CN104603215A - Composition for coating highly refractive layer, and transparent conductive film comprising same - Google Patents

Composition for coating highly refractive layer, and transparent conductive film comprising same Download PDF

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Publication number
CN104603215A
CN104603215A CN201380045906.9A CN201380045906A CN104603215A CN 104603215 A CN104603215 A CN 104603215A CN 201380045906 A CN201380045906 A CN 201380045906A CN 104603215 A CN104603215 A CN 104603215A
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CN
China
Prior art keywords
fluorenes
composition
transparent
high refractor
electrically conductive
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Pending
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CN201380045906.9A
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Chinese (zh)
Inventor
洪琎基
金源国
柳茂善
徐知延
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LG Corp
LX Hausys Ltd
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LG Chemical Co Ltd
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Publication of CN104603215A publication Critical patent/CN104603215A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • 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
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • 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
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/286—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysulphones; polysulfides
    • 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
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
    • 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
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
    • 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
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • 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
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B32B27/365—Layered products comprising a layer of synthetic resin comprising polyesters comprising polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/044—Forming conductive coatings; Forming coatings having anti-static properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/67—Particle size smaller than 100 nm
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • 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
    • B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
    • B32B2264/10—Inorganic particles
    • B32B2264/102—Oxide or hydroxide
    • 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
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/202—Conductive
    • 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
    • B32B2307/412—Transparent
    • 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
    • B32B2307/418—Refractive
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
    • B32B2457/208—Touch screens
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract

Provided is a composition for coating a highly refractive layer, comprising an acrylate resin, a fluorene derivative resin, and metal oxide particles. In addition, a transparent conductive film comprising a highly refractive layer formed by using the composition for coating a highly refractive layer is provided.

Description

High refractor composition for coating and comprise its transparent and electrically conductive film
Technical field
The present invention relates to a kind of high refractor composition for coating and comprise the transparent and electrically conductive film of this high refractor composition for coating.
Background technology
According to the method detecting position, contact panel has optical mode, ultrasonic wave mode, capacitance-type, resistive film mode etc.The structure of the contact panel of resistive film mode is, transparent and electrically conductive film clips partition with the glass being attached with transparent conductor layer, relative configuration, and to transparent and electrically conductive film transmission of electricity, measures the voltage of the glass being attached with transparent conductor layer.On the other hand, the contact panel of capacitance-type, to have transparency conducting layer for basic structure on base material, not have machinery for feature, owing to having high-durability, high-transmission rate, is therefore applicable to vehicle-mounted purposes etc.
Be applicable to the transparent and electrically conductive film of above-mentioned contact panel, it is generally the one side at transparent film base material, formed from above-mentioned film base material side to prime coat and conductive layer successively, No. 2003-197035th, Japanese Laid Open Patent discloses the transparent and electrically conductive film being formed with prime coat between base material film and conductive layer.
But above-mentioned prime coat is formed by 2 layers that specific refractory power is different, and only disclose base material film side configuration thickness be high refractive index zinc oxide-stannic oxide class film and conductive layer side configuration thickness be the structure of silicon oxide film of low-refraction, the concrete composition for coating of high refractor is not recorded, therefore, to the research of the height refraction composition for coating of the adjustment for guaranteeing high refractive index simultaneously and weather resistance also in continuation.
Summary of the invention
the technical problem to be solved in the present invention
An example of the present invention provides a kind of, comprises fluorene derivatives resin, thus while can guaranteeing high refractive index, can also maintain the height refraction composition for coating of the physical properties of transparent and electrically conductive film.
An example more of the present invention provides a kind of, owing to easily regulating optical characteristics, thus reduces pattern visibility meter, guarantees the transparent and electrically conductive film that the transmissivity of the physical propertiess such as hardness is outstanding.
technical scheme
An example of the present invention provides a kind of high refractor composition for coating, and it comprises acrylate (acrylate) resin, fluorenes (fluorene) derivatives resin and metal oxide particle.
Relative to the total solids composition of 100 weight parts, about 1 weight part can be comprised to the aforesaid propylene acid ester resin of about 50 weight parts, about 1 weight part to the above-mentioned fluorene derivatives resin of about 50 weight parts and about 5 weight parts to the above-mentioned metal oxide particle of about 80 weight parts.
