WO2016104592A1 - ディスプレイ装置、合わせガラス用中間膜及び合わせガラス - Google Patents
ディスプレイ装置、合わせガラス用中間膜及び合わせガラス Download PDFInfo
- Publication number
- WO2016104592A1 WO2016104592A1 PCT/JP2015/086005 JP2015086005W WO2016104592A1 WO 2016104592 A1 WO2016104592 A1 WO 2016104592A1 JP 2015086005 W JP2015086005 W JP 2015086005W WO 2016104592 A1 WO2016104592 A1 WO 2016104592A1
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- WO
- WIPO (PCT)
- Prior art keywords
- laminated glass
- light
- interlayer film
- display device
- light emitting
- Prior art date
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10651—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer comprising colorants, e.g. dyes or pigments
- B32B17/10669—Luminescent agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
- B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10165—Functional features of the laminated safety glass or glazing
- B32B17/10541—Functional features of the laminated safety glass or glazing comprising a light source or a light guide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10559—Shape of the cross-section
- B32B17/10568—Shape of the cross-section varying in thickness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10688—Adjustment of the adherence to the glass layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60J—WINDOWS, WINDSCREENS, NON-FIXED ROOFS, DOORS, OR SIMILAR DEVICES FOR VEHICLES; REMOVABLE EXTERNAL PROTECTIVE COVERINGS SPECIALLY ADAPTED FOR VEHICLES
- B60J1/00—Windows; Windscreens; Accessories therefor
- B60J1/02—Windows; Windscreens; Accessories therefor arranged at the vehicle front, e.g. structure of the glazing, mounting of the glazing
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
- G02B27/01—Head-up displays
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02321—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment introduction of substances into an already existing insulating layer
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
-
- 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
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
-
- 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
- H10K85/114—Poly-phenylenevinylene; Derivatives thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/206—Organic displays, e.g. OLED
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
- B32B2605/006—Transparent parts other than made from inorganic glass, e.g. polycarbonate glazings
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
- H10K2102/301—Details of OLEDs
- H10K2102/302—Details of OLEDs of OLED structures
- H10K2102/3023—Direction of light emission
- H10K2102/3026—Top emission
Definitions
- the present invention relates to a display device, an interlayer film for laminated glass, and a laminated glass that can obtain a predetermined initial luminance even when irradiated with a low-intensity light beam.
- Laminated glass is safe because it does not scatter glass fragments even if it is damaged by an external impact, so it can be used as a windshield, side glass, rear glass for vehicles such as automobiles, and window glass for aircraft, buildings, etc. Widely used.
- the laminated glass include a laminated glass obtained by integrating an interlayer film for laminated glass including a liquid plasticizer and a polyvinyl acetal resin between at least a pair of glasses.
- HUD head-up display
- Patent Document 2 the applicant of the present application is for a laminated glass having a light emitting layer containing a binder resin and at least one light emitting material selected from the group consisting of a light emitting particle, a light emitting pigment, and a light emitting dye.
- An interlayer film has been disclosed.
- Luminescent materials such as luminescent particles, luminescent pigments, and luminescent dyes have the property of emitting light when irradiated with light of a specific wavelength.
- An object of this invention is to provide the display apparatus from which the predetermined
- the present invention is a display device having a laminated glass in which an interlayer film for laminated glass containing a thermoplastic resin and a light emitting material is laminated between a pair of glass plates, and an irradiation device for irradiating the laminated glass with light.
- the display device emits light with a luminance of 1 cd / m 2 or more when the output of the light emitted from the irradiation device is 1 mW or less and the laminated glass is irradiated with the light.
- the present invention is described in detail below.
- the present inventors examined a display device that can obtain a predetermined initial luminance even when irradiated with a low-intensity light beam. As a result, it has been found that by using a low-intensity light beam with an output of 1 mW or less, a predetermined initial luminance can be obtained and a safe display device can be obtained, and the present invention has been completed.
- the display device of the present invention is particularly suitable for night vision because a predetermined initial luminance can be obtained even when a low-intensity light beam is irradiated.
- the display device of the present invention includes a laminated glass and an irradiation device that irradiates the laminated glass with light.
- the laminated glass is obtained by laminating an interlayer film for laminated glass containing a thermoplastic resin and a light emitting material between two glass plates.
- thermoplastic resin is not particularly limited.
- polyvinyl acetal resin ethylene-vinyl acetate copolymer resin, ethylene-acrylic copolymer resin, polyurethane resin, polyurethane resin containing sulfur element, polyvinyl alcohol resin, vinyl chloride.
- resins and polyethylene terephthalate resins include resins and polyethylene terephthalate resins.
- a polyvinyl acetal resin is preferable.
- the polyvinyl acetal is not particularly limited as long as it is a polyvinyl acetal obtained by acetalizing polyvinyl alcohol with an aldehyde, but polyvinyl butyral is preferable. Moreover, you may use together 2 or more types of polyvinyl acetal as needed.
- the preferable lower limit of the degree of acetalization of the polyvinyl acetal is 40 mol%, the preferable upper limit is 85 mol%, the more preferable lower limit is 60 mol%, and the more preferable upper limit is 75 mol%.
- the polyvinyl acetal has a preferred lower limit of the hydroxyl group content of 15 mol% and a preferred upper limit of 35 mol%.
- the hydroxyl group amount is 15 mol% or more, the interlayer film for laminated glass can be easily molded.
- the amount of hydroxyl group is 35 mol% or less, handling of the resulting interlayer film for laminated glass becomes easy.
- the degree of acetalization and the amount of hydroxyl groups can be measured in accordance with, for example, JIS K6728 “Testing method for polyvinyl butyral”.
- the polyvinyl acetal can be prepared by acetalizing polyvinyl alcohol with an aldehyde.
- the polyvinyl alcohol is usually obtained by saponifying polyvinyl acetate, and polyvinyl alcohol having a saponification degree of 70 to 99.8 mol% is generally used.
- the preferable lower limit of the polymerization degree of the polyvinyl alcohol is 500, and the preferable upper limit is 4000.
- the polymerization degree of the polyvinyl alcohol is 500 or more, the penetration resistance of the obtained laminated glass is increased.
- the polymerization degree of the polyvinyl alcohol is 4000 or less, the interlayer film for laminated glass can be easily molded.
- the minimum with a more preferable polymerization degree of the said polyvinyl alcohol is 1000, and a more preferable upper limit is 3600.
- the aldehyde is not particularly limited, but generally an aldehyde having 1 to 10 carbon atoms is preferably used.
- the aldehyde having 1 to 10 carbon atoms is not particularly limited.
- n-butyraldehyde, n-hexylaldehyde, and n-valeraldehyde are preferable, and n-butyraldehyde is more preferable.
- These aldehydes may be used alone or in combination of two or more.
- Examples of the light emitting material include lanthanoid complexes having a multidentate ligand containing a halogen atom.
- a lanthanoid complex having a polydentate ligand containing a halogen atom emits light with high emission intensity when irradiated with light.
- Examples of the lanthanoid complex having a polydentate ligand containing a halogen atom include a lanthanoid complex having a bidentate ligand containing a halogen atom, a lanthanoid complex having a tridentate ligand containing a halogen atom, and a tetradentate containing a halogen atom.
- Examples include lanthanoid complexes having a ligand, lanthanoid complexes having a pentadentate ligand containing a halogen atom, and lanthanoid complexes having a hexadentate ligand containing a halogen atom.
- a lanthanoid complex having a bidentate ligand containing a halogen atom or a lanthanoid complex having a tridentate ligand containing a halogen atom has a wavelength of 580 to 780 nm when irradiated with light having a wavelength of 300 to 410 nm.
- Light with extremely high emission intensity Since this light emission is extremely high in intensity, an interlayer film for laminated glass having a light-emitting layer containing the light emission has a power of 1.3 to 165 cd / m 2 even when irradiated with a low-intensity light whose output is 1 mW or less. Light can be emitted with brightness.
- the interlayer film for laminated glass is used, display with sufficient contrast is possible, and even if the light transmitted through the interlayer film for laminated glass is directly observed by a person, the eyes are not dazzled.
- the lanthanoid complex having a bidentate ligand containing a halogen atom or the lanthanoid complex having a tridentate ligand containing a halogen atom is also excellent in heat resistance.
- the windshield is often used in a high temperature environment by being irradiated with infrared rays of sunlight. In such a high temperature environment, the light emitting material may be deteriorated, and the luminance may be significantly lowered particularly at the edge of the laminated glass.
- the luminance of the laminated glass is less likely to change even in a high temperature environment.
- An intermediate film can be obtained.
- An interlayer film for laminated glass that emits light with a luminance of 1.3 to 165 cd / m 2 is also one aspect of the present invention.
- a laminated glass that emits light with a luminance of 1.3 to 165 cd / m 2 when irradiated with a light beam with an output of 1 mW or less is not too bright when the driver observes it even at dark nights. In addition, an image with high visibility that is not too dark can be obtained, which is particularly suitable for night vision applications.
- a laminated glass in which the interlayer film for laminated glass is laminated between a pair of glass plates is also one aspect of the present invention.
- the luminance of light emitted from the interlayer film for laminated glass is obtained by, for example, creating a laminated glass by sandwiching the interlayer film for laminated glass of the present invention between two clear glasses having a thickness of 2.5 mm. It can be measured by a method of measuring luminance. More specifically, a light source (for example, a High Power xenon light source (for example, “REX-250” manufactured by Asahi Spectroscopic Co., Ltd., irradiation) disposed at a position 10 cm away from the surface of the laminated glass in a dark room under a dark room.
- a light source for example, a High Power xenon light source (for example, “REX-250” manufactured by Asahi Spectroscopic Co., Ltd., irradiation) disposed at a position 10 cm away from the surface of the laminated glass in a dark room under a dark room.
- the lanthanoid includes lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium or lutetium. Since higher emission intensity can be obtained, the lanthanoid is preferably neodymium, europium or terbium, more preferably europium or terbium, and still more preferably europium.
- Examples of the lanthanoid complex having a bidentate ligand containing a halogen atom include tris (trifluoroacetylacetone) phenanthroline europium, tris (trifluoroacetylacetone) diphenylphenanthroline europium, tris (hexafluoroacetylacetone) diphenylphenanthroline europium, and tris (hexa). Fluoroacetylacetone) bis (triphenylphosphine) europium, tris (trifluoroacetylacetone) 2,2′-bipyridine europium, tris (hexafluoroacetylacetone) 2,2′-bipyridine europium, and the like.
- Examples of the lanthanoid complex having a tridentate ligand containing a halogen atom include terpyridine trifluoroacetylacetone europium, terpyridine hexafluoroacetylacetone europium, and the like.
- a halogen atom of the lanthanoid complex having a bidentate ligand containing a halogen atom or a lanthanoid complex having a tridentate ligand containing a halogen atom a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom can be used. .
- a fluorine atom is preferable because the structure of the ligand is stabilized.
- the lanthanoid complex having a halogen atom and an acetylacetone skeleton containing a halogen atom is particularly excellent.
- Lanthanoid complexes having a bidentate ligand are preferred.
- Examples of the lanthanoid complex having a bidentate ligand having an acetylacetone skeleton containing a halogen atom include Eu (TFA) 3 phen, Eu (TFA) 3 dpphen, Eu (HFA) 3 phen, and [Eu (FOD) 3 ].
- the structure of a lanthanoid complex having a bidentate ligand having an acetylacetone skeleton containing these halogen atoms is shown.
- the lanthanoid complex having a bidentate ligand containing a halogen atom or the lanthanoid complex having a tridentate ligand containing a halogen atom is preferably particulate. It is easier to finely disperse a lanthanoid complex having a bidentate ligand containing a halogen atom or a lanthanoid complex having a tridentate ligand containing a halogen atom in an interlayer film for laminated glass. It becomes.
- the preferred lower limit of the average particle size of the lanthanoid complex is 0.01 ⁇ m, preferably The upper limit is 10 ⁇ m, the more preferable lower limit is 0.03 ⁇ m, and the more preferable upper limit is 1 ⁇ m.
- the content of the lanthanoid complex having a bidentate ligand containing a halogen atom or the lanthanoid complex having a tridentate ligand containing a halogen atom in the interlayer film for laminated glass is preferably a lower limit relative to 100 parts by weight of the thermoplastic resin. Is 0.001 part by weight, and a preferred upper limit is 10 parts by weight.
- a preferred upper limit is 10 parts by weight.
- the interlayer film for laminated glass is transparent The nature becomes even higher.
- the more preferred lower limit of the content of the lanthanoid complex having a bidentate ligand containing a halogen atom or the lanthanoid complex having a tridentate ligand containing a halogen atom is 0.01 parts by weight, and a more preferred upper limit is 5 parts by weight.
