WO2005001525A1 - 光学積層フィルム、偏光板および光学製品 - Google Patents
光学積層フィルム、偏光板および光学製品 Download PDFInfo
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- WO2005001525A1 WO2005001525A1 PCT/JP2004/009119 JP2004009119W WO2005001525A1 WO 2005001525 A1 WO2005001525 A1 WO 2005001525A1 JP 2004009119 W JP2004009119 W JP 2004009119W WO 2005001525 A1 WO2005001525 A1 WO 2005001525A1
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Classifications
-
- 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
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/111—Anti-reflection coatings using layers comprising organic materials
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
-
- 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
- G02F1/133528—Polarisers
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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
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/42—Polarizing, birefringent, filtering
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
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- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249967—Inorganic matrix in void-containing component
- Y10T428/249969—Of silicon-containing material [e.g., glass, etc.]
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- Y10T428/31652—Of asbestos
- Y10T428/31663—As siloxane, silicone or silane
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- Y10T428/31855—Of addition polymer from unsaturated monomers
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
- Y10T428/31938—Polymer of monoethylenically unsaturated hydrocarbon
Definitions
- the present invention relates to an optical laminated film, and more particularly, useful as an antireflection protective film or a polarizing plate protective film for an optical member, in which a low refractive index layer capable of efficiently realizing a low light reflectance is laminated.
- Optical laminated film Furthermore, the present invention relates to a polarizing plate having an anti-reflection function using the optical laminated film, and an optical product provided with the polarizing plate.
- a polarizing film for a liquid crystal display may be subjected to a processing for providing a low refractive index layer in order to prevent reflection.
- a polarizing film for an LCD used in the outdoors is required to have a high-performance antireflection function. Therefore, a low refractive index layer of a multilayer film or a single layer film is formed on the surface of the base film.
- a low refractive index layer of a multilayer film there is a layer in which a film having a relatively high refractive index and a film having a relatively low refractive index are laminated in this order (for example, see Patent Document 1). .
- Examples of the method for forming a film include a sol-gel method, a vacuum evaporation method, a sputtering method, and a chemical vapor deposition method.
- the resin substrate may be deformed or deteriorated in the high-temperature process, and it is difficult to change the optical characteristics of the film and form a desired antireflection film.
- gas is released from the resin in the vacuum apparatus, so that a high vacuum necessary for forming the film cannot be obtained, and it is difficult to form a reflection preventing film having desired characteristics.
- the coating operation of the film is required twice or more, which complicates the process. There are problems such as difficulty in achieving low light reflectance.
- a multi-component metal oxide film is formed on a glass by a sol-gel method, and then the multi-component metal oxide film is subjected to a phase separation by a heat treatment.
- a metal oxide film that has been etched with hydrofluoric acid to make it porous using the difference in the etching rate of each phase for example, see Non-Patent Document 1
- magnesium oxide on glass by the Zonolleger method After forming a composite film of carbon dioxide and carbon dioxide, it is exposed to a gas containing fluorine at a high temperature to replace oxygen with fluorine (for example, see Non-Patent Document 2).
- Patent Document 2 discloses that a coating liquid containing at least one kind of organosilicon compound containing at least an organosilicon compound having an amino group or a hydrolyzate thereof is applied to the surface of a resin substrate, By drying the coating solution, a primary coating is formed on the surface of the resin substrate, and a silicon dioxide film having a refractive index of 1.40 or less and an uneven surface is formed on the primary coating.
- a low-reflection resin substrate characterized by having been described. According to Patent Document 2, it is described that a low-temperature process can be simultaneously formed over the entire surface of the resin base material with good adhesion.
- the low-reflection resin substrate described in the publication is used particularly in a liquid crystal display device, the visibility (for example, luminance) is deteriorated, and the contrast of light and dark display is deteriorated. There is S power. Therefore, further improvement is required.
- Patent Document 1 JP-A-4-357134
- Patent Document 2 JP-A-2002-328202
- Patent Document 1 S.P.Mukherjee et al., J. Non-Cry st.Solids, Vol. 48, pi 77 (198 2)
- Non-Patent Document 2 J. H. Simmons et al., J. Non-Cryst. Solids, Vol. 178, pl66 (199
- an object of the present invention is to provide a glare with lower light reflectance and a better visibility with less glare than conventional ones, and furthermore, when used in a liquid crystal display device, a contrast in bright and dark display. It is to provide an excellent optical laminated film.
- a hard-coat layer and a low-refractive-index layer consisting of an air-gel are laminated in this order on one side of a base film containing a transparent resin, directly or via another layer.
- the refractive index is n
- the refractive index of the low refractive index layer is n
- the transparent resin is a resin selected from the group consisting of a polymer resin having an alicyclic structure, a cellulose resin, and a polyester resin. ;
- optical laminated film according to (1) or (6) above which is an antireflection protective film for an optical member
- a polarizing plate with an antireflection function which is obtained by laminating a polarizing film on the surface opposite to the surface on which the low refractive index layer is provided of the polarizing plate protective film according to (8);
- an optical laminated film having low glare due to low light reflectivity and excellent visibility due to small glare, and further having excellent contrast in bright and dark display when used in a liquid crystal display device. That can be S.
- FIG. 1 is a sectional view of the layer structure of the optical laminated film of the present invention.
- FIG. 2 is a sectional view of a layer structure of a polarizing plate with an antireflection function of the present invention.
- FIG. 3 is a sectional view of a layer structure in which a polarizing plate with an antireflection function of the present invention is bonded to a liquid crystal display cell.
- FIG. 4 is a sectional view of a layer structure of the liquid crystal display cell shown in FIG. 3.
- a resin having a total light transmittance of 80% or more at a thickness of 1 mm is used.
- the type of the resin is not particularly limited, and examples thereof include a polymer resin having an alicyclic structure, a polyolefin polymer such as polyethylene and polypropylene, a polycarbonate polymer, a polyester polymer, a polysulfone polymer, and a polyether. Examples include a sulfone polymer, a polystyrene polymer, a polyvinyl alcohol polymer, an acyl-modified cellulose polymer, a polyvinyl chloride polymer, and a polymethacrylate polymer.
- acyl-modified cellulose resins such as diacetyl cellulose, propionyl cellulose, triacetyl cellulose, butyryl cellulose, etc., because of their excellent transparency and small birefringence; From the viewpoints of transparency and light weight, which are preferred by the polyester resin and the polymer resin having an alicyclic structure, triacetyl cellulose, polyethylene terephthalate, and a polymer resin having an alicyclic structure are more preferable. From the viewpoints of dimensional stability and film thickness controllability, polyethylene terephthalate and a polymer resin having an alicyclic structure are particularly preferred.
- the polymer resin having an alicyclic structure has an alicyclic structure in a main chain and / or a side chain. Among them, from the viewpoints of mechanical strength, heat resistance and the like, an alicyclic structure is contained in the main chain. Including expression structure Are preferred.
- Examples of the alicyclic structure include a saturated alicyclic hydrocarbon (cycloalkane) structure and an unsaturated alicyclic hydrocarbon (cycloalkene) structure. From the viewpoint of mechanical strength and heat resistance, the cycloalkane structure is preferred. And cycloalkene structures are preferred. Among them, a cycloanolecan structure is most preferable. There is no particular limitation on the number of carbon atoms constituting the alicyclic structure, but when the number is usually 430, preferably 5-20, and more preferably 515, the mechanical strength, Heat resistance and film moldability are highly balanced and suitable.
