WO2013088997A1 - 面発光体および前面フィルム - Google Patents
面発光体および前面フィルム Download PDFInfo
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- WO2013088997A1 WO2013088997A1 PCT/JP2012/081451 JP2012081451W WO2013088997A1 WO 2013088997 A1 WO2013088997 A1 WO 2013088997A1 JP 2012081451 W JP2012081451 W JP 2012081451W WO 2013088997 A1 WO2013088997 A1 WO 2013088997A1
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- Prior art keywords
- particle
- light
- containing layer
- resin
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- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical class OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- CXVGEDCSTKKODG-UHFFFAOYSA-N sulisobenzone Chemical compound C1=C(S(O)(=O)=O)C(OC)=CC(O)=C1C(=O)C1=CC=CC=C1 CXVGEDCSTKKODG-UHFFFAOYSA-N 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
-
- 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
- G02B5/0226—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 having particles on the surface
-
- 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
- G02B5/0236—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element
- G02B5/0242—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element by means of dispersed particles
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0273—Diffusing elements; Afocal elements characterized by the use
- G02B5/0278—Diffusing elements; Afocal elements characterized by the use used in transmission
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
-
- 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
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
-
- 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
- H10K50/86—Arrangements for improving contrast, e.g. preventing reflection of ambient light
- H10K50/865—Arrangements for improving contrast, e.g. preventing reflection of ambient light comprising light absorbing layers, e.g. light-blocking layers
Definitions
- the present invention provides a surface light emitter that has a high light extraction efficiency and a small change in color depending on the viewing angle, and is less likely to scatter fragments when the translucent substrate is cracked, and a front film used therefor About.
- electroluminescence may be abbreviated as EL
- An organic EL element can be used as a light source of a lighting device or a backlight of a display device because the light color can be white or a color close thereto.
- a currently known organic EL element is composed of components such as an organic EL layer, a transparent electrode, and a translucent substrate made of glass or a polymer film, and transmits light generated in the organic EL layer to the outside through the translucent substrate.
- the loss when extracting light is large, and the efficiency of extracting the generated light to the outside (hereinafter referred to as light extraction efficiency) is only about 20%.
- a white organic EL element includes a plurality of light emitting elements such as red, green, blue, yellow, and blue, but the behavior of refraction and reflection in each component depends on the wavelength of light. Because of the difference, a change in color depending on the viewing angle (hereinafter referred to as color shift) is a problem to be solved.
- the translucent substrate used in the current organic EL element is mainly made of glass, and there is a concern that when an impact is applied, it breaks and scatters fragments.
- Patent Document 1 As a method for improving the light extraction efficiency of the organic EL element, a resin layer containing a scattering material is provided on the surface of the translucent substrate opposite to the light emitter (Patent Document 1), and a light diffusing adhesive layer is provided ( A method such as Patent Document 2) has been proposed. Further, as a method for achieving light extraction efficiency, color misregistration reduction, and prevention of scattering when the translucent substrate is cracked, a resin layer containing particles is provided between the transparent electrode and the translucent substrate, and a lens sheet is provided on the light exit surface. A method of providing (Patent Document 3) has been proposed.
- Patent Document 1 does not have a function of preventing the scattering of fragments when the transparent substrate is cracked, or the occurrence of color misregistration cannot be sufficiently prevented.
- Patent Document 3 needs to form a transparent electrode having a thickness of several tens of nanometers on a resin layer having a large surface unevenness due to the influence of light diffusing particles, and lacks feasibility in consideration of actual manufacturing technology. Met.
- the object of the present invention is to solve the above-mentioned problems of the prior art, and in addition to high light extraction efficiency and small color shift, it is scattered when the transparent substrate is cracked. It is an object of the present invention to provide a surface light emitter that is difficult to perform and a front film used therefor.
- a surface light emitter in which at least a three-layer front film having a resin layer containing particles on both sides of a base film is in contact with a light-emitting element having a light-transmitting substrate on one side.
- the resin layer (first particle-containing layer) located on the light incident side of the front film contains 1 to 50% by mass of particles
- the resin layer (second particle-containing layer) located on the light-emitting side of the front film ) Contains 20 to 80% by mass of particles.
- the surface light emitter according to 1 above, wherein a difference in refractive index between the resin constituting the first particle-containing layer and the particles is 0.05 to 0.5. 3.
- FIG. 1 is a schematic diagram showing an example of the configuration of the surface light emitter of the present invention.
- the surface light emitter 1 of the present invention includes a light emitting element 2 and a front film 3, and the light emitting element 2 and the front film 3 are arranged in contact with each other.
- the light-emitting element 2 includes a light-emitting layer 4 and a light-transmitting substrate 5, and the front film 3 includes a first particle-containing layer 6, a base film 7, and a second film in order from the light-transmitting substrate 5 side of the light-emitting element 2.
- It is a laminate having a three-layer configuration of the particle-containing layer 8.
- the surface light emitter 1 of the present invention is not particularly limited as long as it is a planar light emitter.
- the surface shape is not limited to a flat surface, but includes a curved surface having a certain curvature and a surface curved indefinitely, and includes a surface having partial unevenness.
- FIG. 2 is a schematic diagram showing an example of the configuration of the light emitting element used in the present invention.
- the translucent substrate 5 is made of glass or a polymer film substrate. Currently, glass having good gas barrier properties is mainly used.
- the structure of the light emitting layer 4 shows the example by which the sealing layer 9, the back electrode 10, the light-emitting body 11, and the transparent electrode 12 are arrange
- the sealing layer 9 is installed in order to prevent the light emitting body 11 from deteriorating due to intrusion of water and oxygen from the back and side surfaces.
- the back electrode 10 is a reflective electrode, and silver or aluminum is often used. Examples of the light emitter 11 include organic electroluminescent light emitters and inorganic electroluminescent light emitters.
- the light emitting element using an organic electroluminescent light-emitting body is called an organic electroluminescent light-emitting element
- the light-emitting element using an inorganic electroluminescent light-emitting body is called an inorganic electroluminescent light-emitting element.
- an indium-tin oxide film hereinafter referred to as ITO or the like is often used.
- FIG. 3 is a schematic diagram showing a three-layer front film as an example of the structure of the front film used in the present invention. Since the front film 3 is disposed in contact with the translucent substrate 5 of the light emitting element 2 as described with reference to FIG. 1, the side in contact with the translucent substrate 5 is the light incident side of the base film 7. The side opposite to the substrate film from the side is defined as the light exit side. As shown in FIG. 3, the front film has a resin layer containing particles on both sides thereof, the first particle-containing layer 6 on the light incident side, the second particle-containing layer 8 on the light-emitting side, and the first particles.
- the resin constituting the content layer 6 is the resin (A) 13
- the particles contained in the first particle content layer 6 are the particles (A) 14
- the resin constituting the second particle content layer 8 is the resin (B) 15, and the second
- the particles contained in the particle-containing layer 8 are defined as particles (B) 16.
