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WO2015037182A1 - Substrat conducteur transparent et procédé de fabrication de substrat conducteur transparent - Google Patents

Substrat conducteur transparent et procédé de fabrication de substrat conducteur transparent Download PDF

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Publication number
WO2015037182A1
WO2015037182A1 PCT/JP2014/004104 JP2014004104W WO2015037182A1 WO 2015037182 A1 WO2015037182 A1 WO 2015037182A1 JP 2014004104 W JP2014004104 W JP 2014004104W WO 2015037182 A1 WO2015037182 A1 WO 2015037182A1
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Prior art keywords
transparent conductive
transparent
conductive substrate
layer
film
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Ceased
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PCT/JP2014/004104
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English (en)
Japanese (ja)
Inventor
昭造 河添
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ROCK GIKEN KOGYO CO LTD
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ROCK GIKEN KOGYO CO LTD
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Priority to KR1020167007142A priority Critical patent/KR102214745B1/ko
Priority to CN201480049430.0A priority patent/CN105556618B/zh
Priority to JP2015536433A priority patent/JP6106756B2/ja
Publication of WO2015037182A1 publication Critical patent/WO2015037182A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • 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
    • 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
    • G06F3/045—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means using resistive elements, e.g. a single continuous surface or two parallel surfaces put in contact
    • 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
    • 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
    • H05K9/0073—Shielding materials
    • H05K9/0094—Shielding materials being light-transmitting, e.g. transparent, translucent
    • 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
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H10F71/138—Manufacture of transparent electrodes, e.g. transparent conductive oxides [TCO] or indium tin oxide [ITO] electrodes
    • 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
    • H10F77/10—Semiconductor bodies
    • H10F77/16—Material structures, e.g. crystalline structures, film structures or crystal plane orientations
    • H10F77/169—Thin semiconductor films on metallic or insulating substrates
    • 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
    • H10F77/244—Electrodes made of transparent conductive layers, e.g. transparent conductive oxide [TCO] 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/202—Conductive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/412—Transparent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/416—Reflective
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/554—Wear resistance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/584—Scratch resistance
    • 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
    • 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
    • B32B2457/12—Photovoltaic modules
    • 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
    • G—PHYSICS
    • G06—COMPUTING OR CALCULATING; COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
    • G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
    • G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
    • 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
    • G06F3/044—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
    • G06F3/0445—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means using two or more layers of sensing electrodes, e.g. using two layers of electrodes separated by a dielectric layer

Definitions

  • the present invention relates to a transparent conductive substrate that can be used as a touch panel, an electrode for a solar cell, an electrode for an EL device, an electrode for a light emitting diode, a heater, or a substrate for electromagnetic wave / electrostatic shielding, and the transparent conductive substrate It relates to the manufacturing method.
  • a transparent conductive substrate in which a transparent metal oxide conductive layer (ITO, ZnO, etc.) is formed on a transparent substrate is transparent and conductive, and thus, a touch panel, a solar cell, an EL device, an electromagnetic wave / electrostatic shield, or It is used for ultraviolet / infrared shields.
  • a transparent metal oxide conductive layer ITO, ZnO, etc.
  • the transparent conductive substrate on which the conventional metal oxide conductive layer (ITO, ZnO, etc.) is formed has the following problems 1) to 3).
  • the metal oxide conductive layer surface has a large amount of light reflection of visible light and poor transparency.
  • the metal oxide conductive layer absorbs light in the vicinity of near-ultraviolet light, the transmittance at a light wavelength smaller than 450 nm decreases and it becomes yellow.
  • the surface resistance of the large-sized touch panel, the electrode for a solar cell, the electrode for an EL device, the electrode for a light emitting diode, and the heater needs to be reduced. In order to reduce the surface resistance, the thickness of the metal oxide conductive layer is increased.
  • the conventional transparent conductive substrate has a total light transmittance of about 88% when the surface resistance is 100 ⁇ / ⁇ , for example, but in order to increase the film thickness when the surface resistance is 100 ⁇ / ⁇ or less,
  • the properties of the above 1) and 2) are significantly reduced. Further, due to the problems 1) and 2), when the metal oxide conductive layer is used by pattern etching, the difference between the portion with the pattern and the portion without the pattern can be clearly recognized. 3) Since the ITO film is a thin film, scratches due to rubbing occur during transport, processing, and use, and defects such as conductivity deterioration, disconnection, and appearance deterioration occur.
  • Patent Document 1 after performing a high frequency sputter etching process on the surface of a polyethylene terephthalate film, a transparent conductive thin film is formed, and then a transparent dielectric thin film having a film thickness of 10 nm or more is formed on this thin film.
