WO2016088809A1 - 透明導電性フィルム積層体及びその用途 - Google Patents

透明導電性フィルム積層体及びその用途 Download PDF

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Publication number
WO2016088809A1
WO2016088809A1 PCT/JP2015/083903 JP2015083903W WO2016088809A1 WO 2016088809 A1 WO2016088809 A1 WO 2016088809A1 JP 2015083903 W JP2015083903 W JP 2015083903W WO 2016088809 A1 WO2016088809 A1 WO 2016088809A1
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transparent conductive
conductive film
film
resin
layer
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PCT/JP2015/083903
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English (en)
French (fr)
Japanese (ja)
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直樹 津野
基希 拝師
細川　和人
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日東電工株式会社
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Application filed by 日東電工株式会社 filed Critical 日東電工株式会社
Priority to KR1020177016930A priority Critical patent/KR102002235B1/ko
Priority to CN201580065788.7A priority patent/CN107000409B/zh
Publication of WO2016088809A1 publication Critical patent/WO2016088809A1/ja

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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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • 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
    • B32B27/36—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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • 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
    • 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
    • B32B2457/00—Electrical equipment
    • B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
    • B32B2457/208—Touch screens

Definitions

  • the present invention relates to a transparent conductive film laminate and its use, and is a technique particularly useful for preventing film breakage.
  • Patent Document 1 proposes a transparent conductive film using a cycloolefin resin as a low retardation substrate film.
  • a cycloolefin resin is used for the substrate film, the substrate is very brittle and easily damaged. Therefore, in order to convey by a roll to roll manufacturing method, a hard coat process is required for the base film.
  • Patent Document 2 discloses a laminate in which a protective film is laminated on a transparent conductive film in order to prevent breakage of the film and improve handling properties.
  • Such a document discloses a laminate in which a cycloolefin-based resin film is used as a base film of a transparent conductive film and a PET base material is used as a surface protection film, and is laminated via an adhesive layer.
  • the antiblocking layer which has antiblocking property and scratch resistance can be formed by apply
  • the film is easily broken, and this increases the risk that the entire laminate is broken by the roll-to-roll manufacturing method.
  • the object of the present invention is to prevent the transparent resin film from being scratched when a cycloolefin resin or a polycarbonate resin is used as the base material of the transparent conductive film. It is to provide a transparent conductive film laminate capable of securing the subsequent process yield and its application without causing breakage in the transparent conductive film laminate even when the tension is applied.
  • the transparent conductive film laminate of the present invention includes a carrier film having an adhesive layer on one surface side of the protective film, and a transparent conductive film laminated so as to be peelable through the adhesive layer.
  • a transparent conductive film laminate wherein the transparent conductive film has a transparent conductive film, a first cured resin layer, a transparent resin film, and a second cured resin layer in this order, and the transparent conductive film
  • the resin film is made of cycloolefin resin or polycarbonate resin, the thickness of the transparent conductive film is 20 ⁇ m to 150 ⁇ m, and the carrier film is formed with the second cured resin layer of the transparent conductive film.
  • the protective film is made of an amorphous resin, and the arithmetic average surface of the surface side of the protective film that does not have the adhesive layer Roughness Ra is 0.01 ⁇ m or more, and the transparent conductive film laminate does not break when the transparent conductive film laminate is subjected to a 180 ° bending test. It is characterized by being.
  • the various physical property values in the present invention are values measured by the methods employed in Examples and the like.
  • both the anti-breaking property and the anti-blocking property are achieved by providing the arithmetic average surface roughness Ra to the surface of the protective film itself without separately providing an anti-blocking layer.
  • the break of the transparent conductive film laminate is transparent when the long transparent conductive film laminate meanders due to the influence of the heating roll in the apparatus and the heat weight during sputtering during conveyance by the roll-to-roll manufacturing method.
  • Measures such as correcting the meandering by applying tension to the conductive film laminate are often caused by this measure.
  • the tension is applied for the meandering correction, the cured resin layer is broken, and the long transparent conductive film laminate is broken due to the crack.
  • vacuum film-forming methods such as sputtering, it is necessary to form the film in an atmosphere from which impurities such as resin components and water vapor have been removed, but once the transparent conductive film laminate breaks in the vacuum film-forming device Then, it is necessary to open the sputter film formation chamber to the atmosphere and perform from the re-installation of the transparent conductive film laminate to the cleaning, resulting in a significant deterioration in productivity.
  • a transparent conductive film laminate comprising a carrier film having a pressure-sensitive adhesive layer on one surface side of the protective film, and a transparent conductive film laminated releasably via the pressure-sensitive adhesive layer.
  • the transparent conductive film laminate of the present invention is preferably embossed on the surface of the protective film that does not have the pressure-sensitive adhesive layer.
  • embossing one side of the protective film as in the present invention antiblocking properties can be imparted without providing an antiblocking layer that tends to be the starting point of fracture.
  • the protective film in the present invention is preferably made of a melt-extruded polycarbonate resin or a melt-extruded cycloolefin resin. Since processing such as embossing can be performed on one side of the protective film with a satin roll during melt extrusion, antiblocking properties can be efficiently imparted without providing an antiblocking layer that tends to be the starting point of fracture.
