WO2017086048A1 - 光学反射フィルムおよび光学反射体 - Google Patents
光学反射フィルムおよび光学反射体 Download PDFInfo
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Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/08—Mirrors
- G02B5/0816—Multilayer mirrors, i.e. having two or more reflecting layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/023—Optical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/022—Mechanical properties
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/08—Mirrors
- G02B5/0816—Multilayer mirrors, i.e. having two or more reflecting layers
- G02B5/0825—Multilayer mirrors, i.e. having two or more reflecting layers the reflecting layers comprising dielectric materials only
- G02B5/0841—Multilayer mirrors, i.e. having two or more reflecting layers the reflecting layers comprising dielectric materials only comprising organic materials, e.g. polymers
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/26—Reflecting filters
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/28—Interference filters
- G02B5/281—Interference filters designed for the infrared light
- G02B5/282—Interference filters designed for the infrared light reflecting for infrared and transparent for visible light, e.g. heat reflectors, laser protection
Definitions
- the present invention relates to an optical reflection film and an optical reflector.
- an infrared shielding film that is attached to a window glass of a building or vehicle to block the transmission of solar heat rays.
- an optical reflection film including an optical interference film in which high refractive index layers and low refractive index layers are alternately laminated on a substrate is known.
- a high-refractive index layer and a low-refractive index layer are applied on a substrate by applying a wet coating method using a water-based coating liquid containing a water-soluble polymer and metal oxide particles.
- the structure formed by forming is known (see Patent Document 1 below).
- the lowermost layer of the optical interference film provided in contact with the base material contains metal oxide particles and an emulsion resin for the purpose of preventing the occurrence of curling due to thinning.
- a configuration is disclosed in which the thickness of the lowermost layer is 1.2 to 8 times the average thickness of layers other than the lowermost layer (see Patent Document 2 below).
- the infrared shielding film having the above-described structure has a problem of weather resistance that the optical interference film is cracked or peeled off due to repeated expansion and contraction due to moisture or heat after long-term use.
- an object of the present invention is to provide an optical reflection film and a light reflector that are prevented from cracking and peeling off in an optical interference film during long-term use and have excellent weather resistance.
- the present invention includes an optical interference film formed by alternately laminating a high refractive index layer and a low refractive index layer having a refractive index difference on a base material.
- the layer disposed closest to the base material is the bottom layer
- the layer farthest from the base material is the top layer.
- the average elastic modulus of the intermediate layer measured by the nanoindentation method is 2 GPa or more larger than the elastic modulus of the uppermost layer.
- the film thickness of the uppermost layer is 1.2 to 7 times the average film thickness of the intermediate layer.
- this invention is an optical reflector formed by providing such an optical reflection film on at least one surface of the substrate.
- the present invention having the above-described configuration, it is possible to prevent the occurrence of cracking and peeling of the optical interference film during long-term use, as described in the following examples, and to improve the weather resistance. It is possible to provide an optical reflective film and an optical reflector.
- FIG. 1 is a schematic cross-sectional view for explaining the configuration of the optical reflective film of the embodiment.
- the optical reflective film 1 of the embodiment is used by being mounted on a facility 200 exposed to sunlight for a long period of time, such as an outdoor window of a building or an automobile window.
- Such an optical reflection film 1 includes an optical interference film 5 formed by alternately laminating a high refractive index layer 5H and a low refractive index layer 5L having a refractive index difference on one main surface of a substrate 3. I have.
- the optical reflection film 1 may be provided with an adhesive layer 7 on the optical interference film 5, for example, and is attached to the equipment 200 through the adhesive layer 7.
- the configuration of the optical reflection film 1 in which the optical interference film 5 is provided only on one main surface of the base material 3 is illustrated, but the optical reflection film 1 has the optical interference film 5 provided on both surfaces of the base material 3. It may be a configuration.
- optical properties of such an optical reflection film 1 are such that the transmittance in the visible light region shown in JIS R3106-1998 is 50% or more, preferably 75% or more, more preferably 85% or more.
- the optical reflection film 1 is, for example, a near-infrared shielding film, it is preferable that the optical reflection film 1 has a region with a reflectance exceeding 50% in a wavelength region of 900 nm to 1400 nm.
- the embodiment will be described assuming that the reflective film 1 is a near-infrared shielding film.
- the reflective film 1 is not limited to being a near-infrared shielding film, and may be a film that reflects and shields infrared rays and ultraviolet rays, and has a reflectance of 50% in each wavelength region. It is assumed that the film thickness and the constituent material of each layer are set so as to exceed.
- the total thickness of the optical reflection film 1 is preferably 12 ⁇ m to 315 ⁇ m, more preferably 15 ⁇ m to 200 ⁇ m, and still more preferably 20 ⁇ m to 100 ⁇ m.
- the preferred range of the number of layers of the high refractive index layer 5H and the low refractive index layer 5L per one side of the substrate 3 is 100 layers or less, 9 layers or more, more preferably 45 from the viewpoint of productivity. 15 layers or less, more preferably 45 layers or less and 21 layers or more. Note that the preferable range of the total number of layers of the high refractive index layer 5H and the low refractive index layer 5L is applicable even when the layers are laminated only on one side of the substrate 3, and the layers are simultaneously laminated on both sides of the substrate 3.
- the total number of the high refractive index layer 5H and the low refractive index layer 5L on one surface and the other surface of the substrate 3 may be the same or different. It may be.
- a layer farthest from the base material 3 is referred to as an uppermost layer A.
- a layer disposed closest to the base material 3 is referred to as a lowermost layer C.
- each layer laminated between the uppermost layer A and the lowermost layer C is referred to as an intermediate layer B.
- the uppermost layer A and the lowermost layer C may be either the high refractive index layer 5H or the low refractive index layer 5L.
- adhesion to the base material 3 of the lowermost layer C, resistance to liquid drip by the drying air at the time of coating and drying when coating the uppermost layer A, and further application of an adhesive layer or a hard coat layer to the uppermost layer A From the viewpoint of excellent properties and adhesiveness, it is preferable that the lowermost layer C and the uppermost layer A of the optical reflective film 1 are composed of a low refractive index layer 5L as illustrated.
- the elastic properties, the film thickness ratio, other characteristics, the optical characteristics such as the refractive index and the reflectance will be described in order, and then the high refractive index layer 5H and the low refractive index layer 5L.
- the structure and constituent materials will be described.
- the elastic moduli of the uppermost layer A, the intermediate layer B, and the lowermost layer C have a specific relationship. That is, the average elastic modulus [Eb] of the intermediate layer B is 2 GPa or more larger than the elastic modulus [Ea] of the uppermost layer A, and [Eb ⁇ Ea] ⁇ 2 GPa. Further, as a more preferable relationship, the average elastic modulus [Eb] of the intermediate layer B is 2 GPa or more larger than the elastic modulus [Ec] of the lowermost layer C, and [Eb ⁇ Ec] ⁇ 2 GPa.
- the elastic modulus [Ec] of the lowermost layer C is larger than the elastic modulus [Ea] of the uppermost layer A, and [Ec]> [Ea] and [Ec ⁇ Ea]> 0.
- the elastic modulus [Ea] of the uppermost layer A is preferably 8 GPa or more and 15 GPa or less.
- the elastic modulus is an elastic modulus measured by a nanoindentation method, and is a value measured for a single layer film formed on a hard substrate.
- the average elastic modulus [Eb] of the intermediate layer B is an average value of the elastic moduli of the high refractive index layer 5H and the low refractive index layer 5L constituting the intermediate layer B.
- the elastic modulus of the uppermost layer A, the intermediate layer B, and the lowermost layer C in the optical interference film 5 can be adjusted by the material constituting each layer.
- the uppermost layer A, the intermediate layer B, and the lowermost layer C contain a water-soluble polymer, inorganic oxide particles, and an emulsion resin.
- the elastic modulus of the uppermost layer A, the intermediate layer B, and the lowermost layer C is adjusted by adjusting the content of the inorganic oxide particles and the content of at least one of the emulsion resins with respect to the content of the water-soluble polymer.
- the average film thickness [tb] of the intermediate layer B is an average value of the film thicknesses of the high refractive index layer 5H and the low refractive index layer 5L constituting the intermediate layer B.
- the high refractive index layer 5H and the low refractive index layer 5L constituting the optical interference film 5 include water-soluble polymer and inorganic oxide particles as essential components, as will be described in detail later.
- at least one of the uppermost layer A preferably contains an emulsion resin, and in particular, the uppermost layer A preferably contains an emulsion resin.
- the emulsion resin used here preferably has an average particle size of 60 nm or less. Details of the emulsion resin will be described later.
- the refractive index difference between the high refractive index layer 5H and the low refractive index layer 5L adjacent to each other in the optical interference film 5 is preferably 0.1 or more, more preferably 0.25 or more, and further preferably. Is 0.3 or more, more preferably 0.35 or more, and most preferably 0.4 or more.
- This refractive index difference and the required number of layers can be calculated using commercially available optical design software. For example, in order to obtain a near-infrared reflectance of 90% or more, if the difference in refractive index is smaller than 0.1, it is necessary to laminate 200 layers or more, which not only lowers productivity but also causes scattering at the lamination interface. Increases and decreases transparency. For this reason, it may become very difficult to manufacture without trouble.
- the difference in refractive index between the high refractive index layer 5H and the low refractive index layer 5L is preferable as described above. It is preferable to be within a range of a difference in refractive index.
- the uppermost layer A is formed as a layer for protecting the film, or when the lowermost layer C is formed as an adhesion improving layer with the substrate 3, the uppermost layer A or the lowermost layer C is used.
- a configuration outside the range of the preferable refractive index difference may be used.
- the high refractive index layer 5H includes the first water-soluble polymer and the first inorganic oxide particles as essential components, and if necessary, is selected from the group consisting of a curing agent, a surfactant, an emulsion resin, and various additives. It may further contain at least one kind.
- an emulsion resin may be contained in the high refractive index layer 5H.
- an emulsion resin is preferably contained in the high refractive index layer 5H constituting the uppermost layer A.
- the refractive index of the high refractive index layer 5H as described above is preferably 1.80 to 2.50, more preferably 1.90 to 2.20.
- the thickness per layer of the high refractive index layer 5H is preferably 20 to 800 nm, and more preferably 50 to 350 nm. However, the film thickness of each high refractive index layer 5H is set so that the film thicknesses of the uppermost layer A, the intermediate layer B, and the lowermost layer C satisfy the above-described relationship.
- the high refractive index layer 5H and the adjacent low refractive index layer 5L may have a clear interface between them or may be gradually changed.
- the point of [refractive index + ⁇ n / 2] is regarded as the layer interface, and the thickness per layer of the high refractive index layer 5H is measured. The same applies to the measurement of the thickness of the low refractive index layer 5L described later.
- the inorganic oxide concentration profile of the laminated film which is the optical interference film 5 formed by alternately laminating the high refractive index layer 5H and the low refractive index layer 5L, is etched from the surface to the depth direction using a sputtering method. It can be seen by using an XPS surface analysis apparatus, setting the outermost surface to 0 nm, sputtering at a rate of 0.5 nm / min, and measuring the atomic composition ratio. It is also possible to view the cut surface by cutting the laminated film and measuring the atomic composition ratio with an XPS surface analyzer. When the concentration of the inorganic oxide changes discontinuously in the mixed region, the boundary can be seen by a tomographic photograph using a transmission electron microscope (TEM).
- TEM transmission electron microscope
- the XPS surface analyzer is not particularly limited, and any model can be used, but ESCALAB-200R manufactured by VG Scientific Fix Co. was used. Mg is used for the X-ray anode, and measurement is performed at an output of 600 W (acceleration voltage: 15 kV, emission current: 40 mA).
- the first inorganic oxide particles contained in the high refractive index layer 5H are preferably inorganic oxide particles having a refractive index of 2.0 or more.
- Specific examples of the material include metal oxides such as zirconium oxide (ZrO 2 ), zinc oxide (ZnO), and titanium oxide (TiO 2 ). Of these, it is preferable to use titanium oxide (TiO 2 ) from the viewpoint of the stability of the coating solution for forming the high refractive index layer 5H.
- TiO 2 it is particularly preferable to use rutile type titanium oxide having a high refractive index and a low catalytic activity. If the catalytic activity is low, side reactions (photocatalytic reaction) that occur in the high refractive index layer 5H and adjacent layers can be suppressed, and the weather resistance can be increased.
- the first inorganic oxide particles may be particles in which titanium oxide particles are coated with a silicon-containing hydrated oxide (hereinafter referred to as coated particles).
- coated particles mean titanium dioxide (TiO 2 ) particles.
- coating means a state in which a silicon-containing hydrated oxide is adhered to at least a part of the surface of the titanium oxide particles. That is, the surface of the titanium oxide particles used as the first inorganic oxide particles may be completely covered with a silicon-containing hydrated oxide, and a part of the surface of the titanium oxide particles may be hydrated with silicon-containing. It may be coated with an oxide. From the viewpoint that the refractive index of the coated titanium oxide particles is controlled by the coating amount of the silicon-containing hydrated oxide, it is preferable that a part of the surface of the titanium oxide particles is coated with the silicon-containing hydrated oxide. .
- the first inorganic oxide particles may be rutile type titanium oxide particles coated with silicon-containing hydrated oxide, and anatase type titanium oxide particles coated with silicon-containing hydrated oxide. Or a mixture of these. Among these, rutile type titanium oxide particles coated with silicon-containing hydrated oxide are more preferable.
- the rutile type titanium oxide particles have lower photocatalytic activity than the anatase type titanium oxide particles, so the weather resistance of the high refractive index layer 5H and the adjacent low refractive index layer 5L is increased, and the refractive index is further increased. That is why.
