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WO2018147137A1 - Film barrière aux gaz de dépôt d'aluminium en phase vapeur et film stratifié l'utilisant - Google Patents

Film barrière aux gaz de dépôt d'aluminium en phase vapeur et film stratifié l'utilisant Download PDF

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Publication number
WO2018147137A1
WO2018147137A1 PCT/JP2018/003152 JP2018003152W WO2018147137A1 WO 2018147137 A1 WO2018147137 A1 WO 2018147137A1 JP 2018003152 W JP2018003152 W JP 2018003152W WO 2018147137 A1 WO2018147137 A1 WO 2018147137A1
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WIPO (PCT)
Prior art keywords
film
gas barrier
aluminum
layer
vapor deposition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2018/003152
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English (en)
Japanese (ja)
Inventor
鈴木　孝司
貴宏 石井
俊樹 小林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toray Advanced Film Co Ltd
Original Assignee
Toray Advanced Film Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Toray Advanced Film Co Ltd filed Critical Toray Advanced Film Co Ltd
Priority to JP2018567382A priority Critical patent/JP7156592B2/ja
Priority to CN201880015709.5A priority patent/CN110382233B/zh
Priority to KR1020197025266A priority patent/KR102484868B1/ko
Publication of WO2018147137A1 publication Critical patent/WO2018147137A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C23C14/58—After-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • 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
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2518/00—Other type of polymers
    • B05D2518/10—Silicon-containing polymers
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/20—Inorganic coating
    • B32B2255/205—Metallic coating
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • B32B2307/7244—Oxygen barrier
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • B32B2307/7246—Water vapor barrier

Definitions

  • the present invention relates to a gas barrier aluminum deposited film having excellent oxygen and water vapor barrier properties and having laminate strength, flex resistance and tensile resistance.
  • Packaging materials using aluminum foil have light shielding properties and excellent gas barrier performance in addition to the design properties of metallic luster, so packaging materials such as packaging materials for retort foods, heat insulating materials for refrigerators, and housing It is used as an outer packaging material for vacuum heat insulating materials such as heat insulating panels.
  • the packaging material using aluminum foil has a problem that it is difficult to handle the aluminum foil because pinholes are easily generated, and the load on the incinerator is large due to residues after incineration.
  • an aluminum vapor deposited film using a physical vapor deposition method such as a vacuum vapor deposition method is used as a substitute for the aluminum foil on a thermoplastic film such as a polyester film.
  • a physical vapor deposition method such as a vacuum vapor deposition method
  • the aluminum vapor deposition film was not usable because it had insufficient gas barrier performance for boil and retort food applications, and further, the vapor deposited aluminum layer disappeared during boil and retort sterilization, and the gas barrier performance deteriorated significantly.
  • a gas barrier film for use in boil and retort foods, a gas barrier film is disclosed in which a vapor-deposited layer composed of an inorganic oxide or an inorganic nitride and a specific resin layer are laminated on at least one side of a plastic film.
  • a vapor-deposited layer composed of an inorganic oxide or an inorganic nitride and a specific resin layer are laminated on at least one side of a plastic film.
  • a base material (a), a metal vapor deposition layer (b), and a protective layer (c) are this order.
  • a protective layer (c) containing a specific dimer acid-based polyamide resin is disclosed (for example, see Patent Document 2).
  • the thermal conductivity of aluminum is about 200 W / m ⁇ K.
  • the thermal conductivity of polyethylene terephthalate, which is a typical packaging material, is about 0.14 W / m ⁇ K, and the thermal conductivity of air is about 0.
  • the heat insulation material laminated with aluminum foil generates a heat bridge in which heat travels through the aluminum foil part, and the heat insulation performance of the vacuum heat insulation material is greatly reduced because it is larger than 0.02 W / m ⁇ K. was there.
  • the film for a vacuum heat insulating material is required to have excellent gas barrier performance in order to prevent gas (air) from entering from the outside and maintain a vacuum state for a long period of time.
  • the fin portion around the vacuum heat insulating material (welded and sealed portion) has lower heat insulating performance than the portion containing the core material, and the fin portion is bent to maintain the overall heat insulating performance, Further, when the vacuum heat insulating material itself is used in a place having a complicated shape (for example, an arc shape or a right angle shape), it is deformed according to the shape of the storage space. From the above, the film for vacuum heat insulating material is also required not to deteriorate the gas barrier performance upon bending or deformation.
