WO2021187575A1 - 光透過性導電膜および透明導電性フィルム - Google Patents

光透過性導電膜および透明導電性フィルム Download PDF

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Publication number
WO2021187575A1
WO2021187575A1 PCT/JP2021/011150 JP2021011150W WO2021187575A1 WO 2021187575 A1 WO2021187575 A1 WO 2021187575A1 JP 2021011150 W JP2021011150 W JP 2021011150W WO 2021187575 A1 WO2021187575 A1 WO 2021187575A1
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Prior art keywords
conductive film
light
film
transmitting conductive
less
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PCT/JP2021/011150
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English (en)
French (fr)
Japanese (ja)
Inventor
望 藤野
泰介 鴉田
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Nitto Denko Corp
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Nitto Denko Corp
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Priority to KR1020227030808A priority Critical patent/KR20220155285A/ko
Priority to JP2021550146A priority patent/JP7565936B2/ja
Priority to CN202180021855.0A priority patent/CN115298757A/zh
Publication of WO2021187575A1 publication Critical patent/WO2021187575A1/ja
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/023—Optical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/025—Electric or magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5873—Removal of material
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1343—Electrodes
    • G—PHYSICS
    • G06—COMPUTING OR CALCULATING; 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
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • 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
    • 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
    • H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01Q—ANTENNAS, i.e. RADIO AERIALS
    • H01Q1/00—Details of, or arrangements associated with, antennas
    • H01Q1/36—Structural form of radiating elements, e.g. cone, spiral, umbrella; Particular materials used therewith
    • H01Q1/38—Structural form of radiating elements, e.g. cone, spiral, umbrella; Particular materials used therewith formed by a conductive layer on an insulating support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01Q—ANTENNAS, i.e. RADIO AERIALS
    • H01Q1/00—Details of, or arrangements associated with, antennas
    • H01Q1/52—Means for reducing coupling between antennas; Means for reducing coupling between an antenna and another structure
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/20—Electrodes

Definitions

  • the present invention relates to a light-transmitting conductive film and a transparent conductive film.
  • Transparent electrodes in various devices are formed of a film (light-transmitting conductive film) having both light transmission and conductivity.
  • the light-transmitting conductive film may be used as an antistatic layer included in the device.
  • the light-transmitting conductive film is formed, for example, by forming a conductive oxide on a transparent substrate by a sputtering method. In the sputtering method, an inert gas such as argon is used as the sputtering gas for colliding with the target (film-forming material supply material) and ejecting atoms on the target surface.
  • a technique relating to such a light-transmitting conductive film is described in, for example, Patent Document 1 below.
  • the light transmissive conductive film is required to have low resistance.
  • the light-transmitting conductive film is required to have a small internal stress in the film and to be less likely to warp.
  • the present invention provides an amorphous light-transmitting conductive film suitable for obtaining a low-resistance crystalline light-transmitting conductive film in which warpage is suppressed, and a transparent conductive film provided with the light-transmitting conductive film. offer.
  • the present invention [1] is an amorphous light-transmitting conductive film, which contains a conductive oxide containing krypton and has a specific resistance of 4 ⁇ 10 -4 ⁇ ⁇ cm or more. Includes membrane.
  • the present invention [2] includes the light transmissive conductive film according to the above [1], wherein the specific resistance is 20 ⁇ 10 -4 ⁇ ⁇ cm or less.
  • the present invention [3] includes the light-transmitting conductive film according to the above [1] or [2], which has a thickness of more than 40 nm.
  • the present invention [4] includes the light-transmitting conductive film according to any one of the above [1] to [3], which is patterned.
  • the present invention [6] comprises a transparent base material and the light transmissive conductive film according to any one of the above [1] to [5], which is arranged on one side in the thickness direction of the transparent base material.
  • a transparent conductive film comprising.
  • the light-transmitting conductive film of the present invention is amorphous, contains a conductive oxide containing krypton, and has a specific resistance of 4 ⁇ 10 -4 ⁇ ⁇ cm or more, so that warpage is suppressed and is low. Suitable for obtaining a crystalline light-transmitting conductive film of resistance. Since the transparent conductive film of the present invention includes such a light-transmitting conductive film, it is suitable for obtaining a transparent conductive film having a low-resistance crystalline light-transmitting conductive film and suppressed warpage.
  • FIG. 3A shows a step of preparing a transparent resin film
  • FIG. 3B shows a step of forming a functional layer on the transparent resin film
  • FIG. 3C shows a step of forming a light transmissive conductive film on the functional layer. show.
  • the case where the light-transmitting conductive film is patterned in the transparent conductive film shown in FIG. 1 is shown.
  • the transparent conductive film shown in FIG. 1 shows the transparent conductive film shown in FIG.
  • FIG. 1 is a schematic cross-sectional view of the transparent conductive film X, which is an embodiment of the transparent conductive film of the present invention.
  • the transparent conductive film X includes a transparent base material 10 and a light-transmitting conductive film 20 in this order toward one side in the thickness direction D.
  • the transparent conductive film X, the transparent base material 10, and the light-transmitting conductive film 20 each have a shape that spreads in a direction (plane direction) orthogonal to the thickness direction D.
  • the transmissive conductive film X and the light transmissive conductive film 20 included therein are provided in a touch sensor, a dimming element, a photoelectric conversion element, a heat ray control member, an antenna member, an electromagnetic wave shield member, a heater member, an image display device, and the like. It is one element to be.
  • the transparent base material 10 includes a transparent resin film 11 and a functional layer 12 in this order toward one side in the thickness direction D.
  • the transparent resin film 11 is a transparent resin film having flexibility.
  • the material of the transparent resin film 11 include polyester resin, polyolefin resin, acrylic resin, polycarbonate resin, polyether sulfone resin, polyarylate resin, melamine resin, polyamide resin, polyimide resin, cellulose resin, and polystyrene resin. ..
  • the polyester resin include polyethylene terephthalate (PET), polybutylene terephthalate, and polyethylene naphthalate.
  • PET polyethylene terephthalate
  • Polyolefin resins include, for example, polyethylene, polypropylene, and cycloolefin polymers.
  • the acrylic resin include polymethacrylate.
  • polyester resin is preferably used, and PET is more preferably used.
  • the surface of the transparent resin film 11 on the functional layer 12 side may be surface-modified.
  • Examples of the surface modification treatment include corona treatment, plasma treatment, ozone treatment, primer treatment, glow treatment, and coupling agent treatment.