- a more preferred lower limit is 0.05 parts by weight, and a more preferred upper limit is 1 part by weight.
- a light emitting material having a terephthalic acid ester structure can also be used.
- the light emitting material having the terephthalic acid ester structure emits light when irradiated with light.
- Examples of the light emitting material having the terephthalic acid ester structure include a compound having a structure represented by the following general formula (1) and a compound having a structure represented by the following general formula (2). These may be used alone or in combination of two or more.
- R 1 represents an organic group, and x is 1, 2, 3 or 4. Since the transparency of the interlayer film for laminated glass is further increased, x is preferably 1 or 2, more preferably a hydroxyl group at the 2-position or 5-position of the benzene ring, More preferably, it has a hydroxyl group at the 5-position.
- the organic group for R 1 is preferably a hydrocarbon group, more preferably a hydrocarbon group having 1 to 10 carbon atoms, still more preferably a hydrocarbon group having 1 to 5 carbon atoms, Particularly preferred is a hydrocarbon group having 1 to 3 carbon atoms. When the hydrocarbon group has 10 or less carbon atoms, the light-emitting material having the terephthalate structure can be easily dispersed in the interlayer film for laminated glass.
- the hydrocarbon group is preferably an alkyl group.
- Examples of the compound having the structure represented by the general formula (1) include diethyl-2,5-dihydroxyterephthalate, dimethyl-2,5-dihydroxyterephthalate and the like. Among them, since a higher contrast image can be displayed, the compound having the structure represented by the general formula (1) is diethyl-2,5-dihydroxyterephthalate (“2,5-dihydroxyterephthalic acid manufactured by Aldrich). Diethyl ”) is preferred.
- R 2 represents an organic group
- R 3 and R 4 represent a hydrogen atom or an organic group
- y is 1, 2, 3, or 4.
- the organic group for R 2 is preferably a hydrocarbon group, more preferably a hydrocarbon group having 1 to 10 carbon atoms, still more preferably a hydrocarbon group having 1 to 5 carbon atoms, Particularly preferred is a hydrocarbon group having 1 to 3 carbon atoms.
- the hydrocarbon group is preferably an alkyl group.
- NR 3 R 4 is an amino group.
- R 3 and R 4 are preferably hydrogen atoms.
- one hydrogen atom may be the amino group, and two hydrogen atoms may be the amino group.
- the three hydrogen atoms may be the amino group, and the four hydrogen atoms may be the amino group.
- diethyl-2,5-diaminoterephthalate (manufactured by Aldrich) is preferable because an image with higher contrast can be displayed.
- the content of the light emitting material having the terephthalic acid ester structure in the interlayer film for laminated glass is not particularly limited, but a preferable lower limit with respect to 100 parts by weight of the thermoplastic resin is 0.001 part by weight, and a preferable upper limit is 15 parts by weight. .
- a preferable lower limit with respect to 100 parts by weight of the thermoplastic resin is 0.001 part by weight
- a preferable upper limit is 15 parts by weight.
- the more preferable lower limit of the content of the light emitting material having a terephthalic acid ester structure is 0.01 parts by weight, the more preferable upper limit is 10 parts by weight, the still more preferable lower limit is 0.1 parts by weight, and the still more preferable upper limit is 8 parts by weight.
- a preferred lower limit is 0.5 parts by weight, and a particularly preferred upper limit is 5 parts by weight.
- the content of the light emitting material having the terephthalate structure in the interlayer film for laminated glass is preferably 0.007% by weight and preferably 4.5% by weight in 100% by weight of the interlayer film for laminated glass. is there.
- the content of the light-emitting material having the terephthalic acid ester structure is 0.007% by weight or more, an image with higher contrast can be displayed.
- the content of the light emitting material having the terephthalic acid ester structure is 4.5% by weight or less, the transparency of the interlayer film for laminated glass is further enhanced.
- the more preferable lower limit of the content of the light emitting material having the terephthalic acid ester structure is 0.01% by weight, the more preferable upper limit is 4% by weight, the still more preferable lower limit is 0.1% by weight, and the more preferable upper limit is 3.5% by weight. It is.
- the interlayer film for laminated glass may contain potassium, sodium, and magnesium derived from raw materials such as a neutralizing agent used during the production of the thermoplastic resin.
- the total content of potassium, sodium and magnesium contained in the interlayer film for laminated glass is preferably 50 ppm or less.
- Luminescence of a lanthanoid complex having a bidentate ligand containing a halogen atom or a lanthanoid complex having a tridentate ligand containing a halogen atom by using a total content of potassium, sodium and magnesium of 50 ppm or less It is possible to prevent the performance from deteriorating.
- the content of magnesium contained in the interlayer film for laminated glass is preferably 40 ppm or less.
- a lanthanoid complex having a bidentate ligand containing the halogen atom in the interlayer film for laminated glass or a tridentate arrangement containing a halogen atom A decrease in the light emission performance of the lanthanoid complex having a ligand can be more reliably suppressed.
- the content of magnesium contained in the interlayer film for laminated glass is more preferably 35 ppm or less, further preferably 30 ppm or less, and particularly preferably 20 ppm or less.
- the magnesium content in the interlayer film for laminated glass may be 0 ppm.
- thermoplastic resin In order to make the total content of potassium, sodium, and magnesium contained in the interlayer film for laminated glass 50 ppm or less, it is preferable to wash the thermoplastic resin multiple times with an excessive amount of ion-exchanged water.
- the interlayer film for laminated glass preferably further contains a dispersant.
- a dispersant is, for example, a compound having a sulfonic acid structure such as a linear alkylbenzene sulfonate, or an ester structure such as a diester compound, a ricinoleic acid alkyl ester, a phthalic acid ester, an adipic acid ester, a sebacic acid ester, or a phosphoric acid ester.
- Compounds having an ether structure such as polyoxyethylene glycol, polyoxypropylene glycol and alkylphenyl-polyoxyethylene-ether, compounds having a carboxylic acid structure such as polycarboxylic acid, laurylamine, dimethyllauryl
- Compounds having an amine structure such as amines, oleylpropylenediamine, secondary amines of polyoxyethylene, tertiary amines of polyoxyethylene, and diamines of polyoxyethylene
- polyalkylenepolyaminealkyleneoxy Dispersants such as compounds having a polyamine structure such as amides, compounds having an amide structure such as oleic acid diethanolamide and alkanol fatty acid amide, and compounds having a high molecular weight amide structure such as polyvinylpyrrolidone and polyester acid amide amine salts Can be used.
- high molecular weight dispersing agents such as polyoxyethylene alkyl ether phosphoric acid (salt), high molecular polycarboxylic acid, and condensed ricinoleic acid ester.
- the high molecular weight dispersant is defined as a dispersant having a molecular weight of 10,000 or more.
- the lanthanoid complex having a bidentate ligand containing a halogen atom or the lanthanoid complex having a tridentate ligand containing a halogen atom in the interlayer film for laminated glass The preferable lower limit of the content of the dispersant is 1 part by weight, and the preferable upper limit is 50 parts by weight. When the content of the dispersant is within this range, the lanthanoid complex having a bidentate ligand containing a halogen atom or the lanthanoid complex having a tridentate ligand containing a halogen atom is added to the interlayer film for laminated glass. It can be uniformly dispersed.
- the more preferable lower limit of the content of the dispersant is 3 parts by weight, the more preferable upper limit is 30 parts by weight, the still more preferable lower limit is 5 parts by weight, and the still more preferable upper limit is 25 parts by weight.
- the interlayer film for laminated glass may further contain an ultraviolet absorber.
- the interlayer film for laminated glass contains an ultraviolet absorber, the light resistance of the interlayer film for laminated glass is increased. Since an interlayer film for laminated glass capable of displaying an image having a higher contrast is obtained, the preferable upper limit of the content of the ultraviolet absorber in the interlayer film for laminated glass is 1 weight with respect to 100 parts by weight of the thermoplastic resin. Parts, more preferred upper limit is 0.5 parts by weight, still more preferred upper limit is 0.2 parts by weight, and particularly preferred upper limit is 0.1 parts by weight.
- Examples of the ultraviolet absorber include a compound having a malonic ester structure, a compound having an oxalic acid anilide structure, a compound having a benzotriazole structure, a compound having a benzophenone structure, a compound having a triazine structure, a compound having a benzoate structure, and a hindered amine
- Examples include ultraviolet absorbers such as compounds having a structure.
- the interlayer film for laminated glass may further contain a plasticizer.
- the plasticizer is not particularly limited, and examples thereof include organic ester plasticizers such as monobasic organic acid esters and polybasic organic acid esters, phosphoric acid plasticizers such as organic phosphoric acid plasticizers and organic phosphorous acid plasticizers, and the like. Is mentioned.
- the plasticizer is preferably a liquid plasticizer.
- the monobasic organic acid ester is not particularly limited.
- glycol such as triethylene glycol, tetraethylene glycol, tripropylene glycol, butyric acid, isobutyric acid, caproic acid, 2-ethylbutyric acid, heptylic acid, n-octyl
- glycol esters obtained by reaction with monobasic organic acids such as acid, 2-ethylhexyl acid, pelargonic acid (n-nonyl acid), and decyl acid.
- triethylene glycol dicaproate, triethylene glycol di-2-ethylbutyrate, triethylene glycol di-n-octylate, triethylene glycol di-2-ethylhexylate and the like are preferable.
- the polybasic organic acid ester is not particularly limited.
- an ester compound of a polybasic organic acid such as adipic acid, sebacic acid or azelaic acid and an alcohol having a linear or branched structure having 4 to 8 carbon atoms.
- dibutyl sebacic acid ester, dioctyl azelaic acid ester, dibutyl carbitol adipic acid ester and the like are preferable.
- the organic ester plasticizer is not particularly limited, and triethylene glycol di-2-ethylbutyrate, triethylene glycol di-2-ethylhexanoate, triethylene glycol dicaprylate, triethylene glycol di-n-octanoate, Triethylene glycol di-n-heptanoate, tetraethylene glycol di-n-heptanoate, tetraethylene glycol di-2-ethylhexanoate, dibutyl sebacate, dioctyl azelate, dibutyl carbitol adipate, ethylene glycol di-2-ethyl Butyrate, 1,3-propylene glycol di-2-ethyl butyrate, 1,4-butylene glycol di-2-ethyl butyrate, diethylene glycol di-2-ethyl butyrate, diethylene glycol di- -Ethylhexanoate, dipropylene glycol di-2-ethylbutyrate,
- the organophosphate plasticizer is not particularly limited, and examples thereof include tributoxyethyl phosphate, isodecylphenyl phosphate, triisopropyl phosphate, and the like.
- dihexyl adipate DHA
- triethylene glycol di-2-ethylhexanoate 3GO
- tetraethylene glycol di-2-ethylhexanoate 4GO
- the content of the plasticizer in the interlayer film for laminated glass is not particularly limited, but a preferable lower limit with respect to 100 parts by weight of the thermoplastic resin is 30 parts by weight, and a preferable upper limit is 100 parts by weight.
- a preferable lower limit with respect to 100 parts by weight of the thermoplastic resin is 30 parts by weight
- a preferable upper limit is 100 parts by weight.
- the content of the plasticizer is 30 parts by weight or more, the melt viscosity of the laminated glass interlayer film becomes low, so that the laminated glass interlayer film can be easily formed.
- the content of the plasticizer is 100 parts by weight or less, the transparency of the interlayer film for laminated glass increases.
- a more preferred lower limit of the plasticizer content is 35 parts by weight, a more preferred upper limit is 80 parts by weight, a still more preferred lower limit is 45 parts by weight, a still more preferred upper limit is 70 parts by weight, a particularly preferred lower limit is 50 parts by weight, and a particularly preferred upper limit. Is 63 parts by weight.
- the antioxidant is not particularly limited, and examples thereof include an antioxidant having a fail structure, an antioxidant containing sulfur, and an antioxidant containing phosphorus.
- the antioxidant having the phenol structure is an antioxidant having a phenol skeleton.
- antioxidant having a phenol structure examples include 2,6-di-t-butyl-p-cresol (BHT), butylated hydroxyanisole (BHA), 2,6-di-t-butyl-4- Ethylphenol, stearyl- ⁇ - (3,5-di-t-butyl-4-hydroxyphenyl) propionate, 2,2′-methylenebis- (4-methyl-6-butylphenol), 2,2′-methylenebis- ( 4-ethyl-6-t-butylphenol), 4,4'-butylidene-bis- (3-methyl-6-t-butylphenol), 1,1,3-tris- (2-methyl-hydroxy-5-t -Butylphenyl) butane, tetrakis [methylene-3- (3 ', 5'-butyl-4-hydroxyphenyl) propionate] methane, 1,3,3-tris- (2-methyl) 4-hydroxy-5-tert-butylphenol) butane, 1,3,5-trimethyl-2
- the interlayer film for laminated glass may contain additives such as a light stabilizer, an antistatic agent, a blue pigment, a blue dye, a green pigment, and a green dye as necessary.