  • a vapor deposition layer composed of an inorganic oxide or an inorganic nitride, and a specific A vacuum heat insulating material in which a gas barrier film in which a resin layer is laminated is laminated has been developed (see, for example, Patent Document 3).
  • a film for vacuum heat insulating material in which two transparent barrier films are bonded together by extrusion lamination with a polyolefin resin has been proposed (see, for example, Patent Document 4).
  • the gas barrier film according to Patent Document 1 is a transparent gas barrier film and is not a substitute for aluminum foil.
  • the laminate according to Patent Document 2 did not have sufficient gas barrier performance.
  • the vacuum heat insulating material according to Patent Document 3 is a transparent gas barrier film, and heat is transmitted as infrared rays to heat among heat conduction, so that heat is conducted even in vacuum. Was not enough.
  • the film for a vacuum heat insulating material according to Patent Document 4 has a problem that a vapor deposition layer is deteriorated and gas barrier properties are lowered by heat of a polyolefin resin extruded onto a transparent barrier film.
  • An object of the present invention is to provide a gas barrier aluminum deposited film having excellent oxygen and water vapor barrier performance and having laminate strength, flex resistance and tensile resistance, and a laminated film using the same.
  • the present invention has the following configuration.
  • a vapor deposition layer whose composition changes continuously from an aluminum metal layer having a film thickness of 25 nm or more to an aluminum oxide layer having a film thickness of 5 nm or more is further formed.
  • a gas barrier resin layer is formed of a gas barrier composition obtained by polycondensation of a vinyl alcohol resin and an organosilicon compound having an alkoxy group, wherein a gas barrier resin layer of 0.1 to 4 ⁇ m is laminated. Porous aluminum film.
  • a gas barrier aluminum vapor-deposited film having excellent oxygen and water vapor barrier properties, laminate strength, flex resistance, and tensile resistance, and a laminated film using the same are obtained.
  • a vapor deposition layer whose composition changes continuously from an aluminum metal layer having a film thickness of 25 nm or more to an aluminum oxide layer having a film thickness of 5 nm or more is formed on at least one surface of the substrate film surface. Further, a gas barrier resin layer having a thickness of 0.1 to 4 ⁇ m is laminated thereon, and the gas barrier resin layer is formed from a gas barrier composition obtained by polycondensation of a vinyl alcohol resin and an organosilicon compound having an alkoxy group. It is characterized by becoming.
  • the gas barrier performance of the aluminum vapor deposition film according to the prior art is insufficient as compared with the aluminum foil, but the vapor deposition layer and the specific gas barrier resin continuously change in composition from the aluminum metal layer to the aluminum oxide layer.
  • the aluminum oxide vapor deposition layer exhibits the effect of an adhesion strengthening layer between the vapor deposition layer and the gas barrier resin layer, and the resin constituting the gas barrier resin layer Exerts its inherent gas barrier performance.
  • Base film As a base film in the gas barrier aluminum vapor deposition film of the present invention, as long as characteristics such as chemical resistance, mechanical strength (film stiffness, external wear, puncture strength), heat resistance, weather resistance and the like are considered depending on the application. Although not particularly limited, for example, a polyethylene terephthalate film, a polypropylene film, a nylon film, or the like is used. A polyethylene terephthalate film is preferably practical.
  • the base film may be an unstretched film, but a stretched film (uniaxial or biaxial) is excellent in mechanical properties and thickness uniformity, and a biaxially stretched film is more preferable.
  • a conventional stretching method such as roll stretching, roll stretching, belt stretching, tenter stretching, tube stretching, or a combination of these can be applied.
  • the thickness of the base film is not particularly limited, but about 6 ⁇ m to 30 ⁇ m for a polyethylene terephthalate film, about 20 ⁇ m to 40 ⁇ m for a polypropylene film, and about 10 ⁇ m to 30 ⁇ m for a nylon film are practical.
  • the vapor deposition layer which changes a composition continuously from an aluminum metal layer to an aluminum oxide layer is formed on the said base film.