- the aqueous solution containing titanium oxide particles used for the production of the first inorganic oxide particles has a surface of an aqueous titanium oxide sol having a pH of 1.0 to 3.0 and a positive zeta potential of the titanium particles. What was hydrophobized and disperse
- the content of the first inorganic oxide particles in the high refractive index layer 5H is preferably 15 to 95% by mass, and 20 to 88% by mass with respect to 100% by mass of the solid content of the high refractive index layer 5H. More preferably, it is more preferably 30 to 85% by mass.
- the average particle size (primary average particle size) of the first inorganic oxide particles is preferably 2 to 100 nm, more preferably 3 to 50 nm, and even more preferably 4 to 30 nm.
- the average particle size (primary average particle size) of the first inorganic oxide particles is determined by observing the particles themselves or the particles appearing on the cross section or surface of the refractive index layer with an electron microscope, and 1,000 arbitrary particles. The particle size is measured as a simple average value (number average).
- the particle diameter of each particle is represented by a diameter assuming a circle equal to the projected area.
- first inorganic oxide particles are coated particles in which titanium oxide particles are coated with a silicon-containing hydrated oxide
- volume average particles of titanium oxide particles that are not coated with the silicon-containing hydrated oxide is preferably 30 nm or less, more preferably 1 to 30 nm, still more preferably 5 to 15 nm, and most preferably 6 to 10 nm.
- a volume average particle size of 1 nm or more and 30 nm or less is preferable from the viewpoint of low haze and excellent visible light transmittance.
- the volume average particle size of the titanium oxide particles used for the coated particles refers to a method of observing the particles themselves using a laser diffraction scattering method, a dynamic light scattering method, or an electron microscope, and a cross section or surface of the refractive index layer.
- the titanium oxide particles in the coated particles are preferably monodispersed.
- the monodispersion here means that the monodispersity obtained by the following formula is 40% or less. This monodispersity is more preferably 30% or less, and particularly preferably 0.1 to 20%.
- Monodispersity [(standard deviation obtained from volume particle size distribution) / (volume average particle size)] ⁇ 100
- the high refractive index layer 5H and the low refractive index layer 5L are caused by the interaction between the silicon-containing hydrated oxide and the first water-soluble polymer. It is possible to prevent the intermixing of the resin and the problem of water-soluble polymer degradation and choking due to the photocatalytic activity of titanium oxide when using not only rutile-type titanium oxide particles but also anatase-type titanium oxide particles. There is an effect.
- the volume average particle diameter of the coated particles is preferably 2 to 31 nm, more preferably 6 to 16 nm, and further preferably 7 to 11 nm.
- the volume average particle diameter of the first inorganic oxide particles is preferably 2 to 31 nm from the viewpoint of optical properties such as near infrared shielding properties, transparency, and haze.
- the average particle size (primary average particle size) of the titanium oxide particles in the coated particles is preferably 30 nm or less, more preferably 1 to 30 nm, still more preferably 1 to 20 nm. Most preferably, it is 10 nm.
- a primary average particle diameter of 1 nm or more and 30 nm or less is preferable from the viewpoint of low haze and excellent visible light transmittance.
- the average particle diameter (primary average particle diameter) of the coated particles is preferably 2 to 31 nm, more preferably 2 to 21 nm, and further preferably 2 to 11 nm.
- the primary average particle diameter of the coated particles is preferably 2 to 31 nm from the viewpoint of optical properties such as near infrared shielding properties, transparency and haze.
- aqueous solution containing titanium oxide particles is hydrolyzed by heating, or an aqueous solution containing titanium oxide particles is neutralized by adding an alkali to obtain titanium oxide having an average particle size of 1 to 30 nm. Thereafter, a slurry in which the titanium oxide particles and the mineral acid are mixed so that the titanium oxide particles / mineral acid is in a range of 1 / 0.5 to 1/2 in terms of molar ratio is 50 ° C. or more.
- a silicon compound eg, sodium silicate aqueous solution
- silicon hydrous oxide is deposited on the surface of the titanium oxide particles. Surface treatment.
- impurities are removed from the obtained slurry of surface-treated titanium oxide particles (a method described in JP-A-10-158015).
- a titanium oxide sol stabilized at pH in the acidic range obtained by peptizing a titanium oxide such as hydrous titanium oxide with a monobasic acid or a salt thereof, and an alkyl silicate as a dispersion stabilizer are mixed by a conventional method. And neutralization (method described in JP-A-2000-053421).
- a stable aqueous sol of composite colloidal particles containing silicon dioxide is produced.
- silicate eg, sodium silicate aqueous solution
- a stable aqueous sol of composite colloidal particles containing silicon dioxide is produced.
- the obtained composite aqueous sol containing titanium oxide is converted to 100 parts by mass in terms of metal oxide TiO 2
- the obtained composite aqueous sol containing silicon dioxide is converted to 2 to 100 in terms of metal oxide SiO 2.
- aging is carried out at 80 ° C. for 1 hour (the method described in JP-A-2000-063119).
- V a compound selected from a hydrosol of titanium oxide obtained by peptizing hydrous titanium oxide, an organoalkoxysilane (R1nSiX4-n) as a stabilizer, or hydrogen peroxide and an aliphatic or aromatic hydroxycarboxylic acid Is added, the pH of the solution is adjusted to 3 or more and less than 9, and after aging, a desalting treatment is performed (method described in Japanese Patent No. 4550753).
- the first inorganic oxide particles can be produced by the methods (i) to (v) above.
- the following methods (1) to (4) may be mentioned.
- the amount of silicon-containing hydrated oxide is adjusted by adjusting the amount of silicon compound added to the titanium oxide particles used.
- the coating amount of the silicon-containing hydrated oxide is adjusted by adjusting the amount of the corresponding SiO 2 .
- the coating amount of the silicon-containing hydrated oxide is adjusted by adjusting the amount of the organoalkoxysilane used.
- the addition amount of the alkyl silicate is adjusted.
- the first content is 100% by mass with respect to the solid content of the entire suspension.
- the preferred solid content of the inorganic oxide particles is 1 to 40% by mass.
- the solid content is more preferably 15 to 25% by mass. This makes it possible to improve the productivity by increasing the solid content concentration and reducing the solvent volatilization load by setting the solid content to 1% by mass or more, and the solid content is 40% by mass. It is because aggregation by high particle density can be prevented by making it below, and the defect at the time of application
- the pH range of the suspension containing the titanium oxide particles coated with the silicon-containing hydrated oxide is preferably 3 to 9, and preferably 4 to 8. More preferably. It is because the change of the volume average particle diameter due to alkali dissolution can be suppressed by setting the pH of the suspension to 9 or less, and the handleability can be improved by setting the pH of the suspension to 3 or more. .
- the coating amount of the silicon-containing hydrated oxide is preferably 3 to 30% by mass, more preferably 3 to 10% by mass as SiO 2 with respect to the titanium oxide particles. More preferably, it is 3 to 8% by mass.
- the coating amount is 3 to 30% by mass, the high refractive index layer 5H can be easily increased in refractive index, and the coated particles can be stably formed.
- the “silicon-containing hydrated oxide” may be any of a hydrate of an inorganic silicon compound, a hydrolyzate and / or a condensate of an organosilicon compound, and more preferably has a silanol group.
- inorganic oxide particles may be included in addition to the first inorganic oxide particles.
- various ionic dispersants and protective agents can be used so as not to aggregate with the first inorganic oxide particles.
- inorganic oxide particles that can be used in addition to the first inorganic oxide particles include titanium dioxide, zirconium oxide, zinc oxide, synthetic amorphous silica, colloidal silica, alumina, colloidal alumina, lead titanate, and lead oxide.
- the first is a particle in which at least one of the plurality of high refractive index layers 5H is coated with titanium oxide particles with a silicon-containing hydrated oxide.
- the first inorganic oxide particles according to the present invention are particularly preferably included in all layers of the plurality of high refractive index layers 5H.
- the first inorganic oxide particles may be contained in the one high refractive index layer 5H.
- the first water-soluble polymer contained in the high refractive index layer 5H functions as a binder.
- the first water-soluble polymer may be the same component as the second water-soluble polymer contained in the low refractive index layer 5L described below, or may be a different component. More preferably, the constituent components of the water-soluble polymer and the second water-soluble polymer are different.
- the G2 glass filter When the first water-soluble polymer or the second water-soluble polymer described later is dissolved in water at a concentration of 0.5% by mass at the temperature at which the water-soluble polymer is most dissolved, the G2 glass filter ( The mass of the insoluble matter that is filtered off when filtering through a maximum pore of 40 to 50 ⁇ m is within 50 mass% of the added water-soluble polymer.
- first water-soluble polymer examples include polymers having reactive functional groups, gelatin, celluloses, and thickening polysaccharides. These first water-soluble polymers may be used alone or in combination of two or more.
- the first water-soluble polymer may be a synthetic product or a commercially available product. Hereinafter, the first water-soluble polymer will be described in detail.
- Polymer having reactive functional group examples include polyvinyl alcohols, polyvinylpyrrolidones, polyacrylic acid, acrylic acid-acrylonitrile copolymer, potassium acrylate-acrylonitrile copolymer, vinyl acetate-acrylic ester copolymer.
- Acrylic resin such as acrylic acid-acrylic acid ester copolymer, styrene-acrylic acid copolymer, styrene-methacrylic acid copolymer, styrene-methacrylic acid-acrylic acid ester copolymer, styrene- ⁇ - Styrene acrylic resin such as methylstyrene-acrylic acid copolymer or styrene- ⁇ -methylstyrene-acrylic acid-acrylic acid ester copolymer, styrene-sodium styrenesulfonate copolymer, styrene-2-hydroxyethyl acrylate Copolymer Styrene-2-hydroxyethyl acrylate-potassium styrene sulfonate copolymer, styrene-maleic acid copolymer, styrene-maleic anhydride copolymer, vinyl naphthalate
- the polyvinyl alcohol preferably used includes various modified polyvinyl alcohols in addition to ordinary polyvinyl alcohol obtained by hydrolyzing polyvinyl acetate.
- the polyvinyl alcohol obtained by hydrolyzing vinyl acetate preferably has an average degree of polymerization of 1,000 or more, and particularly preferably has an average degree of polymerization of 1,500 to 5,000.
- the degree of saponification is preferably 70 to 100%, particularly preferably 80 to 99.5%.
- Anion-modified polyvinyl alcohol is described in, for example, polyvinyl alcohol having an anionic group as described in JP-A-1-206088, JP-A-61-237681 and JP-A-63-307979.
- examples thereof include a copolymer of vinyl alcohol and a vinyl compound having a water-soluble group, and a modified polyvinyl alcohol having a water-soluble group as described in JP-A-7-285265.
- Nonionic modified polyvinyl alcohol includes, for example, a polyvinyl alcohol derivative in which a polyalkylene oxide group is added to a part of vinyl alcohol as described in JP-A-7-9758, and JP-A-8-25795.
- the block copolymer of the vinyl compound and vinyl alcohol which have the described hydrophobic group is mentioned.
- Polyvinyl alcohol can be used in combination of two or more, such as the degree of polymerization and the type of modification.
- Examples of the cation-modified polyvinyl alcohol include primary to tertiary amino groups and quaternary ammonium groups in the main chain or side chain of the polyvinyl alcohol as described in, for example, JP-A-61-110483. It is obtained by saponifying a copolymer of an ethylenically unsaturated monomer having a cationic group and vinyl acetate.
- Examples of the ethylenically unsaturated monomer having a cationic group include trimethyl- (2-acrylamido-2,2-dimethylethyl) ammonium chloride and trimethyl- (3-acrylamido-3,3-dimethylpropyl) ammonium chloride.
- the ratio of the cation-modified group-containing monomer in the cation-modified polyvinyl alcohol is 0.1 to 10 mol%, preferably 0.2 to 5 mol%, relative to vinyl acetate.
- gelatin As gelatin, various types of gelatin that have been widely used in the field of silver halide photographic light-sensitive materials can be applied. For example, in addition to acid-processed gelatin and alkali-processed gelatin, enzyme processing is performed in the gelatin manufacturing process. Enzyme-treated gelatin and gelatin derivatives, that is, modified by treatment with a reagent having an amino group, an imino group, a hydroxyl group, or a carboxyl group as a functional group in the molecule and a group obtained by reaction with it may be used. Well-known methods for producing gelatin are well known. H. James: The Theory of Photographic Process 4th. ed.
- gelatin When gelatin is used as the first water-soluble polymer, a gelatin hardener can be added as necessary.
- hardener known compounds that are used as hardeners for ordinary photographic emulsion layers can be used.
- vinyl sulfone compounds urea-formalin condensates, melanin-formalin condensates, epoxy compounds And organic hardeners such as aziridine compounds, active olefins and isocyanate compounds, and inorganic polyvalent metal salts such as chromium, aluminum and zirconium.
- a water-soluble cellulose derivative can be preferably used, for example, a water-soluble cellulose derivative such as carboxymethyl cellulose (cellulose carboxymethyl ether), methyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, or a carboxylic acid group.
- a water-soluble cellulose derivative such as carboxymethyl cellulose (cellulose carboxymethyl ether), methyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, or a carboxylic acid group.
- carboxymethyl cellulose (cellulose carboxymethyl ether), carboxyethyl cellulose and the like which are contained celluloses.
- Other examples include cellulose derivatives such as nitrocellulose, cellulose acetate propionate, cellulose acetate, and cellulose sulfate.
- the thickening polysaccharide is not particularly limited, and examples thereof include generally known natural simple polysaccharides, natural complex polysaccharides, synthetic simple polysaccharides, and synthetic complex polysaccharides. Details of these polysaccharides Can refer to “Biochemical Encyclopedia (2nd edition), Tokyo Chemical Doujin Publishing”, “Food Industry”, Vol. 31 (1988), p. 21.
