JP6610803B2 - ガスバリア性積層体 - Google Patents
ガスバリア性積層体 Download PDFInfo
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- JP6610803B2 JP6610803B2 JP2018541443A JP2018541443A JP6610803B2 JP 6610803 B2 JP6610803 B2 JP 6610803B2 JP 2018541443 A JP2018541443 A JP 2018541443A JP 2018541443 A JP2018541443 A JP 2018541443A JP 6610803 B2 JP6610803 B2 JP 6610803B2
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- film
- gas barrier
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- 230000004888 barrier function Effects 0.000 title claims description 41
- 239000010408 film Substances 0.000 claims description 59
- 239000010409 thin film Substances 0.000 claims description 31
- 238000007740 vapor deposition Methods 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 49
- 229910004298 SiO 2 Inorganic materials 0.000 description 22
- 239000010410 layer Substances 0.000 description 21
- 239000002253 acid Substances 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 9
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 8
- 238000001816 cooling Methods 0.000 description 8
- 229910001882 dioxygen Inorganic materials 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 238000004806 packaging method and process Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 229910052814 silicon oxide Inorganic materials 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 238000010030 laminating Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920000620 organic polymer Polymers 0.000 description 5
- -1 polyethylene Polymers 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 238000001771 vacuum deposition Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229920002799 BoPET Polymers 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000005022 packaging material Substances 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000001771 impaired effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000002985 plastic film Substances 0.000 description 3
- 229920006255 plastic film Polymers 0.000 description 3
- 229920000307 polymer substrate Polymers 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- UOBYKYZJUGYBDK-UHFFFAOYSA-N 2-naphthoic acid Chemical compound C1=CC=CC2=CC(C(=O)O)=CC=C21 UOBYKYZJUGYBDK-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 description 1
- 229920000299 Nylon 12 Polymers 0.000 description 1
- 229920001007 Nylon 4 Polymers 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 208000028659 discharge Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000005606 hygroscopic expansion Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
Classifications
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/02—Wrappers or flexible covers
- B65D65/22—Details
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/42—Applications of coated or impregnated materials
-
- 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
- C08J7/06—Coating with compositions not containing macromolecular substances
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D2565/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D2565/38—Packaging materials of special type or form
- B65D2565/381—Details of packaging materials of special type or form
- B65D2565/387—Materials used as gas barriers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D2585/00—Containers, packaging elements or packages specially adapted for particular articles or materials
- B65D2585/68—Containers, packaging elements or packages specially adapted for particular articles or materials for machines, engines, or vehicles in assembled or dismantled form
- B65D2585/86—Containers, packaging elements or packages specially adapted for particular articles or materials for machines, engines, or vehicles in assembled or dismantled form for electrical components