  • the vapor deposition layer whose composition changes continuously from the aluminum metal layer to the aluminum oxide layer is a vapor deposition layer having an inclined structure in which an aluminum metal layer is formed at the initial stage of vapor deposition and changes into aluminum oxide as the film grows.
  • a thin natural oxide film is formed on the surface of the aluminum metal film when it is taken out to the atmosphere after vapor deposition. This natural oxide film is about 3 nm at most, and the aluminum oxide layer in the present invention is described later.
  • the thickness is preferably 10 to 25 nm. If it exceeds 25 nm, the metallic appearance of the aluminum metal layer may be impaired, and the infrared reflectance may be lowered.
  • the film thickness of the aluminum metal layer is 25 nm or more. If it is less than 25 nm, the gas barrier performance is insufficient, and the metallic appearance may be insufficient. Moreover, in a vacuum heat insulating material use, an infrared reflectance may be less than 60% and a heat insulation performance may become inadequate. Preferably, it is 40 to 125 nm. Even when the thickness exceeds 125 nm, the gas barrier performance reaches a peak, the cohesive energy during aluminum metal layer deposition increases, the base film is deformed by heat, and the appearance may not be practical.
  • the total thickness of the deposited layer whose composition changes continuously from the aluminum metal layer to the aluminum oxide layer is preferably 30 to 150 nm.
  • the film thickness is less than 30 nm, it becomes difficult to express the target oxygen barrier performance and water vapor barrier performance.
  • the thickness is 150 nm or more, the cohesive force of the vapor deposition layer decreases, peeling occurs due to cohesive failure in the vapor deposition layer, and the apparent laminate strength decreases.
  • the cohesive energy at the time of vapor deposition becomes large, the base film may be deformed by heat, and the appearance may be unpractical.
  • the method for producing a vapor deposition layer whose composition changes continuously from the aluminum metal layer to the aluminum oxide layer is preferably a method in which a vapor deposition layer whose composition changes continuously from the aluminum metal layer to the aluminum oxide layer is formed in a vacuum chamber.
  • the method for vapor deposition may be performed by a known method such as vapor deposition or sputtering, but the method by vapor deposition is preferable from the viewpoint of productivity, and for that purpose, heating and evaporation of aluminum are also performed by resistance heating, high-frequency heating, electron beam heating, and the like. Is applicable. In these vapor deposition methods, it is preferable to form a vapor deposition layer whose composition changes continuously from an aluminum metal layer to an aluminum oxide layer by reactive vapor deposition.
  • the base film is generally long and is supplied in a roll shape, unwound from the roll in a vacuum chamber and vapor deposited and then wound up again in a roll shape.
  • An aluminum metal layer is formed, oxygen is introduced into the latter half of the vapor deposition, and aluminum oxide is formed by the reaction between the metal aluminum and oxygen.
  • Oxygen introduced in the latter half of the vapor deposition diffuses from the winding side to the unwinding side of the base film, so that the metal aluminum layer and the aluminum oxide layer are not strictly separated and formed.
  • the reaction of oxygen continuously proceeds from the aluminum metal layer to the aluminum oxide layer, and an inclined structure in which the composition continuously changes in the film thickness direction is formed.
  • the gas barrier resin layer is formed by applying a gas barrier resin obtained by polycondensation of a vinyl alcohol resin and an organosilicon compound having an alkoxy group.
  • a gas barrier resin obtained by polycondensation of a vinyl alcohol resin and an organosilicon compound having an alkoxy group.
  • the aluminum vapor deposition layer which is a base layer can be protected and gas barrier property can be improved. That is, a vapor deposition layer made of aluminum metal and aluminum oxide may cause defects such as pinholes, cracks, and grain boundaries, which may deteriorate the gas barrier properties, and the gas barrier resin layer is a defect of the vapor deposition layer.
  • the gas barrier performance itself can be enhanced.
  • a specific method for forming the gas barrier resin layer is based on a vinyl alcohol resin having a high affinity for the vapor deposition layer, an aqueous solution containing either an organosilicon compound having an alkoxy group and a hydrolyzate thereof, or It is formed from an alcohol-mixed aqueous solution.