Above-mentioned fluorene derivatives resin can be selected from by fluorenes, Fluorenone, 2-acetamido fluorenes, 2-ethanoyl fluorenes, 2-acetamidofluorene, 9-bromine fluorenes, 9-bromo-9-phenyl fluorenes, 2, 7-diamino-fluorene, 2, 7-bis-(acetamido) fluorenes, 2, 7-diacetyl fluorenes, 9, two [4-(2-hydroxy ethoxy) phenyl] fluorenes of 9-, 9, 9-two (3, 4-bis-carboxyphenyl) fluorenes acid anhydride, 9, two (3-methyl-4-hydroxyphenyl) fluorenes of 9-, 9, two (4-hydroxyphenyl) fluorenes of 9-, 9, two (4-aminophenyl) fluorenes of 9-, 9, two (the 4-hydroxy-3-methyl phenyl) fluorenes of 9-, 9, two [4-(the 2-acryl oxyethyl group) phenyl] fluorenes of 9-, 9, two [4-(2-hydroxyl-3-acryloxypropyl) phenyl] fluorenes of 9-, 9, two (4-hydroxy phenyl) fluorenes of 9-, 2-vinylformic acid 1, 1'[9H-fluorenes-9-subunit two [4, the sub-benzene oxygen of 1-(2-hydroxyl-3, 1-propyl)]] ester and their combination composition group in one.
Above-mentioned metallic compound particle can be selected from by TiO 2, ZrO 2, Al 2o 3, SnO 2, tin indium oxide (ITO, indium-tin oxide), Sb 2o 5, Nb 2o 3, Y 2o 3, Si O 2and the one in the group of their combination composition.
The median size of above-mentioned metallic compound particle can be about 1nm to about 100nm.
Above-mentioned high refractor composition for coating also can comprise light trigger.
Relative to the total solids composition of 100 weight parts, the above-mentioned light trigger of about 1 weight part to about 15 weight parts can be comprised.
An example more of the present invention provides a kind of transparent and electrically conductive film, and it comprises the high refractor utilizing above-mentioned high refractor composition for coating to be formed.
Above-mentioned transparent and electrically conductive film can be the stepped construction of transparent substrate, above-mentioned high refractor, forming low-refractive-index layer and conductive layer.
The specific refractory power of above-mentioned high refractor can be about 1.6 to about 1.8.
The thickness of above-mentioned high refractor can be about 20nm to about 150nm.
The thickness of above-mentioned forming low-refractive-index layer can be about 5nm to about 100nm.
Above-mentioned transparent substrate can be comprise a kind of unitary film in the group that is selected from and is made up of polyethylene terephthalate (PET), Polyethylene Naphthalate (PEN), polyethersulfone (PES), polycarbonate (PC), polypropylene (PP), polyvinyl chloride (PVC), polyethylene (PE), polymethylmethacrylate (PMMA), ethylene-vinyl alcohol (EVA), polyvinyl alcohol (PVA) and their combination or stacked film.
Above-mentioned conductive layer can comprise tin indium oxide (ITO, Indium Tin Oxide) or Fluorin doped tindioxide (FTO, Fluorine-doped Tin Oxide).
Also hard coat is comprised at the single or double of above-mentioned transparent substrate.
beneficial effect
Expand the ranges of indices of refraction of the high refractor comprising above-mentioned height refraction overlay composition, easily can regulate the optical characteristics of the transparent and electrically conductive film of evaporation conductive layer.
Further, physical properties and the gas barrier properties etc. such as the pencil hardness of above-mentioned transparent and electrically conductive film, dissolubility resistent can be guaranteed, also can have outstanding transmissivity.
Accompanying drawing explanation
Fig. 1 is the figure of the section of the transparent and electrically conductive film briefly expressing one embodiment of the invention.
Fig. 2 is the figure of the section of the transparent and electrically conductive film briefly expressing yet another embodiment of the invention.
Embodiment
Below, example of the present invention is described in detail.But this just illustratively to propose, and the present invention is not limited thereto, the present invention's category claimed according to appended invention defines.
