WO2013122055A1 - 機能性フィルム、およびその製造方法、並びに前記機能性フィルムを含む電子デバイス - Google Patents
機能性フィルム、およびその製造方法、並びに前記機能性フィルムを含む電子デバイス Download PDFInfo
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- WO2013122055A1 WO2013122055A1 PCT/JP2013/053283 JP2013053283W WO2013122055A1 WO 2013122055 A1 WO2013122055 A1 WO 2013122055A1 JP 2013053283 W JP2013053283 W JP 2013053283W WO 2013122055 A1 WO2013122055 A1 WO 2013122055A1
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Images
Classifications
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
- B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B05D7/02—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 macromolecular substances, e.g. rubber
- B05D7/04—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 macromolecular substances, e.g. rubber to surfaces of films or sheets
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Definitions
- the present invention relates to a functional film, a manufacturing method thereof, and an electronic device including the functional film.
- Measures for obtaining a gas barrier film applicable to electronic devices include a method of forming a thick inorganic film on a resin substrate.
- a gas barrier film provided with an organic film as an adhesive layer specifically, a unit composed of an inorganic film and an organic film is formed on a resin substrate.
- Gas barrier films formed by alternately laminating have been proposed (Patent Documents 1 and 2).
- the performance is not always sufficient.
- the gas barrier film that requires flexibility has a large difference in film hardness between the resin base material and the organic film, and the inorganic film. Cracks can occur.
- the electronic device may be in a high temperature and high humidity environment. In such an environment, the resin base material, the organic film, and the inorganic film change their shapes with different expansion and contraction rates. The layer structure can be destroyed. Furthermore, as a result of the elution of the low molecular weight compound from the resin base material or the organic layer, the adhesion between the layers can be further lowered, and the performance of the inorganic film can be deteriorated.
- an object of the present invention is to provide a functional film such as a gas barrier film excellent in bending resistance and stability at high temperature and high humidity, a method for producing the same, and an electronic device including the functional film.
- the hybrid layer is located between the resin substrate and the functional inorganic layer.
- the hybrid layer is disposed on the surface of the functional inorganic layer opposite to the resin substrate.
- Functional film according to 4. Including two or more functional inorganic layers laminated ⁇ 3.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 0.001 to 10. ⁇ 4. Functional film of any one of these; 6).
- a method for producing a functional film comprising a resin substrate, a functional inorganic layer located on the resin substrate, and a hybrid layer disposed on at least one surface of the functional inorganic layer, A production method comprising a step (1) of forming a hybrid layer by applying a first coating liquid containing siloxane and resin fine particles; 9. 7.
- the production method according to 1; 10. 8. the inorganic precursor includes polysilazane; The production method according to 1; 11. 8. The modification treatment is performed by vacuum ultraviolet irradiation. Or 10.
- the production method according to 1; 12 An electronic device body; ⁇ 7. 7. The functional film according to any one of ⁇ 11. And a functional film produced by the method according to any one of the above; 13. 11. The electronic device body is sealed with the functional film.
- the present invention it is possible to provide a functional film excellent in bending resistance and stability at high temperature and high humidity, a method for producing the same, and an electronic device including the functional film.
- a resin base material a functional inorganic layer located on the resin base material, and a hybrid layer disposed on at least one surface of the functional inorganic layer, A functional film is provided.
- the hybrid layer includes polysiloxane and resin fine particles.
- FIG. 1 is a schematic cross-sectional view schematically showing the functional film according to the first embodiment.
- the functional film 11 according to the first embodiment has a resin base 12 in which a bleed-out prevention layer (not shown) is disposed on one surface, and is opposite to the bleed-out prevention layer.
- the hybrid layer 13 disposed on the surface and the functional inorganic layer 14 disposed on the hybrid layer 13 are included.
- the hybrid layer 13 includes polysiloxane and resin fine particles.
- the functional inorganic layer 14 includes silicon oxide and / or silicon oxynitride.
- the functional inorganic layer 14 is a gas barrier inorganic layer having gas barrier properties. Therefore, the functional film 11 which concerns on a 1st form is a gas barrier film.
- FIG. 2 is a schematic cross-sectional view schematically showing the functional film according to the second embodiment.
- the functional film 21 according to the second embodiment includes a resin base material 22 made of a polyester film having a bleed-out prevention layer (not shown) disposed on one surface, and the bleed-out prevention layer.
- the functional inorganic layer 24 arrange
- FIG. 3 is a schematic cross-sectional view schematically showing the functional film according to the third embodiment.
- the functional film 31 according to the second embodiment includes a resin base material 32 made of a polyester film having a bleed-out prevention layer (not shown) disposed on one surface, and the bleed-out prevention layer. And a hybrid layer 33a disposed on the opposite surface of the hybrid layer 33a, a functional inorganic layer 34 disposed on the hybrid layer 33a, and a hybrid layer 33b disposed on the functional inorganic layer 34.
- the hybrid layer 33a and the functional inorganic layer 34 have the same configuration as the first embodiment, and the hybrid layer 33b has the same configuration as the hybrid layer 33a.
- the functional film 31 is also a gas barrier film.
- Each of the functional films according to the first to third embodiments has a surface opposite to the surface on which the functional inorganic layer and the hybrid layer of the resin substrate are disposed, and further includes the first to third embodiments.
- a functional inorganic layer and a hybrid layer selected from the group consisting of may be disposed.
- the resin substrate according to the present invention is not particularly limited, but is preferably a foldable film substrate having flexibility and permeability.
- the resin substrate include acrylic acid ester, methacrylic acid ester, polyethylene terephthalate (PET), polybutylene terephthalate, polyethylene naphthalate (PEN), polycarbonate (PC), polyarylate, polyvinyl chloride (PVC), polyethylene (PE), polypropylene (PP), polystyrene (PS), nylon (Ny), aromatic polyamide, polyetheretherketone, polysulfone, polyethersulfone, polyimide, polyetherimide, and other resin films; having an organic-inorganic hybrid structure Examples thereof include a heat-resistant transparent film (Sila-DEC; manufactured by Chisso Corporation) having silsesquioxane as a basic skeleton.
- Sila-DEC heat-resistant transparent film
- polyethylene terephthalate (PET), polybutylene terephthalate, polyethylene naphthalate (PEN), and polycarbonate (PC) are preferably used from the viewpoints of cost and availability. From the viewpoint of optical transparency, heat resistance, etc., it is preferable to use a heat-resistant transparent film having silsesquioxane having an organic-inorganic hybrid structure as a basic skeleton. These base materials may be used alone or in combination of two or more.
- the resin base material using the above resin film may be an unstretched film or a stretched film.
- the resin substrate using the resin film can be produced by a conventionally known general method.
- an unstretched film that is substantially amorphous and not oriented can be produced by melting a resin as a material with an extruder, extruding it with an annular die or a T-die, and quenching.
- the unstretched film is uniaxially stretched, tenter-type sequential biaxial stretching, tenter-type simultaneous biaxial stretching, tubular-type simultaneous biaxial stretching, and other known methods, such as the flow (vertical axis) direction of the resin substrate, or
- a stretched film can be produced by stretching in the direction perpendicular to the flow direction of the resin substrate (horizontal axis).
- the draw ratio in this case can be appropriately selected according to the resin as the raw material of the resin base material, but is preferably 2 to 10 times in the vertical axis direction and the horizontal axis direction, respectively.
- the thickness of the resin substrate used in the present invention is preferably 5 to 500 ⁇ m, more preferably 25 to 250 ⁇ m.
- the resin base material used in the present invention is preferably transparent. It is because it becomes possible to set it as a transparent functional film as the resin base material is transparent, and to apply to the board
- the resin base material used in the present invention preferably has a linear expansion coefficient of 50 ppm / ° C. or less, preferably 1 to 50 ppm / ° C.
- the linear expansion coefficient of the resin base material is 50 ppm / ° C. or less
- a functional barrier film is applied to an electronic device such as a liquid crystal display device (LCD panel)
- the value measured by the following method shall be employ
- the substrate to be measured was heated to 30-50 ° C. at 5 ° C./min in a nitrogen atmosphere, Maintain a temporary temperature. Thereafter, the substrate is again heated to 30 to 150 ° C. at 5 ° C./min. At this time, the dimensional change of the base material is measured in a tensile mode (load 5 g). A linear expansion coefficient is calculated
- the resin substrate according to the present invention preferably has a light transmittance of visible light (400 nm to 700 nm) of 80% or more, and more preferably 90% or more.
- a light transmittance of visible light (400 nm to 700 nm) of 80% or more, and more preferably 90% or more.
- light transmittance means a spectrophotometer (visible ultraviolet spectrophotometer, UV-2500PC: manufactured by Shimadzu Corporation), and is based on ASTM D-1003 standard. It means the average transmittance in the visible light range, which is calculated by measuring the total transmitted light amount with respect to the incident light amount.
- the resin base material according to the present invention may be subjected to corona treatment.
- the resin base material according to the present invention may appropriately form another layer (intermediate layer).
- an anchor coat layer an easy adhesion layer
- the anchor coating agent that can be used is not particularly limited, but a silane coupling agent is used from the viewpoint of obtaining a high adhesion by forming a thin film of a monomolecular level to a nano level and forming a molecular bond at the layer interface. Is preferred.
- a stress relaxation layer made of a resin or the like, a smoothing layer for smoothing the surface of the resin base material, a bleed out prevention layer for preventing bleed out from the resin base material, or the like can be provided.
- a backcoat layer may be provided on the resin base material for the purpose of improving the curl balance of the functional inorganic layer, improving the device fabrication process resistance, handling suitability, and the like.
- the functional inorganic layer imparts a certain function to the functional film.
- the functional film can be a gas barrier film having gas barrier properties.
- a transparent conductive inorganic layer such as ITO, a heat shielding inorganic layer in which SiO 2 or TiO 2 is laminated, an electrode inorganic layer made of a metal, a metal oxide, or the like, interlayer insulating inorganic layer such as SiO 2, a gate insulating inorganic layer such as SiO 2, TAOS (transparent amorphous oxide semiconductor) oxide semiconductor inorganic layer such as a silver-deposited layer, and the multilayer film and the like having different refractive index.
- the functional inorganic layer can be used for touch panels, flexible printed boards, thin film transistors, various displays, backlights, reflectors, diffuse reflective films for polarizing plates, anti
- gas barrier inorganic layer has a function of imparting gas barrier properties to the functional film.
- gas barrier property means water vapor permeability measured by a method in accordance with JIS K 7129-1992 (temperature: 60 ⁇ 0.5 ° C., relative humidity (RH): 90 ⁇ 2%). Is 3 ⁇ 10 ⁇ 3 g / (m 2 ⁇ 24 h) or less, and the oxygen permeability measured by a method according to JIS K 7126-1987 is 1 ⁇ 10 ⁇ 3 mL / m 2 ⁇ 24 h ⁇ atm or less. It means that there is.
- the gas barrier inorganic layer is not particularly limited as long as it has gas barrier properties.
- an inorganic substance obtained by modifying an inorganic precursor is included.
- Polysilazane is preferably used as the inorganic precursor.
- Polysilazane is a polymer having a bond such as Si—N, Si—H, or N—H in its structure, and is an inorganic precursor such as SiO 2 , Si 3 N 4 , or an intermediate solid solution thereof such as SiO x N y. Functions as a body.
- the polysilazane is not particularly limited, but is preferably a compound which is converted to silica by being ceramicized at a relatively low temperature in consideration of performing the modification treatment.
- a compound which is converted to silica by being ceramicized at a relatively low temperature in consideration of performing the modification treatment.
- JP-A-8-112879 A compound having a main skeleton composed of units represented by the general formula:
- R 1 , R 2 , and R 3 each independently represent a hydrogen atom, an alkyl group, an alkenyl group, a cycloalkyl group, an aryl group, an alkylsilyl group, an alkylamino group, or an alkoxy group. .
- the polysilazane is particularly preferably a perhydropolysilazane (hereinafter also referred to as “PHPS”) in which all of R 1 , R 2 , and R 3 are hydrogen atoms from the viewpoint of the denseness of the resulting gas barrier inorganic layer. .
- PHPS perhydropolysilazane
- Perhydropolysilazane is presumed to have a linear structure and a ring structure centered on 6- and 8-membered rings. Its molecular weight is about 600 to 2000 (polystyrene conversion) in terms of number average molecular weight (Mn), and may be a liquid or solid substance depending on the molecular weight.
- Mn number average molecular weight
- a commercially available product may be used, and examples of the commercially available product include Aquamica NN120, NN110, NAX120, NAX110, NL120A, NL110A, NL150A, NP110, NP140 (manufactured by AZ Electronic Materials Co., Ltd.) and the like. It is done.
- a silicon alkoxide-added polysilazane obtained by reacting a polysilazane represented by the above general formula with a silicon alkoxide (for example, JP-A-5-238827), glycidol is reacted.
- glycidol-added polysilazane eg, JP-A-6-122852
- alcohol-added polysilazane eg, JP-A-6-240208
- metal carboxylate Metal silicic acid salt-added polysilazane for example, JP-A-6-299118
- acetylacetonate complex-added polysilazane obtained by reacting a metal-containing acetylacetonate complex
- metal Add fine particles The resulting metal particles added polysilazane (e.g., JP-A-7-196986 publication), and the like.
- the inorganic substance is not particularly limited as long as it has gas barrier properties, but is preferably an inorganic substance produced by modifying the polysilazane, for example, silicon oxide, silicon nitride, silicon oxynitride or the like. Since the inorganic substance obtained by modifying polysilazane forms a denser gas barrier inorganic layer, it can have a high barrier property.
- the gas barrier inorganic layer may be a single layer or a laminate of two or more layers, but is preferably a laminate of two or more layers. According to the gas barrier inorganic layer laminated two or more layers, it is possible to prevent water vapor permeation due to defects that may exist from the initial stage of production of the gas barrier film. When two or more gas barrier inorganic layers are laminated, each layer may be composed of the same component or a layer composed of different components. Moreover, the gas barrier inorganic layer may be formed on both surfaces of the substrate.
- the film thickness of the gas barrier inorganic layer is preferably 1 nm to 10 ⁇ m, more preferably 10 nm to 5000 ⁇ m, and most preferably 100 to 1000 nm.
- the gas barrier inorganic layer having a thickness of 1 nm or more is preferable because it can have a sufficient gas barrier property.
- the gas barrier inorganic layer has a thickness of 10 ⁇ m or less because cracks are unlikely to occur in the gas barrier inorganic layer.
- two or more gas barrier inorganic layers are laminated
- each film thickness is in the above range.
- the hybrid layer has a function of imparting bending resistance and stability under high temperature and high humidity to the functional inorganic layer.
- the hybrid layer includes polysiloxane and resin fine particles.
- Polysiloxane Polysiloxane has a function of imparting constant heat resistance and film strength to the hybrid layer.
- the polysiloxane that can be used is not particularly limited, but is preferably a polysiloxane formed from an alkoxysilane compound or a polyalkoxysilane compound.
- the alkoxysilane compound is not particularly limited, but is usually an alkoxysilane compound not containing an amino group and an epoxy group, and it is preferable to use a compound represented by the following general formula (1).
- R 4 s may be the same or different, and may be a C1-C6 alkyl group, an alkenyl group such as a vinyl group, an aryl group such as a phenyl group, a methacryloxy group, an isocyanate group, or a ureido.
- R 5 is a C1-C4 alkyl group, and m is 0, 1, or 2.
- the trifunctional alkoxysilane is not particularly limited, but methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, hexyltrimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, vinyl Trimethoxysilane, vinyltriethoxysilane, ⁇ -methacryloxypropyltrimethoxysilane, 3-isocyanatopropyltrimethoxysilane, blocked isocyanate trimethoxysilane blocked with 2-butanooxime, etc., ureidopropyltriethoxysilane , Trifluoropropyltrimethoxysilane, trifluoropropyltriethoxysilane, and the like.