  • the vinyl alcohol resin as the main agent for forming the gas barrier resin layer is not particularly limited as long as it is a vinyl alcohol resin such as polyvinyl alcohol, ethylene / vinyl alcohol copolymer, and modified polyvinyl alcohol. Among them, particularly when polyvinyl alcohol is used for the coating material of the present invention, it is more preferable because of its excellent gas barrier properties.
  • Polyvinyl alcohol as used herein is generally obtained by saponifying polyvinyl acetate, and may be partial saponification obtained by saponifying a part of the acetate group or complete saponification, and is not particularly limited. .
  • An organic silicon compound having an alkoxy group is further added to the coating material for forming the gas barrier resin layer.
  • An alkoxy group has a structure of RO— in which an alkyl group R is bonded to oxygen, and is converted to a silanol group through a dealcoholization reaction by hydrolysis.
  • Typical examples include a methoxy group and an ethoxy group. It is.
  • silicon compound having an alkoxy group examples include tetramethoxysilane, tetraethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxylane, dimethyldiethoxysilane, n-propyltrimethoxysilane, n- Examples thereof include propyltriethoxysilane, hexyltrimethoxysilane, and hexyltriethoxysilane. Among them, tetraethoxysilane is preferable because it is relatively stable in an aqueous solvent after hydrolysis.
  • the range of 40/60 to 60/40 is more preferable.
  • the mass ratio converted to SiO 2 is a value converted from the number of moles of silicon atoms in the organosilicon compound to SiO 2 mass, and is represented by vinyl alcohol resin / organosilicon compound (mass ratio). When this value exceeds 85/15, the vinyl alcohol resin cannot be fixed, and the gas barrier performance may be deteriorated. On the other hand, if it is less than 15/85, the ratio of the organosilicon compound is increased and the gas barrier resin layer is hardened, so that the bending resistance and the tensile performance may be lowered.
  • the gas barrier resin layer is formed by using a coating material comprising an aqueous solution or an alcohol mixed aqueous solution containing at least one of the above vinyl alcohol resin, one or more organosilicon compounds having an alkoxy group and a hydrolyzate thereof. Is done.
  • a coating material comprising an aqueous solution or an alcohol mixed aqueous solution containing at least one of the above vinyl alcohol resin, one or more organosilicon compounds having an alkoxy group and a hydrolyzate thereof.
  • a resin composition comprising a vinyl alcohol resin and an organosilicon compound having an alkoxy group
  • an inorganic structure having a siloxane bond as a skeleton formed by polycondensation between organosilicon compounds and a hydrogen atom at each hydroxyl group of the vinyl alcohol resin By forming a resin composition comprising a vinyl alcohol resin and an organosilicon compound having an alkoxy group, an inorganic structure having a siloxane bond as a skeleton formed by polycondensation between organosilicon compounds and a hydrogen atom at each hydroxyl group of the vinyl alcohol resin.
  • a so-called organic-inorganic hybrid structure having a Si—O— covalent bond via oxygen is formed by dehydration reaction. In such a structure, the molecular chain is more restrained than a single vinyl alcohol resin, and water vapor barrier performance can be exhibited.
  • gas barrier resin layer there is no restriction
  • printing methods such as offset printing method, gravure printing method, silk screen printing method, roll coating method, dip coating method, bar coating method, die coating method, knife edge coating method, gravure coating method, kiss coating method, spin coating method
  • the coating liquid may be coated using a method such as a combination of these.
  • the film thickness of the gas barrier resin layer provided on the vapor deposition layer whose composition changes continuously from the aluminum metal layer to the aluminum oxide layer needs to be 0.1 to 4 ⁇ m, more preferably 0.2 to 1 ⁇ m.
  • the thickness of the gas barrier resin layer is 0.1 ⁇ m or less, gas barrier performance may not be exhibited.
  • the film thickness of the gas barrier resin layer exceeds 4 ⁇ m, the cohesive force of the gas barrier resin layer decreases, peeling occurs due to cohesive failure in the gas barrier resin layer, and the apparent laminate strength decreases.
  • the coating drying conditions require a high temperature for a long time, and the manufacturing cost increases.