- the base film may be composed of two or more layers.
- the functional layer may be disposed in the surface region on the first particle-containing layer side and / or the surface region on the second particle-containing layer side. Good.
- the first particle-containing layer 6 contains 1 to 50 mass% of particles (A) 14.
- the particles (A) 14 are buried and dispersed in the resin (A) 13, and the light-transmitting substrate 5 and the front film of the light-emitting element 2 are formed.
- 3 first particle-containing layers 6 can be disposed in contact with each other.
- being placed in contact means that the translucent substrate 5 and the first particle-containing layer 6 are in close contact. If there is an air layer between the translucent substrate 5 and the first particle-containing layer 6, a loss due to light reflection between the light layer and the air layer increases, so that no light layer is interposed.
- adhered is taken. That is, by taking such a configuration, it is possible to reduce reflection loss between the translucent substrate 5 and the first particle-containing layer 6. In the present invention, for this reason, the amount of minute air entrapment between the translucent substrate 5 and the first particle-containing layer 6 is also small (the air entrapment in this case is expressed as a void). It is preferable that such minute voids are 1% or less per unit area. Further, in the first particle-containing layer 6, the particles (A) 14 are buried and dispersed in the resin (A) 13, so that the refractive index of the resin (A) 13 and the particles (A) 14 is increased. The transmitted light can be scattered by the difference.
- the second particle-containing layer 8 contains 20 to 80% by mass of the particles (B) 16 in the resin (B) 15.
- grain content layer 8 By setting it as the said mass content rate, in the 2nd particle
- the present invention achieves both reduction in color shift and improvement in light extraction efficiency by providing two particle-containing layers and further controlling the mass content of the particles under the above conditions.
- a surface light emitter has been found.
- the base film 7 the surface light emitter 1 that is difficult to be scattered when the translucent substrate is broken can be obtained.
- the material used as the base film is not particularly limited, but a plastic film is preferably used from the viewpoint of supply properties and handling properties.
- the plastic film material include polyolefin, polyester, polycarbonate, polyether, polyamide, polyimide, and polyacryl.
- a polyester film is preferably used from the viewpoint of durability and the like, and polyethylene terephthalate (hereinafter referred to as PET) is particularly preferably used since it is excellent in supplyability.
- the film used as the base film may be a film produced through a uniaxial or biaxial stretching process in the production process, or may be a film produced without undergoing a stretching process.
- a film produced through a stretching process is preferable because of its high strength. What is necessary is just to judge comprehensively from the intensity
- the base film may be transparent, or may be translucent by incorporating various organic and / or inorganic particles and cavities for the purpose of diffusing light, but is colored. Preferably not.
- the film used as the base film may be a so-called single layer film made of one kind of material, or a composite film in which a plurality of materials are laminated, and a functional layer is arranged on the surface. These may be selected according to the characteristics to be obtained.
- the thickness of the base film according to the present invention is not particularly limited, but is preferably 10 ⁇ m or more and 500 ⁇ m or less. If it is less than 10 ⁇ m, handling may be difficult, and if it exceeds 500 ⁇ m, light loss may occur in the base film.
- the thickness of the base film is preferably 30 ⁇ m or more and 300 ⁇ m or less, more preferably 50 ⁇ m or more and 200 ⁇ m or less.
- the boundary between the base film and the first or second particle-containing layer can be determined by observing a cross section with an electron microscope or measuring a layer thickness with a laser microscope.
- a 1st particle content layer contains particle
- resin (A) used for a 1st particle content layer The resin which has an organic component as a main component is preferable, for example, polyester resin, polyurethane resin, acrylic resin, methacrylic resin, polyamide resin, polyethylene resin, polypropylene Examples thereof include resins, polyvinyl chloride resins, polyvinylidene chloride resins, polystyrene resins, polyvinyl acetate resins, fluorine resins, epoxy resins, and silicone resins.
- the resin containing an organic component as a main component refers to a resin containing 60% by mass or more of an organic component in the resin (A) used for the first particle-containing layer, and a resin containing 80% by mass or more of an organic component.
- the main component is defined similarly.
- These resins may be used alone, or two or more copolymers or a mixture thereof may be used.
- polyester resins, polyurethane resins, acrylic resins, or methacrylic resins are preferably used because of their excellent heat resistance, appearance, and particle dispersibility.
- the peel strength between the first particle-containing layer and the translucent substrate is preferably 0.5 N / 25 mm or more, because durability is improved, preferably 1 N / 25 mm or more, and more preferably 2 N / 25 mm or more. Is preferred. Moreover, since the peel strength between the first particle-containing layer and the light-transmitting substrate exceeds 50 N / 25 mm, there is almost no contribution to the improvement of the durability, so 50 N / 25 mm or less is practically sufficient. is there. When scratches or the like occur on the front film 3, only the front film can be peeled and replaced, and therefore, it is preferably 40 N / 25 mm or less, and more preferably 30 N / 25 mm or less.
- the peel strength between the first particle-containing layer and the translucent substrate is measured by the method described in “(6) Peel strength between the first particle-containing layer and the translucent substrate” in Examples described later. Value.
- the resin used for the first particle-containing layer includes a polyester resin, a polyurethane resin, an acrylic resin, and an epoxy resin. And resins such as silicone resins. These resins may be used alone, or two or more copolymers or a mixture thereof may be used.
- the acrylic resin is excellent in reliability such as water resistance, heat resistance, and light resistance in addition to setting the peel strength between the first particle-containing layer and the translucent substrate in such a preferable range. It is preferable because of its high transparency.
- the manufacturing method of the surface emitting body mentioned later it has adhesiveness on the surface applied to the method of (ii) at the time of arrange
- a material for obtaining a low glass transition temperature for example, 220 to 250 K
- a low surface energy for obtaining sufficient wetness for example, 220 to 250 K
- a cohesive force it is preferable to select a material in consideration of conditions such as setting an appropriate molecular weight every time.
- Materials that satisfy these conditions include acrylic adhesives “SK Dyne” (registered trademark) (manufactured by Soken Chemical Co., Ltd.), acrylic adhesives “Olivein” (registered trademark) (manufactured by Toyo Ink Co., Ltd.), etc. Can be used. Furthermore, it is preferable to adjust the crosslinking density according to the type and amount of a crosslinking agent (isocyanate-based curing agent) for optimizing the balance between flow deformation during wetting and resistance during peeling.
- SK Dyne registered trademark
- acrylic adhesives “Olivein” registered trademark
- Toyo Ink Co., Ltd. Toyo Ink Co., Ltd.
- the shape of the particles (A) used in the first particle-containing layer is, for example, a flat shape such as a star shape, a leaf shape or a disk shape, a rhombus shape, a rectangular shape, a needle shape, a confetti shape, or an aspheric shape such as an indefinite shape.