- tetrafunctional alkoxysilane examples include tetramethoxysilane, tetraethoxysilane, tetra-n-propoxysilane, tetraisopropoxysilane, tetra-n-butoxysilane, tetraisobutoxysilane and the like.
- the polyalkoxysilane compound may be a compound in which at least two alkoxysilane compounds described above are bonded through a siloxane bond (Si—O bond).
- Specific examples include polyalkoxysilane compounds (alkoxysilicate compounds) such as silicate 40, silicate 45, silicate 48, M silicate 51, and MTMS-A (manufactured by Tama Chemical Co., Ltd.).
- the resin fine particles have a function of imparting a certain flexibility to the hybrid layer and capturing a low-molecular compound generated from a resin base material, polysiloxane, or the like.
- the resin fine particles that can be used are not particularly limited, but (meth) acrylic ester resin fine particles and styrene resin fine particles are preferable.
- the (meth) acrylic ester resin fine particles and the styrene resin fine particles can be produced by polymerizing raw material monomers, respectively.
- the polymerization method is not particularly limited, and can be produced by a known method such as emulsion polymerization, bulk polymerization, solution polymerization, suspension polymerization and the like.
- emulsion polymerization can be performed by adding a polymerization initiator to water containing a raw material monomer and a surfactant under stirring.
- a known monomer can be used as the raw material monomer.
- raw material monomers that can be used in the production of (meth) acrylic ester resin fine particles, methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, n-butylene (meth) ) Acrylate, t-butyl (meth) acrylate, pentyl (meth) acrylate, isopentyl (meth) acrylate, n-hexyl (meth) acrylate, 2-methylpenter (meth) acrylate, 3-methylpenteracrylate, 4-methylpenter Acrylate, cyclohexyl (meth) acrylate, phenyl (meth) acrylate, 2,3-dimethylbutyl (meth) acrylate, 2,2-dimethylbutyl (meth) acrylate, 3,3-dimethylbutyl (meth) acrylate, 2-methylhex (Met
- the raw material monomer may be polymerized together with a copolymerizable monomer to produce (meth) acrylate resin fine particles and ester resin fine particles.
- the monomer copolymerizable with the raw material monomer is not particularly limited, but (meth) acrylates having an oxyethylene unit such as polyethylene glycol monomethacrylate, polyethylene glycol monoacrylate, methoxypolyethylene glycol monomethacrylate, and methoxypolyethylene glycol monoacrylate.
- the above-mentioned raw material monomers can be used alone or in admixture of two or more.
- the resulting resin fine particles are random copolymers, alternating Any of a copolymer, a block copolymer, and a graft copolymer may be sufficient.
- the solvent, surfactant, polymerization initiator, and the like that can be used in producing the resin fine particles can be appropriately selected by those skilled in the art based on the common general technical knowledge in the technical field.
- the average particle diameter of the resin fine particles is not particularly limited, but is preferably 1 to 200 nm, and preferably 10 to 100 nm. It is preferable that the average particle diameter of the resin fine particles is 1 nm or more because it can contribute to the adhesion to the resin base material. On the other hand, it is preferable that the average particle diameter of the resin fine particles is 200 nm or less because the smoothness of the surface can be maintained.
- the “average particle diameter” is the average value of the particle diameters measured by observing the cross section of the hybrid layer with a TEM (transmission electron microscope) and selecting 10 arbitrary resin fine particles. Shall be adopted.
- the average particle diameter of the resin fine particles can be controlled by reaction conditions when polymerizing the resin.
- the average particle diameter of the resin fine particles is controlled by appropriately adjusting the reaction conditions such as the amount of an additive such as a polymerization initiator and the polymerization temperature. be able to.
- the hybrid layer may be a single layer or a laminate of two or more layers. When two or more layers are laminated, each layer may be composed of the same component or different components. Moreover, a hybrid layer may be formed on both surfaces of a base material.
- the hybrid layer has heat resistance because it contains polysiloxane.
- the hybrid layer contains resin fine particles together with polysiloxane, it can have a suitable film strength, that is, an intermediate film strength between the resin base material and the functional inorganic film.
- the hybrid layer includes both polysiloxane that is an inorganic substance and resin fine particles that are an organic substance, both the organic layer and the inorganic layer can have high adhesiveness.
- the hybrid layer contains resin fine particles, it can have a low molecular compound trapping function.
- the hybrid layer when the hybrid layer exists between a flexible resin base material and a functional inorganic layer having high hardness, the hybrid layer has an intermediate film strength between the resin base material and the functional inorganic layer. And since it has high adhesiveness in both the resin base material which is an organic substance, and the functional inorganic layer which is an inorganic substance, peeling of a functional inorganic layer and generation
- the functional film when the hybrid layer is disposed on the surface of the functional inorganic layer opposite to the resin base material, the functional film has a high adhesiveness with the functional inorganic layer of the hybrid layer and suitable film strength. Expansion of defects such as pinholes in the functional inorganic layer that can occur during bending or under high temperature and high humidity can be suppressed. Moreover, deterioration of the performance of the functional inorganic film can be suppressed by the ability of the hybrid layer to capture the low molecular weight compound.
- the film strength of the hybrid layer can be adjusted by the content of resin fine particles contained in the hybrid layer.
- the content of the resin fine particles is preferably 0.5 to 70% by volume, and more preferably 1 to 50% by volume with respect to the total volume of the hybrid layer.
- required from the cross-sectional observation by TEM (transmission electron microscope) shall be employ
- the film thickness of the hybrid layer is preferably 10 nm to 100 ⁇ m, more preferably 100 nm to 10 ⁇ m.
- the hybrid layer is 10 nm or more, it is preferable because sufficient bending resistance and stability at high temperature and high humidity can be imparted to the functional film.
- the hybrid layer is 100 ⁇ m or less, it is preferable because flexibility can be maintained.
- two or more hybrid layers are laminated
- a hybrid layer is formed on both surfaces, it is preferable that each film thickness exists in the said range.
- the ratio of the film thickness of the functional inorganic layer to the film thickness of the hybrid layer is preferably 0.001 to 10, more preferably 0.01 to 2, and further preferably 0.1 to 1.0.
- the film thickness ratio is within the above range, the resin fine particles in the siloxane matrix contained in the hybrid layer and the hydroxy groups and free radicals that may be present in the functional inorganic layer are firmly bonded to each other, so that the hybrid It is preferable because the effect of improving the interlayer adhesion between the layer and the functional inorganic layer can be suitably obtained.
- the function of the above-mentioned hybrid layer is more suitably exhibited.
- the functional film obtained can have excellent bending resistance and stability at high temperature and high humidity.
- the hybrid layer may further contain an aminosilane compound, an epoxysilane compound, colloidal silica, or the like.
- Aminosilane compound An aminosilane compound can improve adhesion and scratch resistance by being contained in the hybrid layer.
- the aminosilane compound is not particularly limited, but is usually an amino group-containing alkoxysilane compound not containing an epoxy group, and it is preferable to use a compound represented by the following general formula (2).
- R 6 s may be the same or different and each comprises a C1-C4 alkyl group, an alkenyl group such as a vinyl group, an aryl group such as a phenyl group, a methacryloxy group, and an amino group.
- R 5 is a C1-C4 alkyl group, and n is 1 or 2.
- Epoxysilane compound An epoxysilane compound can improve adhesion, scratch resistance, and film formability by being contained in a hybrid layer.
- the epoxysilane compound is not particularly limited, but is usually an epoxy group-containing alkoxysilane compound that does not contain an amino group, and it is preferable to use a compound represented by the following general formula (3).
- R 7 s may be the same or different from each other, and are C1-C4 alkyl groups, alkenyl groups such as vinyl groups, aryl groups such as phenyl groups, methacryloxy groups, glycidoxy groups, and 3 A C1-C3 alkyl group substituted with at least one substituent selected from the group consisting of epoxycycloalkyl groups such as 1,4-epoxycyclohexyl group, wherein at least one of R 7 is glycidoxy A C1-C3 alkyl group substituted with a group or an epoxycycloalkyl group, R 5 is a C1-C4 alkyl group, and n is 1 or 2.
- Colloidal silica can improve scratch resistance by being contained in the hybrid layer.
- Colloidal silica is usually a colloidal suspension of silicon oxide having a Si—OH group on its surface by hydration in water, and is also called colloidal silica or colloidal silicic acid.
- the colloidal silica is not limited to colloidal silica dispersed in water, but includes various colloidal silicas such as non-aqueous dispersions, fine powdered colloidal silica prepared by a gas phase method, and polymerized colloidal silica formed with a siloxane bond. There is a form.
- the particle surface of the colloidal silica is porous, and the colloidal silica dispersed in water is usually negatively charged.
- the colloidal silica may be one prepared by itself or one commercially available.
- a method for preparing colloidal silica known methods can be appropriately referred to.
- colloidal silica in water dispersion can be prepared by adding hydrochloric acid to an aqueous solution of sodium silicate.
- examples of commercially available colloidal silica include ultra-high-purity colloidal silica, Quattron PL series (PL-1, PL-3, PL-7) (manufactured by Fuso Chemical Industry Co., Ltd.), and high-purity organosol (manufactured by Fuso Chemical Industry Co., Ltd.).
- Aqueous silica sol (Snowtex 20, Snowtex 30, Snowtex 40, Snowtex O, Snowtex O-40, Snowtex C, Snowtex N, Snowtex S, Snowtex 20L, Snowtex OL) (Nissan Chemical) Manufactured by Kogyo Co., Ltd.), organosilica sol (methanol silica sol, MA-ST-MS, IPA-ST, IPA-ST-MS, IPA-ST-L, IPA-ST-ZL, IPA-ST-UP, EG-ST, NPC-ST-30, MEK-ST, MEK-ST-MS, MIBK ST, XBA-ST, PMA-ST, DMAC-ST) (manufactured by Nissan Chemical Industries, Ltd.) and the like.
- organosilica sol methanol silica sol, MA-ST-MS, IPA-ST, IPA-ST-MS, IPA-ST-L, IPA-ST-ZL, IPA-ST-UP, EG-ST, NPC-ST-30,
- the average particle size of the colloidal silica is preferably 200 nm or less.
- a resin base material a functional inorganic layer located on the resin base material, and a hybrid layer disposed on at least one surface of the functional inorganic layer
- a method for producing a functional film includes a step (1) of applying the first coating liquid containing polysiloxane and resin fine particles to form the hybrid layer.
- Step (1) is a step of forming the hybrid layer by applying a first coating liquid containing polysiloxane and resin fine particles.
- the first coating liquid may be applied on the resin base material and / or the functional inorganic layer.
- the first coating liquid contains polysiloxane and resin fine particles.
- the polysiloxane and the resin fine particles may be the same as those in the first embodiment.
- the first coating liquid may further contain an aminosilane compound, an epoxysilane compound, colloidal silica, a solvent, and a curing catalyst.
- aminosilane compound As the aminosilane compound, the epoxysilane compound, and the colloidal silica, the same ones as in the first embodiment can be used.
- the polysiloxane contained in the hybrid layer may be formed from an alkoxysilane compound or a polyalkoxysilane compound as described above, the polysiloxane is contained in the first coating solution together with the polysiloxane and / or polysiloxane.
- an alkoxysilane compound and / or a polyalkoxysilane compound may be contained, and a polysiloxane may be prepared in the process (1).
- the alkoxysilane compound and the polyalkoxysilane compound that can be used may be the same as those described in the first embodiment.
- Solvent The solvent that can be contained in the first coating liquid is not particularly limited, and examples thereof include water, alcohol solvents, aromatic hydrocarbon solvents, ether solvents, ketone solvents, and ester solvents.
- Alcohol solvents include methanol, ethanol, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, sec-butyl alcohol, tert-butyl alcohol, n-hexyl alcohol, n-octyl alcohol, ethylene glycol, diethylene glycol, triethylene Examples include glycol, ethylene glycol monobutyl ether, ethylene glycol monoethyl ether acetate, diethylene glycol monoethyl ether, propylene glycol monomethyl ether, propylene monomethyl ether acetate, diacetone alcohol, methyl cellosolve, ethyl cellosolve, propyl cellosolve, and butyl cellosolve.
- Examples of the aromatic hydrocarbon solvent include toluene and xylene.
- Examples of ether solvents include tetrahydrofuran, 1,4-dioxane, 1,2-dimethoxyethane and the like.
- Examples of the ketone solvent include cyclohexanone, acetone, methyl ethyl ketone, and methyl isobutyl ketone.
- Examples of the ester solvent include methyl acetate, ethyl acetate, ethoxyethyl acetate and the like.
- solvents such as dichloroethane and acetic acid may be used. These solvents can be used alone or in admixture of two or more.
- the curing catalyst is a catalyst for hydrolyzing and condensing (curing) the silane compound contained in the first coating solution.
- an inorganic acid an organic acid, an organic metal salt, a Lewis acid, etc.
- inorganic acids include hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, nitrous acid, perchloric acid, sulfamic acid, and the like.
- organic acid include formic acid, acetic acid, propionic acid, butyric acid, oxalic acid, succinic acid, maleic acid, lactic acid, p-toluenesulfonic acid, and citric acid.
- Organic metal salts include lithium hydroxide, sodium hydroxide, potassium hydroxide, n-hexylamine, dimethylamine, tributylamine, diazabicycloundecene, ethanolamine acetate, dimethylaniline formate, tetraethylammonium benzoate, acetic acid Examples thereof include sodium, potassium acetate, sodium propionate, potassium propionate, sodium formate, potassium formate, benzoyltrimethylammonium acetate, tetramethylammonium acetate, tin octylate and the like.
- Lewis acids examples include tetraisopropyl titanate, tetrabutyl titanate, aluminum triisobutoxide, aluminum triisopropoxide, aluminum acetylacetonate, tin chloride (SnCl 4 ), titanium chloride (TiCl 4 ), and zinc chloride (ZnCl 4 ).
- the coating liquid can be highly dispersed even when the content of organic fine particles that can be contained in the first coating liquid together with the silane compound is increased, and from the viewpoint of improving the transparency of the resulting hybrid layer, organic It is preferable to use an acid, more preferably an organic carboxylic acid, and even more preferably acetic acid.
- These curing catalysts may be used alone or in combination of two or more.
- the hybrid layer is formed by applying the first coating liquid on the resin substrate or the functional inorganic layer.
- a coating method of the first coating solution a known method can be adopted as appropriate. Specific examples include spin coating methods, roll coating methods, flow coating methods, ink jet methods, spray coating methods, printing methods, dip coating methods, cast film forming methods, bar coating methods, and gravure printing methods.
- the coating amount of the first coating liquid is not particularly limited, but can be appropriately adjusted so as to be the desired thickness of the hybrid layer.
- drying / curing conditions are not particularly limited, but it is usually preferable to dry and cure at 80 to 190 ° C., preferably 100 to 140 ° C., for 10 minutes to 24 hours, preferably 30 minutes to 3 hours.
- the coating film or hybrid layer obtained in step (1) may be subjected to vacuum ultraviolet irradiation performed in step (2) described later.
- the manufacturing method of the functional film which concerns on 2nd Embodiment apply coats the 2nd coating liquid containing an inorganic precursor further, forms a coating film, modifies the said coating film, and forms a functional inorganic layer. You may have the process (2) to form.
- the functional inorganic layer according to this embodiment includes a physical vapor deposition method (PVD method) in which a metal, an oxide, or the like is evaporated to form a film on a substrate, a source gas (for example, an organosilicon compound typified by tetraethoxysilane (TEOS))
- PVD method physical vapor deposition method
- TEOS tetraethoxysilane
- CVD method chemical vapor deposition method
- Si metal silicon
- it is preferably a functional inorganic layer formed by the step (2).