- the interlayer film for laminated glass may have a single layer structure composed only of a light emitting layer containing the light emitting material, or may have a multilayer structure in which a light emitting layer containing the light emitting material and another layer are laminated.
- the light emitting layer containing the light emitting material may be disposed on the entire surface of the interlayer film for laminated glass, or may be disposed only on a part thereof. It may be arranged on the entire surface in a plane direction perpendicular to the thickness direction of the intermediate film, or may be arranged only in part.
- the light-emitting layer containing the light-emitting material When the light-emitting layer containing the light-emitting material is arranged only in part, information can be displayed only in the light-emitting area with the part as a light-emitting area and the other part as a non-light-emitting area. .
- the interlayer film for laminated glass has a multilayer structure
- various functions can be imparted to the resulting interlayer film for laminated glass by adjusting the constituent components of the light emitting layer containing the light emitting material and other layers. It is.
- the content of the plasticizer hereinafter also referred to as content X
- content Y the content of the plasticizer relative to 100 parts by weight of the thermoplastic resin in this layer
- the content X is preferably 5 parts by weight or more, more preferably 10 parts by weight or more, and still more preferably 15 parts by weight or more than the content Y.
- the difference between the content X and the content Y is preferably 50 parts by weight or less, more preferably 40 parts by weight or less. Preferably, it is 35 parts by weight or less.
- the preferred lower limit of the content X is 45 parts by weight, the preferred upper limit is 80 parts by weight, the more preferred lower limit is 50 parts by weight, the more preferred upper limit is 75 parts by weight, and the still more preferred lower limit is 55 parts by weight. Is 70 parts by weight.
- the preferred lower limit of the content Y is 20 parts by weight, the preferred upper limit is 45 parts by weight, the more preferred lower limit is 30 parts by weight, the more preferred upper limit is 43 parts by weight, and the still more preferred lower limit is 35 parts by weight. Is 41 parts by weight.
- the thermoplastic resin in the light emitting layer is preferably polyvinyl acetal X.
- the polyvinyl acetal X can be prepared by acetalizing polyvinyl alcohol with an aldehyde.
- the polyvinyl alcohol is usually obtained by saponifying polyvinyl acetate.
- a preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 200, and a preferable upper limit is 5000.
- the more preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 500, and the more preferable upper limit is 4000.
- the average degree of polymerization of the polyvinyl alcohol is determined by a method based on JIS K6726 “Testing method for polyvinyl alcohol”.
- the preferable lower limit of the carbon number of the aldehyde for acetalizing the polyvinyl alcohol is 4, and the preferable upper limit is 6.
- the aldehyde having 4 to 6 carbon atoms may be a linear aldehyde or a branched aldehyde, and examples thereof include n-butyraldehyde and n-valeraldehyde. .
- the upper limit with the preferable amount of hydroxyl groups of the said polyvinyl acetal X is 30 mol%.
- the upper limit of the amount of hydroxyl groups in the polyvinyl acetal X is more preferably 28 mol%, more preferably 26 mol%, and particularly preferably 24 mol%, the preferable lower limit is 10 mol%, and the more preferable lower limit is 15 mol%.
- a preferred lower limit is 20 mol%.
- the amount of hydroxyl groups in the polyvinyl acetal X is a value obtained by dividing the amount of ethylene groups to which the hydroxyl groups are bonded by the total amount of ethylene groups in the main chain, as a percentage (mol%).
- the amount of ethylene group to which the hydroxyl group is bonded can be determined, for example, by measuring the amount of ethylene group to which the hydroxyl group of polyvinyl acetal X is bonded by a method based on JIS K6728 “Testing method for polyvinyl butyral”. it can.
- the minimum with the preferable amount of acetal groups of the said polyvinyl acetal X is 60 mol%, and a preferable upper limit is 85 mol%.
- a preferable upper limit is 85 mol%.
- the lower limit of the amount of acetal group of the polyvinyl acetal X is more preferably 65 mol%, still more preferably 68 mol% or more.
- the amount of the acetal group can be determined by measuring the amount of ethylene group to which the acetal group of the polyvinyl acetal X is bonded by a method based on JIS K6728 “Testing method for polyvinyl butyral”.
- the minimum with the preferable amount of acetyl groups of the said polyvinyl acetal X is 0.1 mol%, and a preferable upper limit is 30 mol%.
- a preferable upper limit is 30 mol%.
- the more preferable lower limit of the acetyl group amount of the polyvinyl acetal X is 1 mol%, the more preferable lower limit is 5 mol%, the particularly preferable lower limit is 8 mol%, the more preferable upper limit is 25 mol%, and the more preferable upper limit is 20 mol%. It is.
- the amount of acetyl groups is the value obtained by subtracting the amount of ethylene groups to which acetal groups are bonded and the amount of ethylene groups to which hydroxyl groups are bonded from the total amount of ethylene groups in the main chain. This is a value expressed as a percentage (mol%) of the mole fraction obtained by dividing by.
- the polyvinyl acetal X is a polyvinyl acetal having an acetyl group content of 8 mol% or more, or Polyvinyl acetal having an acetyl group amount of less than 8 mol% and an acetal group amount of 65 mol% or more is preferred.
- the polyvinyl acetal X is a polyvinyl acetal having an acetyl group amount of 8 mol% or more, or a polyvinyl acetal having an acetyl group amount of less than 8 mol% and an acetal group amount of 68 mol% or more. More preferable.
- the thermoplastic resin in the other layer is preferably polyvinyl acetal Y.
- the polyvinyl acetal Y preferably has a larger amount of hydroxyl groups than the polyvinyl acetal X.
- the polyvinyl acetal Y can be prepared by acetalizing polyvinyl alcohol with an aldehyde.
- the polyvinyl alcohol is usually obtained by saponifying polyvinyl acetate.
- the preferable minimum of the average degree of polymerization of the said polyvinyl alcohol is 200, and a preferable upper limit is 5000.
- the more preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 500, and the more preferable upper limit is 4000.
- the preferable lower limit of the carbon number of the aldehyde for acetalizing the polyvinyl alcohol is 3, and the preferable upper limit is 4.
- the aldehyde having 3 to 4 carbon atoms may be a linear aldehyde or a branched aldehyde, and examples thereof include n-butyraldehyde.
- the upper limit with the preferable amount of hydroxyl groups of the said polyvinyl acetal Y is 33 mol%, and a preferable minimum is 28 mol%.
- the minimum with the preferable amount of acetal groups of the said polyvinyl acetal Y is 60 mol%, and a preferable upper limit is 80 mol%.
- a preferable upper limit is 80 mol%.
- the upper limit with the preferable amount of acetyl groups of the said polyvinyl acetal Y is 7 mol%. By making the amount of acetyl groups of the polyvinyl acetal Y 7 mol% or less, the hydrophobicity of other layers can be increased and whitening can be prevented.
- the upper limit with the more preferable amount of acetyl groups of the said polyvinyl acetal Y is 2 mol%, and a preferable minimum is 0.1 mol%.
- the amount of hydroxyl groups, the amount of acetal groups, and the amount of acetyl groups of polyvinyl acetal Y can be measured by the same method as for polyvinyl acetal X.
- heat ray absorption is performed in any one layer, any two layers, or all layers of the light emitting layer containing the light emitting material and other layers.
- An agent can be included.
- the heat ray absorber is not particularly limited as long as it has the ability to shield infrared rays, but is tin-doped indium oxide (ITO) particles, antimony-doped tin oxide (ATO) particles, aluminum-doped zinc oxide (AZO) particles, indium-doped oxide. At least one selected from the group consisting of zinc (IZO) particles, tin-doped zinc oxide particles, silicon-doped zinc oxide particles, lanthanum hexaboride particles and cerium hexaboride particles is preferred.
- the thickness of the interlayer film for laminated glass is not particularly limited, but a preferable lower limit is 50 ⁇ m, a preferable upper limit is 1700 ⁇ m, a more preferable lower limit is 100 ⁇ m, a more preferable upper limit is 1000 ⁇ m, and a further preferable upper limit is 900 ⁇ m.
- the lower limit of the thickness of the interlayer film for laminated glass means the thickness of the minimum thickness portion of the interlayer film for laminated glass, and the upper limit of the thickness of the interlayer film for laminated glass is the maximum of the interlayer film for laminated glass. It means the thickness of the thickness part.
- the thickness of the light emitting layer containing the light emitting material is not particularly limited, but a preferable lower limit is 50 ⁇ m and a preferable upper limit is 1000 ⁇ m.
- a preferable lower limit is 50 ⁇ m and a preferable upper limit is 1000 ⁇ m.
- the thickness of the light emitting layer containing the light emitting material is within this range, light emission with sufficiently high contrast can be obtained when light of a specific wavelength is irradiated.
- the more preferable lower limit of the thickness of the light emitting layer containing the light emitting material is 80 ⁇ m
- the more preferable upper limit is 500 ⁇ m
- the still more preferable lower limit is 90 ⁇ m
- the still more preferable upper limit is 300 ⁇ m.
- the interlayer film for laminated glass of the present invention may have a wedge-shaped cross section. If the cross-sectional shape of the interlayer film for laminated glass is wedge-shaped, it is possible to display an image with the occurrence of double images prevented by adjusting the wedge-shaped wedge angle ⁇ according to the attachment angle of the laminated glass. From the viewpoint of further suppressing double images, the preferable lower limit of the wedge angle ⁇ is 0.1 mrad, the more preferable lower limit is 0.2 mrad, the still more preferable lower limit is 0.3 mrad, the preferable upper limit is 1 mrad, and the more preferable upper limit is 0.9 mrad.
- an interlayer film for laminated glass having a wedge-shaped cross section is manufactured by a method of extruding a resin composition using an extruder, a slightly inner region (specifically, from one end on the thin side) , Where X is the distance between one end and the other end, and has a minimum thickness in the range from 0X to 0.2X inward from one end on the thin side, and one end on the thick side
- the maximum thickness in the region slightly inside specifically, when the distance between one end and the other end is X, the region from 0X to 0.2X inward from one end on the thick side
- It may become the shape which has. In the present specification, such a shape is also included in the wedge shape.
- the cross-sectional shape of the interlayer film for laminated glass of the present invention is wedge-shaped, it preferably has a multilayer structure including a light emitting layer and other layers (hereinafter sometimes referred to as “shape auxiliary layer”). While the thickness of the light emitting layer is kept within a certain range, by laminating the shape auxiliary layer, the cross-sectional shape of the entire interlayer film for laminated glass can be adjusted to a wedge shape with a constant wedge angle.
- the shape auxiliary layer may be laminated only on one surface of the light emitting layer, or may be laminated on both surfaces. Further, a plurality of shape auxiliary layers may be laminated.
- the light emitting layer may have a wedge-shaped cross section or a rectangular shape.
- the difference between the maximum thickness and the minimum thickness of the light emitting layer is preferably 100 ⁇ m or less. Thereby, an image can be displayed with a certain range of luminance.
- the difference between the maximum thickness and the minimum thickness of the light emitting layer is more preferably 95 ⁇ m or less, and still more preferably 90 ⁇ m or less.
- the thickness of the light emitting layer is not particularly limited, but a preferable lower limit is 50 ⁇ m and a preferable upper limit is 700 ⁇ m. When the thickness of the light emitting layer is within this range, a sufficiently high contrast image can be displayed.
- the more preferable lower limit of the thickness of the light emitting layer is 70 ⁇ m
- the more preferable upper limit is 400 ⁇ m
- the still more preferable lower limit is 80 ⁇ m
- the still more preferable upper limit is 150 ⁇ m.
- the lower limit of the thickness of the light emitting layer means the thickness of the minimum thickness portion of the light emitting layer
- the upper limit of the thickness of the light emitting layer means the thickness of the maximum thickness portion of the light emitting layer.
- the shape auxiliary layer has a role of being laminated on the light emitting layer and adjusting the cross sectional shape of the laminated glass intermediate film as a wedge shape having a constant wedge angle.
- the shape auxiliary layer preferably has a wedge-shaped, triangular, trapezoidal or rectangular cross-sectional shape.
- the thickness of the shape auxiliary layer is not particularly limited, but from the viewpoint of practical use and from the viewpoint of sufficiently increasing the adhesive strength and penetration resistance, the preferred lower limit is 10 ⁇ m, the preferred upper limit is 1000 ⁇ m, and the more preferred lower limit is 200 ⁇ m, A more preferable upper limit is 800 ⁇ m, and a further preferable lower limit is 300 ⁇ m.