  • a method of producing the characterized transparent conductive film is described. In this manufacturing method, the formation of a dielectric thin film is intended to improve the scratch resistance and the transparency.
  • a transparent conductive thin film is formed on one side of a transparent film substrate having a thickness of 2 to 120 ⁇ m, and a transparent dielectric thin film is further formed on the conductive thin film, and the other side is formed
  • a transparent conductive laminate in which a transparent substrate is bonded via a transparent pressure-sensitive adhesive layer is described.
  • the formation of the dielectric thin film improves the transparency and the scratch resistance, and also improves the hitting characteristics.
  • the transparent dielectric thin film is an electrical insulating layer, so the metal oxide conductive layer and the electrode provided on the dielectric thin film layer (conductive paste, The conductivity between metal layers etc.) was very poor, and the conductivity was unstable. Further, pattern etching of the metal oxide conductive layer (ITO) film has been difficult due to the presence of the insulating layer.
  • ITO metal oxide conductive layer
  • the transparent conductive base material which provided the dielectric material thin film layer in the metal oxide conductive layer needs the electrode for etching of an ITO film, a lead, etc. like a touch panel, a solar cell, EL device, or a light emitting diode. Applications are limited because it is unsuitable for various applications.
  • Patent Document 3 proposes a transparent conductive substrate in which a transparent conductive thin film layer and a transparent metal oxide layer are laminated in this order on one side or both sides of a substrate in order to improve the conventional problems.
  • the transparent metal oxide layer has a large number of fine pores penetrating to the front and back surfaces, and the pore diameter of the pores on the opposite side is larger than the pore diameter of the pores in the surface in contact with the transparent conductive thin film. doing.
  • the transparent conductive substrate of Patent Document 3 has the following problems. When an Ag paste electrode is formed on the transparent metal oxide layer, the contact resistance between the electrode and the transparent conductive thin film layer is high.
  • the method of forming microvoids according to Patent Document 3 has the following problems because it uses the “oblique vacuum deposition method”.
  • the sputter deposition method by a "sputter deposition machine” is usually used for formation of a transparent conductive thin film layer, since a "diagonal vacuum deposition machine” must be separately introduced, equipment investment and manufacturing cost increase.
  • the oblique deposition method it is necessary to narrow the deposition incidence angle, and the deposition area is significantly reduced, so that the deposition adhesion efficiency of the transparent metal oxide material is significantly reduced (usually several percent). Therefore, in the case of an expensive material such as Si, SiO 2 or SiO x , the cost of materials is significantly increased, the processing speed is decreased, and the cost of manufacturing is increased.
  • the present inventors form the transparent metal oxide layer on the transparent conductive thin film layer by interspersing particles, reduce the coverage of the transparent conductive thin film layer by the transparent metal layer, and make the interparticle transparent.
  • the conductivity of the transparent conductive thin film layer and the metal electrode on the transparent metal oxide layer is significantly increased without lowering the transparency, and the index matching property and the scratch resistance are improved.
  • the inventors of the present invention have found that, by setting the degree of vacuum in sputter deposition to 5 to 20 Pa, particles of a particle diameter suitable for the transparent metal oxide layer can be scattered.
  • the present invention has been completed based on these findings and has been further studied repeatedly, and the conductivity of the transparent conductive thin film layer such as ITO and the electrode such as metal and metal paste is high and the transparency is also high. It is an object of the present invention to provide a transparent conductive substrate which is excellent in index matching property, scratch resistance and etching property.
  • the transparent conductive substrate of the present invention according to claim 1 is a transparent conductive substrate in which a transparent conductive thin film layer and a transparent metal oxide layer are laminated in this order on one side or both sides of the substrate, It is characterized in that the transparent metal oxide layer is formed by interspersing particles.
  • the present invention according to claim 2 is that, in the transparent conductive substrate according to claim 1, the coverage of the transparent conductive thin film layer by the transparent metal oxide layer is 60 to 1%. It features.
  • the present invention according to claim 3 is characterized in that, in the transparent conductive substrate according to claim 1 or 2, the surface resistance of the transparent conductive thin film layer is 100 ( ⁇ / ⁇ ) or less. .
  • the present invention according to claim 4 is the transparent conductive substrate according to any one of claims 1 to 3, wherein the visible light surface reflectance of the transparent metal oxide layer and the visible light of the substrate It is characterized in that the difference with the light ray surface reflectance is less than 4%.
  • the particle diameter of the particles is 20 to 800 nm, and the distance between the particles is 20 to 2000 nm. It is characterized by The invention according to claim 6 is characterized in that, in the transparent conductive substrate according to claim 5, the particle diameter of the particles is 30 to 250 nm, and the distance between the particles is 30 to 1280 nm.