- Step (2) is a step of applying a second coating liquid containing an inorganic precursor to form a coating film, and modifying the coating film to form a functional inorganic layer.
- the second coating liquid may be applied on the resin substrate and / or on the hybrid layer.
- the hybrid layer and the functional inorganic layer are impregnated with the second coating solution up to the inside of the hybrid layer due to the low molecular compound capturing function of the hybrid layer. This is preferable because the adhesion to the substrate is further improved.
- the second coating liquid contains an inorganic precursor.
- the inorganic precursor is not particularly limited, but polysilazane is preferably used.
- the same polysilazane as in the first embodiment can be used.
- the content of polysilazane in the second coating liquid varies depending on the desired functional inorganic layer thickness, pot life of the coating liquid, etc., but is 0.2% by mass relative to the total amount of the second coating liquid. It is preferable that the content be 35% by mass.
- the second coating solution may further contain an amine catalyst, a metal, and a solvent.
- Amine catalyst and metal The amine catalyst and metal can promote the conversion of polysilazane to a silicon oxide compound in the modification treatment described below.
- amine catalysts include N, N, N ′, N′-tetramethyl-1,6-diaminohexane.
- palladium is mentioned as a metal.
- the amine catalyst and the metal are preferably contained in an amount of 0.1 to 10 mass in the first coating solution with respect to polysilazane.
- the amine catalyst is more preferably contained in the first coating solution in an amount of 0.5 to 5% by mass with respect to polysilazane from the viewpoint of improving the coating property and shortening the reaction time.
- the solvent that can be contained in the second coating solution is not particularly limited as long as it does not react with polysilazane, and a known solvent can be used.
- a known solvent can be used.
- Specific examples include hydrocarbon solvents such as aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, and halogenated hydrocarbons; ether solvents such as aliphatic ethers and alicyclic ethers. More specifically, examples of the hydrocarbon solvent include pentane, hexane, cyclohexane, toluene, xylene, solvesso, turben, methylene chloride, trichloroethane, and the like. Examples of ether solvents include dibutyl ether, dioxane, and tetrahydrofuran. These solvents can be used alone or in admixture of two or more.
- a functional inorganic layer is formed by applying a second coating liquid to form a coating film and modifying the coating film.
- the second coating liquid may be applied on a resin base material or a hybrid layer.
- Second Coating Solution As a method for applying the second coating solution, a known method can be adopted as appropriate. Specific examples include spin coating methods, roll coating methods, flow coating methods, ink jet methods, spray coating methods, printing methods, dip coating methods, cast film forming methods, bar coating methods, and gravure printing methods.
- the coating amount of the second coating solution is not particularly limited, but can be appropriately adjusted so as to have the desired thickness of the functional inorganic layer.
- the second coating solution After applying the second coating solution, it is preferable to dry, and annealing is more preferable from the viewpoint of obtaining a uniform coating film.
- the annealing temperature is not particularly limited, but is preferably 60 to 200 ° C, and more preferably 70 to 160 ° C.
- the annealing temperature may be constant, may be changed stepwise, or may be continuously changed (temperature increase and / or temperature decrease).
- the annealing time is not particularly limited, but is preferably 5 seconds to 24 hours, and more preferably 10 seconds to 2 hours.
- the modification of the coating film means that the inorganic precursor constituting the coating film is converted.
- the inorganic precursor constituting the coating film is converted.
- polysilazane contained in the coating film when converted, it can be converted into a silicon oxide compound and / or a silicon oxynitride compound.
- the modification treatment of the coating film can be performed by irradiating ultraviolet rays in an oxidizing gas atmosphere and a low humidity environment.
- a functional inorganic layer having a desired composition by irradiating ultraviolet rays, or active oxygen and / or ozone generated from oxygen in an oxidizing gas atmosphere caused by ultraviolet rays causes an oxidation reaction to the inorganic precursor.
- ozone generated from oxygen is insufficient, ozone may be separately generated by a known method such as a discharge method and introduced into a reaction vessel in which reforming treatment is performed.
- the wavelength of the ultraviolet rays to be irradiated is not particularly limited, but is preferably 10 to 450 nm, more preferably 100 to 300 nm, further preferably 100 to 200 nm, and particularly preferably 100 to 180 nm. .
- ultraviolet light having a high energy of 200 nm or less is particularly referred to as “vacuum ultraviolet light (VUV light)”.
- the ultraviolet rays to be irradiated are preferably vacuum ultraviolet rays from the viewpoint of proceeding the conversion reaction at a lower temperature and in a shorter time.
- the conversion reaction is likely to proceed, and the conversion of oxygen to active oxygen or ozone is also easily performed, so that the conversion reaction can be performed efficiently.
- the functional inorganic film obtained becomes denser and the functional inorganic layer can have high performance.
- the ultraviolet light source is not particularly limited, and a low-pressure mercury lamp, a deuterium lamp, a xenon excimer lamp, a metal halide lamp, an excimer laser, or the like can be used. Among these, it is preferable to use a rare gas excimer lamp such as a xenon excimer lamp.
- the output of the lamp is preferably 400 W to 30 kW.
- the illuminance is preferably 1 mW / cm 2 to 100 kW / cm 2 , and more preferably 1 mW / cm 2 to 10 W / cm 2 .
- the irradiation energy is preferably 10 ⁇ 10000mJ / cm 2, more preferably 100 ⁇ 8000mJ / cm 2.
- a rare gas excimer lamp such as the xenon excimer lamp can irradiate vacuum ultraviolet rays.
- a rare gas atom such as Xe, Kr, Ar, Ne or the like is called an inert gas because it is chemically very inert because the outermost electrons are closed.
- a rare gas atom excited atom
- the rare gas is xenon, e + Xe ⁇ Xe * Xe * + 2Xe ⁇ Xe 2 * + Xe Xe 2 * ⁇ Xe + Xe + h ⁇ (172 nm) It becomes.
- excimer light (vacuum ultraviolet light) of 172 nm is emitted.
- the excimer lamp uses the excimer light. Examples of the method for obtaining the excimer light emission include a method using dielectric barrier discharge and a method using electrodeless field discharge.
- a dielectric barrier discharge is a lightning generated in a gas space when a gas space is arranged between both electrodes via a dielectric (transparent quartz in the case of an excimer lamp) and a high frequency high voltage of several tens of kHz is applied to the electrode. Is a very thin discharge called micro discharge.
- the micro discharge streamer reaches the tube wall (dielectric)
- charges accumulate on the surface of the dielectric, and the micro discharge disappears.
- the micro discharge spreads over the entire wall of the tube and repeats generation / extinction, resulting in flickering of light that can be seen with the naked eye.
- a very high temperature streamer reaches a pipe wall directly locally, there is a possibility that deterioration of the pipe wall may be accelerated.
- the electrodeless field discharge is an electrodeless field discharge due to capacitive coupling, and is also called an RF discharge.
- a lamp, an electrode, and the like are arranged in the same manner as the dielectric barrier discharge, and the high frequency applied between the electrodes is uniform in space and time when a high frequency voltage of several MHz is applied. Discharge. In the method using the electrodeless electric field discharge, there is no flicker and a long-life lamp can be obtained.
- dielectric barrier discharge micro discharge occurs only between the electrodes, so that the outer electrode covers the entire outer surface and transmits light to extract light to the outside in order to discharge in the entire discharge space.
- the external electrode a net-like electrode using a thin metal wire so as not to block light can be used.
- the external electrode can be damaged by ozone generated by irradiation with vacuum ultraviolet rays. Therefore, in order to prevent damage to the electrodes, it is necessary to provide an atmosphere of an inert gas such as nitrogen around the lamp, that is, the inside of the irradiation apparatus, and provide a synthetic quartz window to extract the irradiation light.
- the outer diameter of the double cylindrical lamp is about 25 mm, the difference in the distance to the irradiation surface cannot be ignored between the position directly below the lamp axis and the side surface of the lamp, and a large difference in illuminance occurs depending on the distance. sell. Therefore, even if the lamps are closely arranged, a uniform illuminance distribution is not always obtained. If the irradiation device is provided with a synthetic quartz window, the distance in the oxygen atmosphere can be made uniform, and a uniform illuminance distribution can be obtained. However, the synthetic quartz window is not only an expensive consumable, but can also cause light loss.
- the external electrode in the case of electrodeless electric field discharge, it is not necessary to form the external electrode in a mesh shape, and glow discharge can spread over the entire discharge space only by providing the external electrode on a part of the outer surface of the lamp.
- an electrode that also serves as a light reflector usually made of an aluminum block, can be used on the back of the lamp.
- synthetic quartz is required to obtain a uniform illuminance distribution.
- the biggest feature of the capillary excimer lamp is its simple structure.
- the quartz tube is closed at both ends, and only gas for excimer light emission is sealed inside.
- the outer diameter of the tube of the thin tube lamp is preferably 6 to 12 mm. If it is too thick, a high voltage is required for starting.
- the form of discharge may be dielectric barrier discharge or electrodeless field discharge.
- the electrode may have a flat surface in contact with the lamp, but the lamp can be firmly fixed by making the shape in accordance with the curved surface of the lamp, and the discharge can be more stable when the electrode is in close contact with the lamp. . Also, if the curved surface is made of aluminum, it can function as a light reflector.
- Such an excimer light (vacuum ultraviolet) irradiation device can use a commercially available lamp (for example, manufactured by USHIO INC.).
- Excimer lamps are characterized in that excimer light is concentrated at one wavelength and almost no light other than the necessary light is emitted, and is highly efficient. Moreover, since excess light is not radiated
- the Xe excimer lamp is excellent in luminous efficiency because it emits a short wavelength 172 nm vacuum ultraviolet ray at a single wavelength. Since the Xe excimer lamp has a short wavelength of 172 nm and high energy, it is known that the cutting ability of organic compounds is high.
- the Xe excimer lamp since the Xe excimer lamp has a large oxygen absorption coefficient, it can efficiently generate active oxygen and ozone even with a very small amount of oxygen. Therefore, for example, in contrast to a low-pressure mercury lamp that emits vacuum ultraviolet light having a wavelength of 185 nm, the Xe excimer lamp has a high bond breaking ability of organic compounds, can efficiently generate active oxygen and ozone, and has a low temperature.
- the polysilazane layer can be modified in a short time.
- the Xe excimer lamp has high light generation efficiency, so it can be turned on and off instantaneously with low power, and can emit a single wavelength, thereby shortening process time and equipment area associated with high throughput. It is also preferable from the viewpoints of the economic viewpoint and application to a functional film using a base material that is easily damaged by heat.
- the excimer lamp since the excimer lamp has high light generation efficiency, it can be turned on with low power, and an increase in the surface temperature of the irradiation object can be suppressed. Further, since the number of photons penetrating to the inside increases, the modified film thickness can be increased and / or the film quality can be increased. However, if the irradiation time is too long, the flatness may be deteriorated or other materials of the functional film may be adversely affected. In general, the conversion reaction is examined using the integrated light quantity represented by the product of the irradiation intensity and the irradiation time as an index, but materials having various structural forms are used even if the composition is the same, such as silicon oxide. In some cases, the absolute value of the irradiation intensity may be important.
- the conversion reaction when the conversion reaction is performed by irradiation with vacuum ultraviolet rays, it is preferable to give a maximum irradiation intensity of 100 to 200 mW / cm 2 at least once. It is preferable that the maximum irradiation intensity is 100 mW / cm 2 or more because the reforming efficiency is improved and the conversion reaction can proceed in a short time. On the other hand, it is preferable that the maximum irradiation intensity is 200 mW / cm 2 or less because deterioration of the functional film and deterioration of the lamp itself can be suppressed.
- the irradiation time of the vacuum ultraviolet ray is not particularly limited, but the irradiation time in the high illuminance process is preferably 0.1 second to 3 minutes, and more preferably 0.5 second to 1 minute.
- the oxygen concentration at the time of vacuum ultraviolet irradiation is preferably 500 to 10000 ppm (1%), more preferably 1000 to 5000 ppm. It is preferable that the oxygen concentration is 500 ppm or more because the reforming efficiency becomes high. On the other hand, when the oxygen concentration is 10,000 ppm or less, the substitution time between the atmosphere and oxygen can be shortened, which is preferable.
- the coating film to be irradiated with ultraviolet rays is mixed with oxygen and a small amount of moisture at the time of application, and adsorbed oxygen and adsorbed water may also exist in the substrate and adjacent layers. If oxygen or the like is used, the oxygen source required for generation of active oxygen or ozone for performing the reforming process may be sufficient without newly introducing oxygen into the irradiation chamber. In addition, since 172 nm vacuum ultraviolet rays such as Xe excimer lamps are absorbed by oxygen, the amount of vacuum ultraviolet rays reaching the coating film may decrease. Therefore, when irradiating vacuum ultraviolet rays, the oxygen concentration is set low, It is preferable that the vacuum ultraviolet rays can reach the coating film efficiently.
- the gas other than oxygen in the vacuum ultraviolet irradiation atmosphere is preferably a dry inert gas, and more preferably dry nitrogen gas from the viewpoint of cost.
- the oxygen concentration can be adjusted by measuring the flow rate of oxygen gas, inert gas, or the like introduced into the irradiation chamber and changing the flow rate ratio.
- the generated vacuum ultraviolet light may be irradiated to the polysilazane layer before modification after reflecting the vacuum ultraviolet light from the generation source with a reflector.
- vacuum ultraviolet irradiation can be applied to both batch processing and continuous processing, and can be appropriately selected depending on the shape of the substrate to be coated. For example, when the substrate is in the form of a long film, it is preferable to perform modification by continuously irradiating with vacuum ultraviolet rays while transporting the substrate.
- the reforming treatment is preferably performed in combination with heat treatment. By combining the heat treatment, the conversion reaction can be promoted.
- the heating method is not particularly limited, and a method of heating a coating film by contacting a substrate with a heating element such as a heat block, a method of heating an atmosphere by an external heater such as a resistance wire, an IR heater, etc. Examples include a method using light in the infrared region. These methods can be appropriately selected from the viewpoint of the smoothness of the coating film.
- the temperature of the heat treatment is not particularly limited, but is preferably 50 to 200 ° C, more preferably 80 to 150 ° C.
- the heating time is preferably 1 second to 10 hours, more preferably 10 seconds to 1 hour.
- dew point temperature means a temperature at which condensation starts when air containing water vapor is cooled, and serves as an index representing the amount of moisture in the atmosphere.
- the dew point temperature can be usually measured by directly measuring with a dew point thermometer.
- the water vapor pressure may be obtained from the temperature and relative humidity, and the temperature at which the water vapor pressure is the saturated water vapor pressure may be calculated. In this case, when the relative humidity is 100%, the measurement temperature is the dew point temperature.
- the film thickness, density, etc. of the functional inorganic layer obtained by the above-described modification treatment should be appropriately selected from coating conditions, ultraviolet intensity, irradiation time, wavelength (light energy density), irradiation method, heating temperature, and the like. Can be controlled.
- the film thickness, density, etc. of the functional inorganic layer can be controlled by appropriately selecting the irradiation method of ultraviolet rays from continuous irradiation, irradiation divided into a plurality of times, and so-called pulse irradiation, etc., in which the irradiation of the plurality of times is short. Can be done.
- the formed functional inorganic layer is subjected to XPS surface analysis to obtain each atomic composition ratio of silicon (Si) atoms, nitrogen (N) atoms, oxygen (O) atoms, etc. I can confirm.
- the functional inorganic layer may be a single layer or a laminate of two or more layers. From the viewpoint of efficiently repairing defects caused by foreign matter and nano-level defects such as pinholes, it is preferable to laminate two or more functional inorganic layers.
- each layer may be the same or different.
- the second layer upper layer
- the step (2) is preferably formed by the step (2). The reason for this is that by performing a modification process on the leveled coating film, it is possible to repair the functional inorganic layer with a smooth surface after filling small holes, so that water vapor transmission due to defects existing from the beginning can be prevented. This is because it can be prevented.