- the lower limit of the thickness of the shape auxiliary layer means the thickness of the minimum thickness portion of the shape auxiliary layer, and the upper limit of the thickness of the shape auxiliary layer means the thickness of the maximum thickness portion of the shape auxiliary layer. To do. Further, when a plurality of shape auxiliary layers are used in combination, the total thickness is meant.
- FIGS. 1 to 3 are schematic diagrams for explaining an example of the case where the cross-sectional shape of the interlayer film for laminated glass of the present invention is a wedge shape.
- the thickness and wedge angle ⁇ of the interlayer film for laminated glass and each layer constituting the interlayer film for laminated glass are shown to be different from the actual thickness and wedge angle. Yes.
- FIG. 1 shows a cross section in the thickness direction of the interlayer film 1 for laminated glass.
- the interlayer film 1 for laminated glass has a two-layer structure in which a shape auxiliary layer 12 is laminated on one surface of a light emitting layer 11 containing a light emitting material.
- the light emitting layer 11 has a rectangular shape
- the shape auxiliary layer 12 has a wedge shape, a triangular shape, or a trapezoidal shape, so that the laminated film intermediate film 1 has a wedge angle ⁇ of 0.1 to 1 mrad as a whole. It has a wedge shape.
- FIG. 2 shows a cross section in the thickness direction of the interlayer film 2 for laminated glass.
- the interlayer film 2 for laminated glass has a three-layer structure in which a shape auxiliary layer 22 and a shape auxiliary layer 23 are laminated on both surfaces of a light emitting layer 21 containing a light emitting material.
- the shape auxiliary layer 22 is wedge-shaped, triangular, or trapezoidal so that the interlayer film 2 for laminated glass as a whole is wedged.
- the wedge shape has an angle ⁇ of 0.1 to 1 mrad.
- FIG. 3 shows a cross section in the thickness direction of the interlayer film 3 for laminated glass.
- the interlayer film 3 for laminated glass has a three-layer structure in which a shape auxiliary layer 32 and a shape auxiliary layer 33 are laminated on both surfaces of a light emitting layer 31 containing a light emitting material.
- the light emitting layer 31 has a gentle wedge shape with a difference between the maximum thickness and the minimum thickness of 100 ⁇ m or less.
- the wedge angle ⁇ of the laminated glass intermediate film 3 as a whole is increased. It has a wedge shape of 0.1 to 1 mrad.
- the method for producing the interlayer film for laminated glass is not particularly limited.
- a plasticizer solution containing a plasticizer and a light-emitting material and a thermoplastic resin are sufficiently mixed to produce a resin composition for forming an interlayer film for laminated glass.
- the resin composition for forming the interlayer film for laminated glass can be extruded using an extruder to produce an interlayer film for laminated glass.
- the laminated glass is obtained by laminating the interlayer film for laminated glass between a pair of glass plates.
- the said glass plate can use the transparent plate glass generally used. Examples thereof include inorganic glass such as float plate glass, polished plate glass, template glass, netted glass, wire-containing plate glass, colored plate glass, heat ray absorbing glass, heat ray reflecting glass, and green glass.
- inorganic glass such as float plate glass, polished plate glass, template glass, netted glass, wire-containing plate glass, colored plate glass, heat ray absorbing glass, heat ray reflecting glass, and green glass.
- the ultraviolet shielding glass in which the ultraviolet shielding coating layer was formed in the glass surface can be used, it is preferable to use as a glass plate opposite to the side irradiated with the light ray of a specific wavelength.
- organic plastics plates such as polyethylene terephthalate, polycarbonate, and polyacrylate can be used as the glass plate.
- glass plate Two or more types of glass plates may be used as the glass plate.
- stacked the said intermediate film for laminated glass between transparent float plate glass and colored glass plates like green glass is mentioned.
- the said irradiation apparatus irradiates a light beam to the said laminated glass, Comprising:
- the output of the irradiated light beam is 1 mW or less. When the output is 1 mW or less, it is safe even if the irradiated light passes through the laminated glass interlayer film and is directly observed by a person.
- the preferable upper limit of the output of the irradiated light is 0.9 mW, the more preferable upper limit is 0.8 mW, and the more preferable upper limit is 0.7 mW.
- the lower limit of the output of the light beam to be irradiated is not particularly limited as long as it is an output capable of causing the laminated glass to emit light with a luminance of 1 cd / m 2 or more, but a preferable lower limit is 0.1 mW, and a more preferable lower limit is 0.2 mW. A more preferred lower limit is 0.4 mW.
- the output of the light beam to be irradiated is measured by irradiation intensity measurement using a laser power meter (for example, “Beam Track Power Measurement Sensor 3A-QUAD” manufactured by OFIEL JAPAN Co., Ltd.) disposed at a position 10 cm away from the light source. Can be measured.
- a laser power meter for example, “Beam Track Power Measurement Sensor 3A-QUAD” manufactured by OFIEL JAPAN Co., Ltd.
- the irradiation rays are preferred lower limit is 0.1 mW / cm 2 density, the desirable upper limit is 550 mW / cm 2.
- the density of the light to be irradiated is 0.1 mW / cm 2 or more, the light emission display at night is sufficiently visible, and when it is 550 mW / cm 2 or less, the luminance difference from the surroundings at night does not become uncomfortable. .
- the more preferable lower limit of the density of the irradiated light is 0.2 mW / cm 2, and more preferred upper limit is 530mW / cm 2, still more preferred lower limit 0.3 mW / cm 2, still more preferred upper limit is at 500 mW / cm 2 , especially preferred lower limit is 0.4 mW / cm 2, particularly preferred upper limit is 450 mW / cm 2.
- the density of the irradiated light is measured by measuring the accumulated UV light amount per unit area using an UV integrated light meter (for example, “UIT-250” manufactured by USHIO INC.) Located 10 cm away from the light source. Can be measured.
- the light beam to be irradiated has a preferable lower limit of the irradiation diameter of 0.005 cm ⁇ and a preferable upper limit of 3 cm ⁇ .
- the irradiation diameter of the light beam to be irradiated is 0.005 cm ⁇ or more, it is possible to recognize light emission by visual observation, and when it is 3 cm ⁇ or less, it is possible to perform display with good contrast.
- the more preferable lower limit of the irradiation diameter of the light beam to be irradiated is 0.01 cm ⁇ , the more preferable upper limit is 2.5 cm ⁇ , the still more preferable lower limit is 0.03 cm ⁇ , the still more preferable upper limit is 2 cm ⁇ , and the particularly preferable lower limit is 0.05 cm ⁇ , A particularly preferred upper limit is 1 cm ⁇ .
- the irradiation diameter of the light beam to be irradiated is measured by a CCD sensor and a CMOS sensor (for example, “USB2.0 beam diagnostic camera Laser Cam HR” manufactured by Coherent Japan Co., Ltd.) disposed at a position 10 cm away from the light source. Based on the result, it can be calculated according to the ISO 11146 standard.
- a CCD sensor and a CMOS sensor for example, “USB2.0 beam diagnostic camera Laser Cam HR” manufactured by Coherent Japan Co., Ltd.
- Examples of the irradiation apparatus include spot light sources (manufactured by Hamamatsu Photonics, “LC-8”, etc.), xenon flash lamps (manufactured by Heraeus, “CW lamp”, etc.), black lights (manufactured by Inoue Seieido, “Carry” Hand ”) and the like.
- the laminated glass when the laminated glass is irradiated with light from the irradiation device, the laminated glass emits light with a luminance of 1 cd / m 2 or more. Even when a low-intensity light beam with an output of 1 mW or less is emitted, it is possible to display with sufficient contrast by emitting light with a luminance of 1 cd / m 2 or more, and the light beam transmitted through the interlayer film for laminated glass Even if it is observed directly by a person, it will not be dazzled.
- the measurement of the luminance of the laminated glass is preferably performed at a wavelength at which the light emitting material exhibits maximum intensity at a wavelength of 400 nm or longer, or at a wavelength of 405 nm, and more preferably at a wavelength of 405 nm.
- the display device of the present invention can be suitably used particularly for night vision.
- the display device of the present invention can be particularly suitably used for a windshield of a vehicle.
- the present invention it is possible to provide a display device, an interlayer film for laminated glass, and a laminated glass that can obtain a predetermined initial luminance even when irradiated with a low-intensity light beam.
- Example 1 Preparation of Eu (TFA) 3 phen 12.5 mmol of europium acetate (Eu (CH 3 COO) 3 ) was dissolved in 50 mL of distilled water, and 33.6 mmol of trifluoroacetylacetone (TFA, CH 3 COCH 2 COCF 3 ) was dissolved. The mixture was further stirred at room temperature for 3 hours. The precipitated solid was filtered, washed with water, and recrystallized with methanol and distilled water to obtain Eu (TFA) 3 (H 2 O) 2 .
- the obtained interlayer film for laminated glass was laminated between a pair of clear glass (thickness 2.5 mm) having a length of 5 cm and a width of 5 cm to obtain a laminate.
- the obtained laminate was vacuum-pressed while being held at 90 ° C. for 30 minutes with a vacuum laminator to be pressure-bonded. After the pressure bonding, pressure bonding was performed for 20 minutes using an autoclave under conditions of 140 ° C. and 14 MPa to obtain a laminated glass.
- Example 2 Preparation of Tb (TFA) 3 phen 12.5 mmol of terbium acetate (Tb (CH 3 COO) 3 ) was dissolved in 50 mL of distilled water, and 33.6 mmol of trifluoroacetylacetone (TFA, CH 3 COCH 2 COCF 3 ) was dissolved. The mixture was further stirred at room temperature for 3 hours. The precipitated solid was filtered, washed with water, and recrystallized with methanol and distilled water to obtain Tb (TFA) 3 (H 2 O) 2 .
- Tb (TFA) 3 (H 2 O) 2 Preparation of Tb (TFA) 3 phen 12.5 mmol of terbium acetate (Tb (CH 3 COO) 3 ) was dissolved in 50 mL of distilled water, and 33.6 mmol of trifluoroacetylacetone (TFA, CH 3 COCH 2 COCF 3 ) was dissolved. The mixture was further stirred at room temperature for
- Tb (TFA) 3 (H 2 O) 2 5.77 g
- 1,10-phenanthroline (phen) 2.5 g
- Tb (TFA) 3 phene was obtained by recrystallization from a mixed solvent of toluene and hexane.
- a display device was manufactured in the same manner as in Example 1 except that the irradiation device was adjusted to 4 mW, the light wavelength was 405 nm, the irradiation diameter was 0.05 cm ⁇ , and the light density was 204 mW / cm 2 .
- Example 1 By adjusting the output of the light source, a dedicated bandpass filter (Asahi Spectroscopy, “LX0405”), rod lens (Asahi Spectroscopy) and fiber (Asahi Spectroscopy), the output of light is 10 mW and the wavelength of light is 405 nm.
- a display device was manufactured in the same manner as in Example 1 except that the irradiation device was adjusted so that the irradiation diameter was 0.05 cm ⁇ and the light beam density was 50955 mW / cm 2 .
- the output of the light source is 0.4 mW by adjusting the light source output, a dedicated bandpass filter (manufactured by Asahi Spectroscopic Co., Ltd., “LX0405”), a rod lens (manufactured by Asahi Spectroscopic Co., Ltd.) and a fiber (manufactured by Asahi Spectroscopic Co., Ltd.)
- a display device was manufactured in the same manner as in Example 1 except that the irradiation device was adjusted so that the wavelength of 405 nm was 405 nm, the irradiation diameter was 0.05 cm ⁇ , and the light density was 204 mW / cm 2 .
- Example 6 Except that the content of Eu (HFA) 3 phen was changed to the values shown in Table 2, and the light output, irradiation diameter, and light density of the irradiation device were changed to the values shown in Table 2, the same as in Example 3. Thus, an interlayer film for laminated glass, a laminated glass and a display device were produced.
- Example 7 (1) Preparation of Tb (HFA) 3 phen 3.46 g (12.5 mmol) of terbium acetate (Tb (CH 3 COO) 3 ) was dissolved in 50 mL of distilled water, and hexafluoroacetylacetone (HFA, CF 3 COCH 2 COCF 3 ) 7.00 g (33.6 mmol) was added, and the mixture was stirred at room temperature for 3 hours. The precipitated solid was filtered, washed with water, and recrystallized with methanol and distilled water to obtain Tb (HFA) 3 (H 2 O) 2 .
