WO2013105374A1 - Filtre passe-bande à région étroite - Google Patents

Filtre passe-bande à région étroite Download PDF

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WO2013105374A1
WO2013105374A1 PCT/JP2012/081829 JP2012081829W WO2013105374A1 WO 2013105374 A1 WO2013105374 A1 WO 2013105374A1 JP 2012081829 W JP2012081829 W JP 2012081829W WO 2013105374 A1 WO2013105374 A1 WO 2013105374A1
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film
refractive index
acid
narrow
band
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PCT/JP2012/081829
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English (en)
Japanese (ja)
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苔口　典之
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コニカミノルタアドバンストレイヤー株式会社
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Publication of WO2013105374A1 publication Critical patent/WO2013105374A1/fr

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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A01G13/02—Protective coverings for plants; Coverings for the ground; Devices for laying-out or removing coverings
    • A01G13/0256—Ground coverings
    • A01G13/0268—Mats or sheets, e.g. nets or fabrics
    • A01G13/0275—Films
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/285—Interference filters comprising deposited thin solid films
    • G02B5/288—Interference filters comprising deposited thin solid films comprising at least one thin film resonant cavity, e.g. in bandpass filters
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/206—Filters comprising particles embedded in a solid matrix

Definitions

  • the present invention relates to a narrow band-pass filter having a dielectric multilayer film containing an organic polymer.
  • plant cultivation has an optimal light source wavelength distribution for promoting growth in plant species and plant growth processes, rather than irradiating plants with white light, It is more advantageous to irradiate a specific color. For example, red light of 640 nm to 690 nm is used to promote photosynthesis, and blue light of 420 nm to 470 nm is used to promote normal formation of leaves. It is considered optimal.
  • LEDs as artificial light sources for plant cultivation.
  • the reason for this is that small size, light weight, low power consumption, low heat radiation, and the advantages of being able to use red LED (660 nm) and blue LED (450 nm), which are currently widely used in industry, are contributing. ing.
  • red LED 660 nm
  • blue LED 450 nm
  • To promote the growth of plants, using different LED light sources is certainly a unique point of view, but it is necessary to attach a large number of LED chips to the board, and a circuit system and power supply system for LED control are required. .
  • there is a limit to the use of the LED and it is difficult to cope with a large-scale planting area or an outdoor greenhouse that does not require an artificial light source.
  • the transmission wavelength range is determined by the LED material, the degree of freedom in which the light source wavelength can be arbitrarily designed in accordance with the plant species is limited.
  • Patent Document 1 discloses a narrow-band optical filter in which an inorganic material of thallium oxide and silica is laminated.
  • the filter disclosed in Patent Document 1 is a filter manufactured using a sputtering apparatus, and it is difficult to increase the area in terms of cost, and is formed of a rigid film of an inorganic material. Durability of the film when bent or at high temperature and high humidity is difficult.
  • an object of the present invention is to obtain an optical film that is low in manufacturing cost, can be increased in area, and has excellent film durability when bent or at high temperature and high humidity.
  • the above object of the present invention is achieved by a narrow band-pass filter characterized by having a dielectric multilayer film containing an organic polymer.
  • FIG. 6 is a diagram showing a spectral transmittance curve of a narrow band-pass filter of Sample 4.
  • FIG. It is a figure which shows the spectral transmittance curve of the narrow-band band pass filter of the sample 5.
  • FIG. It is a figure which shows the spectral transmittance curve of the narrow-band band pass filter of the sample 6.
  • FIG. It is a figure which shows the spectral transmittance curve of the narrow-band band pass filter of the sample 9.
  • FIG. 2 is a diagram showing a spectral transmittance curve of a narrow band-pass filter of a sample 10.
  • FIG. It is a figure which shows the spectral transmittance curve of the narrow-band band pass filter of the sample 15.
  • FIG. 2 is a diagram showing a spectral transmittance curve of a narrow band-pass filter of a sample 10.
  • the present invention is a narrow band-pass filter having a dielectric multilayer film containing an organic polymer. That is, the filter of the present invention is characterized in that a narrow band pass band derived from a dielectric multilayer film containing an organic polymer is formed in a spectral transmittance curve.
  • the effects of the present invention by using a polymer material include the following. (1) Compared with a sputtered laminated film of inorganic material, the physical durability at the time of bending of the film itself and at high temperature and high humidity is greatly improved. (2) A production method suitable for increasing the area such as melt stretching or multilayer coating is possible. For this reason, the manufacturing cost is low and the cost can be significantly reduced. (3) Since the dielectric films containing the polymer material are laminated in multiple layers, the fluctuation of the film thickness which occurs about several percent with a relative standard deviation acts on the contrary as error diffusion, and a narrow band pass band with high robustness can be formed.
  • a dielectric multilayer film it is possible to design a sharp transmission wavelength region window having a band edge that cannot be realized by a general light adjustment material such as a coloring dye or a pigment. That is, the degree of freedom in designing the transmission wavelength is high.
  • the narrowband passband is defined as follows.
  • ⁇ 0 is an average wavelength of the wavelengths with a transmittance of 80% (that is, a transmittance of 80%).
  • a band satisfying ⁇ / ⁇ 0 ⁇ 100 ⁇ 15% is defined as a narrowband passband.
  • the value of ⁇ / ⁇ 0 ⁇ 100 is preferably as small as possible, preferably 10% or less, and more preferably 6% or less.
  • the value of ⁇ / ⁇ 0 ⁇ 100 is preferably as small as possible, but is usually 0.5% or more.
  • the number of narrowband passbands can be set according to the purpose, and the number of narrowband passbands is not limited to one, and there may be two or more.
  • the dielectric type narrow band pass band filter of the present invention belongs to the above (3), and unlike (1) and (2), a metal film having poor durability is not used in a constituent layer contributing to band formation. It is a feature.
  • the dielectric type narrow-band bandpass filter has at least one structure in which a high refractive index film and a low refractive index film are adjacent to each other.
  • the terms “high refractive index film” and “low refractive index film” mean that the refractive index film having the higher refractive index is the high refractive index film when the difference in refractive index between two adjacent layers is compared, and the low refractive index film is low. This means that the other refractive index film is a low refractive index film. Therefore, the terms “high refractive index film” and “low refractive index film” are the same when the refractive index films constituting the optical reflection film are focused on two adjacent refractive index films. All forms other than those having a refractive index are included.
  • Examples of suitable configurations included in the dielectric multilayer film of the dielectric type narrow band band-pass filter include the following.
  • (H 1 L 1 ) m means that the layer structure of H 1 L 1 is laminated m times and sH 2 means that H 2 is laminated s times.
  • H 1 , H 2 , H 3 and H 4 each represent a high refractive index film
  • L 1 , L 2 , L 3 and L 4 represent low refractive index films.
  • H 1 , H 2 , H 3 and H 4 may be the same or different in film thickness and film configuration.
  • L 1 , L 2 , L 3 and L 4 may be the same or different in film thickness and film configuration.
  • the optical film thickness of the high refractive index film and the low refractive index film is ⁇ / 4 ⁇ 50% with respect to the maximum transmittance wavelength ⁇ [nm] in the narrow band pass band of the spectral transmittance curve of the filter.
  • ⁇ / 4 ⁇ 50% means “( ⁇ / 4 ⁇ / 4 ⁇ 0.5) or more ( ⁇ / 4 + ⁇ / 4 ⁇ 0.5) or less”).
  • optical film thickness [nm] refractive index ⁇ physical film thickness [nm].
  • each refractive index film is ⁇ / 4 ⁇ 50% (( ⁇ / 4 ⁇ / 4 ⁇ 0.5) or more ( ⁇ / 4 + ⁇ / 4 ⁇ 0.5) or less).
  • m and n are integers of 1 or more. Further, s is an integer of 2 or more, but s is generally 2. In order to adjust the width of the passband, the number of m and n may be adjusted. The smaller the m and n are, the wider the passband is.
  • the upper limits of m and n are not particularly limited, but are usually 100 or less. The upper limit of s is not particularly limited, but is usually 10 or less.
  • any one of the above film configurations may be provided in accordance with a set wavelength to form a laminated structure of a plurality of cavities.
  • the film configuration of the laminated structure corresponding to each pass band may be the same or different.
  • the (HL) may be laminated while shifting the optical film thickness by 3 to 30% instead of repeating the same optical film thickness.
  • These multilayer structures can be designed by using optical simulation (FTG Software Associates Film DESIGN Version 2.23.3700). When only one type of ⁇ / 4 is used, the width of the stop band is about 30 to 100 nm, so it should be somewhat wide.
