WO2014189037A1 - 光取り出しフィルム及びその製造方法、並びに面発光体 - Google Patents
光取り出しフィルム及びその製造方法、並びに面発光体 Download PDFInfo
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- WO2014189037A1 WO2014189037A1 PCT/JP2014/063318 JP2014063318W WO2014189037A1 WO 2014189037 A1 WO2014189037 A1 WO 2014189037A1 JP 2014063318 W JP2014063318 W JP 2014063318W WO 2014189037 A1 WO2014189037 A1 WO 2014189037A1
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- WIPO (PCT)
- Prior art keywords
- light extraction
- extraction film
- meth
- light
- acrylate
- Prior art date
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- FVXBCDWMKCEPCL-UHFFFAOYSA-N nonane-1,1-diol Chemical compound CCCCCCCCC(O)O FVXBCDWMKCEPCL-UHFFFAOYSA-N 0.000 description 1
- OTLDLKLSNZMTTA-UHFFFAOYSA-N octahydro-1h-4,7-methanoindene-1,5-diyldimethanol Chemical compound C1C2C3C(CO)CCC3C1C(CO)C2 OTLDLKLSNZMTTA-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- DXGLGDHPHMLXJC-UHFFFAOYSA-N oxybenzone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1 DXGLGDHPHMLXJC-UHFFFAOYSA-N 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920003055 poly(ester-imide) Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- UFDHBDMSHIXOKF-UHFFFAOYSA-N tetrahydrophthalic acid Natural products OC(=O)C1=C(C(O)=O)CCCC1 UFDHBDMSHIXOKF-UHFFFAOYSA-N 0.000 description 1
- WUPCFMITFBVJMS-UHFFFAOYSA-N tetrakis(1,2,2,6,6-pentamethylpiperidin-4-yl) butane-1,2,3,4-tetracarboxylate Chemical compound C1C(C)(C)N(C)C(C)(C)CC1OC(=O)CC(C(=O)OC1CC(C)(C)N(C)C(C)(C)C1)C(C(=O)OC1CC(C)(C)N(C)C(C)(C)C1)CC(=O)OC1CC(C)(C)N(C)C(C)(C)C1 WUPCFMITFBVJMS-UHFFFAOYSA-N 0.000 description 1
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 1
- 229960002447 thiram Drugs 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/858—Arrangements for extracting light from the devices comprising refractive means, e.g. lenses
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/62—Monocarboxylic acids having ten or more carbon atoms; Derivatives thereof
- C08F220/68—Esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/07—Aldehydes; Ketones
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
- G02B5/021—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures
- G02B5/0221—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures the surface having an irregular structure
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
- H10K85/115—Polyfluorene; Derivatives thereof
Definitions
- the present invention relates to a light extraction film, a method for producing the same, and a surface light emitter including the light extraction film, and in particular, light extraction from an organic EL element in a surface light emitter using an organic EL (electroluminescence) element as a light source. This is related to the technology.
- organic EL elements are expected to be used for flat panel displays, and are also expected to be used for next-generation lighting that can replace fluorescent lamps.
- the structure of the organic EL element is diversified from a simple structure in which an organic thin film serving as a light emitting layer is sandwiched between two films to a multilayer structure.
- Examples of the latter multilayered structure include a structure in which a positive hole transport layer, a light emitting layer, an electron transport layer, and a cathode are laminated on an anode provided on a glass substrate.
- the layers sandwiched between the anode and the cathode are all composed of organic thin films, and the thickness of each organic thin film is very thin, such as several tens of nm.
- the organic EL element is a laminated body of thin films, and the total reflection angle of light between the thin films is determined by the difference in the refractive index of each thin film material. At present, about 80% of the light generated in the light emitting layer is confined inside the organic EL element and cannot be extracted outside. Specifically, when the refractive index of the glass substrate is 1.5 and the refractive index of the air layer is 1.0, the critical angle ⁇ c is 41.8 °, and light having an incident angle smaller than the critical angle ⁇ c. Is emitted from the glass substrate to the air layer. Light having an incident angle larger than the critical angle ⁇ c is totally reflected and confined inside the glass substrate. Therefore, it is required to realize a light extraction function for extracting light trapped inside the glass substrate on the surface of the organic EL element to the outside of the glass substrate, that is, to improve light extraction efficiency and normal luminance.
- an organic EL element that emits isotropically, there is a demand for reducing the emission angle dependency of the wavelength of light emitted from the organic EL element, as well as improving light extraction efficiency and normal luminance. That is, when the light emitted from the light emitting layer passes through the glass substrate and is emitted from the glass substrate, the difference in the emission angle depending on the wavelength is small, in other words, the wavelength dependence of the light distribution from the glass substrate is as small as possible. It is requested.
- Patent Document 1 proposes a surface light emitter using a microlens sheet (optical film) having a fine unit lens made of urethane acrylate resin as a light extraction film.
- the light extraction film proposed in Patent Document 1 has an uneven structure on the surface of the film, so that the light extraction efficiency is improved. However, since the refractive index of the member is low, the light extraction efficiency is improved. The effect is not enough.
- a first object of the present invention is to provide an EL that makes it possible to sufficiently improve the light extraction efficiency and normal luminance of the surface light emitter and sufficiently suppress the emission angle dependence of the emission light wavelength of the surface light emitter.
- Another object of the present invention is to provide a surface light emitter in which the normal luminance is sufficiently improved and the emission angle dependence of the emission light wavelength is sufficiently suppressed.
- the second object of the present invention is to sufficiently improve the light extraction efficiency and normal luminance of the surface light emitter and to sufficiently suppress the emission angle dependence of the emission light wavelength, and to prevent discoloration due to UV exposure.
- An object of the present invention is to provide a light extraction film having excellent long-term stability and a surface light emitter provided with the light extraction film.
- the present inventor as a result, in an EL light extraction film having a concavo-convex structure on the surface, the material constituting the film includes at least one of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton. It has been found that by using the resin (X) having the skeleton, it is possible to sufficiently improve the light extraction efficiency and normal luminance of the surface light emitter and sufficiently suppress the emission angle dependency of the emission light wavelength of the surface light emitter. The present invention has been completed.
- At least one of an ultraviolet absorber and a light stabilizer is used as a material constituting the EL light extraction film having a concavo-convex structure on the surface.
- the light extraction efficiency and normal brightness of the surface light emitter can be sufficiently improved and the emission angle dependence of the emission light wavelength can be sufficiently suppressed, and the light extraction that is difficult to discolor due to UV exposure and has excellent long-term stability. It has been found that a film can be formed.
- the light extraction film of the present invention is a light extraction film laminated on the substrate of the EL element,
- the light extraction film has an uneven structure on the surface
- the material constituting the light extraction film includes a resin (X) having at least one skeleton of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton.
- At least one of an ultraviolet absorber and a light stabilizer is contained.
- the surface light emitter of the present invention includes the light extraction film and an EL element.
- the manufacturing method of the light extraction film of this invention is a manufacturing method of the light extraction film laminated
- a monomer composition containing a monomer (x) having at least one skeleton of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton is supplied between a substrate and a mold having a concavo-convex structure transfer portion.
- the polymer composition is cured.
- the resin (X) having at least one of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton as a material constituting the EL light extraction film having an uneven structure on the surface. It is possible to provide an EL light extraction film that can sufficiently improve the light extraction efficiency and the normal luminance of the surface light emitter and sufficiently suppress the emission angle dependence of the emission light wavelength of the surface light emitter. . Further, by using such a light extraction film, it is possible to provide a surface light emitter in which the light extraction efficiency and the normal luminance are sufficiently improved and the emission angle dependency of the emission light wavelength is sufficiently suppressed.
- the light extraction film of the present invention in addition to the resin (X), by using at least one of an ultraviolet absorber and a light stabilizer, the light extraction efficiency and normal luminance of the surface light emitter are sufficient. It is possible to provide a light extraction film that improves and sufficiently suppresses the emission angle dependency of the emission light wavelength, and is difficult to discolor due to exposure to ultraviolet rays and has excellent long-term stability.
- the light extraction film of the present invention is a light extraction film laminated on a substrate of an EL element, and examples thereof include a light extraction film 10 as shown in FIG.
- the light extraction film 10 exhibits a function of extracting light from the EL element by being combined with an EL element (specifically, an organic EL element) as a light emitting source.
- the light extraction film 10 has an uneven structure 13 on the surface.
- the light extraction film 10 can be easily produced continuously, and is excellent in structural stability (specifically, maintaining the shape of the concavo-convex structure 13) and handleability of the light extraction film 10.
- the light extraction film 10 having the base layer 12 and the concavo-convex structure layer 11 is preferably formed by sequentially laminating the base layer 12 and the concavo-convex structure layer 11 having the concavo-convex structure 13 on the surface (upper surface).
- the material constituting the light extraction film needs to contain a resin (X) having at least one skeleton of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton.
- a resin (X) having at least one skeleton of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton.
- the light extraction efficiency and the normal luminance of the surface light emitter are further improved, and the emission angle dependency of the emission light wavelength of the surface light emitter is further suppressed, so that the light extraction film is configured.
- the content of the resin (X) in the material is preferably 30% by mass or more, more preferably 50% by mass or more, and further preferably in the range of 75 to 99% by mass.
- the resin (X) has at least one skeleton of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton.
- the resin having a fluorene skeleton has a fluorene structure. That is, the structural unit represented by the following formula (1) is included.
- the resin having a fluorene skeleton is preferably a resin having a high light transmittance in the visible light wavelength region (approximately 400 to 700 nm).
- the light transmittance of the resin having a fluorene skeleton is preferably 50 to 95%, because the appearance of the light extraction film 10 is excellent and the light extraction efficiency and normal luminance of the surface light emitter are excellent. 90% is more preferable.
- the light transmittance is a value measured according to JIS K7361.
- the resin having the biphenyl skeleton is a structural unit derived from biphenyl, that is, the following formula (2) Is included.
- the resin having a naphthalene skeleton is a structural unit derived from naphthalene, that is, the following formula (3): Is included.
- the resin (X) may have one of these skeletons alone or in combination of two or more.
- the resin (X) is excellent in the productivity of the light extraction film 10, further improves the light extraction efficiency and normal luminance of the surface light emitter, and further suppresses the emission angle dependence of the emission light wavelength of the surface light emitter.
- resin containing the structural unit represented by following formula (4) is preferable. (Wherein R 1 and R 2 are each independently a hydrogen atom or a methyl group, and a and b are each independently an integer of 0 to 4)
- the content of the structural unit represented by the formula (4) in the resin (X) further improves the light extraction efficiency and the normal luminance of the surface light emitter, and the emission angle dependency of the emission light wavelength of the surface light emitter. From the standpoint of further suppression, 30 to 99% by mass is preferable, and 50 to 95% by mass is more preferable.
- the fluorene skeleton, biphenyl skeleton and naphthalene skeleton that is, the structural unit derived from fluorene, the structural unit derived from biphenyl and the structural unit derived from naphthalene can be incorporated into various resins.
- the various resins include acrylic resins; polycarbonate resins; polyester resins; polyvinyl alcohol resins. These various resins may be used alone or in combination of two or more.