- Example 8 Except that the blending amount of Tb (HFA) 3 phen was changed to the values shown in Table 2, and the light output, irradiation diameter, and light density of the irradiation device were changed to the values shown in Table 2, the same as in Example 7. Thus, an interlayer film for laminated glass, a laminated glass and a display device were produced.
- Example 11 An interlayer film for laminated glass in the same manner as in Example 1 except that Eu (TFA) 3 phen was changed to diethyl-2,5-dihydroxyterephthalate (manufactured by Aldrich, “diethyl 2,5-dihydroxyterephthalate”). And the laminated glass was produced.
- the output of the light source is 1 mW
- the wavelength of the light was manufactured in the same manner as in Example 1 except that the irradiation apparatus was adjusted so that the irradiation diameter was 405 nm, the irradiation diameter was 0.05 cm ⁇ , and the light beam density was 509 mW / cm 2 .
- Example 12 to 14 The content of diethyl-2,5-dihydroxyterephthalate was changed to the values shown in Tables 2 and 3, and the light output, irradiation diameter, and light density of the irradiation device were changed to the values shown in Tables 2 and 3.
- Example 15 (1) Production of interlayer film for laminated glass and laminated glass 40 parts by weight of triethylene glycol di-2-ethylhexanoate (3GO), 0.2 part by weight of Eu (HFA) 3 phene obtained in Example 3 and As an ultraviolet absorber, 0.2 part by weight of 2- (2′-hydroxy-3′-t-butyl-5-methylphenyl) -5-chlorobenzotriazole (“Tinuvin 326” manufactured by BASF) was added to produce a light-emitting plastic. An agent solution was prepared. A resin composition was prepared by sufficiently kneading the total amount of the obtained plasticizer solution and 100 parts by weight of the obtained polyvinyl butyral 1 with a mixing roll.
- 3GO triethylene glycol di-2-ethylhexanoate
- Eu (HFA) 3 phene obtained in Example 3 As an ultraviolet absorber, 0.2 part by weight of 2- (2′-hydroxy-3′-t-butyl-5-methylphenyl) -5-chlorobenz
- the obtained resin composition was extruded using an extruder to obtain an interlayer film for laminated glass (thickness: 760 ⁇ m). Note that the total content of sodium, potassium, and magnesium of the obtained interlayer film for laminated glass was measured using an ICP emission spectrometer (“ICPE-9000” manufactured by Shimadzu Corporation), and found to be 0 ppm. .
- the obtained interlayer film for laminated glass was laminated between a pair of clear glass (thickness 2.5 mm) having a length of 5 cm and a width of 5 cm to obtain a laminate.
- the obtained laminate was vacuum-pressed while being held at 90 ° C. for 30 minutes with a vacuum laminator to be pressure-bonded. After the pressure bonding, pressure bonding was performed for 20 minutes using an autoclave under conditions of 140 ° C. and 14 MPa to obtain a laminated glass.
- Example 16 and 17 Manufacture of interlayer film for laminated glass, laminated glass and display device in the same manner as in Example 15 except that the type of luminescent material, the content of the luminescent material, and the wavelength of the light beam of the irradiation device were changed as shown in Table 4. did.
- Example 18 (1) Preparation of resin compositions for first and second resin layers 40 parts by weight of triethylene glycol di-2-ethylhexanoate (3GO) and 100 parts by weight of polyvinyl butyral 1 are sufficiently kneaded with a mixing roll. By doing so, the 1st, 2nd resin composition for resin layers was prepared.
- 3GO triethylene glycol di-2-ethylhexanoate
- the amount of acetyl groups in PVB2 was 12 mol%, the amount of butyral groups was 65 mol%, and the amount of hydroxyl groups was 23 mol%.
- the resin composition for light emitting layers was prepared by fully knead
- the obtained interlayer film for laminated glass was laminated between a pair of clear glass (thickness 2.5 mm) having a length of 5 cm and a width of 5 cm to obtain a laminate.
- the obtained laminate was vacuum-pressed while being held at 90 ° C. for 30 minutes with a vacuum laminator to be pressure-bonded. After the pressure bonding, pressure bonding was performed for 20 minutes using an autoclave under conditions of 140 ° C. and 14 MPa to obtain a laminated glass.
- Example 19 An interlayer film for laminated glass, a laminated glass, and a display device were produced in the same manner as in Example 18 except that the type of the luminescent material and the wavelength of the light beam of the irradiation device were changed as shown in Table 5.
- Example 21 (1) Production of interlayer film for laminated glass and laminated glass
- the light-emitting layer resin composition obtained in Example 18 and the first and second resin layer resin compositions were co-extruded using a co-extruder. Extrusion was performed to obtain an interlayer film for laminated glass in which the first resin layer, the light emitting layer, and the second resin layer were laminated in this order.
- the mold shape of the co-extruder is a rectangular light emitting layer having a thickness of 100 ⁇ m, a wedge-shaped first resin layer having a thick part thickness of 600 ⁇ m, and a thin part having a thickness of 350 ⁇ m, and The second resin layer having a wedge shape and a thick portion having a thickness of 600 ⁇ m and a thin portion having a thickness of 350 ⁇ m was obtained.
- the shortest distance between one end and the other end in the direction perpendicular to the extrusion direction of the obtained intermediate film was 1 m.
- Example 22 An interlayer film for laminated glass, a laminated glass, and a display device were produced in the same manner as in Example 21 except that the type of the luminescent material and the wavelength of the light beam of the irradiation device were changed as shown in Table 5.
- first and second light emitting layer resin compositions 40 parts by weight of triethylene glycol di-2-ethylhexanoate (3GO) was mixed with Eu (HFA) 3 phen0. 22 parts by weight was added to prepare a luminescent plasticizer solution.
- First and second light emitting layer resin compositions were prepared by sufficiently kneading the total amount of the obtained plasticizer solution and 100 parts by weight of the obtained polyvinyl butyral 1 with a mixing roll.
- Non-light emitting layer resin composition and first and second light emitting layer resin compositions are co-extruded using a co-extruder to produce a first light emission.
- An interlayer film for laminated glass in which a layer, a non-light-emitting layer, and a second light-emitting layer were laminated in this order was obtained.
- the thickness of the non-light emitting layer was 100 ⁇ m
- the thickness of each of the first and second light emitting layers was 350 ⁇ m
- the thickness of the interlayer film for laminated glass was 800 ⁇ m
- the shapes of all the layers were rectangular.
- the obtained interlayer film for laminated glass was laminated between a pair of clear glass (thickness 2.5 mm) having a length of 5 cm and a width of 5 cm to obtain a laminate.
- the obtained laminate was vacuum-pressed while being held at 90 ° C. for 30 minutes with a vacuum laminator to be pressure-bonded. After the pressure bonding, pressure bonding was performed for 20 minutes using an autoclave under conditions of 140 ° C. and 14 MPa to obtain a laminated glass.
- Example 25 An interlayer film for laminated glass, a laminated glass, and a display device were produced in the same manner as in Example 24 except that the type of the luminescent material and the wavelength of the light beam of the irradiation device were changed as shown in Table 6.
- Example 27 (1) Manufacture of interlayer film for laminated glass and laminated glass Non-light emitting layer resin composition obtained in Example 24 and first and second light emitting layer resin compositions using a co-extruder Co-extrusion was performed to obtain an interlayer film for laminated glass in which the first light-emitting layer, the non-light-emitting layer, and the second light-emitting layer were laminated in this order.
- the shape of the mold of the co-extruder is a non-light-emitting layer having a rectangular shape and a thickness of 100 ⁇ m, a wedge-shaped first light-emitting layer having a thickness of 600 ⁇ m and a thin portion having a thickness of 350 ⁇ m, And it changed so that the 2nd light emitting layer which is wedge shape and the thickness of a thick part may be 600 micrometers, and the thickness of a thin part is 350 micrometers.
- the shortest distance between one end and the other end in the direction perpendicular to the extrusion direction of the obtained intermediate film was 1 m.
- the obtained laminated glass interlayer film has a vertical length of 5 cm so that a point 5 cm from the one end on the thin side of the laminated glass interlayer film on the shortest distance between one end and the other end in the direction perpendicular to the extrusion direction of the laminated glass film is the center.
- An intermediate film 5 cm wide was cut out.
- the obtained intermediate film of 5 cm length ⁇ 5 cm width was laminated between a pair of clear glass (thickness 2.5 mm) of 5 cm length ⁇ 5 cm width to obtain a laminate.
- the obtained laminate was vacuum-pressed while being held at 90 ° C. for 30 minutes with a vacuum laminator to be pressure-bonded. After the pressure bonding, pressure bonding was performed for 20 minutes using an autoclave under conditions of 140 ° C. and 14 MPa to obtain a laminated glass.
- Example 28 An interlayer film for laminated glass, a laminated glass and a display device were produced in the same manner as in Example 27 except that the type of the luminescent material and the wavelength of the light beam of the irradiation device were changed as shown in Table 6.
- the light was irradiated to the laminated glass from the irradiation apparatus, and the brightness
- the luminance was measured before and after the laminated glass was heat-treated at 100 ° C. for 4 weeks. Further, the luminance was measured at the center and the end of the laminated glass (site 2 cm from the end of the sample).
- the output of the light beam to be irradiated is measured by irradiation intensity measurement using a laser power meter (Offel Japan, “Beam Track Power Measurement Sensor 3A-QUAD”) located 10 cm away from the light source.
- the density is 10 cm from the light source.
- the density of the irradiated light is 10 cm from the light source by measuring the UV integrated light amount per unit area using an ultraviolet integrated light meter (Ushio Electric Co., Ltd., “UIT-250”) located 10 cm away from the light source. It was obtained by calculating according to the ISO11146 standard based on the measurement results of CCD sensor and CMOS sensor (“USB2.0 beam diagnostic camera Laser Cam HR” manufactured by Coherent Japan Co., Ltd.) arranged at remote positions.
- the present invention it is possible to provide a display device, an interlayer film for laminated glass, and a laminated glass that can obtain a predetermined initial luminance even when irradiated with a low-intensity light beam.