- the thickening polysaccharide here is a polymer of saccharides and has many hydrogen bonding groups in the molecule, and the difference in viscosity at low temperature and viscosity at high temperature due to the difference in hydrogen bonding force between molecules depending on the temperature. Is a polysaccharide with great properties. Further, the thickening polysaccharide causes an increase in viscosity which is considered to be due to hydrogen bonding with the inorganic oxide particles at low temperatures when the inorganic oxide particles are added.
- the viscosity increase width is a polysaccharide which, when added, causes the viscosity at 15 ° C.
- 1.0 mPa ⁇ s or more preferably 5.0 mPa ⁇ s or more, more preferably 10.0 mPa ⁇ s or more. It is a polysaccharide having the ability to increase viscosity.
- Examples of the thickening polysaccharide applicable as the first water-soluble polymer include, for example, galactan (eg, agarose, agaropectin, etc.), galactomannoglycan (eg, locust bean gum, guaran, etc.), xyloglucan (eg, Tamarind gum, etc.), glucomannoglycan (eg, salmon mannan, wood-derived glucomannan, xanthan gum, etc.), galactoglucomannoglycan (eg, softwood-derived glycan), arabinogalactoglycan (eg, soybean-derived glycan, microorganism) Glycans derived), glucolanoglycans (eg gellan gum, etc.), glycosaminoglycans (eg hyaluronic acid, keratan sulfate, etc.), alginic acid and alginates, agar, ⁇ -carrageenan,
- the structural unit has no carboxylic acid group or sulfonic acid group.
- thickening polysaccharides include pentoses such as L-arabitose, D-ribose, 2-deoxyribose and D-xylose, and hexoses such as D-glucose, D-fructose, D-mannose and D-galactose. It is preferable that it is a polysaccharide which consists only of.
- tamarind seed gum known as xyloglucan whose main chain is glucose and side chain is glucose
- guar gum known as galactomannan whose main chain is mannose and side chain is glucose
- cationized guar gum Hydroxypropyl guar gum
- locust bean gum locust bean gum
- tara gum arabinogalactan whose main chain is galactose and whose side chain is arabinose
- tamarind, guar gum, cationized guar gum, and hydroxypropyl guar gum are particularly preferable.
- first water-soluble polymer two or more types of thickening polysaccharides can be used in combination.
- polyvinyl alcohol is preferable as the first water-soluble polymer.
- other water-soluble polymer may be used in combination with polyvinyl alcohol.
- the content of the other water-soluble polymer used in combination is 100% by mass of the solid content of the high refractive index layer 5H. In contrast, 0.5 to 10% by mass can be used.
- the weight average molecular weight of the first water-soluble polymer is preferably 1,000 or more and 300,000 or less, and more preferably 3,000 or more and 200,000 or less.
- the weight average molecular weight in the present invention can be measured by a known method, for example, it can be measured by a static light scattering method, a gel permeation chromatograph method (GPC method), TOFMASS, etc. It is measured by a gel permeation chromatograph method (GPC method) which is a publicly known method.
- the first water-soluble polymer is preferably contained in a range of 5.0% by mass or more and 50% by mass or less with respect to 100% by mass of the solid content of the high refractive index layer 5H, and 10% by mass or more, and It is more preferable to make it contain in 40 mass% or less.
- the emulsion resin when used in combination with the first water-soluble polymer, for example, it may be contained by 3.0% by mass or more. If the amount of water-soluble polymer is small, the film surface is disturbed and the transparency tends to deteriorate during drying after coating the refractive index layer. On the other hand, if the content is 50% by mass or less, the relative content of the inorganic oxide becomes appropriate, and it becomes easy to increase the refractive index difference between the high refractive index layer 5H and the low refractive index layer 5L.
- the curing agent is for curing the first water-soluble polymer as a binder.
- the curing agent that can be used together with the first water-soluble polymer is not particularly limited as long as it causes a curing reaction with the water-soluble polymer.
- boric acid and its salt are preferable as the curing agent.
- known ones can be used, and in general, a compound having a group capable of reacting with polyvinyl alcohol or a compound that promotes the reaction between different groups possessed by polyvinyl alcohol. Select and use.
- the curing agent include, for example, epoxy curing agents (diglycidyl ethyl ether, ethylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether, 1,6-diglycidyl cyclohexane, N, N-diglycidyl- 4-glycidyloxyaniline, sorbitol polyglycidyl ether, glycerol polyglycidyl ether, etc.), aldehyde curing agents (formaldehyde, glioxal, etc.), active halogen curing agents (2,4-dichloro-4-hydroxy-1,3,5) , -S-triazine, etc.), active vinyl compounds (1,3,5-trisacryloyl-hexahydro-s-triazine, bisvinylsulfonylmethyl ether, etc.), aluminum alum, borax and the like.
- epoxy curing agents diglycidyl e
- Boric acid or a salt thereof refers to an oxygen acid having a boron atom as a central atom and a salt thereof, specifically, orthoboric acid, diboric acid, metaboric acid, tetraboric acid, pentaboric acid, and octaboron. Examples include acids and their salts.
- Boric acid having a boron atom and a salt thereof as a curing agent may be used alone or in a mixture of two or more. Particularly preferred is a mixed aqueous solution of boric acid and borax.
- An aqueous solution of boric acid and borax can be added only in a relatively dilute aqueous solution, but a thick aqueous solution can be obtained by mixing the two, and the coating solution can be concentrated. Further, there is an advantage that the pH of the aqueous solution to be added can be controlled relatively freely.
- boric acid it is preferable to use at least one of boric acid, a salt thereof, and borax as a curing agent.
- boric acid and its salt and borax the first inorganic oxide particles and the first water-soluble polymer polyvinyl alcohol OH group and hydrogen bond network are more easily formed, As a result, it is considered that interlayer mixing between the high refractive index layer 5H and the low refractive index layer 5L is suppressed, and a preferable near-infrared shielding characteristic is achieved.
- the film surface temperature of the coating film is once cooled to about 15 ° C., and then the film surface is dried.
- the effect can be expressed more preferably.
- the content of the curing agent in the high refractive index layer 5H is preferably 1 to 10% by mass and more preferably 2 to 6% by mass with respect to 100% by mass of the solid content of the high refractive index layer 5H. .
- the total amount of the curing agent used is preferably 1 mg to 500 mg per 1 g of polyvinyl alcohol, more preferably 20 mg to 200 mg per 1 g of polyvinyl alcohol.
- the surfactant is intended to improve applicability when the high refractive index layer 5H and the low refractive index layer 5L are applied on the substrate in the manufacturing process of the optical reflection film.
- an anionic surfactant As such a surfactant, an anionic surfactant, a nonionic surfactant, an amphoteric surfactant and the like can be used, and an anionic surfactant and an amphoteric surfactant are more preferable.
- Preferred compounds as the anionic surfactant include those containing a hydrophobic group having 8 to 30 carbon atoms and a sulfonic acid group or a salt thereof in one molecule.
- the amphoteric surfactant sulfobetaine type, carbobetaine type and the like are preferably used.
- Anionic surfactants include alkyl benzene sulfonate, alkyl naphthalene sulfonate, alkane or olefin sulfonate, alkyl sulfate ester salt, polyoxyethylene alkyl or alkyl aryl ether sulfate ester, alkyl phosphate, alkyl diphenyl ether
- a surfactant selected from the group consisting of disulfonates, ether carboxylates, alkylsulfosuccinic acid ester salts, ⁇ -sulfo fatty acid esters and fatty acid salts, condensates of higher fatty acids with amino acids, naphthenic acid salts, etc. may be used.
- anionic surfactants are alkylbenzene sulfonates (especially those of linear alkyls), alkanes or olefin sulfonates (especially secondary alkane sulfonates, ⁇ -olefin sulfonates), alkyl sulfates Salts, polyoxyethylene alkyl or alkyl aryl ether sulfates (especially polyoxyethylene alkyl ether sulfates), alkyl phosphates (especially monoalkyl type), ether carboxylates, alkyl sulfosuccinates, ⁇ -sulfo fatty acid esters and A surfactant selected from the group consisting of fatty acid salts, and alkylsulfosuccinate is particularly preferable.
- amphoteric surfactant a surfactant selected from the group consisting of imidazoline type, amidopropyl betaine type, sulfobetaine type, amidoamine oxide type, carbobetaine type and the like can be used.
- amphoteric surfactant preferably used. It is a surfactant selected from the group consisting of sulfobetaine type and carbobetaine type.
- the content of the surfactant in the high refractive index layer 5H is preferably 0.001 to 0.1% by mass, with the total mass of the coating liquid of the high refractive index layer 5H being 100% by mass, preferably 0.005 to More preferably, it is 0.05 mass%.
- the emulsion resin is resin particles obtained by keeping an oil-soluble monomer in an emulsion state in an aqueous solution containing a dispersant and emulsion polymerization using a polymerization initiator.
- the resin constituting the emulsion resin (resin particles) includes homopolymers or copolymers of ethylene monomers such as acrylic esters, methacrylic esters, vinyl compounds, and styrene compounds, and diene compounds such as butadiene and isoprene. Examples thereof include acrylic resins, styrene-butadiene resins, ethylene-vinyl acetate resins, and the like.
- dispersant used in emulsion polymerization of an emulsion resin in addition to a low molecular weight dispersant such as alkyl sulfonate, alkyl benzene sulfonate, diethylamine, ethylenediamine, and quaternary ammonium salt, examples thereof include polymer dispersants such as oxyethylene nonylphenyl ether, polyoxyethylene lauryl ether, hydroxyethyl cellulose, and polyvinylpyrrolidone, and polymer dispersants containing a hydroxyl group.
- the polymer dispersant containing a hydroxyl group is a polymer dispersant having a weight average molecular weight of 10,000 or more, and has a hydroxyl group substituted at the side chain or terminal.
- an acrylic polymer such as sodium polyacrylate or polyacrylamide is used.
- examples of such polymers include 2-ethylhexyl acrylate copolymer, polyethers such as polyethylene glycol and polypropylene glycol, and polyvinyl alcohol. Polyvinyl alcohol is particularly preferable.
- Polyvinyl alcohol used as a polymer dispersant is an anion-modified polyvinyl alcohol having an anionic group such as a cation-modified polyvinyl alcohol or a carboxyl group in addition to ordinary polyvinyl alcohol obtained by hydrolysis of polyvinyl acetate. Further, modified polyvinyl alcohol such as silyl-modified polyvinyl alcohol having a silyl group is also included.
- Polyvinyl alcohol has a greater effect of suppressing the occurrence of cracks when the average degree of polymerization is higher, but when the average degree of polymerization is within 5000, the viscosity of the emulsion resin is not high and is easy to handle during production. Accordingly, the average degree of polymerization is preferably 300 to 5000, more preferably 1500 to 5000, and particularly preferably 3000 to 4500.
- the saponification degree of polyvinyl alcohol is preferably 70 to 100 mol%, more preferably 80 to 99.5 mol%.
- the emulsion containing the emulsion resin one having a pH of 3 to 10 is preferable from the viewpoint of mixing with the resin binder, inorganic oxide particles, other additives, and the like, and the Tg of the resin is preferably 100 ° C. or lower.
- Homopolymers or copolymers of ethylene monomers such as acrylic esters, methacrylic esters, vinyl compounds, styrene compounds, and diene compounds such as butadiene and isoprene used as emulsion resins are commercially available products. Available.
- Mobile 718A, 710A, 731A, LDM7582, 5450, 6960 (manufactured by Nippon Synthetic Chemical Industry Co., Ltd.), Superflex 150, 170, 300, 500M (manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), Adekabon titer HUX-232, HUX-380, HUX-386, HUX-830, HUX-895 (manufactured by ADEKA Co., Ltd.), AE116, AE120A, AE200A, AE336B, AE981A, AE986B (manufactured by Etec Co., Ltd.), and Acryt UW-309, UW-319SX, UW-520 (manufactured by Taisei Fine Chemical Co., Ltd.).
- any of an anionic emulsion resin, a cationic emulsion resin, and a nonionic emulsion resin can be used.
- an anionic emulsion resin is used.
- the average particle size of the emulsion resin used here is a volume average particle size, preferably 150 nm or less, and particularly preferably 60 nm or less.
- emulsion resin has the said average particle diameter, the haze of the optical reflection film obtained can be reduced and transparency can improve.
- the volume average particle size referred to here is a value obtained by measuring emulsion resin particles with a measuring device using a laser diffraction scattering method or a dynamic light scattering method (for example, MASTERSIZER 2000 manufactured by MALVERN).
- the refractive index of the emulsion resin is not particularly limited, but is preferably 1.3 to 1.7, and more preferably 1.4 to 1.6. If it is the said range, since it becomes close to the refractive index of water-soluble resin, the haze of the optical reflection film obtained can be reduced.
- the above-mentioned emulsion resin preferably has a glass transition temperature (Tg) of 20 ° C. or lower, more preferably ⁇ 30 to 10 ° C., from the viewpoint of enhancing flexibility.
- additives can be used in the high refractive index layer 5H as necessary.
- the content of the additive in the high refractive index layer 5H is preferably 0 to 20% by mass with respect to 100% by mass of the solid content of the high refractive index layer 5H. Examples of such additives are described below.
- the high refractive index layer 5H may contain an amino acid having an isoelectric point of 6.5 or less as an additive. By including an amino acid, the dispersibility of the inorganic oxide particles in the high refractive index layer 5H can be improved.
- an amino acid is a compound having an amino group and a carboxyl group in the same molecule, and may be any type of amino acid such as ⁇ -, ⁇ -, and ⁇ -.
- Some amino acids have optical isomers, but there is no difference in effect due to optical isomers, and any isomer can be used alone or in racemic form.