- the proportion of the repeating unit containing an alicyclic structure in the alicyclic structure-containing polymer may be appropriately selected according to the purpose of use, but is preferably 30% by weight or more, more preferably 50% by weight. More preferably, it is at least 70% by weight, most preferably at least 90% by weight.
- the proportion of the repeating unit having an alicyclic structure in the polymer having an alicyclic structure is such a large value, the transparency and heat resistance of the substrate film are increased.
- polymer resin having an alicyclic structure examples include (1) a norbornene-based polymer, (2) a monocyclic cyclic olefin-based polymer, (3) a cyclic conjugated gen-based polymer, (4) Vinyl alicyclic hydrocarbon polymers and hydrogenated products thereof.
- a norbornene-based polymer is more preferable from the viewpoint of transparency and moldability.
- Examples of the norbornene-based polymer include a ring-opened polymer of a norbornene-based monomer, a ring-opened copolymer of a norbornene-based monomer and another monomer capable of ring-opening copolymerization, and hydrogenated products thereof. And an addition polymer of a norbornene-based monomer, and an adduct copolymer of a norbornene-based monomer and another monomer copolymerizable with the norbornene-based monomer.
- a hydrogenated ring-opening (co) polymer of a norbornene-based monomer is particularly preferred from the viewpoint of transparency.
- the polymer resin having an alicyclic structure is selected from known polymers disclosed in, for example, JP-A-2002-321302.
- the glass transition temperature of the transparent resin used for the base film is preferably 80 ° C. or higher, more preferably 100 to 250 ° C.
- a substrate film made of a transparent resin having such a high glass transition temperature has excellent durability without deformation or stress when used at high temperatures.
- the molecular weight of the transparent resin used for the base film is determined by gel 'permeation' chromatography using cyclohexane (toluene when the polymer resin does not dissolve) as a solvent (hereinafter abbreviated as "GPC").
- GPC cyclohexane
- Mw weight average molecular weight
- Mw weight average molecular weight
- S When the weight average molecular weight S is in such a range, the mechanical strength and the moldability of the film are highly balanced and suitable.
- the molecular weight distribution (weight-average molecular weight (Mw), Z-number average molecular weight (Mn)) of the transparent resin is not particularly limited, and is usually S, usually 1.0 10.0, preferably 1.0 to 4.0. , More preferably in the range of 1-3.3.5.
- the base film used in the optical laminated film of the present invention may contain a compounding agent in addition to the transparent resin.
- the compounding agent is not particularly limited, but, for example, inorganic fine particles; stabilizers such as antioxidants, heat stabilizers, light stabilizers, weather stabilizers, ultraviolet absorbers, and near infrared absorbers; lubricants, plasticizers, and the like Resin modifiers; coloring agents such as dyes and pigments; antistatic agents and the like. These compounding agents can be used alone or in combination of two or more.
- the amount is usually 0 to 5 parts by weight, preferably 0 to 3 parts by weight, based on 100 parts by weight of the transparent resin, which is appropriately selected within a range not to impair the object of the present invention.
- the film thickness of the base film from the viewpoint of mechanical strength, preferably 30- 300 beta m, more preferably 40- 200 mu m.
- the thickness of the base film is uniform. Specifically, it is preferable that the change in the thickness over the entire width of the base film is within 3% of the thickness. When the thickness variation of the base film is within 3% of the thickness, the adhesion of the hard coat layer and the surface smoothness of the low refractive index layer laminated thereon can be improved.
- the depth or height of the die line of the base film is preferably 0.1 am or less, more preferably 0.05 z m or less.
- the die line can be measured using a non-contact type three-dimensional surface shape / roughness measuring device.
- the content of the volatile component in the base film is preferably 0.1% by weight or less.
- the content of the volatile component in the base film is so small, the dimensional stability of the base film is improved, and uneven lamination when the hard coat layer is laminated can be reduced. This makes it possible to form a uniform low refractive index layer over the entire surface of the film. As a result, an even antireflection effect can be obtained over the entire surface of the film.
- the volatile component is a substance having a molecular weight of 200 or less contained in a trace amount in the base film, and examples thereof include a residual monomer and a solvent.
- the content of volatile components can be determined by analyzing the base film by gas chromatography as the sum of substances having a molecular weight of 200 or less contained in the transparent resin.
- the saturated water absorption of the base film is preferably 0.01% by weight or less, more preferably 0.007% by weight or less. If the saturated water absorption exceeds 0.01% by weight, the adhesion between the hard coat layer and the base film and the adhesion between the hard coat layer and the low refractive index layer will decrease, resulting in a low refractive index over a long period of use. The separation of the rate layer is likely to occur.
- the saturated water absorption of the base film can be determined by immersing the base film at 23 ° C for one week and measuring the increased weight according to ASTM D530.
- the base film one having one or both surfaces subjected to a surface modification treatment may be used.
- the surface modification treatment include energy beam irradiation treatment and chemical treatment.
- Examples of the energy ray irradiation treatment include corona discharge treatment, plasma treatment, electron beam irradiation treatment, and ultraviolet irradiation treatment. Corona discharge treatment and plasma treatment are preferred in terms of treatment efficiency. Processing is particularly preferred.
- a method of immersing in an aqueous solution of an oxidizing agent such as a potassium dichromate solution or concentrated sulfuric acid and then sufficiently washing with water is employed. Shaking while immersed increases the immersion effect. There is a problem that the surface dissolves or the transparency decreases when the treatment is performed for a long time, and the treatment time may be adjusted according to the reactivity and concentration of the chemicals used.
- Examples of the method of forming the base film include a solution casting method and a melt extrusion molding method. Above all, the melt extrusion molding method is preferred from the viewpoint that the content of the volatile component and the thickness unevenness in the base film can be reduced. Further, examples of the melt extrusion molding method include a method using a die and an inflation method, and a method using a T die is preferable in terms of excellent productivity and thickness accuracy.
- the melting temperature of the transparent resin in an extruder having a T-die should be 80 to 180 ° C higher than the glass transition temperature of the transparent resin. It is more preferable to raise the temperature 100-150 ° C higher than the preferred glass transition temperature. If the melting temperature in the extruder is too low, the fluidity of the transparent resin may be insufficient, and if the melting temperature is too high, the resin may be deteriorated.
- the means for reducing the depth or height of the die line of the base film used in the present invention to 0.1 lxm or less is as follows: (1) A chrome, nickel, titanium, or other plating is provided at the tip of the die lip. (2) Use a die with a coating of TiN, TiAlN, TiC, CrN, DLC (diamond-like carbon) formed on the inner surface of the die lip by PVD (Phisical Vapor Deposition) method, etc. (3) A method using a die on which the tip of the die lip is sprayed with other ceramics, and (4) A method using a die in which the surface of the tip of the die lip is nitrided.
- Such a die has a small friction with a resin having a high surface hardness, it is possible to prevent burning dirt and the like from being mixed into the obtained base material finolem, and to reduce the depth or the depth of the die line.
- the height can be less than 0.1 ⁇ .
- the use of a die having better surface accuracy can reduce thickness unevenness.
- the surface roughness related to the microscopic unevenness of the surface can be represented by “average height Ra”, and the average height Ra of the inner surface of the die, particularly the tip of the die lip is preferably 0 or less, more preferably 0 or less. It is less than lzm.
