WO2017131200A1 - Stratifié optique - Google Patents

Stratifié optique Download PDF

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Publication number
WO2017131200A1
WO2017131200A1 PCT/JP2017/003049 JP2017003049W WO2017131200A1 WO 2017131200 A1 WO2017131200 A1 WO 2017131200A1 JP 2017003049 W JP2017003049 W JP 2017003049W WO 2017131200 A1 WO2017131200 A1 WO 2017131200A1
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WO
WIPO (PCT)
Prior art keywords
oxide layer
layer
optical laminate
stress relaxation
polarizer
Prior art date
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PCT/JP2017/003049
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English (en)
Japanese (ja)
Inventor
幸大 宮本
智剛 梨木
Original Assignee
日東電工株式会社
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Application filed by 日東電工株式会社 filed Critical 日東電工株式会社
Priority to KR1020187021638A priority Critical patent/KR20180107116A/ko
Priority to CN201780008717.2A priority patent/CN108603965A/zh
Publication of WO2017131200A1 publication Critical patent/WO2017131200A1/fr

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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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/023—Optical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
    • 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
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/30—Polarising elements
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/02—Details
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/02—Details
    • H05B33/04—Sealing arrangements, e.g. against humidity
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/20—Inorganic coating
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/51—Elastic
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • B32B2307/7246—Water vapor barrier
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides

Definitions

  • the present invention relates to an optical laminate.
  • this invention relates to the optical laminated body which can function as a barrier film and a polarizing plate.
  • a barrier film is used for an image display device (for example, a liquid crystal display device, an organic electroluminescence (EL) display device).
  • an image display device for example, a liquid crystal display device, an organic electroluminescence (EL) display device.
  • a transparent oxide obtained by adding SiO 2 to an Al—Zn—O (aluminum-added zinc oxide) film as a barrier film having a high film forming speed, a low refractive index, and a good gas barrier property.
  • a material film has been proposed (Patent Document 1).
  • this transparent oxide film has extremely insufficient chemical resistance (for example, acid resistance and alkali resistance).
  • the present invention has been made to solve the above-described conventional problems, and an object of the present invention is to provide an optical layered body that functions as a barrier film and a polarizing plate and that suppresses the occurrence of cracks. It is in.
  • the stress relaxation layer has an elastic modulus of 0.01 MPa to 70 GPa and a thickness of 13 ⁇ m to 200 ⁇ m.
  • the optical layered body further includes a protective layer on at least one side of the polarizer.
  • the stress relaxation layer is made of an adhesive.
  • the stress relaxation layer includes two pressure-sensitive adhesive layers composed of the pressure-sensitive adhesive, and a stress relaxation body disposed between the two pressure-sensitive adhesive layers.
  • the thickness of the first oxide layer is 10 nm to 100 nm.
  • the thickness of the second oxide layer is 10 nm to 100 nm.
  • the optical laminate, moisture permeability is less than 3.0 ⁇ 10 -2 g / m 2 / 24hr.
  • the optical laminate, the gas barrier property is 1.0 ⁇ 10 -7 g / m 2 /24hr ⁇ 0.5g/m 2 / 24hr.
  • the optical laminate, the moisture permeability after dropping hydrochloric acid or sodium hydroxide solution is less than 1.0 ⁇ 10 -1 g / m 2 / 24hr.
  • a laminated structure of a first oxide layer containing ZnO, Al, and SiO 2 and a second oxide layer composed of SiO 2 is adopted as a barrier layer, and further a polarizer.
  • a polarizer By laminating the optical laminate, it is possible to realize an optical laminate having excellent moisture permeability and gas barrier properties and excellent chemical resistance, flexibility and heat resistance. That is, it is possible to realize an optical laminate that can exhibit an excellent function as a barrier film and a polarizing plate.
  • by providing a stress relaxation layer having a predetermined elastic modulus and thickness between the polarizer and the base material excellent characteristics as the barrier film and the polarizing plate as described above can be obtained. While maintaining, generation
  • FIG. 1 is a schematic cross-sectional view of an optical laminate according to one embodiment of the present invention.
  • the optical laminated body 100 of this embodiment has the polarizer 41, the stress relaxation layer 50, the base material 10, the 1st oxide layer 20, and the 2nd oxide layer 30 in this order.
  • the optical layered body according to the embodiment of the present invention can function as both a barrier film and a polarizing plate of an image display device.
  • protective layers 42 and / or 43 are provided on at least one side of the polarizer (in the illustrated example, protective layers 42 and 43 are provided on both sides of the polarizer 41).
  • the polarizer 41 can be introduced into the optical laminate as the polarizing plate 40.
  • the first oxide layer 20 may include ZnO, Al and SiO 2.
  • the second oxide layer 30 is composed of SiO 2.
  • the thickness of the first oxide layer 20 is preferably 10 nm to 100 nm.