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Abstract
Description
HUDとしては、これまでに数々の形態が開発されている。最も一般的なHUDとしてコントロールユニットから送信される速度情報等をインストゥルメンタル・パネルの表示ユニットからフロントガラスに反射させることにより、運転者がフロントガラスと同じ位置、すなわち、同一視野内で速度情報等を視認できるHUDがある。
HUD用の合わせガラス用中間膜として、例えば、特許文献1には、所定の楔角を有する楔形合わせガラス用中間膜等が提案されており、合わせガラスにおいて計器表示が二重に見えるというHUDの欠点を解決することが提案されている。
本発明は、上記現状に鑑み、低強度の光線を照射した場合にも所定の初期輝度が得られるディスプレイ装置、合わせガラス用中間膜及び合わせガラスを提供することを目的とする。
以下に本発明を詳述する。
本発明のディスプレイ装置は、低強度の光線を照射したときでも所定の初期輝度が得られるため、特にナイトビジョンに好適である。
上記合わせガラスは、2枚のガラス板の間に、熱可塑性樹脂及び発光材料を含む合わせガラス用中間膜が積層されたものである。
上記ポリビニルアセタールのアセタール化度の好ましい下限は40モル%、好ましい上限は85モル%であり、より好ましい下限は60モル%、より好ましい上限は75モル%である。
なお、上記アセタール化度及び水酸基量は、例えば、JIS K6728「ポリビニルブチラール試験方法」に準拠して測定できる。
上記ポリビニルアルコールの重合度の好ましい下限は500、好ましい上限は4000である。上記ポリビニルアルコールの重合度が500以上であると、得られる合わせガラスの耐貫通性が高くなる。上記ポリビニルアルコールの重合度が4000以下であると、合わせガラス用中間膜の成形が容易になる。上記ポリビニルアルコールの重合度のより好ましい下限は1000、より好ましい上限は3600である。
ランタノイド錯体のなかでも、ハロゲン原子を含む多座配位子を有するランタノイド錯体は光線を照射することにより高い発光強度で発光する。上記ハロゲン原子を含む多座配位子を有するランタノイド錯体としては、ハロゲン原子を含む二座配位子を有するランタノイド錯体、ハロゲン原子を含む三座配位子を有するランタノイド錯体、ハロゲン原子を含む四座配位子を有するランタノイド錯体、ハロゲン原子を含む五座配位子を有するランタノイド錯体、ハロゲン原子を含む六座配位子を有するランタノイド錯体等が挙げられる。
しかも、上記ハロゲン原子を含む二座配位子を有するランタノイド錯体又はハロゲン原子を含む三座配位子を有するランタノイド錯体は、耐熱性にも優れる。フロントガラスは太陽光の赤外線が照射されることにより、高温環境下で使用されることが多い。このような高温環境下では発光材料が劣化して、特に合わせガラスの端部において著しく輝度が低下してしまうことがある。発光材料として上記ハロゲン原子を含む二座配位子を有するランタノイド錯体又はハロゲン原子を含む三座配位子を有するランタノイド錯体を用いることにより、高温環境下においても、輝度が変化しにくい合わせガラス用中間膜を得ることができる。
出力が1mW以下の光線を照射したときに、1.3~165cd/m2の輝度で発光する合わせガラスであれば、周囲が暗い夜間であっても、運転者が観察した際に明る過ぎず、且つ、暗過ぎない視認性の高い像を得ることができ、ナイトビジョン用途に特に好適である。
更に、該合わせガラス用中間膜が一対のガラス板の間に積層されている合わせガラスもまた、本発明の1つである。
上記ハロゲン原子を含む三座配位子を有するランタノイド錯体は、例えば、ターピリジントリフルオロアセチルアセトンユーロピウム、ターピリジンヘキサフルオロアセチルアセトンユーロピウム等が挙げられる。
上記ハロゲン原子を含むアセチルアセトン骨格を有する二座配位子を有するランタノイド錯体は、例えば、Eu(TFA)3phen、Eu(TFA)3dpphen、Eu(HFA)3phen、[Eu(FOD)3]bpy、[Eu(TFA)3]tmphen、[Eu(FOD)3]phen等が挙げられる。これらのハロゲン原子を含むアセチルアセトン骨格を有する二座配位子を有するランタノイド錯体の構造を示す。
上記ハロゲン原子を含む二座配位子を有するランタノイド錯体又はハロゲン原子を含む三座配位子を有するランタノイド錯体が粒子状である場合、ランタノイド錯体の平均粒子径の好ましい下限は0.01μm、好ましい上限は10μmであり、より好ましい下限は0.03μm、より好ましい上限は1μmである。
これらは単独で用いてもよく、2種以上を用いてもよい。
合わせガラス用中間膜の透明性がより一層高くなることから、xは1又は2であることが好ましく、ベンゼン環の2位又は5位に水酸基を有することがより好ましく、ベンゼン環の2位及び5位に水酸基を有することが更に好ましい。
上記R1の有機基は炭化水素基であることが好ましく、炭素数が1~10の炭化水素基であることがより好ましく、炭素数が1~5の炭化水素基であることが更に好ましく、炭素数が1~3の炭化水素基であることが特に好ましい。
上記炭化水素基の炭素数が10以下であると、上記テレフタル酸エステル構造を有する発光材料を合わせガラス用中間膜に容易に分散させることができる。
上記炭化水素基はアルキル基であることが好ましい。
なかでも、コントラストがより一層高い画像を表示できることから、上記一般式(1)で表される構造を有する化合物はジエチル-2,5-ジヒドロキシルテレフタレート(Aldrich社製「2,5-ジヒドロキシテレフタル酸ジエチル」)であることが好ましい。
上記R2の有機基は炭化水素基であることが好ましく、炭素数が1~10の炭化水素基であることがより好ましく、炭素数が1~5の炭化水素基であることが更に好ましく、炭素数が1~3の炭化水素基であることが特に好ましい。
上記炭化水素基の炭素数が上記上限以下であると、上記テレフタル酸エステル構造を有する発光材料を合わせガラス用中間膜に容易に分散させることができる。
上記炭化水素基はアルキル基であることが好ましい。
上記一般式(2)中、NR3R4はアミノ基である。
R3及びR4は、水素原子であることが好ましい。
上記一般式(2)で表される構造を有する化合物のベンゼン環の水素原子のうち、一つの水素原子が上記アミノ基であってもよく、二つの水素原子が上記アミノ基であってもよく、三つの水素原子が上記アミノ基であってもよく、四つの水素原子が上記アミノ基であってもよい。
上記テレフタル酸エステル構造を有する発光材料の含有量が0.001重量部以上であると、光線が照射されることにより、コントラストがより一層高い画像を表示することができる。
上記テレフタル酸エステル構造を有する発光材料の含有量が15重量部以下であると、合わせガラス用中間膜の透明性がより一層高くなる。
上記テレフタル酸エステル構造を有する発光材料の含有量のより好ましい下限は0.01重量部、より好ましい上限は10重量部、更に好ましい下限は0.1重量部、更に好ましい上限は8重量部、特に好ましい下限は0.5重量部、特に好ましい上限は5重量部である。
上記テレフタル酸エステル構造を有する発光材料の含有量が0.007重量%以上であると、コントラストがより一層高い画像を表示することができる。
上記テレフタル酸エステル構造を有する発光材料の含有量が4.5重量%以下であると、合わせガラス用中間膜の透明性がより一層高くなる。
上記テレフタル酸エステル構造を有する発光材料の含有量のより好ましい下限は0.01重量%、より好ましい上限は4重量%、更に好ましい下限は0.1重量%、更に好ましい上限は3.5重量%である。
カリウム、ナトリウム及びマグネシウムの合計の含有量を50ppm以下とすることにより、併用する上記ハロゲン原子を含む二座配位子を有するランタノイド錯体又はハロゲン原子を含む三座配位子を有するランタノイド錯体の発光性が低下するのを防止することができる。
上記分散剤は、例えば、直鎖アルキルベンゼンスルホン酸塩等のスルホン酸構造を有する化合物や、ジエステル化合物、リシノール酸アルキルエステル、フタル酸エステル、アジピン酸エステル、セバシン酸エステル、リン酸エステル等のエステル構造を有する化合物や、ポリオキシエチレングリコール、ポリオキシプロピレングリコールやアルキルフェニル-ポリオキシエチレン-エーテル等のエーテル構造を有する化合物や、ポリカルボン酸等のカルボン酸構造を有する化合物や、ラウリルアミン、ジメチルラウリルアミン、オレイルプロピレンジアミン、ポリオキシエチレンの2級アミン、ポリオキシエチレンの3級アミン、ポリオキシエチレンのジアミン等のアミン構造を有する化合物や、ポリアルキレンポリアミンアルキレンオキシド等のポリアミン構造を有する化合物や、オレイン酸ジエタノールアミド、アルカノール脂肪酸アミド等のアミド構造を有する化合物や、ポリビニルピロリドン、ポリエステル酸アマイドアミン塩等の高分子量型アミド構造を有する化合物等の分散剤を用いることができる。また、ポリオキシエチレンアルキルエーテルリン酸(塩)や高分子ポリカルボン酸、縮合リシノール酸エステル等の高分子量分散剤を用いてもよい。なお、高分子量分散剤とは、その分子量が1万以上である分散剤と定義される。
コントラストがより一層高い画像を表示できる合わせガラス用中間膜が得られることから、上記合わせガラス用中間膜中における上記紫外線吸収剤の含有量は、上記熱可塑性樹脂100重量部に対する好ましい上限は1重量部、より好ましい上限は0.5重量部、更に好ましい上限は0.2重量部、特に好ましい上限は0.1重量部である。
上記可塑剤は特に限定されず、例えば、一塩基性有機酸エステル、多塩基性有機酸エステル等の有機エステル可塑剤、有機リン酸可塑剤、有機亜リン酸可塑剤等のリン酸可塑剤等が挙げられる。上記可塑剤は液状可塑剤であることが好ましい。
上記酸化防止剤は特に限定されず、フェール構造を有する酸化防止剤、硫黄を含む酸化防止剤、リンを含む酸化防止剤等が挙げられる。
上記フェノール構造を有する酸化防止剤はフェノール骨格を有する酸化防止剤である。上記フェノール構造を有する酸化防止剤としては、例えば、2,6-ジ-t-ブチル-p-クレゾール(BHT)、ブチル化ヒドロキシアニソール(BHA)、2,6-ジ-t-ブチル-4-エチルフェノール、ステアリル-β-(3,5-ジ-t-ブチル-4-ヒドロキシフェニル)プロピオネート、2,2’-メチレンビス-(4-メチル-6-ブチルフェノール)、2,2’-メチレンビス-(4-エチル-6-t-ブチルフェノール)、4,4’-ブチリデン-ビス-(3-メチル-6-t-ブチルフェノール)、1,1,3-トリス-(2-メチル-ヒドロキシ-5-t-ブチルフェニル)ブタン、テトラキス[メチレン-3-(3’,5’-ブチル-4-ヒドロキシフェニル)プロピオネート]メタン、1,3,3-トリス-(2-メチル-4-ヒドロキシ-5-t-ブチルフェノール)ブタン、1,3,5-トリメチル-2,4,6-トリス(3,5-ジ-t-ブチル-4-ヒドロキシベンジル)ベンゼン、ビス(3,3’-t-ブチルフェノール)ブチリックアシッドグリコールエステル、ペンタエリスリトールテトラキス[3-(3,5-ジ-tert-ブチル-4-ヒドロキシフェニル)プロピオナート]等が挙げられる。上記酸化防止剤は、単独で用いてもよいし、2種以上を併用してもよい。
上記合わせガラス用中間膜が多層構造である場合、上記発光材料を含む発光層は合わせガラス用中間膜の全面に配置されていてもよく、一部にのみ配置されていてもよく、合わせガラス用中間膜の厚み方向とは垂直の面方向の全面に配置されていてもよく、一部にのみ配置されていてもよい。上記発光材料を含む発光層が一部にのみ配置されている場合には、該一部を発光エリア、他の部分を非発光エリアとして、発光エリアにおいてのみ情報を表示できるようにすることができる。
例えば、上記合わせガラス用中間膜に遮音性能を付与するために、上記発光材料を含む発光層における熱可塑性樹脂100重量部に対する可塑剤の含有量(以下、含有量Xともいう。)を、他の層における熱可塑性樹脂100重量部に対する可塑剤の含有量(以下、含有量Yともいう。)よりも多くすることができる。この場合、上記含有量Xは上記含有量Yよりも5重量部以上多いことが好ましく、10重量部以上多いことがより好ましく、15重量部以上多いことが更に好ましい。合わせガラス用中間膜の耐貫通性がより一層高くなることから、上記含有量Xと上記含有量Yとの差は、50重量部以下であることが好ましく、40重量部以下であることがより好ましく、35重量部以下であることが更に好ましい。なお、上記含有量Xと上記含有量Yとの差は、(上記含有量Xと上記含有量Yとの差)=(上記含有量X-上記含有量Y)により算出される。
上記含有量Yの好ましい下限は20重量部、好ましい上限は45重量部であり、より好ましい下限は30重量部、より好ましい上限は43重量部であり、更に好ましい下限は35重量部、更に好ましい上限は41重量部である。上記含有量Yを上記好ましい下限以上とすることにより、高い耐貫通性を発揮することができる。上記含有量Yを上記好ましい上限以下とすることにより、可塑剤のブリードアウトの発生を抑止し、合わせガラス用中間膜の透明性や接着性の低下を防止することができる。
上記ポリビニルアセタールXの水酸基量は、水酸基が結合しているエチレン基量を、主鎖の全エチレン基量で除算して求めたモル分率を百分率(モル%)で表した値である。上記水酸基が結合しているエチレン基量は、例えば、JIS K6728「ポリビニルブチラール試験方法」に準拠した方法により、上記ポリビニルアセタールXの水酸基が結合しているエチレン基量を測定することにより求めることができる。
上記アセタール基量は、JIS K6728「ポリビニルブチラール試験方法」に準拠した方法により、上記ポリビニルアセタールXのアセタール基が結合しているエチレン基量を測定することにより求めることができる。
上記アセチル基量は、主鎖の全エチレン基量から、アセタール基が結合しているエチレン基量と、水酸基が結合しているエチレン基量とを差し引いた値を、主鎖の全エチレン基量で除算して求めたモル分率を百分率(モル%)で表した値である。
なお、ポリビニルアセタールYの水酸基量、アセタール基量、及び、アセチル基量は、ポリビニルアセタールXと同様の方法で測定できる。
上記熱線吸収剤は、赤外線を遮蔽する性能を有すれば特に限定されないが、錫ドープ酸化インジウム(ITO)粒子、アンチモンドープ酸化錫(ATO)粒子、アルミニウムドープ酸化亜鉛(AZO)粒子、インジウムドープ酸化亜鉛(IZO)粒子、錫ドープ酸化亜鉛粒子、珪素ドープ酸化亜鉛粒子、6ホウ化ランタン粒子及び6ホウ化セリウム粒子からなる群より選択される少なくとも1種が好適である。
上記合わせガラス用中間膜が多層構造である場合、上記発光材料を含む発光層の厚さは特に限定されないが、好ましい下限は50μm、好ましい上限は1000μmである。上記発光材料を含む発光層の厚さがこの範囲内であると、特定の波長の光線を照射したときに充分にコントラストの高い発光が得られる。上記発光材料を含む発光層の厚さのより好ましい下限は80μm、より好ましい上限は500μm、更に好ましい下限は90μm、更に好ましい上限は300μmである。