- the average height Ra is the same as the "arithmetic average height Ra" defined by JIS B 0601-2001.
- a roughness curve is obtained through a compensating high-pass filter, a fixed reference length is extracted from the roughness curve in the direction of the average line, and the absolute value of the deviation from the average linear force roughness curve of the extracted portion is calculated. Combination It is determined by measuring and averaging.
- the one attached to the die lip (for example, waste dust) is removed; Methods to improve the mold releasability of the die; to make the wettability of the die lip uniform over the entire surface; to reduce the amount of dissolved oxygen and Z or resin powder in the resin pellets; and to install a polymer filter in the melt extruder.
- a transparent resin itself having a small amount of volatile components is used, and (2) melt extrusion.
- Means include forming a base film by a forming method, and (3) preliminarily drying a transparent resin to be used before forming a film. Preliminary drying is performed, for example, using a hot-air dryer or the like after converting the raw materials into pellets or the like.
- the drying temperature is preferably 100 ° C. or more, and the drying time is preferably 2 hours or more.
- the hard coat layer constituting the optical laminated film of the present invention is formed from a material having a hardness of “2H” or more in a pencil hardness test (a test plate is a glass plate) shown in JIS K5600-5-4. .
- a material having a hardness of “2H” or more in a pencil hardness test (a test plate is a glass plate) shown in JIS K5600-5-4.
- Specific examples thereof include organic hard coat materials such as organic silicone-based, melamine-based, epoxy-based, acrylic-based, and urethane acrylate-based materials; and inorganic hard coat materials such as silicon dioxide.
- organic hard coat materials such as organic silicone-based, melamine-based, epoxy-based, acrylic-based, and urethane acrylate-based materials
- inorganic hard coat materials such as silicon dioxide.
- the refractive index n of the hard coat layer and the refractive index of the low refractive index layer are the refractive index n of the hard coat layer and the refractive index of the low refractive index layer
- the refractive index n of the hard coat layer satisfies the following formula [2].
- the refractive index of the hard coat layer is adjusted, the flexural modulus is improved, the volumetric shrinkage is stabilized, and the heat resistance, antistatic property, antiglare property and the like are improved.
- various fillers such as silica, alumina and hydrated alumina may be contained.
- various additives such as an antioxidant, an ultraviolet absorber, a light stabilizer, an antistatic agent, a leveling agent, and an antifoaming agent can be added.
- the refractive index and the antistatic property of the hard coat layer can be easily adjusted among various fillers. Titanium oxide, dinoconium oxide, zinc oxide, tin oxide, cerium oxide, antimony pentoxide, indium oxide (ITO) doped with tin, tin oxide doped with antimony (IZO), and oxide doped with aluminum Antimony pentoxide, ITO, IZ ⁇ , ATO, FT ⁇ are more preferred because zinc (AZO) and fluorine-doped tin oxide (FTO) can maintain the desired transparency.
- the primary particle diameter is 1 nm or more and 100 nm or less, preferably 30 nm or less.
- the hard coat layer contains a filler
- those having an average particle diameter of 0.5-10 / im are preferred, and those having an average particle diameter of 11-7 ⁇ are more preferred.
- a film that imparts anti-glare properties include polymethyl methacrylate resin, vinylidene fluoride resin and other fluorine resins, silicone resin, epoxy resin, nylon resin, polystyrene resin, phenol resin, and polyurethane resin.
- Organic resin fillers such as acrylic resin, crosslinked acrylic resin, crosslinked polystyrene resin, melamine resin, benzoguanamine resin; or titanium oxide, aluminum oxide, indium oxide, zinc oxide, antimony oxide, tin oxide, zirconium oxide, ⁇ , magnesium fluoride And inorganic fillers such as silicon oxide.
- the method for forming the hard coat layer is not particularly limited.
- a coating liquid for forming a hard coat layer is applied on a base film by a known coating method, and cured by heating or irradiation with ultraviolet light. Formed by the method.
- the thickness of the hard coat layer is preferably 0.5 to 30 zm, more preferably 3 to 15 zm. . If the thickness of the hard coat layer is too thin, the hardness of each layer to be formed thereon cannot be maintained, while if it is too thick, the flexibility of the entire optical laminated film decreases, and it takes a long time to cure. There is a possibility that the efficiency may be reduced.
- the low-refractive-index layer of the optical laminated film of the present invention is composed of an air port gel.
- the air port gel if the refractive index n force of the low refractive index layer satisfies the following equations [1] and [3], it is a special feature.
- n is the refractive index of the hard coat layer.
- the configuration of the low refractive index layer may be a multilayer as long as it has at least one layer.
- the low refractive index layer is composed of multiple layers, at least the refractive index of the layer closest to the hard coat layer is n
- the air port gel is a transparent porous body in which fine bubbles are dispersed in a matrix. Bubbles are mostly below 200 nm in size and the content of bubbles is usually 10-60% by volume, preferably 20-40% by volume.
- the air port gel in which minute air bubbles are dispersed include a silica air port gel and a porous body in which hollow particles are dispersed in a matrix.
- Silica airgel was obtained by hydrolysis polymerization of alkoxysilane as disclosed in US Patent No. 4,402,927, US Patent No. 4,432,956, and US Patent No. 4,610,863. It can be produced by drying a wet gel compound comprising a silica skeleton in the presence of a solvent (dispersion medium) such as alcohol or carbon dioxide in a supercritical state at or above the critical point of the solvent.
- a solvent such as alcohol or carbon dioxide
- supercritical drying for example, a gel-like compound is immersed in liquefied diacid carbon, and all or part of the solvent contained in the gel-like compound is replaced with liquefied carbon dioxide having a lower critical point than this solvent.
- the silica air opening gel may be produced in the same manner as above using sodium silicate as a raw material.
- a gel-like compound obtained by hydrolysis and polymerization of alkoxysilane as described above It is preferable to impart hydrophobicity to the silica gel by subjecting the silica to a hydrophobic treatment.
- the hydrophobic silica air opening gel thus imparted with hydrophobicity makes it difficult for moisture or water to infiltrate, thereby preventing the silica air opening gel from deteriorating its performance such as the refractive index and light transmittance.
- the step of hydrophobizing treatment can be performed before or during supercritical drying of the gel compound.
- the hydrophobization treatment is performed to make the hydroxyl group of the silanol group present on the surface of the gel-like compound react with the functional group of the hydrophobizing agent, and to replace the hydrophobic group with the hydrophobic group of the hydrophobizing agent to make the surface hydrophobic. is there.
- the gel is immersed in a hydrophobizing solution in which the hydrophobizing agent is dissolved in a solvent, mixed, etc., and the hydrophobizing agent is permeated into the gel. Then, a method of heating to perform a hydrophobizing reaction may be used.
- Examples of the solvent used for the hydrophobizing treatment include methanol, ethanol, isopropanol, xylene, toluene, benzene, N, N-dimethylformamide, and hexamethyldisiloxane.
- the solvent is not limited to these as long as it can be dissolved in the gel and can be replaced by the solvent contained in the gel before the hydrophobic treatment.
- a medium which can be easily subjected to supercritical drying for example, the same type as or a substitute for methanol, ethanol, isopropanol, liquefied carbon dioxide and the like can be used. It is preferably used.