In order to clearly state the present invention, eliminating and irrelevant part is described, in specification sheets full text, using identical Reference numeral by same or similar structure unit.
In order to more clearly show multiple layer and region in the accompanying drawings, amplifying thickness and representing.And in the accompanying drawings for convenience of explanation, exaggeration shows the layer of a part and the thickness in region.
Below, arbitrary structure is formed in " upper (or under) " of base material " top (or bottom) " or base material, not only mean that arbitrary form touch is formed in the upper surface (or lower surface) of above-mentioned base material, also mean and not limit on above-mentioned base material and base material and do not comprise other structures between the arbitrary structure that (or under) is formed.
High refractor composition for coating
An example of the present invention provides a kind of high refractor composition for coating, and it comprises acrylate resin, fluorene derivatives resin and metal oxide particle.
Generally, when preparing high refractor composition for coating, in order to regulate specific refractory power, usually ZrO is used 2, TiO 2deng Acrylic Acid Monomer and ultraviolet hardening reactive oligomers that metal oxide nanoparticles and specific refractory power are about 1.49 to about 1.53.But, when only regulating the specific refractory power of high refractor composition for coating with the content of above-mentioned metal oxide nanoparticles, the curing degree of high refractor composition for coating can be reduced, thus reduce the physical properties of high refractor, have difficulties in the physical properties guaranteeing high refractor.
To this, above-mentioned high refractor composition for coating comprises metal oxide particle and fluorene derivatives resin simultaneously, even if thus when reducing the content of metal oxide particle, while also guaranteeing the high refractive index of high refractor composition for coating, the physical property strengthened can also be guaranteed.
Above-mentioned high refractor composition for coating can comprise acrylate resin, and aforesaid propylene acid ester resin can be light-cured type.Be cured according to ultraviolet or electron rays isoreactivity energy line, give the patience of weather resistance and the outside atmosphere for high temperature, high humidity, and then can be used as the object of adjustment specific refractory power and use.
Now, aforesaid propylene acid esters can comprise containing alkyl (methyl) acrylate, polyalkylene glycol (methyl) acrylate, carboxyl and (methyl) acrylic compound, (methyl) acrylic compound containing hydroxyl, (methyl) acrylic compound etc. containing nitrogen of comprising unsaturated double-bond combination.Further, epoxy (methyl) acrylate can be comprised, carbamate (methyl) acrylate, polyester (methyl) acrylate, the acrylic acid or the like oligopolymer such as polyethers (methyl) acrylate.
Particularly, aforesaid propylene acid ester resin can be selected from by double pentaerythritol methacrylate, double pentaerythritol C5 methacrylate, pentaerythritol triacrylate, tetramethyl-alcohol methane tetraacrylate, tetramethylmethane triol acrylate, trimethylolpropane triacrylate, 1, 6-hexanediyl ester, polyethyleneglycol diacrylate, diethylene glycol acrylate, triethyleneglycol acrylate, TEG acrylate, six EDIAs, propyl acrylate, butyl acrylate, amyl acrylate, 2-ethylhexyl acrylate, Octyl acrylate, vinylformic acid ester in the ninth of the ten Heavenly Stems, dihydroxyphenyl propane 2-glycidyl diacrylate, bisphenol A epoxy acrylate, oxyethane-bisphenol a diacrylate, one in the group of 2-phenoxyethyl acrylate and their combination composition.
More specifically, relative to the total solids composition of the high refractor composition for coating of 100 weight parts, the aforesaid propylene acid ester resin of about 1 weight part to about 50 weight parts can be comprised.The aforesaid propylene acid ester resin comprised be less than about 1 weight part time, pencil hardness and the close property of composition cannot be guaranteed; And be greater than about 50 weight part time, be difficult to improve specific refractory power, even if regulate metal oxide particle content to improve specific refractory power, also may be difficult to the physical properties guaranteeing composition for coating.Therefore, comprised acrylate resin is maintained in above-mentioned scope, thus while easily can realizing regulating specific refractory power, the advantage of physical properties can be guaranteed.