上記ガラス板は、一般に使用されている透明板ガラスを使用することができる。例えば、フロート板ガラス、磨き板ガラス、型板ガラス、網入りガラス、線入り板ガラス、着色された板ガラス、熱線吸収ガラス、熱線反射ガラス、グリーンガラス等の無機ガラスが挙げられる。また、ガラスの表面に紫外線遮蔽コート層が形成された紫外線遮蔽ガラスも用いることができるが、特定の波長の光線を照射する側とは反対のガラス板として用いることが好ましい。更に、上記ガラス板としてポリエチレンテレフタレート、ポリカーボネート、ポリアクリレート等の有機プラスチックス板を用いることもできる。
上記ガラス板として、2種類以上のガラス板を用いてもよい。例えば、透明フロート板ガラスと、グリーンガラスのような着色されたガラス板との間に、上記合わせガラス用中間膜を積層した合わせガラスが挙げられる。また、上記ガラス板として、2種以上の厚さの異なるガラス板を用いてもよい。
上記照射する光線の出力の下限は、合わせガラスを1cd/m2以上の輝度で発光させることができる出力であれば特に限定されないが、好ましい下限は0.1mW、より好ましい下限は0.2mW、更に好ましい下限は0.4mWである。
なお、上記照射する光線の出力は、光源より10cm離れた位置に配置したレーザーパワーメーター(例えば、オフィールジャパン社製、「ビームトラックパワー測定センサー3A-QUAD」等)を用いた照射強度測定により測定することができる。
なお、上記照射する光線の密度は、光源より10cm離れた位置に配置した紫外線積算光量計(例えば、ウシオ電機社製、「UIT-250」等)を用いて、単位面積当たりの紫外線積算光量測定により測定することができる。
なお、上記照射する光線の照射径は、光源より10cm離れた位置に配置したCCDセンサー及びCMOSセンサー(例えば、コヒレント・ジャパン株式会社製、「USB2.0 ビーム診断カメラ Laser Cam HR」等)による測定結果をもとに、ISO11146規格によって算出することができる。
なお、上記合わせガラスの輝度の測定は、400nm以上の波長において上記発光材料の発光が最大の強度を示す波長又は405nmの波長で行われることが好ましく、405nmの波長で行われることがより好ましい。
本発明のディスプレイ装置は、特にナイトビジョンに好適に用いることができることができる。
本発明のディスプレイ装置は、特に車両のフロントガラスに好適に用いることができることができる。
(1)Eu(TFA)3phenの調製
酢酸ユーロピウム(Eu(CH3COO)3)12.5mmolを50mLの蒸留水へ溶かし、トリフルオロアセチルアセトン(TFA、CH3COCH2COCF3)33.6mmolを加え、室温で3時間撹拌した。沈殿した固体を濾過、水洗後、メタノールと蒸留水で再結晶を行なってEu(TFA)3(H2O)2を得た。得られた錯体Eu(TFA)3(H2O)25.77gと1,10-フェナントロリン(phen)2.5gを100mLのメタノールに溶かし、12時間加熱還流を行なった。12時間後、メタノールを減圧留去により取り除き、白色生成物を得た。この粉末をトルエンで洗浄し、未反応の原料を吸引濾過により取り除いた後、トルエンを減圧留去し、紛体を得た。トルエン、ヘキサンの混合溶媒により再結晶を行なうことにより、Eu(TFA)3phenを得た。
攪拌機を取り付けた2m3反応器に、PVA(重合度1700、けん化度99モル%)の7.5質量%水溶液1700kgとn-ブチルアルデヒド74.6kg、2,6-ジ-t-ブチル-4-メチルフェノール0.13kgを仕込み、全体を14℃に冷却した。これに、濃度30質量%の硝酸99.44Lを添加して、PVAのブチラール化を開始した。添加終了後から10分後に昇温を開始し、90分かけて65℃まで昇温し、更に120分反応を行なった。その後、室温まで冷却して析出した固形分を濾過後、固形分に対して質量で10倍量のイオン交換水で10回洗浄した。その後、0.3質量%の炭酸水素ナトリウム水溶液を用いて十分に中和を行ない、更に固形分に対して質量で10倍量のイオン交換水で10回洗浄し、脱水した後、乾燥させ、ポリビニルブチラール樹脂1(PVB1)を得た。
トリエチレングリコールジ-2-エチルヘキサノエート(3GO)40重量部に、得られたEu(TFA)3phen0.2重量部を加え、発光性の可塑剤溶液を調製した。得られた可塑剤溶液の全量と、得られたポリビニルブチラール1を100重量部とをミキシングロールで充分に混練することにより樹脂組成物を調製した。
得られた樹脂組成物を、押出機を用いて押出し、合わせガラス用中間膜(厚み760μm)を得た。
なお、得られた合わせガラス用中間膜について、ICP発光分析装置(島津製作所社製、「ICPE-9000」)を用いてナトリウム、カリウム及びマグネシウムの含有量の合計を測定したところ、50ppm以下であった。
得られた合わせガラスに、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が0.4mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が204mW/cm2となるように設定した水銀光源(朝日分光社製、「REX-250」)を照射装置として組み合わせてディスプレイ装置を得た。
(1)Tb(TFA)3phenの調製
酢酸テリビウム(Tb(CH3COO)3)12.5mmolを50mLの蒸留水へ溶かし、トリフルオロアセチルアセトン(TFA、CH3COCH2COCF3)33.6mmolを加え、室温で3時間撹拌した。沈殿した固体を濾過、水洗後、メタノールと蒸留水で再結晶を行なってTb(TFA)3(H2O)2を得た。得られた錯体Tb(TFA)3(H2O)25.77gと1,10-フェナントロリン(phen)2.5gを100mLのメタノールに溶かし、12時間加熱還流を行なった。12時間後、メタノールを減圧留去により取り除き、白色生成物を得た。この粉末をトルエンで洗浄し、未反応の原料を吸引濾過により取り除いた後、トルエンを減圧留去し、紛体を得た。トルエン、ヘキサンの混合溶媒により再結晶を行なうことにより、Tb(TFA)3phenを得た。
Eu(TFA)3phenを、得られたTb(TFA)3phenに変更した以外は実施例1と同様にして、合わせガラス用中間膜及び合わせガラスを作製した。また、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、照射装置を光線の出力が0.4mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が204mW/cm2であるように照射装置を調整した以外は実施例1と同様にして、ディスプレイ装置を製造した。
光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が10mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が50955mW/cm2であるように照射装置を調整したこと以外は、実施例1と同様にディスプレイ装置を製造した。
Eu(TFA)3phenを、ナフタルイミド(4,5-ジメチルオキシ-N-(2-エチルオキシル)ナフタルイミド)に変更した以外は実施例1と同様にして、合わせガラス用中間膜及び合わせガラスを作製した。また、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が0.4mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が204mW/cm2であるように照射装置を調整した以外は実施例1と同様にして、ディスプレイ装置を製造した。
(1)Eu(HFA)3phenの調製
酢酸ユーロピウム(Eu(CH3COO)3)3.38g(12.5mmol)を50mLの蒸留水へ溶かし、ヘキサフルオロアセトン(HFA、CF3COCH2COCF3)7.00g(33.6mmol)を加え、室温で3時間撹拌した。沈殿した固体を濾過、水洗後、メタノールと蒸留水で再結晶を行なってEu(HFA)3(H2O)2を得た。得られた錯体Eu(HFA)3(H2O)27.20gと1,10-フェナントロリン(phen)2.5gを100mLのメタノールに溶かし、12時間加熱還流を行なった。12時間後、メタノールを減圧留去により取り除き、白色生成物を得た。この粉末をトルエンで洗浄し、未反応の原料を吸引濾過により取り除いた後、トルエンを減圧留去し、紛体を得た。トルエン、ヘキサンの混合溶媒により再結晶を行なうことにより、Eu(HFA)3phenを得た。
Eu(TFA)3phenを、得られたEu(HFA)3phenに変更した以外は実施例1と同様にして、合わせガラス用中間膜及び合わせガラスを作製した。また、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が509mW/cm2であるように照射装置を調整した以外は実施例1と同様にして、ディスプレイ装置を製造した。
Eu(HFA)3phenの含有量を表2に示す値に変更し、照射装置の光線の出力、照射径、光線の密度を表2に示す値に変更した以外は、実施例3と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
(1)Tb(HFA)3phenの調製
酢酸テリビウム(Tb(CH3COO)3)3.46g(12.5mmol)を50mLの蒸留水へ溶かし、ヘキサフルオロアセチルアセトン(HFA、CF3COCH2COCF3)7.00g(33.6mmol)を加え、室温で3時間撹拌した。沈殿した固体を濾過、水洗後、メタノールと蒸留水で再結晶を行なってTb(HFA)3(H2O)2を得た。得られた錯体Tb(HFA)3(H2O)27.26gと1,10-フェナントロリン(phen)2.5gを100mLのメタノールに溶かし、12時間加熱還流を行なった。12時間後、メタノールを減圧留去により取り除き、白色生成物を得た。この粉末をトルエンで洗浄し、未反応の原料を吸引濾過により取り除いた後、トルエンを減圧留去し、紛体を得た。トルエン、ヘキサンの混合溶媒により再結晶を行なうことにより、Tb(HFA)3phenを得た。
Eu(TFA)3phenを、得られたTb(HFA)3phenに変更した以外は実施例1と同様にして、合わせガラス用中間膜及び合わせガラスを作製した。また、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が365nm、照射径が0.05cmφ、光線の密度が509mW/cm2であるように照射装置を調整した以外は実施例1と同様にして、ディスプレイ装置を製造した。
Tb(HFA)3phenの配合量を表2に示す値に変更し、照射装置の光線の出力、照射径、光線の密度を表2に示す値に変更した以外は、実施例7と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
Eu(TFA)3phenを、ジエチル-2,5-ジヒドロキシテレフタレート(Aldrich社製、「2,5-ジヒドロキシテレフタル酸ジエチル」)に変更した以外は実施例1と同様にして、合わせガラス用中間膜及び合わせガラスを作製した。また、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が509mW/cm2であるように照射装置を調整した以外は実施例1と同様にして、ディスプレイ装置を製造した。
ジエチル-2,5-ジヒドロキシテレフタレートの含有量を表2、表3に示す値に変更し、照射装置の光線の出力、照射径、光線の密度を表2、表3に示す値に変更した以外は、実施例11と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
発光材料の種類、発光材料の含有量、照射装置の光線の出力、波長、照射径、密度を表3に示すように変更した以外は、実施例1と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
(1)合わせガラス用中間膜及び合わせガラスの製造
トリエチレングリコールジ-2-エチルヘキサノエート(3GO)40重量部に、実施例3で得られたEu(HFA)3phen0.2重量部及び紫外線吸収剤として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(BASF社製「Tinuvin326」) 0.2重量部を加え、発光性の可塑剤溶液を調製した。得られた可塑剤溶液の全量と、得られたポリビニルブチラール1 100重量部とをミキシングロールで充分に混練することにより樹脂組成物を調製した。
得られた樹脂組成物を、押出機を用いて押出し、合わせガラス用中間膜(厚み760μm)を得た。
なお、得られた合わせガラス用中間膜について、ICP発光分析装置(島津製作所社製、「ICPE-9000」)を用いてナトリウム、カリウム及びマグネシウムの含有量の合計を測定したところ、0ppmであった。
得られた合わせガラスに、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が509mW/cm2となるように設定した水銀光源(朝日分光社製、「REX-250」)を照射装置として組み合わせてディスプレイ装置を得た。
発光材料の種類、発光材料の含有量、照射装置の光線の波長を表4に示すように変更した以外は、実施例15と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
(1)第1、第2の樹脂層用樹脂組成物の調製
トリエチレングリコールジ-2-エチルヘキサノエート(3GO)40重量部と、ポリビニルブチラール1 100重量部とをミキシングロールで充分に混練することにより第1、第2の樹脂層用樹脂組成物を調製した。
攪拌機を取り付けた2m3反応器に、ポリビニルアルコール(重合度2400、けん化度88モル%)の7.5質量%水溶液1700kgとn-ブチルアルデヒド119.4kg、2,6-ジ-t-ブチル-4-メチルフェノール0.13kgを仕込み、全体を14℃に冷却した。これに、濃度30質量%の硝酸99.44Lを添加して、ポリビニルアルコールのブチラール化を開始した。添加終了後から10分後に昇温を開始し、90分かけて65℃まで昇温し、更に120分反応を行なった。その後、室温まで冷却して析出した固形分を濾過後、固形分に対して質量で10倍量のイオン交換水で10回洗浄した(中和前の洗浄)。その後、0.3質量%の炭酸水素ナトリウム水溶液を用いて十分に中和を行ない、更に固形分に対して質量で10倍量のイオン交換水で10回洗浄し(中和後の洗浄)、脱水した後、乾燥させ、ポリビニルブチラール2(以下、「PVB2」ともいう。)を得た。なお、PVB2のアセチル基量は12モル%、ブチラール基量は65モル%、水酸基量は23モル%であった。トリエチレングリコールジ-2-エチルヘキサノエート(3GO)60重量部に、実施例3で得られたEu(HFA)3phen 0.5重量部を加え、発光性の可塑剤溶液を調製した。得られた可塑剤溶液の全量と、ポリビニルブチラール2 100重量部とをミキシングロールで充分に混練することにより、発光層用樹脂組成物を調製した。