  • a metal electrode is laminated on the transparent conductive thin film layer.
  • the method for producing a transparent conductive substrate of the present invention according to claim 8 is a method for producing a transparent conductive substrate in which a transparent conductive thin film layer and a transparent metal oxide layer are laminated in this order on one side or both sides of the substrate.
  • the method is characterized in that the transparent metal oxide layer is formed of particles having a particle size in the range of 30 to 800 nm by sputter deposition under a vacuum degree of 2.5 to 20 Pa.
  • the touch panel of the present invention according to claim 9 is characterized by comprising the transparent conductive substrate according to any one of claims 1 to 7.
  • the solar cell of the present invention according to claim 10 is characterized by comprising the transparent conductive substrate according to any one of claims 1 to 7.
  • the heater of the present invention according to claim 11 comprises the transparent conductive substrate according to any one of claims 1 to 7.
  • the electromagnetic wave / electrostatic shield substrate of the present invention according to claim 12 is characterized by comprising the transparent conductive substrate according to any one of claims 1 to 7.
  • the EL device of the present invention according to claim 13 is characterized in that the transparent conductive substrate according to any one of claims 1 to 7 is used as an electrode.
  • the light emitting diode of the present invention according to claim 14 is characterized in that the transparent conductive substrate according to any one of claims 1 to 7 is used as an electrode.
  • the transparent electromagnetic wave reflecting material of the present invention according to claim 15 is characterized in that the transparent conductive substrate according to any one of claims 1 to 6 is used.
  • the transparent infrared reflective material of the present invention according to claim 16 is characterized in that the transparent conductive substrate according to any one of claims 1 to 6 is used.
  • the transparent conductive substrate of the present invention has high conductivity between the transparent conductive thin film layer and the metal electrode, is excellent in transparency, index matching property, scratch resistance, can be etched, and is the next generation transparent
  • a conductive substrate, a method of manufacturing the transparent conductive substrate, a touch panel using the same, and the like can be provided.
  • the schematic diagram which shows the cross section of the transparent conductive base material in one Embodiment of this invention The schematic diagram which shows the cross section of the general electrostatic capacitance type touch panel using the transparent conductive base material in this embodiment
  • Typical surface photograph of transparent conductive film by scanning electron microscope Typical surface photograph of transparent conductive film by scanning electron microscope
  • FIG. 1 is a schematic view showing a cross section of a transparent conductive substrate in an embodiment of the present invention.
  • the transparent conductive substrate 10 in the present embodiment has a transparent conductive thin film layer 12 and a transparent metal oxide layer 13 laminated in this order on one surface or both surfaces of the substrate 11, that is, at least one surface of the substrate 11. Is configured.
  • a metal electrode 20 is provided on the transparent metal oxide layer 13.
  • the substrate 11 for example, glass, various plastic films or sheets (plates) having transparency can be used.
  • plastic films and sheets for example, those containing polyester, polycarbonate, polyamide, polyimide, polyolefin, polyvinyl chloride, polyvinylidene chloride, polystyrene, polyvinyl alcohol, polyacrylate, polyarylate, or polyphenylene sulfide as a resin component are used.
  • polyester is particularly preferable, and among polyesters, polyethylene terephthalate is particularly preferable.
  • the thickness of the substrate 11 is not particularly limited, and can be set according to the product characteristics.
  • the thickness of the film is usually 6 to 400 ⁇ m, preferably about 20 to 200 ⁇ m, and the thickness of the sheet (plate) is usually about 400 ⁇ m to 5 mm.
  • the surface of the substrate 11 may be subjected to corona treatment, flame treatment, plasma treatment or the like as a pretreatment before forming the transparent conductive thin film layer 12 on the substrate 11. Physical processing may be performed.
  • an index matching (IM) layer may be formed in advance on the surface of the substrate 11, and the transparent conductive thin film layer 12 may be formed on the IM layer.
  • the IM layer may be formed as a single layer on the surface of the base material 11, but a plurality of layers such as two layers or three layers may be formed with different refractive indices of light. Although the number of layers is not particularly limited, it is better to reduce the number in consideration of cost, productivity, stability and the like.
  • the IM layer in a single layer or the first IM layer in a plurality of layers uses a material having a refractive index greater than that of the substrate 11.
  • MoO having a refractive index of 1.85 to 2.1 is used as the first IM layer in the IM layer or plural layers in a single layer.
  • SiO X a refractive index of 1.6-2.0, the refractive index can be used Al 2 O 3 is 1.64.