Above-mentioned high refractor composition for coating can comprise fluorene derivatives resin, and above-mentioned fluorene derivatives resin is likely photocurable resin.Above-mentioned fluorene derivatives resin comprises using the compound guided centered by the fluorenes of aromatic hydrocarbons, for improving the low-refraction that organism has, improve thermotolerance, substrate adherence, with the compatibility of inorganics.Further, in order to solve the low-solubility that high-density has on molecular structure, Chemical bond can be carried out with the surface of metal oxide particle, can also hydroxyl be comprised.
Particularly, above-mentioned fluorene derivatives resin can be selected from by fluorenes, Fluorenone, 2-acetamido fluorenes, 2-ethanoyl fluorenes, 2-acetamidofluorene, 9-bromine fluorenes, 9-bromo-9-phenyl fluorenes, 2, 7-diamino-fluorene, 2, 7-bis-(acetamido) fluorenes, 2, 7-diacetyl fluorenes, 9, two [4-(2-hydroxy ethoxy) phenyl] fluorenes of 9-, 9, 9-two (3, 4-bis-carboxyphenyl) fluorenes acid anhydride, 9, two (3-methyl-4-hydroxyphenyl) fluorenes of 9-, 9, two (4-hydroxyphenyl) fluorenes of 9-, 9, two (4-aminophenyl) fluorenes of 9-, 9, two (the 4-hydroxy-3-methyl phenyl) fluorenes of 9-, 9, two [4-(the 2-acryl oxyethyl group) phenyl] fluorenes of 9-, 9, two [4-(2-hydroxyl-3-acryloxypropyl) phenyl] fluorenes of 9-, 9, two (4-hydroxy phenyl) fluorenes of 9-, 2-vinylformic acid 1, 1'[9H-fluorenes-9-subunit two [4, the sub-benzene oxygen of 1-(2-hydroxyl-3, 1-propyl)]] ester and their combination composition group in one.
More specifically, relative to the total solids composition of the high refractor composition for coating of 100 weight parts, the above-mentioned fluorene derivatives resin of about 1 weight part to about 50 weight parts can be comprised.The above-mentioned fluorene derivatives resin comprised be less than about 1 weight part time, possibly cannot maintain the high refractive index of composition, the problem comprising excessive metal oxide particle can be there is thus.Further, the above-mentioned fluorene derivatives resin comprised be greater than about 50 weight part time, be difficult to the pencil hardness guaranteeing high refractor, therefore, maintain above-mentioned scope, can in adjustment specific refractory power and guarantee, in physical properties, there is advantage.
Above-mentioned high refractor composition for coating can comprise metal oxide particle.Metal oxide particle refers to and represents with particle shape the compound be made up of metallic element and oxygen element, can present electroconductibility, but, even if above-mentioned high refractor composition for coating comprises metal oxide particle, also can not electroconductibility be presented.
Now, above-mentioned metal oxide particle can be selected from by TiO 2, ZrO 2, Al 2o 3, SnO 2, tin indium oxide, Sb 2o 5, Nb 2o 3, Y 2o 3, Si O 2and the one in the group of their combination composition.
Particularly, relative to the total solids composition of the high refractor composition for coating of 100 weight parts, the above-mentioned metal oxide particle of about 5 weight parts to about 80 weight parts can be comprised.The above-mentioned metal oxide particle comprised be less than about 5 weight part time, exist specific refractory power reduce problem, and be greater than about 80 weight part time, the physical properties guaranteeing composition may be difficult to.Therefore, together comprise above-mentioned fluorene derivatives resin with above-mentioned metal oxide particle, outstanding high refractive index and physical property feature can be shown.
The median size of above-mentioned metal oxide particle is about 1nm to about 100nm, can be about 1nm to about 30nm particularly.Median size is the mean value that the several particle diameter of mensuration calculates, when the median size of above-mentioned metal oxide particle departs from above-mentioned scope, the surface light illumination comprising the high refractor of above-mentioned metal oxide particle may be high, further, mist degree (haze) may be increased due to scattering of light.Therefore, maintain the average particle size range of above-mentioned metal oxide particle, thus easily can realize the outstanding high refractor of optical characteristics.
