and at least one of Kr and Xe. as a contaminant.
- the gas barrier film 1 can reduce the film stress of the inorganic transparent barrier layer 20 .
- an anchor layer for suppressing warpage generated in the inorganic transparent barrier layer 20 cannot be separately provided between the organic substrate 10 and the inorganic transparent barrier layer 20. may Therefore, the barrier material contained in the inorganic transparent barrier layer 20 need not be selected in consideration of the material forming the anchor layer.
- the inorganic transparent barrier layer 20 laminated on the anchor layer is limited to a material containing Si, which readily interacts with C contained in the anchor layer. Since the gas barrier film 1 does not need to provide an anchor layer between the organic substrate 10 and the inorganic transparent barrier layer 20, it is possible to reduce the limitation on the types of barrier materials contained in the inorganic transparent barrier layer 20. Therefore, the gas barrier film 1 can reduce the film stress of the inorganic transparent barrier layer 20 without providing an anchor layer for relaxing the stress of the inorganic transparent barrier layer 20 between the organic base material 10 and the inorganic transparent barrier layer 20. Since the thickness can be kept low, warpage can be suppressed without limiting the barrier material contained in the inorganic transparent barrier layer 20 .
- the gas barrier film 1 can suppress warping, other functional layers can be provided on the gas barrier film 1 with high accuracy. Therefore, the gas barrier film 1 can have excellent barrier properties over a long period of time.
- the amount of warpage of the gas barrier film 1 is defined as the perpendicularity between the surface of the substrate in contact with the gas barrier film 1 and each corner of the gas barrier film 1 when the gas barrier film 1 is placed on the substrate with the convex side of the gas barrier film 1 facing downward. It can be obtained by calculating the average value of the height in the direction. For example, as shown in FIG. 2, when the gas barrier film 1 is formed in a square shape in plan view, the average height in the vertical direction between the installation surface of the gas barrier film 1 with the substrate 2 and the four corners 1a of the gas barrier film 1 is The value is defined as the amount of warpage of the gas barrier film 1 .
- the gas barrier film 1 does not require an additional anchor layer between the organic base material 10 and the inorganic transparent barrier layer 20 to suppress the warping of the inorganic transparent barrier layer 20, the gas barrier film 1 can be easily manufactured. In addition, manufacturing costs can be reduced.
- the total content of Kr and Xe in the inorganic transparent barrier layer 20 can be more than 0 atomic % and 0.2 atomic % or less. As a result, the film stress generated in the inorganic transparent barrier layer 20 can be reliably suppressed, so that the gas barrier film 1 can more reliably suppress warping.
- the inorganic transparent barrier layer 20 can contain an oxide containing at least one component selected from the group consisting of Si, Zn, Sn, Al and Mg. Thereby, the gas barrier film 1 can exhibit high gas barrier properties and can suppress warping.
- the inorganic transparent barrier layer 20 can have a thickness of 10 nm to 500 nm. As a result, the gas barrier film 1 can reduce film stress and suppress warpage while reducing the film thickness.
- the arithmetic average roughness Ra of the inorganic transparent barrier layer 20 can be 0.2 nm to 2.0 nm. Thereby, the gas barrier film 1 can have a more stable and high gas barrier property.
- the gas barrier film 1 has the properties as described above, it can be suitably used for, for example, an image display device, a solar cell, and the like.
- image display devices include organic EL displays and liquid crystal displays.
- solar cells include flexible solar cells.
- Examples 1-1, 2-1, 3-1 and 4-1 are examples, and the other examples are comparative examples.
- Example 1-1 [Production of gas barrier film 1] A polyethylene terephthalate (PET) film (thickness: 125 ⁇ m) as an organic substrate was placed on a film forming plate provided in a film forming chamber of a sputtering apparatus. Next, a target made of AlZnSiOx in which ZnO, Al 2 O 3 and SiO 2 were adjusted to have a mass ratio of 77 wt %/3 wt %/20 wt % was placed in the film forming chamber of the sputtering apparatus.
- PET polyethylene terephthalate
- Kr gas and O 2 gas were introduced into the film formation chamber to create a mixed gas atmosphere of Kr and O 2 in the film formation chamber.
- a power of 100 W was applied to the target from a DC power supply to form an inorganic transparent barrier layer on one main surface of the PET film so as to have a thickness of 100 nm, thereby producing a gas barrier film.
- the total thickness of the gas barrier film was 100 nm.
- Kr content in inorganic transparent barrier layer A sample of the gas barrier film was produced under the same conditions as the gas barrier film.
- the content of Kr which is a contaminant contained in the sample of the gas barrier film, was measured using Rutherford backscattering spectrometry (RBS) using Pelletron 3SDH (manufactured by NEC Corporation), based on the following measurement conditions and evaluation criteria.
- the content of Kr contained as a contaminant in the inorganic transparent barrier layer was measured. When the Kr content was greater than 0 atomic % and 0.2 atomic % or less, it was evaluated that the Kr content was suitably included. Table 1 shows the measurement results of the Kr content.