- a spherical shape (not necessarily a true sphere, but a particle whose cross-sectional shape is surrounded by a curved surface such as a circle, an ellipse, a substantially circle, or a substantially ellipse).
- the particles having these shapes may be porous, non-porous, or hollow, and particles having different particle shapes may be mixed, but a spherical shape in which scattered light is uniformly scattered is preferable.
- the material of the particles (A) used for the first particle-containing layer may be either an organic compound or an inorganic compound, and is not particularly limited. Further, particles of different materials may be mixed and used.
- the organic compound used when the organic compound is applied as the material of the particles (A) used in the first particle-containing layer is preferably a resin mainly composed of a high-melting cross-linked polymer component, such as a polyester resin.
- a resin mainly composed of a high-melting cross-linked polymer component such as a polyester resin.
- Polyamide resin particles such as benzoguanamine, polyurethane resin, acrylic resin, methacrylic resin, polyamide resin, polyethylene resin, polypropylene resin, polyvinyl chloride resin, polyvinylidene chloride resin, polystyrene resin, polyvinyl acetate resin, fluorine resin, A silicone resin etc. are mentioned. These resins may be used alone, or two or more copolymers or a mixture thereof may be used.
- Examples of the inorganic compound used when applying the inorganic compound as the material of the particles (A) used in the first particle-containing layer include calcium carbonate, magnesium carbonate, zinc carbonate, titanium oxide, zinc oxide, cerium oxide, and magnesium oxide. , Barium sulfate, zinc sulfide, calcium phosphate, silica, alumina, mica, mica titanium, talc, clay, kaolin, lithium fluoride, calcium fluoride and the like.
- acrylic resin, methacrylic resin, polyamide resin, epoxy resin, melamine resin, etc. are used as the material of the particles (A) used for the first particle-containing layer because of excellent optical characteristics and solvent resistance. It is preferable.
- the average particle size of the particles used in the first particle-containing layer is preferably from 0.1 to 30 ⁇ m, more preferably from 0.5 to 20 ⁇ m, still more preferably from 1.0 to 10 ⁇ m.
- An average particle diameter here is a number average particle diameter, and shall mean the number average value of the particle diameter which describes the measuring method in an Example (the same applies to the particle (B) in the second particle-containing layer). is there).
- the content ratio of the particles in the first particle-containing layer is 1 to 50% by mass, preferably 1 to 40% by mass, more preferably 1 to 30% by mass, and further preferably 1 to 20% by mass.
- grain is a ratio of the mass of the particle
- the difference in refractive index between the resin constituting the first particle-containing layer and the particles is preferably 0.05 to 0.5, more preferably 0.05 to 0.3. If the difference in refractive index is less than 0.05, light diffusibility may not be obtained, and if the difference in refractive index is greater than 0.5, the internal diffusion is too large and the total light transmittance decreases, As a result, the light extraction efficiency may decrease.
- the first particle-containing layer preferably contains an ultraviolet absorber.
- an ultraviolet absorber it can select from the group similar to the ultraviolet absorber quoted by the below-mentioned 2nd particle content layer.
- the thickness of the first particle-containing layer is not particularly limited, but is preferably 0.3 to 70 ⁇ m. When the thickness is smaller than 0.3 ⁇ m, the appearance may be deteriorated, and when it is larger than 70 ⁇ m, the cost required for the raw material may be increased.
- the thickness of the first particle-containing layer is more preferably 1 to 60 ⁇ m, still more preferably 3 to 50 ⁇ m, and preferably about several times the average particle diameter of the contained particles.
- a 2nd particle content layer contains resin (B) and particle
- the resin (B) used for the second particle-containing layer can be selected from the same group as the resin (A) mentioned in the first particle-containing layer, but is not necessarily the same resin as the first particle-containing layer.
- the shape of the particles (B) used in the second particle-containing layer can be selected from the same group as the particles (A) mentioned in the first particle-containing layer, but is preferably spherical.
- the angle of the extracted light can be more easily concentrated in the front direction, and a surface light emitter that has a bright front direction can be obtained.
- the material of the particles (B) used for the second particle-containing layer can be selected from the same group as the particles (A) mentioned in the first particle-containing layer.
- the average particle size of the particles used in the second particle-containing layer is preferably 0.3 to 30 ⁇ m, more preferably 0.5 to 20 ⁇ m, and still more preferably 1.0 to 10 ⁇ m.
- the average particle diameter is smaller than 0.3 ⁇ m, the optical behavior due to the unevenness provided on the surface of the second particle-containing layer by the particles changes depending on the wavelength, and thus color misregistration may occur.
- the average particle diameter of the particles is larger than 30 ⁇ m, the appearance may be deteriorated.
- the average particle diameter of the particles used in the second particle-containing layer is larger than the average thickness of the second particle-containing layer described in the measurement method in the examples, and the surface of the second particle-containing layer is provided with irregularities due to the particles. It is preferable because it is easy.
- An average particle diameter here is a number average particle diameter, and shall mean the number average value of the particle diameter which describes a measuring method in an Example.
- the content of the particles used in the second particle-containing layer is 20 to 80% by mass, preferably 30 to 80% by mass, and more preferably 40 to 80% by mass.
- grain is a ratio of the mass of a particle
- the second particle-containing layer can contain additives such as a curing agent, a crosslinking agent, and an ultraviolet absorber.
- the second particle-containing layer preferably contains an ultraviolet absorber from the viewpoint of preventing deterioration of the base film and the light emitting element due to ultraviolet rays of external light.
- the second particle-containing layer contains an ultraviolet absorber and a light stabilizer.
- UV absorbers examples include organic UV absorbers such as benzophenone, benzotriazole, triazine, cyanoacrylate, salicylic acid, benzoate, and oxalic acid anilide, as well as titanium oxide, zinc oxide, cerium oxide, An inorganic ultraviolet absorber such as zirconium oxide can also be used.
- Salicylic acid compounds pt-butylphenyl salicylate, p-octylphenyl salicylate benzophenone compounds: 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-5-sulfobenzophenone, 2,2′-4,4′-tetrahydroxybenzophenone, 2,2′-dihydroxy-4-methoxybenzophenone, 2,2′-dihydroxy-4,4′-dimethoxybenzophenone, bis (2-methoxy-4-hydroxy) -5-benzoylphenyl) methanebenzotriazole compounds: 2- (2'-hydroxy-5'-methylphenyl) benzotriazole, 2- (2'-hydroxy-5'-t-butylphenyl) benzotriazole, 2- (2'-hydroxy-3 ', 5'-di- -Butylphenyl) benzotriazole, 2- (2'-(triazole) methanebenzotriazo
- ultraviolet absorbers absorb ultraviolet rays, they do not have the property of trapping organic radicals that are generated by exposure to ultraviolet rays, so degradation may occur due to organic radicals that are generated by exposure to ultraviolet rays. . In such a case, in order to capture organic radicals, it is preferable to use a light stabilizer in combination.
