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WO2015198701A1 - Procédé de fabrication de film fonctionnel - Google Patents

Procédé de fabrication de film fonctionnel Download PDF

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Publication number
WO2015198701A1
WO2015198701A1 PCT/JP2015/062137 JP2015062137W WO2015198701A1 WO 2015198701 A1 WO2015198701 A1 WO 2015198701A1 JP 2015062137 W JP2015062137 W JP 2015062137W WO 2015198701 A1 WO2015198701 A1 WO 2015198701A1
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WO
WIPO (PCT)
Prior art keywords
film
inorganic layer
layer
substrate
inorganic
Prior art date
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Ceased
Application number
PCT/JP2015/062137
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English (en)
Japanese (ja)
Inventor
望月　佳彦
藤縄　淳
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Fujifilm Corp
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Fujifilm Corp
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Filing date
Publication date
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Priority to JP2016529138A priority Critical patent/JPWO2015198701A1/ja
Publication of WO2015198701A1 publication Critical patent/WO2015198701A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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

Definitions

  • the present invention relates to a method for producing a functional film having an inorganic layer.
  • Gas barrier films such as optical elements, display devices such as liquid crystal displays and organic EL displays, various semiconductor devices, parts and components that require moisture resistance in various devices such as solar cells, and packaging materials for packaging food and electronic components
  • the gas barrier film generally has a configuration in which a plastic film such as a polyethylene terephthalate (PET) film is used as a support and a gas barrier layer that exhibits gas barrier properties is formed thereon.
  • PET polyethylene terephthalate
  • the layer which consists of various inorganic compounds, such as a silicon nitride, silicon oxide, aluminum oxide is known, for example.
  • a vacuum film forming method such as sputtering or plasma CVD (chemical vapor deposition) is used.
  • the support has a laminated structure in which an organic layer made of an organic compound and an inorganic layer made of an inorganic compound are alternately laminated.
  • Organic / inorganic laminated gas barrier films (hereinafter also referred to as laminated gas barrier films) are known.
  • laminated gas barrier films an inorganic layer is formed on an organic layer serving as a base, whereby the formation surface of the inorganic layer is smoothed by the organic layer, and the inorganic layer is formed on the organic layer having good smoothness. Form.
  • the uniform inorganic layer without a crack, a crack, etc. is formed, and the outstanding gas barrier performance is acquired.
  • more excellent gas barrier performance can be obtained by repeatedly including a plurality of laminated structures of the organic layer and the inorganic layer.
  • this substrate is sent out from a substrate roll formed by winding a long substrate into a roll shape and conveyed in the longitudinal direction.
  • An apparatus for forming a film by so-called roll-to-roll (hereinafter also referred to as RtoR) is known, in which an inorganic layer is formed while the formed substrate is wound into a roll.
  • RtoR roll-to-roll
  • an organic layer and an inorganic layer are continuously formed while transporting a long substrate. Therefore, a gas barrier film can be produced with very high productivity.
  • an inorganic layer formed on the surface of the substrate due to conveyance by a pair of conveyance rollers, contact with other members, etc. after forming the inorganic layer on the surface of the substrate If the film is damaged, there is a possibility that a functional film having the intended performance cannot be manufactured.
  • the inorganic layer formed on the substrate and the back surface of the substrate are in sliding contact with each other when the substrate is wound after the inorganic layer is formed.
  • a protective film is attached to the surface of the inorganic layer to protect the inorganic layer. That is, after film formation of the inorganic layer, a protective film is attached to the surface of the inorganic layer, and the substrate is transported to the site where the next treatment is performed with the substrate and protective film having the inorganic layer formed on the surface.
  • the substrate with the protective film attached is wound up into a roll once and loaded into a substrate processing apparatus such as a film forming apparatus or a surface processing apparatus for performing the next processing and immediately before performing the next processing.
  • the protective film is peeled off and the substrate surface is treated.
  • Patent Document 1 when a laminated gas barrier film is manufactured by RtoR, an inorganic layer on the surface is prevented from being damaged by contact with a guide roller or the like after the formation of the inorganic layer. It describes that a protective film is stuck on the surface of an inorganic layer immediately after forming a film, and this protective film is peeled off immediately before forming an organic layer to protect the inorganic layer.
  • a peelable protective film is attached to the inorganic layer. It is possible to provide.
  • the gas barrier film when used for a top emission type organic EL device, the gas barrier film is laminated on the passivation film having a gas barrier property covering the organic EL material as the light emitting element by using an adhesive. By doing so, deterioration of the organic EL material can be suitably prevented.
  • a material for forming the passivation film inorganic materials such as silicon nitride, silicon oxide, and silicon oxynitride that exhibit gas barrier properties are used. Therefore, from the viewpoint of adhesiveness, in a gas barrier film used for an organic EL device or the like, the inorganic layer and the passivation film are opposed to each other with the uppermost layer being an inorganic layer, and the inorganic materials are laminated via an adhesive.
  • the outermost layer of the gas barrier film is an inorganic layer, the inorganic layer is easily damaged, and the target barrier performance may not be obtained. Therefore, when supplying such a gas barrier film, in order to prevent damage to the inorganic layer, it is necessary to supply the protective film on the outermost inorganic layer.
  • the adhesion between the inorganic layer and the layer formed on the inorganic layer is reduced when another layer such as an organic layer or an adhesive layer is formed on the inorganic layer after the protective film on the inorganic layer is peeled off.
  • another layer such as an organic layer or an adhesive layer is formed on the inorganic layer after the protective film on the inorganic layer is peeled off.
  • the components of the protective film remain on the surface of the inorganic layer after the protective film is peeled off, and are formed on the inorganic layer and the inorganic layer due to the presence of the transferred component. It was found that the adhesion with the layer was inhibited. Further, it has been found that such a problem occurs when a denser inorganic layer is formed by plasma CVD, or when the conveyance speed is improved to improve manufacturing efficiency.
  • a general protective film is designed so that it can be easily peeled off by adhering with an intermolecular force acting between the adhesive layer of the protective film and the counterpart member.
  • a dense inorganic layer is formed in a vacuum by plasma CVD that can form a dense inorganic layer, and a protective film is applied immediately after that, It was found that the components of the protective film were transferred to the surface of the inorganic layer after peeling off the protective film.
  • the surface activity of the inorganic layer is very high, and there are many unbonded hands, so it is chemically bonded to the components of the protective film. It is estimated that the phenomenon will occur.
  • An object of the present invention is to solve such problems of the prior art, and it is possible to prevent a decrease in adhesion between the inorganic layer after the protective film is peeled off and the layer formed on the inorganic layer. It is providing the manufacturing method of a functional film.
  • the present inventor has obtained a substrate preparation step of preparing a substrate having a surface made of an organic material, and a carbon composition ratio of 5% on the substrate by plasma CVD in a vacuum.
  • a film forming step for forming the following inorganic layer, an inactivation step for deactivating the dangling bonds of the formed inorganic layer, and a protective film made of a plastic film after the deactivation step on the inorganic layer In addition, it has been found that by having a sticking step for sticking in a peelable manner, it is possible to prevent a decrease in adhesion between the inorganic layer after peeling the protective film and the layer formed on the inorganic layer, The present invention has been completed. That is, this invention provides the manufacturing method of the functional film of the following structures.