- an acrylic resin is preferable because it has a high light transmittance in the visible light wavelength region and is excellent in heat resistance, mechanical properties, and molding processability.
- the resin (X) may contain other structural units as long as the performance of the light extraction film 10 is not impaired. Good. Examples of other structural units include polyoxyalkylene glycol di (meth) acrylate units, polyester polyol di (meth) acrylate units, and aromatic ester diol di (meth) acrylate units, but the resin (X) is These structural units may be included alone or in combination of two or more.
- polyoxyalkylene glycol di (meth) acrylate units polyester polyol di (meth) acrylate units and aromatic ester diol di (meth) acrylate units are preferred, and polyoxyalkylene glycol di (meth) acrylate units are preferred. More preferred are alkylene glycol di (meth) acrylate units.
- Content ratio of polyoxyalkylene glycol di (meth) acrylate unit, polyester polyol di (meth) acrylate unit and aromatic ester diol di (meth) acrylate unit in resin (X) The amount is preferably 1 to 70% by mass and more preferably 5 to 50% by mass because the flexibility of the light extraction film 10 is improved.
- the material constituting the light extraction film preferably further includes at least one of an ultraviolet absorber and a light stabilizer.
- an ultraviolet absorber or a light stabilizer By using an ultraviolet absorber or a light stabilizer, it is possible to provide a light extraction film that is not easily discolored by exposure to ultraviolet rays and has excellent long-term stability.
- the content of the ultraviolet absorber in the material constituting the light extraction film is 0.1% by mass. The above is preferable, more preferably 0.5% by mass or more, and further preferably 1% by mass or more.
- the upper limit of the content rate of the ultraviolet absorber in the material which comprises a light extraction film is 20 mass%, and it is more preferable that it is 16 mass%.
- the content of the light stabilizer in the material constituting the light extraction film is 0.1% by mass. The above is preferable, more preferably 0.5% by mass or more, and further preferably 1% by mass or more.
- the upper limit of the content rate of the light stabilizer in the material which comprises a light extraction film is 20 mass%, and it is more preferable that it is 9 mass%.
- UV absorber has a function of absorbing ultraviolet rays, and can absorb the ultraviolet rays incident from the outside such as sunlight to suppress discoloration of the light extraction film 10 when exposed to ultraviolet rays. 10 is excellent in long-term stability.
- Examples of the ultraviolet absorber include 2- (2-hydroxy-5-tert-butylphenyl) -2H-benzotriazole, benzenepropanoic acid-3- (2H-benzotriazol-2-yl) -5- (1,1 -Dimethylethyl) -4-hydroxy 7 to 9 carbon side chain and straight chain alkyl ester, 2- (2H-benzotriazol-2-yl) -4,6-bis (1-methyl-1-phenylethyl) phenol Benzotriazole compounds such as 2- (2H-benzotriazol-2-yl) -6- (1-methyl-1-phenylethyl) -4- (1,1,3,3-tetramethylbutyl) phenol; 2- (4,6-bis (2,4-dimethylphenyl) -1,3,5-triazin-2-yl) -5-hydroxyphenyl and oxirane (for example, (((carbon number The reaction product with 0-16 alkyloxy) methyl) oxiran
- ultraviolet absorbers may be used alone or in combination of two or more.
- benzotriazole compounds and hydroxyphenol triazine compounds are preferable.
- an active energy ray-curable composition described later is used, due to the difference in absorption wavelength.
- a benzotriazole compound is more preferred because the polymerization initiator is efficiently cleaved and has excellent curability.
- the light stabilizer has a function of capturing radicals, and by capturing radicals generated by the incidence of ultraviolet rays such as sunlight, discoloration due to a change in the chemical structure of the light extraction film 10 can be suppressed.
- the take-out film 10 is excellent in long-term stability.
- Examples of the light stabilizer include tetrakis (1,2,2,6,6-pentamethyl-4-piperidinyl) butane-1,2,3,4-tetracarboxylate, tetrakis (2,2,6,6).
- -Tetramethyl-4-piperidinyl) butane-1,2,3,4-tetracarboxylate bis (1,2,2,6,6-pentamethyl-4-piperidyl) ((3,5-bis (1, 1-dimethylethyl) -4-hydroxyphenyl) methyl) butyl malonate, bis (1,2,2,6,6-pentamethyl-4-piperidyl) sebacate, 1,2,2,6,6-pentamethyl-4 -Piperidyl sebacate, bis (2,2,6,6-tetramethyl-1- (octyloxy) -4-piperidyl) ester of decanedioic acid, 1,1-dimethylethyl hydroperoxide Reaction product with o
- These light stabilizers may be used alone or in combination of two or more.
- a hindered amine compound is preferable because of excellent radical scavenging ability, a compound having a nitroxy ether group is more preferable, and bis (2,2,6,6-tetramethyl-decanedioate) is preferable.
- the reaction product of 1- (octyloxy) -4-piperidinyl) ester, 1,1-dimethylethyl hydroperoxide and octane is more preferred.
- the material constituting the light extraction film includes, in addition to the resin (X), the ultraviolet absorber and the light stabilizer, other components as long as the performance of the light extraction film 10 is not impaired. May be included.
- Other components include, for example, light diffusing fine particles, flexibility improvers, viscosity modifiers, plasticizers, fillers, flame retardants, antistatic agents, antioxidants, colorants such as dyes and pigments, release agents, Various additives such as leveling agents, antifouling improvers, dispersion stabilizers and the like can be mentioned.
- the content of the light diffusing fine particles in the material constituting the light extraction film is preferably 20% by mass or less, because the warpage of the light extraction film 10 is suppressed. Is more preferable, and 0% by mass is still more preferable.
- the material constituting the light extraction film is formed of a monomer composition containing the monomer (x) having at least one skeleton of a fluorene skeleton, a biphenyl skeleton, and a naphthalene skeleton. It is preferred that a monomer (x) may be used independently and may be used in combination of 2 or more type.
- the resin (X) is obtained by polymerization of the monomer (x) contained in the monomer composition and a monomer other than the monomer (x) that can be contained as necessary. Can be synthesized.
- the active energy ray-curable monomer composition that can be cured by irradiation with active energy rays Is preferred.
- active energy rays examples include ultraviolet rays, electron beams, X-rays, infrared rays, and visible rays.
- active energy rays examples include ultraviolet rays, electron beams, X-rays, infrared rays, and visible rays.
- ultraviolet rays and electron beams are preferable, and ultraviolet rays are more preferable because the active energy ray-curable monomer composition is excellent in curability and can suppress deterioration of the light extraction film 10.
- the active energy ray-curable monomer composition is not particularly limited as long as it can be cured by active energy rays, but is excellent in handleability and curability and has flexibility, heat resistance, kill resistance, and solvent resistance of the light extraction film 10.
- the active energy ray-curable monomer composition is a monomer other than the monomer (x) and the monomer (x) (crosslinkable monomer) because of excellent physical properties such as light resistance and light transmittance. It preferably contains a monomer (a), a non-crosslinkable monomer (b)) and a polymerization initiator (c), and preferably contains at least one of an ultraviolet absorber and a light stabilizer.
- the monomer having a fluorene skeleton includes a fluorene structure, that is, a structural unit represented by the following formula (1).
- the monomer having a biphenyl skeleton is a structural unit derived from biphenyl, that is, the following formula (2): Is included.
- a monomer having a naphthalene skeleton is a structural unit derived from naphthalene, that is, the following formula (3): Is included.
- the monomer (x) may have one of these skeletons alone or in combination of two or more.
- Monomers (x) include full orange (meth) acrylate, ethylene oxide modified full orange (meth) acrylate, propylene oxide modified full orange (meth) acrylate, 2-hydroxypropylene oxide modified full orange (meth) acrylate, butylene.
- These monomers (x) may be used alone or in combination of two or more.
- the active energy ray-curable monomer composition has excellent handleability and curability
- the light extraction film 10 has heat resistance, kill resistance, solvent resistance, light resistance, and light transmission.
- Fluorene acrylate monomers are preferred because of their excellent physical properties such as surface properties, and excellent light extraction efficiency and normal luminance of surface emitters.
- Bisphenol full orange (meth) acrylates, bisnaphthol full orange (meth) acrylate are more preferred.
- (meth) acrylate refers to acrylate or methacrylate.
- the productivity of the light extraction film is excellent, the light extraction efficiency and the normal luminance of the surface light emitter are further improved, and the emission angle dependency of the emission light wavelength of the surface light emitter is further increased.
- the monomer represented by following formula (5) is preferable. (Wherein R 1 and R 2 are each independently a hydrogen atom or a methyl group, and a and b are each independently an integer of 0 to 4)
- crosslinkable monomer (a) examples include hexa (meth) acrylates such as dipentaerythritol hexa (meth) acrylate and caprolactone-modified dipentaerythritol hexa (meth) acrylate; dipentaerythritol hydroxypenta (meth) acrylate , Penta (meth) acrylates such as caprolactone-modified dipentaerythritol hydroxypenta (meth) acrylate; ditrimethylolpropane tetra (meth) acrylate, pentaerythritol tetra (meth) acrylate, pentaerythritol ethoxy modified tetra (meth) acrylate, dipenta Tests such as erythrole hexa (meth) acrylate, dipentaerystol penta (meth) acrylate, tetramethylolmethan
- polyhydric alcohols ethylene glycol, hexanediol, polyethylene glycol, polytetramethylene glycol, etc.
- polyester di (meth) acrylates such as compounds obtained by reaction with (meth) acrylic acid or derivatives thereof; diisocyanate compounds (Tolylene diisocyanate, isophorone diisocyanate, xylene diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, etc.) and hydroxyl group-containing (meth) acrylate (Multifunctional (meth) acrylates such as 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, pentaerythritol tri (meth) acrylate), etc.)
- a diisocyanate compound is added to the hydroxyl group of a compound or alcohol (one or more of alkane diol, poly
- Urethane polyfunctional (meth) acrylates such as conjugated compounds; divinyl ethers such as diethylene glycol divinyl ether and triethylene glycol divinyl ether; dienes such as butadiene, isoprene and dimethylbutadiene It is below.
- These crosslinkable monomers (a) may be used individually by 1 type, and may use 2 or more types together.
- the light extraction film 10 is excellent in various properties such as flexibility, heat resistance, killing resistance, solvent resistance, and light transmittance.
- the crosslinkable monomer (a) excludes the monomer (x).
- non-crosslinkable monomer (b) examples include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, iso-propyl (meth) acrylate, n-butyl (meth) acrylate, iso-butyl (meth) acrylate, sec-butyl (meth) acrylate, tert-butyl (meth) acrylate, n-hexyl (meth) acrylate, cyclohexyl (meth) acrylate, n-octyl (meth) acrylate, 2-ethylhexyl ( (Meth) acrylate, dodecyl (meth) acrylate, tridecyl (meth) acrylate, stearyl (meth) acrylate, alkyl (meth) acrylate, phenyl (meth) acrylate, benzyl (meth) acryl
- non-crosslinkable monomers (b) may be used individually by 1 type, and may use 2 or more types together.
- the handleability and curability of the active energy ray-curable monomer composition are excellent, and the flexibility, heat resistance, kill resistance, and solvent resistance of the light extraction film 10 are improved.