- the hydrophobizing agent include hexamethinoresilazane, hexamethinoresisiloxane, trimethinolemethoxysilane, dimethinoledimethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, trimethylethoxysilane, and dimethylethylsilane. Toxisilane, methyltriethoxysilane and the like can be mentioned.
- the refractive index of the silica air opening gel freely changes depending on the raw material mixing ratio of the silica air opening gel. The ability to make S.
- the formation method is not particularly limited.
- the gel compound is coated on the hard coat layer by a known coating method, and A method of performing formation by performing supercritical drying is given.
- the hydrophobic treatment may be performed before or during the supercritical drying.
- supercritical drying for example, the gelled compound is immersed in liquefied carbon dioxide, and all or part of the solvent containing the gelled compound is replaced with liquefied carbon dioxide having a lower critical point than this solvent. Thereafter, the drying can be performed by drying under supercritical conditions of a single system of carbon dioxide or a mixed system of carbon dioxide and a solvent.
- Examples of the porous body in which hollow particles are dispersed in a matrix include hollow particles having voids inside fine particles as disclosed in JP-A-2001-233611 and JP-A-2003-149642.
- a porous body in which fine particles are dispersed in a binder resin is exemplified.
- the binder resin a resin that meets conditions such as the dispersibility of hollow fine particles, the transparency of the porous body, and the strength of the porous body can be selected and used.
- Polyester resin acrylic resin, urethane resin, vinyl chloride resin, epoxy resin, melamine resin, fluororesin, silicone resin, butyral resin, phenol resin, butyl acetate resin, ultraviolet curable resin, electron beam curable resin, emulsion resin
- acrylic resins and epoxy resins are preferred in view of the dispersibility of the fine particles and the strength of the porous body.
- hydrolyzable organic silicon compounds such as urethane resins, silicone resins, and alkoxysilanes, and hydrolysates thereof.
- the reflection characteristics and the antifouling property of the low refractive index layer are improved.
- a fluorine resin may be mixed.
- the hydrolyzable organosilicon compound such as the alkoxysilane and the hydrolyzate thereof are formed from one or more compounds selected from the group consisting of the following (a) to (c), In which,-(O-Si) _-(where m represents a natural number) has a bond m
- X is a halogen atom such as a chlorine atom or a bromine atom; a monovalent hydrocarbon group having a substituent; Organic acid groups such as acetate group and nitrate group; ⁇ -diketonate group such as acetylacetonate; inorganic acid groups such as nitrate group and sulfate group; methoxy group, ethoxy group, ⁇ -propoxy group and ⁇ -butoxy group Or a hydroxyl group.
- the monovalent hydrocarbon group having a substituent may be a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group.
- Alkyl groups such as cyclopentyl group and cyclohexyl group; and optionally substituted aryl groups such as phenyl group, 4-methylphenyl group, 1-naphthyl group and 2-naphthyl group.
- Alkenyl groups such as butyl group and aryl group; aralkyl groups such as benzyl group, phenyl group and 3-phenylpropyl group; halo groups such as chloromethyl group and ⁇ -chloropropyl group.
- a perfluoroalkyl group such as a nore group, a heptadecafluorodecyl group, a trifluoropropyl group, a tridecafluorooctyl group; an alkenylcarbonyloxyalkyl group such as a ⁇ -methacryloxypropyl group; ⁇ Alkyl groups having an epoxy group such as -glycidoxypropyl group and 3,4-epoxycyclohexylethyl group; alkyl groups having a mercapto group such as ⁇ -mercaptopropyl group; amino groups such as 3-aminopropyl group. Having an alkyl group; and the like. Among these, an alkyl group having 14 to 14 carbon atoms, a perfluoroalkyl group, and a phenyl group are preferable from the viewpoint of easy synthesis, availability, and low reflection characteristics.
- ⁇ represents a hydrolyzable group.
- the hydrolyzable group refers to a group which is hydrolyzed in the presence of an acid or base catalyst as required to generate a-(o-si) m -o_ bond.
- R ', R", R "' each independently represent a hydrogen atom or a monovalent hydrocarbon group.
- an alkoxy group is preferable in terms of availability and the like.
- the compound (i) _l is preferably a silicon compound in which a is an integer of 0 to 2 in the formula (i) _l.
- alkoxysilanes examples thereof include alkoxysilanes, acetoxysilanes, oxime silanes, enoxysilanes, aminosilanes, aminoxysilanes, amidosilanes and the like. Among these, alkoxysilanes are more preferable from the viewpoint of availability.
- tetraalkoxysilanes in which a is 0 include tetramethoxysilane, tetraethoxysilane, and the like.
- Onoleganotrialkoxysilanes in which a is 1 include methyltrimethoxysilane, Examples thereof include methyltriethoxysilane, methyltriisopropoxysilane, phenolinoletrimethoxysilane, phenolinoletriethoxysilane, and 3,3,3-trifluoropropinoletrimethoxysilane.
- Examples of the diorganodialkoxysilane in which a is 2 include dimethyldimethoxysilane, dimethylethoxysilane, diphenyldimethoxysilane, and diphenyldimethoxysilane. Examples include phenyljetoxysilane and methylphenyldimethoxysilane.
- the molecular weight of compound (i) _1 is not particularly limited, but is preferably from 40 to 300, more preferably from 100 to 200.
- Compound (ii), which is at least one partial hydrolysis product of compound (i), and compound (iii), which is at least one complete hydrolysis product of compound (i), are compound (i) ) Can be obtained by hydrolyzing or condensing one or more of the above or all of them.
- Compound (ii) and compound (iii) are, for example, Si (Or) (r represents a monovalent hydrocarbon group.)
- a catalyst may be used as necessary.
- the catalyst to be used is not particularly limited, but the obtained partial hydrolyzate and / or hydrolyzate has a two-dimensional crosslinked structure, and the condensed compound is easily made porous immediately after the hydrolysis. Acid catalysts are preferred from the viewpoint of reducing the time required for decomposition.
- the acid catalyst to be used is not particularly limited.
- Organic acids such as toluenesulfonic acid and oxalic acid; inorganic acids such as hydrochloric acid, nitric acid and halogenated silane; and acidic sol-like fillers such as acidic colloidal silicide and titania sol.
- These acid catalysts can be used alone or in combination of two or more.
- a base catalyst such as an aqueous solution of a hydroxide of an alkali metal or alkaline earth metal such as sodium hydroxide or calcium hydroxide, an aqueous solution of ammonia water, or an aqueous solution of an amine is used. Moore.
- the molecular weight of compound ( ⁇ ) and compound (m) is not particularly limited, but usually the weight average molecular weight is in the range of 2005,000.
- the hollow fine particles are not particularly limited as long as they are fine particles of an inorganic compound. It is particularly preferable to use silica-based hollow fine particles, which are preferably hollow inorganic fine particles.
- an inorganic oxide is generally used as the inorganic compound.
- SiO, A1 as inorganic oxide is generally used.
- the inorganic hollow fine particles include (A) a single layer of an inorganic oxide, (B) a single layer of a composite oxide composed of different kinds of inorganic oxides, and (C) a single layer of the above (A) and (B). Those containing a double layer of the following can be used.
- the outer shell of the hollow fine particles may be a porous one having pores, or may be one in which the pores are closed and the cavity is sealed from the outside of the outer shell.