  • the thickness of the protective film in the present invention is preferably 20 ⁇ m to 150 ⁇ m.
  • the transparent conductive film laminate of the present invention preferably further includes one or more optical adjustment layers between the first cured resin layer and the transparent conductive film. Since the refractive index can be controlled by the optical adjustment layer, even when the transparent conductive film is patterned, the difference in reflectance between the pattern forming portion and the pattern opening can be reduced, the transparent conductive film pattern is difficult to see, and the touch panel, etc. Visibility is improved in the display device.
  • FIG. 1 is a cross-sectional view schematically showing one embodiment of the transparent conductive film laminate of the present invention
  • FIG. 2 is a schematic cross section of the transparent conductive film laminate according to another embodiment of the present invention.
  • the transparent conductive film laminate includes a carrier film 10 having a pressure-sensitive adhesive layer 2 on one surface side of the protective film 1 and a transparent conductive film 20 laminated so as to be peelable via the pressure-sensitive adhesive layer 2.
  • the said transparent conductive film 20 has the transparent conductive film 6, the 1st cured resin layer 5, the transparent resin film 4, and the 2nd cured resin layer 3 in this order.
  • FIG. 6 has the transparent conductive film 6, the 1st cured resin layer 5, the transparent resin film 4, and the 2nd cured resin layer 3 in this order.
  • one optical adjustment layer 7 can be further provided between the first cured resin layer 5 and the transparent conductive film 6, but two or more optical adjustment layers 7 are provided. Can also be provided.
  • the 1st cured resin layer 5 and the 2nd cured resin layer 3 include what functions as an antiblocking layer or a hard-coat layer.
  • the carrier film 10 is laminated
  • the transparent conductive film has a transparent conductive film, a first cured resin layer, a transparent resin film, and a second cured resin layer in this order.
  • the transparent conductive film can further include one or more optical adjustment layers between the first cured resin layer and the transparent conductive film.
  • the thickness of the transparent conductive film is preferably in the range of 20 to 150 ⁇ m, more preferably in the range of 25 to 100 ⁇ m, and still more preferably in the range of 30 to 80 ⁇ m.
  • the thickness of the transparent conductive film is less than the lower limit of the above range, the mechanical strength is insufficient, and it becomes difficult to continuously form a cured resin layer or a transparent conductive film by making the film base into a roll shape. There is.
  • the thickness exceeds the upper limit of the above range, the scratch resistance of the transparent conductive film and the dot characteristics for touch panels may not be improved.
  • the transparent resin film is formed of a cycloolefin resin or a polycarbonate resin, and has high transparency and low water absorption characteristics. By adopting the cycloolefin resin or the polycarbonate resin, it becomes possible to control the optical characteristics of the transparent conductive film used in the transparent conductive film laminate.
  • the cycloolefin resin is not particularly limited as long as it is a resin having a monomer unit composed of a cyclic olefin (cycloolefin).
  • the cycloolefin resin used for the transparent resin film may be either a cycloolefin polymer (COP) or a cycloolefin copolymer (COC).
  • the cycloolefin copolymer refers to an amorphous cyclic olefin resin that is a copolymer of a cyclic olefin and an olefin such as ethylene.
  • cyclic olefin there are a polycyclic cyclic olefin and a monocyclic cyclic olefin.
  • polycyclic olefins include norbornene, methylnorbornene, dimethylnorbornene, ethylnorbornene, ethylidenenorbornene, butylnorbornene, dicyclopentadiene, dihydrodicyclopentadiene, methyldicyclopentadiene, dimethyldicyclopentadiene, tetracyclododecene.
  • Methyltetracyclododecene dimethylcyclotetradodecene, tricyclopentadiene, tetracyclopentadiene, and the like.
  • monocyclic olefins include cyclobutene, cyclopentene, cyclooctene, cyclooctadiene, cyclooctatriene, and cyclododecatriene.
  • Cycloolefin-based resins are also available as commercial products, such as “ZEONOR” manufactured by ZEON Corporation, “ARTON” manufactured by JSR, “TOPAS” manufactured by Polyplastics, “APEL” manufactured by Mitsui Chemicals, and the like. It is done.
  • the polycarbonate resin is not particularly limited, and examples thereof include aliphatic polycarbonate, aromatic polycarbonate, and aliphatic-aromatic polycarbonate. Specifically, for example, bisphenol A polycarbonate, branched bisphenol A polycarbonate, foamed polycarbonate, copolycarbonate, block copolycarbonate, polyester carbonate, polyphosphonate carbonate, diethylene glycol bisallyl carbonate (CR-) as polycarbonate (PC) using bisphenols 39).
  • Polycarbonate-based resins also include those blended with other components such as bisphenol A polycarbonate blends, polyester blends, ABS blends, polyolefin blends, styrene-maleic anhydride copolymer blends. Examples of commercially available polycarbonate resin include “OPCON” manufactured by Ewa Co., Ltd., “Panlite” manufactured by Teijin Limited, and “Iupilon (UV absorber-containing polycarbonate)” manufactured by Mitsubishi Gas Chemical.