  • the thickness of the second oxide layer 30 is preferably 10 nm to 100 nm.
  • the stress relaxation layer 50 has an elastic modulus of 0.01 MPa to 70 GPa and a thickness of 13 ⁇ m to 200 ⁇ m.
  • the stress relaxation layer may be composed of an adhesive or may be composed of a laminate of an adhesive and a stress relaxation body.
  • the stress relaxation layer is provided between the polarizer (polarizing plate) and the substrate, and the elastic modulus and thickness of the stress relaxation layer are set in the predetermined range, whereby the stress and Strain propagation is mitigated.
  • the generation of cracks mainly resulting from the contraction of the polarizer is remarkably suppressed, and the excellent barrier property due to the laminated structure of the first oxide layer and the second oxide layer can be maintained.
  • the polarizer and the barrier film (a laminate of the base material, the first oxide layer, and the second oxide layer). This is because the thickness of the image display device and the manufacturing process are reduced. Can contribute significantly to simplification. This is a knowledge obtained by trial and error in order to solve the problem recognized only after integrating the polarizer and the barrier film, and is an unexpectedly excellent effect.
  • the optical layered body has a barrier property against moisture and gas (for example, oxygen).
  • the water vapor transmission rate at 90% RH conditions is preferably 1.0 ⁇ 10 -1 g / m less than 2/24 hr or.
  • the lower the lower limit of moisture permeability the better.
  • Measurement limit of moisture permeability for example, 0.1 ⁇ 10 -6 g / m 2 / 24hr approximately.
  • the lower limit of the moisture permeability for example, 0.1 ⁇ 10 -4 g / m 2 / 24hr.
  • the preferable upper limit of moisture permeability can vary depending on the application.
  • the upper limit of moisture permeability for example, an image display device of the indoor (e.g., PC display) in applications was 5.0 ⁇ 10 -2 g / m 2 / 24hr, outdoor image display apparatus in (digital signage) applications 3.0 ⁇ a 10 -2 g / m 2 / 24hr , the indoor harsh environment applications such as automotive display is 1.0 ⁇ 10 -2 g / m 2 / 24hr. 60 ° C. of the optical stack, gas barrier properties 90% RH conditions is preferably 1.0 ⁇ 10 -7 g / m 2 /24hr ⁇ 0.5g/m 2 / 24hr, more preferably 1.
  • moisture permeability and gas barrier properties are within such ranges, when the optical laminate is bonded to the image display device, the image display device can be well protected from moisture and oxygen in the air. Both moisture permeability and gas barrier properties can be measured according to JIS K7126-1.
  • the optical layered body preferably has chemical resistance. More specifically, the optical laminate preferably has acid resistance and alkali resistance.
  • the term “acid resistance” means that a 2% hydrochloric acid solution (pH 0.3) is dropped onto the optical laminate, and the moisture permeability after wiping off the hydrochloric acid solution after 10 minutes is 1.0 ⁇ 10 ⁇ 1 g. / refers to m is less than 2/24 hr or.
  • the "alkali resistance” was added dropwise a 2% sodium hydroxide solution (pH 13.7) to the optical stack, moisture permeability after wiping sodium hydroxide solution after 10 minutes is 1.0 ⁇ 10 - It refers to less than 1 g / m 2 / 24hr.
  • the achievement of such excellent chemical resistance while maintaining the desired barrier properties and transparency as described above is one of the achievements of the present invention.
  • the optical layered body has a flexibility such that cracks and cracks do not occur even when it is bent with a curvature radius of 7 mm, more preferably with a curvature radius of 5 mm.
  • Optical stack are preferably 500 hours at 95 ° C., more preferably 600 hours, more preferably heat as moisture permeability be heated 700 hours is less than 1.0 ⁇ 10 -1 g / m 2 / 24hr Have sex.
  • the optical layered body of the present invention is elongated.
  • the long optical laminate can be stored and / or transported, for example, wound in a roll. Since the optical layered body is excellent in flexibility, no problem occurs even if it is wound into a roll. In this case, the absorption axis direction of the polarizer is typically substantially parallel to the longitudinal direction. If it is such a structure, an optical laminated body can be produced by what is called a roll-to-roll.
  • a retardation layer (not shown) may be provided between the polarizing plate 40 and the stress relaxation layer 50 and / or on the side opposite to the base material of the polarizing plate 40.
  • Optical properties of the retardation layer for example, refractive index ellipsoid, in-plane retardation, thickness direction retardation, Nz coefficient, wavelength dispersion characteristic, photoelastic coefficient), mechanical characteristics, number of arrangements, combinations, etc.
  • a retardation layer that exhibits the wavelength dependence of reverse dispersion and can function as a so-called ⁇ / 4 plate can be disposed on the opposite side of the substrate of the polarizing plate 40.
  • the angle formed by the slow axis of the retardation layer and the absorption axis of the polarizer is typically about 45 °.