- the electronic device containing an electronic device main body and the above-mentioned functional film is provided.
- the functional film described above can be suitably applied to an electronic device because it is excellent in bending resistance and stability under high temperature and high humidity.
- the electronic device is not particularly limited, and examples thereof include a liquid crystal display element (LCD), a solar cell (PV), and organic electroluminescence (EL).
- LCD liquid crystal display element
- PV solar cell
- EL organic electroluminescence
- the use of the functional film is not particularly limited, it can be used as a constituent element of a substrate constituting an electronic device body and a sealing material for sealing the electronic device. Among these, it is preferable to use as a sealing material.
- FIG. 4 is a schematic cross-sectional view of an organic EL panel according to an embodiment.
- the organic EL panel 40 includes a functional film 41, an anode 42 that is a transparent electrode formed on the functional film 41, an organic EL layer 43 formed on the anode 42, and the organic EL layer 43. And a sealing member 46 made of an aluminum foil formed through an adhesive layer 45 so as to cover the organic EL layer 43 and the cathode 44.
- the organic EL layer 43 and the cathode 44 are collectively referred to as an organic EL element.
- the anode 42 can be a part of the organic EL element.
- the functional film 41 according to the present embodiment is used for sealing purposes, whereby deterioration of the organic EL element due to water vapor can be suppressed. As a result, the organic EL panel 40 can have a long lifetime.
- the sealing member 46 may be a functional film according to the present invention in addition to a metal film such as an aluminum foil. When a functional film is used for the sealing member 46, it may be attached with an adhesive so that the resin base material constituting the functional film is disposed outside.
- Organic EL element is not particularly limited, but can usually have the following layer structure.
- Anode / light emitting layer / cathode (2) Anode / hole transport layer / light emitting layer / cathode (3) Anode / light emitting layer / electron transport layer / cathode (4) Anode / hole transport layer / light emitting layer / electron Transport layer / cathode (5) Anode / anode buffer layer (hole injection layer) / hole transport layer / light emitting layer / electron transport layer / cathode buffer layer (electron injection layer) / cathode.
- anode Although it does not restrict
- Specific examples include metals such as gold (Au), conductive transparent materials such as copper iodide (CuI), indium tin oxide (ITO), tin oxide (SnO 2 ), and zinc oxide (ZnO).
- an amorphous material such as IDIXO (In 2 O 3 —ZnO) capable of forming a transparent conductive film may be used.
- the anode can be formed as a thin film by a method such as vapor deposition or sputtering of an electrode material. At this time, pattern formation may be performed by photolithography. If high pattern accuracy (about 100 ⁇ m or more) is not required, the pattern may be formed by vapor deposition using a mask or sputtering.
- the transmittance is preferably 10% or more.
- the sheet resistance of the anode is preferably several hundred ⁇ / ⁇ (square) or less.
- the film thickness of the anode is usually 10 to 1000 nm, preferably 10 to 200 nm.
- the cathode is not particularly limited, but it is preferable to use a metal having a small work function (4 eV or less) (hereinafter also referred to as “electron-injecting metal”), an alloy, an electrically conductive compound, and a mixture thereof.
- a metal having a small work function (4 eV or less) hereinafter also referred to as “electron-injecting metal”
- Specific examples include sodium, sodium-potassium alloy, magnesium, lithium, magnesium / copper mixture, magnesium / silver mixture, magnesium / aluminum mixture, magnesium / indium mixture, aluminum / aluminum oxide (Al 2 O 3 ) mixture, indium, Examples include lithium / aluminum mixtures and rare earth metals.
- an electron injectable metal and a metal mixture having a larger work function value than the electron injectable metal and stable such as a magnesium / silver mixture, magnesium / silver
- an aluminum mixture, a magnesium / indium mixture, an aluminum / aluminum oxide (Al 2 O 3 ) mixture, or a lithium / aluminum mixture it is preferable to use an aluminum mixture, a magnesium / indium mixture, an aluminum / aluminum oxide (Al 2 O 3 ) mixture, or a lithium / aluminum mixture.
- the cathode can be formed as a thin film by a method such as vapor deposition or sputtering of an electrode material.
- the sheet resistance of the cathode is preferably several hundred ⁇ / ⁇ or less.
- the film thickness of the cathode is usually 1 nm to 5 ⁇ m, preferably 50 to 200 nm.
- either the anode or the cathode is transparent or translucent in order to transmit the emitted light and obtain excellent emission luminance.
- a cathode having a thickness of 1 to 20 nm from a metal that can be used as the cathode a conductive transparent material that can be used as the anode is produced on the produced cathode, thereby producing a transparent or translucent material.
- a cathode can be made. By applying this, an element in which both the anode and the cathode are transmissive can be manufactured.
- the injection layer has an electron injection layer (cathode buffer layer) and a hole injection layer (anode buffer layer).
- An electron injection layer and a hole injection layer are provided as necessary, and an anode and a light emitting layer or hole transport. It exists between layers and / or between a cathode and a light emitting layer or an electron transport layer.
- the injection layer is a layer provided between the electrode and the organic layer for lowering the driving voltage and improving the light emission luminance.
- the details of the hole injection layer are described in JP-A-9-45479, JP-A-9-260062, JP-A-8-288069, and the like.
- Examples thereof include a phthalocyanine buffer layer typified by phthalocyanine, an oxide buffer layer typified by vanadium oxide, an amorphous carbon buffer layer, and a polymer buffer layer using a conductive polymer such as polyaniline (emeraldine) or polythiophene.
- JP-A-6-325871, JP-A-9-17574, JP-A-10-74586, and the like are described in JP-A-6-325871, JP-A-9-17574, JP-A-10-74586, and the like.
- strontium Metal buffer layer typified by aluminum and aluminum
- alkali metal compound buffer layer typified by lithium fluoride
- alkaline earth metal compound buffer layer typified by magnesium fluoride
- oxide buffer layer typified by aluminum oxide
- the injection layer is preferably a very thin film, and although it varies depending on the material, the film thickness is preferably 0.1 nm to 5 ⁇ m.
- the light emitting layer is a layer that emits light by recombination of electrons and holes injected from the electrode (cathode, anode) or electron transport layer or hole transport layer, and the light emitting portion is within the layer of the light emitting layer. Alternatively, it may be the interface between the light emitting layer and the adjacent layer.
- the light emitting layer preferably contains a dopant compound (light emitting dopant) and a host compound (light emitting host) from the viewpoint of further increasing the light emission efficiency.
- Luminescent dopant Broadly speaking, there are two types of luminescent dopants: fluorescent dopants that emit fluorescence and phosphorescent dopants that emit phosphorescence.
- the fluorescent dopant is not particularly limited, but is a coumarin dye, pyran dye, cyanine dye, croconium dye, squalium dye, oxobenzanthracene dye, fluorescein dye, rhodamine dye, pyrylium dye, perylene. And dyes, stilbene dyes, polythiophene dyes, rare earth complex phosphors, and the like.
- luminescent dopants may be used alone or in combination of two or more.
- the light emitting host is not particularly limited, but has a basic skeleton such as a carbazole derivative, a triarylamine derivative, an aromatic borane derivative, a nitrogen-containing heterocyclic compound, a thiophene derivative, a furan derivative, an oligoarylene compound, a carboline derivative,
- a diazacarbazole derivative here, the diazacarbazole derivative represents one in which at least one carbon atom of the hydrocarbon ring constituting the carboline ring of the carboline derivative is substituted with a nitrogen atom
- carboline derivatives, diazacarbazole derivatives and the like are preferably used.
- the light emitting layer can be formed by depositing the above compound by a known thinning method such as a vacuum deposition method, a spin coating method, a casting method, an LB method, and an ink jet method.
- the thickness of the light emitting layer is not particularly limited, but is usually 5 nm to 5 ⁇ m, preferably 5 to 200 nm.
- the light emitting layer may have a single layer structure composed of one or more dopant compounds and host compounds, or may have a laminated structure composed of a plurality of layers having the same composition or different compositions.
- the hole transport layer is made of a hole transport material having a function of transporting holes.
- the hole injection layer and the electron blocking layer are also included in the hole transport layer.
- the hole transport layer can be provided as a single layer or a plurality of layers.
- the hole transport material is not particularly limited as long as it has any of hole injection or transport and electron barrier properties, and either an organic material or an inorganic material may be used.
- hole transport materials include triazole derivatives, oxadiazole derivatives, imidazole derivatives, polyarylalkane derivatives, pyrazoline derivatives, pyrazolone derivatives, phenylenediamine derivatives, arylamine derivatives, amino-substituted chalcone derivatives, oxazole derivatives, styrylanthracene.
- Examples thereof include conductive polymer oligomers such as derivatives, fluorenone derivatives, hydrazone derivatives, stilbene derivatives, silazane derivatives, aniline copolymers, thiophene oligomers, and porphyrin compounds, aromatic tertiary amine compounds, and styrylamine compounds. Among these, it is preferable to use an aromatic tertiary amine compound.
- a polymer material in which the above material is introduced into a polymer chain or the above material is a polymer main chain may be used.
- inorganic compounds such as p-type-Si and p-type-SiC may be used.
- the hole transport layer can be formed by thinning the above material by a known method such as a vacuum deposition method, a spin coating method, a casting method, a printing method including an inkjet method, or an LB method.
- the thickness of the hole transport layer is not particularly limited, but is usually 5 nm to 5 ⁇ m, preferably 5 to 200 nm.
- the hole transport layer may have a single layer structure composed of one or more of the above materials.
- the electron transport layer is made of an electron transport material having a function of transporting electrons, and in a broad sense, an electron injection layer and a hole blocking layer are also included in the electron transport layer.
- the electron transport layer can be provided as a single layer or a plurality of layers.
- the electron transport material is not particularly limited as long as it has a function of transmitting electrons injected from the cathode to the light emitting layer, and a known compound can be used.
- electron transport materials include nitro-substituted fluorene derivatives, diphenylquinone derivatives, thiopyrandioxide derivatives, carbodiimides, fluorenylidenemethane derivatives, anthraquinodimethane, anthrone derivatives, oxadiazole derivatives, thiadiazole derivatives, quinoxaline derivatives. Etc.
- a polymer material in which the above materials are introduced into a polymer chain or these materials as a polymer main chain can also be used.
- metal complexes of 8-quinolinol derivatives such as tris (8-quinolinol) aluminum (Alq), tris (5,7-dichloro-8-quinolinol) aluminum, tris (5,7-dibromo-8-quinolinol) aluminum Tris (2-methyl-8-quinolinol) aluminum, tris (5-methyl-8-quinolinol) aluminum, bis (8-quinolinol) zinc (Znq), and the like, and the central metals of these metal complexes are In, Mg, A metal complex replaced with Cu, Ca, Sn, Ga, or Pb may be used.
- metal-free or metal phthalocyanine or those having a terminal substituted with an alkyl group or a sulfonic acid group may be used.
- an inorganic semiconductor such as n-type-Si or n-type-SiC, which can be a material for the hole injection layer, may be used.
- the electron transport layer can be formed by thinning the above material by a known method such as a vacuum deposition method, a spin coating method, a casting method, a printing method including an ink jet method, or an LB method.
- the film thickness of the electron transport layer is not particularly limited, but is usually 5 nm to 5 ⁇ m, preferably 5 to 200 nm.
- the electron transport layer may have a single layer structure composed of one or more of the above materials.
- a method for producing an organic EL element will be described by taking an organic EL element composed of an anode / hole injection layer / hole transport layer / light emitting layer / electron transport layer / electron injection layer / cathode as an example.
- a desired electrode material for example, a thin film made of an anode material is formed on the functional film so as to have a film thickness of 1 ⁇ m or less, preferably 10 to 200 nm, for example, by a method such as vapor deposition, sputtering, plasma CVD, An anode is produced.
- an organic compound thin film of a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, and an electron injection layer, which are organic EL element materials, is formed thereon.
- the method for forming the organic compound thin film include a vapor deposition method and a wet process (spin coating method, casting method, ink jet method, printing method), etc., but it is easy to obtain a uniform film and a pinhole is generated. From the viewpoint of being difficult to perform, it is preferable to use a vacuum deposition method, a spin coating method, an ink jet method, or a printing method. At this time, a different film forming method may be applied to each layer.
- the vapor deposition conditions vary depending on the type of compound used, but generally the boat heating temperature is 50 to 450 ° C., and the degree of vacuum is 10 ⁇ 6 to 10 ⁇ 2 Pa.
- the deposition rate is 0.01 to 50 nm / second, the substrate temperature is ⁇ 50 to 300 ° C., and the film thickness is 0.1 to 5 ⁇ m, preferably 5 to 200 nm.
- a thin film made of a cathode material is formed thereon by a method such as vapor deposition or sputtering so as to have a film thickness of 1 ⁇ m or less, preferably 50 to 200 nm.
- An organic EL element can be produced.
- the organic EL device is produced from the anode and the hole injection layer to the cathode consistently by a single vacuum, it may be taken out halfway and subjected to different film forming methods. At this time, it is necessary to consider that the work is performed in a dry inert gas atmosphere. Alternatively, the order of fabrication may be reversed, and the cathode, electron injection layer, electron transport layer, light emitting layer, hole transport layer, hole injection layer, and anode may be fabricated in this order.
- a DC voltage is applied to a multicolor display device (organic EL panel) provided with the organic EL element thus obtained, the anode is set to positive and the cathode is set to negative polarity. Luminescence can be observed when 40V is applied.
- An alternating voltage may be applied. The alternating current waveform to be applied can be selected as appropriate.
- resin base material having an intermediate layer As a resin base material, Cosmo Shine A4300 (manufactured by Toyobo Co., Ltd.), which is a polyester film having a thickness of 100 ⁇ m and easily bonded on both sides, was used as the resin base material.
- a coating solution containing a UV curable organic / inorganic hybrid hard coat material OPSTAR Z7535 manufactured by JSR Corporation was applied with a wire bar so that the film thickness after drying was 4 ⁇ m. .
- the resulting coating film was irradiated with a high-pressure mercury lamp and cured to form a bleed-out prevention layer. Irradiation was performed at 1.0 J / cm 2 at 80 ° C. for 3 minutes in an air atmosphere.
- a polymerization monomer 150 g of a mixed monomer in which ethyl acrylate, methyl methacrylate, and glycidyl methacrylate were mixed at a weight mixing ratio of 60/40/2 was prepared, and 25 g of the mixed monomer was first dispersed and emulsified in the above solution. While maintaining a constant stirring state, an aqueous copper sulfate solution was added so that the copper sulfate concentration was 5.0 ⁇ 10 ⁇ 7 mol / L.
- a sample tube having a volume of 50 g is charged with 2.8 g of the acrylate resin fine particles prepared above, 8.5 g of 1-methoxy-2-propanol, and 3 g of ion-exchanged water.
- 0.3 g, 2 g of tetramethoxysilane as an alkoxysilane compound, and 0.1 g of 20% p-toluenesulfonic acid methanol solution as a curing catalyst were added dropwise in this order over 1 minute. Then, it stirred at room temperature for 10 minutes and made this A liquid.
- the solution A was added dropwise to the solution B over 2 minutes, and then stirred for 30 minutes at 700 rpm at room temperature.
- the first coating solution was prepared by allowing to stand for 1 week in a dark place at 25 ° C.
- Example 1 Formation of Hybrid Layer
- the first coating solution is applied so that the film thickness after drying becomes 1 ⁇ m (1000 nm), at 120 ° C.
- a hybrid layer was formed by heat treatment for 30 minutes.
- a second coating solution was applied on the hybrid layer by a spin coating method and dried at 80 ° C. for 1 minute to form a coating film having a thickness of 300 nm after drying. At this time, the boundary surface for measuring the thickness was confirmed from a cross-sectional photograph of a TEM (Transmission Electron Microscope).