  • the laminated film prepared using the gas barrier aluminum deposited film of the present invention is formed by laminating a sealant film as a heat-fusible layer, a gas barrier film, and a plastic film as a surface protective layer in this order.
  • the sealant film is not particularly limited as long as it takes into consideration the chemical resistance, mechanical strength (film stiffness, external wear, puncture strength), heat resistance, weather resistance, etc. depending on the application, but polypropylene film, polyethylene film Etc. are used. A polyethylene film is preferable for practical use, and a linear low density polyethylene film is particularly preferable.
  • the gas barrier aluminum vapor deposition film which is a gas barrier film, may have a vapor deposition surface on the plastic film side or a sealant film side, and is selected according to the design.
  • the gas barrier film may be a laminate of a plurality of gas barrier aluminum vapor deposition films as necessary.
  • the vapor deposition surfaces may be bonded together, or the substrate film surfaces may be bonded together.
  • the vapor deposition surface and the substrate film surface may be bonded together.
  • a laminate film of the present invention is constituted by laminating a sealant film on one side of the laminate and a plastic film on the other side.
  • the plastic film is not particularly limited as long as it considers properties such as chemical resistance, mechanical strength (film stiffness, external wear, puncture strength), heat resistance, and weather resistance depending on the application.
  • polyethylene terephthalate film, Polypropylene film, nylon film, etc. are used.
  • an unstretched film may be used, a stretched film (uniaxial or biaxial) is excellent in mechanical properties and thickness uniformity, and a biaxially stretched film is more preferable.
  • the thickness is not particularly limited, but a polyethylene terephthalate film is about 6 ⁇ m to 30 ⁇ m, a polypropylene film is about 20 ⁇ m to 40 ⁇ m, and a nylon film is about 10 ⁇ m to 30 ⁇ m.
  • a laminate of a plurality of these plastic films as required may be used as the surface protective layer.
  • a method for producing a laminated film produced using the gas barrier aluminum deposited film of the present invention can employ a dry laminating method or an extrusion laminating method using a two-component curable urethane adhesive, but is particularly limited. It is not a thing.
  • Adhesion strength between the vapor deposition layer and the gas barrier resin layer (N / 15 mm) A 40 ⁇ m film thickness as a sealant film is formed on the vapor-deposited surface of the gas barrier film through an adhesive composed of a polyester urethane main agent (manufactured by DIC Corporation, LX500) and an aromatic isocyanate curing agent (manufactured by DIC Corporation, KW75).
  • the linear low density polyethylene film was laminated by a dry laminating method to produce a laminated film.
  • the laminated film is cut into a width of 15 mm and a length of 150 mm to prepare a cut sample, and a T-peel method using a tensile tester (Tensilon) as an interface between the gas barrier film and the linear low-density polyethylene film.
  • the peel strength (laminate strength) was measured at a pulling speed of 50 mm / min, and the adhesion strength between the vapor deposition layer and the gas barrier resin layer was evaluated.
  • the adhesion strength value was determined to be 3.0 N / 15 mm or more.
  • Oxygen permeability (cc / m 2 ⁇ 24 hr ⁇ atm) Based on the isobaric method described in JIS K7126-2: 2006, a gas barrier film was used under the conditions of a temperature of 23 ° C. and a humidity of 0% RH using an oxygen transmission meter (OXTRAN 2/20) manufactured by MOCON, USA. The oxygen transmission rate was measured. The value of oxygen permeability was 0.1 cc / m 2 ⁇ 24 hr ⁇ atm or less.
  • Infrared reflectance (%) The gas barrier film is reflected in the wavelength range of 240 nm to 2600 nm including the infrared wavelength region with an infrared spectrophotometer (Hitachi High-Technologies Corporation, U-4000) at a relative reflection angle of 12 degrees of the reflection device. The light intensity was measured. Among these, with respect to the reflected light intensity at three points of wavelengths 1500 nm, 2000 nm, and 2500 nm, the ratio of the reflected light intensity of the gas barrier film to the reflected light intensity of the aluminum vapor deposition flat mirror used as a reference is infrared reflectance (%). The average value of the points was calculated. This value means that the closer to 100%, the better the reflection characteristics, and the value of infrared reflectance is 60% or more.