- Hindered amine compounds bis (2,2,6,6-tetramethyl-4-piperidyl) sebacate, dimethyl succinate 1- (2-hydroxyethyl) -4-hydroxy-2,2,6,6-tetramethyl Piperidine polycondensate benzoate series: 2,4-di-t-butylphenyl-3 ′, 5′-di-t-butyl-4′-hydroxybenzoate, 2,4-di-t-butylphenyl-3 ′, 5'-di-t-butyl-4'-hydroxybenzoate hindered phenol compounds: octadecyl-3- (3,5-di-t-butyl-4-hydroxyphenyl) propionate, N, N'-hexamethylenebis (3,5-di-t-butyl-4-hydroxynnamamide) Among these, hindered amine compounds are preferably used because of their high radical scavenging ability and little coloration.
- the above compounds can be used alone or in combination of two or more.
- the second particle-containing layer contains an ultraviolet absorber
- a) an aspect in which the coating material for the second particle-containing layer contains an ultraviolet absorber, and b) a skeleton of the resin (B) constituting the second particle-containing layer An embodiment using a resin containing an ultraviolet absorber therein, and c) an embodiment using particles containing an ultraviolet absorber as the particles (B) constituting the second particle-containing layer.
- the aspect of b) or c) is preferably used from the viewpoint of suppressing the bleeding out of the ultraviolet absorber.
- the second particle-containing layer has a relatively high content of particles (B) of 20 to 80% by mass, it is more preferable to use at least the aspect (c) from the viewpoint of enhancing the ultraviolet absorption efficiency. ) Is particularly preferred.
- the resin component constituting the resin (B) and the ultraviolet absorber are copolymerized.
- the resin obtained is used.
- the resin is preferably copolymerized with a light stabilizer.
- a resin for example, “HALS HYBRID” (registered trademark) series (manufactured by Nippon Shokubai Co., Ltd.) containing an acrylic monomer, a UV absorber, and a copolymer of a light stabilizer as active ingredients is preferably used.
- grains containing the ultraviolet absorber of (c) are obtained, for example by copolymerizing the ultraviolet absorber which has a reactive double bond, when manufacturing resin which comprises particle
- vinyl monomers such as acrylic and styrene are preferable. Since the styrene vinyl monomer has an aromatic ring, it is easily yellowed, and an acrylic vinyl monomer is most preferable in terms of light resistance.
- 2- (2′-hydroxy-5′-methacryloxyethylphenyl) -2H-benzotriazole ( ⁇ ⁇ ⁇ “RUVA” (registered trademark) -93) is a compound in which a reactive vinyl monomer is bonded to an ultraviolet absorber benzotriazole. ; Otsuka Chemical Co., Ltd.) can be used.
- a hindered amine compound that is a light stabilizer a reactive vinyl monomer is substituted, and 4-methacryloyloxy-2,2,6,6-tetramethylpiperidine (“Adekastab” (registered trademark) LA-82; ADEKA Co., Ltd.) can be used.
- the content of the ultraviolet absorber in the second particle-containing layer is preferably in the range of 0.1 to 30% by mass. If it is less than 0.1% by mass, the ultraviolet ray absorbing ability is not sufficient, and the life of the surface light emitter may be shortened. On the other hand, if it exceeds 30% by mass, absorption in the visible light region having a short wavelength cannot be ignored, resulting in a loss of light emission efficiency or insufficient strength of the second particle-containing layer.
- the content of the ultraviolet absorber in the second particle-containing layer is more preferably in the range of 0.5 to 10% by mass, and still more preferably in the range of 1 to 5% by mass.
- the content rate of an ultraviolet absorber here is the ratio of the mass of an ultraviolet absorber with respect to the total mass of the substance which comprises a 2nd particle content layer.
- the resin (B) is a resin containing an ultraviolet absorber or when the particles (B) are particles containing an ultraviolet absorber, the ultraviolet absorber contained in the resin (B) or the particles (B)
- the content mass ratio can be determined by analysis such as NMR.
- the thickness of the second particle-containing layer is not particularly limited, but is preferably 0.3 to 30 ⁇ m. When the thickness is smaller than 0.3 ⁇ m, the appearance may be deteriorated, and when it is larger than 30 ⁇ m, the cost required for the raw material may be increased.
- the thickness of the second particle-containing layer is more preferably 1 to 20 ⁇ m, still more preferably 3 to 10 ⁇ m, and is preferably about a fraction of the average particle diameter of the contained particles.
- the method for providing the first and second particle-containing layers according to the present invention is not particularly limited, and gravure coating, roll coating, die coating, spin coating, reverse coating, bar coating, screen coating, blade coating, air knife coating, and the like.
- Various coating methods such as dipping can be used.
- it can be applied at the time of production of the film used as the base layer (in-line coating), or can be applied by another process (off-line coating) after winding the film used as the base layer after film formation Good.
- the light-emitting element used in the present invention may have any light-transmitting substrate.
- an indium-tin oxide film hereinafter referred to as ITO
- ITO indium-tin oxide film
- An existing electrode in which a transparent electrode and a light emitting layer are provided and a reflective electrode (silver or aluminum is often used) is laminated may be used.
- a charge transport layer may be provided or a plurality of light emitting layers may be laminated.
- These elements are known to be deteriorated by water or oxygen, and the back surface and side surfaces are preferably sealed with a sealant.
- it is preferable to use the organic electroluminescent light emitting element whose light emitter used for a light emitting layer is an organic electroluminescent light emitter.
- the front film made of the material mentioned in the detailed description of the constituent members of the front film is disposed so that the first particle-containing layer 6 is in contact with the translucent substrate 5.
- a method of arranging the front film in such a case, (i) a method in which an adhesive is applied on the first particle-containing layer and bonded together, or (ii) a resin (A) when forming the first particle-containing layer
- the first particle-containing layer having adhesiveness on the surface by adjusting or selecting the glass transition temperature, molecular weight, cross-linking density, etc. described above, and directly adhering it to the translucent substrate can be mentioned.
- the latter is more preferable because the number of interfaces between layers that may cause loss due to reflection of light is small.
- the surface light emitter was turned on and allowed to stand for 30 minutes.
- the total luminous flux was measured using the viewing angle measuring device EZContrast (ELDIM Co., Ltd.) for the measurement.
- the ratio of each level was determined with the total luminous flux when the front film was not placed on the translucent substrate as 100%.
- the surface light emitter was a rotary microtome manufactured by Nippon Microtome Research Co., Ltd., and the surface light emitter at a knife inclination angle of 3 °. Cut in a direction perpendicular to the plane.
- the scanning electron microscope ABT-32 manufactured by Topcon Co., Ltd. the resulting cross section is appropriately adjusted at an observation magnification of 2500 to 10,000 times and an image contrast so that the film layer is projected in the field of view.
- the particle shape of the first and second particle-containing layers was observed.