  • the dielectric multilayer film has the following formula (1):
  • H 1 , H 2 , and H 3 are dielectric multilayer films having optical film thicknesses of ( ⁇ / 4 ⁇ / 4 ⁇ 0.5) or more and ( ⁇ / 4 + ⁇ / 4 ⁇ 0.5) or less.
  • ⁇ represents the maximum transmittance wavelength in the narrowband passband of the spectral transmittance curve of the filter.
  • m and n are integers of 1 or more, s is an integer of 2 or more, (H 1 L 1 ) m and (L 2 H 3 ) n are (H 1 L 1 ) m times, and This means that (L 2 H 3 ) is repeated n times, and sH 2 is a cavity layer.
  • the specific range and preferred range of m, n, and s are as described above. With such a configuration, durability at the time of bending and high temperature and high humidity is improved. This is thought to be due to a decrease in water and oxygen permeability due to the material type and path length of the coating film and an improvement in stress relaxation due to the mixing of materials having different elasticity and ductility.
  • the pass portion is wide to some extent.
  • sH rather than sL
  • the end of the constituent layer is another organic film.
  • the film for example, a film support.
  • it is more advantageous to contact the high refractive index film than to contact the low refractive index film from the viewpoint of reducing the number of required layers.
  • the layer constituting the outermost surface of the filter is preferably H from the viewpoint of permeability, and more preferably rH (r is an integer of 2 or more).
  • the upper limit of the total number of high refractive index films and low refractive index films is preferably 200 layers or less. More preferably, it is 100 layers or less, More preferably, it is 40 layers or less.
  • the preferable refractive index range of the high refractive index film is 1.70 to 2.50, more preferably 1.8 to 2.1, and still more preferably 1.90 to 2.1.
  • the preferred refractive index range of the low refractive index film is 1.10 to 1.60, more preferably 1.30 to 1.55, and still more preferably 1.3 to 1.45.
  • a preferable refractive index difference between the high refractive index film and the low refractive index film is 0.1 or more, and more preferably 0.3 to 0.7.
  • the refractive index difference is obtained by calculating the refractive indexes of the high refractive index film and the low refractive index film according to the following method, and the difference between the two is defined as the refractive index difference.
  • Each refractive index film is produced as a single film (using a base material if necessary), and after cutting this sample into 10 cm ⁇ 10 cm, the refractive index is determined according to the following method.
  • a U-4000 type manufactured by Hitachi, Ltd.
  • the surface opposite to the measurement surface (back surface) of each sample is roughened, and then light absorption is performed with a black spray. Then, the reflection of light on the back surface is prevented, and the average value is obtained by measuring 25 points of reflectance in the visible light region (400 nm to 700 nm) under the condition of regular reflection at 5 degrees, and the average refractive index is determined from the measurement result.
  • the average value is obtained by measuring 25 points of reflectance in the visible light region (400 nm to 700 nm) under the condition of regular reflection at 5 degrees, and the average refractive index is determined from the measurement result.
  • a light shielding means In the narrow band-pass filter of the present invention, a light shielding means can be further used. By combining further light shielding means, light outside the target wavelength range can be effectively shielded, and the target wavelength range can be effectively transmitted.
  • the light shielding means is preferably a means for shielding light in a wavelength region other than the wavelength region in which the narrow band pass band is formed, and is particularly limited as long as it is such a light shielding means. is not. Alternatively, the total light amount can be adjusted by the light shielding means.
  • the light shielding means is a visible light shielding layer.
  • the light shielding means may be achieved by a dielectric multilayer film that forms a narrow band pass band in the spectral transmittance curve, or other than the dielectric multilayer film that forms a narrow band pass band, a light shielding layer (a narrow band pass band is formed).
  • a dielectric multilayer film other than the dielectric multilayer film to be formed may be provided separately.
  • a dielectric multilayer film other than the dielectric multilayer film forming a narrow band pass band (hereinafter, also simply referred to as “other dielectric multilayer film”) can be used.
  • another dielectric multilayer film a laminated structure in which a high refractive index film and a low refractive index film are repeated at the same optical film thickness, or a high refractive index film and a low refractive index film while shifting the optical film thickness by 5%, for example, A stacked structure in which layers are repeatedly stacked can be used in combination.
  • Such a dielectric multilayer film is preferable from the viewpoint of productivity because the same material as that of the dielectric multilayer film forming the narrow band pass band can be used.
  • a layer containing a light absorbing / reflecting material can be provided as a means other than using a dielectric multilayer film.
  • a light absorbing or reflecting material may be supported in the binder.
  • Preferable binders include polyvinyl butyral resins, ethylene-vinyl acetate copolymer resins, and polyvinyl alcohol resins.
  • plastic polyvinyl butyral manufactured by Sekisui Chemical Co., Ltd., Mitsubishi Monsanto, etc.
  • ethylene-vinyl acetate copolymer manufactured by Takeda Pharmaceutical Co., Ltd., duramin
  • modified ethylene-vinyl acetate copolymer manufactured by Tosoh Corporation.
  • tin oxide, indium oxide, zinc oxide, cadmium oxide, antimony-doped tin oxide (ATO), fluorine-doped tin oxide (FTO), tin-doped indium oxide (ITO), and aluminum-doped zinc oxide (AZO) can be preferably used, and ATO and ITO are particularly preferable.
  • the content of the light absorbing / reflecting material is preferably 1 to 60% with respect to the total mass of the layer.
  • the volume ratio of the light absorbing / reflecting material and the binder is preferably 1: 0.5 to 5.
  • 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 layer containing the light absorption / reflection material.
  • the thickness of the layer containing the light absorbing / reflecting material is preferably 0.1 to 50 ⁇ m, and more preferably 1 to 20 ⁇ m.
  • the dielectric narrow band-pass filter of the present invention includes a dielectric multilayer film containing an organic polymer.
  • the organic polymer contained in the dielectric multilayer film is not particularly limited, and is not particularly limited as long as the polymer can form the dielectric multilayer film.
  • organic polymers described in JP-T-2002-509279 can be used as the organic polymer.
  • specific examples include polyethylene naphthalate (PEN) and its isomers (eg, 2,6-, 1,4-, 1,5-, 2,7- and 2,3-PEN), polyalkylene terephthalates (eg, , Polyethylene terephthalate, polybutylene terephthalate, and poly-1,4-cyclohexanedimethylene terephthalate), polyimide (eg, polyacrylimide), polyetherimide, atactic polystyrene, polycarbonate, polyalkyl methacrylate (eg, polyisobutyl methacrylate, Polypropyl methacrylate, polyethyl methacrylate, and polymethyl methacrylate), polyalkyl acrylates (eg, polybutyl acrylate, and polymethyl acrylate), cellulose derivatives (eg, , Ethylcellulose, acetylcellulose, cellulose prop
  • Copolymers such as copolymers of PEN [e.g. (a) terephthalic acid or ester thereof, (b) isophthalic acid or ester thereof, (c) phthalic acid or ester thereof, (d) alkane glycol, (e) cycloalkane glycol ( (E.g., cyclohexanedimethanoldiol), (f) alkanedicarboxylic acid, and / or (g) cycloalkanedicarboxylic acid (e.g., cyclohexanedicarboxylic acid) and 2,6-, 1,4-, 1,5-, 2, 7- and / or copolymers with 2,3-naphthalenedicarboxylic acid or esters thereof], copolymers of polyalkylene terephthalates [eg (a) naphthalenedicarboxylic acid or esters thereof, (b) isophthalic acid or esters thereof, ( c) phthalic acid or The ester
  • a dielectric multilayer film can be formed by subjecting the polymer to melt extrusion and stretching.
  • a preferred combination of polymers forming the high refractive index film and the low refractive index film includes PEN / PMMA, PEN / polyvinylidene fluoride, and PEN / PET.
  • polyester A a polyester (hereinafter referred to as polyester A) and a polyester (hereinafter referred to as polyester B) containing residues derived from at least three diols of ethylene glycol, spiroglycol and butylene glycol, Can be used.
  • Polyester A is not particularly limited as long as it has a structure obtained by polycondensation of a dicarboxylic acid component and a diol component.
  • Polyester A may be a copolymer.
  • the copolyester has a structure obtained by polycondensation using at least three or more dicarboxylic acid components and diol components.
  • dicarboxylic acid component examples include terephthalic acid, isophthalic acid, phthalic acid, 1,4-naphthalenedicarboxylic acid, 1,5-naphthalenedicarboxylic acid, 2,6-naphthalenedicarboxylic acid, 4,4′-diphenyldicarboxylic acid, Examples thereof include 4′-diphenylsulfone dicarboxylic acid, adipic acid, sebacic acid, dimer acid, cyclohexanedicarboxylic acid and ester-forming derivatives thereof.