  • the thickness of the transparent resin film 11 is preferably 1 ⁇ m or more, more preferably 10 ⁇ m or more, and further preferably 30 ⁇ m or more.
  • the thickness of the transparent resin film 11 is preferably 300 ⁇ m or less, more preferably 200 ⁇ m or less, still more preferably 100 ⁇ m or less, and particularly preferably 75 ⁇ m or less.
  • the total light transmittance (JIS K 7375-2008) of the transparent resin film 11 is preferably 60% or more, more preferably 80% or more, still more preferably 85% or more.
  • Such a configuration is such that when the transparent conductive film X is provided in a touch sensor, a dimming element, a photoelectric conversion element, a heat ray control member, an antenna member, an electromagnetic wave shielding member, a heater member, an image display device, or the like, the transparent conductive film X is provided. It is suitable for ensuring the transparency required for the sex film X.
  • the total light transmittance of the transparent resin film 11 is, for example, 100% or less.
  • the functional layer 12 is located on one surface of the thickness direction D of the transparent resin film 11. Further, in the present embodiment, the functional layer 12 is a hard coat layer for preventing scratches from being formed on the exposed surface (upper surface in FIG. 1) of the light transmissive conductive film 20.
  • the hard coat layer is a cured product of a curable resin composition.
  • the resin contained in the curable resin composition include polyester resin, acrylic resin, urethane resin, amide resin, silicone resin, epoxy resin, and melamine resin.
  • the curable resin composition include an ultraviolet curable resin composition and a thermosetting resin composition.
  • an ultraviolet curable resin composition is preferably used from the viewpoint of helping to improve the production efficiency of the transparent conductive film X because it can be cured without heating at a high temperature.
  • Specific examples of the ultraviolet curable resin composition include the composition for forming a hard coat layer described in JP-A-2016-179686.
  • the surface of the functional layer 12 on the side of the light-transmitting conductive film 20 may be surface-modified.
  • the surface modification treatment include corona treatment, plasma treatment, ozone treatment, primer treatment, glow treatment, and coupling agent treatment.
  • the thickness of the functional layer 12 as the hard coat layer is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more. Such a configuration is suitable for exhibiting sufficient scratch resistance in the light transmissive conductive film 20.
  • the thickness of the functional layer 12 as the hard coat layer is preferably 10 ⁇ m or less, more preferably 5 ⁇ m or less, from the viewpoint of ensuring the transparency of the functional layer 12.
  • the thickness of the transparent base material 10 is preferably 1 ⁇ m or more, more preferably 10 ⁇ m or more, still more preferably 15 ⁇ m or more, and particularly preferably 30 ⁇ m or more.
  • the thickness of the transparent base material 10 is preferably 310 ⁇ m or less, more preferably 210 ⁇ m or less, still more preferably 110 ⁇ m or less, and particularly preferably 80 ⁇ m or less.
  • the total light transmittance (JIS K 7375-2008) of the transparent base material 10 is preferably 60% or more, more preferably 80% or more, still more preferably 85% or more.
  • Such a configuration is such that when the transparent conductive film X is provided in a touch sensor, a dimming element, a photoelectric conversion element, a heat ray control member, an antenna member, an electromagnetic wave shielding member, a heater member, an image display device, or the like, the transparent conductive film X is provided. It is suitable for ensuring the transparency required for the sex film X.
  • the total light transmittance of the transparent base material 10 is, for example, 100% or less.
  • the heat shrinkage rate of the transparent base material 10 in the direction in which the transparent base material 10 shrinks most when it undergoes heat treatment is, for example, 1% or less, preferably 1% or less, from the viewpoint of suppressing warpage of the light transmissive conductive film 20. Is 0.6% or less, more preferably 0.5% or less.
  • the heat shrinkage rate is, for example, 0.0% or more.
  • the heat shrinkage rate can be obtained by measuring the dimensional change of the transparent base material 10 after sequentially performing a heat treatment and allowing the transparent base material 10 to stand at room temperature for 30 minutes.
  • the heating temperature in the heat treatment is the same as the temperature at which the light transmissive conductive film 20 is crystallized, for example, 165 ° C.
  • the heating time in the heat treatment is, for example, 1 hour.
  • the light transmissive conductive film 20 is located on one surface of the thickness direction D of the transparent base material 10.
  • the light-transmitting conductive film 20 is an embodiment of the light-transmitting conductive film of the present invention, and is an amorphous film having both light-transmitting property and conductivity.
  • the amorphous light-transmitting conductive film 20 is converted into a crystalline light-transmitting conductive film (the light-transmitting conductive film 20'described later) by heating, and the specific resistance is lowered.
  • the light transmissive conductive film 20 contains a conductive oxide containing at least krypton (Kr) as a rare gas atom, and preferably comprises a conductive oxide containing at least Kr as a rare gas atom.
  • the rare gas atom in the light transmissive conductive film 20 is derived from the rare gas atom used as the sputtering gas in the sputtering method described later for forming the light transmissive conductive film 20.
  • the light-transmitting conductive film 20 is a film (sputtered film) formed by a sputtering method.
  • the conductive oxide for example, at least one kind of metal selected from the group consisting of In, Sn, Zn, Ga, Sb, Ti, Si, Zr, Mg, Al, Au, Ag, Cu, Pd and W.
  • a metal oxide containing a semi-metal can be mentioned.
  • the conductive oxides include indium tin oxide composite oxide (ITO), indium zinc composite oxide (IZO), indium gallium composite oxide (IGO), indium gallium zinc composite oxide (IGZO), and Antimonthin composite oxide (ATO) can be mentioned.
  • ITO indium tin oxide composite oxide
  • ITO indium tin oxide composite oxide
  • the ITO may contain a metal or a semimetal other than In and Sn in an amount less than the respective contents of In and Sn.
  • the ratio of the tin oxide content to the total content of indium (In 2 O 3 ) and tin oxide (SnO 2) in the ITO is preferably 0.1% by mass. As mentioned above, it is more preferably 3% by mass or more, further preferably 5% by mass or more, and particularly preferably 7% by mass or more.
  • the ratio of the number of tin atoms to the number of indium atoms (number of tin atoms / number of indium atoms) in the ITO used is preferably 0.001 or more, more preferably 0.03 or more, still more preferably 0.05 or more, and particularly preferably 0.05 or more. It is 0.07 or more.
  • the ratio of the tin oxide content to the total content of indium oxide (In 2 O 3 ) and tin oxide (SnO 2 ) in the ITO used is preferably 15% by mass or less, more preferably 13% by mass or less. More preferably, it is 12% by mass or less.