- the thickness of the layer at a point that divides the width of the image into 20 parts is calculated, The arithmetic average value of 21 places including both ends was obtained. This operation was performed at five observation locations at the same magnification, and the average value was defined as the average thickness of the particle-containing layer.
- the average particle diameter was determined from images observed from the surfaces of the first and second particle-containing layers using a laser microscope VK-8700 (manufactured by Keyence Corporation). The image is divided into 11 equal parts vertically and horizontally, a straight line is drawn in the shape of a grid, and the average value of the particle diameters measured from two orthogonal directions of the particles is shown for each of the particles closest to each of the 100 intersections of the straight lines. The particle diameter of the particles was used, and the arithmetic average value was defined as the number average particle diameter. In addition, for the intersection where the closest particles become the same particle, one is excluded from the target, and when the target particle is less than 80, until the number of particles to be measured is 80 or more, An observation image was added.
- Refractive Index Measurement Method After extracting the resin from the particle-containing layer using an organic solvent and distilling off the organic solvent, the measurement was performed with respect to light having a wavelength of 589.3 nm at 25 ° C. by ellipsometry. . The value obtained here was defined as “resin refractive index”. Next, after immersing the particle-containing layer in an organic solvent and peeling and collecting the coating layer, the particles are dropped from the coating layer by pressing and sliding on a slide glass, and then the particles are collected until the total particle amount becomes 10 g. Collected. Using the Becke line detection method, it was confirmed that the outline of the particles became invisible at a temperature at which the refractive index of each liquid organic compound was known. Refractive index ".
- a white organic EL light emitting panel standard panel (Lumiotech Co., Ltd., light emitting area size: 145 mm ⁇ 145 mm) (hereinafter referred to as “light emitting panel A”) was used.
- a PET film “Lumirror” (registered trademark) T60 (manufactured by Toray Industries, Inc.) having a thickness of 125 ⁇ m was used as the base film.
- Example 1 Acrylic resin “Acridic” (registered trademark) A-165 (DIC Corporation, 45% concentration solution) 9.0 g and toluene 9.0 g, Melamine resin / silica composite particle “Optobeads” (registered trademark) 2000M Coating agent A was prepared by mixing 0.5 g (manufactured by Nissan Chemical Industries, Ltd., number average particle size: 2.0 ⁇ m).
- the refractive index of the resin (A) of the first particle-containing layer produced using the coating agent A is 1.50, the refractive index of the particles (A) is 1.65, and the difference in refractive index is 0.15. there were.
- Acrylic resin “Acridic” (registered trademark) A-165 (manufactured by DIC Co., Ltd., 9.0 g, 45 mass% solution) 9.0 g and toluene 15.0 g, crosslinked polymethyl methacrylate particles “TECHPOLYMER” (registered trademark) MBX series MBX-5 (manufactured by Sekisui Plastics Co., Ltd., number average particle size: 5.0 ⁇ m) was mixed with 6.0 g to prepare a coating agent B. Coating A was applied to one surface of the substrate film using Metabar # 16, and heated and dried at 120 ° C. for 1 minute to form a first particle-containing layer.
- Coating B was applied to the opposite surface of the base film using wire bar # 16 and heated and dried at 120 ° C. for 1 minute to form a second particle-containing layer.
- an acrylic pressure-sensitive adhesive TD43A manufactured by Yodogawa Paper Co., Ltd.
- the first particle-containing layer of the front film and the light-emitting panel A are bonded so as not to bite air, and 2 kg / 25 mm.
- the rubber roller was reciprocated once and pressed to produce a pseudo sample of the surface light emitter.
- Example 2 Acrylic adhesive “SK Dyne” (registered trademark) 811L (manufactured by Soken Chemical Co., Ltd., concentration 23% by mass solution) 100.0 g, isocyanate curing agent “D-90” (manufactured by Soken Chemical Co., Ltd., concentration 90)
- a coating agent C was prepared by mixing 1.5 g of a mass% solution) and 2.9 g of epoxy particles “Trepal” (registered trademark) EP-B (manufactured by Toray Industries, Inc., number average particle diameter 5.5 ⁇ m).
- the refractive index of the resin (A) of the first particle-containing layer prepared using the coating agent C is 1.51, the refractive index of the particles (A) is 1.59, and the difference in refractive index is 0.08. there were.
- the coating material B was applied on one surface of the base film using Metabar # 12, and then heated and dried at 120 ° C. for 1 minute to form a second particle-containing layer.
- a first particle-containing layer having adhesiveness is formed by applying the coating agent C at a coating thickness of 100 ⁇ m before drying using an applicator and then heating and drying at 100 ° C. for 2 minutes.
- a film was prepared.
- the first particle-containing layer of the front film and the light emitting panel A are bonded so that air does not get caught, and a rubber roller is reciprocated once under a pressure condition of 2 kg / 25 mm to make a pseudo sample of a surface light emitter. did.
- Coating solution D was prepared by mixing 2.7 g of epoxy solution “Trepearl” (registered trademark) EP-B (manufactured by Toray Industries, Inc., number average particle size 5.5 ⁇ m).
- the refractive index of the resin (A) is 1.51
- the refractive index of the particles (A) is 1.59
- the difference in refractive index is 0.08.
- the coating material B was applied on one surface of the base film using Metabar # 12, and then heated and dried at 120 ° C. for 1 minute to form a second particle-containing layer.
- On the opposite surface of the base film after applying the coating D with a coating thickness of 100 ⁇ m before drying using an applicator, heat-dried at 100 ° C. for 2 minutes to form a first particle-containing layer having adhesiveness.
- a film was prepared.
- the first particle-containing layer of the front film and the light emitting panel A are bonded so that air does not get caught, and a rubber roller is reciprocated once under a pressure condition of 2 kg / 25 mm to make a pseudo sample of a surface light emitter. did.
- Example 4 A benzotriazole-containing acrylic copolymer resin “Hals Hybrid” (registered trademark) UV-G720T (manufactured by Nippon Shokubai Co., Ltd., concentration 40% by mass solution) 10.0 g, ethyl acetate 14.0 g, and the following particles 1.0 g Coating E was prepared by mixing.
- Particles were produced by the following method.
- the dispersion was cooled to room temperature.
- the dispersion was filtered using a mesh filter having an opening of 40 ⁇ m to remove aggregates and the like.
- the obtained dispersion had no aggregates and the filterability of this dispersion was very good.
- the average particle size of the particles dispersed in the dispersion thus filtered was 6.4 ⁇ m, and this shape was spherical.
- the particle dispersion was filtered to separate the particles and the dispersion medium, and the separated particles were dried.
- the coating material E was applied on one surface of the base film using Metabar # 12, and then heated and dried at 120 ° C. for 1 minute to form a second particle-containing layer.
- a first particle-containing layer having adhesiveness is formed by applying the coating agent C at a coating thickness of 100 ⁇ m before drying using an applicator and then heating and drying at 100 ° C. for 2 minutes.