  • the polarizer 41 can typically be introduced into the optical laminate as the polarizing plate 40.
  • the polarizing plate 40 (substantially the protective layer 42 and the polarizer 41 when the protective layer 42 is not present) is typically bonded to the substrate 10 through the stress relaxation layer 50.
  • the resin film forming the polarizer may be a single-layer resin film or a laminate of two or more layers.
  • polarizers composed of a single-layer resin film include hydrophilic polymer films such as polyvinyl alcohol (PVA) films, partially formalized PVA films, and ethylene / vinyl acetate copolymer partially saponified films.
  • PVA polyvinyl alcohol
  • polyene-based oriented films such as those subjected to dyeing treatment and stretching treatment with dichroic substances such as iodine and dichroic dyes, PVA dehydrated products and polyvinyl chloride dehydrochlorinated products.
  • a polarizer obtained by dyeing a PVA film with iodine and uniaxially stretching is used because of excellent optical properties.
  • the dyeing with iodine is performed, for example, by immersing a PVA film in an aqueous iodine solution.
  • the stretching ratio of the uniaxial stretching is preferably 3 to 7 times.
  • the stretching may be performed after the dyeing treatment or may be performed while dyeing. Moreover, you may dye
  • the PVA film is subjected to swelling treatment, crosslinking treatment, washing treatment, drying treatment and the like. For example, by immersing the PVA film in water and washing it before dyeing, not only can the surface of the PVA film be cleaned of dirt and anti-blocking agents, but the PVA film can be swollen to cause uneven staining. Can be prevented.
  • a polarizer obtained by using a laminate a laminate of a resin substrate and a PVA resin layer (PVA resin film) laminated on the resin substrate, or a resin substrate and the resin
  • a polarizer obtained by using a laminate with a PVA resin layer applied and formed on a substrate examples thereof include a polarizer obtained by using a laminate with a PVA resin layer applied and formed on a substrate.
  • a polarizer obtained by using a laminate of a resin base material and a PVA resin layer applied and formed on the resin base material may be obtained by, for example, applying a PVA resin solution to a resin base material and drying it.
  • a PVA-based resin layer is formed thereon to obtain a laminate of a resin base material and a PVA-based resin layer; the laminate is stretched and dyed to make the PVA-based resin layer a polarizer; obtain.
  • stretching typically includes immersing the laminate in an aqueous boric acid solution and stretching.
  • the stretching may further include, if necessary, stretching the laminate in the air at a high temperature (for example, 95 ° C. or higher) before stretching in the aqueous boric acid solution.
  • the obtained resin base material / polarizer laminate may be used as it is (that is, the resin base material may be used as a protective layer of the polarizer), and the resin base material is peeled from the resin base material / polarizer laminate.
  • Any appropriate protective layer according to the purpose may be laminated on the release surface. Details of a method for manufacturing such a polarizer are described in, for example, Japanese Patent Application Laid-Open No. 2012-73580. This publication is incorporated herein by reference in its entirety.
  • the thickness of the polarizer is preferably 15 ⁇ m or less, more preferably 1 ⁇ m to 12 ⁇ m, still more preferably 3 ⁇ m to 10 ⁇ m, and particularly preferably 3 ⁇ m to 8 ⁇ m.
  • the thickness of the polarizer is in such a range, curling during heating can be satisfactorily suppressed, and good appearance durability during heating can be obtained.
  • the thickness of the polarizer is in such a range, it can contribute to the thinning of the optical laminate (as a result, the organic EL display device).
  • the polarizer preferably exhibits absorption dichroism at any wavelength between 380 nm and 780 nm.
  • the single transmittance of the polarizer is preferably 43.0% to 46.0%, more preferably 44.5% to 46.0%.
  • the polarization degree of the polarizer is preferably 97.0% or more, more preferably 99.0% or more, and further preferably 99.9% or more.
  • the protective layer 42 is formed of any suitable film that can be used as a protective layer for a polarizer.
  • the material as the main component of the film include cellulose resins such as triacetyl cellulose (TAC), polyester-based, polyvinyl alcohol-based, polycarbonate-based, polyamide-based, polyimide-based, polyethersulfone-based, and polysulfone-based materials.
  • transparent resins such as polystyrene, polynorbornene, polyolefin, (meth) acryl, and acetate.
  • thermosetting resins such as (meth) acrylic, urethane-based, (meth) acrylurethane-based, epoxy-based, and silicone-based or ultraviolet curable resins are also included.
  • a glassy polymer such as a siloxane polymer is also included.
  • a polymer film described in JP-A-2001-343529 (WO01 / 37007) can also be used.
  • a resin composition containing a thermoplastic resin having a substituted or unsubstituted imide group in the side chain and a thermoplastic resin having a substituted or unsubstituted phenyl group and nitrile group in the side chain for example, a resin composition having an alternating copolymer of isobutene and N-methylmaleimide and an acrylonitrile / styrene copolymer can be mentioned.