  • glycol component examples include ethylene glycol, 1,2-propanediol, 1,3-butanediol, 1,4-butanediol, 1,5-pentadiol, diethylene glycol, polyalkylene glycol, 2,2-bis (4 ′ - ⁇ -hydroxyethoxyphenyl) propane, isosorbate, 1,4-cyclohexanedimethanol, spiroglycol, and ester-forming derivatives thereof.
  • Polyester A is preferably polyethylene terephthalate or polyethylene naphthalate.
  • the polyester B includes residues derived from at least three kinds of diols, ethylene glycol, spiroglycol and butylene glycol. Typical examples include copolymerized polyesters having a structure obtained by copolymerization using ethylene glycol, spiroglycol and butylene glycol, and polyesters having a structure obtained by polymerization using these three diols. There is polyester obtained by blending. This configuration is preferable because it is easy to form and difficult to delaminate. Moreover, it is preferable that the polyester B is a polyester containing residues derived from at least two dicarboxylic acids of terephthalic acid / cyclohexanedicarboxylic acid.
  • Such polyesters include copolyesters copolymerized with terephthalic acid / cyclohexanedicarboxylic acid, or those obtained by blending polyesters containing terephthalic acid residues and polyesters containing cyclohexanedicarboxylic acid residues.
  • the polyester containing the cyclohexanedicarboxylic acid residue has a large difference between the in-plane average refractive index of the A layer and the in-plane average refractive index of the B layer, and a high reflectance is obtained.
  • the glass transition temperature difference with polyethylene terephthalate or polyethylene naphthalate is small, it is difficult to be overstretched at the time of molding, and it is preferable that delamination is difficult.
  • a water-soluble polymer as the polymer.
  • the water-soluble polymer is preferable because it does not use an organic solvent, has a low environmental load, and has high flexibility, so that the durability of the film during bending is improved.
  • water-soluble polymer examples include polyvinyl alcohols, polyvinyl pyrrolidones, polyacrylic acid, acrylic acid-acrylonitrile copolymer, potassium acrylate-acrylonitrile copolymer, vinyl acetate-acrylic ester copolymer, Or 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- ⁇ -methylstyrene -Styrene acrylic resin such as acrylic acid copolymer or styrene- ⁇ -methylstyrene-acrylic acid-acrylic acid ester copolymer, styrene-sodium styrenesulfonate copolymer, styrene-2-hydroxyethyl acrylate copolymer Co
  • particularly preferred examples include polyvinyl alcohol, polyvinylpyrrolidones and copolymers containing them, gelatin, thickening polysaccharides (particularly celluloses) from the viewpoint of handling during production and film flexibility. Is mentioned. These water-soluble polymers may be used alone or in combination of two or more.
  • Preferred polyvinyl alcohol includes modified polyvinyl alcohol in addition to ordinary polyvinyl alcohol obtained by hydrolyzing polyvinyl acetate.
  • modified polyvinyl alcohol include cation-modified polyvinyl alcohol, anion-modified polyvinyl alcohol, nonion-modified polyvinyl alcohol, and vinyl alcohol polymers.
  • 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 mol%, particularly preferably 80 to 99.5 mol%.
  • Examples of the cation-modified polyvinyl alcohol have primary to tertiary amino groups and quaternary ammonium groups in the main chain or side chain of the polyvinyl alcohol as described in JP-A-61-10383.
  • Polyvinyl alcohol which 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.
  • Anion-modified polyvinyl alcohol is, for example, polyvinyl alcohol having an anionic group as described in JP-A-1-206088, as described in 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 modified polyvinyl alcohol having a water-soluble group as described in JP-A-7-285265.
  • Nonionic modified polyvinyl alcohols include, for example, polyvinyl alcohol derivatives obtained by adding a polyalkylene oxide group to a part of vinyl alcohol as described in JP-A-7-9758, and described in JP-A-8-25795.
  • the vinyl alcohol polymer include Exeval (trade name: manufactured by Kuraray Co., Ltd.) and Nichigo G polymer (trade name: manufactured by Nippon Synthetic Chemical Industry Co., Ltd.).
  • Polyvinyl alcohol can be used in combination of two or more, such as the degree of polymerization and the type of modification.
  • gelatin in addition to lime-processed gelatin, acid-processed gelatin may be used, and gelatin hydrolyzate and gelatin enzyme-decomposed product can also be used.
  • thickening polysaccharides examples include natural simple polysaccharides, natural complex polysaccharides, synthetic simple polysaccharides and synthetic complex polysaccharides that are generally known. Reference can be made to the encyclopedia (2nd edition), Tokyo Kagaku Doujin Publishing, “Food Industry”, Vol. 31 (1988), p. 21.
  • the thickening polysaccharide as used herein is a polymer of saccharides and has many hydrogen bonding groups in the molecule. Due to the difference in hydrogen bonding strength between molecules depending on the temperature, the viscosity at low temperature and the viscosity at high temperature are It is a polysaccharide with a large viscosity difference, and when metal oxide fine particles are added, the viscosity rises due to hydrogen bonding with the metal oxide fine particles at low temperatures.
  • thickening polysaccharide examples include ⁇ 1-4 glucan (eg, carboxymethylcellulose, carboxyethylcellulose, etc.), galactan (eg, agarose, agaropectin, etc.), galactomannoglycan (eg, locust bean gum, guaran, etc.), xylo Glucan (eg, tamarind gum, etc.), glucomannoglycan (eg, salmon mannan, wood-derived glucomannan, xanthan gum, etc.), galactoglucomannoglycan (eg, softwood-derived glycan), arabinogalactoglycan (eg, soybean) Glycans derived from microorganisms, glycans derived from microorganisms, etc.), glucoraminoglycans (eg, gellan gum, etc.), glycosaminoglycans (eg, hyaluronic acid, keratan sul
  • the structural unit does not have a carboxylic acid group or a sulfonic acid group.
  • polysaccharides include, for example, 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 only. It is preferable that it is a polysaccharide.
  • tamarind seed gum known as xyloglucan whose main chain is glucose and side chain is xylose
  • guar gum known as galactomannan whose main chain is mannose and side chain is galactose
  • locust bean gum Tara gum or arabinogalactan whose main chain is galactose and whose side chain is arabinose
  • xyloglucan whose main chain is glucose and side chain is xylose
  • galactomannan whose main chain is mannose and side chain is galactose
  • locust bean gum Tara gum or arabinogalactan whose main chain is galactose and whose side chain is arabinose
  • Two or more thickening polysaccharides may be used in combination.
  • the weight average molecular weight of the water-soluble polymer is preferably 1,000 or more and 200,000 or less. Furthermore, 3,000 or more and 40,000 or less are more preferable. In this specification, the value measured on the following measurement conditions using gel permeation chromatography (GPC) is employ
  • a curing agent may be used to cure the water-soluble polymer as a binder.
  • the curing agent is not particularly limited as long as it causes a curing reaction with the water-soluble polymer, but boric acid and its salt are preferable when the water-soluble polymer is polyvinyl alcohol.
  • the curing agent other known ones can be used.
  • the curing agent is a compound having a group capable of reacting with a water-soluble polymer or a compound that promotes the reaction between different groups of the water-soluble polymer. Depending on the type of water-soluble polymer, it is appropriately selected and used.
  • 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-tris-acryloyl-hexahydro-s-triazine, bisvinylsulfonylmethyl ether, etc.), aluminum alum and the like.
  • epoxy curing agents diglycidyl ethyl
  • water-soluble polymer is gelatin
  • organic hardeners such as vinylsulfone compounds, urea-formalin condensates, melanin-formalin condensates, epoxy compounds, aziridine compounds, active olefins, isocyanate compounds, etc.
  • Inorganic polyvalent metal salts such as chromium, aluminum and zirconium.
  • the content of the organic polymer is preferably 10% by mass or more, and preferably 25% by mass or more with respect to the total mass of the refractive index film (the upper limit is 100% by mass).
  • the dielectric multilayer film forming the narrow band pass band preferably further contains metal oxide particles.
  • metal oxide particles By containing metal oxide particles, the refractive index difference between the refractive index films can be increased, the number of stacked layers can be reduced, and a thin film can be obtained. In addition, there is an advantage that stress relaxation works and film physical properties (flexibility at the time of bending and high temperature and high humidity) are improved.
  • the metal oxide particles may be contained in any of the films constituting the dielectric multilayer film, but a preferable form is that at least the high refractive index film contains metal oxide particles, and a more preferable form is a high refractive index. Both the film and the low refractive index film have a form containing metal oxide particles.