- preferred amino acids include aspartic acid, glutamic acid, glycine, serine, and the like, with glycine and serine being particularly preferred.
- the isoelectric point of an amino acid refers to this pH value because an amino acid balances the positive and negative charges in the molecule at a specific pH and the overall charge is zero.
- the isoelectric point of each amino acid can be determined by isoelectric focusing at a low ionic strength.
- additives examples include ultraviolet absorbers described in JP-A-57-74193, JP-A-57-87988, and JP-A-62-261476, JP-A-57-74192, and 57- Various interfaces of anti-fading agents, anions, cations or nonions described in JP-A-887989, JP-A-60-72785, JP-A-61-146591, JP-A-1-95091 and JP-A-3-13376 Activators, fluorescent whitening agents described in JP-A-59-42993, JP-A-59-52689, JP-A-62-280069, JP-A-61-228771 and JP-A-4-219266 , Sulfuric acid, phosphoric acid, acetic acid, citric acid, sodium hydroxide, potassium hydroxide, potassium carbonate and other pH adjusters, antifoaming agents, polyethylene Lubricants such as glycols, preservatives, antistatic agents, may contain various known additives such as
- the silicon oxide hydrated oxide and the first water-soluble polymer can be obtained by including the titanium oxide particles coated with the silicon-containing hydrated oxide in the high refractive index layer 5H. And the intermixing of the high refractive index layer 5H and the low refractive index layer 5L is suppressed, and problems such as binder deterioration and choking due to the photocatalytic activity of the titanium oxide particles can be prevented. Therefore, the optical reflective film of the present invention has excellent durability and film flexibility, high visible light transmittance, and excellent near-infrared shielding properties.
- the low refractive index layer 5L includes the second water-soluble polymer and the second inorganic oxide particles as essential components, and if necessary, is selected from the group consisting of a curing agent, a surfactant, an emulsion resin, and a seed additive. It may further contain at least one kind.
- the low refractive index layer 5L may contain an emulsion resin.
- an emulsion resin is preferably contained in the low refractive index layer 5L constituting the uppermost layer A.
- the refractive index of the low refractive index layer 5L as described above is preferably 1.10 to 1.60, more preferably 1.30 to 1.50.
- the thickness per layer of the low refractive index layer 5L is preferably 20 to 800 nm, and more preferably 50 to 350 nm. However, the film thickness of each low refractive index layer 5L is set so that the film thicknesses of the uppermost layer A, the intermediate layer B, and the lowermost layer C satisfy the above-described relationship.
- Silica sicon dioxide
- silica sol is more preferably used, and colloidal silica sol dispersed in an organic solvent is more preferably used.
- hollow fine particles having pores inside the particles can be used as the second inorganic oxide particles, and silica (silicon dioxide) hollow fine particles are particularly preferable.
- well-known inorganic oxide particles other than a silica can also be used.
- the colloidal silica used as the second inorganic oxide particles is obtained by heating and aging a silica sol obtained by metathesis with an acid of sodium silicate or the like and passing through an ion exchange resin layer.
- colloidal silica may be a synthetic product or a commercially available product.
- the surface of the colloidal silica may be cation-modified, or may be treated with Al, Ca, Mg, Ba or the like.
- the hollow fine particles used as the second inorganic oxide particles preferably have an average particle pore size of 3 to 70 nm, more preferably 5 to 50 nm, and further preferably 5 to 45 nm.
- the average particle pore size of the hollow fine particles is an average value of the inner diameters of the hollow fine particles. If the average particle hole diameter of the hollow fine particles is within the above range, the refractive index of the low refractive index layer 5L is sufficiently lowered.
- the average particle diameter is 50 or more at random, which can be observed as an ellipse in a circular, elliptical or substantially circular shape by electron microscope observation, and obtains the pore diameter of each particle. Is obtained.
- the average particle hole diameter said here means the minimum distance among the distance which pinched
- the content of the second inorganic oxide particles in the low refractive index layer 5L is preferably 0.1 to 70% by mass, and preferably 30 to 70% by mass with respect to 100% by mass of the solid content of the low refractive index layer 5L. % Is more preferable, and 45 to 65% by mass is even more preferable.
- the second inorganic oxide particles preferably silicon dioxide
- the second inorganic oxide particles preferably have a primary average particle size of 3 to 100 nm.
- the average particle size of primary particles of silicon dioxide dispersed in the primary particle state is more preferably 3 to 50 nm, and more preferably 3 to 40 nm. More preferably, it is 3 to 20 nm, particularly preferably 4 to 10 nm.
- grains it is preferable from a viewpoint with few hazes and excellent visible light transmittance
- the particle diameter of the second inorganic oxide particles can be determined by the volume average particle diameter in addition to the primary average particle diameter.
- the primary average particle size and volume average particle size of the second inorganic oxide particles are the same as those of the first inorganic oxide particles.
- preferred weight average molecular weights, and the like of the second water-soluble polymer are the same as those described in the column of the first water-soluble polymer, and thus the description thereof is omitted here.
- polyvinyl alcohol is preferably used, and a polyvinyl alcohol of a type different from the polyvinyl alcohol preferably used as the first water-soluble polymer is more preferably used.
- the type of polyvinyl alcohol different from the first water-soluble polymer means that at least one selected from the group consisting of the type of modification, the degree of saponification, the degree of polymerization, and the weight average molecular weight is the first water-soluble polymer. It is different from polyvinyl alcohol used as a conductive polymer.
- the second water-soluble polymer may be used in combination with other water-soluble polymers together with polyvinyl alcohol, and the content of the other polymer used together is 100% by mass of the solid content of the low refractive index layer 5L. On the other hand, it is preferably used at 0.5 to 10% by mass.
- the content of the second water-soluble polymer in the low refractive index layer 5L is preferably 30 to 99.9% by mass, and 35 to 55% by mass with respect to 100% by mass of the solid content of the low refractive index layer 5L. % Is more preferable.
- the curing agent is not particularly limited as long as it is for curing the second water-soluble polymer as a binder and causes a curing reaction with the second water-soluble polymer.
- a curing agent when polyvinyl alcohol is used as the second water-soluble polymer, at least one of boric acid, a salt thereof, and borax is preferable. Besides these, known ones can be used.
- the content of the curing agent in the low refractive index layer 5L is preferably 1 to 10% by mass and more preferably 2 to 6% by mass with respect to 100% by mass of the solid content of the low refractive index layer 5L. .
- the total amount of the curing agent used is preferably 1 mg to 500 mg per 1 g of polyvinyl alcohol, and more preferably 20 mg to 200 mg per 1 g of polyvinyl alcohol.
- the low refractive index layer 5L like the high refractive index layer 5H, preferably contains a surfactant from the viewpoint of coatability, and is the same as the surfactant described as contained in the high refractive index layer 5H. Since a thing can be used, description is abbreviate
- the content of the surfactant in the low refractive index layer 5L is preferably 0.001 to 0.1% by mass, based on 100% by mass of the total coating liquid of the low refractive index layer 5L, and preferably 0.005 to 0%. More preferably, it is 0.05 mass%.
- the emulsion resin contained in the low refractive index layer 5L can be the same as the emulsion resin contained in the high refractive index layer 5H, and the emulsion resin content ratio, average particle size and volume average particle size are also high. Since it is the same as that described in the refractive index layer 5H, the description is omitted here.
- the base material 3 is a support for the optical reflection film 1.
- the thickness of the substrate 3 is preferably 5 to 200 ⁇ m, more preferably 15 to 150 ⁇ m.
- the base material 3 may be a laminate or a laminate of two or more, and in this case, the type may be the same or different.
- the base material 3 applied to the optical reflection film 1 is not particularly limited as long as it is transparent, and various resin films can be used.
- resin film polyolefin films (polyethylene, polypropylene, etc.), polyester films (polyethylene terephthalate, polyethylene naphthalate, etc.), polyvinyl chloride, cellulose acetate, etc. can be used, and polyester films are preferred.
- polyester film but it does not specifically limit as a polyester film (henceforth polyester), It is preferable that it is polyester which has the film formation property which has a dicarboxylic acid component and a diol component as main structural components.
- the main constituent dicarboxylic acid components include terephthalic acid, isophthalic acid, phthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, diphenylsulfone dicarboxylic acid, diphenyl ether dicarboxylic acid, diphenylethanedicarboxylic acid, Examples thereof include cyclohexane dicarboxylic acid, diphenyl dicarboxylic acid, diphenyl thioether dicarboxylic acid, diphenyl ketone dicarboxylic acid, and phenylindane dicarboxylic acid.
- diol component examples include ethylene glycol, propylene glycol, tetramethylene glycol, cyclohexanedimethanol, 2,2-bis (4-hydroxyphenyl) propane, 2,2-bis (4-hydroxyethoxyphenyl) propane, bis ( 4-Hydroxyphenyl) sulfone, bisphenol fluorene hydroxyethyl ether, diethylene glycol, neopentyl glycol, hydroquinone, cyclohexanediol and the like.
- polyesters having these as main components from the viewpoints of transparency, mechanical strength, dimensional stability, etc., dicarboxylic acid components such as terephthalic acid, 2,6-naphthalenedicarboxylic acid, diol components such as ethylene glycol and 1 Polyester having 1,4-cyclohexanedimethanol as the main constituent is preferred.
- polyesters mainly composed of polyethylene terephthalate and polyethylene naphthalate, copolymerized polyesters composed of terephthalic acid, 2,6-naphthalenedicarboxylic acid and ethylene glycol, and mixtures of two or more of these polyesters are mainly used. Polyester as a constituent component is preferable.
- the substrate 3 preferably has a visible light region transmittance of 85% or more shown in JIS R3106-1998, and particularly preferably 90% or more.
- the substrate 3 having the above transmittance or more is advantageous and preferable in that the transmittance in the visible light region shown in JIS R3106-1998 when it is used as an optical reflection film is 50% or more.
- the resin film used as the substrate may be an unstretched film or a stretched film.
- a stretched film is preferable from the viewpoint of strength improvement and thermal expansion suppression.
- the base material 3 can be manufactured by a conventionally known general method.
- an unstretched substrate 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 base material is subjected to a known method such as uniaxial stretching, tenter-type sequential biaxial stretching, tenter-type simultaneous biaxial stretching, tubular-type simultaneous biaxial stretching, or the flow direction of the base material (vertical axis), or A stretched substrate can be produced by stretching in the direction perpendicular to the flow direction of the substrate (horizontal axis).
- the draw ratio in this case can be appropriately selected according to the resin as the raw material of the base material, but is preferably 2 to 10 times in each of the vertical axis direction and the horizontal axis direction.
- the base material 3 may be subjected to a relaxation treatment or an offline heat treatment in terms of dimensional stability.
- the relaxation treatment is performed in a process from the heat setting in the stretching process of the polyester film to the winding in the transversely stretched tenter or after exiting the tenter.
- the relaxation treatment is preferably performed at a treatment temperature of 80 to 200 ° C., more preferably a treatment temperature of 100 to 180 ° C.
- the relaxation rate is preferably in the range of 0.1 to 10% in both the longitudinal direction and the width direction, and more preferably, the relaxation rate is 2 to 6%.
- the relaxed base material is subjected to the following off-line heat treatment to improve heat resistance and to improve dimensional stability.
- the base material 3 is preferably one in which the undercoat layer coating solution is applied inline on one side or both sides in the film forming process, that is, one that has been subjected to inline subbing.
- the resin used for the undercoat layer coating solution is polyester resin, acrylic modified polyester resin, polyurethane resin, acrylic resin, vinyl resin, vinylidene chloride resin, polyethyleneimine vinylidene resin, polyethyleneimine resin, polyvinyl alcohol resin, modified polyvinyl alcohol resin. And gelatin and the like, and any of them can be preferably used.
- a conventionally well-known additive can also be added to the undercoat layer comprised using these resin.
- the undercoat layer coating solution can be applied by a known method such as roll coating, gravure coating, knife coating, dip coating or spray coating.
- the coating amount of the undercoat layer is preferably about 0.01 to 2 g / m 2 (dry state).
- Optical Reflective Film 1 There is no restriction
- the high refractive index layer 5H and the low refractive index layer 5L are simultaneously applied on the main surface of the substrate 3 and dried to form a laminate. It is preferable. More specifically, the high refractive index layer 5H coating liquid and the low refractive index layer 5L coating liquid are simultaneously applied on the substrate 3 and dried, and then the high refractive index layer 5H and the low refractive index layer 5L. A method of forming an optical reflective film containing is preferred.
- a curtain coating method for example, a curtain coating method, a slide bead coating method using a hopper described in U.S. Pat. Nos. 2,761,419 and 2,761,791, an extrusion coating method and the like are preferably used. It is done.
- the solvent for preparing the high refractive index layer 5H coating solution and the low refractive index layer 5L coating solution is not particularly limited, but water, an organic solvent, or a mixed solvent thereof is preferable. In consideration of environmental aspects due to the scattering of the organic solvent, water or a mixed solvent of water and a small amount of an organic solvent is more preferable, and water is particularly preferable.
- organic solvent used here examples include alcohols such as methanol, ethanol, 2-propanol and 1-butanol, esters such as ethyl acetate, butyl acetate, propylene glycol monomethyl ether acetate and propylene glycol monoethyl ether acetate, Examples include ethers such as diethyl ether, propylene glycol monomethyl ether, and ethylene glycol monoethyl ether; amides such as dimethylformamide and N-methylpyrrolidone; and ketones such as acetone, methyl ethyl ketone, acetylacetone, and cyclohexanone. These organic solvents may be used alone or in combination of two or more. From the viewpoint of environment and simplicity of operation, the solvent of the coating solution is particularly preferably water or a mixed solvent of water and methanol, ethanol, 2-propanol, or ethyl acetate, and more preferably water.