  • the polymer film can be, for example, an extruded product of the resin composition.
  • the optical layered body of the present invention is typically disposed on the viewing side of the image display device, and the protective layer 42 is typically disposed on the viewing side. Therefore, the protective layer 42 may be subjected to surface treatment such as hard coat treatment, antireflection treatment, antisticking treatment, and antiglare treatment as necessary. Further / or, if necessary, the protective layer 42 is provided with a treatment for improving visibility when viewed through polarized sunglasses (typically, an (elliptical) circular polarization function is imparted, an ultrahigh phase difference is provided. May be applied). By performing such processing, excellent visibility can be achieved even when the display screen is viewed through a polarizing lens such as polarized sunglasses. Therefore, the optical laminate can be suitably applied to an image display device that can be used outdoors.
  • polarized sunglasses typically, an (elliptical) circular polarization function is imparted, an ultrahigh phase difference is provided. May be applied.
  • the thickness of the protective layer 42 is preferably 20 ⁇ m to 200 ⁇ m, more preferably 30 ⁇ m to 100 ⁇ m, and still more preferably 35 ⁇ m to 95 ⁇ m.
  • the protective layer 43 is preferably optically isotropic.
  • “optically isotropic” means that the in-plane retardation Re (550) is 0 nm to 10 nm and the thickness direction retardation Rth (550) is ⁇ 10 nm to +10 nm.
  • the in-plane retardation Re (550) of the substrate is preferably 0 nm to 5 nm, and the thickness direction retardation Rth (550) is preferably -5 nm to +5 nm.
  • Rth (550) is a retardation in the thickness direction of the film measured with light having a wavelength of 550 nm at 23 ° C.
  • Re (nx ⁇ nz) ⁇ determined by d.
  • nx is the refractive index in the direction in which the in-plane refractive index is maximum (that is, the slow axis direction)
  • ny is the direction orthogonal to the slow axis in the plane (that is, fast phase). (Nz direction)
  • nz is the refractive index in the thickness direction.
  • the material, thickness, and the like of the protective layer 43 are as described above for the protective layer 42.
  • the protective layers 42 and 43 are typically bonded to the polarizer 41 via any appropriate adhesive layer (for example, a PVA resin adhesive layer).
  • the stress relaxation layer 50 has an elastic modulus (Young's modulus) at 95 ° C. of 0.01 MPa to 70 GPa as described above, preferably 0.03 MPa to 5 GPa, more preferably 0.05 MPa to 0.005. 3 GPa. If the elastic modulus of the stress relaxation layer is in such a range, the stress of the substrate due to the contraction of the polarizer can be relaxed well. As a result, the occurrence of cracks in the first oxide layer and / or the second oxide layer can be significantly suppressed.
  • an elastic modulus Young's modulus
  • the shear storage modulus G ′ (95 ° C.) at 95 ° C. of the stress relaxation layer is preferably 5.0 ⁇ 10 4 Pa to 1.0 ⁇ 10 11 Pa, more preferably 1.5 ⁇ 10 5 Pa to 7.0 ⁇ 10 9 Pa, more preferably 2.5 ⁇ 10 5 Pa to 4.0 ⁇ 10 8 Pa.
  • G ′ (95 ° C.) of the stress relaxation layer is in such a range, propagation of stress and the like due to the contraction of the polarizer can be relaxed satisfactorily. As a result, the occurrence of cracks in the first oxide layer and / or the second oxide layer can be significantly suppressed.
  • G ′ (95 ° C.) is measured by dynamic viscoelasticity measurement.
  • the thickness of the stress relaxation layer is 13 ⁇ m to 200 ⁇ m, preferably 15 ⁇ m to 200 ⁇ m, more preferably 20 ⁇ m to 150 ⁇ m. If the thickness of the stress relaxation layer is in such a range, the stress of the base material due to the contraction of the polarizer can be well relaxed by a synergistic effect with the above elastic modulus. That is, in the embodiment of the present invention, a stress relaxation layer is provided between the polarizer and the base material, and functions as a barrier film and a polarizing plate by combining and optimizing the elastic modulus and thickness. In the optical laminate, the occurrence of cracks in the first oxide layer and / or the second oxide layer can be remarkably suppressed while maintaining excellent properties as a barrier film and a polarizing plate.
  • the stress relaxation layer preferably has a total light transmittance of visible light (for example, light having a wavelength of 550 nm) of 85% or more, more preferably 90% or more, and still more preferably 95% or more. Further, the stress relaxation layer has a haze of preferably 1.5% or less, more preferably 1.0% or less.
  • the stress relaxation layer any appropriate configuration having the above characteristics can be adopted.
  • the stress relaxation layer may be composed of a pressure-sensitive adhesive, and a laminate of the pressure-sensitive adhesive and the stress relaxation body (more specifically, the two pressure-sensitive adhesive layers and the two pressure-sensitive adhesive layers). A laminate having a stress relieving body disposed therebetween).