  • the ratio of the number of tin atoms to the number of indium atoms in the ITO used is preferably 0.16 or less, more preferably 0.14 or less, still more preferably 0.13 or less.
  • the ratio of the number of tin atoms to the number of indium atoms in ITO can be obtained, for example, by specifying the abundance ratio of indium atoms and tin atoms in the object to be measured by X-ray Photoelectron Spectroscopy.
  • the above-mentioned content ratio of tin oxide in ITO is obtained from, for example, the abundance ratio of the indium atom and the tin atom thus specified.
  • the above-mentioned content ratio of tin oxide in ITO may be judged from the tin oxide (SnO 2) content ratio of the ITO target used at the time of sputtering film formation.
  • the light-transmitting conductive film 20 has a Kr content of preferably 1.0 atomic% or less, more preferably 0.7 atomic% or less, still more preferably 0.5 atomic% or less, and even more preferably 0.3.
  • the Kr content ratio of the region is, for example, 0.0001 atomic% or more.
  • the light transmissive conductive film 20 satisfies such a Kr content ratio in the entire area in the thickness direction D.
  • the content ratio of Kr in the light transmissive conductive film 20 is preferably 1.0 atomic% or less, more preferably 0.7 atomic% or less, and further preferably 0. It is 5 atomic% or less, more preferably 0.3 atomic% or less, very preferably 0.2 atomic% or less, and particularly preferably less than 0.1 atomic%.
  • These configurations are suitable for achieving good crystal growth and forming large crystal grains when heated to crystallize the light transmissive conductive film 20, thus providing a low resistance light transmissive conductive film 20'. Suitable for obtaining (the larger the crystal grains in the crystalline light-transmitting conductive film 20', the lower the resistance of the light-transmitting conductive film 20').
  • the presence or absence and content of rare gas atoms such as Kr in the light transmissive conductive film 20 are identified by, for example, Rutherford Backscattering Spectrometry, which will be described later with respect to Examples.
  • the presence or absence of rare gas atoms such as Kr in the light transmissive conductive film 20 is identified by, for example, fluorescent X-ray analysis described later with respect to Examples.
  • the noble gas atom content cannot be quantified because it is not above the detection limit (lower limit), and according to fluorescent X-ray analysis, the presence of noble gas atoms.
  • it is determined that the light-transmitting conductive film contains a region in which the content ratio of rare gas atoms such as Kr is 0.0001 atomic% or more.
  • the light transmissive conductive film 20 may contain a rare gas atom other than Kr.
  • the noble gas atom other than Kr include argon (Ar), xenon (Xe), and radon (Rn), and from the viewpoint of suppressing the production cost of the light-transmitting conductive film 20 and the transparent conductive film X, examples thereof.
  • Ar is used.
  • the content ratio of the rare gas atom in the light transmissive conductive film 20 (for example, the total content ratio of Kr and Ar) is thick.
  • the entire direction D preferably 1.2 atomic% or less, more preferably 1.1 atomic% or less, still more preferably 1.0 atomic% or less, even more preferably 0.8 atomic% or less, still more preferably. It is 0.5 atomic% or less, more preferably 0.4 atomic% or less, very preferably 0.3 atomic% or less, and particularly preferably 0.2 atomic% or less.
  • Such a configuration is suitable for reducing the scattering of impurities of carriers in the light transmissive conductive film 20 because the content of rare gas atoms (impurity atoms) is small, and therefore the light transmissive conductive film 20 having low resistance. 'Suitable for getting.
  • the light transmissive conductive film 20 may contain Kr over the entire area in the thickness direction D.
  • the light transmissive conductive film 20 may contain only Kr as a rare gas atom over the entire area in the thickness direction D, or may contain a rare gas atom other than Kr in addition to Kr.
  • the light transmissive conductive film 20 may contain Kr in a part of the thickness direction D.
  • FIG. 2A shows a case where the light transmissive conductive film 20 includes the first region 21 and the second region 22 in this order toward one side in the thickness direction D.
  • the first region 21 contains Kr and the second region 22 does not contain Kr.
  • FIG. 2B shows a case where the light transmissive conductive film 20 includes the second region 22 and the first region 21 in this order toward one side in the thickness direction D.
  • FIG. 2C shows a case where the light transmissive conductive film 20 includes the first region 21, the second region 22, and the first region 21 in this order toward one side in the thickness direction D.
  • FIG. 2D shows a case where the light transmissive conductive film 20 includes the second region 22, the first region 21, and the second region 22 in this order toward one side in the thickness direction D.
  • the boundary between the first region 21 and the second region 22 is drawn by a virtual line, the first region 21 and the second region 22 have a composition other than the rare gas atom whose content is very small. When they are not significantly different, the boundary between the first region 21 and the second region 22 may not be clearly discriminated.
  • the ratio of the total thickness of the plurality of first regions 21) is preferably 1% or more, more preferably 20% or more, still more preferably more than 50%, still more preferably 60% or more, and particularly preferably 64%. That is all. The same ratio is less than 100%. Further, the ratio of the thickness of the second region 22 to the total thickness of the first region 21 and the second region 22 (in the plurality of second regions 22, the total thickness of the plurality of second regions 22) is preferably.
  • the configuration relating to the respective thickness ratios of the first region 21 and the second region 22 is suitable for forming the low resistance light transmissive conductive film 20'from the light transmissive conductive film 20.
  • the content ratio of Kr in the first region 21 is preferably 1.0 atomic% or less, more preferably 0.7 atomic% or less, still more preferably 0. It is 5 atomic% or less, more preferably 0.3 atomic% or less, more preferably 0.2 atomic% or less, and particularly preferably less than 0.1 atomic%.
  • Such a configuration is suitable for achieving good crystal growth and forming large crystal grains when heated for crystallization of the light transmissive conductive film 20, and therefore the light transmissive conductive film 20 having low resistance. (The larger the crystal grains in the crystalline light-transmitting conductive film 20', the lower the resistance of the light-transmitting conductive film 20').
  • the content ratio of Kr in the first region 21 is, for example, 0.0001 atomic% or more in the entire area of the thickness direction D of the first region 21.
  • the content ratio of Kr in the first region 21 may be non-uniform in the thickness direction D of the first region 21.
  • the Kr content ratio may gradually increase or decrease as the distance from the transparent base material 10 increases.
  • the partial region in which the Kr content ratio gradually increases as the distance from the transparent base material 10 increases is located on the transparent base material 10 side, and the Kr content ratio increases as the distance from the transparent base material 10 increases.