- the outer shell is preferably a plurality of inorganic oxide coating layers including an inner first inorganic oxide coating layer and an outer second inorganic oxide coating layer. By providing the second inorganic oxide coating layer on the outside, it is possible to close the pores of the outer shell to make the outer shell denser, and to obtain inorganic hollow fine particles in which the inner cavity is sealed.
- the obtained particles have a lower refractive index and can be used in an organic solvent. It is also effective because it has the effect of imparting the antifouling property of a layer having a low refractive index, as well as the dispersibility of the layer.
- a fluorine-containing organosilicon compound include 3,3,3-trifluoropropyltrimethoxysilane and methyl-3,3,3-trimethylsilane.
- heptadecafluorodecyltrichlorosilane heptadecafluorodecyltrimethoxysilane, trifluoropropyltrimethoxysilane, and tridecafluorooctyltrimethoxysilane.
- the thickness of the outer shell is preferably in the range of 1 to 50 nm, particularly 5 to 20 nm.
- the inorganic hollow fine particles may not be able to maintain a predetermined particle shape.
- the thickness of the outer shell exceeds 50 nm, the cavities in the inorganic hollow fine particles are small, and as a result, the proportion of the cavities may be reduced and the refractive index may not be sufficiently reduced.
- the thickness of the outer shell is preferably in the range of 1/50 to 1/5 of the average particle diameter of the inorganic hollow fine particles.
- the total force of the thicknesses of these layers is set to be in the range of the above 150 nm.
- the thickness of the second inorganic oxide coating layer is preferably in the range of 20 to 40 nm particularly for the densified outer shell.
- the cavity may contain the solvent used for preparing the inorganic hollow fine particles and Z or a gas that infiltrates during drying. Is left in the cavity.
- the precursor substance is a porous substance remaining after removing some of the constituent components of the core particles from the core particles surrounded by the outer shell.
- the core particles porous composite oxide particles composed of different types of inorganic oxides are used.
- the precursor material may adhere to the outer shell and remain slightly, or may occupy most of the cavity.
- the solvent or gas may be present in the pores of the porous substance. At this time, if the removal amount of the constituent components of the core particles increases, the volume of the cavity increases, and inorganic hollow fine particles having a low refractive index are obtained.
- the transparent coating obtained by blending the inorganic hollow fine particles has a low refractive index to reflect. Excellent prevention performance.
- the average particle diameter of the inorganic hollow fine particles is not particularly limited, but is preferably in the range of 5 to 2,000 nm, more preferably 20 to 100 nm. If it is smaller than 5 nm, the effect of lowering the refractive index due to the hollow is small. Conversely, if it is larger than 2,000 nm, the transparency becomes extremely poor, and the contribution of diffuse reflection increases.
- the average particle size is a number average particle size determined by observation with a transmission electron microscope.
- the blending amount of the inorganic fine particles is not particularly limited, but is preferably 1030% by weight based on the entire low refractive index layer. When the amount of the inorganic fine particles is within this range, low refraction An optical laminated film having both efficiency and abrasion resistance can be obtained.
- the inorganic fine particles can also be used in the form of a dispersion.
- the type of the organic solvent used for the dispersion is not particularly limited.
- lower aliphatic alcohols such as methanol, ethanol, isopropanol (IPA), n-butanol, and isobutanol
- Ethylene glycol derivatives such as ethylene glycol monobutyl ether and ethylene glycol monoethyl ether acetate
- diethylene glycol derivatives such as diethylene glycol and ethylene glycol monobutyl ether
- diacetone alcohol aromatic hydrocarbons such as toluene and xylene
- n-hexane n Aliphatic hydrocarbons such as heptane
- esters such as ethyl acetate and butyl acetate
- ketones such as acetone, methyl ethyl ketone and methyl isobutyl ketone
- These organic solvents can be used alone or in combination
- the forming method is not particularly limited, and for example, a void is formed at least inside the fine particles on the hard coat layer.
- the temperature of the optional heating is usually 50-200 ° C, preferably 80-150 ° C.
- the thickness of the low refractive index layer is 10 to 1000 nm, preferably 30 to 500 nm. Further, as described above, the low refractive index layer may be a multilayer having at least one layer.
- the optical laminated film of the present invention has a refractive index n of the hard coat layer and a low refractive index.
- the refractive index nL of the refractive index layer is expressed by the formula [l] n ⁇ 1.37, the formula [2] n ⁇ 1.53, and the formula [3] n— 0.
- Equation [4] 1 ⁇ 25 ⁇ n ⁇ 1.35
- the optical reflectance of the optical laminated film can be reduced, and an optical product excellent in visibility, scratch resistance and strength can be obtained.
- the optical laminated film of the present invention preferably has a reflectance of 0.7% or less at a wavelength of 550 nm and a reflectance of 1.5% or less at a wavelength of 430 nm and 700 nm. 0.6% or less and reflectance at wavelength 430nm 700nm More preferably, it is not more than 4%.
- FIG. 1 shows an example of a layer configuration of the optical laminated film of the present invention.
- the optical laminated film 50 shown in FIG. 1 includes a base film layer 11, a hard coat layer 21, a low refractive index layer 31, and an antifouling layer 41 from the lower side in the figure.
- another layer can be interposed between the base film 11 and the hard coat layer 21.
- Other layers include a primer layer (not shown).
- the primer layer is formed for the purpose of imparting and improving the adhesion between the base film and the hard coat layer.
- the material constituting the primer layer include polyester urethane resins, polyether urethane resins, polyisocyanate resins, polyolefin resins, resins having a hydrocarbon skeleton and / or polybutadiene skeleton in the main chain, polyamide resins, and acrylic resins. Resins, polyester resins, vinyl chloride-vinyl acetate copolymers, chlorinated rubbers, cyclized rubbers, and modified products obtained by introducing a polar group into these polymers.
- a modified resin having a hydrocarbon skeleton and / or a polybutadiene skeleton in the main chain and a modified cyclized rubber are preferable.
- a resin having a hydrocarbon skeleton and / or polybutadiene skeleton in the main chain a resin having a polybutadiene skeleton or a skeleton obtained by hydrogenating at least a part thereof, specifically, a polybutadiene resin, a hydrogenated polybutadiene resin And styrene 'butadiene' styrene block copolymer (SBS copolymer) and its hydrogenated product (SEBS copolymer).
- SBS copolymer hydrogenated polybutadiene resin
- SEBS copolymer hydrogenated product
- a modified product of a hydrogenated styrene / butadiene / styrene block copolymer is preferred.
- the polar group to be introduced is preferably a carboxylic acid or a derivative thereof.
- Specific examples include unsaturated carboxylic acids such as acrylic acid, methacrylic acid, maleic acid, and fumaric acid; maleic chloride, maleimide, and anhydride.
- Halogenated compounds of unsaturated carboxylic acids such as maleic acid and citraconic anhydride; and derivatives of carboxylic acids such as amides, imides, anhydrides and esters; and the like.
- Acrylic acid, methacrylic acid, maleic acid, and maleic anhydride are more preferable, and a maleic acid and maleic anhydride are particularly preferable. 2 such as these unsaturated carboxylic acids
- a mixture of two or more species may be used for modification.
- the method for forming the primer layer is not particularly limited, and includes, for example, a method in which a coating liquid for forming a primer layer is applied on a substrate film by a known coating method.
- the thickness of the primer layer is not particularly limited, but is usually 0.3 to 5 ⁇ m, preferably 0.5 to 5 ⁇ m.