- the content of water in the mixed solvent is preferably 80 to 99.9% by mass, based on 100% by mass of the entire mixed solvent, and preferably 90 to 99%. More preferably, it is 5 mass%.
- volume fluctuation due to solvent volatilization can be reduced, handling is improved, and by setting it to 99.9% by mass or less, homogeneity at the time of liquid addition is increased and stable. This is because the obtained liquid properties can be obtained.
- the concentration of the first water-soluble polymer in the high refractive index layer 5H coating solution is preferably 1 to 10% by mass.
- the concentration of the first inorganic oxide particles in the high refractive index layer 5H coating solution is preferably 1 to 50% by mass.
- the concentration of the second water-soluble polymer in the low refractive index layer 5L coating solution is preferably 1 to 10% by mass.
- the concentration of the second inorganic oxide particles in the low refractive index layer 5L coating solution is preferably 1 to 50% by mass.
- the method for preparing the high refractive index layer 5H coating solution and the low refractive index layer 5L coating solution is not particularly limited.
- inorganic oxide particles, a water-soluble polymer, and other additives added as necessary.
- the method of adding and stirring and mixing is mentioned.
- the order of addition of the respective components is not particularly limited, and the respective components may be sequentially added and mixed while stirring, or may be added and mixed at one time while stirring. If necessary, it is further adjusted to an appropriate viscosity using a solvent.
- the high refractive index layer 5H it is preferable to form the high refractive index layer 5H using an aqueous high refractive index layer 5H coating solution prepared by adding and dispersing the first inorganic oxide particles.
- the first inorganic oxide particles are prepared by adding the high refractive index layer 5H coating solution as a sol having a pH of 5.0 or more and 7.5 or less and a negative zeta potential of the particles. It is preferable to do.
- the temperature of the high-refractive index layer 5H coating solution and the low-refractive index layer 5L coating solution at the time of simultaneous multilayer coating is preferably 25 to 60 ° C. and 30 to 45 ° C. when using the slide bead coating method. A temperature range is more preferred. When the curtain coating method is used, a temperature range of 25 to 60 ° C. is preferable, and a temperature range of 30 to 45 ° C. is more preferable.
- the viscosity of the high refractive index layer 5H coating liquid and the low refractive index layer 5L coating liquid when performing simultaneous multilayer coating is not particularly limited.
- the slide bead coating method it is preferably in the range of 5 to 500 mPa ⁇ s, more preferably in the range of 10 to 200 mPa ⁇ s, in the preferable temperature range of the coating solution.
- the curtain coating method it is preferably in the range of 5 to 1200 mPa ⁇ s, more preferably in the range of 25 to 500 mPa ⁇ s, in the preferable temperature range of the coating solution. If it is the range of such a viscosity, simultaneous multilayer coating can be performed efficiently.
- the viscosity of the coating solution at 15 ° C. is preferably 100 mPa ⁇ s or more, more preferably 100 to 30,000 mPa ⁇ s, still more preferably 3,000 to 30,000 mPa ⁇ s, and most preferably 5 , 30,000 to 30,000 mPa ⁇ s.
- the high refractive index layer 5H coating solution and the low refractive index layer 5L coating solution are heated to 30 ° C. or more and applied, and then the temperature of the formed coating film is set to 1 to 15 ° C. It is preferable to cool once and dry at 10 ° C. or higher. More preferably, the drying conditions are a wet bulb temperature of 5 to 50 ° C. and a film surface temperature of 10 to 50 ° C. Moreover, as a cooling method immediately after application
- the optical reflective film 1 has one or more functional layers for the purpose of adding further functions on the surface of the substrate 3 where the optical interference film 5 is not provided or on the uppermost layer A of the optical interference film 5. You may do it.
- Such functional layers include, for example, conductive layers, antistatic layers, gas barrier layers, easy adhesion layers, antifouling layers, deodorant layers, flow drop layers, easy slip layers, hard coat layers, wear resistant layers, reflective layers.
- Prevention layer electromagnetic shielding layer, ultraviolet absorption layer, infrared absorption layer, printing layer, fluorescent light emitting layer, hologram layer, release layer, adhesive layer, adhesive layer, infrared other than the above-described high refractive index layer 5H and low refractive index layer 5L
- Examples thereof include a cut layer (metal layer, liquid crystal layer), a colored layer (visible light absorption layer), and an interlayer film used for laminated glass. The order of stacking these functional layers is not particularly limited.
- the optical reflective film 1 has a specification that can be bonded to the equipment 200 such as a window glass, as shown in the drawing, the optical reflective film 1 is formed on the upper surface of the optical interference film 5 provided on one main surface side of the base material 3.
- a preferred example is a form in which the adhesive layer 7 is laminated and a hard coat layer (not shown here) is coated on the other main surface side of the substrate 3 opposite to the adhesive layer 7.
- the order may be the adhesive layer, the base material 3, the optical interference film 5, and the hard coat layer.
- curable resin used in the hard coat layer examples include a thermosetting resin and an ultraviolet curable resin.
- an ultraviolet curable resin is preferable because it is easy to mold, and among them, those having a pencil hardness of at least 2H. More preferred.
- curable resins can be used singly or in combination of two or more.
- the ultraviolet curable resin examples include (meth) acrylate, urethane acrylate, polyester acrylate, epoxy acrylate, epoxy resin, and oxetane resin, and these can also be used as a solvent-free resin composition.
- the ultraviolet curable resin it is preferable to add a photopolymerization initiator to accelerate curing.
- Photoinitiators include acetophenones, benzophenones, ketals, anthraquinones, thioxanthones, azo compounds, peroxides, 2,3-dialkyldione compounds, disulfide compounds, thiuram compounds, fluoroamine compounds Etc. are used.
- Specific examples of the photopolymerization initiator include 2,2′-diethoxyacetophenone, p-dimethylacetophenone, 1-hydroxycyclohexyl phenyl ketone, 1-hydroxydimethylphenyl ketone, 2-methyl-4′-methylthio-2-mori.
- Acetophenones such as holinopropiophenone and 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone 1, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzyldimethylletal, etc.
- photopolymerization initiators may be used alone, in combination of two or more, or in a eutectic mixture.
- acetophenones are preferably used from the viewpoints of stability of the curable composition and polymerization reactivity.
- a commercial item may be used for such a photoinitiator, for example, Irgacure (trademark) 819, 184, 907, 651 by BASF Japan, etc. are mentioned as a preferable illustration.
- the thickness of the hard coat layer is preferably from 0.1 ⁇ m to 50 ⁇ m, more preferably from 1 to 20 ⁇ m, from the viewpoints of improving the hard coat properties and improving the transparency of the optical reflection film.
- the method for forming the hard coat layer is not particularly limited. For example, after preparing a hard coat layer coating solution containing the above components, the coating solution is applied with a wire bar or the like, and the coating solution is cured with heat and / or UV. And a method of forming a hard coat layer.
- optical reflection film 1 is attached to the inside of the window glass 200 or the outside is attached to the outside.
- the optical reflection film 1 as described above can be applied to a wide range of fields. For example, it is attached to a facility 200 that is exposed to sunlight for a long time, such as an outdoor window of a building or an automobile window, to provide an effect of shielding light in a target wavelength region. Moreover, the optical reflection film 1 is mainly used for the purpose of improving weather resistance as a film for window pasting, a film for agricultural greenhouses, and the like. In particular, the optical reflection film 1 is suitable for a member that is bonded to a substrate such as glass or a glass substitute resin directly or via an adhesive.
- FIG. 2 is a schematic cross-sectional view for explaining the configuration of the optical reflector according to the embodiment.
- the optical reflector 100 according to the embodiment includes the optical reflective film 1, a base 101, and an adhesive layer 103 sandwiched between them.
- the substrate 101 include, for example, glass, polycarbonate resin, polysulfone resin, acrylic resin, polyolefin resin, polyether resin, polyester resin, polyamide resin, polysulfide resin, unsaturated polyester resin, epoxy resin, melamine resin, Examples thereof include phenol resin, diallyl phthalate resin, polyimide resin, urethane resin, polyvinyl acetate resin, polyvinyl alcohol resin, styrene resin, vinyl chloride resin, metal plate, ceramic and the like.
- the type of resin may be any of a thermoplastic resin, a thermosetting resin, and an ionizing radiation curable resin, and two or more of these may be used in combination.
- the substrate 101 used here can be manufactured by a known method such as extrusion molding, calendar molding, injection molding, hollow molding, compression molding or the like.
- the thickness of the substrate is not particularly limited, but is usually 0.1 mm to 5 cm.
- the adhesive layer 103 is for bonding the optical reflective film 1 and the substrate 101 together.
- Such an adhesive layer 103 is disposed between the optical interference film 5 and the substrate 101 in the optical reflection film 1 as shown in the figure, or, contrary to the illustrated example, the substrate 3 and the substrate in the optical reflection film 1. 101.
- an adhesive mainly composed of a photocurable or thermosetting resin can be used as the adhesive layer 103 as described above.
- the adhesive layer 103 preferably has durability against ultraviolet rays, and is preferably an acrylic adhesive or a silicone adhesive. Furthermore, an acrylic adhesive is preferable from the viewpoint of adhesive properties and cost. In particular, a solvent system is preferable in the acrylic pressure-sensitive adhesive because the peel strength can be easily controlled. When a solution polymerization polymer is used as the acrylic solvent-based pressure-sensitive adhesive, known monomers can be used as the monomer.
- the adhesive layer 103 may be made of polyvinyl butyral resin or ethylene-vinyl acetate copolymer resin used as an intermediate layer of laminated glass. Specifically, plastic polyvinyl butyral (manufactured by Sekisui Chemical Co., Ltd., Mitsubishi Monsanto, etc.), ethylene-vinyl acetate copolymer (manufactured by DuPont, Takeda Pharmaceutical Co., Ltd., duramin), modified ethylene-vinyl acetate copolymer (Mersen G, manufactured by Tosoh Corporation). Note that an ultraviolet absorber, an antioxidant, an antistatic agent, a heat stabilizer, a lubricant, a filler, a coloring agent, an adhesion adjusting agent, and the like may be appropriately added to the adhesive layer 103.
- plastic polyvinyl butyral manufactured by Sekisui Chemical Co., Ltd., Mitsubishi Monsanto, etc.
- ethylene-vinyl acetate copolymer
- the optical reflector 100 as described above is preferably installed so that the optical interference film 5 is located on the incident side of the external light with respect to the adhesive layer 103. Further, when the optical reflector 100 is mounted on a window glass or the like, it is preferable to install the optical reflector film 1 so that the optical reflection film 1 is sandwiched between the window glass and the substrate 101. This is preferable because the optical reflective film 1 can be sealed from surrounding gas such as moisture and has excellent durability.
- the optical reflection film 1 having the configuration described above and the optical reflector 100 using the same are the uppermost layer A and the intermediate layer B in the optical interference film 5 in which the high refractive index layers 5H and the low refractive index layers 5L are alternately stacked.
- the elastic modulus and the film thickness ratio are limited.
- Such an optical reflection film 1 and an optical reflector 100 using the optical reflection film 1 are not cracked in the optical interference film 5 without deteriorating the light shielding performance in long-term use, as will be described in the following examples. The occurrence of peeling is prevented, and the weather resistance is improved.
- colloidal silica 10% by mass
- boric acid aqueous solution 385% Parts by weight of polyviny
- a low refractive index layer coating liquid L2 was prepared in the same manner as the preparation of the low refractive index layer coating liquid L1, except that the amount of colloidal silica was changed to 372 parts by mass.
- the coating for the low refractive index layer is the same as the preparation of the coating solution L1 for the low refractive index layer, except that the amount of the colloidal silica is changed to 50 parts by mass and the amount of the surfactant is changed to 9 parts by mass. Liquid L3 was prepared.
- coating liquid H for high refractive index layer for intermediate layer 15.0% by mass of titanium oxide sol (SRD-W, volume average particle size: 5 nm, rutile titanium dioxide particles, manufactured by Sakai Chemical Co., Ltd.) is added to 2 parts by mass of pure water and heated to 90 ° C. did. Subsequently, 0.5 parts by mass of an aqueous silicic acid solution (sodium silicate 4 (manufactured by Nippon Chemical Co., Ltd.) diluted with pure water so that the SiO 2 concentration becomes 0.5% by mass) was gradually added.
- SRD-W volume average particle size: 5 nm, rutile titanium dioxide particles, manufactured by Sakai Chemical Co., Ltd.
- a high refractive index layer coating solution H was prepared.
- the lower layer C is formed using the lower layer low refractive index layer coating liquid L1
- the intermediate layer B is formed using the intermediate layer low refractive index layer coating liquid L2 and the high refractive index layer.
- the uppermost layer A was formed by using the uppermost layer low-refractive index layer coating liquid L3.
- the film thickness [ta] of the uppermost layer A and the film thickness [tc] of the lowermost layer C are 280 nm
- the film thickness of the high refractive index layer 5H as the intermediate layer B is 130 nm
- the intermediate layer B The low refractive index layer 5L was 150 nm in thickness, and the intermediate layer B was coated so that the average thickness [tb] was about 140 nm.
- the optical reflection film 1 of Example 1 produced as described above has a high refractive index layer 5H containing titanium oxide particles as the first inorganic oxide particles on the substrate 3 made of a polyethylene terephthalate film, and a second inorganic film.
- An optical interference film 5 in which low refractive index layers 5L containing silica (silicon dioxide) as oxide particles are alternately laminated is provided.
- the uppermost layer A and the lowermost layer C in the optical interference film 5 are the low refractive index layer 5L.
- the produced optical reflection film 1 of Example 1 has a particle ratio in each layer constituting the optical interference film 5 of 15% by volume in the low refractive index layer 5L of the uppermost layer A, and the lowermost layer.