  • a substrate preparation step of preparing a substrate having a surface made of an organic material A film forming step of forming an inorganic layer having a carbon composition ratio of 5% or less on the substrate by plasma CVD in vacuum; An inactivation step for inactivating dangling bonds of the deposited inorganic layer;
  • the manufacturing method of a functional film which has the sticking process of sticking the protective film which consists of a plastic film on an inorganic layer so that peeling is possible after an inactivation process.
  • the substrate preparation step prepares a substrate roll formed by winding a long substrate, The function according to any one of (1) to (6), wherein a long substrate is fed from a substrate roll and conveyed in the longitudinal direction of the substrate while performing a film forming step, an inactivation step, and a pasting step For producing a conductive film.
  • the manufacturing method of the functional film which can prevent the fall of the adhesiveness of the inorganic layer after peeling a protective film and the layer formed on this inorganic layer can be provided. .
  • FIG. 1 (A) is a film-forming apparatus of an inorganic layer
  • FIG.1 (B) is film-forming of an organic layer.
  • Device It is a figure which shows notionally an example of the stepped roller of the film-forming apparatus shown to FIG. 1 (A).
  • FIG. 4 (A) to 4 (C) are cross-sectional views showing an enlarged part of the functional film for explaining the method for producing the functional film of the present invention.
  • FIG. 5A to FIG. 5C are cross-sectional views showing an enlarged part of the functional film for explaining the method for producing the functional film of the present invention.
  • the production method of the present invention includes: A substrate preparation step of preparing a substrate having a surface made of an organic material; A film forming process for forming an inorganic layer having a carbon composition ratio of 5% or less on a substrate by plasma CVD in a vacuum; An inactivation step of inactivating dangling bonds of the deposited inorganic layer, and After the inactivation step, there is a sticking step of sticking a protective film made of a plastic film on the inorganic layer in a peelable manner.
  • the production method of the present invention has, as a preferred aspect, After the sticking step, a peeling step for peeling the protective film, An organic layer forming step of forming an organic layer on the surface of the inorganic layer on the side where the protective film is peeled off.
  • a peeling step for peeling the protective film An organic layer forming step of forming an organic layer on the surface of the inorganic layer on the side where the protective film is peeled off.
  • FIG. 1 (A) and FIG. 1 (B) are diagrams conceptually showing an example of a production apparatus for carrying out the functional film production method of the present invention.
  • 4 (A) to 4 (C) and FIGS. 5 (A) to 5 (C) are enlarged views of a part of the functional film for explaining the method for producing the functional film of the present invention.
  • FIG. In the following description, an example in which the method for producing a functional film is used for the method for producing a gas barrier film will be described.
  • the manufacturing method of the functional film of this invention is not limited to the manufacturing method of a gas barrier film. That is, this invention can be utilized as a manufacturing method of well-known functional films, such as various optical films, such as a filter which permeate
  • the functional film having an inorganic layer produced by the method for producing a functional film of the present invention it is the inorganic layer that mainly exhibits the intended function. Therefore, what is necessary is just to comprise the manufacturing method of the functional film of this invention according to the inorganic layer which expresses the target functions, such as the light transmittance of a specific wavelength.
  • the gas barrier film greatly affects the barrier performance when the inorganic layer is in contact with other members and cracks. Therefore, in order to protect the formed inorganic layer, it is necessary to stick a protective film with the first guide roller after the film formation.
  • a protective film with the first guide roller after the film formation.
  • the present invention as will be described later, even when a high-density inorganic layer is formed in vacuum by plasma CVD capable of forming a dense film and then a protective film is adhered, It can prevent that the component of a protective film transfers to the surface of the inorganic layer after peeling a film. Therefore, the present invention is more suitably used for a gas barrier film that is formed at a high density and has a high gas barrier property.
  • 1A and 1B are respectively an inorganic film forming apparatus 32 that performs a film forming process, an inactivation process, and an attaching process, and an organic that performs a peeling process and an organic layer forming process.
  • This is a film forming apparatus 30.
  • Both the inorganic film forming apparatus 32 shown in FIG. 1A and the organic film forming apparatus 30 shown in FIG. 1B send out the forming material from a roll formed by winding a long forming material,
  • the above-mentioned RtoR Roll to Roll
  • Such RtoR can produce an efficient functional film with high productivity.
  • the manufacturing apparatus shown in FIG. 1 (A) and FIG. 1 (B) has an inorganic layer 14 and an organic layer 16 alternately on the surface of a long substrate 12 as shown in FIG. 4 (C).
  • the formed gas barrier film 10c and the like are manufactured.
  • the film forming material Za is the long substrate 12 and one or more layers formed on the surface of the substrate 12, and the surface is organic. It is the material of the layer 16.
  • the film forming material Zb is formed by forming one or more layers on the surface of the substrate 12, and the surface is the inorganic layer 14, and the inorganic layer on this surface.
  • 14 is a material in which a protective film 18 is attached to 14.
  • the production method of the present invention is not limited to the production of a functional film such as a gas barrier film by RtoR using a long substrate, but a so-called single wafer type composition using a cut sheet substrate.
  • a functional film may be produced using a membrane method.
  • a plurality of organic layers 16 and / or inorganic layers 14 may be alternately formed. In that case, the formation method may be the same or different in each layer.
  • the substrate 12 is not particularly limited as long as the surface is made of various organic materials such as a polymer material and a resin material. Various materials can be used for the substrate 12 as long as the surface is formed of an organic material and an inorganic layer can be formed by plasma CVD. Specifically, the substrate 12 made of a polymer material such as polyethylene terephthalate (PET), polyethylene naphthalate, polyethylene, polypropylene, polystyrene, polyamide, polyvinyl chloride, polycarbonate, polyacrylonitrile, polyimide, polyacrylate, polymethacrylate, It is exemplified as a suitable example. In the present invention, the substrate 12 is a film-like object such as a long film or a cut sheet-like film.
  • PET polyethylene terephthalate
  • polyethylene naphthalate polyethylene
  • polypropylene polystyrene
  • polyamide polyvinyl chloride
  • polycarbonate polyacrylonitrile
  • polyimide polyacrylate
  • the substrate 12 has a plastic film, an article made of an organic material, a metal film or a glass plate, various metal articles as a main body, and a protective layer, an adhesive layer, a light reflection layer, an antireflection layer, An organic layer made of an organic material for obtaining various functions, such as a light shielding layer, a planarizing layer, a buffer layer, and a stress relaxation layer, may be formed.
  • these functional layers are not limited to one layer, and a substrate in which a plurality of functional layers are formed may be used as the substrate 12.
  • An inorganic film forming apparatus 32 shown in FIG. 1A is an apparatus for forming the inorganic layer 14 by plasma CVD as an example of a manufacturing apparatus that performs the method for manufacturing a functional film of the present invention.
  • the inorganic film forming apparatus 32 is an apparatus for forming the inorganic layer 14 on the surface of the film formation material Za by a vapor deposition method.