  • metal oxide particles examples include titanium dioxide, zirconium oxide, zinc oxide, silicon dioxide (synthetic amorphous silica, colloidal silica), alumina, colloidal alumina, lead titanate, red lead, yellow lead, zinc yellow, oxidation
  • metal oxide particles include chromium, ferric oxide, iron black, copper oxide, magnesium oxide, magnesium hydroxide, strontium titanate, yttrium oxide, niobium oxide, europium oxide, lanthanum oxide, zircon, and tin oxide.
  • the metal oxide particles have an average particle size of 100 nm or less, preferably 4 to 50 nm, more preferably 4 to 30 nm.
  • the average particle size of the metal oxide particles is determined by observing the particles themselves or the particles appearing on the cross section or surface of the layer with an electron microscope and measuring the particle size of 1,000 arbitrary particles. Average).
  • the particle diameter of each particle is represented by a diameter assuming a circle equal to the projected area.
  • the content of metal oxide particles in each refractive index film is preferably 20 to 90% by mass, and more preferably 40 to 75% by mass with respect to the total mass of the refractive index film.
  • metal oxide particles it is preferable to use solid fine particles selected from titanium dioxide, silicon dioxide, and alumina.
  • silicon dioxide silicon dioxide
  • acidic colloidal silica sol acidic colloidal silica sol
  • silicon dioxide As silicon dioxide (silica) that can be used in the present invention, silica synthesized by an ordinary wet method, colloidal silica, silica synthesized by a gas phase method, or the like is preferably used, but is particularly preferably used in the present invention.
  • the fine particle silica colloidal silica or fine particle silica synthesized by a vapor phase method is preferable.
  • the metal oxide particles are preferably in a state where the fine particle dispersion before mixing with the cationic polymer is dispersed to the primary particles.
  • the average particle size (particle size in the dispersion state before coating) of the metal oxide fine particles dispersed in the primary particle state is 100 nm or less. More preferably, it is 4 to 50 nm, and most preferably 4 to 20 nm.
  • Aerosil manufactured by Nippon Aerosil Co., Ltd. is commercially available as the silica synthesized by the vapor phase method in which the average particle diameter of primary particles is 4 to 20 nm.
  • the vapor phase fine particle silica can be dispersed to primary particles relatively easily by being sucked and dispersed in water, for example, by a jet stream inductor mixer manufactured by Mitamura Riken Kogyo Co., Ltd.
  • the colloidal silica preferably used in the present invention 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.
  • Commercially available products include the Snowtex series (Snowtex 20, Snowtex 30, Snowtex 40, Snowtex O, Snowtex OS, Snowtex OXS, Snowtex XS, Snowtex sold by Nissan Chemical Industries, Ltd. O-40, Snowtex C, Snowtex N, Snowtex S, Snowtex 20L, Snowtex OL).
  • the preferred average particle size (number average; diameter) of colloidal silica is usually 5 to 100 nm, but an average particle size of 7 to 30 nm is particularly preferable.
  • Silica and colloidal silica synthesized by a vapor phase method may be those whose surfaces are cation-modified, or those treated with Al, Ca, Mg, Ba, or the like.
  • TiO 2 , ZnO, and ZrO 2 are preferable, and TiO 2 is used from the viewpoint of the stability of the metal oxide particle-containing composition described later for forming the high refractive index film. Is more preferable, and titanium dioxide sol is more preferable.
  • TiO 2 rutile type is more preferable than anatase type because it has low catalytic activity, and thus the weather resistance of the high refractive index film and the adjacent layer is high, and the refractive index is high.
  • the first step in the production method of rutile type fine particle titanium dioxide includes at least one basic compound selected from the group consisting of an alkali metal hydroxide and an alkaline earth metal hydroxide. It is the process (process 1) processed by this.
  • Titanium dioxide hydrate can be obtained by hydrolysis of water-soluble titanium compounds such as titanium sulfate and titanium chloride.
  • the method of hydrolysis is not particularly limited, and a known method can be applied. Especially, it is preferable that it was obtained by thermal hydrolysis of titanium sulfate.
  • the step (1) can be performed, for example, by adding the basic compound to an aqueous suspension of the titanium dioxide hydrate and treating (reacting) it under a predetermined temperature condition for a predetermined time. it can.
  • the method for preparing the titanium dioxide hydrate as an aqueous suspension is not particularly limited, and can be performed by adding the titanium dioxide hydrate to water and stirring.
  • the concentration of the suspension is not particularly limited.
  • the concentration of TiO 2 is 30 to 150 g / L in the suspension. By setting it within the above range, the reaction (treatment) can proceed efficiently.
  • the at least one basic compound selected from the group consisting of alkali metal hydroxides and alkaline earth metal hydroxides used in the step (1) is not particularly limited. Examples include potassium, magnesium hydroxide, calcium hydroxide, and the like.
  • the amount of the basic compound added in the step (1) is preferably 30 to 300 g / L in terms of the basic compound concentration in the reaction (treatment) suspension.
  • the above step (1) is preferably performed at a reaction (treatment) temperature of 60 to 120 ° C.
  • the reaction (treatment) time varies depending on the reaction (treatment) temperature, but is preferably 2 to 10 hours.
  • the reaction (treatment) is preferably performed by adding an aqueous solution of sodium hydroxide, potassium hydroxide, magnesium hydroxide, or calcium hydroxide to a suspension of titanium dioxide hydrate. After the reaction (treatment), the reaction (treatment) mixture is cooled, neutralized with an inorganic acid such as hydrochloric acid as necessary, and then filtered and washed with water to obtain fine particle titanium dioxide hydrate.
  • the compound obtained in step (1) may be treated with a carboxylic acid group-containing compound and an inorganic acid.
  • the method of treating the compound obtained in the above step (1) with an inorganic acid in the production of rutile type fine particle titanium dioxide is a known method, but in addition to the inorganic acid, a carboxylic acid group-containing compound is used. Can be adjusted.
  • the carboxylic acid group-containing compound is an organic compound having a —COOH group.
  • the carboxylic acid group-containing compound is preferably a polycarboxylic acid having 2 or more, more preferably 2 or more and 4 or less carboxylic acid groups. Since the polycarboxylic acid has a coordination ability to a metal atom, it is presumed that agglomeration between fine particles can be suppressed by coordination, whereby rutile type fine particle titanium dioxide can be suitably obtained.
  • the carboxylic acid group-containing compound is not particularly limited, and examples thereof include dicarboxylic acids such as succinic acid, malonic acid, succinic acid, glutaric acid, adipic acid, propylmalonic acid, and maleic acid; hydroxys such as malic acid, tartaric acid, and citric acid.
  • dicarboxylic acids such as succinic acid, malonic acid, succinic acid, glutaric acid, adipic acid, propylmalonic acid, and maleic acid
  • hydroxys such as malic acid, tartaric acid, and citric acid.
  • two or more compounds may be used in combination.
  • carboxylic acid group-containing compound may be a neutralized product of an organic compound having a —COOH group (for example, an organic compound having a —COONa group or the like).
  • the inorganic acid is not particularly limited, and examples thereof include hydrochloric acid, sulfuric acid, nitric acid and the like.
  • the inorganic acid may be added so that the concentration in the reaction (treatment) solution is 0.5 to 2.5 mol / L, more preferably 0.8 to 1.4 mol / L.
  • the step (2) is preferably performed by suspending the compound obtained in the step (1) in pure water and heating it with stirring as necessary.
  • the carboxylic acid group-containing compound and the inorganic acid may be added simultaneously or sequentially, but it is preferable to add them sequentially.
  • the addition may be to add an inorganic acid after the addition of the carboxylic acid group-containing compound, or to add the carboxylic acid group-containing compound after the addition of the inorganic acid.
  • a carboxyl group-containing compound is added to the suspension of the compound obtained by the above step (1), heating is started, and the inorganic acid is added when the liquid temperature is 60 ° C. or higher, preferably 90 ° C. or higher. Adding and maintaining the liquid temperature, preferably stirring for 15 minutes to 5 hours, more preferably 2 to 3 hours (Method 1); heating the suspension of the compound obtained by the above step (1)
  • an inorganic acid is added when the liquid temperature is 60 ° C. or higher, preferably 90 ° C. or higher, and a carboxylic acid group-containing compound is added 10 to 15 minutes after the inorganic acid addition, and the liquid temperature is preferably maintained.
  • a method of stirring for 15 minutes to 5 hours, more preferably 2 to 3 hours (Method 2).