  • the transparent resin film is preliminarily subjected to etching treatment such as sputtering, corona discharge, flame, ultraviolet irradiation, electron beam irradiation, chemical conversion, oxidation, and undercoating treatment on the surface, and a cured resin layer formed on the transparent resin film or transparent You may make it improve adhesiveness with an electrically conductive film. Moreover, before forming a cured resin layer and a transparent conductive film, you may remove and clean the surface of a transparent resin film by solvent washing
  • the thickness of the transparent resin film is preferably in the range of 20 to 150 ⁇ m, more preferably in the range of 25 to 100 ⁇ m, and still more preferably in the range of 30 to 80 ⁇ m.
  • the glass transition temperature of the cycloolefin resin or polycarbonate resin forming the transparent resin film is preferably 130 ° C. or higher, and more preferably 140 ° C. or higher.
  • the transparent resin film can be easily a low retardation film having an in-plane retardation (R0) of 0 nm to 10 nm or a ⁇ / 4 film having an in-plane retardation of about 80 nm to 150 nm. When used together, the visibility can be improved.
  • the in-plane retardation (R0) refers to an in-plane retardation value measured with light having a wavelength of 589 nm at 23 ° C.
  • the cured resin layer includes a first cured resin layer provided on one surface side of the transparent resin film and a second cured resin layer provided on the other surface side.
  • the transparent resin film formed of cycloolefin resin or polycarbonate resin is easily scratched in each process such as formation of a transparent conductive film, patterning of a transparent conductive film, or mounting on an electronic device.
  • the first cured resin layer and the second cured resin layer are formed on both sides of the transparent resin film.
  • the cured resin layer is a layer obtained by curing a curable resin.
  • the resin to be used those having sufficient strength as a film after forming the cured resin layer and having transparency can be used without particular limitation, but thermosetting resin, ultraviolet curable resin, electron beam curable resin, two-component Examples thereof include mixed resins.
  • thermosetting resin, ultraviolet curable resin, electron beam curable resin, two-component Examples thereof include mixed resins.
  • an ultraviolet curable resin that can efficiently form a cured resin layer by a simple processing operation by a curing treatment by ultraviolet irradiation is preferable.
  • the ultraviolet curable resin examples include polyesters, acrylics, urethanes, amides, silicones, epoxies, and the like, and ultraviolet curable monomers, oligomers, polymers, and the like are included.
  • the ultraviolet curable resin preferably used is an acrylic resin or an epoxy resin, more preferably an acrylic resin.
  • the cured resin layer may contain particles. By blending the particles in the cured resin layer, ridges can be formed on the surface of the cured resin layer, and blocking resistance can be suitably imparted to the transparent conductive film.
  • inorganic particles such as silica, alumina, titania, zirconia, calcium oxide, polymethyl methacrylate, polystyrene, polyurethane, acrylic resin, acryl-styrene copolymer, benzoguanamine, melamine, polycarbonate, and other cross-linked or uncrosslinked polymers.
  • examples include crosslinked organic particles and silicone particles.
  • the particles can be used by appropriately selecting one type or two or more types, but organic particles are preferable.
  • the organic particles are preferably acrylic resins from the viewpoint of refractive index.
  • the mode particle diameter of the particles can be appropriately set in consideration of the degree of protrusion of the cured resin layer and the thickness of a flat region other than the protrusion, and is not particularly limited. From the viewpoint of sufficiently imparting blocking resistance to the transparent conductive film and sufficiently suppressing increase in haze, the mode particle diameter of the particles is within the range of ⁇ 50% of the thickness of the cured resin layer. It is preferable to use a diameter.
  • “mode particle size” means a particle size showing the maximum value of the particle distribution, and a flow type particle image analyzer (product name “FPTA-3000S” manufactured by Sysmex) is used.
  • the measurement sample is prepared by diluting the particles to 1.0% by weight with ethyl acetate and uniformly dispersing the particles using an ultrasonic cleaner.
  • the content of the particles is preferably 0.05 to 1.0 part by weight, more preferably 0.1 to 0.5 part by weight, based on 100 parts by weight of the solid content of the resin composition. More preferably, it is 1 to 0.2 parts by weight.
  • the content of the particles in the cured resin layer is small, there is a tendency that bulges sufficient to impart blocking resistance and slipperiness to the surface of the cured resin layer are hardly formed.
  • the content of the particles is too large, the haze of the transparent conductive film increases due to light scattering by the particles, and the visibility tends to decrease.
  • the cured resin layer is formed by applying a resin composition containing particles, a crosslinking agent, an initiator, a sensitizer and the like to be added to each curable resin as necessary on a transparent resin film, and the resin composition contains a solvent. Is obtained by drying the solvent and curing by application of either heat, active energy rays or both.
  • heat known means such as an air circulation oven or an IR heater can be used, but it is not limited to these methods.
  • active energy rays include, but are not limited to, ultraviolet rays, electron beams, and gamma rays.
  • the cured resin layer can be formed by a wet coating method (coating method) or the like using the above materials.
  • a wet coating method coating method
  • the crystallization time of the transparent conductive film can be shortened if the surface of the cured resin layer that is the base layer is smooth.