- the low refractive index layer 5L of C was 52% by volume
- each low refractive index layer 5L constituting the intermediate layer B was 50% by volume
- each high refractive index layer 5H was 45% by volume.
- the particle ratio is the ratio of the first inorganic oxide particles or the second inorganic oxide particles to the total amount of each layer.
- Table 1 below also shows the particle ratios and film thickness ratios of the respective layers in the optical reflective films 1 of Examples 2 to 23 and Comparative Examples 1 to 5 below.
- Table 1 below also shows the elastic modulus measured for each layer in the optical reflective film 1.
- a sample is prepared by coating each layer (high refractive index layer 5H, low refractive index layer 5L) whose elastic modulus is to be measured as a single layer.
- the modulus of elasticity was measured at a maximum load of 50 ⁇ N by a nanoindentation method using a combination of TriboScope made by Hitachi High-Technology Corporation and NanoNaviII made by Hitachi Highte Science Co., Ltd. using a CubeCorner indenter as an indenter.
- the elastic moduli of the high refractive index layer 5H and the low refractive index layer 5L constituting the intermediate layer B were measured, and Table 1 shows the average elastic modulus [Eb].
- Example 2 to Example 5 Among the production procedures of Example 1, the above [3. In Adjustment of Coating Liquid L3 for Low Refractive Index Layer for Uppermost Layer], the particle ratio of the low refractive index layer 5L constituting the uppermost layer A was changed by adjusting the amount of colloidal silica to produce an optical reflective film. Thereby, the particle ratio of the low refractive index layer 5L constituting the uppermost layer A is 26% by volume in Example 2, 30% by volume in Example 3, 35% by volume in Example 4, and 40% by volume in Example 5. It was. In addition, as described below, the elastic modulus of the uppermost layer A in Examples 2 to 5 was adjusted.
- Example 11 to Example 13 Among the production procedures of Example 4, the above [1. In Preparation of Coating Liquid L1 for Lower Refractive Index Layer for Lowermost Layer], by adjusting the amount of colloidal silica, the particle ratio of the low refractive index layer 5L constituting the lowermost layer C was changed to produce an optical reflective film 1 . Thereby, the particle ratio of the low refractive index layer 5L constituting the lowermost layer C was 41 vol% in Example 11, 37 vol% in Example 12, and 35 vol% in Example 13. In addition, as described below, the elastic modulus of the lowermost layer C in Examples 11 to 13 was adjusted.
- Example 14 to Example 16> Among the production procedures of Example 11, the above [5. Optical film]], the film thickness [tc] of the lowermost layer C is changed to the respective values by adjusting the supply flow rate of the slide hopper coating device for the coating liquid L1 for the lower refractive index layer for the lowermost layer. A reflective film 1 was produced.
- [tc / tb] 7.
- Example 17 Among the production procedures of Example 12, the above [5. In the production of the optical reflection film], the film thickness [tc] of the lowermost layer C is changed by adjusting the supply flow rate of the slide hopper coating apparatus for the coating liquid L1 for the lower refractive index layer for the lowermost layer, and the lower layer for the lowermost layer.
- the optical reflection film 1 was produced by changing the film thickness [ta] of the uppermost layer A by adjusting the coating of the refractive index layer coating liquid L3 with the wire bar.
- Example 18 to Example 20> Among the production procedures of Example 17, [3. In the adjustment of the coating liquid L3 for the low refractive index layer for the uppermost layer], the optical reflection film 1 was prepared by adding the emulsion resin to the uppermost layer A by performing the following additional procedure.
- a coating liquid L3 was prepared.
- the ratio of the emulsion resin to the total amount of the binder and the emulsion resin was set to each value.
- the ratio of the emulsion resin to the binder was 7% by mass in Example 18, 15% by mass in Example 19, and 45% by mass in Example 20.
- Example 21 Among the production procedures of Example 19, the above [1. In the preparation of the coating solution L1 for the lower refractive index layer for the lowermost layer], an emulsion resin is added to the lowermost layer C by further adding an anionic emulsion similar to that described in Example 18 to Example 20. An optical reflection film 1 was produced. The ratio of the emulsion resin to the binder was 15% by mass.
- Example 22 to Example 23> Among the production procedures of Example 21, the above [1. 2. Preparation of coating solution L1 for the low refractive index layer for the lowest layer] and [3. The anionic emulsion used in the adjustment of the coating liquid L3 for the low refractive index layer for the uppermost layer] was changed. Thereby, the average particle diameter of emulsion resin was changed and the optical reflection film 1 was produced.
- the average particle size of the emulsion resin was set to 80 nm by using Cybinol EC-657B (manufactured by Seiden Chemical Co., Ltd.) as the anionic emulsion.
- an average particle size of the emulsion resin was set to 100 nm by using Adekabon titer HUX-830 (manufactured by ADEKA Corporation) as an anionic emulsion.
- Example 1 Among the production procedures of Example 1, the above [1. 2. Preparation of coating solution L1 for the low refractive index layer for the lowest layer] and [3. In Adjustment of Coating Liquid L3 for Low Refractive Index Layer for Uppermost Layer], the particle ratio of the low refractive index layer 5L constituting the uppermost layer A and the lowermost layer C was changed by adjusting the amount of colloidal silica. As a result, the particle ratio of the uppermost layer A was 55% by volume, and the particle ratio of the lowermost layer C was 40%.
- the film of the lowermost layer C is adjusted by adjusting the supply flow rate of the slide hopper coating device of the coating liquid L1 for the lower refractive index layer and the coating liquid L3 for the uppermost layer.
- the thickness [tc] and the film thickness [ta] of the uppermost layer A were changed.
- Comparative Example 2 Among the production procedures of Comparative Example 1, the above [1. In the preparation of the coating solution L1 for the lower refractive index layer for the lowermost layer], an additional procedure similar to that described in Example 18 to Example 20 is further performed, so that the emulsion resin is contained in the uppermost layer C and optical. A reflective film was prepared. The ratio of the emulsion resin to the binder was 15% by mass.
- the film of the lowermost layer C is adjusted by adjusting the supply flow rate of the slide hopper coating device of the coating liquid L1 for the lower refractive index layer and the coating liquid L3 for the uppermost layer.
- the thickness [tc] and the film thickness [ta] of the uppermost layer A were changed.
- / Tb] 1.
- a spectrophotometer U-4000 type (manufactured by Hitachi, Ltd.) was used. After roughening the back side of the measurement side of each sample, light absorption treatment is performed with a black spray to prevent reflection of light on the back side, and in the visible light region (400 nm to The refractive index was determined from the measurement result of the reflectance at 700 nm. And the refractive index difference was computed from the obtained refractive index. As a result, the refractive index difference between the high refractive index layer 5H formed in Examples 1 to 23 and Comparative Examples 1 to 5 and the low refractive index layer 5L including the uppermost layer A and the lowermost layer C is 0. 4.
- a xenon lamp light source using an xenon weather meter manufactured by Suga Test Instruments Co., Ltd .; emits light very close to sunlight
- Irradiation 180 W / m 2