  • the carboxylic acid group-containing compound is preferably used in an amount of 0.25 to 1.5 mol% with respect to 100 mol% of TiO 2 , and 0.4 to More preferably, it is used at a ratio of 0.8 mol%.
  • the addition amount of the carboxylic acid group-containing compound is less than 0.25 mol%, there is a possibility that particle growth proceeds and particles having the target particle size may not be obtained.
  • the amount is more than 5 mol%, rutile conversion of the particles does not proceed and anatase particles may be formed.
  • the carboxylic acid group-containing compound is preferably used in an amount of 1.6 to 4.0 mol% with respect to 100 mol% of TiO 2 , and is preferably 2.0 to It is more preferable to use it at a ratio of 2.4 mol%.
  • the addition amount of the carboxylic acid group-containing compound is less than 1.6 mol%, there is a possibility that the particle growth proceeds and particles having the target particle size may not be obtained, and the addition amount of the carboxylic acid group-containing compound is 4. If the amount is more than 0 mol%, the rutile conversion of the particles may not proceed and anatase particles may be formed. Even if the amount of the carboxylic acid group-containing compound exceeds 4.0 mol%, the effect will be good. It is economically disadvantageous. Further, if the addition of the carboxylic acid group-containing compound is performed in less than 10 minutes after the addition of the inorganic acid, there is a possibility that the rutileization will not proceed and anatase-type particles may be formed. In some cases, the particle growth proceeds excessively, and particles having a target particle size cannot be obtained.
  • step (2) it is preferable to cool after completion of the reaction (treatment) and further neutralize to pH 5.0 to 10.0.
  • the neutralization can be performed with an alkaline compound such as an aqueous sodium hydroxide solution or aqueous ammonia.
  • the target rutile type fine particle titanium dioxide can be separated by filtering and washing with water after neutralization.
  • titanium dioxide fine particles As other methods for producing titanium dioxide fine particles, known methods described in “Titanium oxide—physical properties and applied technology” (Kagino Kiyono, pp 255-258 (2000) Gihodo Publishing Co., Ltd.) can be used.
  • JP-A-2000-053421 comprising alkyl silicate as a dispersion stabilizer, and silicon in the alkyl silicate is changed to SiO 2.
  • the titanium oxide particles may be coated with a silicon-containing hydrated oxide.
  • the coating amount of the silicon-containing hydrated compound is 3 to 30% by mass, preferably 3 to 10% by mass, more preferably 3 to 8% by mass. This is because if the coating amount is 30% by mass or less, a desired refractive index of the high refractive index film can be obtained, and if the coating amount is 3% or more, particles can be stably formed.
  • titanium oxide particles with a silicon-containing hydrated oxide it can be produced by a conventionally known method.
  • JP-A-10-158015 Si / Al hydration to rutile titanium oxide) Oxide treatment
  • a method for producing a titanium oxide sol in which a hydrous oxide of silicon and / or aluminum is deposited on the surface of titanium oxide after peptization in the alkaline region of the titanate cake JP 2000-204301 A (A sol in which a rutile-type titanium oxide is coated with a complex oxide of Si and Zr and / or Al.
  • JP 2007-246351 Oxidation obtained by peptizing hydrous titanium oxide
  • titanium to hydrosol
  • R 1 n SiX 4-n wherein R 1 as stabilizer C 1 -C 8 alkyl group, glycidyloxy substituted C 1 -C 8 Alkyl group or a C 2 -C 8 alkenyl group, X is an alkoxy group, n is 1 or 2.
  • Sodium silicate added in the alkaline range the compound having a complexing effect on organoalkoxysilanes or titanium oxide Alternatively, it is possible to refer to matters described in, for example, a method for producing a titanium oxide hydrosol coated with a hydrous oxide of silicon by adding, adjusting pH, and aging a silica sol solution.
  • a titanium oxide sol stabilized at a pH in an 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.
  • Neutralization method Japanese Patent Laid-Open No.
  • Colloidal aggregates are formed, and then the electrolyte in the aggregate slurry is removed to produce a stable aqueous sol of composite colloidal particles comprising titanium oxide; silicates (e.g., sodium silicate)
  • silicates e.g., sodium silicate
  • a stable aqueous sol of composite colloidal particles containing silicon dioxide is produced by preparing an aqueous solution containing the aqueous solution) and removing the cations present in the aqueous solution; the resulting composite containing titanium oxide 100 parts by weight of the aqueous sol in terms of metal oxide TiO 2 and 2 to 100 parts by weight of the resulting composite aqueous sol containing silicon dioxide in terms of metal oxide SiO 2 were mixed together.
  • Japanese Patent Laid-Open No. 2000-063119 Japanese Patent Laid-Open No. 2000-063119
  • adding hydroperoxide to hydrous titanic acid gel or sol to dissolve hydrous titanic acid, and obtaining peroxotitanic acid A silicon compound or the like is added to the aqueous solution and heated to obtain a dispersion of core particles composed of a complex solid solution oxide having a rutile structure, and then the silicon compound or the like is added to the dispersion of the core particles.
  • the volume average particle diameter of the titanium oxide particles is preferably 30 nm or less, more preferably 1 to 30 nm, and even more preferably 5 to 15 nm.
  • a volume average particle size of 30 nm or less is preferable from the viewpoint of low haze and excellent visible light transmittance.
  • the volume average particle diameter is a volume average particle diameter of primary particles or secondary particles dispersed in a medium, and can be measured by a laser diffraction / scattering method, a dynamic light scattering method, or the like.
  • the particles themselves or the particles appearing on the cross section or surface of the refractive index film are observed with an electron microscope, and the particle diameters of 1,000 arbitrary particles are measured, and d1, d2,. ...
  • Nk particles each having a particle size of dk the volume average particle size when the volume per particle is vi
  • colloidal silica composite emulsion can also be used as a metal oxide in the low refractive index film.
  • the colloidal silica composite emulsion preferably used in the present invention has a central part of a particle mainly composed of a polymer or copolymer, and is described in JP-A-59-71316 and JP-A-60-127371. It is obtained by polymerizing a monomer having an ethylenically unsaturated bond in the presence of colloidal silica which has been conventionally known by an emulsion polymerization method.
  • the particle diameter of colloidal silica applied to the composite emulsion is preferably less than 40 nm.
  • the colloidal silica used for the preparation of this composite emulsion usually includes primary particles of 2 to 100 nm.
  • the ethylenic monomer include (meth) acrylic acid ester having 1 to 18 carbon atoms, aryl group, or allyl group, styrene, ⁇ -methylstyrene, vinyl toluene, acrylonitrile, vinyl chloride, vinylidene chloride. , Vinyl acetate, vinyl propionate, acrylamide, N-methylol acrylamide, ethylene, butadiene, and other materials known in the latex industry, and if necessary, vinyl trimethoate is used to improve compatibility with colloidal silica.
  • Vinyl silanes such as oxysilane, vinyltriethoxysilane, ⁇ -methacrylooxypropyltrimethoxysilane, etc. are also used to stabilize the dispersion of (meth) acrylic acid, maleic acid, maleic anhydride, fumaric acid, crotonic acid.
  • Anionic monomers such as -Is used as an auxiliary agent.
  • two or more types of ethylenic monomers can be used together as necessary.
  • the ratio of ethylenic monomer / colloidal silica in the emulsion polymerization is preferably 100/1 to 200 in terms of solid content.
  • colloidal silica composite emulsions used in the present invention those having a glass transition point in the range of ⁇ 30 to 30 ° C. are preferable.
  • compositions include ethylenic monomers such as acrylic acid esters and methacrylic acid esters, and particularly preferred are copolymers of (meth) acrylic acid esters and styrene, alkyl (meth) acrylates.
  • ethylenic monomers such as acrylic acid esters and methacrylic acid esters
  • copolymers of (meth) acrylic acid esters and styrene, alkyl (meth) acrylates examples thereof include a copolymer of ester and (meth) acrylic acid aralkyl ester, and a (meth) acrylic acid alkyl ester and (meth) acrylic acid aryl ester copolymer.
  • emulsifiers used in emulsion polymerization include alkyl allyl polyether sulfonic acid soda salt, lauryl sulfonic acid soda salt, alkyl benzene sulfonic acid soda salt, polyoxyethylene nonylphenyl ether sodium nitrate salt, alkyl allyl sulfosuccinate soda salt, sulfo Examples include propyl maleic acid monoalkyl ester soda salt.
  • Each refractive index film forming the dielectric multilayer film can contain various additives as required.