- (Meth) acrylates, epoxy (meth) acrylates, aromatic vinyls, and olefins are preferable, and (meth) acrylates and epoxy (meth) acrylates are preferable. More preferred.
- the non-crosslinkable monomer (b) excludes the monomer (x) and the crosslinkable monomer (a).
- polymerization initiator (c) examples include benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin isobutyl ether, acetoin, benzyl, benzophenone, p-methoxybenzophenone, 2,2-diethoxyacetophenone, ⁇ , ⁇ -Dimethoxy- ⁇ -phenylacetophenone, benzyldimethyl ketal, methylphenylglyoxylate, ethylphenylglyoxylate, 4,4′-bis (dimethylamino) benzophenone, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2- Carbonyl compounds such as methyl-1-phenylpropan-1-one and 2-ethylanthraquinone; tetramethylthiuram monosulfide, tetramethylthiuram disulfide, etc.
- Sulfur compounds 2,4,6-trimethylbenzoyl diphenylphosphine oxide, acylphosphine oxide such as benzo dichloride ethoxy phosphine oxide, and the like.
- These polymerization initiators (c) may be used alone or in combination of two or more.
- carbonyl compounds and acylphosphine oxides are preferable because they are excellent in handleability and curability of the active energy ray-curable monomer composition and light transmittance of the light extraction film 10.
- the benzotriazole-based compound absorbs light of 400 nm or less, and the active energy ray-curable monomer composition can be efficiently cured with light of 400 nm or more. Since it can do, acylphosphine oxides are more preferable.
- the active energy ray-curable monomer composition includes monomers (x) and monomers other than monomer (x) (crosslinkable monomer (a) and non-crosslinkable monomer (b)).
- monomers (x) and monomers other than monomer (x) crosslinkable monomer (a) and non-crosslinkable monomer (b)
- other components may be included as long as the performance of the light extraction film 10 is not impaired.
- Other components include, for example, light diffusing fine particles, flexibility improvers, viscosity modifiers, plasticizers, fillers, flame retardants, antistatic agents, antioxidants, colorants such as dyes and pigments, release agents, Various additives such as leveling agents, antifouling improvers, dispersion stabilizers and the like can be mentioned.
- the content of the monomer (x) in the active energy ray-curable monomer composition is preferably 20 to 93% by mass, more preferably 25 to 89% by mass, and more preferably 30 to 90% by mass in the total amount of the monomer composition. 86 mass% is still more preferable.
- the content of the monomer (x) is 20% by mass or more, the light extraction efficiency and normal luminance of the surface light emitter are excellent. Further, when the content of the monomer (x) is 30% by mass or more, the light extraction efficiency and the normal luminance of the surface light emitter are further improved.
- the handleability of an active energy ray hardening composition is excellent in the content rate of a monomer (x) being 93 mass% or less.
- the content of the crosslinkable monomer (a) in the active energy ray-curable monomer composition is preferably 5 to 60% by mass, more preferably 8 to 55% by mass, based on the total amount of the monomer composition. More preferably, it is 10 to 50% by mass.
- the content of the crosslinkable monomer (a) is 5% by mass or more, the crosslinkability of the monomer composition is excellent and the flexibility of the light extraction film 10 is excellent.
- the content of the non-crosslinkable monomer (b) in the active energy ray-curable monomer composition is preferably 1 to 60% by mass and more preferably 2 to 55% by mass in the total amount of the monomer composition. 3 to 50% by mass is more preferable.
- the content of the non-crosslinkable monomer (b) is 1% by mass or more, the handleability of the monomer composition is excellent.
- the content of the non-crosslinkable monomer (b) is 60% by mass or less, the monomer composition is excellent in crosslinkability and curability and the light extraction film 10 is excellent in solvent resistance.
- the content of the polymerization initiator (c) in the active energy ray-curable monomer composition is preferably 0.1 to 10% by mass, more preferably 0.5 to 8% by mass in the total amount of the monomer composition. It is preferably 1 to 5% by mass.
- the content of the polymerization initiator (c) is 0.1% by mass or more, the handleability and curability of the monomer composition are excellent.
- the content of the ultraviolet absorber in the active energy ray-curable monomer composition is preferably from 0.1 to 20% by mass, more preferably from 0.3 to 15% by mass, based on the total amount of the monomer composition. More preferably, the content is 5 to 10% by mass.
- the content of the ultraviolet absorber is 0.1% by mass or more, discoloration of the light extraction film 10 upon exposure to ultraviolet rays can be suppressed, and the long-term stability is excellent.
- the content of the light stabilizer in the active energy ray-curable monomer composition is preferably 0.1 to 9% by mass, more preferably 0.3% to 7% by mass, based on the total amount of the monomer composition. 0.5 to 5% by mass is more preferable.
- the content of the light stabilizer is 0.1% by mass or more, discoloration of the light extraction film 10 due to exposure to ultraviolet light can be suppressed, and long-term stability is excellent.
- the refractive index of the light extraction film is excellent in the light transmittance of the light extraction film 10, and is excellent in the light extraction efficiency and normal luminance of the surface light emitter. It is preferable that In addition, let a refractive index be the value measured using the sodium D line
- the ratio (A1 / A2) of the peak area derived from the aromatic (A1) to the peak area (A2) derived from a part other than the aromatic measured by 13 C-NMR of the light extraction film is: It is preferably 0.1 or more, more preferably 0.3 to 3.0.
- the peak area ratio A1 / A2 is 0.1 or more, the monomer (x) unit content is high, the light extraction efficiency and normal brightness of the surface light emitter are sufficiently improved, and the light emitted from the surface light emitter. Sufficient suppression of the emission angle dependence of the wavelength can be achieved.
- the peak area (A1) derived from the carbon of the portion showing the aromaticity of the light extraction film and the peak area (A2) derived from the carbon of the portion other than the portion showing the aromaticity of the light extraction film are solid 13 It can be determined using C-NMR.
- the peak located in the range of 115 to 160 ppm of the chemical shift of carbon is defined as a peak derived from carbon at a portion exhibiting aromaticity, and the peak at other positions is other than the portion exhibiting aromaticity. This peak was derived from the carbon of the part.
- the light extraction film 10 is not particularly limited as long as light from the EL element can be extracted efficiently, but is excellent in the structural stability of the light extraction film 10 and excellent in the light extraction efficiency and normal luminance of the surface light emitter. It is preferable to have the uneven structure layer 11 and the base layer 12.
- the light extraction film 10 achieves sufficient improvement of the light extraction efficiency and normal luminance of the surface light emitter, and sufficient suppression of the emission angle dependence of the emission light wavelength, and further the discoloration of the light extraction film 10 when exposed to ultraviolet rays. Since long-term stability can be improved by suppressing the above, it is preferable that the material constituting the light extraction film is formed of the above-described monomer composition.
- the concavo-convex structure layer 11 and the base layer 12 may have the same or different resin composition. However, since the productivity of the light extraction film 10 is excellent, the resin composition is preferably the same.
- the uneven structure layer 11 has an uneven structure 13. Thereby, it has a role which improves the light extraction efficiency and normal line brightness
- the concavo-convex structure 13 may be a protrusion or a depression, but a protrusion is preferable because the productivity of the light extraction film 10 is excellent.
- a spherical notch shape, a spherical notch shape, an ellipsoidal spherical shape (a shape obtained by cutting a spheroid on one plane), an ellipsoidal spherical notch shape (a spheroid is mutually connected) Shape cut by two parallel planes), pyramid shape, truncated pyramid shape, cone shape, truncated cone shape, and related roof shape (spherical shape, spherical truncated shape, ellipsoidal spherical shape, elliptical shape) And a truncated cone shape, a pyramid shape, a truncated pyramid shape, a cone shape, or a shape in which a truncated cone shape extends along the bottom surface portion).
- These concavo-convex structures 13 may be used singly or in combination of two or more.
- the surface light emitter is excellent in light extraction efficiency and normal luminance, so that it has a spherical notch shape, a spherical notch shape, an ellipsoidal spherical notch shape, an ellipsoidal spherical notch shape, and a pyramid shape.
- a truncated pyramid shape is preferable, a spherical notch shape, an ellipsoidal spherical shape, and a pyramidal shape are more preferable.
- FIG. 2A An arrangement example of the uneven structure 13 is shown in FIG.
- FIG. 2B An arrangement example of the concavo-convex structure 13 is shown in FIG.
- FIG. 2A a hexagonal arrangement
- FIG. 2B a rectangular arrangement
- FIG. 2C a rhombic arrangement
- FIG. 2D a linear arrangement
- FIG. 2E Circular arrangement
- FIG. 2F random arrangement
- a hexagonal arrangement, a rectangular arrangement, and a rhombus arrangement are preferable, and a hexagonal arrangement and a rectangular arrangement are more preferable because of excellent light extraction efficiency and normal luminance of the surface light emitter.
- the bottom surface portion 15 of the concavo-convex structure 13 refers to a virtual planar portion surrounded by the outer peripheral edge of the bottom portion of the concavo-convex structure 13 (the contact surface with the base layer 12 when the base layer 12 is provided).
- the longest diameter L of the bottom surface portion 15 of the concavo-convex structure 13 means the length of the longest portion of the bottom surface portion 15 of the concavo-convex structure 13, and the average longest diameter L of the bottom surface portion 15 of the concavo-convex structure 13.
- the surface of the light extraction film 10 having the concavo-convex structure 13 was photographed with a scanning microscope, the longest diameter L of the bottom surface portion 15 of the concavo-convex structure 13 was measured at five locations, and the average value was obtained.
- the height H of the concavo-convex structure 13 means the height from the bottom surface portion 15 of the concavo-convex structure 13 to the highest portion in the case of the protrusion structure, and the bottom surface of the concavo-convex structure 13 in the case of the recess structure.
- the average height H ave of the concavo-convex structure 13 is measured with a scanning microscope, and the height H of the concavo-convex structure 13 is measured at five locations. The average value was used.
- the average longest diameter L ave of the bottom surface portion 15 of the concavo-convex structure 13 is preferably 0.5 to 150 ⁇ m, more preferably 1 to 130 ⁇ m, and more preferably 2 to 2 to further improve the light extraction efficiency and normal luminance of the surface light emitter. More preferably, it is 100 ⁇ m.
- the average height H ave of the concavo-convex structure 13 is preferably 0.25 to 75 ⁇ m, more preferably 0.5 to 65 ⁇ m, and more preferably 1 to 50 ⁇ m in order to further improve the light extraction efficiency and normal luminance of the surface light emitter. Further preferred.
- the aspect ratio of the concavo-convex structure 13 is preferably 0.3 to 1.4, more preferably 0.35 to 1.3, in order to further improve the light extraction efficiency and normal luminance of the surface light emitter. Is more preferably 1.0.
- the aspect ratio of the concavo-convex structure 13 was calculated from the average height H ave of the concavo-convex structure 13 / average longest diameter L ave of the bottom surface portion 15 of the concavo-convex structure 13.
- Examples of the shape of the bottom surface portion 15 of the concavo-convex structure 13 include a polygon such as a triangle and a quadrangle; a circle such as a true circle and an ellipse; and an indefinite shape.
- a polygonal shape and a circular shape are preferable, and a circular shape is more preferable because the light extraction efficiency and normal luminance of the surface light emitter are further improved.