Above-mentioned high refractor composition for coating, except acrylate resin, fluorene derivatives resin and metal oxide particle, also can comprise light trigger.Light trigger uses to form high refractor composition for coating to carry out photocuring reaction.Particularly, relative to the total solids composition of 100 weight parts, comprise the above-mentioned light trigger of about 1 weight part to about 15 weight parts, thus can photocuring reaction be promoted.
Can use as above-mentioned light trigger is selected from by 1-hydroxy-cyclohexyl-phenyl-one, 2-methyl isophthalic acid-[4-(methylthio group) phenyl]-2-morpholinopropane-1-ketone, benzyl dimethyl ketal, 1-(4-dodecylphenyl)-2-hydroxy-2-methyl propane-1-ketone, 2-hydroxy-2-methyl-1-phenyl-propane-1-ketone, 1-(4-isopropyl benzene)-2-hydroxy-2-methyl propane-1-ketone, benzophenone, 2, 2-dimethoxy-2-phenyl acetophenone, 2, 2-diethoxy-2-phenyl acetophenone, 2-hydroxy-2-methyl-1-propane-1-ketone, 4, 4 '-diethylin benzophenone, dichloro benzophenone, 2-methylanthraquinone, 2-ethyl-anthraquinone, 2-methyl thioxanthone, 2-ethyl thioxanthone, 2, 4-dimethyl thioxanthone, 2, one in the group of 4-diethyl thioxanthone and their combination composition.
Transparent and electrically conductive film
Provide transparent and electrically conductive film at another example of the present invention, it comprises the high refractor utilizing the high refractor composition for coating comprising acrylate resin, fluorene derivatives resin and metal oxide particle to be formed.
Fig. 1 is the figure of the section of the transparent and electrically conductive film briefly expressing one embodiment of the invention.With reference to Fig. 1, above-mentioned transparent and electrically conductive film 10 is the stepped construction of transparent substrate 1, hard coat 2, high refractor 3, forming low-refractive-index layer 4 and conductive layer 5.
Transparent substrate 1 can comprise transparent and that intensity is outstanding film.Particularly, above-mentioned transparent substrate 1 can be the form comprising a kind of unitary film in the group that is selected from and is made up of polyethylene terephthalate (PET), Polyethylene Naphthalate (PEN), polyethersulfone (PES), polycarbonate (PC), polypropylene (PP), polyvinyl chloride (PVC), polyethylene (PE), polymethylmethacrylate (PMMA), ethylene-vinyl alcohol (EVA), polyvinyl alcohol (PVA) and their combination or stacked film.
Above-mentioned high refractor 3 and forming low-refractive-index layer 4 play the effect improving insulativity and transmission between transparent substrate 1 and conductive layer 5, and now, high refractor can utilize above-mentioned high refractor composition for coating to be formed.
The specific refractory power of above-mentioned high refractor can be about 1.6 to about 1.8.In the process forming above-mentioned high refractor, utilize the result comprising the high refractor composition for coating of acrylate resin, fluorene derivatives resin and metal oxide particle, can be about 1.6 to about 1.8 by adjustable refractive index, and the visibility meter of transparent and electrically conductive film entirety and total light transmittance can be improved.
The thickness of above-mentioned high refractor 3 can be about 20nm to about 150nm, and the thickness of above-mentioned forming low-refractive-index layer 4 can be about 5nm to about 100nm.Such as, the aggregate thickness of above-mentioned high refractor 3 and forming low-refractive-index layer 4 can be about 25nm to about 250nm, when the aggregate thickness of above-mentioned high refractor 3 and forming low-refractive-index layer 4 is less than about 25nm, because thickness is excessively thin, thus there is transmissivity and visual improve the insufficient problem of effect; And the aggregate thickness of above-mentioned high refractor 3 and forming low-refractive-index layer 4 is when being greater than 250nm, such as, when the thickness of forming low-refractive-index layer 4 is greater than about 100nm, because the stress of each layer aggravates, likely there is crackle (Crack) and curling (Curl).
Above-mentioned conductive layer 3 is formed at the top of above-mentioned forming low-refractive-index layer 4, can comprise tin indium oxide or Fluorin doped tindioxide.