- the produced gas barrier film was cut into a size of 10 cm square in plan view, and the cut gas barrier film was placed on a flat plate so that the inorganic transparent barrier layer was on the lower side. At this time, the temperature was room temperature (23° C.). After 1 minute had elapsed, the four corners of the gas barrier film were warped, and the amount of warpage at each corner, that is, the height in the vertical direction between the installation surface of the flat plate and the four corners was measured, and the average value was calculated. The amount of warpage of the gas barrier film was determined (see FIG. 2). When the amount of warp was 2.5 mm or less, the warp of the gas barrier film was evaluated as good. Table 1 shows the measurement results of the amount of warpage.
- the gas barrier property was evaluated by measuring the water vapor transmission rate of the gas barrier film using a water vapor transmission rate measuring device (DELTAPERM, manufactured by Technolox) under the conditions of a temperature of 40°C, a humidity of 90% RH, and a measurement area of 50 cm 2 . . Table 1 shows the measurement results.
- Example 1-1 the procedure was carried out in the same manner as in Example 1-1, except that the mixing ratio of Kr gas and O 2 gas was changed to change the Kr content of the inorganic transparent barrier layer as shown in Table 1. rice field.
- the Kr content was less than 0.02 at %, which is the detection limit measurable by Pelletron 3SDH (manufactured by NEC), and was evaluated as 0.
- Examples 2-1 and 2-2 The procedure was carried out in the same manner as in Example 1-1, except that the type of organic substrate was changed from PET film to COP film (thickness: 40 ⁇ m). Note that the Kr content in Example 2-2 was less than the detection limit of 0.02 atomic % and was evaluated as 0, as in Example 1-2.
- Examples 3-1 and 3-2 In Example 1-1, the sputtering target was changed to a sputtering target made of ZnSnOx in which ZnO and SnO 2 were adjusted to a mass ratio of 39.1 wt%/60.9 wt%, and the type of inorganic transparent barrier layer was changed from AlZnSiOx to ZnSnOx. The procedure was carried out in the same manner as in Example 1-1, except that it was changed to Note that the Kr content in Example 3-2 was less than the detection limit of 0.02 atomic %, similarly to Example 1-2, and was evaluated as 0.
- Example 1-1 the sputtering target was changed to a sputtering target made of ZnSnMgOx in which the mass ratio of ZnO, SnO 2 and MgO was adjusted to 35.5 wt%/53.8 wt%/10.7 wt%, and the inorganic transparent barrier Example 1-1 was repeated except that the type of layer was changed from AlZnSiOx to ZnSnMgOx. Note that the Kr content in Example 4-2 was less than the detection limit of 0.02 atomic %, similarly to Example 1-2, and was evaluated as 0.
- Table 1 shows the type of organic substrate, the type of the main component of the inorganic transparent barrier layer, the measurement results of the Kr content of the inorganic transparent barrier layer, and the measurement results of the amount of warp and water vapor transmission rate of the gas barrier film of each example. shown in
- Examples 1-1, 2-1, 3-1 and 4-1 are warped more than Examples 1-2, 2-2, 3-2 and 4-2, respectively. It was confirmed that the amount and water vapor transmission rate could be reduced.
- the gas barrier films of Examples 1-1, 2-1, 3-1 and 4-1 differ from the gas barrier films of the other examples in that the Kr content is greater than 0 atomic % and 0.2 atomic % or less.
- the ratio is within the range, warping can be suppressed regardless of the material of the gas barrier layer, so it can be said that the gas barrier film can stably exhibit excellent gas barrier properties.