- the test was conducted for 450 cycles in total, with 18 minutes under the rain conditions by light irradiation and surface spraying and 22 minutes under the sunny conditions with only light irradiation as one cycle.
- the elastic modulus [Ec] of the lowermost layer C is the elastic modulus of the uppermost layer A.
- the average elastic modulus [Eb] of the intermediate layer B and the elastic modulus [Ec] of the lowermost layer C are (2 ′) [Eb ⁇ Ec] ⁇ 2 Gpa.
- the elastic modulus [Ea] of the uppermost layer A is 8 GPa or more and 15 GPa or less. In such an optical reflection film, it was confirmed that the difference in haze values before and after the weather resistance test was suppressed to 0.9 or less and the weather resistance was improved.
- the rainbow unevenness evaluation results are kept at practical levels A to C, the amount of change (difference) in haze before and after the weather resistance test is suppressed to 1.1 or less, and cracks are evaluated. The result was also confirmed to be a practical level A to D.
- the optical reflective films of Examples 18 to 23 contain an emulsion resin in one or both of the uppermost layer A and the lowermost layer C.
- Such a light-shielding film had a small difference in haze value, and a good tendency was observed for cracks at levels A and B.
- Example 1 to 5 only the particle ratio in the uppermost layer A is changed. In these Examples 1 to 5, as can be seen by comparing the particle ratio of the uppermost layer A and (3) the elastic modulus of the uppermost layer, the particle ratio is within the range of up to 40% by volume. The elastic modulus also increased as the value increased, and it was confirmed that the effect of suppressing the occurrence of rainbow unevenness was high.
- Examples 18 to 20 only the ratio of the emulsion resin to the total amount of the binder and the emulsion resin in the uppermost layer A is changed.
- these embodiments 18 to 20 as can be seen by comparing the ratio of the emulsion resin in the uppermost layer A and (3) the elastic modulus of the uppermost layer, if the ratio is in the range of up to 45%, the ratio is large. It can be seen that the elastic modulus decreases. Thereby, by controlling the ratio of the emulsion resin, it is possible to improve the quality by changing the elastic modulus of each layer constituting the optical reflection film while ensuring the particle ratio for obtaining desired optical characteristics. It was confirmed.
- the average particle size of the emulsion particles (6) and (6 ′) is 60 nm or less, which is outside this range.
- the difference in haze value is small and suppressed to a low value of 0.4 or less, and an improvement in weather resistance was confirmed.
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Abstract
Description
以下、本発明の実施の形態を、図面に基づいて詳細に説明する。図1は、実施形態の光学反射フィルムの構成を説明するための断面模式図である。
光学干渉膜5において、基材3の片面あたりの高屈折率層5Hと低屈折率層5Lとの好ましい積層数の範囲は、生産性の観点から、100層以下9層以上、より好ましくは45層以下15層以上、さらに好ましくは45層以下21層以上である。なお、前記の好ましい高屈折率層5Hおよび低屈折率層5Lの総層数の範囲は、基材3の片面にのみ積層される場合においても適応可能であり、基材3の両面に同時に積層される場合においても適応可能である。基材3の両面に積層される場合において、基材3における一の面と他の面との高屈折率層5Hおよび低屈折率層5Lの総層数は、同じであってもよく、異なっていてもよい。
光学干渉膜5は、最上層A、中間層B、および最下層Cの弾性率が、特定の関係を有している。すなわち、中間層Bの平均弾性率[Eb]は、最上層Aの弾性率[Ea]よりも2GPa以上大きく、[Eb-Ea]≧2GPaである。また、さらに好ましい関係として、中間層Bの平均弾性率[Eb]は、最下層Cの弾性率[Ec]よりも2GPa以上大きく、[Eb-Ec]≧2GPaである。さらに最下層Cの弾性率[Ec]は、最上層Aの弾性率[Ea]よりも大きく、[Ec]>[Ea]であって、[Ec-Ea]>0である。また、最上層Aの弾性率[Ea]は、8GPa以上、15GPa以下であることが好ましい。
光学干渉膜5は、最上層A、中間層B、および最下層Cの膜厚が、特定の関係を有している。すなわち、最上層Aの膜厚[ta]が、中間層Bの平均膜厚[tb]の1.2倍~7倍であり、[ta/tb]=1.2~7である。また好ましくは、最下層Cの膜厚[tc]が、中間層Bの平均膜厚[tb]の1.2倍~7倍であり、[tc/tb]=1.2~7である。
光学干渉膜5を構成する高屈折率層5Hと低屈折率層5Lは、以降に詳細に説明するように、水溶性高分子および無機酸化物粒子を必須成分として含むが、そのうちの最下層Cおよび最上層Aのうちの少なくとも一方が、エマルジョン樹脂を含有することが好ましく、特に、最上層Aに対して、エマルジョン樹脂を含有させることが好ましい。ここで用いられるエマルジョン樹脂は、平均粒径が60nm以下であることが好ましい。エマルジョン樹脂の詳細は、以降に説明する。
光学反射フィルム1においては、高屈折率層5Hと低屈折率層5Lとの屈折率の差を大きく設計することが、少ない層数で近赤外線反射率を高くすることができるという観点から好ましい。このような観点から、光学干渉膜5において隣接する高屈折率層5Hと低屈折率層5Lとの屈折率差は、0.1以上が好ましく、より好ましくは0.25以上であり、さらに好ましくは0.3以上であり、よりさらに好ましくは0.35以上であり、もっとも好ましくは0.4以上である。
高屈折率層5Hは、第1の水溶性高分子および第1の無機酸化物粒子を必須成分として含み、必要により、硬化剤、界面活性剤、エマルジョン樹脂、および各種添加剤からなる群から選択される少なくとも1種をさらに含んでもよい。
次に、高屈折率層5Hを構成する各成分の詳細を説明する。
高屈折率層5Hに含まれる第1の無機酸化物粒子は、屈折率が2.0以上の無機酸化物粒子であることが好ましい。具体的な材質としては、酸化ジルコニウム(ZrO2)、酸化亜鉛(ZnO)、酸化チタン(TiO2)等の金属酸化物が挙げられる。これらのうち、高屈折率層5Hを形成するための塗布液の安定性の観点から、酸化チタン(TiO2)を用いることが好ましい。また、TiO2の中でも、特に屈折率が高く、触媒活性が低いルチル型の酸化チタンを用いることが好ましい。なお、触媒活性が低いと、高屈折率層5Hや隣接する層で生じる副反応(光触媒反応)が抑制されて耐候性が高くなりうる。
高屈折率層5Hにおける第1の無機酸化物粒子の含有量としては、高屈折率層5Hの固形分100質量%に対して、15~95質量%であることが好ましく、20~88質量%であることがより好ましく、30~85質量%であることがさらに好ましい。
第1の無機酸化物粒子の平均粒径(一次平均粒径)は、2~100nmであることが好ましく、3~50nmであることがより好ましく、4~30nmであることがさらに好ましい。当該第1の無機酸化物粒子の平均粒径(一次平均粒径)は、粒子そのもの、または屈折率層の断面や表面に現れた粒子を電子顕微鏡で観察し、1,000個の任意の粒子の粒径を測定し、その単純平均値(個数平均)として求められる。ここで個々の粒子の粒径は、その投影面積に等しい円を仮定したときの直径で表したものである。
第1の無機酸化物粒子の製造方法としては、公知の方法を採用することができ、例えば、以下の(i)~(v)に示す方法を挙げることができる。
(3)上記方法(v)において、使用するオルガノアルコキシシランの添加量を調整することによって、含ケイ素の水和酸化物の被覆量を調整する。
(4)上記方法(ii)において、アルキルシリケートの添加量を調整する。
高屈折率層5Hにおいて、第1の無機酸化物粒子以外に、他の無機酸化物粒子が含まれていてもよい。他の無機酸化物粒子を併用する場合には、第1の無機酸化物粒子と電荷的に凝集しないよう、各種のイオン性分散剤や保護剤を用いることができる。第1の無機酸化物粒子以外に用いることのできる無機酸化物粒子は、例えば、二酸化チタン、酸化ジルコニウム、酸化亜鉛、合成非晶質シリカ、コロイダルシリカ、アルミナ、コロイダルアルミナ、チタン酸鉛、鉛丹、黄鉛、亜鉛黄、酸化クロム、酸化第二鉄、鉄黒、酸化銅、酸化マグネシウム、水酸化マグネシウム、チタン酸ストロンチウム、酸化イットリウム、酸化ニオブ、酸化ユーロピウム、酸化ランタン、ジルコン、酸化スズなどが挙げられる。上記のような第1の無機酸化物粒子以外の他の無機酸化物粒子が、高屈折率層5Hに含有される場合の含有量は、効果を奏することができる範囲であれば特に制限されるものではない。
高屈折率層5Hに含まれる第1の水溶性高分子は、バインダーとして機能するものである。第1の水溶性高分子は、以降に説明する低屈折率層5Lに含まれる第2の水溶性高分子と同じ構成成分であってもよく、異なる構成成分であってもよいが、第1の水溶性高分子と第2の水溶性高分子の構成成分が異なることがより好ましい。
反応性官能基を有するポリマーとしては、例えば、ポリビニルアルコール類、ポリビニルピロリドン類、ポリアクリル酸、アクリル酸-アクリルニトリル共重合体、アクリル酸カリウム-アクリルニトリル共重合体、酢酸ビニル-アクリル酸エステル共重合体、もしくはアクリル酸-アクリル酸エステル共重合体などのアクリル樹脂、スチレン-アクリル酸共重合体、スチレン-メタクリル酸共重合体、スチレン-メタクリル酸-アクリル酸エステル共重合体、スチレン-α-メチルスチレン-アクリル酸共重合体、もしくはスチレン-α-メチルスチレン-アクリル酸-アクリル酸エステル共重合体などのスチレンアクリル酸樹脂、スチレン-スチレンスルホン酸ナトリウム共重合体、スチレン-2-ヒドロキシエチルアクリレート共重合体、スチレン-2-ヒドロキシエチルアクリレート-スチレンスルホン酸カリウム共重合体、スチレン-マレイン酸共重合体、スチレン-無水マレイン酸共重合体、ビニルナフタレン-アクリル酸共重合体、ビニルナフタレン-マレイン酸共重合体、酢酸ビニル-マレイン酸エステル共重合体、酢酸ビニル-クロトン酸共重合体、酢酸ビニル-アクリル酸共重合体などの酢酸ビニル系共重合体及びそれらの塩が挙げられる。これらの中でも、 本発明において、ポリビニルアルコールが特に好ましく用いられる。以下では、ポリビニルアルコールについて説明する。
ゼラチンとしては、従来、ハロゲン化銀写真感光材料分野で広く用いられてきた各種ゼラチンを適用することができ、例えば、酸処理ゼラチン、アルカリ処理ゼラチンの他に、ゼラチンの製造過程で酵素処理をする酵素処理ゼラチンおよびゼラチン誘導体、すなわち分子中に官能基としてのアミノ基、イミノ基、ヒドロキシル基、カルボキシル基を有し、それと反応して得る基を持った試薬で処理し改質したものでもよい。ゼラチンの一般的製造法に関してはよく知られており、例えば、T.H.James:The Theory of Photographic Process 4th. ed. 1977(Macmillan)55項、科学写真便覧(上)72~75項(丸善)、写真工学の基礎-銀塩写真編119~124頁(コロナ社)等の記載を参考にすることができる。また、リサーチ・ディスクロージャー誌第176巻、No.17643(1978年12月)のIX項に記載されているゼラチンを挙げることができる。
セルロース類としては、水溶性のセルロース誘導体が好ましく用いることができ、例えば、カルボキシメチルセルロース(セルロースカルボキシメチルエーテル)、メチルセルロース、ヒドロキシメチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロース等の水溶性セルロース誘導体や、カルボン酸基含有セルロース類であるカルボキシメチルセルロース(セルロースカルボキシメチルエーテル)、カルボキシエチルセルロース等を挙げることができる。その他には、ニトロセルロース、セルロースアセテートプロピオネート、酢酸セルロース、セルロース硫酸エステル等のセルロース誘導体を挙げることができる。
増粘多糖類としては、特に制限はなく、例えば、一般に知られている天然単純多糖類、天然複合多糖類、合成単純多糖類及び合成複合多糖類に挙げることができ、これら多糖類の詳細については、「生化学事典(第2版),東京化学同人出版」、「食品工業」第31巻(1988)21頁等を参照することができる。
硬化剤は、バインダーである第1の水溶性高分子を硬化させるためのものである。第1の水溶性高分子と共に用いることのできる硬化剤としては、当該水溶性高分子と硬化反応を起こすものであれば特に制限はない。例えば、第1の水溶性高分子として、ポリビニルアルコールを用いる場合では、硬化剤として、ホウ酸及びその塩が好ましい。ホウ酸及びその塩以外にも公知のものが使用でき、一般的には、ポリビニルアルコールと反応し得る基を有する化合物あるいはポリビニルアルコールが有する異なる基同士の反応を促進するような化合物であり、適宜選択して用いられる。硬化剤の具体例としては、例えば、エポキシ系硬化剤(ジグリシジルエチルエーテル、エチレングリコールジグリシジルエーテル、1,4-ブタンジオールジグリシジルエーテル、1,6-ジグリシジルシクロヘキサン、N,N-ジグリシジル-4-グリシジルオキシアニリン、ソルビトールポリグリシジルエーテル、グリセロールポリグリシジルエーテル等)、アルデヒド系硬化剤(ホルムアルデヒド、グリオキザール等)、活性ハロゲン系硬化剤(2,4-ジクロロ-4-ヒドロキシ-1,3,5,-s-トリアジン等)、活性ビニル系化合物(1,3,5-トリスアクリロイル-ヘキサヒドロ-s-トリアジン、ビスビニルスルホニルメチルエーテル等)、アルミニウム明礬、ホウ砂等が挙げられる。
界面活性剤は、光学反射フィルムの製造工程において基材上に高屈折率層5Hおよび低屈折率層5Lを塗布する際の塗布性の向上を図るためのものである。
エマルジョン樹脂は、油溶性のモノマーを、分散剤を含む水溶液中でエマルジョン状態に保ち、重合開始剤を用いて乳化重合させた樹脂粒子である。
エマルジョン樹脂の含有比率としては、最下層Cまたは最上層Aを構成する高屈折率層5Hのバインダー樹脂である第1の水溶性子分子に対して、柔軟性、膜強度、赤外反射率などの面から、5質量%~45質量%、好ましくは10質量%~30質量%がよい。
ここで用いられるエマルジョン樹脂の平均粒径は体積平均粒径で、150nm以下が好ましく、特に60nm以下であることが好ましい。エマルジョン樹脂が上記平均粒径を有することにより、得られる光学反射フィルムのヘイズが低減され、透明性が向上しうる。
上述したエマルジョン樹脂は、柔軟性を高める観点から、ガラス転移温度(Tg)が20℃以下であることが好ましく、-30~10℃であることがより好ましい。
高屈折率層5Hには、必要に応じて各種の添加剤を用いることができる。また、高屈折率層5Hにおける添加剤の含有量は、高屈折率層5Hの固形分100質量%に対して、0~20質量%であることが好ましい。当該添加剤の例を以下に記載する。