  • any appropriate pressure-sensitive adhesive can be used for the stress relaxation layer as long as it has the above properties.
  • Specific examples include acrylic adhesives, rubber adhesives, vinyl alkyl ether adhesives, silicone adhesives, polyester adhesives, polyamide adhesives, urethane adhesives, fluorine adhesives, and epoxy adhesives.
  • An adhesive may be used independently and may be used in combination of 2 or more type. Arbitrary appropriate forms can also be employ
  • An acrylic pressure-sensitive adhesive is preferable. This is because the monomer component can be selected from a wide range, whereby the elastic modulus can be easily adjusted. Furthermore, the acrylic pressure-sensitive adhesive has excellent transparency and weather resistance, and also has an advantage of low cost.
  • the acrylic pressure-sensitive adhesive contains a (meth) acrylic polymer as a main component.
  • the content of the acrylic polymer in the pressure-sensitive adhesive is preferably 65 parts by weight or more (for example, from 65 parts by weight to 100 parts by weight), more preferably from 70 parts by weight to 100 parts by weight of the solid content of the pressure-sensitive adhesive. 99.999 parts by weight.
  • (meth) acryl means acryl and / or methacryl.
  • Typical monomer components constituting the (meth) acrylic polymer include alkyl (meth) acrylate, hydroxyalkyl (meth) acrylate, (meth) acrylic acid, heterocyclic-containing acrylic monomer, acrylamide, and glycidyl acrylate. It is done.
  • a pressure-sensitive adhesive having a desired elastic modulus can be obtained by adjusting the type, combination, copolymerization ratio, and the like of the monomer components.
  • the pressure-sensitive adhesive may contain a crosslinking agent.
  • the pressure-sensitive adhesive may contain any appropriate additive.
  • the additive include tackifiers, plasticizers, glass fibers, fillers, pigments, colorants, antioxidants, ultraviolet absorbers, silane coupling agents, and light diffusing fine particles. The content, type, number, combination, and the like of the additive can be appropriately set according to the purpose.
  • the pressure-sensitive adhesive can contain a filler (filler) for the purpose of controlling the elastic modulus.
  • a filler for the purpose of controlling the elastic modulus.
  • the filler are polystyrene, organic fillers made of an organic material such as polycarbonate; titania (TiO 2), silica (SiO 2), alumina (Al 2 O 3), zirconia (ZrO 2), calcia (CaO), magnesia Metal oxide or non-metal oxide such as (MgO), or copper (Cu), silver (Ag), gold (Au), aluminum (Al), palladium (Pd), titanium (Ti), nickel (Ni)
  • An inorganic filler made of a metal such as The blending ratio of the filler can be appropriately selected according to the type of filler and the target elastic modulus.
  • the filler can be contained, for example, in a proportion of 10% by weight to 70% by weight with respect to the total weight of the pressure-sensitive adhesive (pressure-sensitive adhesive composition).
  • Any appropriate shape may be adopted as the shape of the filler depending on the purpose. Specific examples include true sphere, oval sphere, needle shape, disk shape, star shape, and scale shape. Any appropriate size of the filler may be adopted depending on the purpose.
  • the size of the filler can vary, for example, from the nano order of about 10 nm to the micro order of about 10 ⁇ m. Details of the filler are described in, for example, WO2009 / 145005. The description of this publication is incorporated herein by reference.
  • the stress relaxation layer is composed of a laminate of an adhesive and a stress relief body (more specifically, a laminate having two adhesive layers and a stress relaxation body disposed between the two adhesive layers).
  • the stress relaxation body has a thermal shrinkage rate at 95 ° C. of preferably 0.5% or less, more preferably 0.3% or less, and still more preferably 0.1% or less.
  • the heat shrinkage rate can be measured according to JIS K 7133.
  • said adhesive can be used for an adhesive.
  • any appropriate material can be used as long as it has the above characteristics.
  • the materials are roughly classified into organic materials and inorganic materials.
  • organic materials include polyester polymers such as polyethylene terephthalate and polyethylene naphthalate, cellulose polymers such as diacetyl cellulose and triacetyl cellulose, acrylic polymers such as polymethyl methacrylate, polystyrene, acrylonitrile / styrene copolymers ( AS resin), styrene polymer, polycarbonate polymer, polyethylene, polypropylene, polyolefin having cyclo or norbornene structure, polyolefin polymer such as ethylene / propylene copolymer, vinyl chloride polymer, nylon, aromatic polyamide, etc.