- the ratio of the area of the bottom surface 15 of the concavo-convex structure 13 (the area surrounded by the dotted line in FIG. 4) to the area of the light extraction film 10 (the area surrounded by the solid line in FIG. 4) is the light extraction of the surface light emitter.
- 20 to 99% is preferable, 25 to 95% is more preferable, 30 to 93% is still more preferable, and 70 to 90% is still more preferable.
- the ratio of the area of the bottom surface portion 15 of the concavo-convex structure 13 to the area of the light extraction film 10 is referred to as “occupation ratio of the concavo-convex structure”.
- the maximum value of the ratio of the area of the bottom face part 15 of the concavo-convex structure 13 to the area of the light extraction film 10 is about 91%.
- the base layer 12 Since the uneven structure 13 of the uneven structure layer 11 is supported, the base layer 12 is preferably provided.
- the base layer 12 has a role of relaxing the stress accompanying polymerization shrinkage and the like at the time of curing of the monomer composition and maintaining the shape of the concavo-convex structure 13.
- the thickness of the base layer 12 is preferably 3 to 60 ⁇ m, more preferably 5 to 50 ⁇ m, and even more preferably 10 to 40 ⁇ m because of excellent flexibility of the light extraction film 10 and excellent adhesion to the base material 14 described later.
- the thickness of the base layer 12 is 3 ⁇ m or more, suppression of the emission angle dependency of the emission light wavelength of the surface light emitter is further improved.
- the thickness of the base layer 12 is 60 ⁇ m or less, the light extraction efficiency and normal luminance of the surface light emitter are further improved.
- the light extraction film of the present invention forms a surface light emitter in combination with an EL element.
- the surface without the uneven structure 13 of the light extraction film 10 In other words, the base material 14 may be provided between the light extraction film 10 and the EL element.
- the base material 14 is on the surface (the lower surface in FIG. 1) opposite to the surface (the upper surface in FIG. 1) of the base layer 12 to which the uneven structure layer 11 is attached. Attached.
- the substrate 14 is preferably a substrate that transmits active energy rays because the active energy ray-curable monomer composition is excellent in curability.
- the refractive index of the substrate 14 is preferably 1.55 to 1.65.
- Examples of the material of the substrate 14 include acrylic resin; polycarbonate resin; polyester resin such as polyethylene terephthalate, polybutylene terephthalate, and polyethylene naphthalate; styrene resin such as polystyrene and ABS resin; vinyl chloride resin; diacetyl cellulose, triacetyl cellulose.
- Cellulose resins such as: Imide resins such as polyimide and polyimideamide; Glass; Metals.
- acrylic resin, polycarbonate resin, polyester resin, styrene resin, cellulose resin, and imide resin are preferable because of excellent flexibility and active energy ray permeability, and acrylic resin and polycarbonate resin. Resins, polyester resins, and imide resins are more preferable, and polyester resins are more preferable.
- the thickness of the base material 14 is preferably 10 to 1000 ⁇ m, more preferably 20 to 500 ⁇ m, since it is excellent in the handleability of the light extraction film 10 and excellent in the curability of the active energy ray-curable monomer composition. More preferably, it is in the range of 300 ⁇ m.
- the base material 14 may perform an easily bonding process on the surface of the base material 14 as needed.
- the easy-adhesion treatment method include a method of forming an easy-adhesion layer made of a polyester resin, an acrylic resin, a urethane resin or the like on the surface of the base material 14, a method of roughening the surface of the base material 14, and the like. It is done.
- the base material 14 may be subjected to a surface treatment such as antistatic, antireflection, and adhesion prevention between the substrates, if necessary, in addition to the easy adhesion treatment.
- the light extraction film of the present invention is excellent in ease of attachment to an EL element and handleability of the light extraction film, for example, as shown in FIG. 1, the surface of the substrate 14 on which the light extraction film 10 is formed.
- the adhesive layer 21 and the protective film 22 may be sequentially laminated on the opposite surface (lower surface).
- an adhesive layer 21 Since the light extraction film of the present invention adheres to the EL element 30 on the light incident surface side, an adhesive layer 21 may be provided as shown in FIG. When the base material 14 is attached to the light extraction film 10, an adhesive layer 21 may be provided on the surface of the base material 14 as shown in FIG. 1. Examples of the adhesive layer 21 include known adhesives.
- the refractive index of the adhesive layer 21 is preferably 1.48 to 1.58.
- a protective film 22 may be provided on the surface of the adhesive layer 21 as shown in FIG.
- the protective film 22 may be peeled off from the light extraction film 10 or the like when the light extraction film 10 or the like is pasted on the surface of the EL element 30.
- Examples of the protective film 22 include known protective films.
- the method for producing a light extraction film of the present invention is a method for producing a light extraction film laminated on a substrate of an EL element, and includes a fluorene skeleton and a biphenyl skeleton between a substrate and a mold having a concavo-convex structure transfer portion. And a monomer composition containing a monomer (x) having at least one skeleton of a naphthalene skeleton is supplied, and the monomer composition is cured.
- the content of the monomer (x) is preferably 30% by mass or more, and more preferably 30 to 86% by mass.
- the monomer composition is cured to cause polymerization of the monomer (x) with a monomer other than the monomer (x) that can be included as necessary, thereby synthesizing the resin (X). be able to.
- Examples of the method for producing the light extraction film 10 include a method using an apparatus 50 as shown in FIG.
- the manufacturing method of the light extraction film 10 using the apparatus 50 shown in FIG. 5 is demonstrated, it is not limited to the manufacturing method using the apparatus 50 shown in FIG.
- a monomer composition 51 for forming a material constituting the light extraction film 10 is prepared by a conventional method, and the monomer composition 51 is placed in a storage tank 55 in advance.
- the monomer composition 51 here is an active energy ray-curable monomer composition.
- the substrate 14 is introduced between a cylindrical roll mold 52 having a concavo-convex structure transfer portion and a rubber nip roll 53.
- the monomer composition 51 is supplied between the rotating roll mold 52 and the base material 14 through a pipe 56 having a nozzle attached to the tip from the tank 55.
- the monomer composition 51 sandwiched between the rotating roll mold 52 and the base material 14 is cured by active energy rays in the vicinity of the active energy ray irradiation device 54.
- the light extraction film 10 with the base material 14 is obtained.
- the viscosity of the monomer composition 51 is preferably from 10 to 3000 mPa ⁇ s, more preferably from 20 to 2500 mPa ⁇ s, and even more preferably from 30 to 2000 mPa ⁇ s, since it is excellent in handleability during production of the light extraction film 10. .
- Examples of the roll mold 52 include molds such as aluminum, brass, and steel; resin molds such as silicone resin, urethane resin, epoxy resin, ABS resin, fluororesin, and polymethylpentene resin; molds obtained by plating the resin; Examples include a mold made of a material obtained by mixing various metal powders with a resin.
- a mold is preferable because of excellent heat resistance and mechanical strength and suitable for continuous production.
- the mold is preferable in many respects such as being resistant to polymerization heat generation, hardly deforming, hardly scratched, temperature controllable, and suitable for precision molding.
- a transfer surface having protrusions or depressions for forming the uneven structure 13 of the light extraction film 10 that is, a transfer portion having an uneven structure.
- the method for producing the transfer surface include cutting with a diamond tool, etching as described in International Publication No. 2008/069324, and the like. Among these methods for producing a transfer surface, etching as described in International Publication No. 2008/069324 is preferable because it is easy to form a curved protrusion or depression.
- a metal thin film produced by using an electroforming method is wound around a roll core member from a master mold having a depression or a projection obtained by inverting a projection or a depression on the transfer surface, and is cylindrical.
- the method of manufacturing the roll mold 52 can be used.
- heat source equipment such as a sheathed heater or a hot water jacket may be provided inside or outside the roll mold 52 as necessary.
- Examples of the active energy rays generated by the active energy ray irradiation device 54 include ultraviolet rays, electron beams, X-rays, infrared rays, and visible rays. Among these active energy rays, ultraviolet rays and electron beams are preferable, and ultraviolet rays are more preferable because the active energy ray-curable monomer composition is excellent in curability and can suppress deterioration of the light extraction film 10.
- Examples of the active energy ray light source of the active energy ray irradiation device 54 include a chemical lamp, a low-pressure mercury lamp, a high-pressure mercury lamp, a metal halide lamp, an electrodeless ultraviolet lamp, a visible light halogen lamp, and a xenon lamp.
- the integrated light amount of the active energy ray of the active energy ray irradiation device 54 is not particularly limited, but it is excellent in curability of the active energy ray curable composition and suppresses deterioration of the light extraction film 10. Therefore, 0.01 to 10 J / Cm 2 is preferable, and 0.5 to 8 J / cm 2 is more preferable.
- heat source equipment such as a sheathed heater or a hot water jacket may be provided as necessary.
- the surface light emitter of the present invention includes the light extraction film of the present invention and an EL element, and has a substrate (preferably a polyester resin substrate) or an adhesive layer between the light extraction film and the EL element. Is preferred.
- Examples of the surface light emitter of the present invention include a surface light emitter as shown in FIG. Hereinafter, the surface light emitter of FIG. 6 will be described, but the surface light emitter of the present invention is not limited to the surface light emitter of FIG.
- the surface light emitter shown in FIG. 6 has a glass substrate 31, an anode 32, a light emitting layer 33, and a cathode 34 sequentially laminated on the surface of the glass substrate 31 of the EL element 30 via the adhesive layer 21 and the base material 14.
- a light extraction film 10 is provided.
- the substrate of the EL element preferably has a refractive index of 1.45 to 1.55.
- the surface light emitter in which the light extraction film 10 is provided on the EL element 30 is excellent in light extraction efficiency and normal luminance, and can suppress the emission angle dependency of the emission light wavelength.
- the surface light emitter of the present invention preferably has a chromaticity change amount of 0.03 or less, and more preferably 0.01 or less.
- the lower limit of the chromaticity change amount in the surface light emitter of the present invention is about 0.0001.
- the chromaticity change amount is a change amount of chromaticity of the xy color system measured by a luminance meter. If the chromaticity change amount is 0.01 or less, the emission wavelength of the surface light emitter is not changed. The emission angle dependency can be sufficiently suppressed.
- the 13 C-NMR peak area ratio of the light extraction film was measured by solid 13 C-NMR.
- the resin (X) was finely cut and placed in a sample tube having an inner diameter of 2.5 mm.
- measurement was performed by the DD-MAS method at 90 °, a pulse width of 3 ⁇ s, a sample rotation number of 16 kHz, an integration number of 4096 times, and a repetition waiting time of 60 seconds.
- the peak area (A1) derived from aromatics located in the range of 115 to 160 ppm of chemical shift of carbon and the peak area (A2) derived from parts other than aromatics in other ranges are obtained.
- the peak area ratio (A1 / A2) was calculated.
- chromium plating was applied to obtain a roll mold.
- a mold having a transfer portion in which hemispherical depressions having a diameter of 30 ⁇ m and a depth of 18 ⁇ m are arranged in a hexagonal array at a minimum interval of 2 ⁇ m on a copper plating layer was obtained by the same method.