- a film was prepared. The first particle-containing layer of the front film and the light emitting panel A are bonded so that air does not get caught, and a rubber roller is reciprocated once under a pressure condition of 2 kg / 25 mm to make a pseudo sample of a surface light emitter. did.
- the coating material B was apply
- acrylic pressure-sensitive adhesive TD43A manufactured by Yodogawa Paper Co., Ltd.
- the opposite surface of the second particle-containing layer of the front film and the light-emitting panel A are bonded so as not to bite air
- a rubber roller was reciprocated once under a pressure condition of 2 kg / 25 mm and pressed to prepare a pseudo sample of a surface light emitter.
- the first particle-containing layer was formed on one surface of the base film by applying the coating agent C with an application thickness of 100 ⁇ m before drying using an applicator and then heating and drying at 100 ° C. for 2 minutes.
- the first particle-containing layer of the front film and the light emitting panel A are bonded so that air does not get caught, and a rubber roller is reciprocated once under a pressure condition of 2 kg / 25 mm to make a pseudo sample of a surface light emitter. did.
- Table 1 shows the evaluation results of the above examples and comparative examples.
Abstract
Description
1.片面に透光性基板を有する発光素子の該透光性基板の側に、基材フィルムの両面に粒子を含む樹脂層を有する少なくとも3層構成の前面フィルムが接して配置された面発光体であって、前記前面フィルムの入光側に位置する樹脂層(第1粒子含有層)が粒子を1~50質量%含有し、前記前面フィルムの出光側に位置する樹脂層(第2粒子含有層)が粒子を20~80質量%含有することを特徴とする面発光体。
2.前記第1粒子含有層を構成する樹脂と粒子の屈折率の差が0.05~0.5である、上記1に記載の面発光体。
3.前記第1粒子含有層と透光性基板との間の剥離強度が0.5N/25mm以上である、上記1または2に記載の面発光体。
4.前記第2粒子含有層が紫外線吸収剤を含有する、上記1~3のいずれかに記載の面発光体。
5.前記第2粒子含有層における樹脂が紫外線吸収剤を含有する樹脂である、上記1~4のいずれかに記載の面発光体。
6.前記第2粒子含有層における粒子が紫外線吸収剤を含有する粒子である、上記1~5のいずれかに記載の面発光体。
7.前記面発光体に用いられる発光素子が有機エレクトロルミネセンス発光素子である、上記1~6のいずれかに記載の面発光体。
8.上記1~6のいずれかに記載の面発光体に用いられる前面フィルム。
以下、前面フィルムの部分の構成部材について詳細に説明する。
基材フィルムとして用いられる材料は特に制限されないが、供給性やハンドリング性の観点からプラスチックフィルムが好ましく用いられる。プラスチックフィルムの材料としてはポリオレフィン系、ポリエステル系、ポリカーボネート系、ポリエーテル系、ポリアミド系、ポリイミド系、ポリアクリル等が挙げられる。中でもポリエステル系のフィルムが耐久性等の観点から好ましく用いられ、ポリエチレンテレフタレート(以下PETという)が供給性にも優れていることから、特に好ましく用いられる。
第1粒子含有層は、樹脂(A)中に、粒子(A)を含む。
第1粒子含有層に用いる樹脂(A)としては、特に限定されないが、有機成分を主成分とする樹脂が好ましく、例えばポリエステル樹脂、ポリウレタン樹脂、アクリル樹脂、メタクリル樹脂、ポリアミド樹脂、ポリエチレン樹脂、ポリプロピレン樹脂、ポリ塩化ビニル樹脂、ポリ塩化ビニリデン樹脂、ポリスチレン樹脂、ポリ酢酸ビニル樹脂、フッ素系樹脂、エポキシ樹脂、シリコーン系樹脂などを挙げることができる。ここで、有機成分を主成分とする樹脂とは、第1粒子含有層に用いる樹脂(A)中に有機成分が60質量%以上含まれる樹脂をいい、有機成分が80質量%以上含まれる樹脂であればより好ましい(以下、「主成分」については同様の定義とする)。これらの樹脂は単独で用いてもよく、あるいは2種以上の共重合体もしくは混合物としたものを用いてもよい。中でもポリエステル樹脂、ポリウレタン樹脂、アクリル樹脂または、メタクリル樹脂が耐熱性、外観、粒子分散性が優れる点から好ましく使用される。
第2粒子含有層は、樹脂(B)および粒子(B)を含む。
第2粒子含有層に用いる樹脂(B)は、第1粒子含有層で挙げた樹脂(A)と同様の群から選択できるが、必ずしも第1粒子含有層と同一の樹脂である必要はない。
サリチル酸系化合物:p-t-ブチルフェニルサリシレート、p-オクチルフェニルサリシレート
ベンゾフェノン系化合物:2,4-ジヒドロキシベンゾフェノン、2-ヒドロキシ-4-メトキシベンゾフェノン、2-ヒドロキシ-4-メトキシ-5-スルホベンゾフェノン、2,2’-4,4’-テトラヒドロキシベンゾフェノン、2,2’-ジヒドロキシ-4-メトキシベンゾフェノン、2,2’-ジヒドロキシ-4,4’-ジメトキシベンゾフェノン、ビス(2-メトキシ-4-ヒドロキシ-5-ベンゾイルフェニル)メタン
ベンゾトリアゾール系化合物:2-(2’-ヒドロキシ-5’-メチルフェニル)ベンゾトリアゾール、2-(2’-ヒドロキシ-5’-t-ブチルフェニル)ベンゾトリアゾール、2-(2’-ヒドロキシ-3’,5’-ジ-t-ブチルフェニル)ベンゾトリアゾール、2-(2’-ヒドロキシ-3’-t-ブチル-5’-メチルフェニル)-5-クロロベンゾトリアゾール、2-(2’-ヒドロキシ-3’,5’-ジ・t-ブチルフェニル)-5-クロロベンゾトリアゾール、2-(2’-ヒドロキシ-5’-t-オクチルフェノール)ベンゾトリアゾール、2-(2’-ヒドロキシ-3’,5’-ジ・t-アミルフェニル)ベンゾトリアゾール、2,2’-メチレンビス[4-(1,1,3,3-テトラメチルブチル)-6-(2H-ベンゾトリアゾール-2-イル)フェノール]、2(2’ヒドロキシ-5’-メタアクリロキシフェニル)-2H-ベンゾトリアゾール、2-[2’-ヒドロキシ-3’-(3”,4”,5”,6”-テトラヒドロフタルイミドメチル)-5’-メチルフェニル]ベンゾトリアゾール