  • the cured resin layer is preferably formed by a wet coating method.
  • the thickness of the cured resin layer is preferably 0.5 ⁇ m to 5 ⁇ m, more preferably 0.7 ⁇ m to 3 ⁇ m, and most preferably 0.8 ⁇ m to 2 ⁇ m.
  • the thickness of the cured resin layer is within the above range, it is possible to prevent scratching and film wrinkles in the cured shrinkage of the cured resin layer, and to prevent the visibility of a touch panel and the like from being deteriorated.
  • Transparent conductive film It is preferable that a transparent conductive film is provided on the 1st cured resin layer provided in the one surface side of the transparent resin film.
  • the constituent material of the transparent conductive film is not particularly limited as long as it contains an inorganic substance. From the group consisting of indium, tin, zinc, gallium, antimony, titanium, silicon, zirconium, magnesium, aluminum, gold, silver, copper, palladium, tungsten A metal oxide of at least one selected metal is preferably used.
  • the metal oxide may further contain a metal atom shown in the above group, if necessary.
  • ITO indium oxide
  • ATO tin oxide
  • the thickness of the transparent conductive film is not particularly limited, but the thickness is preferably 10 nm or more in order to obtain a continuous film having good conductivity with a surface resistance of 1 ⁇ 10 3 ⁇ / ⁇ or less.
  • the film thickness is preferably 15 to 35 nm, more preferably in the range of 20 to 30 nm, since transparency is lowered when the film thickness becomes too thick.
  • the thickness of the transparent conductive film is less than 10 nm, the electrical resistance of the film surface increases and it becomes difficult to form a continuous film. Further, when the thickness of the transparent conductive film exceeds 35 nm, the transparency may be lowered.
  • the formation method of the transparent conductive film is not particularly limited, and a conventionally known method can be adopted. Specific examples include dry processes such as vacuum deposition, sputtering, and ion plating. In addition, an appropriate method can be adopted depending on the required film thickness.
  • dry processes such as vacuum deposition, sputtering, and ion plating.
  • an appropriate method can be adopted depending on the required film thickness.
  • the transparent conductive film is formed by dry processes, such as sputtering method, the surface of a transparent conductive film is the 1st hardening which is the foundation layer The surface shape of the resin layer is substantially maintained. Therefore, when a protrusion exists in the 1st cured resin layer, blocking resistance and slipperiness can be suitably given also to the transparent conductive film surface.
  • the transparent conductive film can be crystallized by performing a heat annealing treatment (for example, at 80 to 150 ° C. for about 30 to 90 minutes in an air atmosphere) as necessary. By crystallizing the transparent conductive film, the transparency and durability are improved in addition to the resistance of the transparent conductive film being reduced.
  • the means for converting the amorphous transparent conductive film into crystalline is not particularly limited, and an air circulation oven, an IR heater, or the like is used.
  • a transparent conductive film in which a transparent conductive film is formed on a transparent resin film is immersed in hydrochloric acid having a concentration of 5% by weight at 20 ° C. for 15 minutes, then washed with water and dried for 15 mm.
  • hydrochloric acid having a concentration of 5% by weight at 20 ° C. for 15 minutes, then washed with water and dried for 15 mm.
  • the surface resistance value can be measured by the 4-terminal method according to JIS K7194.
  • the transparent conductive film may be patterned by etching or the like.
  • the patterning of the transparent conductive film can be performed using a conventionally known photolithography technique.
  • An acid is preferably used as the etching solution.
  • the acid include inorganic acids such as hydrogen chloride, hydrogen bromide, sulfuric acid, nitric acid, phosphoric acid, organic acids such as acetic acid, mixtures thereof, and aqueous solutions thereof.
  • the transparent conductive film is preferably patterned in a stripe shape.
  • the transparent conductive film is patterned by etching, if the transparent conductive film is first crystallized, patterning by etching may be difficult. Therefore, it is preferable to perform the annealing treatment of the transparent conductive film after patterning the transparent conductive film.
  • the transparent conductive film when the transparent conductive film is formed by a dry process such as a sputtering method, a transparent resin film formed on both surfaces of the first cured resin layer and the second cured resin layer is formed on a protective film described later. It is preferable to laminate
  • the transparent conductive film is preferably annealed continuously as a long transparent conductive film laminate while being conveyed by a roll-to-roll manufacturing method.
  • the transparent conductive film may include metal nanowires.
  • a metal nanowire is a conductive material having a metal material, a needle shape or a thread shape, and a diameter of nanometer.
  • the metal nanowire may be linear or curved. If a transparent conductive layer composed of metal nanowires is used, the metal nanowires can be formed into a mesh shape, so that even with a small amount of metal nanowires, a good electrical conduction path can be formed, and transparent with low electrical resistance. A conductive film can be obtained. Furthermore, when the metal nanowire has a mesh shape, an opening is formed in the mesh space, and a transparent conductive film having high light transmittance can be obtained.
  • any appropriate metal can be used as long as it is a highly conductive metal.
  • a metal which comprises the said metal nanowire silver, gold
  • silver, copper, or gold is preferable from the viewpoint of conductivity, and silver is more preferable.