  • the gas barrier film is linearly low with a film thickness of 40 ⁇ m as a sealant film through an adhesive composed of a polyester urethane base agent (LX500 manufactured by DIC Corporation) and an aromatic isocyanate curing agent (KW75 manufactured by DIC Corporation).
  • Density polyethylene film Tiix FC-S manufactured by Mitsui Chemicals Tosero Co., Ltd.
  • biaxially stretched nylon film OMM manufactured by Unitika Co., Ltd.
  • a laminated film was produced by laminating by a dry laminating method so as to be on the plastic film side.
  • the puncture strength of the laminated film was measured based on the method described in JIS Z1707-1997 by using a 50 mm ⁇ 50 mm sample piece and using a tensile tester (Tensilon).
  • Deposition film thickness measurement Depth direction composition analysis evaluation is performed with a scanning Auger electron spectrometer (SAM-670 model manufactured by ULVAC-PHI), and the film configuration of aluminum oxide / metal aluminum is confirmed by the depth profile. did. Focusing on the Al concentration and O concentration, collecting data while performing Ar ion etching from the surface layer of the deposited film, and when the concentration ratio of the Al concentration and O concentration is 50:50 is defined as the interface The film thicknesses of the aluminum oxide vapor deposition layer and the aluminum vapor deposition layer were calculated.
  • SAM-670 model manufactured by ULVAC-PHI scanning Auger electron spectrometer
  • a metal aluminum film whose thickness is known by cross-sectional observation with a transmission electron microscope is etched by the same etching method, and the etching time is converted into the absolute value of the etching depth by calculating the etching rate. did.
  • Example 1 A 12 ⁇ m-thick biaxially stretched polyethylene terephthalate film (“Lumirror” (registered trademark) P60, manufactured by Toray Industries, Inc.) is used as the base film, and high-frequency induction heating crucible type aluminum using a roll-to-roll vacuum deposition machine Using an evaporation source, the film was continuously formed so that the aluminum metal layer thickness was 40 nm and the aluminum oxide layer thickness was 10 nm. On the base film, a film having a composition corresponding to the position is sequentially formed in the thickness direction in a zone having a constant width in the base film traveling direction on the cooled rotating drum. By supplying oxygen from the position where vapor deposition is finally received, a vapor deposition layer that continuously changes from an aluminum metal layer to an aluminum oxide layer was formed.
  • Limirror registered trademark
  • P60 manufactured by Toray Industries, Inc.
  • an aqueous solution having the following composition was applied and dried by a gravure coating method to form a gas barrier resin layer having a film thickness of 0.3 ⁇ m, thereby producing a gas barrier aluminum vapor deposition film.
  • the mixing ratio (% by weight) with (A liquid) / (B liquid) having the following composition was 35/65.
  • Liquid A Hydrochloric acid (0.1N) was added to tetraethoxysilane (TEOS) and hydrolyzed by stirring for 120 minutes to prepare liquid A (solid content 30 wt%: converted to SiO 2 ).
  • Liquid B A 10% by weight aqueous solution of polyvinyl alcohol (PVA, polymerization degree 1,700, saponification degree 98.5%) and methyl alcohol were mixed at 35/65 (weight ratio) and stirred, liquid B Adjusted.
  • PVA polyvinyl alcohol
  • Example 2 A gas barrier aluminum deposited film was obtained in the same manner as in Example 1 except that the deposited layer had an aluminum metal layer thickness of 25 nm and an aluminum oxide layer thickness of 5 nm.
  • Example 3 A gas barrier aluminum deposited film was obtained in the same manner as in Example 1 except that the deposited layer had an aluminum metal layer thickness of 80 nm and an aluminum oxide layer thickness of 20 nm.
  • Example 4 A gas barrier aluminum deposited film was obtained in the same manner as in Example 1 except that the thickness of the gas barrier resin layer was 0.1 ⁇ m.
  • Example 1 A gas barrier aluminum deposited film was obtained in the same manner as in Example 1 except that the film thickness was 50 nm with only the aluminum metal layer without supplying oxygen to the deposited layer.
  • Example 2 A gas barrier aluminum vapor deposition film was obtained in the same manner as in Example 1 except that metal aluminum was evaporated while supplying oxygen gas to the entire surface of the vapor deposition layer, and the film thickness was 10 nm only with the aluminum oxide layer.