  • the partial region where is gradually reduced may be located on the opposite side of the transparent base material 10.
  • the partial region in which the Kr content ratio gradually decreases as the distance from the transparent base material 10 increases is located on the transparent base material 10 side, and the Kr content ratio increases as the distance from the transparent base material 10 increases.
  • the partial region where is gradually increased may be located on the opposite side of the transparent base material 10.
  • the thickness of the light transmissive conductive film 20 is, for example, 10 nm or more.
  • the thickness of the light-transmitting conductive film 20 is preferably more than 40 nm, more preferably 70 nm or more, still more preferably 100 nm or more, and particularly preferably 130 nm or more.
  • Such a configuration is suitable for reducing the resistance of the light-transmitting conductive film 20'obtained by crystallizing the light-transmitting conductive film 20.
  • the thickness of the light-transmitting conductive film 20 is preferably 1000 nm or less, more preferably 250 nm or less, still more preferably 200 nm or less, particularly preferably 160 nm or less, and most preferably less than 150 nm.
  • Such a configuration is suitable for suppressing warpage in the transparent conductive film X provided with the light-transmitting conductive film 20'obtained by crystallizing the light-transmitting conductive film 20.
  • the surface resistance of the light transmissive conductive film 20 is, for example, 500 ⁇ / ⁇ or less, preferably 200 ⁇ / ⁇ or less, more preferably 100 ⁇ / ⁇ or less, and further preferably 80 ⁇ / ⁇ or less.
  • the surface resistance of the light transmissive conductive film 20 is, for example, 1 ⁇ / ⁇ or more.
  • the surface resistance can be measured by the 4-terminal method based on JIS K7194.
  • the specific resistance of the light transmissive conductive film 20 is 4 ⁇ 10 -4 ⁇ ⁇ cm or more, preferably 4.3 ⁇ 10 -4 ⁇ ⁇ cm or more, and more preferably 4.5 ⁇ 10 -4 ⁇ ⁇ cm.
  • the above is more preferably 4.8 ⁇ 10 -4 ⁇ ⁇ cm or more, further preferably 5 ⁇ 10 -4 ⁇ ⁇ cm or more, and particularly preferably 5.2 ⁇ 10 -4 ⁇ ⁇ cm or more.
  • the specific resistance of the light transmissive conductive film 20 is preferably 20 ⁇ 10 -4 ⁇ ⁇ cm or less, more preferably 12 ⁇ 10 -4 ⁇ ⁇ cm or less, still more preferably 11 ⁇ 10 -4 ⁇ ⁇ cm or less, particularly.
  • Such a configuration with respect to specific resistance is suitable for forming a low-resistance light-transmitting conductive film 20'from the light-transmitting conductive film 20.
  • the specific resistance is obtained by multiplying the surface resistance by the thickness.
  • the resistivity can be controlled by, for example, adjusting the Kr content ratio in the light transmissive conductive film 20 and adjusting various conditions when the light transmissive conductive film 20 is sputter-deposited.
  • the conditions include, for example, the temperature of the substrate (transparent substrate 10 in this embodiment) on which the light transmissive conductive film 20 is formed, the amount of oxygen introduced into the film forming chamber, the pressure in the film forming chamber, and the target.
  • the above horizontal magnetic field strength can be mentioned.
  • the specific resistance of the light transmissive conductive film 20 after heat treatment at 165 ° C. for 1 hour is preferably 3 ⁇ 10 -4 ⁇ ⁇ cm or less, more preferably 2.8 ⁇ 10 -4 ⁇ ⁇ cm or less, and further. It is preferably 2.5 ⁇ 10 -4 ⁇ ⁇ cm or less, more preferably 2 ⁇ 10 -4 ⁇ ⁇ cm or less, and particularly preferably 1.8 ⁇ 10 -4 ⁇ ⁇ cm or less.
  • the specific resistance of the light-transmitting conductive film 20 after heat treatment at 165 ° C. for 1 hour is preferably 0.1 ⁇ 10 -4 ⁇ ⁇ cm or more, more preferably 0.5 ⁇ 10 -4 ⁇ ⁇ cm.
  • Such a configuration is obtained by crystallizing the light transmissive conductive film 20 in a touch sensor, a light control element, a photoelectric conversion element, a heat ray control member, an antenna member, an electromagnetic wave shield member, a heater member, an image display device, or the like.
  • the light-transmitting conductive film 20' is provided, it is suitable for ensuring the low resistance required for the light-transmitting conductive film 20'.
  • the total light transmittance (JIS K 7375-2008) of the light transmissive conductive film 20 is preferably 60% or more, more preferably 80% or more, still more preferably 85% or more. Such a configuration is suitable for ensuring transparency in the light-transmitting conductive film 20'obtained by crystallizing the light-transmitting conductive film 20. Further, the total light transmittance of the light transmissive conductive film 20 is, for example, 100% or less.
  • the light-transmitting conductive film is amorphous, for example, it can be determined as follows. First, the light-transmitting conductive film (in the case of the transparent conductive film X, the light-transmitting conductive film 20 on the transparent base material 10) is immersed in hydrochloric acid having a concentration of 5% by mass at 20 ° C. for 15 minutes. Next, the light-transmitting conductive film is washed with water and then dried. Next, in the exposed plane of the light-transmitting conductive film (in the transparent conductive film X, the surface of the light-transmitting conductive film 20 opposite to the transparent base material 10), the resistance between the pair of terminals having a separation distance of 15 mm. Measure (resistance between terminals). In this measurement, when the resistance between terminals exceeds 10 k ⁇ , the light transmitting conductive film is amorphous.
  • the transparent conductive film X is manufactured as follows, for example.
  • the transparent resin film 11 is prepared.
  • the functional layer 12 is formed on one surface of the transparent resin film 11 in the thickness direction D.
  • the transparent base material 10 is produced by forming the functional layer 12 on the transparent resin film 11.
  • the above-mentioned functional layer 12 as a hard coat layer can be formed by applying a curable resin composition on a transparent resin film 11 to form a coating film, and then curing the coating film.
  • the curable resin composition contains an ultraviolet-forming resin
  • the coating film is cured by ultraviolet irradiation.
  • the curable resin composition contains a thermosetting resin
  • the coating film is cured by heating.
  • the exposed surface of the functional layer 12 formed on the transparent resin film 11 is surface-modified, if necessary.
  • plasma treatment for example, argon gas is used as the inert gas.
  • the discharge power in the plasma processing is, for example, 10 W or more, and for example, 5000 W or less.