  • polyester polymers such as polyethylene terephthalate and polyethylene naphthalate
  • cellulose polymers such as diacetyl cellulose and triacetyl cellulose
  • acrylic polymers such as polymethyl methacrylate, polystyrene, acrylonitrile / styrene copolymers ( AS resin), styrene poly
  • Amide polymer imide polymer, sulfone polymer, polyethersulfone polymer, polyetheretherketone polymer , Polyphenylene sulfide polymers, vinyl alcohol polymers, vinylidene chloride polymers, vinyl butyral polymers, arylate polymers, polyoxymethylene-based polymers, epoxy-based polymers. These polymers may be used alone or in combination (for example, blend, copolymerization) of two or more.
  • inorganic materials include silica glass such as soda lime glass and alkali-free glass, borosilicate glass, quartz glass, zirconia (ZrO 2 ), alumina (Al 2 O 3 ), fluorite (CaF 2), and the like. Sex crystals.
  • the stress relieving body may contain any appropriate additive depending on the purpose.
  • the additive include a filler, an ultraviolet absorber, an antioxidant, a lubricant, a plasticizer, a mold release agent, a coloring inhibitor, a flame retardant, a nucleating agent, an antistatic agent, a pigment, and a coloring agent.
  • the content, type, number, combination, and the like of the additive can be appropriately set according to the purpose. Details of the additive are as described for the pressure-sensitive adhesive. Further, the control of the elastic modulus is as described for the pressure-sensitive adhesive.
  • the base material 10 is preferably transparent.
  • the total light transmittance of visible light (for example, light having a wavelength of 550 nm) is preferably 85% or more, more preferably 90% or more, and further preferably 95% or more.
  • the substrate 10 is optically isotropic in one embodiment. With such a configuration, when the optical laminate is applied to an image display device, adverse effects on the display characteristics of the image display device can be prevented.
  • the average refractive index of the substrate is preferably less than 1.7, more preferably 1.59 or less, and further preferably 1.4 to 1.55.
  • the average refractive index is in such a range, there is an advantage that back surface reflection can be suppressed and high light transmittance can be achieved.
  • the surface roughness Ra of the surface on the first oxide layer side of the substrate is preferably 0.30 nm or more, more preferably 0.40 nm or more, still more preferably 0.50 nm or more, particularly preferably. Is 0.60 nm or more.
  • the upper limit of the surface roughness Ra of the surface is, for example, 50 nm. If the surface roughness of the surface is in such a range, as described above, excellent adhesion between the substrate and the first oxide layer is realized, and as a result, the first due to the contraction of the polarizer. Cracks in the oxide layer and / or the second oxide layer (typically cracks in the thickness direction) can be further significantly suppressed.
  • Such surface roughness can be realized by any appropriate roughening treatment. Examples of the roughening treatment include embossing, sand blasting, stretching and bending, and introduction of fine particles.
  • the surface roughness Ra can be measured according to JIS B 0601.
  • any appropriate material that can satisfy the above characteristics can be used.
  • the material constituting the substrate include resins having no conjugated system such as norbornene resins and olefin resins, resins having a cyclic structure such as a lactone ring and a glutarimide ring in the acrylic main chain, and polyester-based materials. Examples thereof include resins and polycarbonate resins. With such a material, when the base material is formed, the expression of the phase difference accompanying the orientation of the molecular chain can be kept small.
  • the base material may have a predetermined phase difference in another embodiment.
  • the substrate may have an in-plane retardation that can function as a so-called ⁇ / 4 plate.
  • a good circular polarization function is imparted to the optical laminate without separately providing a retardation layer, so that the optical laminate is not only used as a barrier film for an image display device but also an antireflection film.
  • the angle formed by the slow axis of the substrate and the absorption axis of the polarizer 41 is typically about 45 °.
  • Such a substrate can be formed, for example, by stretching a film of norbornene resin or polycarbonate resin under appropriate conditions.
  • the thickness of the substrate is preferably 10 ⁇ m to 50 ⁇ m or less, and more preferably 20 ⁇ m to 35 ⁇ m or less.
  • the first oxide layer 20 includes ZnO, Al, and SiO 2 as described above.
  • the first oxide layer preferably contains Al in a proportion of 2.5% to 3.5% by weight and SiO 2 preferably in a proportion of 20.0% to 62.4% by weight with respect to the total weight. .
  • ZnO is preferably the remaining amount.
  • the thickness of the first oxide layer is preferably 10 nm to 100 nm, more preferably 10 nm to 60 nm, and still more preferably 20 nm to 40 nm. If the thickness is in such a range, there is an advantage that both high light transmittance and excellent barrier properties can be achieved.
  • the average refractive index of the first oxide layer is preferably 1.59 to 1.80.
  • the average refractive index is in such a range, there is an advantage that high light transmittance can be achieved.
  • the first oxide layer is preferably transparent.
  • the first oxide layer preferably has a total light transmittance of visible light (for example, light having a wavelength of 550 nm) of 85% or more, more preferably 90% or more, and further preferably 95% or more. .
  • the first oxide layer can be typically formed on the substrate by sputtering.