- an antifouling layer (reference numeral 41 in FIG. 1) is provided on the low refractive index layer in order to protect the low refractive index layer and enhance antifouling performance. You may have more.
- the material constituting the antifouling layer is not particularly limited as long as the function of the low refractive index layer is not hindered and the required performance as the antifouling layer is satisfied.
- a compound having a hydrophobic group can be preferably used.
- perfluoroalkylsilane compounds, perfluoropolyethersilane compounds, and fluorine-containing silicone compounds can be used.
- the method for forming the antifouling layer can be, for example, a physical vapor deposition method such as vapor deposition or sputtering, a chemical vapor deposition method such as CVD, or a wet coating method, depending on the material to be formed. .
- the thickness of the antifouling layer is not particularly limited, but is usually preferably 20 nm or less, more preferably 1-1 Onm.
- the optical laminated film of the present invention has excellent optical properties and low light reflectance, and is therefore suitable as an antireflection protective film for optical members.
- antireflection protective films are used in optical devices such as touch panels and image display devices such as liquid crystal display devices, plasma display panels, EL elements, and cathode ray tube display devices to reduce contrast caused by reflection of external light. It is used to prevent reflection of images.
- These antireflective protective films are often provided as antireflective protective films for optical members usually formed on the uppermost layer on the viewing side in each optical device.
- the optical laminated film of the present invention is preferably applied as a protective film of a polarizing plate in a liquid crystal display device as the optical member.
- the polarizing plate with an antireflection function of the present invention is characterized in that a polarizing plate is laminated on one surface of the base film of the optical laminated film of the present invention on which the antireflection layer is not provided.
- the polarizing film that can be used in the present invention is not particularly limited as long as it has a function as a polarizer.
- a polyvinyl alcohol (PVA) -based or polyene-based polarizing film can be used.
- a polarizing film having a polarization degree of 99.9% or more is preferably used.
- the degree of polarization is defined as the transmittance (H) when two polarizing films are superimposed so that their polarization axes are parallel, and the transmission when orthogonally superimposed.
- H and H are the visibility corrected Y
- the method for producing the polarizing film is not particularly limited.
- a method of manufacturing a PVA-based polarizing film a method of uniaxially stretching after adsorbing iodine ions to a PVA-based film, a method of uniaxially stretching a PVA-based film and then adsorbing iodine ions, A method in which iodine ion adsorption and uniaxial stretching are performed simultaneously, a method in which a PVA-based film is uniaxially stretched after dyeing with a dichroic dye, a method in which a PVA-based film is uniaxially stretched and then absorbed with a dichroic dye, PVA-based There is a method of simultaneously dyeing a film with a dichroic dye and uniaxially stretching the film.
- Polyene-based polarizing films can be produced by uniaxially stretching a PVA-based film and then heating and dehydrating it in the presence of a dehydration catalyst, or by uniaxially stretching a polychlorinated vinyl-based film and then removing a hydrochloric acid catalyst.
- Known methods such as a method of heating and dehydrating in the presence, may be mentioned.
- the polarizing plate with an antireflection function of the present invention can be manufactured by laminating a polarizing film on one surface of the base film of the optical laminated film of the present invention on which the antireflection layer is not provided. it can.
- FIG. 2 shows a cross-sectional view of the layer configuration of the polarizing plate with an antireflection function of the present invention.
- the polarizing plate 81 with an anti-reflection function shown in FIG. 2 includes a layer 61 made of an adhesive or a pressure-sensitive adhesive on the side of the base film 11 of the optical laminated film 50 of the present invention where the low refractive index layer 31 is not provided. It has a structure in which the polarizing film 71 is laminated via the intermediary.
- another protective film is provided on the side of the polarizing film on which the base film is not laminated via a layer 61 made of an adhesive or a pressure-sensitive adhesive. (Not shown) may be stacked.
- the protective film is preferably a material having a low optical anisotropy.
- the material having a low optical anisotropy is not particularly limited, and examples thereof include a cellulose ester such as triacetyl cellulose and a polymer resin having an alicyclic structure. Polymer resins having an alicyclic structure are preferred because of their excellent properties.
- Examples of the polymer resin having an alicyclic structure include those similar to those described in the section of the base film of the present invention.
- Examples of the adhesive or the pressure-sensitive adhesive include the same as the adhesive or the adhesive used for laminating the polarizing plate protective film and the polarizing film.
- the thickness of the polarizing plate with an antireflection function of the present invention is not particularly limited, but is usually in a range of 60 / im-2 mm.
- the optical product of the present invention includes the polarizing plate with an antireflection function of the present invention.
- Preferred specific examples of the optical product including the polarizing plate with an anti-reflection function include a liquid crystal display device and a touch panel.
- FIG. 3 shows a layer configuration example of a liquid crystal display device including the polarizing plate with an antireflection function of the present invention.
- the liquid crystal display element 98 shown in FIG. 3 includes, in order from the bottom, a polarizing plate 91, a retardation plate 92, a liquid crystal cell 93, and a polarizing plate 81 with an antireflection function of the present invention.
- the polarizing plate 81 with an anti-reflection function is formed on the liquid crystal cell 93 by adhering to the polarizing plate surface via an adhesive or a pressure-sensitive adhesive (not shown).
- FIG. 4 for example, as shown in FIG.
- the liquid crystal cell 93 has two electrode substrates 95 each having a transparent electrode 94 arranged at a predetermined interval in a state where the transparent electrodes 94 are opposed to each other. It is produced by enclosing. Both edges of the liquid crystal 96 enclosure are sealed with a seal 97.
- a liquid crystal display device for example, a brightness enhancement film, a prism array sheet
- a prism array sheet One or two or more layers of appropriate components such as a lens array sheet, a light guide plate, a light diffusion plate, and a backlight can be arranged at appropriate positions.
- the liquid crystal mode of the liquid crystal 96 is not particularly limited.
- As the liquid crystal mode for example, TN (Twisted Nematic) type, STN (Super Twisted Nematic) type, HAN (Hybrid Alignment Nematic) type, MVA (Multiple Vertical Alignment) type, IPS (In Plane Switching) type, ⁇ CB (Optical Compensated Bend) type, etc.
- the liquid crystal display device 98 shown in FIG. 3 has a normally white mode in which the display is bright when the applied voltage is low, and is ⁇ when the applied voltage is high. Can also be used in the normally black mode.
- the optical product of the present invention includes a polarizing plate with an antireflection function that can achieve low light reflectance over a wide band. Therefore, particularly when used in a liquid crystal display device, the visibility is excellent (there is no glare or glare) and the contrast of light and dark display is excellent.
- the film was cut out every 100 mm in the length direction, and the cut out film was measured every 0.48 mm in the width direction of the film using a contact-type web thickness gauge (RC-101, manufactured by Meissan Co., Ltd.).
- the arithmetic average value of the measured values is defined as a reference film thickness T (zm).
- the film thickness variation is calculated from the following equation, with the maximum value of the measured film thickness as T ( ⁇ m) and the minimum value as T ( ⁇ m).
- Thickness variation (%) ( ⁇ - ⁇ ) / TX 100
- 200 mg of the base film is placed in a 4 mm inside diameter glass tube sample container from which water and organic substances adsorbed on the surface have been completely removed.
- the container is heated at a temperature of 100 ° C for 60 minutes, and the gas that has come out of the container is continuously collected. Then, the collected gas is thermally deaerated. It is analyzed by a gas chromatography-mass spectrometer (TDS-GC-MS), and the total amount of components having a molecular weight of 200 or less is measured as a residual volatile component.