  • the light transmissive conductive film 20 is formed on the transparent base material 10. Specifically, a material is formed on the functional layer 12 of the transparent base material 10 by a sputtering method to form a light-transmitting conductive film 20.
  • the transparent base film 10 is run from the feeding roll to the winding roll provided in the apparatus while running the transparent base film 10.
  • a material is formed on the material 10 to form a light-transmitting conductive film 20.
  • a sputtering film forming apparatus provided with one film forming chamber may be used, or a sputtering film forming apparatus including a plurality of film forming chambers sequentially arranged along a traveling path of the transparent base material 10 may be used.
  • An apparatus may be used (when forming the light transmissive conductive film 20 including the above-mentioned second region 22, a sputtering film forming apparatus including a plurality of film forming chambers is used).
  • a sputtering gas in the sputtering method, specifically, while introducing a sputtering gas (inert gas) into the film forming chamber provided in the sputtering film forming apparatus under vacuum conditions, a negative voltage is applied to the target arranged on the cathode in the film forming chamber. Is applied. As a result, a glow discharge is generated to ionize gas atoms, the gas ions collide with the target surface at high speed, the target material is ejected from the target surface, and the ejected target material is placed on the functional layer 12 of the transparent base material 10. To deposit in.
  • a sputtering gas in the film forming chamber provided in the sputtering film forming apparatus under vacuum conditions
  • the above-mentioned conductive oxide for forming the light transmissive conductive film 20 is used, and ITO is preferably used.
  • the ratio of the tin oxide content to the total content of tin oxide and indium oxide in ITO is preferably 0.1% by mass or more, more preferably 1% by mass or more, still more preferably 3% by mass or more, still more preferably 5. It is mass% or more, particularly preferably 7% by mass or more, and preferably 15% by mass or less, more preferably 13% by mass or less, still more preferably 12% by mass or less.
  • the sputtering method is preferably a reactive sputtering method.
  • a reactive gas is introduced into the film forming chamber in addition to the sputtering gas.
  • the gas introduced into one or more film forming chambers provided in the sputtering film forming apparatus is , Kr as a sputtering gas and oxygen as a reactive gas.
  • the sputtering gas may contain an inert gas other than Kr.
  • the inert gas other than Kr include rare gas atoms other than Kr.
  • the noble gas atom include Ar, Xe, and Rn.
  • the content ratio is preferably 80% by volume or less, more preferably 50% by volume or less.
  • the gas introduced into the film forming chamber for forming the first region 21 is It contains Kr as a sputtering gas and oxygen as a reactive gas.
  • the sputtering gas may contain an inert gas other than Kr.
  • the type and content ratio of the inert gas other than Kr are the same as those described above for the inert gas other than Kr in the first case.
  • the gas introduced into the film forming chamber for forming the second region 22 contains an inert gas other than Kr as a sputtering gas and oxygen as a reactive gas.
  • the inert gas other than Kr include the above-mentioned inert gas as the inert gas other than Kr in the first case.
  • the ratio of the amount of oxygen introduced to the total amount of sputtering gas and oxygen introduced into the film forming chamber in the reactive sputtering method is, for example, 0.01 flow rate% or more, and for example, 15 flow rate% or less.
  • the air pressure in the film formation chamber during film formation (sputter film formation) by the sputtering method is, for example, 0.02 Pa or more, and for example, 1 Pa or less.
  • the temperature of the transparent substrate 10 during the sputtering film formation is, for example, 100 ° C. or lower. In order to suppress the thermal expansion of the transparent base material 10 during the sputter film formation, it is preferable to cool the transparent base material 10. Suppression of thermal expansion of the transparent substrate 10 during sputter film formation is useful for obtaining a low-resistance light-transmitting conductive film 20'(crystalline light-transmitting conductive film) in which warpage is suppressed.
  • the temperature of the transparent substrate 10 during the sputtering film formation is preferably 20 ° C. or lower, more preferably 10 ° C. or lower, still more preferably 5 ° C. or lower, particularly preferably 0 ° C. or lower, and also. For example, it is ⁇ 50 ° C. or higher, preferably ⁇ 20 ° C. or higher, more preferably ⁇ 10 ° C. or higher, and even more preferably ⁇ 7 ° C. or higher.
  • Examples of the power supply for applying a voltage to the target include a DC power supply, an AC power supply, an MF power supply, and an RF power supply.
  • a DC power source and an RF power source may be used in combination.
  • the absolute value of the discharge voltage during the sputtering film formation is, for example, 50 V or more, and is, for example, 500 V or less, preferably 400 V or less.
  • the transparent conductive film X can be manufactured as described above.
  • the light-transmitting conductive film 20 in the transparent conductive film X may be patterned as schematically shown in FIG.
  • the light-transmitting conductive film 20 can be patterned by etching the light-transmitting conductive film 20 through a predetermined etching mask.
  • the patterned light-transmitting conductive film 20 functions as, for example, a wiring pattern.
  • the light-transmitting conductive film 20 in the transparent conductive film X is converted into a crystalline light-transmitting conductive film 20'(shown in FIG. 5) by heating.
  • the heating means include an infrared heater and an oven (heat medium heating type oven, hot air heating type oven).
  • the heating environment may be either a vacuum environment or an atmospheric environment.
  • heating is carried out in the presence of oxygen.
  • the heating temperature is, for example, 100 ° C. or higher, preferably 120 ° C. or higher, from the viewpoint of ensuring a high crystallization rate.
  • the heating temperature is, for example, 200 ° C. or lower, preferably 180 ° C. or lower, more preferably 170 ° C.
  • the heating time is, for example, less than 600 minutes, preferably less than 120 minutes, more preferably 90 minutes or less, still more preferably 60 minutes or less, and for example, 1 minute or more, preferably 5 minutes or more.
  • the above-mentioned patterning of the light-transmitting conductive film 20 may be performed before heating for crystallization, or may be performed after heating for crystallization.
  • the surface resistance of the crystalline light-transmitting conductive film 20' is, for example, 200 ⁇ / ⁇ or less, preferably 100 ⁇ / ⁇ or less, more preferably 70 ⁇ / ⁇ or less, still more preferably 50 ⁇ / ⁇ or less, and further preferably 30 ⁇ / ⁇ . ⁇ or less, particularly preferably 20 ⁇ / ⁇ or less.
  • the surface resistance of the light transmissive conductive film 20' is, for example, 1 ⁇ / ⁇ or more. The surface resistance can be measured by the 4-terminal method based on JIS K7194.