発光層用樹脂組成物、及び、第1、第2の樹脂層用樹脂組成物を、共押出機を用いて共押出し、第1の樹脂層と発光層と第2の樹脂層とがこの順に積層された合わせガラス用中間膜を得た。なお、発光層の厚みは100μm、第1、第2の樹脂層の厚みはそれぞれ350μmであり、合わせガラス用中間膜の厚みは800μmであり、全ての層の形状が矩形状であった。
得られた合わせガラスに、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が509mW/cm2となるように設定した水銀光源(朝日分光社製、「REX-250」)を照射装置として組み合わせてディスプレイ装置を得た。
発光材料の種類、照射装置の光線の波長を表5に示すように変更した以外は、実施例18と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
(1)合わせガラス用中間膜及び合わせガラスの製造
実施例18で得られた発光層用樹脂組成物、及び、第1、第2の樹脂層用樹脂組成物を、共押出機を用いて共押出し、第1の樹脂層と発光層と第2の樹脂層とがこの順に積層された合わせガラス用中間膜を得た。その際、共押出機の金型の形状を、矩形状であり厚み100μmである発光層、楔形状であり厚い部分の厚みが600μm、薄い部分の厚みが350μmである第1の樹脂層、及び、楔形状であり厚い部分の厚みが600μm、薄い部分の厚みが350μmである第2の樹脂層が得られるように変更した。なお、得られた中間膜の押出方向に対する垂直方向における一端と他端の最短距離を測定すると1mであった。
得られた合わせガラスに、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が509mW/cm2となるように設定した水銀光源(朝日分光社製、「REX-250」)を照射装置として組み合わせてディスプレイ装置を得た。
発光材料の種類、照射装置の光線の波長を表5に示すように変更した以外は、実施例21と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
(1)第1、第2の発光層用樹脂組成物の調製
トリエチレングリコールジ-2-エチルヘキサノエート(3GO)40重量部に、実施例3で得られたEu(HFA)3phen0.22重量部を加え、発光性の可塑剤溶液を調製した。得られた可塑剤溶液の全量と、得られたポリビニルブチラール1 100重量部とをミキシングロールで充分に混練することにより第1、第2の発光層用樹脂組成物を調製した。
トリエチレングリコールジ-2-エチルヘキサノエート(3GO)60重量部と、ポリビニルブチラール2 100重量部とをミキシングロールで充分に混練することにより非発光層用樹脂組成物を調製した。
非発光層用樹脂組成物、及び、第1、第2の発光層用樹脂組成物を、共押出機を用いて共押出し、第1の発光層と非発光層と第2の発光層とがこの順に積層された合わせガラス用中間膜を得た。なお、非発光層の厚みは100μm、第1、第2の発光層の厚みはそれぞれ350μmであり、合わせガラス用中間膜の厚みは800μmであり、全ての層の形状が矩形状であった。
得られた合わせガラスに、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が509mW/cm2となるように設定した水銀光源(朝日分光社製、「REX-250」)を照射装置として組み合わせてディスプレイ装置を得た。
発光材料の種類、照射装置の光線の波長を表6に示すように変更した以外は、実施例24と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
(1)合わせガラス用中間膜及び合わせガラスの製造
実施例24で得られた非発光層用樹脂組成物、及び、第1、第2の発光層用樹脂組成物を、共押出機を用いて共押出し、第1の発光層と非発光層と第2の発光層とがこの順に積層された合わせガラス用中間膜を得た。その際、共押出機の金型の形状を、矩形状であり厚み100μmである非発光層、楔形状であり厚い部分の厚みが600μm、薄い部分の厚みが350μmである第1の発光層、及び、楔形状であり厚い部分の厚みが600μm、薄い部分の厚みが350μmである第2の発光層が得られるように変更した。なお、得られた中間膜の押出方向に対する垂直方向における一端と他端の最短距離を測定すると1mであった。
得られた合わせガラスに、光源の出力調整、専用のバンドパスフィルター(朝日分光社製、「LX0405」)、ロッドレンズ(朝日分光社製)及びファイバー(朝日分光社製)によって、光線の出力が1mW、光線の波長が405nm、照射径が0.05cmφ、光線の密度が509mW/cm2となるように設定した水銀光源(朝日分光社製、「REX-250」)を照射装置として組み合わせてディスプレイ装置を得た。
発光材料の種類、照射装置の光線の波長を表6に示すように変更した以外は、実施例27と同様にして、合わせガラス用中間膜、合わせガラス及びディスプレイ装置を製造した。
実施例及び比較例で得られた合わせガラスについて、以下の方法で光線を照射したときの輝度の評価及び安全性の評価を行った。
結果を表1~表6に示した。
実施例1~29及び比較例1~9で得られた縦5cm×横5cmの合わせガラスを、暗室下に配置し、合わせガラスの面に対して垂直方向に10cm離れた位置に実施例1~29及び比較例1~9の照射装置を配置した。次に、光を照射した合わせガラスの面から45度の角度で、合わせガラスの面からの最短距離が35cmとなる位置であり、かつ光を照射した側に配置した輝度計(トプコンテクノハウス社製、「SR-3AR」)を配置した。そして、照射装置から合わせガラスへと光を照射し、合わせガラスの輝度を測定した。
輝度の測定は、合わせガラスを100℃、4週間熱処理する前後において行った。
また、輝度の測定は、合わせガラスの中央部及び端部(サンプルの端から2cmの部位)において行った。
合わせガラスの耐熱性について、中央部及び端部で測定した輝度の100℃、4週間熱処理前後での変化量の絶対値が5cd/m2以下であった場合を「○」と、5cd/m2を超えた場合を「×」と評価した。なお、初期輝度が5cd/m2未満である合わせガラスに関しては、耐熱性の評価を行わなかった。
実施例及び比較例で得られたディスプレイ装置を暗室下に静置し、作動させた。ディスプレイ装置に生じた像から1m離れた位置に観察者の眼が来るように、光源と同じ側に観察者を立たせた。20人の観察者に作動中のディスプレイ装置を観察させ、像が見やすいと感じた観察者が15人以上である場合を「○○」、10人以上15人未満である場合を「○」、10人未満である場合を「×」としてナイトビジョン性能を評価した。
ディスプレイ装置の安全性について、照射装置から照射される光線の出力が1mW以下である場合を「○」と、1mWを超える場合を「×」と評価した。
11 発光層
12 形状補助層
2 合わせガラス用中間膜
21 発光層
22 形状補助層
23 形状補助層
3 合わせガラス用中間膜
31 発光層
32 形状補助層
33 形状補助層
Claims (10)
- 一対のガラス板の間に、熱可塑性樹脂及び発光材料を含む合わせガラス用中間膜が積層された合わせガラスと、前記合わせガラスに光線を照射する照射装置とを有するディスプレイ装置であって、前記照射装置から照射される光線の出力が1mW以下であり、前記光線を前記合わせガラスに照射したときに、合わせガラスが1cd/m2以上の輝度で発光することを特徴とするディスプレイ装置。
- 照射装置から照射される光線の密度が0.1~550mW/cm2、かつ、照射径が0.005~3cmφであることを特徴とする請求項1記載のディスプレイ装置。
- ナイトビジョンに用いるものであることを特徴とする請求項1又は2記載のディスプレイ装置。
- 車両のフロントガラスに用いるものであることを特徴とする請求項1又は2記載のディスプレイ装置。
- 熱可塑性樹脂と、ハロゲン原子を含む多座配位子を有するランタノイド錯体とを含有する発光層を有し、出力が1mW以下の光線を照射したときに1.3~165cd/m2の輝度で発光することを特徴とする合わせガラス用中間膜。
- ハロゲン原子を含む多座配位子を有するランタノイド錯体は、ハロゲン原子を含む二座配位子を有するランタノイド錯体又はハロゲン原子を含む三座配位子を有するランタノイド錯体であることを特徴とする請求項5記載の合わせガラス用中間膜。
- 発光層に含まれるカリウム、ナトリウム及びマグネシウムの合計の含有量が50ppm以下であることを特徴とする請求項5又は6記載の合わせガラス用中間膜。
- ハロゲン原子は、フッ素原子であることを特徴とする請求項5、6又は7記載の合わせガラス用中間膜。
- 発光層は、ハロゲン原子を含むアセチルアセトン骨格を有する二座配位子を有するランタノイド錯体を含むことを特徴とする請求項5、6、7又は8記載の合わせガラス用中間膜。
- 請求項5、6、7、8又は9記載の合わせガラス用中間膜が一対のガラス板の間に積層されていることを特徴とする合わせガラス。
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MX2017000889A (es) * | 2014-08-01 | 2017-05-01 | Sekisui Chemical Co Ltd | Pelicula intermedia para vidrio laminado, y vidrio laminado. |
JP5973083B2 (ja) * | 2014-08-01 | 2016-08-23 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
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2015
- 2015-12-24 JP JP2016503471A patent/JP6027704B1/ja active Active
- 2015-12-24 CN CN202010919405.0A patent/CN112009049A/zh active Pending
- 2015-12-24 WO PCT/JP2015/086005 patent/WO2016104592A1/ja active Application Filing
- 2015-12-24 EP EP15873160.4A patent/EP3239113A4/en not_active Withdrawn
- 2015-12-24 MX MX2017007116A patent/MX2017007116A/es unknown
- 2015-12-24 KR KR1020177017707A patent/KR20170097060A/ko not_active Application Discontinuation
- 2015-12-24 CN CN201580027112.9A patent/CN106458745B/zh active Active
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2016
- 2016-10-11 JP JP2016199994A patent/JP6595963B2/ja active Active
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2017
- 2017-06-15 US US15/623,785 patent/US10636668B2/en active Active
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2020
- 2020-03-18 US US16/822,650 patent/US20200219731A1/en not_active Abandoned
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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JPWO2018181687A1 (ja) * | 2017-03-30 | 2019-04-04 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
KR20190091412A (ko) * | 2017-03-30 | 2019-08-06 | 세키스이가가쿠 고교가부시키가이샤 | 접합 유리용 중간막 및 접합 유리 |
JP2020073423A (ja) * | 2017-03-30 | 2020-05-14 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
KR102350188B1 (ko) | 2017-03-30 | 2022-01-14 | 세키스이가가쿠 고교가부시키가이샤 | 접합 유리용 중간막 및 접합 유리 |
US11685143B2 (en) | 2017-03-30 | 2023-06-27 | Sekisui Chemical Co., Ltd. | Intermediate film for laminated glasses, and laminated glass |
WO2020189784A1 (ja) * | 2019-03-20 | 2020-09-24 | 積水化学工業株式会社 | 熱可塑性フィルム、及び合わせガラス |
CN113573890A (zh) * | 2019-03-20 | 2021-10-29 | 积水化学工业株式会社 | 热塑性膜及夹层玻璃 |
US11801667B2 (en) | 2019-03-20 | 2023-10-31 | Sekisui Chemical Co., Ltd. | Thermoplastic film and laminated glass |
Also Published As
Publication number | Publication date |
---|---|
CN112009049A (zh) | 2020-12-01 |
US20170287369A1 (en) | 2017-10-05 |
EP3239113A4 (en) | 2018-06-27 |
JP6595963B2 (ja) | 2019-10-23 |
KR20170097060A (ko) | 2017-08-25 |
US20200219731A1 (en) | 2020-07-09 |
CN106458745B (zh) | 2020-09-29 |
JPWO2016104592A1 (ja) | 2017-04-27 |
JP2017095344A (ja) | 2017-06-01 |
US10636668B2 (en) | 2020-04-28 |
MX2017007116A (es) | 2017-08-18 |
CN106458745A (zh) | 2017-02-22 |
EP3239113A1 (en) | 2017-11-01 |
JP6027704B1 (ja) | 2016-11-16 |
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