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Abstract
Description
本発明の実施形態に係るガスバリアフィルムについて説明する。図1は、本実施形態に係るガスバリアフィルムの構成を示す概略断面図である。図1に示すように、本実施形態に係るガスバリアフィルム1は、有機基材10と、有機基材10の上面10a側に設けられる無機透明バリア層20とを備え、無機透明バリア層20は、バリア材料を主成分として含みつつ、クリプトン(Kr)及びキセノン(Xe)の少なくとも一方を混入成分として含む。
[ガスバリアフィルム1の製造]
有機基材としてポリエチレンテレフタレート(PET)フィルム(厚さ:125μm)をスパッタリング装置の成膜室内に設けた成膜板に設置した。次いで、ZnOとAl2O3とSiO2とが質量比で77wt%/3wt%/20wt%に調整されたAlZnSiOxからなるターゲットをスパッタリング装置の成膜室に配置した。成膜室内を真空排気した後、KrガスとO2ガス(Krガス:O2ガス=98:2)を成膜室内に導入し、成膜室内をKrとO2との混合ガス雰囲気とした。その後、ターゲットにDC電源から100Wの電力を印加して、PETフィルムの一方の主面に無機透明バリア層を厚さが100nmとなるように成膜し、ガスバリアフィルムを製造した。ガスバリアフィルムの全体の厚さは、100nmとした。
なお、ガスバリアフィルムと同様の条件で作製したガスバリアフィルムのサンプルを作製した。ガスバリアフィルムのサンプルに含まれる混入成分であるKrの含有量を、ラザフォード後方散乱分析法(RBS)を用いて、Pelletron 3SDH(NEC社製)を使用し、下記測定条件及び評価基準に基づいて、無機透明バリア層内に混入成分として含まれるKrの含有量を測定した。Kr含有量が0at%よりも大きく0.2at%以下である場合、Kr含有量は好適に含まれると評価した。Kr含有量の測定結果を表1に示す。
((測定条件))
・入射イオン:4He++
・入射エネルギー:2300keV
・入射角:0deg
・散乱角:108deg
・試料電流:24nA
・ビーム径:2mmφ
・面内回転:無
・照射量:80μC
ガスバリアフィルムの反り量及び水蒸気透過率を測定し、評価した。
作製したガスバリアフィルムを平面視で10cm四方のサイズにカットし、カットしたガスバリアフィルムを無機透明バリア層が下側になるように、平板上に設置した。このとき、温度は、室温(23℃)であった。1分経過後に、ガスバリアフィルムの各四隅が反り上がり、それぞれの反り上がり量、即ち、平板の設置面と各四隅との垂直方向における高さを測定し、これらの平均値を算出することで、ガスバリアフィルムの反り量を求めた(図2参照)。反り量が2.5mm以下である場合、ガスバリアフィルムの反りは良好であると評価した。反り量の測定結果を表1に示す。
温度40℃、湿度90%RH、測定面積50cm2の条件で、水蒸気透過率測定装置(DELTAPERM、テクノロックス社製)を使用して、ガスバリアフィルムの水蒸気透過率を測定し、ガスバリア性を評価した。測定結果を表1に示す。
例1-1において、KrガスとO2ガスとの混合比を変更して、無機透明バリア層のKr含有量を表1のように変更したこと以外は、例1-1と同様にして行った。なお、Kr含有量は、Pelletron 3SDH(NEC社製)で測定可能な検出限界である0.02at%未満であり、0と評価した。
例1-1において、有機基材の種類をPETフィルムからCOPフィルム(厚さ:40μm)に変更したこと以外は、例1-1と同様にして行った。なお、例2-2のKr含有量は、例1-2と同様、検出限界である0.02at%未満であり、0と評価した。
例1-1において、スパッタリングターゲットをZnOとSnO2とが質量比で39.1wt%/60.9wt%に調整されたZnSnOxからなるスパッタリングターゲットに変更し、無機透明バリア層の種類をAlZnSiOxからZnSnOxに変更したこと以外は、例1-1と同様にして行った。なお、例3-2のKr含有量は、例1-2と同様、検出限界である0.02at%未満であり、0と評価した。
例1-1において、スパッタリングターゲットをZnOとSnO2とMgOとが質量比で35.5wt%/53.8wt%/10.7wt%に調整されたZnSnMgOxからなるスパッタリングターゲットに変更し、無機透明バリア層の種類をAlZnSiOxからZnSnMgOxに変更したこと以外は、例1-1と同様にして行った。なお、例4-2のKr含有量は、例1-2と同様、検出限界である0.02at%未満であり、0と評価した。
10 有機基材
20 無機透明バリア層
Claims (7)
- 有機基材と、
前記有機基材の一方の面側に設けられる無機透明バリア層とを備え、
前記無機透明バリア層は、バリア材料を主成分として含み、かつKr及びXeの少なくとも一方を含む、ガスバリアフィルム。 - 前記無機透明バリア層のKrとXeとの合計含有量が、0at%超え0.2at%以下である請求項1に記載のガスバリアフィルム。
- 前記無機透明バリア層は、Zn、Si、Sn、Al及びMgからなる群から選択される少なくとも1つの成分を有する酸化物を含む請求項1又は2に記載のガスバリアフィルム。
- 前記無機透明バリア層の厚さが、10nm~500nmである請求項1~3の何れか一項に記載のガスバリアフィルム。
- 前記無機透明バリア層の算術平均粗さRaが、0.2nm~2.0nmである請求項1~4の何れか一項に記載のガスバリアフィルム。
- 請求項1~5の何れか一項に記載のガスバリアフィルムの製造方法であって、
Kr及びXeの少なくとも一方を含むガス雰囲気において、Znを含むターゲットを用いて、有機基材上に、Kr及びXeの少なくとも一方を含みつつバリア材料をスパッタリングすることにより前記無機透明バリア層を成膜するガスバリアフィルムの製造方法。 - 真空度が、0.1Pa~2.0Paである請求項6に記載のガスバリアフィルムの製造方法。
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WO2012039355A1 (ja) * | 2010-09-21 | 2012-03-29 | リンテック株式会社 | ガスバリアフィルム、その製造方法、電子デバイス用部材及び電子デバイス |
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WO2012039355A1 (ja) * | 2010-09-21 | 2012-03-29 | リンテック株式会社 | ガスバリアフィルム、その製造方法、電子デバイス用部材及び電子デバイス |
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