Fig. 2 is the figure of the section of the transparent and electrically conductive film briefly expressing yet another embodiment of the invention, in Fig. 2, is also formed with hard coat 2 in the bottom of transparent substrate 1.Hard coat 2 plays the effect improving surface hardness, as long as acrylic compounds etc. can be used in formation hard coat, just can utilize ad lib.
As shown in Figure 1, above-mentioned hard coat 2 only can be formed in the one side of transparent substrate 1, but as shown in Figure 2, can be formed in the two-sided of transparent substrate 1.
Below, specific embodiments of the invention are proposed.But the embodiment below recorded is only used to illustrate particularly or illustrate of the present invention, and the present invention is not limited thereto.
< preparation example >
Preparation example 1: high refractor composition for coating
High refractor composition for coating matter is prepared according to comprising ultraviolet hardening acrylate resin, ultraviolet hardening fluorene derivatives resin and metal oxide nanoparticles with the structure recorded in following table 1 and content.
Table 1
* two [4-(2-acryloyl-oxyethyl) phenyl] fluorine of fluorene derivatives: 9,9-
Preparation example 2: hard coating composition
Relative to the total solids composition of 100 weight parts, mix the HX-920UV (Kyoeisha of the double pentaerythritol methacrylate of 20 weight parts, 60 weight parts, common prosperity society), the silica microparticle (trade name: XBA-ST of 15 weight parts, one mountain chemistry), gorgeous good solid-184 (Ciba of Photoepolymerizationinitiater initiater of 5 weight parts, vapour Bagong department) after, dilute with diluting solvent methyl ethyl ketone (MEK), prepare the hard coating composition (specific refractory power 1.52) that solids component is 45%.
Preparation example 3: forming low-refractive-index layer composition for coating
Tetraethoxy orthosilicic acid and water, ethanol are mixed with the ratio of 1:2:2, and drops into the salpeter solution of 0.1mol, carry out the reaction of 24 hours, synthesize the colloidal sol that specific refractory power is 1.43.Utilize methyl ethyl ketone to dilute the colloidal sol of synthesis, prepare the forming low-refractive-index layer composition for coating that solids component is 5%.
< embodiment and comparative example >
Embodiment 1
Utilize the hard coating composition that U.S. sub-rod (Meyer bar) will be prepared by preparation example 2, on the polyethylene terephthalates of 125 μm (PET) film, the thickness being applied as desciccator diaphragm is 1.5 μm, recycle the ultraviolet of the high-pressure mercury light irradiation 300mJ of 180W and be cured, preparing film.At the reverse side of above-mentioned prepared film, the thickness using the method identical with aforesaid method the hard coating composition prepared by preparation example 2 to be applied as desciccator diaphragm is 1.5 μm, and after being cured, prepares the two-sided film all comprising hard coat.
Afterwards, at the two-sided one side all comprising the film of hard coat, utilize the high refractor composition for coating prepared by preparation example 1-1, the thickness being applied as desciccator diaphragm is 50nm, utilize the ultraviolet of the high-pressure mercury light irradiation 300mJ of 180W and be cured, thus forming high refractor.Thereafter, at above-mentioned high refractor, utilize the forming low-refractive-index layer coating liquid composition prepared by preparation example 3, the thickness being applied as desciccator diaphragm is 20nm, carries out the solidification of 1 minute in the baking box of 150 DEG C, thus forms forming low-refractive-index layer.Now, utilize indium: tin indium oxide (ITO) target of tin=95:5, form at forming low-refractive-index layer tin indium oxide (ITO) layer that film thickness is 20nm, thus prepare transparent and electrically conductive film.
Embodiment 2
Except high refractor composition for coating is suitable for preparation example 1-2, being applied as high refractor thickness is beyond 45nm, prepares transparent and electrically conductive film with the method identical with above-described embodiment 1.
Embodiment 3
Except high refractor composition for coating is suitable for preparation example 1-3, being applied as high refractor thickness is beyond 40nm, prepares transparent and electrically conductive film with the method identical with above-described embodiment 1.
Comparative example 1
Except high refractor composition for coating is suitable for preparation example 1-4, being applied as high refractor thickness is beyond 50nm, prepares transparent and electrically conductive film with the method identical with above-described embodiment 1.