シアノアクリレート系化合物:エチル-2-シアノ-3,3’-ジフェニルアクリレート
上記以外の化合物:2-エトキシ-2’-エチルオキザックアシッドビスアニリド、2-(4,6-ジフェニル-1,3,5-トリアジン-2-イル)-5-[(ヘキシル)オキシ]-フェノール
上記の化合物は、単独でも使用してもよいし、2種類以上を併用してもよい。
ヒンダードアミン系化合物:ビス(2,2,6,6-テトラメチル-4-ピペリジル)セバケート、コハク酸ジメチル・1-(2-ヒドロキシエチル)-4-ヒドロキシ-2,2,6,6-テトラメチルピペリジン重縮合物
ベンゾエート系:2,4-ジ-t-ブチルフェニル-3’,5’-ジ・t-ブチル-4’-ヒドロキシベンゾエート、2,4-ジ・t-ブチルフェニル-3’,5’-ジ・t-ブチル-4’-ハイドロキシベンゾエート
ヒンダードフェノール系化合物:オクタデシル-3-(3,5-ジ-t-ブチル-4-ヒドロキシフェニル)プロピオネート、N,N’-ヘキサメチレンビス(3,5-ジ-t-ブチル-4-ヒドロキシンナマミド)
これらの中でもヒンダードアミン系化合物が、ラジカル捕捉能が高く、着色が少ないため好適に使用される。
なお、樹脂(B)が紫外線吸収剤を含有する樹脂である場合あるいは粒子(B)が紫外線吸収剤を含有する粒子である場合、樹脂(B)あるいは粒子(B)に含有する紫外線吸収剤の含有質量比はNMR等の分析により求めることができる。
本発明に使用する発光素子は、透光性基板を有するものであればよく、例えば、ガラス、高分子フィルムなどの透光性基板上に、インジウム-錫酸化物膜(以下、ITO)等からなる透明電極と、発光層とが設けられ、さらに反射性を有する電極(銀やアルミニウムが用いられることが多い)が積層されてなる既存のものを用いればよい。また、必要に応じて、電荷輸送層が設けられたり、複数の発光層を積層したりしてもよい。これらの素子は水や酸素により劣化することが知られており、背面や側面も封止剤により封止されることが好ましい。本発明においては、発光層に用いられる発光体が有機エレクトロルミネセンス発光体である有機エレクトロルミネセンス発光素子を用いることが好ましい。
本発明における面発光体の製造方法は、特に限定されないが、以下のような方法が挙げられる。
本実施例における測定方法及び評価方法は下記の通りである。特に断らない限り、n数は1で評価を行った。
面発光体を点灯させ、30分静置した後に測定を実施した。測定には視野角測定機EZContrast(ELDIM(株)製)を用い、全光束を測定した。透光性基板上に前面フィルムを設置しないときの全光束を100%として、各水準の比率を求めた。
面発光体を点灯させ、30分静置した後に評価を実施した。各水準のサンプルを、サンプル面に対して法線方向を0度として、0~60度の範囲で目視確認し、色ずれの程度を5段階評価した。
1 前面フィルム無しの面発光体と同程度の色ずれが視認される
2 1と3の間(1より改善はされているが、実用上問題あり)
3 色ずれが視認されるが実用上問題ないぎりぎりのレベル
4 3と5の間
5 色ずれが視認されない。
面発光体を日本ミクロトーム研究所(株)製ロータリー式ミクロトームにて、ナイフ傾斜角度3°にて面発光体平面に垂直な方向に切断した。得られた断面を、(株)トプコン製走査型電子顕微鏡ABT-32を用いて、フィルム層が視野領域に映し出されるように、観察倍率2500~10000倍にて、また、画像のコントラストを適宜調節しながら、第1、第2粒子含有層の粒子形状を観察した。また、同じ断面観察画像を用いてその画像の幅を20等分する点での層の厚み(当該点で粒子や突起が含まれている場合には粒子の厚さを含む)を算出し、両端を含めた21箇所の算術平均値を求めた。この作業を同一倍率で5箇所の観察箇所について実施し、その平均値を粒子含有層の平均厚みとした。
平均粒子径は、レーザーマイクロスコープVK-8700((株)キーエンス製)を用い、第1、第2粒子含有層の表面からの観察画像から求めた。画像を縦横11等分して、方眼状に直線を引き、直線の各交点100点に最も近くに存在する粒子について、それらの粒子の直交する2方向から測定した粒子径の平均値を各々の粒子の粒子径とし、これらの算術平均値を数平均粒子径とした。なお、最も近くに存在する粒子が同一の粒子となる交点については一方を対象から外し、対象となる粒子が80個に満たない場合には、測定対象となる粒子が80個以上となるまで、観察画像を追加した。
粒子含有層から有機溶剤を用いて樹脂を抽出し、有機溶剤を留去した後、エリプソメトリー法によって、25℃における589.3nmの波長の光に関して測定を行った。ここで得られた値を「樹脂の屈折率」とした。
次いで、粒子含有層を有機溶剤に浸漬して、塗布層を剥離採取した後、スライドガラスに圧着・摺動することで粒子を塗布層から脱落させた後、粒子総量が10gになるまで粒子を採取した。採取した粒子をベッケ線検出法により、各液体有機系化合物の屈折率既知の温度に於いて、粒子の輪郭が見えなくなることを確認し、このとき用いた液体有機系化合物の屈折率を「粒子の屈折率」とした。
面発光体の前面フィルムを幅25mmに切断し、測定用サンプルを作製した。この測定用サンプルを温度23℃、相対湿度50%の雰囲気下で30分保管後、同雰囲気下で、引張試験機(例えば、(株)オリエンテック製の「テンシロンRTM-100」)用い、JIS-Z0237(2000)に準じて引張速度300mm/分で180度剥離した際の剥離強度を測定した。
アクリル樹脂“アクリディック”(登録商標)A-165(DIC(株)製、濃度45質量%溶液)9.0gとトルエン9.0g、メラミン樹脂・シリカ複合粒子“オプトビーズ”(登録商標)2000M(日産化学工業(株)製、数平均粒子径2.0μm)0.5gを混合することで塗剤Aを調製した。塗剤Aを用いて作製した第1粒子含有層の、樹脂(A)の屈折率は1.50、粒子(A)の屈折率は1.65であり、屈折率の差は0.15であった。
アクリル樹脂“アクリディック”(登録商標)A-165(DIC(株)製、濃度45質量%溶液)9.0gとトルエン15.0g、架橋ポリメタクリル酸メチル粒子“TECHPOLYMER”(登録商標)MBXシリーズ、MBX-5(積水化成品工業(株)製、数平均粒子径5.0μm)6.0gを混合することで塗剤Bを調製した。基材フィルムの一面に塗剤Aをメタバー#16を使用して塗布し、120℃で1分間加熱乾燥させ第1粒子含有層を形成した。基材フィルムの反対面には塗剤Bをワイヤーバー#16を使用して塗布し、120℃で1分間加熱乾燥させ第2粒子含有層を形成した。粘着剤としてアクリル系粘着剤TD43A((株)巴川製紙所製)を使用して、前面フィルムの第1粒子含有層と発光パネルAとを空気を噛み込まないように貼合し、2kg/25mmの加圧条件でゴムローラを1往復させて圧着し、面発光体の疑似サンプルを作製した。
アクリル系粘着剤“SKダイン” (登録商標)811L(総研化学(株)製、濃度23質量%溶液)100.0g、イソシアネート系硬化剤“D-90”(総研化学(株)製、濃度90質量%溶液)1.5g、エポキシ粒子“トレパール” (登録商標)EP-B(東レ(株)製、数平均粒子径5.5μm)2.9gを混合することで塗剤Cを調製した。塗剤Cを用いて作製した第1粒子含有層の、樹脂(A)の屈折率は1.51、粒子(A)の屈折率は1.59であり、屈折率の差は0.08であった。