  • the inorganic film forming apparatus 32 includes a vacuum chamber 52 and an unwinding chamber 54 formed in the vacuum chamber 52.
  • the film forming chamber 56 and the drum 80 are included.
  • the inorganic film forming apparatus 32 conveys a long material to be formed such as a conveying roller pair, a guide member that regulates the position of the film forming material Za in the width direction, and various sensors.
  • a guide member that regulates the position of the film forming material Za in the width direction
  • various sensors such as a laser scanner, a laser scanner, a laser scanner, a laser scanner, and various sensors.
  • various members provided in a known apparatus that performs film formation by a vapor deposition method may be included.
  • the inorganic film forming apparatus 32 that uses RtoR synchronizes the feeding of the film forming material Za from the material roll 61 and the winding of the film forming material Za with the inorganic layer formed on the winding shaft 92. Then, the inorganic layer 14 is formed in the film formation chamber 56 while the long film formation material Za is conveyed in the longitudinal direction while being wound around the drum 80. After a predetermined time has elapsed, in the unwinding chamber 54, a protective film is attached to the surface of the inorganic layer 14, wound around the winding shaft 92, and wound into a roll.
  • the drum 80 is a cylindrical member that rotates in the clockwise direction in the drawing around a rotation axis that passes through the center of the drum 80 and is parallel to a direction perpendicular to the paper surface.
  • the drum 80 conveys in a longitudinal direction a film forming material Za guided by a guide roller 84a of an unwinding chamber 54, which will be described later, around a predetermined area on the peripheral surface and held in a predetermined position. Then, after being transferred into the film forming chamber 56, it is sent to the stepped roller 84 b in the unwinding chamber 54.
  • the drum 80 also functions as a counter electrode of a film forming electrode 82 of the film forming chamber 56 described later, and is grounded. That is, the drum 80 and the film forming electrode 82 constitute an electrode pair.
  • the drum 80 may be connected to a bias power source for applying a bias voltage to the drum 80.
  • a bias power source for applying a bias voltage to the drum 80.
  • the ground and the bias power supply may be connected to be switchable.
  • the bias power source all known power sources such as a high frequency power source and a pulse power source for applying a bias voltage, which are used in various film forming apparatuses, can be used.
  • the drum 80 may include a temperature adjusting means, and the film forming material Za may be cooled, for example, during the film formation of the inorganic layer 14.
  • the unwinding chamber 54 is a region in the vacuum chamber 52 other than the film forming chamber 56 described later. That is, the unwind chamber 54 is formed by the inner wall surface of the vacuum chamber 52, the peripheral surface of the drum 80, and the partition walls 60a and 60b extending from the inner wall surface of the vacuum chamber 52 to the vicinity of the peripheral surface of the drum 80. Space.
  • the leading ends of the partition walls 60a and 60b on the drum 80 side are close to the peripheral surface of the drum 80 to a position where they do not come into contact with the film forming material Za to be conveyed, and the unwind chamber 54, the film forming chamber 56, Are separated in a substantially airtight manner.
  • Such an unwinding chamber 54 includes the winding shaft 92, the guide rollers 68, 84a, 90a and 90b, the stepped roller 84b, the rotating shaft 64, the rotating shaft 86, and the vacuum exhaust means 70. Have.
  • the rotating shaft 64 is loaded with a material roll 61 around which a long film-forming material Za is wound.
  • the guide rollers 68 and 84a are ordinary guide rollers that guide the film forming material Za on the upstream side of the drum 80 in the transport path of the film forming material Za.
  • the stepped roller 84 b is a normal stepped roller that guides the film forming material Za on the downstream side of the drum 80.
  • the guide rollers 90a and 90b are ordinary guide rollers that guide the film forming material Za on the downstream side of the stepped roller 84b.
  • the take-up shaft 92 is a known elongate take-up shaft for taking up the film-forming material Za having the inorganic layer formed thereon.
  • the guide roller 90b also functions as a sticking roller for sticking the protective film 18 on the deposited inorganic layer 14. In the following description, the guide roller 90b is also referred to as a sticking roller 90b. The sticking roller 90b will be described in detail later.
  • the stepped roller 84 b is a so-called stepped roller in which the diameter of the end portion is larger than the diameter of the other region.
  • the stepped roller 84b conveys the film forming material Za while guiding it without contacting the inorganic layer 14 formed on the film forming material Za.
  • a stepped roller 84b is disposed between the drum 80 and the adhering roller 90b, and the film forming material Za separated from the drum 80 is conveyed by using the stepped roller 84b, whereby the adhering from the film forming chamber 56 is performed.
  • the conveying distance to the landing roller 90b can be increased. That is, the time from the formation of the inorganic layer 14 to the attachment of the protective film 18 can be increased.
  • reducing the activity of the surface of the inorganic layer 14 when the protective film 18 is adhered by setting the time from the formation of the inorganic layer 14 to the adhesion of the protective film 18 to 15 seconds or more. Can do. Therefore, since the protective film 18 is attached to the inorganic layer 14 having a low surface activity, that is, the inorganic layer 14 having a reduced number of dangling bonds on the surface, the inorganic layer and the components of the protective film are chemically treated. Binding can be suppressed. Thus, the process of leaving a time interval of 15 seconds or more from the film formation to the attachment of the protective film is an inactivation process in the present invention.
  • the time from film formation to sticking in the inactivation step is preferably 25 seconds or more. Thereby, the activity of the inorganic layer 14 surface can be reduced more suitably.
  • one stepped roller 84b is disposed between the drum 80 and the adhering roller 90b.
  • the present invention is not limited to this. Accordingly, two or more stepped rollers may be arranged.
  • a stepped roller may be disposed as a guide roller that contacts the surface on which the inorganic layer 14 of the film formation material Za is formed, and the surface on the side on which the inorganic layer 14 of the film formation material Za is formed.
  • a normal guide roller may be used as the guide roller in contact with the opposite surface.
  • the time from the formation of the inorganic layer 14 to the attachment of the protective film 18 is set to 15 seconds or more, but is not limited thereto. As long as the time from non-deposition to sticking can be set to 15 seconds or more, a configuration without using a stepped roller may be used.
  • a material roll 61 formed by winding a long film-forming material Za in a roll shape is mounted on a rotating shaft 64.
  • the film forming material Za passes through the guide rollers 68 and 84a, the drum 80, the stepped roller 84b, the guide roller 90a, and the sticking roller 90b.
  • a predetermined path to the winding shaft 92 is passed.
  • the film forming material Za from the material roll 61 is sent out and the film forming material Za with the inorganic layer formed on the winding shaft 92 is synchronously wound.
  • the film forming material Za and the protective film 18 are continuously attached while the film forming material Za is transported in the longitudinal direction along a predetermined transport path.
  • the rotating shaft 86 is loaded with a film roll 87 formed by winding a protective film 18 for protecting the deposited inorganic layer 14 in a roll shape, and rotates in synchronization with the conveyance of the film forming material Za to protect it.
  • the film 18 is sent out.
  • the rotating shaft 86 is rotated by a driving source (not shown).
  • the protective film 18 sent out from the film roll 87 is brought into contact with the surface of the inorganic layer 14 by the adhering roller 90b, and is laminated / adhered to the film forming material Za.