Comparative example 2
Except high refractor composition for coating is suitable for preparation example 1-5, being applied as high refractor thickness is beyond 50nm, prepares transparent and electrically conductive film with the method identical with above-described embodiment 1.
Comparative example 3
Except high refractor composition for coating is suitable for preparation example 1-6, being applied as high refractor thickness is beyond 45nm, prepares transparent and electrically conductive film with the method identical with above-described embodiment 1.
< experimental example >: the physical property of transparent and electrically conductive film
Utilize the transparent and electrically conductive film of above-described embodiment and comparative example to measure following multiple physical properties, and its result is recorded in lower list 2.
1) specific refractory power: utilize prism coupler (Prism coupler), use the specific refractory power in each wavelength of laser determination of 532nm, 632.8nm, 830nm, and obtain the specific refractory power in 550nm by Cauchy's theorem (caushy plot).
2) pencil hardness: be as the criterion with JIS K 5600-5-4 and measure.
3) close property: utilize cutting unit by overlay surface, with the width × length of the spacing of 1mm and 10mm × 10mm, after cutting into chessboard apperance, utilize scotch tape (Nichiban, meter Qi Bang company) to carry out stripping test.Utilize adhesive tape to carry out 3 stripping tests to same position, after evaluation, mark by/100 the numeral be close to.
4) transmissivity, transmission b*/reflection b*: utilize CM-5 (Konica minolta, Konica Minolta company), measure total light transmittance and transmission b*/reflection b* value.
5) etch (Etching) to evaluate: utilize the face shield of square patterning at indium tin oxide layer coating sensing optical activity resin, after carrying out dry solidification, at 25 DEG C, dipping 1 minute in the aqueous hydrochloric acid of 5%, thus implement the etching evaluation of indium tin oxide layer.
6) measure the difference (Δ R) of the front/rear reflectivity of etching (Etching) and confirm the hidden power of pattern: measuring reflectivity at the front/rear CM-5 that utilizes of etching (Etching), try to achieve the difference of reflectivity, and confirm the hidden power of pattern by naked eyes.
Table 2
◎: very outstanding, zero: outstanding, △: general, ×: poor
By measurement result, the transparent and electrically conductive film can understanding embodiment 1 to embodiment 3 has outstanding hardness, transmissivity and visibility meter.Particularly, comprise the situation of the transparent and electrically conductive film of the comparative example 1 of the high refractor formed by the composition for coating of the preparation example 1-4 not comprising fluorene derivatives, the specific refractory power of the high refractor be measured to is low.Further, the transmissivity be measured to and to etch the difference of front/rear reflectivity higher than embodiment 1 to embodiment 3, the hidden power of pattern is also poor, therefore, it is possible to understand not outstanding as the optical property of transparent and electrically conductive film.
Comprise the situation of the transparent and electrically conductive film of the comparative example 2 of the high refractor formed by the composition for coating of the preparation example 1-5 not comprising fluorene derivatives, because the specific refractory power of high refractor is similar to embodiment 1, therefore, there is outstanding optical characteristics and the hidden power of pattern, but physical property cannot be guaranteed in pencil hardness and close property aspect.
And, comprise by comprising fluorene derivatives, but the situation of the transparent and electrically conductive film of the comparative example 3 of the high refractor that the composition for coating not comprising the preparation example 1-6 of ultraviolet hardening acrylate is formed, owing to comprising fluorene derivatives, therefore in the specific refractory power of high refractor, higher specific refractory power is measured to, but the evaluation obtained in pencil hardness and close property generally, so, be difficult to be applicable to transparent and electrically conductive film.
In sum, known, the specific refractory power of the high refractor formed by the high refractor composition for coating comprising ultraviolet hardening acrylate resin, ultraviolet hardening fluorene derivatives resin and metal oxide nanoparticles simultaneously can be 1.6 to 1.8, and the transparent and electrically conductive film comprising this high refractor composition for coating can guarantee the optical characteristics transitivity that hardness, transmissivity, visibility meter etc. are outstanding simultaneously.

Claims (16)

1. a high refractor composition for coating, is characterized in that, comprises acrylate resin, fluorene derivatives resin and metal oxide particle.