基材フィルムの一面に、塗剤Bをメタバー#12を使用して塗布後、120℃で1分間加熱乾燥させ第2粒子含有層を形成した。基材フィルムの反対面には、アプリケーターを使用して乾燥前塗布厚み100μmで塗剤Cを塗布後、100℃で2分間加熱乾燥させて粘着性を有する第1粒子含有層を形成し、前面フィルムを作製した。前面フィルムの第1粒子含有層と発光パネルAとを空気を噛み込まないように貼合し、2kg/25mmの加圧条件でゴムローラを1往復させて圧着し、面発光体の疑似サンプルを作製した。
アクリル系粘着剤“オリバイン” (登録商標)EG-655(東洋インキ(株)製、濃度21質量%溶液)109.5g、イソシアネート系硬化剤“BXX5627”(東洋インキ(株)製、濃度50質量%溶液)2.7g、エポキシ粒子“トレパール” (登録商標)EP-B(東レ(株)製、数平均粒子径5.5μm)2.9gを混合することで塗剤Dを調製した。塗剤Dを用いて作製した第1粒子含有層の、樹脂(A)の屈折率は1.51、粒子(A)の屈折率は1.59であり、屈折率の差は0.08であった。
基材フィルムの一面に、塗剤Bをメタバー#12を使用して塗布後、120℃で1分間加熱乾燥させ第2粒子含有層を形成した。基材フィルムの反対面には、アプリケーターを使用して乾燥前塗布厚み100μmで塗剤Dを塗布後、100℃で2分間加熱乾燥させて粘着性を有する第1粒子含有層を形成し、前面フィルムを作製した。前面フィルムの第1粒子含有層と発光パネルAとを空気を噛み込まないように貼合し、2kg/25mmの加圧条件でゴムローラを1往復させて圧着し、面発光体の疑似サンプルを作製した。
ベンゾトリアゾール含有アクリル系共重合体樹脂“ハルスハイブリッド”(登録商標)UV-G720T((株)日本触媒製、濃度40質量%溶液)10.0gと酢酸エチル14.0g、下記粒子1.0gを混合することで塗剤Eを調製した。
基材フィルムの一面に、塗剤Bをメタバー#12を使用して塗布し、120℃で1分間加熱乾燥させ第2粒子含有層を形成した。粘着剤としてアクリル系粘着剤TD43A((株)巴川製紙所製)を使用して、前面フィルムの第2粒子含有層の反対面と発光パネルAとを空気を噛み込まないように貼合し、2kg/25mmの加圧条件でゴムローラを1往復させて圧着し、面発光体の疑似サンプルを作製した。
基材フィルムの一面に、アプリケーターを使用して乾燥前塗布厚み100μmで塗剤Cを塗布後、100℃で2分間加熱乾燥させて第1粒子含有層を形成した。前面フィルムの第1粒子含有層と発光パネルAとを空気を噛み込まないように貼合し、2kg/25mmの加圧条件でゴムローラを1往復させて圧着し、面発光体の疑似サンプルを作製した。
2 発光素子
3 前面フィルム
4 発光層
5 透光性基板
6 第1粒子含有層
7 基材フィルム
8 第2粒子含有層
9 封止層
10 背面電極
11 発光体
12 透明電極
13 樹脂(A)
14 粒子(A)
15 樹脂(B)
16 粒子(B)
Claims (8)
- 片面に透光性基板を有する発光素子の該透光性基板の側に、基材フィルムの両面に粒子を含む樹脂層を有する少なくとも3層構成の前面フィルムが接して配置された面発光体であって、前記前面フィルムの入光側に位置する樹脂層(第1粒子含有層)が粒子を1~50質量%含有し、前記前面フィルムの出光側に位置する樹脂層(第2粒子含有層)が粒子を20~80質量%含有することを特徴とする面発光体。
- 前記第1粒子含有層を構成する樹脂と粒子の屈折率の差が0.05~0.5である、請求項1に記載の面発光体。
- 前記第1粒子含有層と透光性基板との間の剥離強度が0.5N/25mm以上である、請求項1または2に記載の面発光体。
- 前記第2粒子含有層が紫外線吸収剤を含有する、請求項1~3のいずれかに記載の面発光体。
- 前記第2粒子含有層における樹脂が紫外線吸収剤を含有する樹脂である、請求項1~4のいずれかに記載の面発光体。
- 前記第2粒子含有層における粒子が紫外線吸収剤を含有する粒子である、請求項1~5のいずれかに記載の面発光体。
- 前記面発光体に用いられる発光素子が有機エレクトロルミネセンス発光素子である、請求項1~6のいずれかに記載の面発光体。
- 請求項1~6のいずれかの面発光体に用いられる前面フィルム。
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JP2013513309A JP6156143B2 (ja) | 2011-12-15 | 2012-12-05 | 面発光体 |
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JP2015159033A (ja) * | 2014-02-24 | 2015-09-03 | 三菱レイヨン株式会社 | 光取り出しフィルム、面発光体及び光取り出しフィルムの製造方法 |
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KR101642120B1 (ko) * | 2014-12-24 | 2016-07-22 | 코닝정밀소재 주식회사 | 유기발광소자용 광추출 기판 제조방법, 유기발광소자용 광추출 기판 및 이를 포함하는 유기발광소자 |
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CN106450026A (zh) * | 2016-10-17 | 2017-02-22 | 深圳市华星光电技术有限公司 | Oled显示器及其制作方法 |
CN109065755B (zh) * | 2018-08-03 | 2019-12-31 | 武汉华星光电半导体显示技术有限公司 | 显示面板及封装构件 |
US10651421B2 (en) | 2018-08-03 | 2020-05-12 | Wuhan China Star Optoelectronics Semiconductor Display Technology Co. Ltd. | Display panel and encapsulation component |
CN109841758B (zh) | 2019-03-29 | 2021-01-26 | 京东方科技集团股份有限公司 | 显示面板及其制造方法、显示装置 |
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TW201332178A (zh) | 2013-08-01 |
EP2793531A1 (en) | 2014-10-22 |
US20140320000A1 (en) | 2014-10-30 |
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CN103975647A (zh) | 2014-08-06 |
US9237630B2 (en) | 2016-01-12 |
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JP6156143B2 (ja) | 2017-07-05 |
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