  • various anionic, cationic or nonionic surfactants include various anionic, cationic or nonionic surfactants; dispersants such as polycarboxylic acid ammonium salt, allyl ether copolymer, benzenesulfonic acid sodium salt, graft compound dispersant, polyethylene glycol type nonionic dispersant; Organic acid salts such as acetate, propionate or citrate; organic ester plasticizers such as monobasic organic acid esters and polybasic organic acid esters, organic phosphate plasticizers, organic phosphorous acid plasticizers, etc.
  • dispersants such as polycarboxylic acid ammonium salt, allyl ether copolymer, benzenesulfonic acid sodium salt, graft compound dispersant, polyethylene glycol type nonionic dispersant
  • Organic acid salts such as acetate, propionate or citrate
  • organic ester plasticizers such as monobasic organic acid esters and polybasic organic acid esters, organic phosphat
  • Plasticizers such as phosphoric acid plasticizers; ultraviolet absorbers described in JP-A-57-74193, JP-A-57-87988, and JP-A-62-261476, JP-A-57-74192, JP-A-57 -87989, 60-72785, 61-14659, JP-A-1-95091 and 3-13376, etc .; Japanese Patent Laid-Open Nos. 59-42993, 59-52689, 62-280069, 61-242871, and Japanese Patent Laid-Open No.
  • Optical brighteners described in the Gazettes, etc . pH adjusters such as sulfuric acid, phosphoric acid, acetic acid, citric acid, sodium hydroxide, potassium hydroxide, potassium carbonate; antifoaming agents; lubricants such as diethylene glycol; Agents; antistatic agents; may contain various known additives such as matting agents.
  • the above-mentioned dielectric multilayer film can be laminated on a film support if necessary.
  • various resin films can be used, such as polyolefin films (polyethylene, polypropylene, etc.), polyester films (polyethylene terephthalate, polyethylene naphthalate, etc.), polyvinyl chloride, cellulose acetate, etc. Can be used, and a polyester film is preferable.
  • 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 component dicarboxylic acid component includes 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 thickness of the film support used in the present invention is preferably 10 to 300 ⁇ m, particularly 20 to 150 ⁇ m.
  • the film support of the present invention may be a laminate of two sheets. In this case, the type may be the same or different.
  • the functional layer is not particularly limited, but is a conductive layer, an antistatic layer, a gas barrier layer, an easy adhesion layer (adhesion layer), an antifouling layer, a deodorant layer, a droplet layer, an easy slip layer, Used for hard coat layer, abrasion-resistant layer, antireflection layer, electromagnetic wave shielding layer, ultraviolet absorption layer, infrared absorption layer, printing layer, fluorescent light emitting layer, hologram layer, release layer, adhesive layer, adhesive layer, laminated glass Examples include an intermediate film layer, a heat insulating layer, a heat ray reflective layer, and a heat dissipation layer.
  • the ultraviolet absorber used in the ultraviolet absorbing layer for example, the ultraviolet absorbers described in JP-A-57-74193, JP-A-57-87988, and JP-A-62-261476 can be used.
  • the thickness of the functional layer is preferably 0.1 ⁇ m to 50 ⁇ m, more preferably 1 to 20 ⁇ m.
  • the filter of the present invention preferably includes a hard coat layer as a surface protective layer for enhancing the scratch resistance. Specifically, it is preferable to laminate a hard coat layer containing a resin that is cured by heat, ultraviolet rays, or the like on the uppermost layer on the side opposite to the side having the dielectric multilayer film.
  • the 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.
  • Such cured resins can be used singly or in combination of two or more.
  • an ultraviolet curable resin it is synthesized from, for example, a polyfunctional acrylate resin such as acrylic acid or methacrylic acid ester having a polyhydric alcohol, and acrylic acid or methacrylic acid having a diisocyanate and a polyhydric alcohol.
  • a polyfunctional acrylate resin such as acrylic acid or methacrylic acid ester having a polyhydric alcohol, and acrylic acid or methacrylic acid having a diisocyanate and a polyhydric alcohol.
  • polyfunctional urethane acrylate resins can be mentioned.
  • polyether resins, polyester resins, epoxy resins, alkyd resins, spiroacetal resins, polybutadiene resins or polythiol polyene resins having an acrylate-based functional group can also be suitably used.
  • benzoins such as benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzyl methyl ketal and the like Alkyl ethers; acetophenones such as acetophenone, 2,2-dimethoxy-2-phenylacetophenone, 1-hydroxycyclohexyl phenyl ketone; anthraquinones such as methylanthraquinone, 2-ethylanthraquinone, 2-amylanthraquinone; thioxanthone, 2,4 -Thioxanthones such as diethylthioxanthone and 2,4-diisopropylthioxanthone; Ketals such as acetophenone dimethyl ketal and benzyldimethyl ketal; Benzophenone and 4,4-b
  • tertiary amines such as triethanolamine and methyldiethanolamine
  • photoinitiators such as 2-dimethylaminoethylbenzoic acid and benzoic acid derivatives such as ethyl 4-dimethylaminobenzoate
  • radical polymerization initiators are used in an amount of 0.5 to 20 parts by weight, preferably 1 to 15 parts by weight, based on 100 parts by weight of the polymerizable component of the resin.
  • a well-known general paint additive with the above-mentioned cured resin as needed.
  • a silicone-based or fluorine-based paint additive that imparts leveling or surface slip properties is effective in preventing scratches on the surface of a cured film, and in the case of using ultraviolet rays as active energy rays, When the additive bleeds to the air interface, the inhibition of curing of the resin by oxygen can be reduced, and an effective degree of curing can be obtained even under low irradiation intensity conditions.
  • the hard coat layer preferably contains inorganic fine particles.
  • Preferable inorganic fine particles include fine particles of an inorganic compound containing a metal such as titanium, silica, zirconium, aluminum, magnesium, antimony, zinc or tin.
  • the average particle size of the inorganic fine particles is preferably 1000 nm or less, and more preferably in the range of 10 to 500 nm, from the viewpoint of ensuring visible light transmittance.
  • the inorganic fine particles have a higher bond strength with the cured resin forming the hard coat layer, and can be prevented from falling off the hard coat layer. Therefore, a photosensitive group having photopolymerization reactivity such as monofunctional or polyfunctional acrylate. Those in which is introduced into the surface are preferred.
  • the thickness of the hard coat layer is preferably 0.1 ⁇ m to 50 ⁇ m, more preferably 1 to 20 ⁇ m. If it is 0.1 ⁇ m or more, the hard coat property tends to be improved. Conversely, if it is 50 ⁇ m or less, the transparency tends to be improved.
  • the method for forming the hard coat layer is not particularly limited. For example, after preparing a coating liquid for hard coat layer containing the above components, the coating liquid is applied with a wire bar or the like, and the coating liquid is cured with heat and / or UV. And a method of forming a hard coat layer.
  • the filter of the present invention can be used for various applications.
  • a colored film for decoration a color filter that modulates the color of the light source
  • a reflective mirror for visible light or infrared light
  • a white LED for visible light or infrared light
  • a white LED for visible light or infrared light
  • a white LED for visible light or infrared light
  • a white LED for visible light or infrared light
  • a white LED a white LED
  • a fluorescent light a color filter for organic EL lighting
  • it is preferably used for agriculture where light from a light source is modulated to promote plant growth.
  • narrow band light with a band edge such as red light of 640 nm to 690 nm and blue light of 420 nm to 470 nm are optimal for promoting photosynthesis and normal formation of leaves.
  • the transmission wavelength region is determined depending on the material, so it cannot be designed to transmit the desired wavelength, but in the filter of the present invention, a filter is formed in accordance with the target set wavelength. Therefore, it can be used particularly for plant growth promotion. Therefore, a narrow band-pass filter that exhibits maximum transmittance in a blue light region of 400 nm to 500 nm or a red light region of 630 to 700 nm is suitable.
  • the present invention also includes a plant growth promoting method for promoting plant growth using the narrow band-pass filter.
  • the target wavelength is appropriately set depending on the plant species and the plant part that is desired to promote growth.
  • Specific examples of the method (1) include the following forms: (1) A high refractive index film coating solution is applied on a substrate and dried to form a high refractive index film. A method of forming a low refractive index film by applying a refractive film coating liquid and drying; (2) A low refractive index film coating liquid is applied and dried on a substrate to form a low refractive index film.
  • a method of forming a film by applying a high refractive index film coating liquid and drying to form a film (3) coating a high refractive index film coating liquid and a low refractive index film on the substrate
  • a method of forming a film including a high refractive index film and a low refractive index film by alternately coating and drying the liquid alternately and successively (4) A high refractive index film coating liquid and a low refractive index on a substrate
  • a method of forming a film containing a high refractive index film and a low refractive index film by simultaneously applying a multilayer coating with a film coating solution and drying Especially, it is preferable that it is simultaneous multilayer coating of (4) from a viewpoint of production efficiency.