-
- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- 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
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
Landscapes
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Laminated Bodies (AREA)
- Physical Vapour Deposition (AREA)
Description
(処理後のAl含有量)/(処理前のAl含有量)×100 ≧75・・・(式1)
(処理後のAl含有量)/(処理前のAl含有量)×100 ≧75・・・(式1)
好ましくは、(処理後のAl含有量)/(処理前のAl含有量)×100 ≧80である。
また、各粒子の大きさは、蒸着時の圧力が変化しないように適当な大きさにする必要がある。粒径の好ましい範囲は、直径3mm以上20mm以下であることが好ましく、さらに好ましくは3mm以上10mm以下である。粒子径が大きすぎると、熱を加えられてから蒸発までに時間がかかるために、圧力の変動が大きくなり、小さすぎると突沸を起こして粒子がフィルムに付着し、外観品位の低下や、膜に欠陥が発生する原因となる。
反応性ガスは、配管11を用いて真空チャンバー1内に導入される。配管の形状やガスの導入位置に関しては特に限定されないが、反応性ガス導入方向12に示された方向のように、蒸着材料が配置される坩堝9と基材が走行する冷却ドラム2との間に、ガスが供給されるように配置されることが反応性の観点から好ましい。また、配管11は蒸着材料が付着しない様に防着板13で覆われていることが好ましい。
1) 膜厚、およびAl、Si比の算出
蛍光X線分析装置(理学電気製システム3270)を用いて測定した。X線の発生はロジウム管球を用い、50kV、50mAで行い、Al2O3/SiO2の複合膜において組成比の異なるサンプルより作成した検量線を用いて定量化した。
2) 酸素透過率
作成したガスバリアフィルムの酸素透過率を酸素透過率測定装置(モダンコントロールズ社製OX−TRAN100)を用いて23℃、65%R.H.の条件で測定した。
4)光線透過率
ヘイズメーター(日本電色製ヘイズメーター NDH5000)を用いて全光線透過率を測定した。
5)酸耐性
1mol/Lに調製した塩酸水溶液に50mm×50mm角にカットしたサンプルを無機薄膜層が液面側に来るように浸漬させ、1時間静置した。その後、30分間蒸留水に浸漬させて水洗し、風乾した後に蛍光X線分析装置を用いてAlのピーク強度を測定し、浸漬前後でのAl含有率の変化を算出した。計算式は、(浸漬後のAl含有量)/(浸漬前のAl含有量)×100とした。
蒸着源として、7mm〜9mm程度の粒子状のAl(純度99.9%)と4mm〜7mm程度のSiO2(純度99.9%)を用いて、図1に示した真空蒸着装置で、12μm厚のPETフィルム(東洋紡(株):E5100)上に複合酸化薄膜の形成を行った。上記2種の蒸着材料は混合せずに、ハース内のAl2O3から成る空孔を有した坩堝にAlを投入して、周囲にSiO2を投入することで材料を区切った。加熱源として一台の電子銃を用い、AlとSiO2の各々を時分割で加熱した。電子ビームの出力は、0.7Aとし、AlとSiO2への加熱比(時間比)を40:60とし、フィルムの送り速度は200m/minで19.1nm厚の複合膜を作った。酸素ガスの流量は100sccmとし、蒸着時の圧力が9.4×10−2Paとした。また、蒸着時のフィルムを冷却する為のコーティングロールの温度を−10℃に調整して、本発明の積層体を得た。これらの成膜条件を表1に示す。
このようにして得られた積層体の膜厚およびAl、Si比率を蛍光X線分析装置で測定し、作製した積層体を用いて、ガスバリア性として酸素透過率を測定し、光学特性として光線透過率を測定した。また、酸耐性を評価した。
蒸着源として、7mm〜9mm程度の粒子状のAl(純度99.9%)と4mm〜7mm程度のSiO2(純度99.9%)を用いて、図1に示した真空蒸着装置で、12μm厚のPETフィルム(東洋紡(株):E5100)上に複合酸化薄膜の形成を行った。上記2種の蒸着材料は混合せずに、ハース内のAl2O3から成る空孔を有した坩堝にAlを投入して、周囲にSiO2を投入することで材料を区切った。加熱源として一台の電子銃を用い、AlとSiO2の各々を時分割で加熱した。電子ビームの出力は、0.6Aとし、AlとSiO2への加熱比(時間比)を49:51とし、フィルムの送り速度は100m/minで36.4nm厚の複合膜を作った。酸素ガスの流量は100sccmとし、蒸着時の圧力が6.5×10−2Paとした。また、蒸着時のフィルムを冷却する為のコーティングロールの温度を−10℃に調整して、本発明の積層体を得た。これらの成膜条件を表1に示す。
このようにして得られた積層体の膜厚およびAl、Si比率を蛍光X線分析装置で測定し、作製した積層体を用いて、ガスバリア性として酸素透過率を測定し、光学特性として光線透過率を測定した。また、酸耐性を評価した。
(比較例1)
蒸着源として、7mm〜9mm程度の粒子状のAl(純度99.9%)と4mm〜7mm程度のSiO2(純度99.9%)を用いて、図1に示した真空蒸着装置で、12μm厚のPETフィルム(東洋紡(株):E5100)上に複合酸化薄膜の形成を行った。上記2種の蒸着材料は混合せずに、ハース内のAl2O3から成る空孔を有した坩堝にAlを投入して、周囲にSiO2を投入することで材料を区切った。加熱源として一台の電子銃を用い、AlとSiO2の各々を時分割で加熱した。電子ビームの出力は、0.5Aとし、AlとSiO2への加熱比(時間比)を53:47とし、フィルムの送り速度は50m/minで54.5nm厚の複合膜を作った。酸素ガスの流量は150sccmとし、蒸着時の圧力が8.5×10−2Paとした。また、蒸着時のフィルムを冷却する為のコーティングロールの温度を−10℃に調整して、本発明の積層体を得た。これらの成膜条件を表1に示す。
このようにして得られた積層体の膜厚およびAl、Si比率を蛍光X線分析装置で測定し、作製した積層体を用いて、ガスバリア性として酸素透過率を測定し、光学特性として光線透過率を測定した。また、酸耐性を評価した。
(比較例2)
蒸着源として、7mm〜9mm程度の粒子状のAl(純度99.9%)と4mm〜7mm程度のSiO2(純度99.9%)を用いて、図1に示した真空蒸着装置で、12μm厚のPETフィルム(東洋紡(株):E5100)上に複合酸化薄膜の形成を行った。上記2種の蒸着材料は混合せずに、ハース内のAl2O3から成る空孔を有した坩堝にAlを投入して、周囲にSiO2を投入することで材料を区切った。加熱源として一台の電子銃を用い、AlとSiO2の各々を時分割で加熱した。電子ビームの出力は、0.4Aとし、AlとSiO2への加熱比(時間比)を60:40とし、フィルムの送り速度は200m/minで18.9nm厚の複合膜を作った。酸素ガスは導入しなかった。蒸着時のフィルムを冷却する為のコーティングロールの温度を−10℃に調整して、本発明の積層体を得た。これらの成膜条件を表1に示す。
このようにして得られた積層体の膜厚およびAl、Si比率を蛍光X線分析装置で測定し、作製した積層体を用いて、ガスバリア性として酸素透過率を測定し、光学特性として光線透過率を測定した。また、酸耐性を評価した。
2・・・冷却ドラム
3・・・巻出し部
4・・・巻取り部
5・・・ガイドロール
6・・・基材フィルム
7・・・無機薄膜層積層体
8・・・電子銃
9・・・ハース
10・・・真空ポンプ
11・・・反応性ガス導入配管
12・・・反応性ガス導入方向
13・・・防着板
Claims (2)
- 高分子基材の少なくとも一方の面に無機薄膜層を積層した積層体において、該無機薄膜層は、主としてAlとSiを含み、かつ濃度が1mol/Lの塩酸水溶液に1時間浸漬する処理を行った際の、処理前後の無機薄膜層中のAl含有量の比が以下の式1を満たすことを特徴とするガスバリア性積層体。
(処理後のAl含有量)/(処理前のAl含有量)×100 ≧75・・・(式1) - 該無機薄膜層が、AlとSiを含む複合酸化化合物からなる蒸着膜層であることを特徴とする、請求項1に記載のガスバリア性積層体。
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