  • optical adjustment layer One or more optical adjustment layers may be further included between the first cured resin layer and the transparent conductive film.
  • the optical adjustment layer increases the transmittance of the transparent conductive film, or when the transparent conductive film is patterned, the transmittance difference or reflectance difference between the pattern part where the pattern remains and the opening part where the pattern does not remain. Is used to obtain a transparent conductive film excellent in visibility.
  • the optical adjustment layer is formed of an inorganic material, an organic material, or a mixture of an inorganic material and an organic material.
  • a material for forming the optical adjustment layer NaF, Na 3 AlF 6 , LiF, MgF 2 , CaF 2, SiO 2 , LaF 3 , CeF 3 , Al 2 O 3 , TiO 2 , Ta 2 O 5 , ZrO 2 .
  • inorganic substances such as ZnO, ZnS, and SiO x (x is 1.5 or more and less than 2)
  • organic substances such as acrylic resins, epoxy resins, urethane resins, melamine resins, alkyd resins, and siloxane polymers.
  • thermosetting resin made of a mixture of a melamine resin, an alkyd resin, and an organic silane condensate as the organic substance.
  • the optical adjustment layer can be formed using the above materials by a coating method such as a wet method, a gravure coating method or a bar coating method, a vacuum deposition method, a sputtering method, an ion plating method, or the like.
  • the optical adjustment layer may have nanoparticles having an average particle diameter of 1 nm to 500 nm.
  • the content of the nanoparticles in the optical adjustment layer is preferably 0.1% by weight to 90% by weight.
  • the average particle diameter of the nanoparticles used in the optical adjustment layer is preferably in the range of 1 nm to 500 nm, and more preferably 5 nm to 300 nm.
  • the content of the nanoparticles in the optical adjustment layer is more preferably 10% by weight to 80% by weight, and further preferably 20% by weight to 70% by weight.
  • Examples of the inorganic oxide forming the nano fine particles include fine particles such as silicon oxide (silica), hollow nano silica, titanium oxide, aluminum oxide, zinc oxide, tin oxide, zirconium oxide, and niobium oxide.
  • fine particles of silicon oxide (silica), titanium oxide, aluminum oxide, zinc oxide, tin oxide, zirconium oxide, and niobium oxide are preferable. These may be used alone or in combination of two or more.
  • the thickness of the optical adjustment layer is preferably 10 nm to 200 nm, more preferably 20 nm to 150 nm, and even more preferably 30 nm to 130 nm. If the thickness of the optical adjustment layer is too small, it is difficult to form a continuous film. Moreover, when the thickness of the optical adjustment layer is excessively large, the transparency of the transparent conductive film tends to be reduced or cracks tend to occur.
  • the metal wiring can be formed by etching after forming the metal layer on the transparent conductive film.
  • a photosensitive metal paste as follows. That is, after the transparent conductive film is patterned, the metal wiring is formed by applying a photosensitive conductive paste described later on the transparent resin film or the transparent conductive film, forming a photosensitive metal paste layer, and forming a photomask. The photosensitive metal paste layer is exposed through a photomask after being laminated or brought close to each other, then developed and patterned to obtain a drying process. That is, the metal wiring pattern can be formed by a known photolithography method or the like.
  • the photosensitive conductive paste preferably contains conductive particles such as metal powder and a photosensitive organic component.
  • the material of the conductive particles of the metal powder preferably contains at least one selected from the group consisting of Ag, Au, Pd, Ni, Cu, Al, and Pt, and more preferably Ag.
  • the volume average particle diameter of the conductive particles of the metal powder is preferably 0.1 ⁇ m to 2.5 ⁇ m.
  • the conductive particles other than the metal powder may be metal-coated resin particles in which the resin particle surfaces are coated with metal.
  • the material of the resin particles the above-mentioned particles are included, but an acrylic resin is preferable.
  • the metal-coated resin particles are obtained by reacting the surface of the resin particles with a silane coupling agent and coating the surface with metal. By using the silane coupling agent, the dispersion of the resin component is stabilized, and uniform metal-coated resin particles can be formed.
  • the photosensitive conductive paste may further contain glass frit.
  • the glass frit preferably has a volume average particle size of 0.1 to 1.4 ⁇ m, a 90% particle size of 1 to 2 ⁇ m, and a top size of 4.5 ⁇ m or less.
  • the composition of the glass frit is not particularly limited, but Bi 2 O 3 is preferably blended in the range of 30 wt% to 70 wt% with respect to the whole.
  • Examples of the oxide that may be contained in addition to Bi 2 O 3 may include SiO 2 , B 2 O 3 , ZrO 2 , and Al 2 O 3 .
  • Na 2 O, K 2 O, and Li 2 O are preferably alkali-free glass frit that is substantially free of them.
  • the photosensitive organic component preferably contains a photosensitive polymer and / or a photosensitive monomer.
  • Photosensitive polymers include polymers of components selected from compounds having carbon-carbon double bonds such as methyl (meth) acrylate and ethyl (meth) acrylate, and side chains or molecules of acrylic resins comprising these copolymers. Those having a photoreactive group added to the terminal are preferably used.