  • the specific resistance of the light transmissive conductive film 20' is preferably 3 ⁇ 10 -4 ⁇ ⁇ cm or less, more preferably 2.8 ⁇ 10 -4 ⁇ ⁇ cm or less, and even more preferably 2.5 ⁇ 10 -4 ⁇ . ⁇ Cm or less, more preferably 2 ⁇ 10 -4 ⁇ ⁇ cm or less, particularly preferably 1.8 ⁇ 10 -4 ⁇ ⁇ cm or less.
  • the specific resistance of the light transmissive conductive film 20' is preferably 0.1 ⁇ 10 -4 ⁇ ⁇ cm or more, more preferably 0.5 ⁇ 10 -4 ⁇ ⁇ cm or more, still more preferably 1.0 ⁇ . It is 10 -4 ⁇ ⁇ cm or more.
  • the total light transmittance (JIS K 7375-2008) of the light transmissive conductive film 20' is preferably 65% or more, more preferably 80% or more, and further preferably 85% or more. Further, the total light transmittance of the light transmissive conductive film 20 is, for example, 100% or less.
  • the light-transmitting conductive film 20 of the transparent conductive film X is amorphous, contains a conductive oxide containing krypton, and has a specific resistance of 4 ⁇ 10 -4 ⁇ ⁇ cm or more. It is preferably 4.5 ⁇ 10 -4 ⁇ ⁇ cm or more, more preferably 4.8 ⁇ 10 -4 ⁇ ⁇ cm or more, still more preferably 5 ⁇ 10 -4 ⁇ ⁇ cm or more, and particularly preferably 5.2. ⁇ 10 -4 ⁇ ⁇ cm or more.
  • Such a configuration is suitable for obtaining a low-resistance light-transmitting conductive film 20'(crystalline light-transmitting conductive film) in which warpage is suppressed.
  • the transparent conductive film X includes such a light-transmitting conductive film 20, it is suitable for providing a low-resistance light-transmitting conductive film 20'(crystalline light-transmitting conductive film) and suppressing warpage. ..
  • the functional layer 12 has high adhesion of the light-transmitting conductive film 20 (the light-transmitting conductive film 20'after the crystallization of the light-transmitting conductive film 20; the same applies hereinafter) to the transparent base material 10. It may be an adhesion improving layer for realizing the above.
  • the configuration in which the functional layer 12 is an adhesion improving layer is suitable for ensuring the adhesion between the transparent base material 10 and the light transmissive conductive film 20.
  • the functional layer 12 may be an index-matching layer for adjusting the reflectance of the surface of the transparent base material 10 (one surface in the thickness direction D).
  • the configuration in which the functional layer 12 is the refractive index adjusting layer makes it difficult to visually recognize the pattern shape of the light transmissive conductive film 20 when the light transmissive conductive film 20 on the transparent base material 10 is patterned. Suitable.
  • the functional layer 12 may be a peeling functional layer for practically peeling the light-transmitting conductive film 20 from the transparent base material 10.
  • the structure in which the functional layer 12 is a peeling functional layer is suitable for peeling the light-transmitting conductive film 20 from the transparent base material 10 and transferring the light-transmitting conductive film 20 to another member.
  • the functional layer 12 may be a composite layer in which a plurality of layers are connected in the thickness direction D.
  • the composite layer preferably includes two or more layers selected from the group consisting of a hard coat layer, an adhesion improving layer, a refractive index adjusting layer, and a peeling functional layer.
  • Such a configuration is suitable for complex expression of the above-mentioned functions of each selected layer in the functional layer 12.
  • the functional layer 12 includes an adhesion improving layer, a hard coat layer, and a refractive index adjusting layer on the transparent resin film 11 in this order toward one side in the thickness direction D.
  • the functional layer 12 includes a peeling functional layer, a hard coat layer, and a refractive index adjusting layer on the transparent resin film 11 in this order toward one side in the thickness direction D.
  • the transparent conductive film X is used in a state of being fixed to an article and, if necessary, a light transmissive conductive film 20'patterned.
  • the transparent conductive film X is attached to the article via, for example, a fixing functional layer.
  • Examples of articles include elements, members, and devices. That is, examples of the article with a transparent conductive film include an element with a transparent conductive film, a member with a transparent conductive film, and a device with a transparent conductive film.
  • Examples of the element include a dimming element and a photoelectric conversion element.
  • Examples of the dimming element include a current-driven dimming element and an electric field-driven dimming element.
  • Examples of the current-driven dimming element include an electrochromic (EC) dimming element.
  • Examples of the electric field drive type dimming element include a PDLC (polymer dispersed liquid crystal) dimming element, a PNLC (polymer network liquid crystal) dimming element, and an SPD (suspended particle device) dimming element.
  • Examples of the photoelectric conversion element include a solar cell and the like.
  • Examples of the solar cell include an organic thin-film solar cell and a dye-sensitized solar cell.
  • Examples of the member include an electromagnetic wave shield member, a heat ray control member, a heater member, and an antenna member.
  • Examples of the device include a touch sensor device, a lighting device, and an image display device.
  • the fixing functional layer examples include an adhesive layer and an adhesive layer.
  • the material of the fixing function layer any material having transparency and exhibiting the fixing function can be used without particular limitation.
  • the fixing functional layer is preferably formed of a resin.
  • the resin include acrylic resin, silicone resin, polyester resin, polyurethane resin, polyamide resin, polyvinyl ether resin, vinyl acetate / vinyl chloride copolymer, modified polyolefin resin, epoxy resin, fluororesin, natural rubber, and synthetic rubber. Be done.
  • Acrylic resin is preferable as the resin because it exhibits adhesive properties such as cohesiveness, adhesiveness, and appropriate wettability, is excellent in transparency, and is excellent in weather resistance and heat resistance.
  • a corrosion inhibitor may be added to the fixing functional layer (resin forming the fixing functional layer) in order to suppress corrosion of the light-transmitting conductive film 20'.
  • a migration inhibitor for example, a material disclosed in Japanese Patent Application Laid-Open No. 2015-0222397 is blended in the fixing functional layer (resin forming the fixing functional layer) in order to suppress migration of the light transmissive conductive film 20'. May be good.
  • the fixing functional layer (resin forming the fixing functional layer) may be blended with an ultraviolet absorber in order to suppress deterioration of the article when it is used outdoors. Examples of the ultraviolet absorber include benzophenone compounds, benzotriazole compounds, salicylic acid compounds, oxalic acid anilides compounds, cyanoacrylate compounds, and triazine compounds.