  • a synthetic polymer such as polyvinyl alcohol, a water-soluble polymer such as gelatin and a thickening polysaccharide is used as a binder for preparing each layer coating liquid and laminating by simultaneous multilayering. It can be used suitably.
  • a water-soluble polymer is contained as an organic polymer.
  • a plurality of constituent layers including a high-refractive index film and a low-refractive index film can be appropriately selected from known coating methods, and simultaneously coated in water on a support, and then set and dried.
  • the coating method include a roll coating method, a rod bar coating method, an air knife coating method, a spray coating method, a curtain coating method, or US Pat. Nos. 2,761,419 and 2,761,791.
  • a slide bead coating method using an hopper, an extrusion coating method, or the like is preferably used.
  • the refractive index film contains a water-soluble polymer and metal oxide particles
  • a multilayer body is formed by multilayer coating, so that the mass ratio (F / B) of the water-soluble polymer and metal oxide particles in each film coating solution. Is preferably in the range of 0.3 to 10, more preferably 0.5 to 5.
  • the time from simultaneous multilayer coating to sol-gel transition and setting is within 5 minutes, preferably within 2 minutes. Moreover, it is preferable to take time of 45 seconds or more.
  • Adjust the set time by adjusting the viscosity according to the concentration of metal oxide particles and other components, adjusting the binder mass ratio, and adding various known gelling agents such as gelatin, pectin, agar, carrageenan and gellan gum. It can be performed by adjustment.
  • the term “set” refers to, for example, increasing the viscosity of the coating composition by lowering the temperature by applying cold air or the like to the coating, reducing the fluidity of the material between each layer and each layer, or gelling.
  • the time from application to set is what the finger has when the cold air of 5-10 ° C is applied to the coating film from the surface and the finger is pressed against the surface. Let's say lost time.
  • the temperature condition when using cold air is preferably 25 ° C. or lower, more preferably 10 ° C. or lower.
  • the time for which the coating film is exposed to the cold air is preferably 10 seconds or more and 120 seconds or less, although it depends on the coating conveyance speed.
  • the solvent for preparing each coating solution for simultaneous multilayer coating is not particularly limited, but water, an organic solvent, or a mixed solvent thereof is preferable.
  • an aqueous solvent can be used because polyvinyl alcohol is mainly used as the resin binder. Compared to the case where an organic solvent is used, the aqueous solvent does not require a large-scale production facility, so that it is preferable in terms of productivity and also in terms of environmental conservation.
  • the organic solvent 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, diethyl ether, Examples thereof include ethers such as 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 preferably water or a mixed solvent of water and methanol, ethanol, or ethyl acetate, and more preferably water.
  • the viscosity of each coating solution at the time of simultaneous multilayer coating is preferably in the range of 5 to 100 mPa ⁇ s, more preferably 10 to 50 mPa ⁇ s in the temperature range of 25 to 60 ° C. It is the range of s.
  • the range of 5 to 1200 mPa ⁇ s is preferable, and the range of 25 to 500 mPa ⁇ s is more preferable.
  • 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 10 , 30,000 to 30,000 mPa ⁇ s.
  • the coating solution is heated to 30 ° C. or higher and coated, and then the temperature of the formed coating film is once cooled to 1 to 15 ° C. and dried 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 method described in US Pat. No. 6,049,419 can be used. That is, a high-refractive-index film material polymer and other additives (high-refractive-index film-forming composition) and a low-refractive-film material polymer and other additives (low-refractive-index film-forming composition) are co-extruded. Can be used to form a high refractive index film and a low refractive index film.
  • each refractive index film material is melted at 85 to 300 ° C. so as to have a viscosity suitable for extrusion, and various additives are added as necessary, so that both polymers are alternately formed into two layers.
  • the extruded laminated film is cooled and solidified by a cooling drum or the like to obtain a laminated body.
  • the laminate is heated and then stretched in two directions to obtain a narrow band filter.
  • the unstretched film obtained by peeling from the above-mentioned cooling drum is subjected to a glass transition temperature (Tg) of ⁇ 50 ° C. to Tg + 100 ° C. via a plurality of roll groups and / or a heating device such as an infrared heater. It is preferable that the film is heated inside and stretched in one or more stages in the film conveying direction (also referred to as the longitudinal direction). Next, it is also preferable to stretch the stretched film obtained as described above in a direction perpendicular to the film transport direction (also referred to as the width direction). In order to stretch the film in the width direction, it is preferable to use a tenter device.
  • Tg glass transition temperature
  • heat processing can be performed subsequent to stretching.
  • the thermal processing is preferably carried out in the range of Tg-100 ° C. to Tg + 50 ° C., usually for 0.5 to 300 seconds.
  • the heat processing means is not particularly limited and can be generally performed with hot air, infrared rays, a heating roll, microwaves, or the like, but is preferably performed with hot air in terms of simplicity.
  • the heating of the film is preferably increased stepwise.
  • the heat-processed film is usually cooled to Tg or less, and the clip gripping portions at both ends of the film are cut and wound.
  • the cooling is gradually performed from the final heat processing temperature to Tg at a cooling rate of 100 ° C. or less per second.
  • the means for cooling is not particularly limited, and can be performed by a conventionally known means. In particular, it is preferable to perform these treatments while sequentially cooling in a plurality of temperature ranges from the viewpoint of improving the dimensional stability of the film.
  • the cooling rate is a value obtained by (T1 ⁇ Tg) / t, where T1 is the final heat processing temperature and t is the time until the film reaches Tg from the final heat processing temperature.
  • PET polyethylene terephthalate
  • the optical film thickness of each refractive index layer in the narrow-band bandpass filter of Comparative Example 1 is ( ⁇ / 4-96). %) To ( ⁇ / 4 + 44%), where ⁇ / 4-96% means ⁇ / 4- ⁇ / 4 ⁇ 96/100, and so on.
  • the numerical value in parentheses described next to the material of the layer structure is the physical film thickness value of each refractive index film.
  • Example 2 Comparative Example 2
  • silver, TiO 2 , SiO 2 , and MgF 2 are converted into PET / TiO 2 (76 nm) / (SiO 2 (100 nm) / TiO 2 (64 nm)) 3 / MgF 2 using a known sputtering method.
  • Example 3 Comparative Example 3
  • Ta 2 O 5 and SiO 2 are changed into PET / (Ta 2 O 5 (70 nm) / SiO 2 (106 nm)) 5 / Ta 2 O 5 (70 nm) / SiO 2.
  • the optical film thickness of each refractive index layer in the narrow-band bandpass filter of Example 2 was in the range of ( ⁇ / 4-67%) to ( ⁇ / 4 + 43%).
  • PBT Toraycon 1401-X06, manufactured by Toray Industries, Inc.
  • Example 9 Example 6 (Preparation of coating solution for low refractive index film)
  • water-soluble resin PVA224 manufactured by Kuraray Co., Ltd., saponification degree 88%, polymerization degree 1000
  • water-soluble resin R1130 manufactured by Kuraray Co., Ltd., By adding 5.0 parts by mass of silanol-modified polyvinyl alcohol
  • water-soluble resin Nichigo G polymer AZF8035W manufactured by Nippon Synthetic Chemical Industry Co., Ltd.
  • the entire amount of the water-soluble resin aqueous solution was added to and mixed with 350 parts by mass of 10% by mass acidic silica sol (Snowtex (registered trademark) OXS, manufactured by Nissan Chemical Industries, Ltd.) containing silica fine particles having an average particle diameter of 5 nm. Furthermore, 0.3 parts by mass of Lapisol A30 (manufactured by Nippon Oil & Fats Co., Ltd.) was added as an anionic activator, and after stirring for 1 hour, the coating solution for low refractive index film was prepared by finishing to 1000.0 g with pure water .
  • Snowtex registered trademark
  • OXS organic silica sol
  • Lapisol A30 manufactured by Nippon Oil & Fats Co., Ltd.
  • aqueous dispersion of titanium oxide sol Sodium hydroxide aqueous solution (concentration 10 mol / L) was added to 10 L of an aqueous suspension (TiO 2 concentration 100 g / L) in which titanium oxide hydrate was suspended in water with stirring, and the temperature was raised to 90 ° C. After warming and aging for 5 hours, it was neutralized with hydrochloric acid, filtered and washed with water.
  • titanium oxide hydrate was obtained by thermal hydrolysis of an aqueous titanium sulfate solution according to a known method.
  • the titanium oxide hydrate treated with the base was suspended in pure water so that the TiO 2 concentration was 20 g / L, and 0.4 mol% of citric acid was added to the amount of TiO 2 with stirring to raise the temperature.