  • Example 3 A gas barrier aluminum deposited film was obtained in the same manner as in Example 1 except that the thickness of the gas barrier resin layer was 5 ⁇ m.
  • Example 4 A gas barrier aluminum deposited film was obtained in the same manner as in Example 1 except that the thickness of the gas barrier resin layer was 0.05 ⁇ m.
  • Example 5 A gas barrier aluminum deposited film was obtained in the same manner as in Example 1 except that an aqueous solution having the following composition was applied by a gravure coating method and dried to form a gas barrier resin layer having a film thickness of 0.3 ⁇ m.
  • the mixing ratio (% by weight) with (A liquid) / (B liquid) having the following composition was 20/80.
  • liquid B Xylylene diisocyanate and methyl ethyl ketone were blended at 10/90 and stirred to prepare liquid B.
  • Table 1 shows the composition and characteristics of the films prepared in Examples and Comparative Examples.
  • the gas barrier film is an aluminum foil having a thickness of 6 ⁇ m, and a linear low density polyethylene film having a thickness of 40 ⁇ m is used as a sealant film as in Example 1, and a biaxially stretched nylon film having a thickness of 15 ⁇ m is used as a plastic film by a dry laminating method. It laminated
  • the gas barrier aluminum deposited film of the present invention is excellent in oxygen barrier performance and water vapor barrier performance, and can maintain these gas barrier performance against tension and bending. there were.
  • Comparative Example 1 has inferior laminate strength due to low adhesion between the aluminum layer and the gas barrier resin layer
  • Comparative Example 2 has inferior infrared reflectance because there is no aluminum layer
  • Comparative Example 3 has a thick gas barrier resin layer. Peeling occurred due to cohesive failure in the gas barrier resin layer, resulting in low adhesion strength between the vapor deposition layer and the gas barrier resin layer.
  • the gas barrier resin layer is thin and the barrier property is poor
  • the gas barrier resin layer is not an organosilicon compound having a vinyl alcohol resin and an alkoxy group. Performance and water vapor barrier properties decreased.
  • the gas barrier aluminum deposited film of the present invention has excellent oxygen barrier performance and water vapor barrier performance, and is therefore useful as a vacuum heat insulating material exterior material that requires high gas barrier properties.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Laminated Bodies (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

Le but de la présente invention est de fournir un film barrière aux gaz de dépôt d'aluminium en phase vapeur qui est caractérisé en ce qu'il est produit en formant une couche de dépôt en phase vapeur sur au moins une surface de la surface de film de matériau de base, la composition de la couche de dépôt en phase vapeur changeant continuellement d'une couche métallique d'aluminium ayant une épaisseur de film supérieure ou égale à 25 nm à une couche d'oxyde d'aluminium ayant une épaisseur de film supérieure ou égale à 5 nm, et en stratifiant en outre cette dernière sur une couche de résine barrière aux gaz ayant une épaisseur de film de 0,1 à 4 µm ; la couche de résine barrière aux gaz étant constituée d'une composition barrière aux gaz obtenue par polycondensation d'une résine à base d'alcool de vinyle et d'un composé de silicium organique ayant un groupe alcoxy. L'invention concerne : un film barrière aux gaz de dépôt d'aluminium en phase vapeur qui présente d'excellentes propriétés de barrière à l'oxygène et à la vapeur d'eau, une solidité de stratification, une résistance à la flexion et une résistance à la traction ; un film stratifié l'utilisant.