- the functional film in which the resin base material-hybrid layer-functional inorganic layer was laminated in this order was manufactured by subjecting the coating film to a modification treatment by irradiation with vacuum ultraviolet rays (VUV).
- VUV vacuum ultraviolet
- the vacuum ultraviolet (VUV) irradiation uses a stage movable xenon excimer irradiation device MECL-M-1-200 (manufactured by M.D. excimer) as a vacuum ultraviolet irradiation device, and the distance between the lamp and the sample (both Gap). Sample) was set to 3 mm and irradiated under the following conditions.
- Illuminance 140 mW / cm 2 (172 nm)
- Stage temperature 100 ° C
- Stage movable speed and number of times of conveyance 16 times of conveyance at 10 mm / sec.
- Excimer light exposure integrated amount 6000 mJ / cm 2 .
- the irradiation time was adjusted by appropriately changing the movable speed of the movable stage.
- the oxygen concentration at the time of vacuum ultraviolet irradiation measured the flow rate of the nitrogen gas introduced into the irradiation chamber and the oxygen gas with a flow meter, and was adjusted by the nitrogen gas / oxygen gas flow ratio of the gas introduced into the chamber.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the gas barrier film produced in Example 1 is 0.3. .
- Example 2 A functional inorganic layer was formed by the same method as in Example 1 on the surface opposite to the bleed-out prevention layer of the produced resin base material. Further, a hybrid layer is formed on the formed functional inorganic layer in the same manner as in Example 1, and a functional film in which the resin base material-functional inorganic layer-hybrid layer is laminated in this order is manufactured. did.
- Example 3 A hybrid layer is further formed on the functional inorganic layer of the functional film produced in Example 1 by the same method as in Example 1, and the resin base material-hybrid layer-functional inorganic layer-hybrid layer is in this order. A laminated functional film was produced.
- Example 4 Formation of Hybrid Layer
- the first coating solution is applied so that the film thickness after drying becomes 1 ⁇ m, and 120 ° C. for 1 minute. After the heat treatment, vacuum ultraviolet irradiation was performed to form a hybrid layer. At this time, vacuum ultraviolet irradiation was performed under the following conditions.
- Illuminance 140 mW / cm 2 (172 nm)
- Stage temperature 100 ° C
- Stage movable speed and number of times of conveyance 3 times of conveyance at 10 mm / sec.
- Excimer light exposure integrated amount 1200 mJ / cm 2 .
- the second coating liquid is applied by spin coating, and dried at 80 ° C. for 1 minute to form a coating film having a thickness of 300 nm after drying,
- the coating film was modified by irradiation with vacuum ultraviolet rays.
- a functional inorganic layer in which two layers were laminated was formed, and a functional film in which a resin base material-hybrid layer-functional inorganic layer (two layers) were laminated in this order was produced.
- the conditions for vacuum ultraviolet irradiation are the same as those described in Example 1.
- Example 5 A functional inorganic layer (two layers) was formed by the same method as in Example 4 on the surface opposite to the bleed-out prevention layer of the produced resin base material. Further, a hybrid layer is formed on the formed functional inorganic layer in the same manner as in Example 4, and the resin base material-functional inorganic layer (two layers) -hybrid layer is laminated in this order. An adhesive film was produced.
- Example 6 Except that the method for forming the functional inorganic layer was changed to the atmospheric pressure plasma CVD method (AGP method), the resin base material-hybrid layer-functional inorganic layer was formed in this order in the same manner as in Example 1. A laminated functional film was produced.
- the atmospheric pressure plasma CVD method was performed under the following thin film formation conditions using a roll-to-roll atmospheric pressure plasma film forming apparatus (see, for example, FIG. 3 of JP-A-2008-56967).
- Discharge gas Nitrogen gas 94.9% by volume
- Thin film forming gas Tetraethoxysilane 0.1% by volume
- Additional gas Oxygen gas 5.0% by volume
- Deposition conditions ⁇ First electrode side> Power supply type: PHF-6k 100kHz (continuous mode) (manufactured by HEIDEN Laboratory) Frequency: 100kHz Output density: 10 W / cm 2 Electrode temperature: 120 ° C ⁇ Second electrode side> Power supply type: CF-5000-13M 13.56 MHz (made by Pearl Industry Co., Ltd.) Frequency: 13.56 MHz Output density: 10 W / cm 2 Electrode temperature: 90 ° C.
- Example 7 Except that the functional inorganic layer described in Example 2 was formed by the method of Example 6, the resin substrate-functional inorganic layer-hybrid layer was formed in this order in the same manner as in Example 2. A laminated functional film was produced.
- Example 8 The resin base material-hybrid layer-functional inorganic layer-hybrid layer was prepared in the same manner as in Example 3 except that the functional inorganic layer described in Example 3 was formed by the method of Example 6. A functional film laminated in this order was manufactured.
- Example 1 A functional inorganic layer was formed on the resin base material produced in the same manner as in Example 1, and a functional film in which the resin base material-functional inorganic layer was laminated in this order was produced.
- Example 2 Comparative Example 2 Except that the first coating solution was changed to a solution prepared by dissolving 2 g of methylsilsesquioxane (MSQ) (manufactured by Konishi Chemical Industry Co., Ltd.) with methyl ethyl ketone (MEK), the same method as in Example 1 was used. A functional film in which a resin substrate, an MSQ-containing layer, and a functional inorganic layer were laminated in this order was produced.
- MSQ methylsilsesquioxane
- MEK methyl ethyl ketone
- Example 3 The first coating solution was changed to a solution in which 2 g of methyl silsesquioxane (MSQ) (manufactured by Konishi Chemical Industry Co., Ltd.) and 0.5 g of colloidal silica IPA-ST (Nissan Chemical Industry Co., Ltd.) were dissolved in MEK. Except for the above, a functional film in which a resin base material-MSQ / colloidal silica-containing layer-functional inorganic layer was laminated in this order was produced in the same manner as in Example 1.
- MSQ methyl silsesquioxane
- Example 4 A solution containing a UV curable organic / inorganic hybrid hard coat material OPSTAR Z7501 (manufactured by JSR Corporation) on the surface opposite to the bleed-out preventing layer of the resin base, and a film thickness after drying of 1 ⁇ m Example 1 except that it was changed to a urethane acrylate layer cured under a curing condition of 1 J / cm 2 under an air atmosphere using a high-pressure mercury lamp, and then dried at 80 ° C. for 3 minutes. In the same manner as described above, a functional film in which a resin base material-urethane acrylate layer-functional inorganic layer was laminated in this order was produced.
- OPSTAR Z7501 manufactured by JSR Corporation
- Example 6 Comparative Example 6 Except that the first coating solution was changed to a solution in which 2 g of methylsilsesquioxane (MSQ) (manufactured by Konishi Chemical Industry Co., Ltd.) was dissolved in MEK, the resin base was changed in the same manner as in Example 2. A functional film in which a material, a functional inorganic layer, and an MSQ-containing layer were laminated in this order was produced.
- MSQ methylsilsesquioxane
- Example 7 The first coating solution was changed to a solution in which 2 g of methyl silsesquioxane (MSQ) (manufactured by Konishi Chemical Industry Co., Ltd.) and 0.5 g of colloidal silica IPA-ST (Nissan Chemical Industry Co., Ltd.) were dissolved in MEK. Except for this, a functional film in which a resin base material-functional inorganic layer-MSQ / colloidal silica-containing layer was laminated in this order was produced in the same manner as in Example 2.
- MSQ methyl silsesquioxane
- Example 8 A solution containing a UV curable organic / inorganic hybrid hard coat material OPSTAR Z7501 (manufactured by JSR Corporation) on the surface opposite to the bleed-out preventing layer of the resin base, and a film thickness after drying of 1 ⁇ m Example 2 except that it was changed to a urethane acrylate layer cured under curing conditions of 1 J / cm 2 in an air atmosphere using a high-pressure mercury lamp, dried at 80 ° C. for 3 minutes, and then cured.
- a functional film in which a resin substrate, a functional inorganic layer, and a urethane acrylate layer were laminated in this order was produced in the same manner as described above.
- Example 9 The resin base material-hybrid layer-functional inorganic layer is formed in the same manner as in Example 1 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 500 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 9 is 0.5. .
- Example 10 The resin base material-hybrid layer-functional inorganic layer is the same as in Example 1 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 600 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 10 is 0.6. .
- Example 11 The resin base material-hybrid layer-functional inorganic layer is formed in the same manner as in Example 1 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 700 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 11 is 0.7. .
- Example 12 The resin base material-hybrid layer-functional inorganic layer is formed in the same manner as in Example 1 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 1000 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 12 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 1.0. .
- Example 13 The resin base material-hybrid layer-functional inorganic layer is formed in the same manner as in Example 1 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 1100 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 13 is 1.1. .
- Example 14 The resin base material-hybrid layer-functional inorganic layer is formed in the same manner as in Example 1 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 90 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 14 is 0.09. .
- Example 15 The resin base material-hybrid layer-functional inorganic layer is formed in the same manner as in Example 1 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 9 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film produced in Example 15 is 0.009. .
- Example 16 Except that the first coating solution was applied so that the thickness of the hybrid layer was 5000 nm, the resin base material-hybrid layer-functional inorganic layer was in this order in the same manner as in Example 1. A laminated functional film was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 16 is 0.06. .
- Example 17 Except that the first coating solution was applied so that the thickness of the hybrid layer was 5000 nm, the resin base material-hybrid layer-functional inorganic layer was in this order in the same manner as in Example 9. A laminated functional film was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 17 is 0.10. .
- Example 18 Except that the first coating solution was applied so that the film thickness of the hybrid layer was 5000 nm, the resin base material-hybrid layer-functional inorganic layer was formed in this order in the same manner as in Example 10. A laminated functional film was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film produced in Example 18 is 0.12. .
- Example 19 Except for applying the first coating liquid so that the film thickness of the hybrid layer is 5000 nm and applying the second coating liquid so that the film thickness of the functional inorganic layer is 4800 nm.
- a functional film in which a resin base material-hybrid layer-functional inorganic layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 19 is 0.96. .
- Example 20 Except that the first coating solution was applied so that the thickness of the hybrid layer was 10000 nm, the resin base material-hybrid layer-functional inorganic layer was formed in this order in the same manner as in Example 14. A laminated functional film was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 20 is 0.009. .
- Example 21 Except that the first coating solution was applied so that the film thickness of the hybrid layer was 10000 nm, the resin substrate-hybrid layer-functional inorganic layer was formed in this order in the same manner as in Example 10. A laminated functional film was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 20 is 0.06. .
- Example 22 Except that the first coating solution was applied so that the thickness of the hybrid layer was 10,000 nm, and the second coating solution was applied so that the thickness of the functional inorganic layer was 900 nm. In the same manner as in Example 1, a functional film in which a resin base material-hybrid layer-functional inorganic layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 22 is 0.09. .
- Example 23 Except that the first coating solution was applied so that the film thickness of the hybrid layer was 10,000 nm, the resin base material-hybrid layer-functional inorganic layer was in this order in the same manner as in Example 12. A laminated functional film was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 23 is 0.10. .
- Example 24 Except that the first coating solution was applied so that the thickness of the hybrid layer was 10,000 nm, and the second coating solution was applied so that the thickness of the functional inorganic layer was 9000 nm. In the same manner as in Example 1, a functional film in which a resin base material-hybrid layer-functional inorganic layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 24 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 0.9. .
- Example 25 Except that the first coating solution was applied so that the film thickness of the hybrid layer was 10,000 nm, and the second coating solution was applied so that the film thickness of the functional inorganic layer was 11000 nm. In the same manner as in Example 1, a functional film in which a resin base material-hybrid layer-functional inorganic layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 25 is 1.1. .
- Example 26 The resin base material-functional inorganic layer-hybrid layer is formed in the same manner as in Example 2 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 500 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 26 is 0.5. .
- Example 27 The resin base material-functional inorganic layer-hybrid layer is formed in the same manner as in Example 2 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 600 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 27 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 0.6. .
- Example 28 The resin base material-functional inorganic layer-hybrid layer was formed in the same manner as in Example 2 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 700 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film produced in Example 28 is 0.7. .
- Example 29 The resin base material-functional inorganic layer-hybrid layer is formed in the same manner as in Example 2 except that the second coating solution is applied so that the thickness of the functional inorganic layer is 1000 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 29 is 1.0. .
- Example 30 The resin base material-functional inorganic layer-hybrid layer was formed in the same manner as in Example 2 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 1100 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 30 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 1.1. .
- Example 31 The resin base material-functional inorganic layer-hybrid layer was formed in the same manner as in Example 2 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 90 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 31 is 0.09. .
- Example 32 The resin base material-functional inorganic layer-hybrid layer was formed in the same manner as in Example 2 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 9 nm. A functional film laminated in order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 32 is 0.009. .
- Example 33 Resin substrate-hybrid layer-functional inorganic layer-hybrid in the same manner as in Example 3 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 500 nm. A functional film in which the layers were laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 33 is 0.5. .
- Example 34 Resin substrate-hybrid layer-functional inorganic layer-hybrid in the same manner as in Example 3 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 600 nm. A functional film in which the layers were laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 34 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 0.6. .
- Example 35 Resin substrate-hybrid layer-functional inorganic layer-hybrid in the same manner as in Example 3 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 700 nm. A functional film in which the layers were laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 35 is 0.7. .
- Example 36 Resin substrate-hybrid layer-functional inorganic layer-hybrid in the same manner as in Example 3 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 1000 nm. A functional film in which the layers were laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 36 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 1.0. .
- Example 37 Resin base material-hybrid layer-functional inorganic layer-hybrid in the same manner as in Example 3 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 1100 nm. A functional film in which the layers were laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 37 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 1.1. .
- Example 38 Resin substrate-hybrid layer-functional inorganic layer-hybrid in the same manner as in Example 3 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 90 nm. A functional film in which the layers were laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 38 is 0.09. .
- Example 39 Resin base material-hybrid layer-functional inorganic layer-hybrid in the same manner as in Example 3 except that the second coating solution was applied so that the thickness of the functional inorganic layer was 9 nm. A functional film in which the layers were laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film produced in Example 39 is 0.009. .
- Example 40 The resin base material-hybrid layer-functional inorganic layer-hybrid layer was prepared in the same manner as in Example 3 except that the first coating solution was applied so that the thickness of the hybrid layer was 5000 nm. A functional film laminated in this order was manufactured.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 40 is 0.06. .
- Example 41 The resin base material-hybrid layer-functional inorganic layer-hybrid layer was prepared in the same manner as in Example 33 except that the first coating solution was applied so that the thickness of the hybrid layer was 5000 nm. A functional film laminated in this order was manufactured.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 41 is 0.1. .
- Example 42 The resin base material-hybrid layer-functional inorganic layer-hybrid layer was prepared in the same manner as in Example 34 except that the first coating solution was applied so that the thickness of the hybrid layer was 5000 nm. A functional film laminated in this order was manufactured.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 42 is 0.12. .
- Example 43 Except for applying the first coating liquid so that the film thickness of the hybrid layer is 5000 nm and applying the second coating liquid so that the film thickness of the functional inorganic layer is 4800 nm.
- a functional film in which a resin base material-hybrid layer-functional inorganic layer-hybrid layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 43 is 0.96. .
- Example 44 Except that the first coating solution was applied so that the film thickness of the hybrid layer was 10,000 nm, and the second coating solution was applied so that the film thickness of the functional inorganic layer was 90 nm. In the same manner as in Example 3, a functional film in which a resin base material-hybrid layer-functional inorganic layer-hybrid layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film produced in Example 44 is 0.009. .
- Example 45 The resin base material-hybrid layer-functional inorganic layer-hybrid layer was prepared in the same manner as in Example 34 except that the first coating solution was applied so that the thickness of the hybrid layer was 10,000 nm. A functional film laminated in this order was manufactured.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 45 is 0.12. .