高屈折率層5Hには、添加材として、等電点が6.5以下のアミノ酸を含有していてもよい。アミノ酸を含むことにより、高屈折率層5H中の無機酸化物粒子の分散性が向上しうる。
低屈折率層5Lは、第2の水溶性高分子および第2の無機酸化物粒子を必須成分として含み、必要により、硬化剤、界面活性剤、エマルジョン樹脂、および種添加剤からなる群から選択される少なくとも1種をさらに含んでもよい。
低屈折率層5Lに含まれる第2の無機酸化物粒子は、シリカ(二酸化ケイ素)を用いることが好ましく、具体的な例として合成非晶質シリカ、コロイダルシリカ等が挙げられる。これらのうち、酸性のコロイダルシリカゾルを用いることがより好ましく、有機溶媒に分散させたコロイダルシリカゾルを用いることがさらに好ましい。また、屈折率をより低減させるためには、第2の無機酸化物粒子として、粒子の内部に空孔を有する中空微粒子を用いることができ、特にシリカ(二酸化ケイ素)の中空微粒子が好ましい。また、シリカ以外の公知の無機酸化物粒子も使用することができる。
低屈折率層5Lにおける第2の無機酸化物粒子の含有量は、低屈折率層5Lの固形分100質量%に対して、0.1~70質量%であることが好ましく、30~70質量%であることがより好ましく、45~65質量%であることがさらに好ましい。
第2の無機酸化物粒子(好ましくは二酸化ケイ素)は、その一次平均粒径が3~100nmであることが好ましい。一次粒子の状態で分散された二酸化ケイ素の一次粒子の平均粒径(塗布前の分散液状態での一次平均粒径)は、3~50nmであるのがより好ましく、3~40nmであるのがさらに好ましく、3~20nmであるのが特に好ましく、4~10nmであるのがもっとも好ましい。また、二次粒子の平均粒径としては、30nm以下であることが、ヘイズが少なく可視光透過性に優れる観点で好ましい。
第2の水溶性高分子の具体例、好ましい重量平均分子量等は、上記の第1の水溶性高分子の欄で説明した内容と同様であるので、ここでは説明を省略する。特に、第2の水溶性高分子としては、ポリビニルアルコールが好ましく用いられ、さらに、第1の水溶性高分子として好ましく用いられるポリビニルアルコールと異なる種類のポリビニルアルコールがより好ましく用いられる。ここで、第1の水溶性高分子とは異なる種類のポリビニルアルコールとは、変性の種類、ケン化度、重合度、および重量平均分子量からなる群より選択される少なくとも1つが、第1の水溶性高分子として用いられるポリビニルアルコールとは異なるものをいう。
硬化剤は、バインダーである第2の水溶性高分子を硬化させるためのものであり、第2の水溶性高分子と硬化反応を起こすものであれば、特に制限されない。特に、第2の水溶性高分子としてポリビニルアルコールを用いた場合の硬化剤としては、ホウ酸およびその塩ならびにホウ砂の少なくとも一方が好ましい。また、これら以外にも公知のものが使用できる。
低屈折率層5Lは、高屈折率層5Hと同様に、塗布性の観点から界面活性剤を含有することが好ましく、上記の高屈折率層5Hが含有するとして説明した界面活性剤と同様のものを使用することができるので、ここでは説明を省略する。
低屈折率層5Lに含有されるエマルジョン樹脂は、高屈折率層5Hに含有されるエマルジョン樹脂と同様ものを用いることができ、またエマルジョン樹脂の含有比率、平均粒径および体積平均粒径も高屈折率層5Hにおいて説明したと同様であるため、ここでは説明を省略する。
低屈折率層5Lには、必要に応じて各種添加剤を用いることができ、当該低屈折率層5Lにおける各種添加物は、上記の高屈折率層5Hに使用した添加物と同一のものを使用することができるので、ここでは説明を省略する。
基材3は、光学反射フィルム1の支持体となるものである。基材3の厚みは、5~200μmであることが好ましく、より好ましくは15~150μmである。また、基材3は、2枚以上を重ねたものあるいは貼りあわせたものであっても良く、この場合、その種類が同じでも異なってもよい。
光学反射フィルム1の製造方法について特に制限はなく、基材3上に、高屈折率層5Hと低屈折率層5Lとから構成されるユニットを少なくとも2つ形成することができるのであれば、いかなる方法でも用いられうる。
光学反射フィルム1は、基材3において光学干渉膜5が設けられていない面上、または光学干渉膜5の最上層Aの上部に、さらなる機能の付加を目的とした機能層を1つ以上有していてもよい。このような機能層は、例えば、導電性層、帯電防止層、ガスバリア層、易接着層、防汚層、消臭層、流滴層、易滑層、ハードコート層、耐摩耗性層、反射防止層、電磁波シールド層、紫外線吸収層、赤外線吸収層、印刷層、蛍光発光層、ホログラム層、剥離層、粘着層、接着層、上述した高屈折率層5Hおよび低屈折率層5L以外の赤外線カット層(金属層、液晶層)、着色層(可視光線吸収層)、合わせガラスに利用される中間膜層などである。これらの機能層の積層順は、特に制限されない。
上記紫外線硬化型樹脂を用いる場合、硬化促進のために、光重合開始剤を添加することが好ましい。
このような光重合開始剤は市販品を用いてもよく、例えば、例えば、BASFジャパン社製のイルガキュア(登録商標)819、184、907、651などが好ましい例示として挙げられる。
図2は、実施形態の光学反射体の構成を説明するための断面模式図である。図2に示すように、実施形態の光学反射体100は、光学反射フィルム1と、基体101と、これらの間に挟持された接着層103とを備えている。
以上説明した構成の光学反射フィルム1およびこれを用いた光学反射体100は、高屈折率層5Hと低屈折率層5Lとを交互に積層した光学干渉膜5において、最上層Aおよび中間層Bの弾性率および膜厚比が限定されたものである。このような光学反射フィルム1およびこれを用いた光学反射体100は、以降の実施例で説明するように、長期間の使用において、光の遮蔽性能を低下させることなく光学干渉膜5のひび割れや剥離の発生を防止され、耐候性の向上が図られたものとなる。
[1.最下層用の低屈折率層用塗布液L1の調製]
320質量部のコロイダルシリカ(10質量%)(スノーテックスOXS、一次粒子の平均粒径=4~6nm;日産化学工業株式会社製)、50質量部のホウ酸水溶液(3質量%)、385質量部のポリビニルアルコール(4質量%)(JP-45;重合度:4500、ケン化度:88mol%;日本酢ビ・ポバール株式会社製)、3質量部の界面活性剤(5質量%)(ソフタゾリンLSB-R;川研ファインケミカル株式会社製)を、37℃でこの順に添加した。そして、純水で1000質量部に仕上げ、低屈折率層用塗布液L1を調製した。
コロイダルシリカの分量を372質量部に変更したこと以外は、低屈折率層用塗布液L1の調製と同様の方法で低屈折率層用塗布液L2を調製した。
コロイダルシリカの分量を50質量部に変更したこと、界面活性剤の分量を9質量部に変更したこと以外は、低屈折率層用塗布液L1の調製と同様の方法で低屈折率層用塗布液L3を調製した。
15.0質量%酸化チタンゾル(SRD-W、体積平均粒径:5nm、ルチル型二酸化チタン粒子、堺化学社製)0.5質量部に純水2質量部を加えた後、90℃に加熱した。次いで、ケイ酸水溶液(ケイ酸ソーダ4号(日本化学社製)をSiO2濃度が0.5質量%となるように純水で希釈したもの)0.5質量部を徐々に添加し、ついでオートクレーブ中、175℃で18時間加熱処理を行い、冷却後、限外濾過膜にて濃縮することにより、固形分濃度が6質量%のSiO2を表面に付着させた二酸化チタンゾル(以下、シリカ付着二酸化チタンゾル)(体積平均粒径:9nm)を得た。
スライドホッパー塗布装置を用い、先に調製した低屈折率層用塗布液L1,L2,L3および高屈折率層用塗布液Hを45℃に保温しながら、樹脂フィルム(厚さ50μmのポリエチレンテレフタレートフィルム;東洋紡株式会社製、コスモシャインA4300)上に、21層同時重層塗布(熱線反射層の全膜厚;1.5μm)を行った。その直後、膜面が15℃以下となる条件で冷風を1分間吹き付けてセットさせた後、80℃の温風を吹き付けて乾燥させた。この際、最下層Cの形成には最下層用の低屈折率層用塗布液L1を用い、中間層Bの形成には中間層用の低屈折率層用塗布液L2と高屈折率層用塗布液Hと交互に用い、最上層Aの形成には最上層用の低屈折率層用塗布液L3を用いた。
実施例1の製造手順のうち、上記[3.最上層用の低屈折率層用塗布液L3の調整]において、コロイダルシリカの分量の調整により、最上層Aを構成する低屈折率層5Lの粒子比率を変更して光学反射フィルムを作製した。これにより、最上層Aを構成する低屈折率層5Lの粒子比率を、実施例2において26体積%、実施例3において30体積%、実施例4において35体積%、実施例5において40体積%とした。またこれにより、以降に説明するように、実施例2~実施例5における最上層Aの弾性率を調整した。
実施例4の製造手順のうち、上記[5.光学反射フィルムの作製]において、最下層用の低屈折率層用塗布液L1のスライドホッパー塗布装置の供給流量調整により、最下層Cの膜厚[tc]を140nmとし、中間層Bの平均膜厚[tb]に対する最下層Cの膜厚[tc]を、[tc/tb]=1に変更して光学反射フィルム1を作製した。
実施例4の製造手順のうち、上記[5.光学反射フィルムの作製]において、最上層用の低屈折率層用塗布液L3のスライドホッパー塗布装置の供給流量調整により、最上層Aの膜厚[ta]をそれぞれの値に変更して光学反射フィルムを作製した。これにより、中間層Bの平均膜厚[tb]に対する最上層Aの膜厚[ta]は、実施例7において[ta/tb]=1.2、実施例8において[ta/tb]=3、実施例9において[ta/tb]=5、実施例10において[ta/tb]=7となった。
実施例4の製造手順のうち、上記[1.最下層用の低屈折率層用塗布液L1の調製]において、コロイダルシリカの分量の調整により、最下層Cを構成する低屈折率層5Lの粒子比率を変更して光学反射フィルム1を作製した。これにより、最下層Cを構成する低屈折率層5Lの粒子比率を、実施例11において41体積%、実施例12において37体積%、実施例13において35体積%とした。またこれにより、以降に説明するように、実施例11~実施例13における最下層Cの弾性率を調整した。
実施例11の製造手順のうち、上記[5.光学反射フィルムの作製]において、最下層用の低屈折率層用塗布液L1のスライドホッパー塗布装置の供給流量の調整により、最下層Cの膜厚[tc]をそれぞれの値に変更して光学反射フィルム1を作製した。これにより、中間層Bの平均膜厚[tb]に対する最下層Cの膜厚[tc]を、実施例14において[tc/tb]=3、実施例15において[tc/tb]=5、実施例16において[tc/tb]=7とした。
実施例12の製造手順のうち、上記[5.光学反射フィルムの作製]において、最下層用の低屈折率層用塗布液L1のスライドホッパー塗布装置の供給流量の調整により最下層Cの膜厚[tc]を変更し、また最上層用の低屈折率層用塗布液L3のワイヤーバー塗布の調整により最上層Aの膜厚[ta]を変更して光学反射フィルム1を作製した。これにより中間層Cの平均膜厚[tb]に対する最上層Aの膜厚[ta」および最下層Cの膜厚[tc]を、[ta/tb]=3、[tc/tb]=4とした。
実施例17の製造手順のうち、上記[3.最上層用の低屈折率層用塗布液L3の調整]において、以下の追加手順を実施したことにより、最上層Aにエマルジョン樹脂を含有させて光学反射フィルム1を作製した。
実施例19の製造手順のうち、上記[1.最下層用の低屈折率層用塗布液L1の調製]において、さらに実施例18~実施例20で説明したと同様のアニオン系エマルジョンを添加することにより、最下層Cにエマルジョン樹脂を含有させて光学反射フィルム1を作製した。バインダーに対するエマルジョン樹脂の比率は、15質量%とした。
実施例21の製造手順のうち、上記[1.最下層用の低屈折率層用塗布液L1の調製]および[3.最上層用の低屈折率層用塗布液L3の調整]において用いたアニオン系エマルジョンを変更した。これにより、エマルジョン樹脂の平均粒径を変更して光学反射フィルム1を作製した。実施例22では、アニオン系エマルジョンとしてサイビノールEC-657B(サイデン化学株式会社製)を用いることで、エマルジョン樹脂の平均粒径を80nmとした。実施例23では、アニオン系エマルジョンとしてアデカボンタイターHUX-830(ADEKA株式会社製)を用いることで、エマルジョン樹脂の平均粒径を100nmとした。
実施例1の製造手順のうち、上記[1.最下層用の低屈折率層用塗布液L1の調製]および[3.最上層用の低屈折率層用塗布液L3の調整]において、コロイダルシリカの分量の調整により最上層Aおよび最下層Cを構成する低屈折率層5Lの粒子比率を変更した。これにより、最上層Aの粒子比率を55体積%、最下層Cの粒子比率を40%とした。
比較例1の製造手順のうち、上記[1.最下層用の低屈折率層用塗布液L1の調製]において、さらに実施例18~実施例20で説明したと同様の追加手順を実施すことにより、最上層Cにエマルジョン樹脂を含有させて光学反射フィルムを作製した。バインダーに対するエマルジョン樹脂の比率は、15質量%とした。
比較例1の製造手順のうち、上記[1.最下層用の低屈折率層用塗布液L1の調製]および[3.最上層用の低屈折率層用塗布液L3の調整]において、コロイダルシリカの分量の調整により最上層Aおよび最下層Cを構成する低屈折率層5Lの粒子比率を変更した。これにより、最上層Aの粒子比率を比較例3,4で42体積%、比較例5で35体積%とした。また、最下層Cの粒子比率を比較例3,4で55体積%、比較例5で35体積%とした
以上のようにして作製した実施例1~実施例23および比較例1~比較例5の各光学反射フィルム1について、下記の性能評価を行った。
基材(PETフィルム)上に、屈折率を測定する対象の層(高屈折率層5H、低屈折率層5L)をそれぞれ単層で塗設したサンプルを作製し、下記の方法に従って屈折率を求めた。
分光光度計(積分球使用、株式会社日立製作所製、U-4000型)を用い、各光学反射フィルムの300nm~2000nmの領域における透過率を測定した。その結果、全ての光学反射フィルムにおいて、550nmにおける可視光透過率は75%以上、1200nmにおける赤外透過率は25%以下であり、ここで作製した光学反射フィルムが、十分な赤外遮蔽性を有することが確認された。
各光学反射フィルムを構成する各層について測定した弾性率から、中間層Bを構成する高屈折率層5Hおよび低屈折率層5Lの弾性率の平均弾性率[Eb]と、最上層Aの弾性率[Ea]との弾性率差[Eb-Ea]、および平均弾性率[Eb]と最下層Cの弾性率[Ec]との弾性率差[Eb-Ec]算出した。これらの結果を下記表2に示す。なお、下記表2には、各光学反射フィルム1の構成のうちの一部を合わせて示した。
作製した光学反射フィルムを210mm×297mmの大きさに裁断した。裁断した光学反射フィルムを目視で観察し、下記の基準に従って、虹ムラの有無を評価した。評価結果を下記表2に示す。なお、A~Cが実用可能なレベルである。
B:わずかにムラが認められる
C:ムラが認められ少量のロスが発生
D:全体にムラが認められ実用不可(NG)
ヘイズメーター(日本電色工業社製、NDH2000)を用いて、ヘイズ値を測定した。測定結果を下記表2に示す。
下記粘着層形成塗布液を中本パックス製セパレータ(NS23MA)のシリコーン離型面に対して、コンマコーターにて乾燥膜厚が10μmになるように塗工し、90℃、1分間乾乾燥して粘着層を形成した。この粘着層に、上記実施例および比較例で製造した光学反射フィルムを貼りあわせ、光学反射フィルム上に粘着層を形成した。
粘着剤であるコーポニールN-6941M(日本合成化学社製)に対して、硬化剤であるコロネートL-55E(日本ポリウレタン工業株式会社製)を3質量%添加し、さらに紫外線吸収剤であるチヌビン477(BASFジャパン株式会社製)を5質量%添加し、溶媒としての酢酸エチルで固形分が10質量%になるように希釈して、粘着層形成塗布液を調製した。
上記耐候性試験後の各光学反射フィルムについて、ヘイズメーター(日本電色工業社製、NDH2000)を用いて、ヘイズ値を測定した。測定結果を下記表2に示す。
作製した光学反射フィルムを目視で観察し、下記の基準に従ってひび割れを評価した。評価結果を下記表2に示す。なお、A~Dが実用可能なレベルである。
B:100cm2あたりに1mm未満のひび割れが5個未満発生
C:100cm2あたりに1mm未満のひび割れが5個~20個以内発生
D:100cm2あたりに1mm以上3mm未満のひび割れが20個以内発生
E:100cm2あたりに3mm以上のひび割れが発生(NG)
3…基材
5…光学干渉膜
5H…高屈折率層
5L…低屈折率層
100…光学反射体
101…基体
A…最上層
B…中間層
C…最下層
Claims (7)
- 基材上に、屈折率差を有する高屈折率層と低屈折率層とを交互に積層して形成された光学干渉膜を備え、
前記光学干渉膜を構成する高屈折率層と低屈折率層のうち、前記基材に対して最も近接して配置された層を最下層とし、前記基材から最も遠く配置された層を最上層とし、前記最下層と前記最上層との間に配置された各層を中間層とした場合、
ナノインデンテーション法によって測定した前記中間層の平均弾性率が、前記最上層の弾性率よりも2GPa以上大きく、
前記最上層の膜厚が、前記中間層の平均膜厚の1.2倍~7倍である
光学反射フィルム。 - ナノインデンテーション法によって測定した前記中間層の平均弾性率が、前記最下層の弾性率よりも2GPa以上大きく、
ナノインデンテーション法によって測定した前記最下層の弾性率が、前記最上層の弾性率よりも大きい
請求項1記載の光学反射フィルム。 - ナノインデンテーション法によって測定した前記最上層の弾性率が、8GPa以上、15GPa以下である
請求項1または2に記載の光学反射フィルム。 - 前記最下層の膜厚が、前記中間層の平均膜厚の1.2倍~7倍であることを特徴とする請求項1~3の何れかに記載の光学反射フィルム。
- 前記高屈折率層および前記低屈折率層は、無機酸化物粒子を含有し、
前記最下層および前記最上層のうちの少なくとも一方にエマルジョン樹脂を含有する
請求項1~4の何れかに記載の光学反射フィルム。 - 前記エマルジョン樹脂の平均粒径が60nm以下である
請求項5に記載の光学反射フィルム。 - 請求項1~6の何れかに記載の光学反射フィルムを、基体の少なくとも一方の面に設けてなる光学反射体。
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