  • the sticking roller 90b may have a heating means.
  • sticking of the protective film 18 is performed after an inactivation process.
  • the protective film 18 is stuck to the inorganic layer 14 in a state where the surface activity is low, that is, the inorganic layer 14 in a state where the number of dangling bonds on the surface is reduced, the inorganic layer and the components of the protective film are bonded. It is possible to suppress chemical bonding. This will be described in detail later.
  • the inorganic layer 14 can be protected by sticking the protective film 18 to the surface of the inorganic layer 14 in a peelable manner.
  • the inorganic layer 14 is hard and brittle because it is dense. Therefore, it is easily damaged when it receives an impact directly from the outside.
  • the gas barrier film produced by the production method of the present invention it is the inorganic layer 14 that mainly exhibits gas barrier properties. Therefore, when the inorganic layer 14 is damaged, the gas barrier property is lowered.
  • the protective film 18 is not particularly limited, and various known plastic films used for protecting the inorganic layer 14 formed by a vapor deposition method, such as a low density polyethylene film, can be used.
  • the thickness of the protective film 18 will not be specifically limited if it is the thickness which can prevent the crack of the inorganic layer 14, etc.
  • the thickness of the protective film 18 is preferably 20 ⁇ m or more.
  • 100 micrometers or less are preferable from viewpoints, such as flexibility of a gas barrier film, size reduction and weight reduction, and the ease of winding in a roll form.
  • the vacuum exhaust means 70 is a vacuum pump for reducing the pressure in the unwind chamber 54 to a predetermined degree of vacuum.
  • the vacuum evacuation means 70 makes the inside of the unwinding chamber 54 a pressure that does not affect the pressure in the film forming chamber 56.
  • the vacuum evacuation means 70 is not particularly limited, and various known vacuum evacuation means used in a vacuum film formation apparatus such as a vacuum pump such as a turbo pump, a mechanical booster pump, a dry pump, and a rotary pump, Is available. In this regard, the same applies to other vacuum exhaust means 74 described later.
  • a film forming chamber 56 is disposed downstream of the unwind chamber 54 in the transport direction of the film forming material Za.
  • the film forming chamber 56 is a part where a film forming process is performed by plasma CVD, and an inorganic layer is formed on the surface of the substrate 12 or the organic layer 16 which is the film forming material Za by a vapor deposition method.
  • the film forming chamber 56 is a space formed by an inner wall surface of the vacuum chamber 52, a peripheral surface of the drum 80, and partition walls 60 a and 60 b extending from the inner wall surface of the vacuum chamber 52 to the vicinity of the peripheral surface of the drum 80. It is.
  • the film forming chamber 56 forms a film on the surface of the film forming material Za by CCP (Capacitively Coupled Plasma) -CVD as an example. And a high-frequency power source 83 and a vacuum exhaust means 74.
  • the film forming material Za wound around a predetermined position of the drum 80 and transported to the film forming chamber 56 is transported in the longitudinal direction while being positioned at the predetermined position by the drum 80 to continuously form the inorganic layer 14.
  • the film forming electrode 82 constitutes an electrode pair together with the drum 80 when the inorganic film forming apparatus 32 forms a film by CCP-CVD.
  • the film forming electrode 82 is a known film forming electrode used in a vacuum film forming apparatus such as plasma CVD.
  • a so-called shower electrode is used as the film forming electrode 82.
  • the shower electrode has a hollow, substantially rectangular parallelepiped shape, and is disposed with the discharge surface, which is one maximum surface, facing the peripheral surface of the drum 80, and the discharge surface, which is the surface facing the drum 80, has many through holes. Is formed entirely.
  • the film formation electrode 82 generates plasma for film formation between the discharge surface and the peripheral surface of the drum 80 forming the electrode pair, thereby forming a film formation region.
  • a source gas is supplied to a film forming region between the film forming electrode 82 and the drum 80 by a source gas supply unit (not shown).
  • a source gas supply unit (not shown).
  • the source gas supply means supplies the source gas into the shower electrode.
  • a large number of through holes are formed on the surface of the shower electrode facing the drum 80. Therefore, the source gas supplied to the shower electrode is introduced between the film forming electrode 82 and the drum 80 from this through hole.
  • a known reaction gas corresponding to the inorganic layer 14 to be formed may be used.
  • silane gas and ammonia gas and / or nitrogen gas may be used.
  • a silicon oxide film is formed.
  • silane gas and oxygen gas may be used as the source gas.
  • various gases such as an inert gas such as helium gas, neon gas, argon gas, krypton gas, xenon gas, and radon gas, hydrogen gas, and the like may be used in combination with the source gas.
  • the vacuum evacuation means 74 is for evacuating the inside of the film forming chamber 56 to obtain a degree of vacuum corresponding to the formation of the inorganic layer 14.
  • the film formation chamber 56 is configured to form an inorganic layer by CCP-CVD.
  • CCP-CVD inductively coupled plasma CVD
  • CVD is available.
  • the inside of the film forming chamber 56 is composed of various members according to the vapor deposition method to be performed.
  • the film forming chamber 56 forms the inorganic layer 14 by the ICP-CVD method, an induction coil for forming an induction magnetic field and a gas supply means for supplying a reaction gas to the film forming region And so on.
  • the formation conditions of the inorganic layer 14, such as temperature and pressure, may be appropriately set according to the film formation method, the target film thickness, film formation rate, and the like.
  • the pressure in the film formation chamber 56 is preferably 20 Pa to 200 Pa, and the temperature is preferably 0 ° C. to 80 ° C.
  • the pressure in the film formation chamber 56 is preferably 0.1 Pa to 10 Pa and the temperature is preferably 0 ° C. to 80 ° C.
  • the inorganic layer 14 formed in the film formation chamber 56 is a layer made of an inorganic compound not containing carbon.
  • metal oxides such as aluminum oxide, magnesium oxide, tantalum oxide, zirconium oxide, titanium oxide, and indium tin oxide (ITO); metal nitrides such as aluminum nitride; silicon such as silicon oxide and silicon oxynitride
  • ITO indium tin oxide
  • metal nitrides such as aluminum nitride
  • silicon such as silicon oxide and silicon oxynitride
  • Inorganic compounds such as oxides; silicon nitrides such as silicon nitride; hydrides thereof; mixtures of two or more of these; and hydrogen-containing substances thereof are preferably exemplified.
  • an inorganic compound composed of a combination of elements selected from the group consisting of Si, Al, O, N, and H is suitable.
  • silicon nitride, silicon oxide, silicon oxynitride, and aluminum oxide are suitably used for the gas barrier film because they are highly transparent and can exhibit excellent gas barrier properties.
  • silicon nitride is particularly suitable for its excellent gas barrier properties and high transparency.
  • the inorganic layer 14 may contain 5% or less of carbon as an unavoidable impurity. Or in order to express a predetermined function, you may contain 5% or less of carbon. That is, the inorganic layer 14 may not contain carbon, but may contain carbon as an inevitable impurity derived from the material used as the raw material of the inorganic layer.
  • carbon can be contained in the inorganic layer derived from an organic silane such as Si (OCH 3 ) 4 as a raw material.