- TDS-GC-MS gas chromatography-mass spectrometer
- Non-contact three-dimensional surface shape ⁇ Using a roughness measuring device (Zigo), with a field of view of 5.6 mm (width) x 4.4 mm (length), 480 damage in the vertical direction, 640 damage in the vertical direction, 640 damage in the horizontal direction Observe at X480 square.
- Zigo roughness measuring device
- 0 and H are the visibility-corrected Y values.
- the reflection spectrum was measured at an incident angle of 5 ° using a spectrophotometer (manufactured by JASCO Corporation: “UV-visible near-infrared spectrophotometer V-570”), and the wavelength was measured.
- the light reflectance at 430-700 nm is obtained, and the maximum value of the light reflectance at 550-nm and the maximum value of the light reflectance at 430-700 nm are defined as the light reflectance at 430-700 nm.
- the obtained polarizing plate is cut out to an appropriate size (10 inch square), and the polarizing plate (upper side of FIG. 3) is attached to the liquid crystal display element shown in FIG.
- a liquid crystal display device is manufactured by incorporating the polarizing plate 21).
- a commercially available light box product Name: LightViewer-7000PR ⁇ , manufactured by Kuba Photo Industry Co., Ltd.
- a simple liquid crystal panel is fabricated by mounting a liquid crystal display element, the display of the liquid crystal display element is blackened, and the panel is visually observed from the front. Then, the evaluation is performed in the following three stages.
- Glare caused by the appearance of points or surfaces with excessively high brightness in the field of view. ⁇ Difficult to see, meaning glaring glare directly or indirectly received from the light source) or reflection Not at all.
- the liquid crystal display element 98 shown in FIG. 3 is configured by laminating a polarizing plate 81 with an anti-reflection function on one side of a liquid crystal cell 93 and a lower polarizing plate 91 on the other side via a retardation plate 92. Is done.
- the liquid crystal sensor 93 is formed by forming an alignment film on the transparent electrode 94 surface of an electrode substrate 95 having a transparent electrode 94, and then forming two transparent electrode substrates 95 each having the transparent electrode 94. It is produced by arranging the electrodes 94 at a predetermined interval in a state where they face each other and enclosing a liquid crystal 96 in the gap. 97 is a seal.
- the liquid crystal display element 98 is held by being fixed to a plastic frame.
- an optical laminated film 50 is laminated on the polarizing film 71 via a layer 61 made of an adhesive or an adhesive on the polarizing film. .
- the obtained base film 1A had a volatile component content of 0.01% by weight or less and a saturated water absorption of 0.01% by weight or less.
- the base film 1A had a reference film thickness of 40 xm, a film thickness variation of 2.3%, and a die line depth of 0.01 xm.
- Liquid A was prepared by mixing an oligomer of tetramethoxysilane (“Methylsilicate 51” manufactured by Colcoat Co., Ltd.) with methanol at a mass ratio of 47:75, and prepared water, ammonia water (28% by weight of ammonia), and methanol.
- Solution B was prepared by mixing at a weight ratio of 60: 1.2: 97.2.
- a silicon alkoxide solution 2 was obtained in the same manner as in Production Example 3, except that the tetramethoxysilane oligomer and methanol were mixed at a mass ratio of 47:78.
- a silicon alkoxide solution 3 was obtained in the same manner as in Production Example 3, except that an oligomer of tetramethoxysilane (“Methylsilicate 51” manufactured by Colcoat) methanol was mixed at a mass ratio of 47:79. .
- a 45 zm thick PVA finolem (degree of polymerization: 2400, degree of saponification: 99.9%) is swollen in pure water, then immersed in a mixed aqueous solution containing 1% by weight of iodine and 3% by weight of potassium iodide. The film was dyed. Next, this film was immersed in a 4.5% by weight aqueous boric acid solution, stretched 5.3 times in the machine direction, and then immersed in a 5% by weight aqueous borax solution, so that the total stretching ratio in the longitudinal direction was 5.5. It was stretched so as to be twice as large. After stretching, the moisture on the film surface was removed and dried at 50 ° C. to prepare a polarizing film. The thickness of this polarizing film was 18 ⁇ m, and the degree of polarization was 99.95%.
- the hard coat layer forming composition 1 prepared in Production Example 2 was applied to one surface of the base film 1B using a die coater so that the thickness of the hard coat layer after hardening was 5 ⁇ m. It was applied continuously. Next, after drying at 80 ° C. for 5 minutes, the composition for forming a hard coat layer was cured by irradiating ultraviolet rays (integrated light amount 300 mj / cm 2 ) to obtain a hard coat layer laminated film 1C.
- the cured hard coat layer had a thickness of 5 ⁇ , a surface roughness of 0.2 / im, and a refractive index of 1.62.
- the silicon alkoxide solution 1 obtained in Production Example 3 was dropped on the high-refractive-index laminated film 1C (length 15 cm x width 15 cm), and the spin coater was used.
- the laminated film 1C was put in a rotating chamber, and the laminated film 1C was rotated to spin-coat the surface of the laminated film 1C with a silicon alkoxide solution.
- methanol was previously introduced into the rotation chamber of the spin coater so that the atmosphere became a methanol atmosphere, and the glass plate was rotated at a rotation speed of 700 rpm for 10 seconds.
- Silicon Alco After spin-coating the oxide solution, it was left for 1 minute and 15 seconds to obtain a thin film in which silicon alkoxide was gelled.
- this gel-like thin film was immersed for 5 minutes in a curing solution having a composition of water, 28% ammonia water and methanol mixed at a mass ratio of 162: 4: 640, and cured at room temperature for one day and night. did. Furthermore, the gel-like thin film thus cured was immersed in a 10% solution of hexamethyldisilazane in isopropanol to perform a hydrophobic treatment.
- the thin film-like gel-like compound subjected to the hydrophobizing treatment is washed by immersing it in isopropanol, then placed in a high-pressure vessel, and the high-pressure vessel is filled with liquefied carbon dioxide.
- a silica air port gel thin film (hereinafter, referred to as a “low refractive index layer”) having a thickness of 100 nm is formed on the surface of the laminated film 1 C.
- the obtained laminated film 1D was obtained.
- the measured refractive index of the low refractive index layer of this laminated film was 1.33.
- a fluorine-based surface antifouling coating agent (“Optool DSX", manufactured by Daikin Industries, Ltd.) was applied to the surface of the laminated film 1D where the low refractive index layer was formed, as an antifouling layer. It was diluted to 0.1% by weight with xan and applied by dip coating. After the application, the coating was heated and dried at 60 ° C. for 1 minute to form an antifouling layer having a thickness of 5 nm to obtain an optical laminated film 1E (a polarizing plate protective film).
- Optool DSX manufactured by Daikin Industries, Ltd.
- a production example was performed using an acrylic adhesive ("DP-8005 clear", manufactured by Sumitomo 3LEM) on the surface of the obtained optical laminated film 1E on which the low refractive index layer and the like were not formed.
- the polarizing film obtained in 7 was adhered to obtain a polarizing plate 1F having an antireflection function.
- the optical performance was evaluated using this polarizing plate. Table 1 shows the evaluation results.