  • the light transmissive conductive film 20' (the light transmissive conductive film after patterning) is formed in the transparent conductive film X. (Including 20') is exposed.
  • the cover layer may be arranged on the exposed surface of the light transmissive conductive film 20'.
  • the cover layer is a layer that covers the light-transmitting conductive film 20', and can improve the reliability of the light-transmitting conductive film 20'and suppress functional deterioration due to damage to the light-transmitting conductive film 20'.
  • Such a cover layer is preferably formed of a dielectric material, more preferably of a composite material of a resin and an inorganic material.
  • the resin include the above-mentioned resins for the fixing functional layer.
  • the inorganic material include inorganic oxides and fluorides.
  • the inorganic oxide include silicon oxide, titanium oxide, niobium oxide, aluminum oxide, zirconium dioxide, and calcium oxide.
  • the fluoride include magnesium fluoride.
  • the cover layer (mixture of resin and inorganic material) may contain the above-mentioned corrosion inhibitor, migration inhibitor, and ultraviolet absorber.
  • the present invention will be specifically described below with reference to examples.
  • the present invention is not limited to the examples.
  • the specific numerical values such as the compounding amount (content), the physical property value, the parameter, etc. described below are the compounding amounts corresponding to them described in the above-mentioned "mode for carrying out the invention”. It can be replaced with an upper limit (numerical value defined as “less than or equal to” or “less than”) or a lower limit (numerical value defined as "greater than or equal to” or “greater than or equal to”) such as content), physical property value, and parameter.
  • Example 1 As a transparent base material, a long PET film with a double-sided hard coat layer (product name "KB film CANIA, thickness 54 ⁇ m, manufactured by Kimoto Co., Ltd.) was prepared. This transparent base material was heat-treated at 165 ° C. for 1 hour. Later, the heat shrinkage rate of the transparent base material in the direction of maximum shrinkage (maximum heat shrinkage rate, heat shrinkage rate of the base material in the MD direction in this embodiment) is 0.65%.
  • an amorphous light-transmitting conductive film having a thickness of 150 nm was formed on the hard coat layer of the transparent substrate by the reactive sputtering method.
  • a sputtering film forming apparatus DC magnetron sputtering apparatus capable of carrying out a film forming process by a roll-to-roll method was used.
  • the conditions for sputter film formation in this example are as follows.
  • a sintered body of indium oxide and tin oxide (tin oxide concentration was 10% by mass) was used.
  • a DC power source was used as the power source for applying the voltage to the target (horizontal magnetic field strength on the target was 90 mT).
  • the film formation temperature (the temperature of the transparent substrate on which the light-transmitting conductive film is laminated) was set to ⁇ 5 ° C. Further, after the film forming chamber is evacuated until the ultimate vacuum degree in the film forming chamber of the apparatus reaches 0.8 ⁇ 10 -4 Pa, Kr as a sputtering gas and Kr as a reactive gas are used in the film forming chamber. Oxygen was introduced, and the air pressure in the film forming chamber was set to 0.4 Pa.
  • the ratio of the oxygen introduction amount to the total introduction amount of Kr and oxygen introduced into the film forming chamber is about 2.5 flow rate%, and the oxygen introduction amount is the specific resistance-oxygen introduction amount curve as shown in FIG.
  • the value of the specific resistance of the formed film was adjusted to be 6.2 ⁇ 10 -4 ⁇ ⁇ cm within the region R of.
  • the resistivity-oxygen introduction amount curve shown in FIG. 6 shows the specific resistance of the light-transmitting conductive film when the light-transmitting conductive film is formed by the reactive sputtering method under the same conditions as above except for the oxygen introduction amount.
  • the dependence on the amount of oxygen introduced can be investigated and created in advance.
  • the transparent conductive film of Example 1 was produced.
  • the light-transmitting conductive film (thickness 150 nm, amorphous) of the transparent conductive film of Example 1 is composed of a single Kr-containing ITO layer.
  • Example 2 to 7, 10 In the sputter film formation, the pressure in the film forming chamber was set to 0.2 Pa instead of 0.4 Pa, the thickness of the light-transmitting conductive film formed was set to 130 nm instead of 150 nm, and the film was formed. resistivity in place of the 6.2 ⁇ 10 -4 ⁇ ⁇ cm 6.5 ⁇ 10 -4 ⁇ ⁇ cm ( example 2), 7.5 ⁇ 10 -4 ⁇ ⁇ cm ( example 3), 10.
  • Example 4 ⁇ 10 -4 ⁇ ⁇ cm (Example 4), 8.8 ⁇ 10 -4 ⁇ ⁇ cm (Example 5), 11.6 ⁇ 10 -4 ⁇ ⁇ cm (Example 6), 5.0 ⁇
  • the transparent conductive film of Example 1 except that the amount of oxygen introduced was adjusted to 10 -4 ⁇ ⁇ cm (Example 7) or 8.2 ⁇ 10 -4 ⁇ ⁇ cm (Example 10).
  • the light-transmitting conductive film (thickness 130 nm) of each of the transparent conductive films of Examples 2 to 7 and 10 comprises a single Kr-containing ITO layer.
  • Example 8 In the formation of the light-transmitting conductive film, the first sputter film formation in which the first region (thickness 85 nm) of the light-transmitting conductive film is formed on the transparent substrate and the light-transmitting conductive film on the first region.
  • the transparent conductive film of Example 8 was produced in the same manner as the transparent conductive film of Example 1 except that the second sputter film formation for forming the second region (thickness 45 nm) was sequentially carried out. ..
  • the conditions for the first sputter film formation in this example are as follows.
  • a target a sintered body of indium oxide and tin oxide (tin oxide concentration was 10% by mass) was used.
  • a DC power source was used as the power source for applying the voltage to the target (horizontal magnetic field strength on the target was 90 mT).
  • the film formation temperature was ⁇ 5 ° C.
  • Kr as a sputtering gas and oxygen as a reactive gas were introduced into the film forming chamber.
  • the air pressure in the film forming chamber was set to 0.2 Pa.
  • the amount of oxygen introduced into the film forming chamber was adjusted so that the value of the specific resistance of the film to be formed was 6.5 ⁇ 10 -4 ⁇ ⁇ cm.
  • the conditions for the second sputter film formation in this example are as follows. After setting the ultimate vacuum degree in the second film forming chamber of the apparatus to 0.8 ⁇ 10 -4 Pa, Ar as a sputtering gas and oxygen as a reactive gas are introduced into the film forming chamber to form a film. The air pressure in the room was set to 0.4 Pa. In this embodiment, the other conditions in the second sputter film formation are the same as those in the first sputter film formation.