  • composition ratio of carbon in the inorganic layer was determined by measuring the number of atoms of Si, Al, O, N, and C in the inorganic layer 14 by XPS measurement (X-ray photoelectron spectroscopy measurement). And calculated as the ratio of C atoms.
  • the thickness of the inorganic layer 14 to be formed is not particularly limited, but is preferably 10 to 200 nm. By setting the thickness of the inorganic layer 14 to 10 nm or more, the inorganic layer 14 that stably expresses sufficient gas barrier performance can be formed. Further, the inorganic layer 14 is generally brittle, and if it is too thick, there is a possibility that cracks, cracks, peeling, etc. may occur. However, if the thickness of the inorganic layer 14 is 200 nm or less, cracks will occur. Can be prevented. In consideration of such points, the thickness of the inorganic layer 14 is preferably 15 to 100 nm, and more preferably 20 to 75 nm.
  • the present invention can be suitably used when the dense inorganic layer 14 is formed in order to develop a high gas barrier property.
  • the film density of the inorganic layer is preferably 1.8 to 2.2 g / cm 3.
  • the film of the inorganic layer is preferable.
  • the density is preferably 2.1 to 2.5 g / cm 3.
  • the film density of the inorganic layer is preferably 2.0 to 2.4 g / cm 3 .
  • the film density of the inorganic layer is preferably 2.7 to 3.2 g / cm 3 .
  • the protective film 18 is attached by the attaching roller 90b.
  • the inorganic layer immediately after being formed at a high density in a vacuum by plasma CVD has a high surface activity, and it is presumed that many dangling bonds exist.
  • a dense inorganic layer is formed by increasing the applied power or the like, the number of atoms constituting the inorganic layer increases, and it is considered that more dangling bonds are generated.
  • the atmosphere it is considered that the dangling bonds react with elements in the atmosphere and deactivate, but in vacuum, there is no bonding partner, so it is considered that more dangling bonds remain.
  • the protective film when the protective film is peeled off and another layer is formed on the inorganic layer, the protective film components remain on the surface of the inorganic layer, and the presence of the transferred components causes the inorganic layer and the inorganic layer to remain on the surface. There was a problem that the adhesion with the formed layer was hindered.
  • the present invention by performing an inactivation step with a time interval of 15 seconds or more from the formation of the inorganic layer 14 to the attachment of the protective film, the surface of the inorganic layer 14 is not present.
  • the bond is inactivated, and the surface activity of the inorganic layer 14 is reduced.
  • a protective film 18 for protecting the inorganic layer 14 is pasted even when the applied power is increased or the conveyance speed is increased to improve the production efficiency. When it does, it can suppress that the inorganic layer and the component of a protective film couple
  • the gas barrier film has a possibility that the barrier performance is greatly deteriorated when the inorganic layer is in contact with other members and cracks even a little, and the influence on the contact with the surface of the inorganic layer is great. Therefore, it is necessary to protect the inorganic layer formed by attaching a protective film with the first guide roller immediately after the film formation and before contacting the other members.
  • a gas barrier film requires high gas barrier performance, it is necessary to form a particularly dense inorganic layer. In order to form a dense inorganic layer, it is necessary to increase the applied power. Therefore, in the production of a gas barrier film, the surface of the inorganic layer after film formation is in a very high activity state.
  • the method for producing a functional film of the present invention is more suitably used for a method for producing a gas barrier film that is formed at a high density and has a high gas barrier property.
  • the protective film 18 is attached and the material roll 93 wound in a roll shape is supplied to the organic film forming apparatus 30, or the gas barrier film 10a shown in FIG.
  • the material roll 93 that is rotated is supplied to the next process.
  • the organic film forming apparatus 30 shown in FIG. 1 (B) applies a coating material to be the organic layer 16 while transporting a long film-forming material Zb in the longitudinal direction, and after drying, coats the coating film by light irradiation.
  • This is an apparatus for forming an organic layer 16 by crosslinking and curing an organic compound contained therein.
  • the organic film forming apparatus 30 includes, as an example, a coating unit 36, a drying unit 38, a light irradiation unit 40, a rotating shaft 42, a winding shaft 46, and a pair of conveying rollers 48 and 50. .
  • the organic film forming apparatus 30 also has a take-up shaft 44 that peels off and winds up the protective film 18 attached by the inorganic film forming apparatus 32 that forms the inorganic layer 14.
  • the organic film forming apparatus 30 performs film formation by coating while conveying a long material to be formed such as a pair of transport rollers, a guide member for the material to be deposited Zb, and various sensors. You may have the various members provided in a well-known apparatus.
  • a material roll 93 formed by winding a long film forming material Zb in which the inorganic layer 14 or the like is formed on the substrate 12 is loaded on the rotating shaft 42.
  • the film-forming material Zb is pulled out from the material roll 93, passes through the conveying roller pair 48, passes through the coating unit 36, the drying unit 38, and the light irradiation unit 40. Then, it passes through a predetermined conveying path that reaches the winding shaft 46 through the conveying roller pair 50.
  • the film forming material Zb is fed out from the material roll 93 and the film forming material Zb on which the organic layer is formed on the take-up shaft 46 is synchronously performed.
  • the coating material 36 is applied with the coating material that is an organic layer
  • the drying device 38 is used to dry the coating material
  • the light irradiation device 40 is used.
  • the organic layer is formed by curing.
  • the transport roller pair 48 also functions as a peeling roller for the protective film 18. That is, the organic film forming apparatus 30 performs an organic layer forming process after the peeling process.
  • the organic layer 16 formed in the organic layer forming step is a layer made of an organic compound, and is basically a cross-linked organic compound that becomes the organic layer 16.
  • the material for forming the organic layer 16 is not limited, and various known organic compounds can be used. Specifically, polyester, acrylic resin, methacrylic resin, methacrylic acid-maleic acid copolymer, polystyrene, transparent fluororesin, polyimide, fluorinated polyimide, polyamide, polyamideimide, polyetherimide, cellulose acylate, polyurethane, poly Ether ether ketone, polycarbonate, alicyclic polyolefin, polyarylate, polyether sulfone, polysulfone, fluorene ring modified polycarbonate, alicyclic modified polycarbonate, fluorene ring modified polyester, acryloyl compound, thermoplastic resin, or polysiloxane, etc.
  • An organic silicon compound film is preferably exemplified. A plurality of these may be used in combination.
  • the thickness of the organic layer 16 formed in the organic layer forming step is not particularly limited, but is preferably 0.1 to 50 ⁇ m.
  • the thickness of the organic layer 16 is more preferably 0.15 to 5 ⁇ m.
  • the coating means 36 applies a paint for forming the organic layer 16 prepared in advance on the surface of the film forming material Zb.
  • This paint is obtained by dissolving an organic compound such as a monomer, a dimer, a trimer, or an oligomer, which becomes the organic layer 16 by crosslinking and polymerizing in an organic solvent, in the organic solvent.
  • the coating material contains a silane coupling agent in order to improve the adhesion of the organic layer 16.
  • necessary components such as a surfactant, a polymerization initiator, and an increasing viscosity agent may be appropriately added to this paint.