- Example 1 The active energy ray-curable monomer composition A was applied to the roll type obtained in Production Example 10, and a polyethylene terephthalate base material having a thickness of 125 ⁇ m (trade name “Diafoil T910E125”, Mitsubishi Plastics Corporation) ), Refractive index: 1.60), and the active energy ray-curable monomer composition A was uniformly extended with a nip roll so that the thickness of the base layer was 20 ⁇ m. Then, the active energy ray-curable monomer composition A sandwiched between the roll mold and the base material is cured by irradiating ultraviolet rays from above the base material, and the resulting cured product-base material bonded body is obtained.
- a polyethylene terephthalate base material having a thickness of 125 ⁇ m (trade name “Diafoil T910E125”, Mitsubishi Plastics Corporation) ), Refractive index: 1.60)
- the active energy ray-curable monomer composition A was uniformly extended with a nip roll
- the refractive index of the cured active energy ray-curable monomer composition A was 1.61.
- the size of the concavo-convex structure of the light extraction film calculated from the image of the obtained light extraction film taken with a scanning microscope is such that the average longest diameter L ave is 48.2 ⁇ m and the average height H ave is 26.0 ⁇ m.
- a concavo-convex structure composed of a sphere-shaped projection substantially corresponding to the size of the roll-shaped depression was obtained.
- the uneven structure of the obtained light extraction film is arranged in a hexagonal array with a minimum interval of 3 ⁇ m corresponding to the roll type, and the area of the light extraction film is The ratio of the total area of the bottom surface of the concavo-convex structure (occupation ratio of the concavo-convex structure) was 76%.
- Cargill standard refraction liquid (refractive index 1.52, manufactured by Moritex Co., Ltd.) was applied to the light emitting surface of the EL element A as an adhesive layer.
- the surface of the base material attached to the light extraction film was optically adhered to the adhesive layer to obtain a surface light emitter.
- Table 1 The measurement results of light extraction efficiency, normal luminance, and chromaticity change amount of the obtained surface light emitter are shown in Table 1 together with the refractive index of the cured active energy ray-curable monomer composition.
- Example 2 to 12 Comparative Example 1
- the active energy ray-curable monomer composition used in the production of the light extraction film is changed to the one described in the “Composition” column of Table 1, and the roll-shaped transfer part is described in the “Uneven structure” column of Table 1.
- a surface light emitter was obtained in the same manner as in Example 1 except that the surface light emitter was changed.
- Example 9 a mold provided with a transfer portion having a minimum interval between hemispherical depressions of 1 ⁇ m was used.
- Example 10 a mold provided with a transfer portion having a minimum interval between hemispherical depressions of 2 ⁇ m was used.
- the measurement results of light extraction efficiency, normal luminance, and chromaticity change amount of the obtained surface light emitter are shown in Table 1 together with the refractive index of the cured active energy ray-curable monomer composition.
- An active energy ray-curable monomer composition C was applied on a 125 ⁇ m thick polyethylene terephthalate substrate (trade name “Diafoil T910E125”, manufactured by Mitsubishi Plastics, Inc., refractive index: 1.60)
- a polyethylene terephthalate substrate (trade name “Diafoil T910E125”, manufactured by Mitsubishi Plastics, Inc., refractive index: 1.60) is placed on the substrate, and active energy ray curing is performed so that the base layer has a thickness of 20 ⁇ m.
- the polymerizable monomer composition C was uniformly stretched with a nip roll.
- the ultraviolet ray is irradiated from above the base material, the active energy ray-curable monomer composition C sandwiched between the base materials is cured, one base material is peeled from the obtained cured product, and the other base material is peeled off.
- a light extraction film with a substrate was obtained.
- a Cargill standard refraction liquid (refractive index 1.52, manufactured by Moritex Co., Ltd.) was applied to the light emitting surface of the EL element A as an adhesive layer.
- the surface of the base material attached to the light extraction film was optically adhered to the adhesive layer to obtain a surface light emitter.
- Table 1 The measurement results of light extraction efficiency, normal luminance, and chromaticity change amount of the obtained surface light emitter are shown in Table 1 together with the refractive index of the cured active energy ray-curable monomer composition.
- the surface light emitters obtained in Examples 1 to 12 including the light extraction film of the present invention were excellent in light extraction efficiency and normal luminance, and excellent in suppressing the emission angle dependency of the emission light wavelength.
- the surface light-emitting body obtained in Comparative Example 1 using the light extraction film manufactured using the monomer composition not containing the monomer (x) is sufficiently improved in light extraction efficiency and normal luminance. It was not.
- the surface light-emitting body obtained in Comparative Example 2 did not have an uneven structure on the surface of the light extraction film, the light extraction efficiency and the normal luminance were not sufficiently improved.
- Example 13 (Production of active energy ray-curable monomer composition J) 40 parts of full orange acrylate represented by the following formula (12) (trade name “EA-0100”, manufactured by Osaka Gas Chemical Co., Ltd.), dimethacrylate represented by the following formula (8) (trade name “Acryester PBOM2000”) ”, 10 parts by Mitsubishi Rayon Co., Ltd., 20 parts by dimethacrylate (trade name“ ABE-300 ”, manufactured by Shin-Nakamura Chemical Co., Ltd.) represented by the following formula (9), 30 parts of the acrylate (trade name “New Frontier PHE”, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) and 1 part of a polymerization initiator (trade name “Lucirin TPO”, manufactured by BASF) are mixed to prepare a pre-monomer A composition was obtained.
- formula (12) trade name “EA-0100”, manufactured by Osaka Gas Chemical Co., Ltd.
- dimethacrylate represented by the following formula (8) (
- the cured product of the obtained pre-monomer composition had a refractive index of 1.58, and the peak derived from the non-aromatic portion of the aromatic-derived peak area (A1) measured by 13 C-NMR.
- the ratio (A1 / A2) to area (A2) is 0.70.
- the obtained active energy ray-curable monomer composition J is applied to the obtained roll mold, and a polyethylene terephthalate base material having a thickness of 125 ⁇ m (trade name “Diafoil T910E125”, Mitsubishi Plastics Co., Ltd.) Made, refractive index: 1.60), and uniformly stretched with a nip roll. Then, the active energy ray-curable monomer composition J sandwiched between the roll mold and the substrate is cured by irradiating ultraviolet rays from above the substrate, and the cured product of the monomer composition J is peeled from the roll mold. Thus, a light extraction film with a substrate was obtained.
- the thickness of the base layer can be controlled by controlling the pressing of the roll mold.
- the thickness of the base layer was set to 30 ⁇ m.
- the size of the concavo-convex structure of the light extraction film calculated from an image taken with a scanning microscope of the obtained light extraction film is such that the average longest diameter L ave is 48.0 ⁇ m and the average height H ave is 27.1 ⁇ m.
- a spherically-shaped protrusion substantially corresponding to the size of the roll-shaped depression was obtained.
- the uneven structure of the light extraction film obtained from an image taken with a scanning microscope corresponds to a roll type and is arranged in a hexagonal array with a minimum interval of 10 ⁇ m, and the area of the bottom surface of the spherical protrusion relative to the area of the light extraction film
- the ratio (occupancy ratio of the concavo-convex structure) was 73%.
- Cargill standard refraction liquid (refractive index 1.52, manufactured by Moritex Co., Ltd.) is applied as an adhesive layer to the light emitting surface side of the EL element, and the surface of the substrate attached to the obtained light extraction film is optically applied. Adhering to each other, a surface light emitter was obtained. Table 2 shows the light extraction efficiency, normal luminance, and chromaticity change amount of the obtained surface light emitter.
- the EL element an EL element from which the light extraction film on the light emitting surface side of Symfos OLED-010K (manufactured by Konica Minolta, white OLED element) was peeled off was used.
- Example 14 to 18 Except having changed the content rate of a ultraviolet absorber and the content rate of a light stabilizer as shown in Table 2, it operated similarly to Example 13 and obtained the light extraction film and the surface light-emitting body. Table 2 shows the evaluation results of the obtained surface light emitter.
- a hindered amine compound (trade name “Tinuvin 123”, manufactured by BASF) was used.
- Example 2 The EL element used in Example 13, that is, the EL element from which the light extraction film on the light emitting surface side of Symfos OLED-010K (manufactured by Konica Minolta, Inc., white OLED element) was peeled off, was used as a surface light emitter. Note that the refractive index of the glass substrate of the EL element is 1.50.
- the surface light emitters obtained in Examples 13 to 18 were improved in light extraction efficiency and normal luminance, and the emission angle dependency of the emission light wavelength could be suppressed. In addition, it was found that the surface light emitters obtained in Examples 13 to 18 can suppress changes in optical characteristics before and after ultraviolet irradiation (before and after the accelerated deterioration test) and are excellent in long-term stability.
- the light extraction film of the present invention it is possible to obtain a surface light emitter excellent in light extraction efficiency and normal luminance, and excellent in suppressing the emission angle dependency of the emitted light wavelength. It can be suitably used for a screen or the like.
- the light extraction film of the present invention can sufficiently improve the light extraction efficiency and normal luminance of the surface light emitter and can depend on the emission angle of the emitted light wavelength by using at least one of an ultraviolet absorber and a light stabilizer.
- the surface light emitter using the light extraction film of the present invention is preferably used for, for example, illumination, display, screen, etc. be able to.