  • the transparent conductive film of Example 8 was produced.
  • the light-transmitting conductive film (thickness 130 nm) of the transparent conductive film of Example 8 has a first region (thickness 85 nm) made of a Kr-containing ITO layer and a second region (thickness 45 nm) made of an Ar-containing ITO layer. ), In order from the transparent substrate side.
  • Example 9 In the formation of the light-transmitting conductive film, the first sputter film formation in which the second region (thickness 42 nm) of the light-transmitting conductive film is formed on the transparent substrate and the light-transmitting conductive film on the second region.
  • the transparent conductive film of Example 9 was produced in the same manner as the transparent conductive film of Example 1 except that the second sputter film formation for forming the first region (thickness 76 nm) was sequentially carried out. ..
  • the conditions for the first sputter film formation in this example are the same as the conditions for the second sputter film formation in Example 8.
  • the conditions for the second sputter film formation in this example are the same as the conditions for the first sputter film formation in Example 8.
  • the transparent conductive film of Example 9 was produced.
  • the light-transmitting conductive film (thickness 118 nm) of the transparent conductive film of Example 9 has a second region (thickness 42 nm) composed of an Ar-containing ITO layer and a first region (thickness 76 nm) composed of a Kr-containing ITO layer. ), In order from the transparent substrate side.
  • Example 11 The transparent conductive film of Example 11 was produced in the same manner as the transparent conductive film of Example 1 except for the following matters in the sputtering film formation.
  • a mixed gas of krypton and argon (Kr90% by volume, Ar10% by volume) was used as the sputtering gas.
  • the air pressure in the film forming chamber was set to 0.2 Pa.
  • the ratio of the oxygen introduction amount to the total introduction amount of the mixed gas and oxygen introduced into the film forming chamber is about 2.7 flow rate%, and the oxygen introduction amount is such that the value of the specific resistance of the formed film is 5.7 ⁇ . It was adjusted to 10 -4 ⁇ ⁇ cm.
  • the thickness of the light-transmitting conductive film formed was 146 nm.
  • the light-transmitting conductive film (thickness 146 nm) of the transparent conductive film of Example 11 is composed of a single ITO layer containing Kr and Ar.
  • Example 1 A light-transmitting conductive film was formed in the same manner as in Example 1 except that the film formation temperature was set to 30 ° C. instead of ⁇ 5 ° C. in the sputter film formation (Kr introduction amount and oxygen introduction in Comparative Example 1). The amount is the same as the amount of Kr introduced and the amount of oxygen introduced in Example 1). As a result, the transparent conductive film of Comparative Example 1 was produced.
  • the light-transmitting conductive film (thickness 150 nm) of the transparent conductive film of Comparative Example 1 is composed of a single Kr-containing ITO layer.
  • Example 2 A light transmissive conductive film was formed in the same manner as in Example 2 except that Ar was used instead of Kr as the sputtering gas in the sputtering film formation (the amount of Ar introduced and the amount of oxygen introduced in Comparative Example 2 were the same. It is the same as the amount of Kr introduced and the amount of oxygen introduced in Example 2). As a result, the transparent conductive film of Comparative Example 2 was produced.
  • the light-transmitting conductive film (thickness 130 nm) of the transparent conductive film of Comparative Example 2 is composed of a single Ar-containing ITO layer.
  • each light-transmitting conductive film in Examples 1 to 11 and Comparative Examples 1 and 2 was measured by FE-TEM observation. Specifically, first, a cross-section observation sample of each light-transmitting conductive film in Examples 1 to 11 and Comparative Examples 1 and 2 was prepared by the FIB microsampling method. In the FIB microsampling method, an FIB device (trade name "FB2200", manufactured by Hitachi) was used, and the acceleration voltage was set to 10 kV. Next, the thickness of the light-transmitting conductive film in the cross-section observation sample was measured by FE-TEM observation. In the FE-TEM observation, an FE-TEM device (trade name "JEM-2800", manufactured by JEOL) was used, and the acceleration voltage was set to 200 kV.
  • FE-TEM observation an FE-TEM device (trade name "JEM-2800", manufactured by JEOL) was used, and the acceleration voltage was set to 200 kV.
  • Example 8 For the thickness of the first region of the light transmissive conductive film in Example 8, a cross-section observation sample was prepared from the intermediate product before forming the second region on the first region, and the sample was FE-. It was measured by TEM observation. The thickness of the second region of the light-transmitting conductive film in Example 8 was obtained by subtracting the thickness of the first region from the total thickness of the light-transmitting conductive film in Example 8. The ratio of the first region in the thickness direction of the light-transmitting conductive film of Example 8 was 65.4%.
  • Example 9 For the thickness of the second region of the light transmissive conductive film in Example 9, a cross-section observation sample was prepared from the intermediate product before forming the first region on the second region, and the sample was FE-. It was measured by TEM observation. The thickness of the first region of the light-transmitting conductive film in Example 9 was obtained by subtracting the thickness of the second region from the total thickness of the light-transmitting conductive film in Example 9. The ratio of the first region in the thickness direction of the light-transmitting conductive film of Example 9 was 64.4%.
  • the sample was allowed to stand for 10 minutes in a room temperature (24 ° C.) environment.
  • 175 mm of each was cut off from both ends in the long side direction of the sample.
  • a measurement sample having a size of 50 mm ⁇ 50 mm was prepared.
  • the measurement sample was placed on a work table having a horizontal plane (the light-transmitting conductive film of the measurement sample was placed so as to be located on the side opposite to the horizontal plane). Then, each dimension of each of the four sides of the measurement sample (specifically, the distance between the two vertices on each side) was measured.
  • the Kr content (atomic%) and Ar content (atomic% are listed in Table 1.
  • the detection limit value (lower limit value) or more The detection limit may vary depending on the thickness of the light-transmitting conductive film attached to the measurement). Therefore, Table 1 shows the Kr content of the light-transmitting conductive film. , In order to show that it is below the detection limit value in the thickness of the same film, it is described as " ⁇ Specific detection limit value in the thickness of the light transmissive conductive film attached to the measurement" (contains rare gas atoms). The same applies to the notation of quantities).
  • the light-transmitting conductive film of the present invention can be used as a conductor film for forming a pattern of transparent electrodes in various devices such as liquid crystal displays, touch panels, and optical sensors.
  • the transparent conductive film of the present invention can be used as a feed material for such a conductor film.

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