  • the application of the paint is all known coating methods such as die coating, dip coating, air knife coating, curtain coating, roller coating, wire bar coating, gravure coating, slide coating, etc. Is available. Above all, because the coating can be applied in a non-contact manner, the surface of the film-forming material Zb is not damaged, and the bead formation is excellent in the embedding of the surface of the film-forming material Zb, etc. Are preferably used.
  • the film forming material Zb is then transported to the drying unit 38, and the coating material applied by the coating unit 36 is dried.
  • the method of drying the paint by the drying means 38 is not limited, and before the film-forming material Zb reaches the light irradiation means 40, the paint is dried and the organic solvent is removed so that crosslinking is possible. Any known drying means can be used if possible. As an example, heat drying with a heater, heat drying with warm air, and the like are exemplified.
  • the temperature of the film formation material Zb at the time of drying in the drying means 38 is preferably 70 ° C. or higher.
  • the adhesion between the organic layer 16 and the inorganic layer 14 is further improved by drying the coating material with the film-forming material Zb at a temperature of 70 ° C. or higher. preferable.
  • the film formation material Zb is then transported to the light irradiation means 40.
  • the light irradiation means 40 irradiates the coating material applied by the application means 36 and dried by the drying means 38 with ultraviolet rays or visible light, or crosslinks an organic compound such as a monomer contained in the coating material by heating or the like.
  • the organic layer 16 is cured.
  • the protective film 18 is adhered after reducing the activity of the surface of the inorganic layer 14 with a time interval of 15 seconds or more. Therefore, when the protective film 18 is peeled off in order to form the organic layer 16 on the inorganic layer 14, the remaining components of the protective film 18 can be reduced. Therefore, the adhesion between the inorganic layer 14 and the organic layer 16 formed on the inorganic layer 14 can be improved.
  • the coating material that forms the organic layer 16 contains a silane coupling agent
  • the component of the protective film 18 such as carbon remains on the surface of the inorganic layer 14
  • the silane coupling agent The effect of improving the adhesion due to may not be obtained, and the adhesion between the inorganic layer 14 and the organic layer 16 may be reduced.
  • the effect of improving the adhesion by the silane coupling agent can be sufficiently expressed. And the adhesion between the inorganic layer 14 and the organic layer 16 can be improved.
  • the light irradiation area by the light irradiation means 40 in the film forming material Zb may be made an inert atmosphere by nitrogen substitution or the like, if necessary. Further, if necessary, a temperature of the film forming material Zb, that is, the coating film, may be adjusted at the time of curing by using a backup roller or the like that contacts the back surface.
  • the temperature of the film forming material Zb when the coating film is cured by the light irradiation means 40 is preferably 30 ° C. or higher, more preferably 50 ° C. or higher, and more preferably 60 ° C. or higher.
  • the crosslinking of the organic compound that becomes the organic layer is not limited to photopolymerization. That is, various methods according to the organic compound used as the organic layer 16 can be used for crosslinking of the organic compound, such as heat polymerization, electron beam polymerization, and plasma polymerization.
  • various methods according to the organic compound used as the organic layer 16 can be used for crosslinking of the organic compound, such as heat polymerization, electron beam polymerization, and plasma polymerization.
  • an acrylic resin such as an acrylic resin or a methacrylic resin is preferably used as the organic layer 16
  • photopolymerization is preferably used.
  • the film-forming material Zb on which the organic layer 16 has been formed in this manner is nipped and conveyed by the conveyance roller pair 50 to reach the take-up shaft 46, and is taken up again in a roll shape by the take-up shaft 46.
  • the material roll 61 is formed by winding the film forming material Zb on which the layer 16 is formed.
  • the material roll 61 is supplied to the inorganic film forming apparatus 32 as a material roll 61 formed by winding the film forming material Zb on which the organic layer 16 is formed, or is shipped or stored as a product, or the next process or the like. To be supplied.
  • a gas barrier film in which two inorganic layers 14 and one organic layer 16 shown in FIG. 5 (A) are formed and a protective film 18 is laminated The production method of the present invention will be described in more detail by explaining the action when producing 10d.
  • a gas barrier film having other layer configuration such as the gas barrier film 10a shown in FIG. 4A, depending on the number of inorganic layers 14 and the number of organic layers 16 to be formed, and the layer configuration, The formation of the similar inorganic layer 14 and organic layer 16 may be repeated.
  • a material roll 61 formed by winding the substrate 12 is prepared.
  • the inorganic film forming apparatus 32 when the material roll 61 formed by winding the substrate 12 is loaded on the rotating shaft 64, the substrate 12 as the film forming material Za is drawn out, and the film forming chamber 56 is extracted from the unwind chamber 54. Through a predetermined path to the take-up shaft 92 of the unwind chamber 54.
  • the film formation material Za sent out from the material roll 61 is guided by the guide rollers 68 and 84a, wound around the drum 80, supported by the drum 80, and conveyed to the film formation chamber 56 while being conveyed through a predetermined path. Is done.
  • the film forming material Za transferred to the film forming chamber 56 is supported by the drum 80 and transferred through a predetermined path as a film forming process, and the first inorganic layer 14 is formed by, for example, CCP-CVD. It is formed.
  • the film forming material Za on which the inorganic layer 14 is formed is conveyed to the unwinding chamber 54 as an inactivation step, separated from the drum 80, and guided to the stepped roller 84b and the guide roller 90a to be a sticking roller. Up to 90b. At this time, the time required for conveyance from the film forming chamber 56 to the sticking roller 90b is set to 15 seconds or more, and the dangling bonds on the surface of the inorganic layer 14 are inactivated.
  • the protective film 18 sent out from the film roll 87 is stuck to the film-forming material Za conveyed to the sticking roller 90b as the sticking step on the first inorganic layer 14 (FIG. 4 ( A)).
  • the film forming material Za to which the protective film 18 is attached that is, the film forming material Zb, is wound into a roll shape by the take-up shaft 92 to form a material roll 93.
  • a material roll 93 formed by winding the substrate 12 on which the first inorganic layer 14 is formed and the protective film 18 is laminated is loaded on the rotating shaft 42 of the organic film forming apparatus 30.
  • the material roll 93 is loaded on the rotating shaft 42, the substrate 12 on which the first inorganic layer 14 that is the film formation material Zb is formed is pulled out of the material roll 93 and applied through the conveying roller pair 48. It passes through the means 36, the drying means 38, and the light irradiation means 40, passes through a pair of transport rollers 50, and passes through a predetermined transport path to the winding shaft 46.
  • the film forming material Zb drawn from the material roll 93 is subjected to the organic layer forming step after the protective film 18 is peeled off by the transport roller pair 48 (see FIG. 4B) as a peeling step. That is, the film-forming material Zb from which the protective film 18 has been peeled is transported to the coating means 36, and the coating material to be the organic layer 16 is applied to the surface.
  • the paint to be the organic layer 16 is obtained by dissolving an organic compound such as a monomer, a silan coupling agent, a polymerization initiator, and the like in an organic solvent according to the organic layer 16 to be formed.
  • the film-forming material Zb to which the coating material to be the organic layer 16 is applied is then heated by the drying means 38 to remove the organic solvent and dry the coating material.