- Example 46 Except that the first coating solution was applied so that the thickness of the hybrid layer was 10,000 nm, and the second coating solution was applied so that the thickness of the functional inorganic layer was 900 nm. In the same manner as in Example 3, a functional film in which a resin base material-hybrid layer-functional inorganic layer-hybrid layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 46 is 0.09. .
- Example 47 The resin base material-hybrid layer-functional inorganic layer-hybrid layer was prepared in the same manner as in Example 36 except that the first coating solution was applied so that the thickness of the hybrid layer was 10,000 nm. A functional film laminated in this order was manufactured.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 47 is 0.1. .
- Example 48 Except that the first coating solution was applied so that the thickness of the hybrid layer was 10,000 nm, and the second coating solution was applied so that the thickness of the functional inorganic layer was 9000 nm. In the same manner as in Example 3, a functional film in which a resin base material-hybrid layer-functional inorganic layer-hybrid layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film produced in Example 48 (the thickness of the functional inorganic layer / the thickness of the hybrid layer) is 0.9. .
- Example 49 Except that the first coating solution was applied so that the film thickness of the hybrid layer was 10,000 nm, and the second coating solution was applied so that the film thickness of the functional inorganic layer was 11000 nm. In the same manner as in Example 3, a functional film in which a resin base material-hybrid layer-functional inorganic layer-hybrid layer was laminated in this order was produced.
- the ratio of the thickness of the functional inorganic layer to the thickness of the hybrid layer of the functional film manufactured in Example 49 is 1.1. .
- Example 1 and Examples 9 to 25, Example 2 and Examples 26 to 32, and Example 3 and Examples 33 to 49 are shown in Tables 2 to 4 below, respectively.
- a parallel plate type electrode was used, the functional film of Example 1 was placed between the electrodes, and a mixed gas was introduced to form a thin film.
- the following was used as a ground (ground) electrode.
- a 200 mm ⁇ 200 mm ⁇ 2 mm stainless steel plate is coated with a high-density, high-adhesion alumina sprayed film, a solution obtained by diluting tetramethoxysilane with ethyl acetate is applied and dried, and then cured by UV irradiation and sealed.
- a hole-treated electrode was prepared by polishing and sealing the surface of the dielectric material that had been sealed, so that the Rmax was 5 ⁇ m.
- an electrode obtained by coating a dielectric on a hollow square pure titanium pipe under the same conditions as the ground electrode was used.
- a plurality of application electrodes were prepared and provided to face the ground electrode to form a discharge space.
- a power source used for generating plasma a high frequency power source CF-5000-13M (manufactured by Pearl Industry Co., Ltd.) was used, and 5 W / cm 2 of power was supplied at a frequency of 13.56 MHz.
- a mixed gas having the following composition is caused to flow between the electrodes to form a plasma state, the functional film is subjected to atmospheric pressure plasma treatment, and an indium tin oxide (ITO) film is formed to a thickness of 100 nm on the intermediate layer, With a transparent conductive film was formed.
- ITO indium tin oxide
- Discharge gas Helium 98.5% by volume Reactive gas 1: 0.25% by volume of oxygen Reactive gas 2: Indium acetylacetonate 1.2% by volume Reactive gas 3: Dibutyltin diacetate 0.05% by volume.
- the obtained transparent conductive film 100 mm ⁇ 80 mm was used as a functional film substrate, and after patterning the functional film substrate, the functional film substrate provided with the ITO transparent electrode was ultrasonically cleaned with isopropyl alcohol, Dry with dry nitrogen gas. Thereafter, the functional film substrate was fixed to a substrate holder of a commercially available vacuum deposition apparatus.
- ⁇ -NPD 200 mg is used in a resistance heating boat made of molybdenum
- 200 mg of CBP as a host compound is added to another resistance heating boat made of molybdenum
- 200 mg of bathocuproin (BCP) is added to another resistance heating boat made of molybdenum.
- Ir-1 100 mg was put into a boat, and Alq 3 200 mg was put into another molybdenum resistance heating boat, respectively, and attached to a vacuum deposition apparatus.
- the heating boat containing ⁇ -NPD is heated by energization so that the deposition rate is 0.1 nm / sec.
- the film was vapor-deposited in an area of 80 mm ⁇ 60 mm to provide a hole transport layer.
- the heating boat containing CBP and Ir-1 was heated by energization and co-evaporated on the hole transport layer at a deposition rate of 0.2 nm / second and 0.012 nm / second, respectively, to provide a light emitting layer.
- the temperature of the functional film substrate at the time of vapor deposition was room temperature.
- the said heating boat containing BCP was heated by electricity supply, and it vapor-deposited on the said light emitting layer with the vapor deposition rate of 0.1 nm / second, and provided the 10-nm-thick hole blocking layer. Furthermore, the heating boat containing Alq 3 was further heated by energization, and deposited on the hole blocking layer at a deposition rate of 0.1 nm / second to provide an electron transport layer having a thickness of 40 nm. In addition, the temperature of the functional film substrate at the time of vapor deposition was room temperature.
- the water vapor transmission rate of the functional film was evaluated from the corrosion amount of metallic calcium.
- a comparative sample using a 0.2 mm thick quartz glass plate instead of the functional film sample is prepared. And stored under high temperature and high humidity of 60 ° C. and 90% RH. In the case of the comparative sample, it was confirmed that no corrosion of metallic calcium occurred even after 3000 hours.
- Corrosion point expansion rate evaluation The water vapor barrier property evaluation cell is stored in a constant temperature and humidity oven Yamato Humidic Chamber IG47M under high temperature and high humidity of 60 ° C and 90% RH, and the expansion rate of the corrosion point in the calcium deposition region is observed. The corrosion point expansion rate was evaluated. The corrosion point expansion rate was evaluated according to the following criteria.
- Peripheral shrinkage evaluation Water vapor barrier property evaluation cell is stored under constant temperature and humidity oven Yamato Humidic Chamber IG47M under high temperature and high humidity of 60 ° C. and 90% RH. Then, the shrinkage of the remaining area of calcium deposition was observed, and the peripheral shrinkage was evaluated. The corrosion area was evaluated according to the following criteria.
- the organic EL element was energized in an environment of 60 ° C. and 90% RH, and light emission unevenness such as generation of dark spots and luminance unevenness from 0 to 120 days was visually observed.
- the light emission unevenness evaluation was performed according to the following criteria.
- Is 2 A dark spot or luminance unevenness is observed on the 0th day, the non-light emitting area is 1% or less, and the non-light emitting area after 120 days exceeds 10% of the total light emitting area, or the 0th day A dark spot or luminance unevenness is observed, the non-light emitting area exceeds 1%, and the non-light emitting area after 120 days is more than 1.0% and 10.0% or less of the total light emitting area; A dark spot or luminance unevenness is observed on day 1: 0, the non-light-emitting region exceeds 1%, and the non-light-emitting region after 120 days passes exceeds 10% of the total light-emitting area.
- a non-light-emitting area that is, a light-emitting area
- a non-light-emitting area accompanying the progress of corrosion from the periphery of the element sealed with a film by energizing an organic EL element sample in an environment of 40 ° C. and 90% RH was observed from day 0 to day 120, and the shrinkage of the peripheral light-emitting region was evaluated.
- the shrinkage evaluation of the peripheral light emitting region was evaluated according to the following criteria.
- the non-light-emitting region after 120 days is 1.0% or less of the total light-emitting region
- 4 No reduction of the light emitting area was observed on the 0th day, and the non-light emitting area after 120 days passed was more than 1.0% and less than 10.0% of the total light emitting area, or the non-light emitting area on the 0th day More than 0% of the total emission region and 0.5% or less, and the non-emission region after 120 days is 1.0% or less of the total emission region
- 3 The non-light emitting area on day 0 is more than 0% and less than 0.5% of the total light emitting area, and the non-light emitting area after 120 days is more than 1.0% and less than 10.0% of the entire light emitting area.
- the non-light-emitting area on the 0th day is more than 0% and less than 0.5% of the total light-emitting area, and the non-light-emitting area after 120 days is over 10.0% of the total light-emitting area, or 0
- the day non-light emitting area is more than 0.5% of the total light emitting area, and the non light emitting area after 120 days is more than 1.0% and not more than 10.0% of the total light emitting area
- the non-light emitting area on day 1: 0 is more than 0.5% of the total light emitting area, and the non light emitting area after 120 days is over 10.0% of the total light emitting area.