- TAC triacetyl cellulose
- base film 1A a polyethylene terephthalate film with a thickness of 50 ⁇ (manufactured by Toyobo Co., Ltd., trade name “Cosmoshine 4300”, hereinafter referred to as “base finolem 3 ⁇ ”) is used as the base film. Except for using, the same operation as in Example 1 was performed to obtain 3% of an optical laminated film and 3F of a polarizing plate with a reflection function. At this time, the refractive index of the hard coat layer was 1.62, and the refractive index of the low refractive index layer was 1.33. The optical performance was evaluated using this polarizing plate. Table 1 shows the evaluation results.
- Example 1 was repeated except that, instead of the base film 1A, a polarizing plate using a triacetyl cellulose film (manufactured by Pola Techno Co., Ltd., trade name “Super High Contrast Polarizing Plate SKN_18243T”, degree of polarization 99.993%) was used.
- a hard coat layer and a low refractive index layer were formed to obtain an optical laminated film 4E. Since the optical laminated film 4E has a polarizing film laminated thereon, the optical performance was evaluated using this film as it was as a polarizing plate with a reflector function. Table 1 shows the evaluation results.
- Example 1 When forming the low refractive index layer, the same operation as in Example 1 was performed, except that the silicon alkoxide solution 2 obtained in Production Example 4 was used instead of the silicon alkoxide solution 1, to thereby form a polarizing plate protective film 5E. Further, a polarizing plate 5F having an antireflection function was obtained. At this time, the refractive index of the hard coat layer was 1.62, and the refractive index of the low refractive index layer was 1.39. The optical performance was evaluated using this polarizing plate. Table 1 shows the evaluation results.
- Example 2 In forming the low refractive index layer, the same operation as in Example 1 was performed except that the silicon alkoxide solution 3 obtained in Production Example 5 was used instead of the silicon alkoxide solution 1, and the optical lamination was performed. Film 6E (polarizing plate protective film) and polarizing plate 6F with an antireflection function were obtained. At this time, the refractive index of the hard coat layer was 1.62, and the refractive index of the low refractive index layer was 1.40. The optical performance was evaluated using this polarizing plate. Table 1 shows the evaluation results. [0155] Comparative Example 3
- composition for forming a hard coat layer As the composition for forming a hard coat layer, a composition 2 for forming a hard coat layer (ultraviolet curable high refractive index agent; Daicure Clear SD-715, manufactured by Dainippon Ink Co., Ltd.) was used. The same operation as in Example 1 was carried out except that the composition for forming a low refractive index layer obtained in Production Example 6 was used, to obtain an optical laminated film 7E and a polarizing plate with an antireflection function 7F. At this time, the refractive index of the hard coat layer was 1.52, and the refractive index of the low refractive index layer was 1.45. The optical performance was evaluated using this polarizing plate. Table 1 shows the evaluation results.
- Example 1 Example 2 Example 3
- Example 4 • Comparative example 1 Comparative example 2 Comparative example 3
- the optical laminated film that satisfies the above conditions (Examples 13 to 13) has small light reflectance at a wavelength of 550 nm and light reflectance at a wavelength of 430 to 700 nm, and is excellent in visibility and contrast of light and dark display.
- the optical laminated film that does not satisfy the formulas [1], [2] and [3] has a large light reflectance at a wavelength of 550 nm and a light reflectance at a wavelength of 430 to 700 nm.
- the contrast of the light and dark display is poor only because of poor visibility.
- the optical laminated film of the present invention is suitable as an antireflective protective film for an optical member because of its excellent optical properties and low light reflectance.
- the polarizing plate having an antireflection function provided with the optical laminated film can achieve low light reflectance over a wide band, and is used for optical products such as a liquid crystal display device, a touch panel, and an electorescence display device. These optical products have excellent glare with low light reflectivity and low glare, and excellent visibility. In particular, the liquid crystal display device is further excellent in contrast in light and dark display.
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Nonlinear Science (AREA)
- Chemical & Material Sciences (AREA)
- Mathematical Physics (AREA)
- Toxicology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Laminated Bodies (AREA)
- Liquid Crystal (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Devices For Indicating Variable Information By Combining Individual Elements (AREA)
- Polarising Elements (AREA)
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020057024810A KR101078127B1 (ko) | 2003-06-26 | 2004-06-28 | 광학 적층 필름, 편광판 및 광학 제품 |
JP2005511072A JPWO2005001525A1 (ja) | 2003-06-26 | 2004-06-28 | 光学積層フィルム、偏光板および光学製品 |
EP04746588.5A EP1640748A4 (en) | 2003-06-26 | 2004-06-28 | OPTICAL MULTILAYER FILM, POLARIZATION PLATE AND OPTICAL PRODUCT |
US10/562,567 US7285323B2 (en) | 2003-06-26 | 2004-06-28 | Optical multilayer film, polarizing plate and optical product |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2003181987 | 2003-06-26 | ||
JP2003-181987 | 2003-06-26 | ||
JP2003272229 | 2003-07-09 | ||
JP2003-272229 | 2003-07-09 |
Publications (1)
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WO2005001525A1 true WO2005001525A1 (ja) | 2005-01-06 |
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ID=33554449
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2004/009119 WO2005001525A1 (ja) | 2003-06-26 | 2004-06-28 | 光学積層フィルム、偏光板および光学製品 |
Country Status (6)
Country | Link |
---|---|
US (1) | US7285323B2 (ja) |
EP (1) | EP1640748A4 (ja) |
JP (2) | JPWO2005001525A1 (ja) |
KR (1) | KR101078127B1 (ja) |
TW (1) | TWI339741B (ja) |
WO (1) | WO2005001525A1 (ja) |
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JP2005037927A (ja) * | 2003-06-26 | 2005-02-10 | Nippon Zeon Co Ltd | 光学積層フィルム |
TWI395667B (zh) * | 2005-01-20 | 2013-05-11 | Lintec Corp | 抗反射薄膜 |
JP2006297329A (ja) * | 2005-04-22 | 2006-11-02 | Pentax Corp | シリカエアロゲル膜及びその製造方法 |
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JP2007286554A (ja) * | 2006-04-20 | 2007-11-01 | Kaneka Corp | 反射防止膜、反射防止基材、及び当該反射防止基材が設けられた光電変換装置 |
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JP2015165401A (ja) * | 2014-02-28 | 2015-09-17 | ティーピーケイ タッチ ソリューションズ(シアメン)インコーポレーテッド | 複合基板構造、及び、それを備えるタッチパネル |
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US10738197B2 (en) | 2015-09-11 | 2020-08-11 | Canon Kabushiki Kaisha | Optical member and method for manufacturing the same |
WO2024090540A1 (ja) * | 2022-10-28 | 2024-05-02 | 東山フイルム株式会社 | 反射防止フィルム |
Also Published As
Publication number | Publication date |
---|---|
JP5045823B2 (ja) | 2012-10-10 |
KR20060072099A (ko) | 2006-06-27 |
EP1640748A4 (en) | 2015-11-11 |
TWI339741B (en) | 2011-04-01 |
JP2011126279A (ja) | 2011-06-30 |
JPWO2005001525A1 (ja) | 2007-09-20 |
TW200508647A (en) | 2005-03-01 |
US7285323B2 (en) | 2007-10-23 |
KR101078127B1 (ko) | 2011-10-28 |
EP1640748A1 (en) | 2006-03-29 |
US20060164740A1 (en) | 2006-07-27 |
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