  • Preferred photoreactive groups include ethylenically unsaturated groups such as vinyl, allyl, acrylic and methacrylic groups.
  • the content of the photosensitive polymer is preferably 1 to 30% by weight and 2 to 30% by weight.
  • photosensitive monomer examples include (meth) acrylate monomers such as methacryl acrylate and ethyl acrylate, ⁇ -methacryloxypropyltrimethoxysilane, and 1-vinyl-2-pyrrolidone. can do.
  • the photosensitive organic component is preferably contained in an amount of 5 to 40% by weight with respect to 100 parts by weight of the metal powder in terms of light sensitivity, and more preferably 10 to 30 parts by weight.
  • the photosensitive conductive paste of the present invention preferably uses a photopolymerization initiator, a sensitizer, a polymerization inhibitor, and an organic solvent as necessary.
  • the thickness of the metal layer is not particularly limited.
  • the thickness of the metal layer is appropriately set so that the formed pattern wiring has a desired resistance value. Therefore, the thickness of the metal layer is preferably 0.01 to 200 ⁇ m, and more preferably 0.05 to 100 ⁇ m.
  • the resistance of the pattern wiring does not become too high, and the power consumption of the device does not increase.
  • the production efficiency of the metal layer is increased, the integrated heat amount during the film formation is reduced, and the film is less likely to be thermally wrinkled.
  • the transparent conductive film is a transparent conductive film for a touch panel used in combination with a display
  • the portion corresponding to the display portion is formed by a patterned transparent conductive film, and a metal wiring made from a photosensitive conductive paste Is used for the wiring part of the non-display part (for example, peripheral part).
  • the transparent conductive film may be used even in a non-display portion, and in that case, metal wiring may be formed on the transparent conductive film.
  • the carrier film has an adhesive layer on one surface side of the protective film.
  • the carrier film forms a transparent conductive film laminate by laminating the transparent conductive film that can be peeled off through the adhesive layer and the surface side on which the second cured resin layer of the transparent conductive film is formed. To do.
  • an adhesive layer may be peeled with a protective film, and only a protective film may be peeled.
  • the protective film is peeled off and discarded when laminated with other films such as a wave plate and a polarizing plate.
  • the material for forming the protective film is An amorphous resin is preferred.
  • the amorphous resin is not particularly limited, but is preferably excellent in transparency, mechanical strength, thermal stability, moisture barrier property, isotropy, and the like.
  • the glass transition temperature of the amorphous resin forming the protective film is preferably 130 ° C. or higher, and more preferably 140 ° C. or higher.
  • the protective film is subjected to an etching process such as sputtering, corona discharge, flame, ultraviolet irradiation, electron beam irradiation, chemical conversion, oxidation, and undercoating on the surface, and a pressure-sensitive adhesive layer on the protective film, etc. You may make it improve adhesiveness.
  • the surface of the protective film may be removed and cleaned by solvent cleaning or ultrasonic cleaning as necessary.
  • the protective film of the present invention is preferably produced by melt extrusion molding, and particularly preferably made of melt-extruded polycarbonate resin or melt-extruded cycloolefin resin. Thereby, it is easy to emboss after melt extrusion molding, and embossing can be performed efficiently.
  • a method of supplying a polycarbonate resin or the like to one extruder connected to a T die, melt-kneading, extruding, taking out by cooling with water, and forming a protective film can be exemplified.
  • the screw type of the extruder used for melting may be uniaxial or biaxial, and additives such as a plasticizer or an antioxidant optimal for the resin may be added.
  • the molding temperature can be appropriately set, but when the glass transition temperature of the resin is Tg (° C.), (Tg + 80) ° C. to (Tg + 150) ° C. is preferable, and (Tg + 100) ° C. to (Tg + 130) ° C. is more preferable. If the molding temperature is too low, the resin does not have fluidity and may not be molded. If the molding temperature is too high, the resin viscosity will be low, and there may be a problem in production stability such as uneven thickness of the molded product. In the case of a multilayer molded product, it is preferable to set a resin having a higher glass transition temperature.
  • the thickness of the protective film is preferably 20 to 150 ⁇ m, more preferably 30 to 100 ⁇ m, still more preferably 40 to 80 ⁇ m. Moreover, it is preferable that the thickness of a protective film is more than the thickness of a transparent resin film from a viewpoint of preventing the fracture
  • the arithmetic average surface roughness Ra of the surface of the protective film not having the pressure-sensitive adhesive layer is preferably 0.01 ⁇ m or more, more preferably 0.01 to 5 ⁇ m, and more preferably 0.05 to 2 ⁇ m. Is more preferable, and 0.1 to 1 ⁇ m is particularly preferable. When it is in the above range, anti-blocking properties can be imparted, and conveyance by a roll-to-roll manufacturing method is facilitated, and subsequent process yields can be ensured.
  • the pressure-sensitive adhesive layer can be used without particular limitation as long as it has transparency. Specifically, for example, acrylic polymers, silicone polymers, polyesters, polyurethanes, polyamides, polyvinyl ethers, vinyl acetate / vinyl chloride copolymers, modified polyolefins, epoxy systems, fluorine systems, natural rubbers, rubbers such as synthetic rubbers, etc. Those having the above polymer as a base polymer can be appropriately selected and used.