2. high refractor composition for coating according to claim 1, is characterized in that, described acrylate resin or described fluorene derivatives resin are photocurable resin.
3. high refractor composition for coating according to claim 1, it is characterized in that, relative to the total solids composition of 100 weight parts, comprise the described acrylate resin of 1 weight part to 50 weight part, the described fluorene derivatives resin of 1 weight part to 50 weight part and the described metal oxide particle of 5 weight part to 80 weight parts.
4. high refractor composition for coating according to claim 1, is characterized in that, described fluorene derivatives resin is selected from by fluorenes, Fluorenone, 2-acetamido fluorenes, 2-ethanoyl fluorenes, 2-acetamidofluorene, 9-bromine fluorenes, 9-bromo-9-phenyl fluorenes, 2,7 diamin of luorene, 2,7-bis-(acetamido) fluorenes, 2,7-diacetyl fluorenes, two [4-(2-hydroxy ethoxy) phenyl] fluorenes of 9,9-, two (3,4-bis-carboxyphenyl) the fluorenes acid anhydride of 9,9-, two (3-methyl-4-hydroxyphenyl) fluorenes of 9,9-, two (4-hydroxyphenyl) fluorenes of 9,9-, two (4-aminophenyl) fluorenes of 9,9-, two (the 4-hydroxy-3-methyl phenyl) fluorenes of 9,9-, two [4-(the 2-acryl oxyethyl group) phenyl] fluorenes of 9,9-, two [4-(2-hydroxyl-3-acryloxypropyl) phenyl] fluorenes of 9,9-, two (4-hydroxy phenyl) fluorenes of 9,9-, 2-vinylformic acid 1,1'[9H-fluorenes-9-subunit two [sub-benzene oxygen (2-hydroxyl-3,1-propyl) of 4,1-]] ester and their combination compositions group in one.
5. high refractor composition for coating according to claim 1, is characterized in that, described metallic compound particle is selected from by TiO 2, ZrO 2, Al 2o 3, SnO 2, tin indium oxide, Sb 2o 5, Nb 2o 3, Y 2o 3, SiO 2and the one in the group of their combination composition.
6. high refractor composition for coating according to claim 1, is characterized in that, the median size of described metallic compound particle is 1nm to 100nm.
7. high refractor composition for coating according to claim 1, is characterized in that, also comprise light trigger.
8. high refractor composition for coating according to claim 7, is characterized in that, relative to the total solids composition of 100 weight parts, comprises the described light trigger of 1 weight part to 15 weight part.
9. a transparent and electrically conductive film, is characterized in that, comprises the high refractor utilizing the high refractor composition for coating in claim 1 to be formed.
10. transparent and electrically conductive film according to claim 9, is characterized in that, described transparent and electrically conductive film is the stepped construction of transparent substrate, described high refractor, forming low-refractive-index layer and conductive layer.
11. transparent and electrically conductive films according to claim 9, is characterized in that, the specific refractory power of described high refractor is 1.6 to 1.8.
12. transparent and electrically conductive films according to claim 9, is characterized in that, the thickness of described high refractor is 20nm to 150nm.
13. transparent and electrically conductive films according to claim 10, is characterized in that, the thickness of described forming low-refractive-index layer is 5nm to 100nm.
14. transparent and electrically conductive films according to claim 10, it is characterized in that, described transparent substrate comprises a kind of unitary film in the group that is selected from and is made up of polyethylene terephthalate, Polyethylene Naphthalate, polyethersulfone, polycarbonate, polypropylene, polyvinyl chloride, polyethylene, polymethylmethacrylate, ethylene-vinyl alcohol, polyvinyl alcohol and their combination or stacked film.
15. transparent and electrically conductive films according to claim 10, is characterized in that, described conductive layer comprises tin indium oxide or Fluorin doped tindioxide.
16. transparent and electrically conductive films according to claim 10, is characterized in that, also comprise hard coat at the single or double of described transparent substrate.
CN201380045906.9A 2012-09-03 2013-01-08 Composition for coating highly refractive layer, and transparent conductive film comprising same Pending CN104603215A (en)

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