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Abstract
Description
光取り出しフィルムは、表面に凹凸構造を有し、
光取り出しフィルムを構成する材料は、フルオレン骨格、ビフェニル骨格及びナフタレン骨格の少なくとも1種の骨格を有する樹脂(X)を含むことを特徴とする。
基材と凹凸構造の転写部を有する型との間に、フルオレン骨格、ビフェニル骨格及びナフタレン骨格の少なくとも1種の骨格を有する単量体(x)を含む単量体組成物を供給し、単量体組成物を硬化させることを特徴とする。
本発明の光取り出しフィルムは、EL素子の基板上に積層する光取り出しフィルムであって、例えば、図1に示すような光取り出しフィルム10が挙げられる。光取り出しフィルム10は、発光源としてのEL素子(具体的には有機EL素子)と組み合わせられることで、当該EL素子からの光取り出しの機能を発揮する。
光取り出しフィルム10は、表面に凹凸構造13を有する。光取り出しフィルム10は、連続的な生産を容易にでき、光取り出しフィルム10の構造安定性(具体的には凹凸構造13の形状の維持)や取り扱い性に優れることから、基材14の一方の表面(上面)に、ベース層12及び凹凸構造13を有する凹凸構造層11を順次積層し、ベース層12と凹凸構造層11とを有する光取り出しフィルム10が形成されるのが好ましい。
樹脂(X)は、フルオレン骨格、ビフェニル骨格及びナフタレン骨格の少なくとも1種の骨格を有するものであるが、ここで、樹脂(X)がフルオレン骨格を有する場合、フルオレン骨格を有する樹脂は、フルオレン構造、即ち、下記式(1)で表される構成単位を含む。
なお、光透過率は、JIS K7361に準拠して測定した値とする。
で表される構成単位を含む。
一方、樹脂(X)がナフタレン骨格を有する場合、ナフタレン骨格を有する樹脂は、ナフタレンに由来する構造単位、即ち下記式(3)
で表される構成単位を含む。
なお、樹脂(X)は、これら骨格の1種を単独で有してもよいし、2種以上を組み合わせて有してもよい。
(式中、R1及びR2は、それぞれ独立して水素原子又はメチル基であり、a及びbは、それぞれ独立して0~4の整数である。)
他の構成単位としては、例えば、ポリオキシアルキレングリコールジ(メタ)アクリレート単位、ポリエステルポリオールジ(メタ)アクリレート単位及び芳香族エステルジオールジ(メタ)アクリレート単位等が挙げられるが、樹脂(X)は、これら構成単位の1種を単独で又は2種以上を組み合わせて含むことができる。
なお、光取り出しフィルム10の柔軟性を向上させる観点から、ポリオキシアルキレングリコールジ(メタ)アクリレート単位、ポリエステルポリオールジ(メタ)アクリレート単位及び芳香族エステルジオールジ(メタ)アクリレート単位が好ましく、ポリオキシアルキレングリコールジ(メタ)アクリレート単位がより好ましい。
樹脂(X)中のポリオキシアルキレングリコールジ(メタ)アクリレート単位、ポリエステルポリオールジ(メタ)アクリレート単位及び芳香族エステルジオールジ(メタ)アクリレート単位の含有率(複数の単位を含む場合はその合計含有量)は、光取り出しフィルム10の柔軟性が向上することから、1~70質量%が好ましく、5~50質量%がより好ましい。
ここで、本発明の光取り出しフィルムにおいては、紫外線暴露での変色を抑制でき長期安定性に優れることから、光取り出しフィルムを構成する材料中の紫外線吸収剤の含有率が、0.1質量%以上が好ましく、0.5質量%以上であることが更に好ましく、1質量%以上であることが一層好ましい。なお、光取り出しフィルムを構成する材料中の紫外線吸収剤の含有率の上限は20質量%であることが好ましく、16質量%であることがより好ましい。
また、本発明の光取り出しフィルムにおいては、紫外線暴露での変色を抑制でき長期安定性に優れることから、光取り出しフィルムを構成する材料中の光安定化剤の含有率が、0.1質量%以上が好ましく、0.5質量%以上であることが更に好ましく、1質量%以上であることが一層好ましい。なお、光取り出しフィルムを構成する材料中の光安定化剤の含有率の上限は20質量%であることが好ましく、9質量%であることがより好ましい。
紫外線吸収剤は、紫外線を吸収する機能を有し、太陽光等による外部から入射される紫外線を吸収することで、光取り出しフィルム10の紫外線暴露での変色の抑制することができ、光取り出しフィルム10が長期安定性に優れる。
光安定化剤は、ラジカルを捕捉する機能を有し、太陽光等の紫外線の入射により発生するラジカルを捕捉することで、光取り出しフィルム10の化学構造変化による変色の抑制することができ、光取り出しフィルム10が長期安定性に優れる。
他の成分としては、例えば、光拡散微粒子、柔軟性向上剤、粘度調整剤、可塑剤、充填剤、難燃剤、帯電防止剤、酸化防止剤、染料及び顔料等の着色剤、離型剤、レベリング剤、防汚性向上剤、分散安定剤等の各種添加剤等が挙げられる。
なお、本発明の光取り出しフィルムにおいて、光取り出しフィルムを構成する材料中の光拡散微粒子の含有率は、光取り出しフィルム10の反りを抑制することから、20質量%以下が好ましく、10質量%以下がより好ましく、0質量%が更に好ましい。
本発明の光取り出しフィルムにおいて、上述の光取り出しフィルムを構成する材料は、フルオレン骨格、ビフェニル骨格及びナフタレン骨格の少なくとも1種の骨格を有する単量体(x)を含む単量体組成物により形成されることが好ましい。なお、単量体(x)は、単独で用いてもよく、二種以上を組み合わせて用いてもよい。また、本発明においては、単量体組成物中に含まれる単量体(x)と、必要に応じて含まれ得る単量体(x)以外の単量体との重合によって樹脂(X)を合成することができる。
また、ビフェニル骨格を有する単量体は、ビフェニルに由来する構成単位、即ち下記式(2)
で表される構成単位を含む。
一方、ナフタレン骨格を有する単量体は、ナフタレンに由来する構造単位、即ち下記式(3)
で表される構成単位を含む。
なお、単量体(x)は、これら骨格の1種を単独で有してもよいし、2種以上を組み合わせて有してもよい。
なお、本明細書において、(メタ)アクリレートとは、アクリレート又はメタクリレートをいう。
(式中、R1及びR2は、それぞれ独立して水素原子又はメチル基であり、a及びbは、それぞれ独立して0~4の整数である。)
なお、架橋性単量体(a)は、単量体(x)を除く。
なお、非架橋性単量体(b)は、単量体(x)と架橋性単量体(a)を除く。
他の成分としては、例えば、光拡散微粒子、柔軟性向上剤、粘度調整剤、可塑剤、充填剤、難燃剤、帯電防止剤、酸化防止剤、染料及び顔料等の着色剤、離型剤、レベリング剤、防汚性向上剤、分散安定剤等の各種添加剤等が挙げられる。
なお、屈折率は、20℃でナトリウムD線を用いて測定した値とする。
凹凸構造層11は、凹凸構造13を有する。これにより、EL素子との組み合わせることで構成される面発光体の光取り出し効率及び法線輝度を向上させる役割を有する。
凹凸構造13は、突起であっても窪みであってもよいが、光取り出しフィルム10の生産性に優れることから、突起が好ましい。
凹凸構造13の配置としては、例えば、六方配列(図2(a))、矩形配列(図2(b))、菱形配列(図2(c))、直線状配列(図2(d))、円状配列(図2(e))、ランダム配置(図2(f))等が挙げられる。これらの凹凸構造13の配置の中でも、面発光体の光取り出し効率や法線輝度に優れることから、六方配列、矩形配列、菱形配列が好ましく、六方配列、矩形配列がより好ましい。
本明細書において、凹凸構造13の底面部15とは、凹凸構造13の底部(ベース層12を有する場合は、ベース層12との接面)の外周縁により囲まれる仮想的な面状部分をいう。
また、本明細書において、凹凸構造13の底面部15の最長径Lとは、凹凸構造13の底面部15における最も長い部分の長さをいい、凹凸構造13の底面部15の平均最長径Laveは、光取り出しフィルム10の凹凸構造13を有する表面を走査型顕微鏡にて撮影し、凹凸構造13の底面部15の最長径Lを5箇所測定し、その平均値とした。
更に、本明細書において、凹凸構造13の高さHとは、突起構造の場合は凹凸構造13の底面部15から最も高い部位までの高さをいい、窪み構造の場合は凹凸構造13の底面部15から最も低い部位までの高さをいい、凹凸構造13の平均高さHaveは、光取り出し10の断面を走査型顕微鏡にて撮影し、凹凸構造13の高さHを5箇所測定し、その平均値とした。
なお、凹凸構造13のアスペクト比は、凹凸構造13の平均高さHave/凹凸構造13の底面部15の平均最長径Laveから算出した。
光取り出しフィルム10の面積(図4でいう実線で囲まれた面積)に対する凹凸構造13の底面部15の面積(図4でいう点線で囲まれた面積)の割合は、面発光体の光取り出し効率や法線輝度を一層向上させることから、20~99%が好ましく、25~95%がより好ましく、30~93%が更に好ましく、70~90%が一層好ましい。本明細書においては、光取り出しフィルム10の面積に対する凹凸構造13の底面部15の面積の割合を「凹凸構造の占有率」という。
なお、凹凸構造13の底面部15がすべて同一の大きさの円形である場合、光取り出しフィルム10の面積に対する凹凸構造13の底面部15の面積の割合の最大値は、91%程度となる。
凹凸構造層11の凹凸構造13を支持することから、ベース層12を設けることが好ましい。ベース層12は、単量体組成物の硬化時の重合収縮等に伴う応力を緩和して、凹凸構造13の形状を維持する役割を有する。
本発明の光取り出しフィルムは、後述するように、EL素子と組み合わせて面発光体を構成するが、ここで、光取り出しフィルム10の形状を保つため、光取り出しフィルム10の凹凸構造13がない面に、言い換えれば光取り出しフィルム10とEL素子との間に、基材14を設けてもよい。
光取り出しフィルム10がベース層12を含む場合には、基材14は、凹凸構造層11が付されたベース層12の面(図1では上面)の反対側の面(図1では下面)に、付される。
また、基材14の屈折率は、1.55~1.65であることが好ましい。
易接着処理の方法としては、例えば、基材14の表面にポリエステル樹脂、アクリル樹脂、ウレタン樹脂等からなる易接着層を形成する方法、基材14の表面を粗面化処理する方法等が挙げられる。
本発明の光取り出しフィルムは、光入射面側の表面に、EL素子30へ接着するため、図1に示すように粘着層21を設けてもよい。光取り出しフィルム10に基材14が付けられている場合には、図1に示すように基材14の表面に粘着層21を設ければよい。
粘着層21としては、例えば、公知の粘着剤等が挙げられる。
また、粘着層21の屈折率は、1.48~1.58であることが好ましい。
粘着層21の表面には、光取り出しフィルム10の取り扱い性を高めるため、図1に示すように保護フィルム22を設けてもよい。保護フィルム22は、EL素子30の表面に光取り出しフィルム10等を貼る際に、光取り出しフィルム10等から剥がせばよい。
保護フィルム22としては、例えば、公知の保護フィルム等が挙げられる。
本発明の光取り出しフィルムの製造方法は、EL素子の基板上に積層する光取り出しフィルムの製造方法であって、基材と凹凸構造の転写部を有する型との間に、フルオレン骨格、ビフェニル骨格及びナフタレン骨格の少なくとも1種の骨格を有する単量体(x)を含む単量体組成物を供給し、単量体組成物を硬化させることを特徴とし、該単量体組成物中の単量体(x)の含有量は、30質量%以上が好ましく、30~86質量%が更に好ましい。なお、単量体組成物の硬化により、単量体(x)と、必要に応じて含まれ得る単量体(x)以外の単量体との重合が起こり、樹脂(X)を合成することができる。
光取り出しフィルム10の製造方法としては、例えば、図5に示すような装置50を用いる方法等が挙げられる。
以下、図5に示す装置50を用いた光取り出しフィルム10の製造方法について説明するが、図5に示す装置50を用いた製造方法に限定されるものではない。