PCT/JP2018/003152 2017-02-07 2018-01-31 Film barrière aux gaz de dépôt d'aluminium en phase vapeur et film stratifié l'utilisant Ceased WO2018147137A1 (fr)

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CN201880015709.5A CN110382233B (zh) 2017-02-07 2018-01-31 气体阻隔性铝蒸镀膜及使用其的层叠膜
KR1020197025266A KR102484868B1 (ko) 2017-02-07 2018-01-31 가스 배리어성 알루미늄 증착 필름 및 그것을 사용한 적층 필름

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JP2020049736A (ja) * 2018-09-26 2020-04-02 東レ株式会社 積層体およびそれを用いた封止部材
WO2020241621A1 (fr) * 2019-05-31 2020-12-03 東洋紡株式会社 Film barrière contre les gaz transparent et son procédé de production
JP2020198290A (ja) * 2019-05-31 2020-12-10 寧徳時代新能源科技股▲分▼有限公司Ｃｏｎｔｅｍｐｏｒａｒｙ Ａｍｐｅｒｅｘ Ｔｅｃｈｎｏｌｏｇｙ Ｃｏ．， Ｌｉｍｉｔｅｄ リチウムイオン二次電池、セル及び負極シート
JPWO2020122065A1 (ja) * 2018-12-11 2021-10-28 凸版印刷株式会社 真空断熱材用積層体およびそれを用いた真空断熱材
US20220298623A1 (en) * 2018-10-30 2022-09-22 Fres-Co System Usa, Inc. Methods of making films and laminates with high oxygen barrier
US11646424B2 (en) 2019-05-31 2023-05-09 Contemporary Amperex Technology Co., Limited Lithium-ion secondary battery
JP2023092795A (ja) * 2021-12-22 2023-07-04 株式会社クラレ 繊維製品の保管方法
US12319035B2 (en) 2022-02-14 2025-06-03 Toppan Holdings Inc. Laminated film and packaging bag

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KR102305248B1 (ko) * 2020-02-12 2021-09-24 도레이첨단소재 주식회사 가스 배리어 알루미늄 증착필름 및 그의 제조방법

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JP7273475B2 (ja) 2018-09-26 2023-05-15 東レフィルム加工株式会社 積層体およびそれを用いた封止部材
JP2020049736A (ja) * 2018-09-26 2020-04-02 東レ株式会社 積層体およびそれを用いた封止部材
US20220298623A1 (en) * 2018-10-30 2022-09-22 Fres-Co System Usa, Inc. Methods of making films and laminates with high oxygen barrier
JP7660019B2 (ja) 2018-12-11 2025-04-10 Ｔｏｐｐａｎホールディングス株式会社 バリアフィルム
JPWO2020122065A1 (ja) * 2018-12-11 2021-10-28 凸版印刷株式会社 真空断熱材用積層体およびそれを用いた真空断熱材
JP2021183416A (ja) * 2018-12-11 2021-12-02 凸版印刷株式会社 バリアフィルム
US11611081B2 (en) 2019-05-31 2023-03-21 Contemporary Amperex Technology Co., Limited Lithium ion secondary battery, battery core, negative electrode plate, and apparatus
CN113874543A (zh) * 2019-05-31 2021-12-31 东洋纺株式会社 透明阻气薄膜和其制造方法
JP2020198290A (ja) * 2019-05-31 2020-12-10 寧徳時代新能源科技股▲分▼有限公司Ｃｏｎｔｅｍｐｏｒａｒｙ Ａｍｐｅｒｅｘ Ｔｅｃｈｎｏｌｏｇｙ Ｃｏ．， Ｌｉｍｉｔｅｄ リチウムイオン二次電池、セル及び負極シート
US11646424B2 (en) 2019-05-31 2023-05-09 Contemporary Amperex Technology Co., Limited Lithium-ion secondary battery
JP7271390B2 (ja) 2019-05-31 2023-05-11 寧徳時代新能源科技股▲分▼有限公司 リチウムイオン二次電池、セル及び負極シート
JPWO2020241621A1 (fr) * 2019-05-31 2020-12-03
JP7472905B2 (ja) 2019-05-31 2024-04-23 東洋紡株式会社 透明ガスガリアフィルム及びその製造方法
TWI856106B (zh) * 2019-05-31 2024-09-21 日商東洋紡股份有限公司 透明阻氣性薄膜及其製造方法
WO2020241621A1 (fr) * 2019-05-31 2020-12-03 東洋紡株式会社 Film barrière contre les gaz transparent et son procédé de production
JP2023092795A (ja) * 2021-12-22 2023-07-04 株式会社クラレ 繊維製品の保管方法
US12319035B2 (en) 2022-02-14 2025-06-03 Toppan Holdings Inc. Laminated film and packaging bag

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KR20190116340A (ko) 2019-10-14
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