- Table 5 below shows the evaluation results of the functional films of Examples 1 to 8 and Comparative Examples 1 to 9, and the organic EL devices produced using the functional films.
- the functional film according to the present invention is excellent in bending resistance and stability under high temperature and high humidity. Moreover, it turns out that the organic EL element using the said functional film is excellent in performance.
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Abstract
Description
前記ハイブリッド層が、ポリシロキサンおよび樹脂微粒子を含む、機能性フィルム;
2.前記ハイブリッド層が、前記樹脂基材と前記機能性無機層との間に位置する、1.に記載の機能性フィルム;
3.前記機能性無機層の前記樹脂基材とは反対側の面に前記ハイブリッド層が配置された、1.または2.に記載の機能性フィルム;
4.2層以上積層された機能性無機層を含む、1.~3.のいずれか1つに記載の機能性フィルム;
5.ハイブリッド層の膜厚に対する機能性無機層の膜厚の比(機能性無機層の膜厚/ハイブリッド層の膜厚)が、0.001~10である、1.~4.のいずれか1項に記載の機能性フィルム;
6.前記樹脂基材の両面に、前記機能性無機層と、前記機能性無機層の少なくとも一方の面に配置されたハイブリッド層とを有する、1.~5.のいずれか1つに記載の機能性フィルム;
7.前記機能性無機層が、ガスバリア性無機層である、1.~6.のいずれか1つに記載の機能性フィルム;
8.樹脂基材と、前記樹脂基材上に位置する機能性無機層と、前記機能性無機層の少なくとも一方の面に配置されたハイブリッド層と、を含む機能性フィルムの製造方法であって、ポリシロキサンおよび樹脂微粒子を含む第1の塗布液を塗布して、前記ハイブリッド層を形成する工程(1)を含む、製造方法;
9.無機前駆体を含む第2の塗布液を塗布して塗膜を形成し、前記塗膜を改質処理して機能性無機層を形成する工程(2)をさらに含む、8.に記載の製造方法;
10.前記無機前駆体が、ポリシラザンを含む、9.に記載の製造方法;
11.前記改質処理が、真空紫外線照射によって行われる、9.または10.に記載の製造方法;
12.電子デバイス本体と、請求項1.~7.のいずれか1つに記載の機能性フィルム、または8.~11.のいずれか1つに記載の方法によって製造された機能性フィルムと、を含む、電子デバイス;
13.前記電子デバイス本体が、前記機能性フィルムによって封止されてなる、12.に記載の電子デバイス。
本発明の第1の実施形態によれば、樹脂基材と、前記樹脂基材上に位置する機能性無機層と、前記機能性無機層の少なくとも一方の面に配置されたハイブリッド層と、を含む、機能性フィルムが提供される。この際、前記ハイブリッド層は、ポリシロキサンおよび樹脂微粒子を含む。
図1は、第1の形態に係る機能性フィルムを模式的に表した断面概略図である。図1によれば、第1の形態に係る機能性フィルム11は、ブリードアウト防止層(図示せず)が一方の面に配置された樹脂基材12と、前記ブリードアウト防止層とは反対の面に配置されたハイブリッド層13と、前記ハイブリッド層13上に配置された機能性無機層14と、を有する。前記ハイブリッド層13は、ポリシロキサンおよび樹脂微粒子を含む。また、前記機能性無機層14は、酸化ケイ素、および/または酸窒化ケイ素を含む。当該機能性無機層14は、ガスバリア性を有するガスバリア性無機層である。よって、第1の形態に係る機能性フィルム11は、ガスバリア性フィルムである。
本発明に係る樹脂基材は、特に限定されないが、可撓性および透過性を有する折り曲げ可能なフィルム基材であることが好ましい。
機能性無機層は機能性フィルムに一定の機能を付与する。例えば、機能性無機層がガスバリア性無機層である場合には、機能性フィルムはガスバリア性を有するガスバリア性フィルムとなりうる。また、ガスバリア性無機層以外の機能性無機層としては、ITO等の透明導電性無機層、SiO2やTiO2が積層された遮熱無機層、金属や金属酸化物等からなる電極無機層、SiO2等の層間絶縁無機層、SiO2等のゲート絶縁無機層、TAOS(透明アモルファス酸化物半導体)等の酸化物半導体無機層、銀蒸着層、および屈折率の異なる多層膜等が挙げられる。上記機能性無機層は、タッチパネルやフレキシブルプリント基板、薄膜トランジスタ、各種ディスプレイ、バックライト、反射板、偏光板用拡散反射フィルム、反射防止フィルム等に使用されうる。
ガスバリア性無機層は、機能性フィルムにガスバリア性を付与する機能を有する。なお、本明細書において「ガスバリア性」とは、JIS K 7129-1992に準拠した方法で測定された水蒸気透過度(温度:60±0.5℃、相対湿度(RH):90±2%)が3×10-3g/(m2・24h)以下であり、JIS K 7126-1987に準拠した方法で測定された酸素透過度が1×10-3mL/m2・24h・atm以下であることを意味する。
ポリシラザンとは、その構造内にSi-N、Si-H、N-H等の結合を有するポリマーであり、SiO2、Si3N4、およびこれらの中間固溶体SiOxNy等の無機前駆体として機能する。
無機物は、ガスバリア性を有するものであれば特に制限されないが、上記ポリシラザンを改質処理して生成する無機物、例えば、酸化ケイ素、窒化ケイ素、酸窒化ケイ素等であることが好ましい。ポリシラザンを改質処理することによって得られる前記無機物は、より緻密なガスバリア性無機層を形成することから、高いバリア性を有しうる。
ハイブリッド層は、機能性無機層に屈曲耐性および高温高湿下での安定性を付与する機能を有する。前記ハイブリッド層は、ポリシロキサンおよび樹脂微粒子を含む。
ポリシロキサンは、ハイブリッド層に一定の耐熱性および膜強度を付与する機能を有する。
樹脂微粒子は、ハイブリッド層に一定の柔軟性を付与し、かつ、樹脂基材やポリシロキサン等から生じる低分子化合物を捕捉する機能を有する。
アミノシラン化合物は、ハイブリッド層に含有されることによって密着性、耐傷性を向上しうる。
エポキシシラン化合物は、ハイブリッド層に含有されることによって密着性、耐傷性、成膜性を向上しうる。
コロイダルシリカは、ハイブリッド層に含有されることによって耐傷性を向上しうる。
本発明の第2の実施形態によれば、樹脂基材と、前記樹脂基材上に位置する機能性無機層と、前記機能性無機層の少なくとも一方の面に配置されたハイブリッド層と、を含む機能性フィルムの製造方法が提供される。当該機能性フィルムの製造方法は、ポリシロキサンおよび樹脂微粒子を含む第1の塗布液を塗布して、前記ハイブリッド層を形成する工程(1)を含む。
工程(1)は、ポリシロキサンおよび樹脂微粒子を含む第1の塗布液を塗布して、前記ハイブリッド層を形成する工程である。前記第1の塗布液は、樹脂基材上および/または機能性無機層上に塗布されうる。
第1の塗布液は、ポリシロキサンおよび樹脂微粒子を含む。前記ポリシロキサンおよび樹脂微粒子は、第1の実施形態と同様のものでありうる。
第1の塗布液に含有されうる溶媒としては、特に制限されないが、水、アルコール系溶媒、芳香族炭化水素系溶媒、エーテル系溶媒、ケトン系溶媒、エステル系溶媒等が挙げられる。アルコール系溶媒としては、メタノール、エタノール、n-プロピルアルコール、イソプロピルアルコール、n-ブチルアルコール、sec-ブチルアルコール、tert-ブチルアルコール、n-ヘキシルアルコール、n-オクチルアルコール、エチレングリコール、ジエチレングリコール、トリエチレングリコール、エチレングリコールモノブチルエーテル、エチレングリコールモノエチルエーテルアセテート、ジエチレングリコールモノエチルエーテル、プロピレングリコールモノメチルエーテル、プロピレンモノメチルエーテルアセテート、ジアセトンアルコール、メチルセロソルブ、エチルセロソルブ、プロピルセロソルブ、ブチルセロソルブ等が挙げられる。芳香族炭化水素系溶媒としては、トルエン、キシレン等が挙げられる。エーテル系溶媒としては、テトラヒドロフラン、1,4-ジオキサン、1,2-ジメトキシエタン等が挙げられる。ケトン系溶媒としては、シクロヘキサノン、アセトン、メチルエチルケトン、メチルイソブチルケトン等が挙げられる。エステル系溶媒としては、酢酸メチル、酢酸エチル、酢酸エトキシエチル等が挙げられる。これらの他、ジクロロエタン、酢酸等の溶媒を用いてもよい。これらの溶媒は、単独で、または2種以上を混合して用いられうる。
硬化触媒は、第1の塗布液に含有されるシラン化合物を加水分解、縮合(硬化)させる触媒である。
ハイブリッド層は、第1の塗布液を樹脂基材上または機能性無機層上に塗布して形成される。第1の塗布液の塗布方法としては、適宜公知の方法が採用されうる。具体的には、スピンコート法、ロールコート法、フローコート法、インクジェット法、スプレーコート法、プリント法、ディップコート法、流延成膜法、バーコート法、グラビア印刷法等が挙げられる。
工程(2)は、無機前駆体を含む第2の塗布液を塗布して塗膜を形成し、前記塗膜を改質処理して機能性無機層を形成する工程である。前記第2の塗布液は、樹脂基材上および/またはハイブリッド層上に塗布されうる。特に、第2の塗布液をハイブリッド層上に塗布する場合には、ハイブリッド層が有する低分子化合物捕捉機能により、第2の塗布液がハイブリッド層内部にまで含浸され、ハイブリッド層と機能性無機層との接着性がより向上することから好ましい。
第2の塗布液は、無機前駆体を含む。
無機前駆体としては、特に制限されないが、ポリシラザンを用いることが好ましい。
アミン触媒および金属は、後述する改質処理において、ポリシラザンの酸化ケイ素化合物への転化を促進しうる。アミン触媒としては、N,N,N’,N’-テトラメチル-1,6-ジアミノヘキサンが挙げられる。また、金属としては、パラジウムが挙げられる。アミン触媒および金属は、ポリシラザンに対して、第1の塗布液中に0.1~10質量含むことが好ましい。特にアミン触媒については、塗布性の向上および反応の時間の短縮の観点から、ポリシラザンに対して、第1の塗布液中に0.5~5質量%含むことがより好ましい。
第2の塗布液に含有されうる溶媒としては、ポリシラザンと反応するものでなければ特に制限はなく、公知の溶媒が用いられうる。具体的には、脂肪族炭化水素、脂環式炭化水素、芳香族炭化水素、ハロゲン化炭化水素等の炭化水素系溶媒;脂肪族エーテル、脂環式エーテル等のエーテル系溶媒が挙げられる。より詳細には、炭化水素溶媒としては、ペンタン、ヘキサン、シクロヘキサン、トルエン、キシレン、ソルベッソ、ターベン、塩化メチレン、トリクロロエタン等が挙げられる。また、エーテル系溶媒としては、ジブチルエーテル、ジオキサン、テトラヒドロフラン等が挙げられる。これらの溶媒は単独で、または2種以上を混合して用いられうる。
工程(2)では、第2の塗布液を塗布して塗膜を形成し、前記塗膜を改質処理することによって、機能性無機層を形成する。前記第2の塗布液は、樹脂基材上またはハイブリッド層上に塗布されうる。
第2の塗布液の塗布方法としては、適宜公知の方法が採用されうる。具体的には、スピンコート法、ロールコート法、フローコート法、インクジェット法、スプレーコート法、プリント法、ディップコート法、流延成膜法、バーコート法、グラビア印刷法等が挙げられる。
塗膜の改質とは、塗膜を構成する無機前駆体が転化されることを意味する。例えば、塗膜中に含まれるポリシラザンが転化されると、酸化ケイ素化合物および/または酸窒化ケイ素化合物に転化しうる。
e+Xe→Xe*
Xe*+2Xe→Xe2 *+Xe
Xe2 *→Xe+Xe+hν(172nm)
となる。この際、励起されたエキシマ分子であるXe2 *が基底状態に遷移するとき、172nmのエキシマ光(真空紫外線)を発光する。上記エキシマランプは前記エキシマ光を利用する。前記エキシマ発光を得る方法としては、例えば、誘電体バリア放電を用いる方法および無電極電界放電を用いる方法が挙げられる。
本発明の第3の実施形態によれば、電子デバイス本体と、上述の機能性フィルムと、を含む電子デバイスが提供される。上述の機能性フィルムは、屈曲耐性および高温高湿下での安定性に優れることから、電子デバイスに好適に適用されうる。
図4は、一実施形態における有機ELパネルの断面概略図である。
有機EL素子は、特に制限されないが、通常、下記の層構成を有しうる。
(2)陽極/正孔輸送層/発光層/陰極
(3)陽極/発光層/電子輸送層/陰極
(4)陽極/正孔輸送層/発光層/電子輸送層/陰極
(5)陽極/陽極バッファー層(正孔注入層)/正孔輸送層/発光層/電子輸送層/陰極バッファー層(電子注入層)/陰極。
陽極としては、特に制限されないが、仕事関数の大きい(4eV以上)金属、合金、電気伝導性化合物、およびこれらの混合物を用いることが好ましい。具体例としては、金(Au)等の金属、ヨウ化銅(CuI)、インジウムスズ酸化物(ITO)、酸化スズ(SnO2)、酸化亜鉛(ZnO)等の導電性透明材料が挙げられる。また、IDIXO(In2O3-ZnO)等の非晶質で透明導電膜を作製可能な材料を用いてもよい。
陰極としては、特に制限されないが、仕事関数の小さい(4eV以下)金属(以下、「電子注入性金属」とも称する)、合金、電気伝導性化合物、およびこれらの混合物を用いることが好ましい。具体例としては、ナトリウム、ナトリウム-カリウム合金、マグネシウム、リチウム、マグネシウム/銅混合物、マグネシウム/銀混合物、マグネシウム/アルミニウム混合物、マグネシウム/インジウム混合物、アルミニウム/酸化アルミニウム(Al2O3)混合物、インジウム、リチウム/アルミニウム混合物、希土類金属等が挙げられる。これらのうち、電子注入性および酸化等に対する耐久性の観点から、電子注入性金属および前記電子注入性金属よりも仕事関数の値が大きく安定な金属の混合物、例えば、マグネシウム/銀混合物、マグネシウム/アルミニウム混合物、マグネシウム/インジウム混合物、アルミニウム/酸化アルミニウム(Al2O3)混合物、リチウム/アルミニウム混合物を用いることが好ましい。
注入層には電子注入層(陰極バッファー層)と正孔注入層(陽極バッファー層)とがあり、電子注入層と正孔注入層とを必要に応じて設け、陽極と発光層もしくは正孔輸送層の間、および/または陰極と発光層もしくは電子輸送層との間に存在させる。
発光層は、電極(陰極、陽極)または電子輸送層、正孔輸送層から注入されてくる電子および正孔が再結合して発光する層であり、発光する部分は発光層の層内であっても発光層と隣接層との界面であってもよい。
発光ドーパントは、大別すると、蛍光を発光する蛍光性ドーパントとリン光を発光するリン光性ドーパントの2種類がある。
発光ホスト(単に「ホスト」とも称する)とは、2種以上の化合物を含む発光層中にて混合比(質量)の最も多い化合物のことを意味し、それ以外の化合物についてはドーパント化合物(単に、「ドーパント」とも称する)である。例えば、発光層を化合物A、化合物Bという2種で構成し、その混合比がA:B=10:90であれば化合物Aがドーパント化合物であり、化合物Bがホスト化合物である。さらに発光層を化合物A、化合物B、化合物Cの3種から構成し、その混合比がA:B:C=5:10:85であれば、化合物Aおよび化合物Bがドーパント化合物であり、化合物Cがホスト化合物である。
正孔輸送層とは、正孔を輸送する機能を有する正孔輸送材料からなり、広い意味で正孔注入層や電子阻止層についても正孔輸送層に含まれる。正孔輸送層は単層または複数層設けることができる。
電子輸送層とは、電子を輸送する機能を有する電子輸送材料からなり、広い意味で電子注入層や正孔阻止層についても電子輸送層に含まれる。電子輸送層は単層または複数層設けることができる。
有機EL素子の作製方法について、陽極/正孔注入層/正孔輸送層/発光層/電子輸送層/電子注入層/陰極からなる有機EL素子を例に挙げて説明する。
樹脂基材として両面に易接着加工された厚さ100μmのポリエステルフィルムであるコスモシャインA4300(東洋紡績株式会社製)を樹脂基材として用いた。
ガス導入管、還流冷却器、pH測定用複合ガラス電極、およびかき混ぜ装置を備えた500mL容量の4つ口フラスコを用い、蒸留水200g中に、濃度が5.0g/100mLとなるように反応性乳化剤(リン酸エステル系乳化剤)ニューフロンティアA-229E(第一工業製薬株式会社製)を溶解し、50~60℃に保った。重合モノマーとして、アクリル酸エチル、メタクリル酸メチル、グリシジルメタクリレートを重量混合比60/40/2の割合で混合した混合モノマー150gを準備し、はじめにそのうち25gを上記溶液中に分散乳化させた。一定の撹拌状態を保ちながら、硫酸銅の濃度が5.0×10-7mol/Lとなるように硫酸銅水溶液を添加した。レドックス重合開始剤である過硫酸カリウム-チオ硫酸ナトリウムの等モル量混合物を濃度が3.0×10-3mol/Lとなるように添加して重合を開始させた(温度:50~60℃、pH=4~7)。上記混合モノマーの残り125gを徐々に滴下し、重合熱による昇温を防ぎながら重合を行った。重合時間は15~30分程度として、アクリル酸エステル系樹脂微粒子を得た。
容積50gのサンプル管に、上記調製したアクリル酸エステル系樹脂微粒子2.8g、1-メトキシ─2-プロパノール8.5g、およびイオン交換水3gを仕込み、700rpmで撹拌しながら、硬化触媒である酢酸0.3g、アルコキシシラン化合物であるテトラメトキシシラン2g、硬化触媒である20%p-トルエンスルホン酸メタノール液0.1gをこの順にそれぞれ1分間かけて滴下した。その後、室温で10分撹拌し、これをA液とした。
20質量%のパーヒドロポリシラザン(PHPS)(アクアミカ NN120-20)のジブチルエーテル溶液、および5質量%のアミン触媒(N,N,N’,N’-テトラメチル-1,6-ジアミノヘキサン)を含む溶液(NAX120-20、AZエレクトロニックマテリアルズ株式会社製)を、パーヒドロポリシラザン(PHPS)濃度に対してアミン触媒の含有量が1.0質量%となるように混合し、第2の塗布液を調製した。
(実施例1)
ハイブリッド層の形成
上記作製した樹脂基材のブリードアウト防止層とは反対の表面に、前記第1の塗布液を、乾燥後の膜厚が1μm(1000nm)となるように塗布し、120℃で30分間の加熱処理をすることで、ハイブリッド層を形成した。
前記ハイブリッド層上に、第2の塗布液をスピンコート法により塗布し、80℃で1分間乾燥させて、乾燥後の厚さが300nmの塗膜を形成した。この際、前記厚さを測定する際の境界面は、TEM(Transmission Electron Microscope:透過電子顕微鏡)の断面写真より確認された。
ステージ温度:100℃
処理環境:ドライ窒素ガス雰囲気下
処理環境の酸素濃度:0.1%
ステージ可動速度と搬送回数:10mm/秒で16回搬送
エキシマ光露光積算量:6000mJ/cm2。
上記作製した樹脂基材のブリードアウト防止層とは反対の表面に、実施例1と同様の方法により機能性無機層を形成した。また、形成された前記機能性無機層上に実施例1と同様の方法でハイブリッド層を形成して、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
実施例1で製造した機能性フィルムの機能性無機層上にさらに、実施例1と同様の方法でハイブリッド層を形成し、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の形成
上記作製した樹脂基材のブリードアウト防止層とは反対の表面に、前記第1の塗布液を、乾燥後の膜厚が1μmとなるように塗布し、120℃、1分間の加熱処理を行った後、真空紫外線照射を行ってハイブリッド層を形成した。この際、真空紫外線照射の条件は、以下の条件により行った。
ステージ温度:100℃
処理環境:ドライ窒素ガス雰囲気下
処理環境の酸素濃度:0.1%
ステージ可動速度と搬送回数:10mm/秒で3回搬送
エキシマ光露光積算量:1200mJ/cm2。
前記ハイブリッド層上に、前記第2の塗布液をスピンコート法により塗布し、80℃で1分間乾燥させて、乾燥後の厚さが300nmの塗膜を形成し、前記塗膜を真空紫外線照射により改質処理を行った。上記工程を再度繰り返すことで、2層が積層された機能性無機層を形成し、樹脂基材-ハイブリッド層-機能性無機層(2層)がこの順で積層された機能性フィルムを製造した。なお真空紫外線照射の条件は実施例1に記載の条件と同様である。
上記作製した樹脂基材のブリードアウト防止層とは反対の表面に、実施例4と同様の方法により機能性無機層(2層)を形成した。また、形成された前記機能性無機層上に実施例4と同様の方法でハイブリッド層を形成して、樹脂基材-機能性無機層(2層)-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の形成方法を、大気圧プラズマCVD法(AGP法)に変更したことを除いては、実施例1と同様の方法で樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。なお、大気圧プラズマCVD法は、ロールツーロール形態の大気圧プラズマ製膜装置(例えば、特開2008-56967号の図3を参照)を用いて、以下の薄膜形成条件で行った。
放電ガス:窒素ガス 94.9体積%
薄膜形成ガス:テトラエトキシシラン 0.1体積%
添加ガス:酸素ガス 5.0体積%
成膜条件
〈第1電極側〉
電源種類:PHF-6k 100kHz(連続モード)(株式会社ハイデン研究所製)
周波数 :100kHz
出力密度:10W/cm2
電極温度:120℃
〈第2電極側〉
電源種類:CF-5000-13M 13.56MHz(パール工業株式会社製)
周波数 :13.56MHz
出力密度:10W/cm2
電極温度:90℃。
実施例2に記載の機能性無機層を、実施例6の方法で形成したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
実施例3に記載の機能性無機層を、実施例6の方法で形成したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
上記作製した樹脂基材上に、実施例1と同様の方法で機能性無機層を形成し、樹脂基材-機能性無機層がこの順で積層された機能性フィルムを製造した。