  • an acrylic pressure-sensitive adhesive is preferably used from the viewpoint that it is excellent in optical transparency, exhibits adhesive properties such as appropriate wettability, cohesiveness and adhesiveness, and is excellent in weather resistance and heat resistance.
  • the method for forming the pressure-sensitive adhesive layer is not particularly limited.
  • the pressure-sensitive adhesive composition is applied to a release liner, dried and then transferred to a base film (transfer method), and the pressure-sensitive adhesive composition is directly applied to a protective film. And a drying method (direct copying method) and a co-extrusion method.
  • a tackifier, a plasticizer, a filler, an antioxidant, an ultraviolet absorber, a silane coupling agent, and the like can be appropriately used as the pressure-sensitive adhesive.
  • the preferable thickness of the pressure-sensitive adhesive layer is 5 ⁇ m to 100 ⁇ m, more preferably 10 ⁇ m to 50 ⁇ m, and more preferably 15 ⁇ m to 35 ⁇ m.
  • a transparent conductive film laminated body contains the carrier film which has an adhesive layer on the one surface side of a protective film, and the transparent conductive film laminated
  • the carrier film is laminated
  • the transparent conductive film laminate does not break. Thereby, it is possible to prevent the transparent resin film from being scratched, and even when a tension is applied during transportation of the transparent conductive film laminate, the transparent conductive film laminate does not break, and the subsequent process yield can be secured.
  • “rupture of the transparent conductive film laminate” means a state where at least a part of the transparent conductive film laminate is cut over the entire thickness direction.
  • the transparent conductive film which peeled the carrier film or the protective film from the transparent conductive film laminated body can be suitably applied as a transparent electrode of an electronic device such as a touch panel such as a capacitance method or a resistance film method.
  • another base material such as glass or a polymer film can be bonded to one or both main surfaces of the transparent conductive film described above via a transparent adhesive layer.
  • a transparent adhesive layer For example, you may form the laminated body by which the transparent base
  • the transparent substrate may be composed of a single substrate film or may be a laminate of two or more substrate films (for example, laminated via a transparent adhesive layer).
  • a hard coat layer can also be provided on the outer surface of the transparent substrate to be bonded to the transparent conductive film.
  • the pressure-sensitive adhesive layer used for bonding the transparent conductive film and the substrate can be used without particular limitation as long as it has transparency.
  • the amount and direction of curling after a heating process such as drying can be controlled, which facilitates transport of the transparent conductive film laminate and handling during touch panel formation. Excellent in properties. Therefore, a touch panel excellent in transparency and visibility can be manufactured with high productivity. If it is other than a touch panel use, it can be used for the shield use which shields the electromagnetic waves and noise which are emitted from an electronic device.
  • Example 1 (Preparation of curable resin composition containing spherical particles) Acrylic spherical particles (trade name “MX-180TA” manufactured by Soken Chemical Co., Ltd.) having 100 parts by weight of an ultraviolet curable resin composition (trade name “OPSTA-Z7540” manufactured by JSR) and a mode particle diameter of 1.9 ⁇ m. ) Containing 0.2 parts by weight of a curable resin composition containing spherical particles.
  • Acrylic spherical particles (trade name “MX-180TA” manufactured by Soken Chemical Co., Ltd.) having 100 parts by weight of an ultraviolet curable resin composition (trade name “OPSTA-Z7540” manufactured by JSR) and a mode particle diameter of 1.9 ⁇ m. ) Containing 0.2 parts by weight of a curable resin composition containing spherical particles.
  • the prepared curable resin composition containing spherical particles was subjected to corona treatment on one surface of a polycycloolefin film (trade name “ZEONOR (registered trademark)” manufactured by Nippon Zeon Co., Ltd.) having a thickness of 35 ⁇ m and a glass transition temperature of 165 ° C. After coating, a coating layer was formed. Subsequently, the coating layer was irradiated with ultraviolet rays from the side on which the coating layer was formed, and a second cured resin layer was formed so as to have a thickness of 2.0 ⁇ m. A first cured resin layer was formed on the other surface of the polycycloolefin film by the same method except that spherical particles were not added, so that the thickness was 2.0 ⁇ m.
  • a zirconia particle-containing ultraviolet curable composition having a refractive index of 1.62 as an optical adjustment layer on the first cured resin layer side of the polycycloolefin film having cured resin layers formed on both sides (trade name “OPSTA Z7412 manufactured by JSR Corporation”). was applied to form a coating layer. Then, the coating layer was irradiated with ultraviolet rays from the side where the coating layer was formed, and an optical adjustment layer was formed so that the thickness was 100 nm.
  • the polycycloolefin film on which the optical adjustment layer is formed is put into a take-up sputtering apparatus, and an amorphous indium tin oxide layer (composition: SnO) having a thickness of 27 nm is formed on the surface of the optical adjustment layer. 2 10 wt%).
  • SnO amorphous indium tin oxide layer
  • An acrylic pressure-sensitive adhesive was prepared by adding 6 parts by weight of an epoxy-based crosslinking agent (trade name “Tetrad C (registered trademark)” manufactured by Mitsubishi Gas Chemical) to 100 parts by weight of the acrylic polymer.