  • concentrated hydrochloric acid was added to a hydrochloric acid concentration of 30 g / L, and the mixture was stirred for 3 hours while maintaining the liquid temperature.
  • the pH and zeta potential of the obtained titanium oxide sol solution were measured, the pH was 1.4 and the zeta potential was +40 mV. Furthermore, when the particle size was measured with a Zetasizer Nano manufactured by Malvern, the average particle size was 35 nm, and the monodispersity was 16%. Also, the titanium oxide sol solution was dried at 105 ° C. for 3 hours to obtain a particle powder, and X-ray diffraction measurement was performed using JDX-3530 type manufactured by JEOL Datum Co., Ltd. to confirm that the particles were rutile type particles. did. Moreover, the volume average particle diameter was 10 nm.
  • the coating apparatus a slide hopper coating apparatus capable of simultaneously coating 21 layers was used. On the 30 cm ⁇ 30 cm size 50 ⁇ m thick polyethylene terephthalate (PET) film (A4300: double-sided easy-adhesive layer, manufactured by Toyobo Co., Ltd.), the coating solution for the low refractive index film and the coating solution for the high refractive index film prepared above are used.
  • PET polyethylene terephthalate
  • the layers were applied simultaneously. Immediately after that, after setting the film surface by blowing cold air for 1 minute under the condition that the film surface is 15 ° C.
  • the dielectric multilayer film is a dielectric film containing an organic polymer and a metal oxide by drying by blowing hot air of 80 ° C.
  • the optical film thickness of each refractive index layer in the narrowband bandpass filter of Example 6 is ( ⁇ / 4-11%) to ( ⁇ / 4 + 36%).
  • the layer structure is PET / (low refractive index film (119 nm) / high refractive index film (78 nm) 5 / low refractive index film (119 nm) / high refractive index film (157 nm) / low refractive index film ( 119 nm) / (High refractive index film (78 nm) / Low refractive index film (119 nm)) 5 /
  • the dielectric multilayer film contains an organic polymer and a metal oxide, except that it is a high refractive index film (157 nm). Then, a dielectric type narrow band-pass filter (FIG.
  • Sample 11 Example 8
  • Sample 11 was prepared in the same manner as Sample 10 except that a visible light shielding layer was provided.
  • Example 12 Example 9
  • PVA224, TINUVIN-P manufactured by Ciba Japan Co., Ltd.
  • TINUVIN326 manufactured by Ciba Japan Co., Ltd.
  • a functional film having a dry film thickness of 3 ⁇ m containing 80/15/5 in volume ratio.
  • UV curable hard coat material UV-7600B, manufactured by Nippon Synthetic Chemical Industry Co., Ltd.
  • UV-7600B manufactured by Nippon Synthetic Chemical Industry Co., Ltd.
  • a photopolymerization initiator Irgacure (registered trademark) 184, Ciba Specialty) (Chemicals Co., Ltd.) 0.5 parts by mass was added and stirred and mixed.
  • ATO powder ultrasonine particle ATO, manufactured by Sumitomo Metal Mining Co., Ltd.
  • the hard coat layer coating solution is applied with a wire bar to a dry film thickness of 3 ⁇ m, and hot air is applied at 70 ° C. for 3 minutes. Dried. After that, by curing with an irradiation amount of 400 mJ / cm 2 with a UV curing device (using a high-pressure mercury lamp) manufactured by Eye Graphics Co., Ltd. in the atmosphere, an infrared light blocking hard coat layer is formed. Sample 13 was produced.
  • Example 14 Comparative Example 4
  • Ta 2 O 5 and SiO 2 are changed into PET / (SiO 2 (110 nm) / Ta 2 O 5 (64.5 nm) 5 / SiO 2 (110 nm) / Ta 2 ).
  • Example 15 Layer structure is PET / (low refractive index film (119 nm) / high refractive index film (78 nm) 5 / low refractive index film (119 nm) / high refractive index film (180 nm) / low refractive index film (119 nm) / (high refractive index
  • the dielectric multilayer film contains an organic polymer and a metal oxide in the same manner as in Example 10 except that the refractive index film (78 nm) / low refractive index film (119 nm)) 5 / high refractive index film (180 nm) is used.
  • a dielectric type narrow band-pass filter (FIG.
  • each refractive index layer was in the range of ( ⁇ / 4-9%) to ( ⁇ / 4 + 5%).
  • a spectrophotometer (U-4000 model, manufactured by Hitachi, Ltd.) is attached with a transmission unit, and after baseline correction by blank measurement, the surface side of the dielectric multilayer film is used as the measurement surface, and 0.5 nm in the region of 400 to 700 nm.
  • the transmittance at 600 points was measured at intervals, and the wavelength and transmittance of the narrowband passband were obtained.
  • Table 2 shows the durability evaluation results. It can be seen that the configuration satisfying the present invention is excellent in durability in both the bending test and the forced deterioration test with little decrease in wavelength transmittance in a narrow band pass band.

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Abstract

L'objectif de la présente invention est d'obtenir un film optique dont le coût de production est réduit, qui peut être produit de façon à avoir une plus grande surface et qui présente une excellente durabilité lorsqu'il est plié ou utilisé dans des conditions de température et d'humidité élevées. Pour ce faire, l'invention concerne un filtre passe-bande à région étroite comprenant un film diélectrique multicouches obtenu à partir de polymères organiques.
PCT/JP2012/081829 2012-01-13 2012-12-07 Filtre passe-bande à région étroite WO2013105374A1 (fr)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015230477A (ja) * 2014-06-06 2015-12-21 コニカミノルタ株式会社 光学反射フィルム
KR20200088125A (ko) * 2019-01-14 2020-07-22 경기대학교 산학협력단 전자기파의 선택적 필터링 소자 및 이를 이용한 전자기파 센서 시스템
TWI705269B (zh) * 2019-03-27 2020-09-21 群光電子股份有限公司 影像擷取裝置、濾光膜及濾光膜的製作方法
US10837905B2 (en) 2018-09-14 2020-11-17 Kabushiki Kaisha Toshiba Optical sensor
KR20210030526A (ko) * 2019-09-09 2021-03-18 킹레이 테크놀로지 컴퍼니 리미티드 적외선 협대역 통과 필터링 구조 및 이를 이용한 적외선 협대역 통과 여파기

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03245104A (ja) * 1990-02-23 1991-10-31 Matsushita Electric Works Ltd 多層干渉膜
JPH08160220A (ja) * 1994-12-05 1996-06-21 Fujikura Ltd 光学多層膜フィルタ
JP2002509271A (ja) * 1998-01-13 2002-03-26 ミネソタ マイニング アンド マニュファクチャリング カンパニー カラーシフトフィルム
JP2002535735A (ja) * 1999-01-29 2002-10-22 キネティック リミテッド 多層光フィルタ

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03245104A (ja) * 1990-02-23 1991-10-31 Matsushita Electric Works Ltd 多層干渉膜
JPH08160220A (ja) * 1994-12-05 1996-06-21 Fujikura Ltd 光学多層膜フィルタ
JP2002509271A (ja) * 1998-01-13 2002-03-26 ミネソタ マイニング アンド マニュファクチャリング カンパニー カラーシフトフィルム
JP2002535735A (ja) * 1999-01-29 2002-10-22 キネティック リミテッド 多層光フィルタ

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015230477A (ja) * 2014-06-06 2015-12-21 コニカミノルタ株式会社 光学反射フィルム
US10837905B2 (en) 2018-09-14 2020-11-17 Kabushiki Kaisha Toshiba Optical sensor
KR20200088125A (ko) * 2019-01-14 2020-07-22 경기대학교 산학협력단 전자기파의 선택적 필터링 소자 및 이를 이용한 전자기파 센서 시스템
KR102250409B1 (ko) 2019-01-14 2021-05-12 경기대학교 산학협력단 전자기파의 선택적 필터링 소자 및 이를 이용한 전자기파 센서 시스템
TWI705269B (zh) * 2019-03-27 2020-09-21 群光電子股份有限公司 影像擷取裝置、濾光膜及濾光膜的製作方法
KR20210030526A (ko) * 2019-09-09 2021-03-18 킹레이 테크놀로지 컴퍼니 리미티드 적외선 협대역 통과 필터링 구조 및 이를 이용한 적외선 협대역 통과 여파기
KR102288217B1 (ko) 2019-09-09 2021-08-10 킹레이 테크놀로지 컴퍼니 리미티드 적외선 협대역 통과 필터링 구조 및 이를 이용한 적외선 협대역 통과 여파기

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