  • the film-forming material Zb from which the paint has been dried is then irradiated with ultraviolet rays or the like by the light irradiation unit, and the organic compound is polymerized and cured to form the first organic layer 16 (FIG. 4C). reference).
  • the organic compound that becomes the organic layer 16 may be cured in an inert atmosphere such as a nitrogen atmosphere. Further, the substrate 12 may be heated when the organic compound that becomes the organic layer 16 is cured.
  • the film-forming material Zb on which the first organic layer 16 is formed is conveyed by the conveying roller pair 50 and wound in a roll shape by the take-up shaft 46, and the inorganic layer 14 and the organic layer 16 are layered one by one.
  • a material roll 61 formed by winding the formed substrate 12 is supplied again to the inorganic film forming apparatus 32 shown in FIG.
  • the material roll 61 formed by winding the substrate 12 on which the inorganic layer 14 and the organic layer 16 are formed one by one is loaded on the rotating shaft 64 of the inorganic film forming apparatus 32 as described above.
  • the substrate 12 on which the inorganic layer 14 and the organic layer 16 are formed is drawn out as a film forming material Za and passed through the take-up shaft 92, and the second inorganic layer 14 is formed on the first organic layer 16.
  • the protective film 18 was further stuck, and the organic / inorganic laminate composed of the inorganic layer 14, the organic layer 16, and the inorganic layer 14 and the protective film 18 were laminated.
  • the gas barrier film 10d is wound around the winding shaft 92 in a roll shape, and is shipped or stored as a product as a material roll 93 around which the gas barrier film 10d is wound, or is supplied to the next step or the like.
  • the material roll 93 may be further supplied to the organic film forming apparatus 30, the protective film 18 may be peeled off (FIG. 5B), and the organic layer 16 may be formed (FIG. 5C).
  • the bonding roller 90b is used. Since the protective film 18 is adhered, the remaining of the components of the protective film 18 when the protective film 18 is peeled from the inorganic layer 14 can be reduced, and the organic layer formed on the inorganic layer 14 and the inorganic layer 14. Adhesion with 16 can be improved.
  • FIG. 3 is an example of an inorganic film forming apparatus for carrying out another example of the inactivation step in the present invention.
  • the inorganic film forming apparatus 110 shown in FIG. 3 has the same configuration as the inorganic film forming apparatus 32 shown in FIG. 1A except that it has a sticking roller 114 instead of the stepped roller 84b.
  • the same reference numerals are given to the components, and detailed description thereof is omitted.
  • the inorganic film forming apparatus 110 includes a vacuum chamber 52, an unwinding chamber 112 formed in the vacuum chamber 52, a film forming chamber 56, and a drum 80.
  • the unwinding chamber 112 is a region other than the film forming chamber 56 in the vacuum chamber 52.
  • the unwinding chamber 112 has a winding shaft 92, guide rollers 68, 84 a and 90, a sticking roller 114, a rotating shaft 64, a rotating shaft 86, and a vacuum exhaust means 70.
  • the adhering roller 114 is an adhering roller that is disposed downstream of the drum 80 and adheres the protective film 18 onto the inorganic layer 14 that has been formed.
  • the sticking roller 114 is cooled to 15 ° C. or less by a cooling means (not shown). By cooling the sticking roller 114 to 15 ° C. or lower, the substrate 12 is sufficiently cooled when the protective film 18 is stuck to the film forming material Za.
  • the bonding roller 114 is cooled to 10 ° C. or lower to sufficiently cool the substrate 12 when the protective film 18 is bonded to the film forming material Za, thereby inactivating the unbonded hands on the surface of the inorganic layer 14. can do. Thereby, when the protective film 18 is stuck, it can suppress that an inorganic layer and the component of a protective film couple
  • the temperature of the substrate 12 when the protective film 18 is stuck is preferably 15 ° C. or less, and more preferably 10 ° C. or less. Thereby, the activity of the inorganic layer 14 surface can be reduced more suitably.
  • the adhering roller 114 is cooled.
  • the present invention is not limited to this, and a guide roller is disposed between the drum 80 and the adhering roller 114, and this guide roller is used. It is good also as a structure which cools and the board
  • a known cooling means such as a device for blowing cold air is disposed between the drum 80 and the sticking roller 114 to cool the substrate 12 and inactivate the unbonded hands on the surface of the inorganic layer 14. Also good.
  • the deactivation step may be a combination of a configuration in which the time from the formation of the inorganic layer 14 to the attachment of the protective film 18 is 15 seconds or more and a configuration in which the substrate 12 is cooled.
  • the substrate 12 may be cooled by cooling the sticking roller 90b.
  • Example 1 (Board preparation process)
  • the substrate 12 was prepared by forming an organic layer made of acrylate on the surface of a long PET film having a width of 1000 mm and a thickness of 100 ⁇ m (Cosmo Shine A4300 manufactured by Toyobo Co., Ltd.).
  • This organic layer is formed on a long PET film by the same method as the method for forming the organic layer 16 by the organic film forming apparatus 30.
  • a material roll 61 formed by winding a substrate 12 to be a film forming material Za is loaded on the rotation shaft of the inorganic film forming apparatus 32 shown in FIG. 1A, and the film forming material Za is placed on a predetermined transport path.
  • the following film formation process, inactivation process, and sticking process were performed while being inserted and conveyed.
  • the inorganic layer 14 made of silicon nitride having a thickness of 50 nm was formed on the surface of the substrate 12 transferred to the film formation chamber 56.
  • Silane gas (SiH 4 ), ammonia gas (NH 3 ), and hydrogen gas (H 2 ) were used as source gases supplied to the film forming chamber 56.
  • the flow rate converted to the volume at 0 ° C. and 0.1013 MPa was 100 mL / min for silane gas, 400 mL / min for ammonia gas, and 1000 mL / min for hydrogen gas.
  • the following description is the flow volume converted into the volume in 0 degreeC and 0.1013 MPa similarly.
  • the film forming pressure was 50 Pa.
  • a plasma excitation power of 2 kW at a frequency of 13.5 MHz was supplied from the high frequency power supply 83 to the film forming electrode 82.
  • the composition ratio of carbon in the deposited inorganic layer 14 was measured by XPS and found to be 1% or less.
  • the protective film 18 was stuck to the film forming material Za by the sticking roller 90b.
  • a long polyethylene film having a width of 1000 mm and a thickness of 50 ⁇ m (SUNYTECT PAC-2, manufactured by Sanei Kaken Co., Ltd.) was used.
  • the unwind chamber 54 and the film-forming chamber 56 are finished. Cleaned dry air was introduced to open the atmosphere.
  • a material roll 93 (see FIG. 4A) formed by winding the substrate 12 on which the inorganic layer 14 was formed and the protective film 18 was attached was taken out from the unwind chamber 54.
  • the organic layer 16 having a thickness of 3 ⁇ m is formed on the surface of the inorganic layer 14 by the coating unit 36, the drying unit 38, and the light irradiation unit 40, and the gas barrier film 10c shown in FIG. did.