  • the acrylic pressure-sensitive adhesive obtained as described above was applied onto the release-treated surface of the release-treated PET film, and heated at 120 ° C. for 60 seconds to form a pressure-sensitive adhesive layer having a thickness of 20 ⁇ m.
  • a PET film is adhered to the surface of the unembossed side of a single layer polycarbonate resin film (trade name “OPCON PC” manufactured by Keiwa) with a thickness of 75 ⁇ m, a glass transition temperature of 145 ° C., and embossed on one side. It bonded together through the agent layer. Thereafter, the release-treated PET film was peeled off to prepare a carrier film having an adhesive layer on one surface of the protective film.
  • OPCON PC manufactured by Keiwa
  • Example 2 a transparent conductive film was prepared in the same manner as in Example 1, except that a polycycloolefin film having a thickness of 50 ⁇ m (trade name “ZEONOR (registered trademark)” manufactured by Nippon Zeon Co., Ltd.) was used as the transparent resin film. A film laminate was prepared.
  • Example 3 In Example 1, a transparent conductive film was prepared in the same manner as in Example 1 except that a polycycloolefin film having a thickness of 75 ⁇ m (trade name “ZEONOR (registered trademark)” manufactured by Nippon Zeon Co., Ltd.) was used as the transparent resin film. A film laminate was prepared.
  • a polycycloolefin film having a thickness of 75 ⁇ m trade name “ZEONOR (registered trademark)” manufactured by Nippon Zeon Co., Ltd.
  • Example 4 In Example 1, as the transparent resin film, Example 1 except that a polycycloolefin film having a thickness of 50 ⁇ m and a glass transition temperature of 136 ° C. (trade name “ZEONOR (registered trademark)” manufactured by Nippon Zeon Co., Ltd.) was used. A transparent conductive film laminate was produced in the same manner.
  • a polycycloolefin film having a thickness of 50 ⁇ m and a glass transition temperature of 136 ° C. trade name “ZEONOR (registered trademark)” manufactured by Nippon Zeon Co., Ltd.
  • Example 5 In Example 1, a transparent conductive film was prepared in the same manner as in Example 1 except that a polycarbonate resin having a thickness of 75 ⁇ m and a glass transition temperature of 141 ° C. (trade name “Panlite” manufactured by Teijin) was used as the transparent resin film. A conductive film laminate was produced.
  • a polycarbonate resin having a thickness of 75 ⁇ m and a glass transition temperature of 141 ° C. (trade name “Panlite” manufactured by Teijin) was used as the transparent resin film.
  • a conductive film laminate was produced.
  • Example 6 In Example 1, as a protective film, a single-layer polycycloolefin film having a thickness of 50 ⁇ m and a glass transition temperature of 165 ° C. embossed on one side (trade name “ZEONOR (registered trademark) (ZF16)” manufactured by ZEON) A transparent conductive film laminate was produced in the same manner as in Example 1 except that was used.
  • ZEONOR registered trademark
  • Example 1 a transparent conductive film laminate was produced in the same manner as in Example 1 except that the following protective film was used instead of the embossed protective film.
  • a protective film that has not been embossed a surface of the protective film on which the adhesive layer is not formed using a polycarbonate resin film having a thickness of 75 ⁇ m and a glass transition temperature of 145 ° C. (trade name “OPCON” manufactured by Keiwa)
  • the curable resin composition containing spherical particles prepared as described above was applied to form a coating layer.
  • the coating layer was irradiated with ultraviolet rays from the side on which the coating layer was formed, and a protective film having an anti-blocking layer formed on the protective film so as to have a thickness of 2.0 ⁇ m was produced.
  • Example 5 In Example 5, the following protective film was used instead of the embossed protective film, and a polycarbonate resin having a glass transition temperature of 145 ° C. (trade name “Panlite” manufactured by Teijin) was used as the transparent resin film. Except for this, a transparent conductive film laminate was produced in the same manner as in Example 5. That is, as an unembossed protective film, a polycycloolefin film having a thickness of 75 ⁇ m and a glass transition temperature of 165 ° C. (trade name “ZEONOR (registered trademark)” manufactured by Nippon Zeon Co., Ltd.) is used.
  • ZEONOR registered trademark
  • the spherical particle-containing curable resin composition prepared as described above was applied to form a coating layer. Subsequently, the coating layer was irradiated with ultraviolet rays from the side on which the coating layer was formed, and a protective film having an anti-blocking layer formed on the protective film so as to have a thickness of 2.0 ⁇ m was produced.
  • the transparent conductive film laminates of Examples 1 to 6 does not break in the 180 ° bending test, and the roll does not break the transparent conductive film laminate when used in an actual machine. It could be transported by the to-roll manufacturing method.
  • the transparent conductive film laminates of Comparative Examples 1 and 2 were broken in the 180 ° bending test of the transparent conductive film laminates and could not be transported by the actual machine. As for the occurrence of breakage in the actual machine test, it is estimated that film wrinkles occur after passing through the heating roll, local bending occurs in the film, and breakage occurs.

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