第1の塗布液を、メチルシルセスキオキサン(MSQ)(小西化学工業株式会社製)2gをメチルエチルケトン(MEK)で溶解した溶液に変更したことを除いては、実施例1と同様の方法で、樹脂基材-MSQ含有層-機能性無機層がこの順で積層された機能性フィルムを製造した。
第1の塗布液を、メチルシルセスキオキサン(MSQ)(小西化学工業株式会社製)2gおよびコロイダルシリカIPA-ST(日産化学工業株式会社製)0.5gをMEKで溶解した溶液に変更したことを除いては、実施例1と同様の方法で、樹脂基材-MSQ・コロイダルシリカ含有層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層を、樹脂基材のブリードアウト防止層とは反対の表面に、UV硬化型有機/無機ハイブリッドハードコート材OPSTAR Z7501(JSR株式会社製)を含む溶液を、乾燥後の膜厚が1μmとなるように塗布し、80℃で3分間乾燥させ、高圧水銀ランプを用いて、空気雰囲気下、1J/cm2の硬化条件で硬化したウレタンアクリレート層に変更したことを除いては、実施例1と同様の方法で樹脂基材-ウレタンアクリレート層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層を、樹脂基材のブリードアウト防止層とは反対の表面に、ポリマー型アクリレートであるUNIDIC V-684(DIC株式会社製)3.2gおよびコロイダルシリカIPA-ST(日産化学工業株式会社製)0.5gをMEKで溶解した溶液を、乾燥後の膜厚が1μmとなるように塗布し、80℃で3分間乾燥させ、高圧水銀ランプを用いて、空気雰囲気下、1J/cm2の硬化条件で硬化したアクリレート層に変更したことを除いては、実施例1と同様の方法で樹脂基材-アクリレート層-機能性無機層がこの順で積層された機能性フィルムを製造した。
第1の塗布液を、メチルシルセスキオキサン(MSQ)(小西化学工業株式会社製)2gをMEKで溶解した溶液に変更したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-MSQ含有層がこの順で積層された機能性フィルムを製造した。
第1の塗布液を、メチルシルセスキオキサン(MSQ)(小西化学工業株式会社製)2gおよびコロイダルシリカIPA-ST(日産化学工業株式会社製)0.5gをMEKで溶解した溶液に変更したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-MSQ・コロイダルシリカ含有層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層を、樹脂基材のブリードアウト防止層とは反対の表面に、UV硬化型有機/無機ハイブリッドハードコート材OPSTAR Z7501(JSR株式会社製)を含む溶液を、乾燥後の膜厚が1μmとなるように塗布し、80℃で3分間乾燥させ、高圧水銀ランプを用いて、空気雰囲気下、1J/cm2の硬化条件で硬化したウレタンアクリレート層に変更したことを除いては、実施例2と同様の方法で樹脂基材-機能性無機層-ウレタンアクリレート層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層を、樹脂基材のブリードアウト防止層とは反対の表面に、ポリマー型アクリレートであるUNIDIC V-684(DIC株式会社製)3.2gおよびコロイダルシリカIPA-ST(日産化学工業株式会社製)0.5gをMEKで溶解した溶液を、乾燥後の膜厚が1μmとなるように塗布し、80℃で3分間乾燥させ、高圧水銀ランプを用いて、空気雰囲気下、1J/cm2の硬化条件で硬化したアクリレート層に変更したことを除いては、実施例2と同様の方法で樹脂基材-アクリレート層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が500nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が600nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が700nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が1000nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が1100nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が90nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が9nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布したことを除いては、実施例9と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布したことを除いては、実施例10と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が4800nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布したことを除いては、実施例14と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布したことを除いては、実施例10と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が900nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布したことを除いては、実施例12と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が9000nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が11000nmとなるように、第2の塗布液を塗布したことを除いては、実施例1と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が500nmとなるように、第2の塗布液を塗布したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が600nmとなるように、第2の塗布液を塗布したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が700nmとなるように、第2の塗布液を塗布したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が1000nmとなるように、第2の塗布液を塗布したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が1100nmとなるように、第2の塗布液を塗布したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が90nmとなるように、第2の塗布液を塗布したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が9nmとなるように、第2の塗布液を塗布したことを除いては、実施例2と同様の方法で、樹脂基材-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が500nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が600nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が700nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が1000nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が1100nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が90nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
機能性無機層の膜厚が9nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布したことを除いては、実施例33と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布したことを除いては、実施例34と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が5000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が4800nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が90nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布したことを除いては、実施例34と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が900nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布したことを除いては、実施例36と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が9000nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
ハイブリッド層の膜厚が10000nmとなるように、第1の塗布液を塗布し、機能性無機層の膜厚が11000nmとなるように、第2の塗布液を塗布したことを除いては、実施例3と同様の方法で、樹脂基材-ハイブリッド層-機能性無機層-ハイブリッド層がこの順で積層された機能性フィルムを製造した。
(製造例1)
上記製造した実施例1に記載の機能性フィルムを用いて、有機EL素子を作製した。
プラズマ放電装置としては電極が平行平板型のものを用い、この電極間に実施例1の機能性フィルムを載置し、かつ、混合ガスを導入して薄膜形成を行った。なお、アース(接地)電極としては、以下のものを用いた。具体的には、200mm×200mm×2mmのステンレス板に高密度、高密着性のアルミナ溶射膜を被覆し、テトラメトキシシランを酢酸エチルで希釈した溶液を塗布乾燥後、紫外線照射により硬化させて封孔処理を行い、前記封孔処理した誘電体表面を研磨し、平滑にしてRmaxが5μmとなるように加工した電極を用いた。また、印加電極としては、中空の角型の純チタンパイプに対し、アース電極と同様の条件にて誘電体を被覆した電極を用いた。印加電極は複数作製し、アース電極に対向して設け放電空間を形成した。また、プラズマ発生に用いる電源としては、高周波電源CF-5000-13M(パール工業株式会社製)を用い、周波数13.56MHzで、5W/cm2の電力を供給した。
反応性ガス1:酸素 0.25体積%
反応性ガス2:インジウムアセチルアセトナート 1.2体積%
反応性ガス3:ジブチルスズジアセテート 0.05体積%。
得られた透明導電膜の100mm×80mmを機能性フィルム基板とし、これにパターニングを行った後、このITO透明電極を設けた機能性フィルム基板をイソプロピルアルコールで超音波洗浄し、乾燥窒素ガスで乾燥した。その後、機能性フィルム基板を市販の真空蒸着装置の基板ホルダーに固定した。一方で、モリブデン製抵抗加熱ボートにα-NPD200mgを、別のモリブデン製抵抗加熱ボートにホスト化合物としてCBP200mgを、さらに別のモリブデン製抵抗加熱ボートにバソキュプロイン(BCP)200mgを、別のモリブデン製抵抗加熱ボートにIr-1 100mgを、さらに別のモリブデン製抵抗加熱ボートにAlq3200mgをそれぞれ投入し、真空蒸着装置に取り付けた。
(機能性フィルムの評価)
機能性フィルムについては、ガスバリア性(水蒸気バリア性)の評価を行った。
水蒸気バリア性の評価
真空蒸着装置JEE-400(日本電子株式会社製)を用い、製造した機能性フィルムの表面に、水分と反応して腐食する金属である金属カルシウム(粒状)を蒸着させた。その後、乾燥窒素ガス雰囲気下で、厚さ0.2mmの石英ガラスに封止用紫外線硬化樹脂(ナガセケムテックス株式会社製)を介して金属カルシウム蒸着面を対面させて接着し、紫外線を照射して前記紫外線硬化樹脂を硬化させて本封止し、水蒸気バリア性評価用セルを作製した。
水蒸気バリア性評価用セルを、恒温恒湿度オーブンYamato Humidic ChamberIG47Mを用いて、60℃、90%RHの高温高湿下で保存し、カルシウム蒸着領域の腐食点の拡大速度を観察し、腐食点拡大速度評価を行った。前記腐食点拡大速度評価は、下記基準に従って評価を行った。
4:フィルムで封止されたカルシウム蒸着領域内において、腐食面積が5.0%に到達するまでの時間が1000時間以上2000時間未満である;
3:フィルムで封止されたカルシウム蒸着領域内において、腐食面積が5.0%に到達するまでの時間が500時間以上1000時間未満である;
2:フィルムで封止されたカルシウム蒸着領域内において、腐食面積が5.0%に到達するまでの時間が100時間以上500時間未満である;
1:フィルムで封止されたカルシウム蒸着領域内において、腐食面積が5.0%に到達するまでの時間が100時間未満である、あるいは、腐食が急激に進行するために腐食点拡大速度を判断できない。
水蒸気バリア性評価用セルを、恒温恒湿度オーブンYamato Humidic ChamberIG47Mを用いて、60℃、90%RHの高温高湿下で保存し、素子周辺部からのカルシウム腐食領域の拡大に伴う、カルシウム蒸着の残存領域の収縮を観察し、周辺収縮量評価を行った。前記腐食面積評価は、下記基準に従って評価を行った。
4:フィルムで封止されたカルシウム蒸着領域内において、周辺部からの面積の収縮が5.0%に到達するまでの時間が1000時間以上2000時間未満である;
3:フィルムで封止されたカルシウム蒸着領域内において、周辺部からの面積の収縮が5.0%に到達するまでの時間が500時間以上1000時間未満である;
2:フィルムで封止されたカルシウム蒸着領域内において、周辺部からの面積の収縮が5.0%に到達するまでの時間が100時間以上500時間未満である;
1:フィルムで封止されたカルシウム蒸着領域内において、周辺部からの面積の収縮が5.0%に到達するまでの時間が100時間未満である、あるいは、腐食が急激に進行するために周辺部からの面積の収縮の有無を判断できない。
機能性フィルムについて、半径6mmの曲率になるように180度の角度で100回の屈曲を繰り返す、屈曲耐久性試験を行った。当該屈曲耐性試験後の機能性フィルムについても、1に記載の未処理の機能性フィルムと同様に、水蒸気バリア性について評価を行った。
作製した有機EL素子については、以下の評価を行った。
有機EL素子を60℃、90%RHの環境下で通電を行い、0日から120日までのダークスポットや輝度ムラの発生等、発光ムラを目視で観察した。前記発光ムラ評価は、下記基準に従って評価を行った。
4:0日目でダークスポットまたは輝度ムラは観察されず、かつ、120日経過後の非発光領域が全発光面積の1.0%超10.0%以下である、あるいは、0日目にダークスポットまたは輝度ムラが観察され、その非発光領域が1%以下であり、かつ、120日経過後の非発光領域が全発光面積の1.0%以下である;
3:0日目にダークスポットまたは輝度ムラが観察され、その非発光領域が1%以下であり、かつ、120日経過後の非発光領域が全発光面積の1.0%超10.0%以下である;
2:0日目にダークスポットまたは輝度ムラが観察され、その非発光領域が1%以下であり、かつ、120日経過後の非発光領域が全発光面積の10%を超える、あるいは、0日目にダークスポットまたは輝度ムラが観察され、その非発光領域が1%を超えており、かつ、120日経過後の非発光領域が全発光面積の1.0%超10.0%以下である;
1:0日目にダークスポットまたは輝度ムラが観察され、その非発光領域が1%を超えており、かつ、120日経過後の非発光領域が全発光面積の10%を超える。
有機EL素子試料を40℃、90%RHの環境下で通電を行い、フィルムで封止された素子周辺部からの腐食の進行に伴う非発光領域(すなわち、発光領域の収縮の度合い)を0日から120日まで観察し、周辺部発光領域の収縮評価を行った。前記周辺部発光領域の収縮評価は、下記の基準に従って評価を行った。
4:0日目で発光領域の縮小は観察されず、120日経過後の非発光領域が全発光領域の1.0%超10.0%以下である、あるいは、0日目の非発光領域が全発光領域の0%超0.5%以下であり、かつ、120日経過後の非発光領域が全発光領域の1.0%以下である;
3:0日目の非発光領域が全発光領域は0%超0.5%以下であり、かつ、120日経過後の非発光領域が全発光領域の1.0%超10.0%以下である;
2:0日目の非発光領域が全発光領域の0%超0.5%以下であり、かつ、120日経過後の非発光領域が全発光領域の10.0%超である、あるいは、0日目非発光領域が全発光領域の0.5%超であり、かつ、120日経過後の非発光領域が全発光領域の1.0%超10.0%以下である;
1:0日目非発光領域が全発光領域の0.5%超であり、かつ、120日経過後の非発光領域が全発光領域の10.0%を超える。
12、22、32 樹脂基材、
13、23、33a、33b ハイブリッド層、
40 有機ELパネル、
41 機能性フィルム、
42 陽極、
43 有機EL層、
44 陰極、
45 接着剤層、
46 封止部材。
Claims (13)
- 樹脂基材と、前記樹脂基材上に位置する機能性無機層と、前記機能性無機層の少なくとも一方の面に配置されたハイブリッド層と、を含み、
前記ハイブリッド層が、ポリシロキサンおよび樹脂微粒子を含む、機能性フィルム。 - 前記ハイブリッド層が、前記樹脂基材と前記機能性無機層との間に位置する、請求項1に記載の機能性フィルム。
- 前記機能性無機層の前記樹脂基材とは反対側の面に前記ハイブリッド層が配置された、請求項1または2に記載の機能性フィルム。
- 2層以上積層された機能性無機層を含む、請求項1~3のいずれか1項に記載の機能性フィルム。
- ハイブリッド層の膜厚に対する機能性無機層の膜厚の比(機能性無機層の膜厚/ハイブリッド層の膜厚)が、0.001~10である、請求項1~4のいずれか1項に記載の機能性フィルム。
- 前記樹脂基材の両面に、前記機能性無機層と、前記機能性無機層の少なくとも一方の面に配置されたハイブリッド層とを有する、請求項1~5のいずれか1項に記載の機能性フィルム。
- 前記機能性無機層が、ガスバリア性無機層である、請求項1~6のいずれか1項に記載の機能性フィルム。
- 樹脂基材と、前記樹脂基材上に位置する機能性無機層と、前記機能性無機層の少なくとも一方の面に配置されたハイブリッド層と、を含む機能性フィルムの製造方法であって、
ポリシロキサンおよび樹脂微粒子を含む第1の塗布液を塗布して、前記ハイブリッド層を形成する工程(1)を含む、製造方法。 - 無機前駆体を含む第2の塗布液を塗布して塗膜を形成し、前記塗膜を改質処理して機能性無機層を形成する工程(2)をさらに含む、請求項8に記載の製造方法。
- 前記無機前駆体が、ポリシラザンを含む、請求項9に記載の製造方法。
- 前記改質処理が、真空紫外線照射によって行われる、請求項9または10に記載の製造方法。
- 電子デバイス本体と、請求項1~7のいずれか1項に記載の機能性フィルム、または請求項8~11のいずれか1項に記載の方法によって製造された機能性フィルムと、を含む、電子デバイス。
- 前記電子デバイス本体が、前記機能性フィルムによって封止されてなる、請求項12に記載の電子デバイス。
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WO2015029859A1 (ja) * | 2013-08-28 | 2015-03-05 | コニカミノルタ株式会社 | ガスバリアーフィルム及びガスバリアーフィルムの製造方法 |
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KR101642589B1 (ko) * | 2013-09-30 | 2016-07-29 | 주식회사 엘지화학 | 유기전자소자용 기판 및 이의 제조방법 |
US10424747B2 (en) | 2013-09-30 | 2019-09-24 | Lg Chem, Ltd. | Substrate for organic electronic device and method of manufacturing the same |
CN106103084A (zh) * | 2014-03-19 | 2016-11-09 | 富士胶片株式会社 | 功能性层叠膜、功能性层叠膜的制造方法、及包含功能性层叠膜的有机电致发光装置 |
JP2020104462A (ja) * | 2018-12-28 | 2020-07-09 | 株式会社レニアス | 透明積層体の製造方法 |
WO2024047806A1 (ja) * | 2022-08-31 | 2024-03-07 | 株式会社レニアス | 透明積層体の製造方法 |
Also Published As
Publication number | Publication date |
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CN104114362A (zh) | 2014-10-22 |
EP2815880A4 (en) | 2015-10-21 |
US9362527B2 (en) | 2016-06-07 |
JPWO2013122055A1 (ja) | 2015-05-11 |
EP2815880A1 (en) | 2014-12-24 |
CN104114362B (zh) | 2016-09-28 |
KR20140113717A (ko) | 2014-09-24 |
US20160013443A1 (en) | 2016-01-14 |
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