  • the first oxide layer can be formed by a sputtering method in an inert gas atmosphere containing oxygen using, for example, a sputtering target containing Al, SiO 2 and ZnO.
  • a sputtering method a magnetron sputtering method, an RF sputtering method, an RF superimposed DC sputtering method, a pulse sputtering method, a dual magnetron sputtering method, or the like can be employed.
  • the heating temperature of the substrate is, for example, ⁇ 8 ° C. to 200 ° C.
  • the gas partial pressure of oxygen with respect to the whole atmospheric gas of oxygen and inert gas is, for example, 0.05 or more.
  • the second oxide layer 30 is made of SiO 2 (it may contain inevitable impurities). By forming such a second oxide layer on the surface of the first oxide layer, the chemical resistance and transparency of the optical laminate can be improved while maintaining good characteristics of the first oxide layer. It can be improved significantly. Furthermore, since the second oxide layer can function as a low refractive index layer, it is possible to impart good antireflection characteristics to the optical laminate.
  • the thickness of the second oxide layer is preferably 10 nm to 100 nm, more preferably 50 nm to 100 nm, and still more preferably 60 nm to 100 nm.
  • the thickness is in such a range, there is an advantage that both high light transmittance, excellent barrier properties, and excellent chemical resistance can be achieved.
  • the average refractive index of the second oxide layer is preferably 1.44 to 1.50.
  • the second oxide layer can function well as a low refractive index layer (antireflection layer).
  • the second oxide layer is preferably transparent.
  • the total light transmittance of visible light (for example, light having a wavelength of 550 nm) is preferably 85% or more, more preferably 90% or more, and further preferably 95% or more. .
  • the second oxide layer can be formed on the first oxide layer, typically by sputtering.
  • the second oxide layer is sputtered using, for example, Si, SiC, SiN, or SiO, and an inert gas containing oxygen (for example, argon, nitrogen, CO, CO 2 , or a mixed gas thereof). Can be formed. Since both the first oxide layer and the second oxide layer contain SiO 2 , the adhesion between the first oxide layer and the second oxide layer is very excellent. Therefore, in order to develop a sufficient barrier function at the interface between the first oxide layer and the second oxide layer, the thickness of the first oxide layer is 10 nm or more as described above. Is preferred.
  • the ratio of the so-called incubation layer, which is the initial growth film, can be sufficiently reduced, and an oxide layer having the desired physical properties can be formed.
  • the total thickness of the first oxide layer and the second oxide layer is preferably 200 nm or less, and more preferably 140 nm or less.
  • optical laminate of the present invention can be suitably used as an optical member having the functions of both a barrier layer (barrier film) and a polarizing plate of an image display device. More specifically, the optical laminate of the present invention can be used as an optical member of a liquid crystal display device and an organic EL display device, preferably an organic EL display device, more preferably a bendable organic EL display device.
  • the present invention will be specifically described by way of examples, but the present invention is not limited to these examples.
  • the measuring method of each characteristic is as follows.
  • the thicknesses of the first oxide layer and the second oxide layer were measured by observing a cross section using a transmission electron microscope (H-7650 manufactured by Hitachi, Ltd.). The thickness of other components of the optical laminate was measured using a film thickness meter (Digital Dial Gauge DG-205 manufactured by Peacock).
  • a film thickness meter Digital Dial Gauge DG-205 manufactured by Peacock.
  • the temperature dependence of the storage elastic modulus G ′ was measured by a dynamic viscoelasticity measuring device (trade name: ARES, manufactured by Rheometrics), The measured value G ′ (95 ° C.) at 95 ° C. was defined as the elastic modulus.
  • optical laminates obtained in the examples and comparative examples were cut into 50 mm ⁇ 50 mm sizes and used as measurement samples.
  • This measurement sample was bonded to quartz glass, stored in an oven at 95 ° C. for 1000 hours, measured for moisture permeability after storage, and evaluated according to the following criteria.
  • ⁇ 1.0 ⁇ 10 -1 g / m 2 / 24hr less
  • ⁇ 1.0 ⁇ 10 -1 g / m 2 / 24hr or more (4) obtained in moisture permeability
  • Comparative Examples optical laminate A 10 cm ⁇ circular shape was cut out and used as a measurement sample. About this measurement sample, moisture permeability was measured on 40 degreeC and 90% RH test conditions using "DELTATAPERM" by Technolox.
  • Example 1> (Production of laminated barrier film) A commercially available COP film (trade name “Zeonor”, manufactured by Nippon Zeon Co., Ltd., thickness 40 ⁇ m) is used as a base material, and a sputtering target containing Al, SiO 2 and ZnO is used to form the first on the base material by DC magnetron sputtering. An oxide layer (thickness 30 nm) was formed. Next, a second oxide layer (50 nm) was formed on the first oxide layer of the base material / first oxide layer stack using a Si target. In this way, a laminated barrier film having a configuration of base material / first oxide layer (AZO) / second oxide layer (SiO 2 ) was produced.