  • the paint for forming the organic layer 16 is MEK (methyl ethyl ketone), TMPTA (manufactured by Daicel Cytec Co., Ltd.), photopolymerization initiator (Irg189 manufactured by Ciba Chemicals Co., Ltd.), silane coupling agent (Shin-Etsu Chemical Co., Ltd., Shin-Etsu). Silicone KBM5103) was added to prepare. That is, the organic layer 16 is a layer formed by polymerizing TMPTA.
  • the addition amount of the photopolymerization initiator was 2% by mass in a concentration excluding the organic solvent, and the addition amount of the silane coupling agent was 10% by mass in the concentration excluding the organic solvent. That is, TMPTA in solid content was 88 mass%.
  • the solid content concentration of the paint obtained by diluting the components blended in these ratios with MEK was 15% by mass. That is, MEK was 85 mass%.
  • the coating means 36 used a die coater.
  • the drying means 38 used the apparatus which blows off the drying wind from a nozzle, and drying was performed at 80 degreeC.
  • the light irradiation means 40 was irradiated with ultraviolet rays to carry out polymerization. The curing with ultraviolet rays was carried out while heating the substrate 12 to 80 ° C. from the back side so that the irradiation amount of the ultraviolet rays was about 500 mJ / cm 2 in terms of the integrated irradiation amount.
  • Example 2 A gas barrier film was produced in the same manner as in Example 1 except that the treatment conditions in the film formation step were changed as follows and the time of the inactivation step was changed to 16 seconds.
  • Two film formation chambers 56 are arranged in series in the transport direction, and the supply amount of the raw material gas in each film formation chamber is 250 mL / min for silane gas, 1000 mL / min for ammonia gas, and 2500 mL / min for hydrogen gas.
  • the plasma excitation power supplied to the film forming electrode 82 was 5 kW.
  • the composition ratio of carbon in the deposited inorganic layer 14 was measured by XPS and found to be 1% or less.
  • Example 3 Between the drum 80 and the adhering roller 90b, two stepped rollers 84b and two guide rollers 90a are arranged, and in the inactivation process, until the film is transferred from the film forming chamber 56 to the adhering roller 90b.
  • a gas barrier film was produced in the same manner as in Example 2 except that the time was set to 25 seconds.
  • Example 4 In the deactivation process, instead of the configuration in which the stepped roller 84b is arranged and the time from the film formation process to the bonding process is set to 15 seconds or more, the bonding roller is cooled to cool the substrate 12. Except for the above, a gas barrier film was produced in the same manner as in Example 1. That is, in Example 4, instead of the inorganic film forming apparatus 32 shown in FIG. 1 (A), the inorganic film forming apparatus 110 shown in FIG. It was. The cooling temperature of the sticking roller 114 was 10 ° C.
  • Example 5 A gas barrier film was produced in the same manner as in Example 4 except that the cooling temperature of the sticking roller 114 was 0 ° C.
  • Example 6 A gas barrier film was produced in the same manner as in Example 5 except that the processing conditions in the film forming step were changed as follows.
  • Two film formation chambers 56 are arranged in series in the transport direction, and the supply amount of the raw material gas in each film formation chamber is 250 mL / min for silane gas, 1000 mL / min for ammonia gas, and 2500 mL / min for hydrogen gas.
  • the plasma excitation power supplied to the film forming electrode 82 was 5 kW.
  • the composition ratio of carbon in the deposited inorganic layer 14 was measured by XPS and found to be 1% or less.
  • Example 7 A gas barrier film was produced in the same manner as in Example 6 except that the cooling temperature of the sticking roller 114 was ⁇ 15 ° C.
  • Example 4 A gas barrier film was produced in the same manner as in Example 2 except that the stepped roller was not disposed, the inactivation step was not performed, and the sticking step was not performed.
  • the gas barrier film 10 c having the organic layer 16 formed on the inorganic layer 14 was subjected to a cross-cut test to evaluate the adhesion between the inorganic layer 14 and the organic layer 16.
  • the cross-cut test is based on JIS-K5600, and the organic layer 16 is 1 mm wide, cut, and peeled off with an adhesive tape (Cello Tape (registered trademark) CT-24 manufactured by Nichiban Co., Ltd.). The residual mass was measured and the adhesion was evaluated.
  • Comparative Examples 1 to 3 in which the protective film was stuck without performing the inactivation step decreased the adhesion with the organic layer formed on the inorganic layer after the protective film was peeled off.
  • Comparative Example 4 in which the protective film is not attached cannot prevent the inorganic layer from being cracked, and thus the gas barrier property is lowered. From the above results, the effects of the present invention are clear.

Landscapes

  • Chemical Vapour Deposition (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention fournit un procédé de fabrication de film fonctionnel qui permet d'empêcher une baisse d'adhésion entre une couche inorganique après pelage d'un film protecteur, et une couche formée sur cette couche inorganique. Le procédé de l'invention présente : une étape de préparation de substrat au cours de laquelle est préparé un substrat qui possède une surface constituée d'un matériau organique ; une étape de formation de film au cours de laquelle la couche inorganique dont le rapport de composition en carbone est inférieur ou égal à 5%, est formée sur le substrat par dépôt chimique en phase vapeur par plasma sous vide ; une étape d'inactivation au cours de laquelle des liaisons pendantes de la couche inorganique après formation du film, sont inactivées ; et une étape de collage au cours de laquelle le film protecteur constitué d'un film plastique est collé de manière à autoriser son pelage sur la couche inorganique, après l'étape d'inactivation.
PCT/JP2015/062137 2014-06-27 2015-04-21 Procédé de fabrication de film fonctionnel Ceased WO2015198701A1 (fr)

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JP2018144283A (ja) * 2017-03-02 2018-09-20 コニカミノルタ株式会社 機能性フィルム積層体の製造方法
CN114211850A (zh) * 2021-12-29 2022-03-22 深圳双十科技股份有限公司 一种多膜层全自动同步连续生产覆膜设备及其加工方法

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JP2014074221A (ja) * 2012-09-13 2014-04-24 Oji Holdings Corp 真空成膜装置及び真空成膜方法
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WO2012118037A1 (fr) * 2011-02-28 2012-09-07 富士フイルム株式会社 Procédé et appareil pour la fabrication de film fonctionnel
JP2012192738A (ja) * 2011-03-02 2012-10-11 Fujifilm Corp 機能性フィルムの製造方法
JP2014074221A (ja) * 2012-09-13 2014-04-24 Oji Holdings Corp 真空成膜装置及び真空成膜方法
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WO2017211989A1 (fr) * 2016-06-10 2017-12-14 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e. V. Procédé de revêtement d'un substrat flexible muni d'un film de protection
US10907249B2 (en) 2016-06-10 2021-02-02 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method for coating a flexible substrate provided with a protective film
JP2018144283A (ja) * 2017-03-02 2018-09-20 コニカミノルタ株式会社 機能性フィルム積層体の製造方法
CN114211850A (zh) * 2021-12-29 2022-03-22 深圳双十科技股份有限公司 一种多膜层全自动同步连续生产覆膜设备及其加工方法
CN114211850B (zh) * 2021-12-29 2024-02-09 深圳双十科技股份有限公司 一种多膜层全自动同步连续生产覆膜设备及其加工方法

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