凹凸構造の転写部を有する円筒形のロール型52とゴム製のニップロール53との間に、基材14を導入する。この状態で、回転するロール型52と基材14との間に、タンク55から先端にノズルを取り付けた配管56を通して、単量体組成物51を供給する。
回転するロール型52と基材14との間に挟まれた単量体組成物51は、活性エネルギー線照射装置54付近で活性エネルギー線により硬化される。得られた硬化物をロール型52から離型することで、基材14が付いた光取り出しフィルム10が得られる。
転写面の作製方法としては、例えば、ダイヤモンドバイトによる切削、国際公開第2008/069324号に記載されるようなエッチング等が挙げられる。これらの転写面の作製方法の中でも、曲面を有する突起又は窪みの形成が容易であることから、国際公開第2008/069324号に記載されるようなエッチングが好ましい。
また、転写面の作製方法としては、転写面の突起又は窪みを反転させた窪み又は突起を有するマスター型から、電鋳法を用いて作製した金属薄膜をロール芯部材に巻きつけて、円筒形のロール型52を製造する方法を用いることができる。
ロール型52の内部又は外部には、表面温度を維持するために、必要に応じて、シーズヒータや温水ジャケット等の熱源設備を設けてもよい。
活性エネルギー線照射装置54の活性エネルギー線の発光光源としては、例えば、ケミカルランプ、低圧水銀ランプ、高圧水銀ランプ、メタルハライドランプ、無電極紫外線ランプ、可視光ハロゲンランプ、キセノンランプ等が挙げられる。
活性エネルギー線照射装置54の活性エネルギー線の積算光量は、特に限定されないが、活性エネルギー線硬化性組成物の硬化性に優れ、光取り出しフィルム10の劣化を抑制することから、0.01~10J/cm2が好ましく、0.5~8J/cm2がより好ましい。
本発明の面発光体は、本発明の光取り出しフィルム及びEL素子を含むことを特徴とし、光取り出しフィルムとEL素子との間に基材(好ましくはポリエステル樹脂基材)や粘着層を有することが好ましい。本発明の面発光体としては、例えば、図6に示すような面発光体が挙げられる。
以下、図6の面発光体について説明するが、本発明の面発光体は図6の面発光体に限定されるものではない。
EL素子30に光取り出しフィルム10を設けた面発光体は、光取り出し効率や法線輝度に優れ、出射光波長の出射角度依存性を抑制することができる。
なお、実施例中の「部」及び「%」は、「質量部」及び「質量%」を示す。
実施例及び比較例で得られた光取り出しフィルムを、超促進耐候性試験機(機種名「メタルウェザー」、ダイプラ・ウィンテス(株)製)を用いて、照度140mW、フィルター「KF-2」、温度30℃、湿度70%RH、時間24時間の条件で、紫外線による加速劣化試験を行った。
実施例、比較例及び参考例で得られた面発光体上に、直径10mmの穴の空いた厚さ0.1mmの遮光シートを配置し、これを、積分球(ラブスフェア社製、大きさ6インチ)のサンプル開口部に配置した。この状態で、EL素子に10mAの電流を通電して点灯した時の、遮光シートの直径10mmの穴から出射する光を、分光計測器(分光器:機種名「PMA-12」(浜松フォトニクス社製)、ソフトウェア:ソフト名「PMA用基本ソフトウェアU6039-01ver.3.3.1」)にて測定し、標準視感度曲線による補正を行って、面発光体の光子数を算出した。
参考例で得られた面発光体の光子数を100%としたときの、実施例及び比較例で得られた面発光体の光子数の割合を、光取り出し効率とした。
実施例、比較例及び参考例で得られた面発光体上に、直径10mmの穴の空いた厚さ0.1mmの遮光シートを配置した。この状態で、EL素子に1.5Aの電流を通電した点灯した時の、遮光シートの直径10mmの穴から出射する光を、輝度計(機種名「BM-7」、トプコン社製)にて、面発光体の法線方向から測定し、面発光体の輝度値を得た。
参考例で得られた面発光体の輝度値を100%としたときの、実施例及び比較例で得られた面発光体の輝度値の割合を、法線輝度とした。
実施例、比較例及び参考例で得られた面発光体上に、直径10mmの穴の空いた厚さ0.1mmの遮光シートを配置した。この状態で、EL素子に1.5Aの電流を通電した点灯した時の、遮光シートの直径10mmの穴から出射する光を、輝度計(機種名「BM-7」、トプコン社製)にて、面発光体の法線方向(0°)、面発光体の法線方向から10°傾けた方向、面発光体の法線方向から20°傾けた方向、面発光体の法線方向から30°傾けた方向、面発光体の法線方向から40°傾けた方向、面発光体の法線方向から50°傾けた方向、面発光体の法線方向から60°傾けた方向、面発光体の法線方向から70°傾けた方向、面発光体の法線方向から75°傾けた方向、面発光体の法線方向から80°傾けた方向から、それぞれxy表色系の色度u’、v’を測定した。各角度のu’の値及びu’の平均値を横軸に、各角度のv’の値及びv’の平均値を縦軸にプロットし、u’及びv’の平均値をプロットした点から各角度のu’及びv’の値をプロットした点までの距離を算出し、その距離が最も長くなる時の値を色度変化量とした。
なお、色度変化量が小さいほど、面発光体の出射光波長の出射角度依存性が抑制されたことを意味する。
光取り出しフィルムの13C-NMRのピーク面積比を、固体13C-NMRで測定した。まず、樹脂(X)を細かく切り刻んで、内径2.5mmのサンプル管内に入れた。次いで、DD-MAS法にて90°、パルス幅3μ秒、サンプル回転数16kHz、積算数4096回、繰り返し待ち時間60秒にて測定を行った。得られたスペクトルにおいて、カーボンのケミカルシフト115~160ppmの範囲に位置する芳香族由来のピーク面積(A1)と、それ以外の範囲にある芳香族以外の部分由来のピーク面積(A2)とを求めて、ピーク面積比(A1/A2)を算出した。
(活性エネルギー線硬化性単量体組成物Aの製造)
下記式(6)で表されるフルオレンジアクリレート50部、下記式(7)で表されるアクリレート(商品名「NKエステルA-LEN-10」、新中村化学工業(株)製)50部及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Aを得た。
なお、単量体組成物Aの硬化物の屈折率は、1.61である。
(活性エネルギー線硬化性単量体組成物Bの製造)
上記式(6)で表されるフルオレンジアクリレート50部、下記式(8)で表されるジメタクリレート20部(商品名「アクリルエステルPBOM2000」、三菱レイヨン(株)製)、下記式(9)で表されるジアクリレート20部(商品名「ABE-300」、新中村化学工業(株)製)、下記式(10)で表されるアクリレート10部(商品名「ニューフロンティアPHE」、第一工業製薬(株)製)及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性樹脂単量体組成物Bを得た。
なお、単量体組成物Bの硬化物の屈折率は、1.59である。
(活性エネルギー線硬化性単量体組成物Cの製造)
上記式(6)で表されるフルオレンジアクリレート40部、上記式(7)で表されるアクリレート40部、上記式(8)で表されるジメタクリレート20部及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Cを得た。
なお、単量体組成物Cの硬化物の屈折率は、1.58である。
(活性エネルギー線硬化性単量体組成物Dの製造)
上記式(6)で表されるフルオレンジアクリレート70部、上記式(10)で表されるアクリレート30部及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Dを得た。
なお、単量体組成物Dの硬化物の屈折率は、1.59である。
(活性エネルギー線硬化性単量体組成物Eの製造)
上記式(6)で表されるフルオレンジアクリレート70部、上記式(8)で表されるジメタクリレート30部及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Eを得た。
なお、単量体組成物Eの硬化物の屈折率は、1.58である。
(活性エネルギー線硬化性単量体組成物Fの製造)
上記式(6)で表されるフルオレンジアクリレート36部、上記式(7)で表されるアクリレート36部、上記式(8)で表されるジメタクリレート18部、シリコーン樹脂球状微粒子(商品名「TSR9000」、モメンティブ・パフォーマンス・マテリアルズ社製)10部、屈折率:1.42、体積平均粒子径:2μm)及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Fを得た。
なお、単量体組成物Fの硬化物の屈折率は、1.58である。
(活性エネルギー線硬化性単量体組成物Gの製造)
上記式(6)で表されるフルオレンジアクリレート32部、上記式(7)で表されるアクリレート32部、上記式(8)で表されるジメタクリレート16部、シリコーン樹脂球状微粒子(商品名「TSR9000」、モメンティブ・パフォーマンス・マテリアルズ社製)20部、屈折率:1.42、体積平均粒子径:2μm)及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Gを得た。
なお、単量体組成物Gの硬化物の屈折率は、1.58である。
(活性エネルギー線硬化性単量体組成物Hの製造)
上記式(6)で表されるフルオレンジアクリレート10部、上記式(7)で表されるアクリレート60部、上記式(8)で表されるジメタクリレート30部及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Hを得た。
なお、単量体組成物Hの硬化物の屈折率は、1.51である。
(活性エネルギー線硬化性単量体組成物Iの製造)
下記式(11)で表されるウレタンアクリレート(商品名「M-315」、日本化薬(株)製)100部及び1-ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュア184」、BASF社製)1.6部を混合し、活性エネルギー線硬化性単量体組成物Iを得た。
なお、単量体組成物Iの硬化物の屈折率は、1.50である。
(球欠形状の転写部を備えるロール型の製造)
外径200mm、軸方向の長さ320mmの鋼製のロールの外周面に、厚さ200μm、ビッカース硬度230Hvの銅めっきを施した。銅めっき層の表面に感光剤を塗布し、レーザ露光、現像及びエッチングを行い、銅めっき層に直径50μm、深さ25μmの半球状の窪みが最小間隔3μmで六方配列に並んでいる転写部が形成された型を得た。得られた型の表面に、防錆性及び耐久性を付与するため、クロムめっきを施し、ロール型を得た。
(楕円球欠形状の転写部を備えるロール型の製造)
外径200mm、軸方向の長さ320mmの鋼製のロールの外周面に、厚さ200μm、ビッカース硬度230Hvの銅めっきを施した。楕円輪郭を有するボールエンドミル刃をエアスピンドルで回転させながら、銅めっき層に切削することで、銅めっき層に直径30μm、深さ18μmの半球状の窪みが最小間隔1μmで六方配列に並んでいる転写部が形成された型を得た。得られた型の表面に、防錆性及び耐久性を付与するため、クロムめっきを施し、ロール型を得た。
また、銅めっき層に直径30μm、深さ18μmの半球状の窪みが最小間隔2μmで六方配列に並んでいる転写部を備える型を同様の方法で得た。
(角錐形状の転写部を備えるロール型の製造)
外径200mm、軸方向の長さ320mmの鋼製のロールの外周面に、厚さ200μm、ビッカース硬度230Hvの銅めっきを施した。先端角90°の単結晶ダイヤモンド工具を用い、銅めっき層に切削することで、銅めっき層に一辺50μm、深さ25μmの四角錘状の窪みが隙間なく並んでいる転写部(占有率100%)が形成された型を得た。得られた型の表面に、防錆性及び耐久性を付与するため、クロムめっきを施し、ロール型を得た。
Symfos OLED-010K(コニカミノルタ社製、白色OLED素子)の光出射面側の表面の光取り出しフィルムを剥離したEL素子Aを、そのまま面発光体とした。