  • polarizer (Production of polarizer)
  • a long roll of polyvinyl alcohol (PVA) resin film (product name “PE3000”, manufactured by Kuraray Co., Ltd.) having a thickness of 30 ⁇ m is uniaxially stretched in the longitudinal direction so as to be 5.9 times in the longitudinal direction by a roll stretching machine.
  • Swelling, dyeing, crosslinking, and washing treatment were performed, and finally a drying treatment was performed to produce a polarizer having a thickness of 12 ⁇ m.
  • the swelling treatment was stretched 2.2 times while being treated with pure water at 20 ° C.
  • the dyeing treatment is performed in an aqueous solution at 30 ° C.
  • the weight ratio of iodine and potassium iodide is 1: 7, the iodine concentration of which is adjusted so that the single transmittance of the obtained polarizer is 45.0%.
  • the film was stretched 1.4 times.
  • the crosslinking treatment employed a two-stage crosslinking treatment, and the first-stage crosslinking treatment was stretched 1.2 times while being treated in an aqueous solution in which boric acid and potassium iodide were dissolved at 40 ° C.
  • the boric acid content of the aqueous solution of the first-stage crosslinking treatment was 5.0% by weight, and the potassium iodide content was 3.0% by weight.
  • the cross-linking treatment at the second stage was stretched 1.6 times while being treated in an aqueous solution in which boric acid and potassium iodide were dissolved at 65 ° C.
  • the boric acid content of the aqueous solution of the second crosslinking treatment was 4.3% by weight, and the potassium iodide content was 5.0% by weight.
  • the cleaning treatment was performed with an aqueous potassium iodide solution at 20 ° C.
  • the potassium iodide content of the aqueous solution for the washing treatment was 2.6% by weight.
  • the drying process was performed at 70 ° C. for 5 minutes to obtain a polarizer.
  • HC-TAC film (thickness 32 ⁇ m) having a hard coat (HC) layer formed on one side of the TAC film by a hard coat treatment on one side of the polarizer via a polyvinyl alcohol adhesive on the other side
  • a normal TAC film (thickness 25 ⁇ m) was bonded to each other with a roll-to-roll through a polyvinyl alcohol-based adhesive to obtain a long polarizing plate having a protective layer / polarizer / protective layer configuration.
  • the pressure-sensitive adhesive layer was applied to a dried PET film having a thickness of 25 ⁇ m, dried and crosslinked at 130 ° C. for 3 minutes, transferred to the HC-TAC surface of the polarizing plate obtained above, As a result, a stress relaxation layer (elastic modulus at 95 ° C .: 8 ⁇ 10 ⁇ 3 GPa) made of an adhesive was obtained.
  • Example 2 The optical laminate was prepared in the same manner as in Example 1 except that the stress relaxation layer was composed of the pressure-sensitive adhesive (13 ⁇ m) used in Example 1 / the stress relaxation body / the pressure-sensitive adhesive (13 ⁇ m) used in Example 1. Produced. A commercially available PET film (manufactured by Mitsubishi Plastics, trade name “Diafoil”, thickness 23 ⁇ m) was used as the stress relaxation body. The obtained optical laminate was subjected to the same evaluation as in Example 1. The results are shown in Table 1.
  • Example 3 An optical laminate was prepared in the same manner as in Example 2 except that a commercially available thin glass (made by Corning, trade name “willow glass”, thickness 100 ⁇ m) was used as the stress relaxation body. The obtained optical laminate was subjected to the same evaluation as in Example 1. The results are shown in Table 1.
  • the optical layered body of the present invention can be suitably used as an optical member having the functions of both a barrier layer (barrier film) and a polarizing plate of an image display device. More specifically, the optical laminate of the present invention can be used as an optical member of a liquid crystal display device and an organic EL display device, preferably an organic EL display device, more preferably a bendable organic EL display device.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Nonlinear Science (AREA)
  • Mathematical Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Polarising Elements (AREA)
  • Electroluminescent Light Sources (AREA)
  • Physical Vapour Deposition (AREA)
  • Liquid Crystal (AREA)

Abstract

L'invention concerne un stratifié optique qui fait office de film barrière et de plaque de polarisation et qui résiste à la fissuration. Le stratifié optique selon l'invention comprend, dans l'ordre, un polariseur, une couche de soulagement des contraintes, un substrat, une première couche d'oxyde qui contient du ZnO, de l'Al et du SiO2, et une deuxième couche d'oxyde qui est constituée de SiO2. Le module élastique de la couche de soulagement des contraintes est de 0,01 MPa à 70 GPa, et l'épaisseur de la couche de soulagement des contraintes est de 13 à 200 µm. Dans un mode de réalisation, la couche de soulagement des contraintes est constituée d'un adhésif.
PCT/JP2017/003049 2016-01-29 2017-01-27 Stratifié optique WO2017131200A1 (fr)

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