なお、EL素子Aのガラス基板の屈折率は、1.50である。
製造例10で得られたロール型に、活性エネルギー線硬化性単量体組成物Aを塗布し、その上に厚さ125μmのポリエチレンテレフタレート基材(商品名「ダイヤホイルT910E125」、三菱樹脂(株)製、屈折率:1.60)を置き、ベース層の厚さが20μmになるように活性エネルギー線硬化性単量体組成物Aをニップロールで均一に伸ばした。その後、基材の上から紫外線を照射し、ロール型と基材とに挟まれた活性エネルギー線硬化性単量体組成物Aを硬化させ、得られた硬化物と基材との接合体をロール型から剥離し、基材が付いた光取り出しフィルムを得た。
硬化した活性エネルギー線硬化性単量体組成物Aの屈折率は、表1の「屈折率」欄に記載されるように、1.61であった。
得られた光取り出しフィルムの走査型顕微鏡にて撮影した画像から算出した光取り出しフィルムの凹凸構造の大きさは、平均最長径Laveが48.2μm、平均高さHaveが26.0μmであり、ほぼロール型の窪みの大きさに対応した球欠形状の突起からなる凹凸構造が得られた。また、得られた光取り出しフィルムの走査型顕微鏡にて撮影した画像から、得られた光取り出しフィルムの凹凸構造は、ロール型に対応し最小間隔3μmで六方配列に並び、光取り出しフィルムの面積に対する凹凸構造の底面部の総面積の割合(凹凸構造の占有率)は、76%であった。
上記EL素子Aの光出射面に、粘着層としてカーギル標準屈折液(屈折率1.52、(株)モリテックス製)を塗布した。この粘着層に、上記光取り出しフィルムに付けられている基材の面を光学密着させ、面発光体を得た。得られた面発光体の光取り出し効率、法線輝度及び色度変化量の測定結果を、硬化した活性エネルギー線硬化性単量体組成物の屈折率と共に、表1に示す。
光取り出しフィルム製造に際して用いる活性エネルギー線硬化性単量体組成物を表1の「組成」欄に記載のものに変更し、ロール型の転写部を表1の「凹凸構造形状」の欄に記載のものに変更した以外は、実施例1と同様に操作を行い、面発光体を得た。なお、実施例9では、半球状窪みの最小間隔が1μmである転写部を備えた型を用いており、実施例10では、半球状窪みの最小間隔が2μmである転写部を備えた型を用いた。得られた面発光体の光取り出し効率、法線輝度及び色度変化量の測定結果を、硬化した活性エネルギー線硬化性単量体組成物の屈折率と共に、表1に示す。
厚さ125μmのポリエチレンテレフタレート基材(商品名「ダイヤホイルT910E125」、三菱樹脂(株)製、屈折率:1.60)上に活性エネルギー線硬化性単量体組成物Cを塗布し、その上に厚さ125μmのポリエチレンテレフタレート基材(商品名「ダイヤホイルT910E125」、三菱樹脂(株)製、屈折率:1.60)を置き、ベース層の厚さが20μmになるように活性エネルギー線硬化性単量体組成物Cをニップロールで均一に伸ばした。その後、基材の上から紫外線を照射し、基材間に挟まれた活性エネルギー線硬化性単量体組成物Cを硬化させ、一方の基材を得られた硬化物から剥離し、他方の基材が付いた光取り出しフィルムを得た。
次に、上記EL素子Aの光出射面に、粘着層としてカーギル標準屈折液(屈折率1.52、(株)モリテックス製)を塗布した。この粘着層に、上記光取り出しフィルムに付けられている基材の面を光学密着させ、面発光体を得た。得られた面発光体の光取り出し効率、法線輝度及び色度変化量の測定結果を、硬化した活性エネルギー線硬化性単量体組成物の屈折率と共に、表1に示す。
一方、単量体(x)を含まない単量体組成物を用いて製造した光取り出しフィルムを用いた比較例1で得られた面発光体は、光取り出し効率及び法線輝度の向上が十分でなかった。
なお、比較例2で得られた面発光体は、光取り出しフィルムの表面に凹凸構造を有しないため、光取り出し効率及び法線輝度の向上が十分でなかった。
(活性エネルギー線硬化性単量体組成物Jの製造)
下記式(12)で表されるフルオレンジアクリレート(商品名「EA-0100」、大阪ガスケミカル(株)製)40部、下記式(8)で表されるジメタクリレート(商品名「アクリエステルPBOM2000」、三菱レイヨン(株)製)10部、下記式(9)で表されるジメタクリレート(商品名「ABE-300」、新中村化学工業(株)製)20部、下記式(13)で表されるアクリレート(商品名「ニューフロンティアPHE」、第一工業製薬(株)製)30部及び重合開始剤(商品名「Lucirin TPO」、BASF社製)1部を混合し、予備単量体組成物を得た。
なお、得られた予備単量体組成物の硬化物は、屈折率が1.58であり、13C-NMRで測定した芳香族由来のピーク面積(A1)の芳香族以外の部分由来のピーク面積(A2)に対する比(A1/A2)が0.70である。
外径200mm、軸方向の長さ320mmの鋼製のロールの外周面に、厚さ200μm、ビッカース硬度230Hvの銅めっきを施した。銅めっき層の表面に感光剤を塗布し、レーザ露光、現像及びエッチングを行い、銅めっき層に直径50μm、深さ25μmの半球状の窪みが最小間隔5μmで六方配列に並んでいる転写部が形成された型を得た。得られた型の表面に、防錆性及び耐久性を付与するため、クロムめっきを施し、ロール型を得た。
得られたロール型に、得られた活性エネルギー線硬化性単量体組成物Jを塗布し、その上に厚さ125μmのポリエチレンテレフタレート基材(商品名「ダイヤホイルT910E125」、三菱樹脂(株)製、屈折率:1.60)を置き、ニップロールで均一に伸ばした。その後、基材の上から紫外線を照射し、ロール型と基材に挟まれた活性エネルギー線硬化性単量体組成物Jを硬化させ、ロール型から単量体組成物Jの硬化物を剥離し、基材が付いた光取り出しフィルムを得た。硬化の際に、ロール型の押圧を制御することでベース層の厚さを制御することができ、実施例13ではベース層の厚さが30μmになるように設定した。
得られた光取り出しフィルムの走査型顕微鏡にて撮影した画像から算出した光取り出しフィルムの凹凸構造の大きさは、平均最長径Laveが48.0μm、平均高さHaveが27.1μmで、ほぼロール型の窪みの大きさに対応した球欠形状の突起が得られた。また、走査型顕微鏡にて撮影した画像から、得られた光取り出しフィルムの凹凸構造は、ロール型に対応し最小間隔10μmで六方配列に並び、光取り出しフィルムの面積に対する球状突起の底面部の面積の割合(凹凸構造の占有率)は、73%であった。
EL素子の光出射面側に、粘着層としてカーギル標準屈折液(屈折率1.52、(株)モリテックス製)を塗布し、得られた光取り出しフィルムに付けられている基材の面を光学密着させ、面発光体を得た。得られた面発光体の光取り出し効率、法線輝度、色度変化量を表2に示す。
なお、EL素子として、Symfos OLED-010K(コニカミノルタ社製、白色OLED素子)の光出射面側の表面の光取り出しフィルムを剥離したEL素子を用いた。
紫外線吸収剤の含有率と光安定化剤の含有率を表2のように変更した以外は、実施例13と同様に操作を行い、光取り出しフィルム及び面発光体を得た。得られた面発光体の評価結果を表2に示す。
なお、光安定化剤として、ヒンダードアミン系化合物(商品名「Tinuvin123」、BASF社製)を用いた。
実施例13で用いたEL素子、即ちSymfos OLED-010K(コニカミノルタ社製、白色OLED素子)の光出射面側の表面の光取り出しフィルムを剥離したEL素子を、そのまま面発光体とした。
なお、EL素子のガラス基板の屈折率は、1.50である。
11 凹凸構造層
12 ベース層
13 凹凸構造
14 基材
15 凹凸構造の底面部
21 粘着層
22 保護フィルム
30 EL素子
31 ガラス基板
32 陽極
33 発光層
34 陰極
50 装置
51 単量体組成物
52 ロール型
53 ニップロール
54 活性エネルギー線照射装置
55 タンク
56 配管
Claims (19)
- EL素子の基板上に積層する光取り出しフィルムであって、
光取り出しフィルムは、表面に凹凸構造を有し、
光取り出しフィルムを構成する材料は、フルオレン骨格、ビフェニル骨格及びナフタレン骨格の少なくとも1種の骨格を有する樹脂(X)を含む、
光取り出しフィルム。 - 光取り出しフィルムを構成する材料中の樹脂(X)の含有率が、50質量%以上である、請求項1~3のいずれかに記載の光取り出しフィルム。
- 光取り出しフィルムを13C-NMRで測定した芳香族由来のピーク面積(A1)の芳香族以外の部分由来のピーク面積(A2)に対する比(A1/A2)が、0.1以上である、請求項1~4のいずれかに記載の光取り出しフィルム。
- 光取り出しフィルムの屈折率が、1.55~1.65である、請求項1~5のいずれかに記載の光取り出しフィルム。
- 樹脂(X)が、ポリオキシアルキレングリコールジ(メタ)アクリレート単位、ポリエステルポリオールジ(メタ)アクリレート単位及び芳香族エステルジオールジ(メタ)アクリレート単位の少なくとも1種の構成単位を含む、請求項1~6のいずれかに記載の光取り出しフィルム。
- 凹凸構造の形状が、球欠形状、球欠台形状、楕円体球欠形状、楕円体球欠台形状、角錐形状及び角錐台形状の少なくとも1種である、請求項1~7のいずれかに記載の光取り出しフィルム。
- 凹凸構造の形状が、球欠形状及び楕円体球欠形状の少なくとも1種であり、凹凸構造の占有率が、70~90%である、請求項1~8のいずれかに記載の光取り出しフィルム。
- 光取り出しフィルムを構成する材料中の光拡散微粒子の含有率が、20質量%以下である、請求項1~9のいずれかに記載の光取り出しフィルム。
- 光取り出しフィルムを構成する材料が、紫外線吸収剤を含む、請求項1~10のいずれかに記載の光取り出しフィルム。
- 光取り出しフィルムを構成する材料が、光安定化剤を含む、請求項1~11のいずれかに記載の光取り出しフィルム。
- 請求項1~12のいずれかに記載の光取り出しフィルム及びEL素子を含む、面発光体。
- 光取り出しフィルムとEL素子との間にポリエステル樹脂基材を有する、請求項13に記載の面発光体。
- EL素子の基板は、屈折率が1.45~1.55のガラスである、請求項13又は14に記載の面発光体。
- 光取り出しフィルムとEL素子との間に粘着層を有し、粘着層の屈折率が、1.48~1.58である、請求項13~15のいずれかに記載の面発光体。
- 面発光体の色度変化量が、0.01以下である、請求項13~16のいずれかに記載の面発光体。
- EL素子の基板上に積層する光取り出しフィルムの製造方法であって、
基材と凹凸構造の転写部を有する型との間に、フルオレン骨格、ビフェニル骨格及びナフタレン骨格の少なくとも1種の骨格を有する単量体(x)を含む単量体組成物を供給し、単量体組成物を硬化する、光取り出しフィルムの製造方法。 - 単量体組成物中の単量体(x)の含有率が、30質量%以上である、請求項18に記載の光取り出しフィルムの製造方法。
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JP2018039988A (ja) * | 2016-08-23 | 2018-03-15 | 三洋化成工業株式会社 | 光硬化性組成物 |
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US10153461B1 (en) * | 2017-09-13 | 2018-12-11 | Int Tech Co., Ltd. | Display panel and method for manufacturing the same |
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CN116841080A (zh) * | 2022-03-24 | 2023-10-03 | 咏巨科技有限公司 | 光学膜及应用其的发光模块 |
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