  • high refractive materials such as TiO 2 , Ta 2 O 5 , ZrO 2 or Nb 2 O 5 can be used.
  • a material having a refractive index smaller than that of the first IM layer is suitable.
  • SiO 2 or other SiO x having a refractive index of 1.47 may be used. it can.
  • the combination of these refractive indices and the selection of the material are not particularly limited.
  • the formation method of IM layer can use a well-known vacuum evaporation method, sputtering method, the coating method, the printing method etc., and another method may be used.
  • the easy adhesion layer and the hard coat layer may be formed on one side or both sides of the substrate 11.
  • dust removal and cleaning may be performed by solvent cleaning or ultrasonic cleaning.
  • the material of the transparent conductive thin film layer 12 is not particularly limited as long as it has transparency and conductivity, and, for example, indium oxide containing tin oxide (also referred to as ITO) and tin oxide containing antimony Zinc oxide, metal Ag, carbon or the like can be used.
  • ITO indium oxide containing tin oxide
  • tin oxide containing antimony Zinc oxide, metal Ag, carbon or the like can be used as a method of forming the transparent conductive thin film layer 12.
  • conventionally known techniques such as a vacuum evaporation method, a sputtering method, or an ion plating method can be used.
  • materials having conductivity such as indium oxide containing tin oxide (also referred to as ITO), tin oxide containing antimony, zinc oxide, metal Ag, or carbon can be used as transparent resin in the form of nano- or micron-level particles.
  • Conventionally known techniques such as a coating method and a printing method can be used by mixing. In terms of transparent conductivity,
  • the thickness of the transparent conductive thin film layer 12 is not particularly limited, but is usually 5 to 2000 nm, preferably 10 to 1000 nm. Within this range, both conductivity and transparency are excellent. Also, in order to improve the adhesion of the transparent metal oxide layer 13, plasma treatment or the like on the surface of the transparent conductive thin film layer 12 as a pretreatment before forming the transparent metal oxide layer 13 on the transparent conductive thin film layer 12 You may
  • the transparent metal oxide layer 13 is formed by interspersing particles 13 a. That is, the respective particles 13a are provided discontinuously at certain intervals. However, a plurality of particles 13a may be adjacent to each other or may overlap with each other.
  • the transparent conductive thin film layer 12 is exposed on the surface of the transparent metal oxide layer 13, and the particles 13a do not cover the entire transparent conductive thin film layer 12.
  • the particle diameter of the particles 13a is preferably in the range of 20 to 800 nm, and a remarkable effect can be confirmed in at least the range of 30 to 250 nm. When the particle size of the particles 13a is smaller than 20 nm, improvement in transparency can not be expected, and when the particle size is larger than 800 nm, the haze value increases.
  • the transmittance is lowered and the resolution of characters and images is lowered, which is not preferable.
  • the distance between the adjacent particles 13a is preferably in the range of 20 to 2000 nm, and a remarkable effect can be confirmed in at least the range of 30 to 1280 nm.
  • the transparent metal oxide layer 13 is not a continuous film in which the particles 13a are connected to each other, but a discontinuous film in which adjacent particles 13a have an interval of 30 nm or more. In consideration of the etching of the transparent conductive thin film layer 12 and the conductivity between the transparent metal oxide layer 13 and the metal electrode 20, it is preferable to increase the distance between adjacent particles 13a to expose the transparent conductive thin film layer 12 .
  • the spacing between adjacent particles 13a may not be uniform in the range of 20 to 2000 nm, and a partially overlapped state may occur, or a spacing exceeding 2000 nm may partially occur.
  • the average thickness of the transparent metal oxide layer 13 is a thickness for optically improving the transmittance, and can be measured by a contact surface roughness tester in general.
  • the material of the transparent metal oxide layer 13 may be any material that can form a transparent metal oxide layer.
  • TiO 2 , Ta 2 O 5 , ZrO 2 , SiO x , SiO 2 , Al 2 O 3 , SnO 2 , In 2 O 3 , MgO, MoO 3 are used.
  • the transmittance improvement or It is preferable because it is easy to use.
  • These transparent metal oxide layers 13 are electrically insulating materials, and they may be used singly or as a mixture of two or more, adjusted to have a desired refractive index.
  • the particles 13a forming the metal oxide layer 13 may be mixed with a transparent resin, or a necessary refractive material may be made of a transparent resin.
  • the transparent metal oxide layer 13 can be formed, for example, by the method described later.
  • the surface area of the transparent conductive thin film layer 12 can be determined as ⁇ 100 (%) (where r is the particle size).
  • the surface coverage is set in the range of 1 to 80%, preferably 2 to 60%. The lower the surface coverage, the lower the contact resistance with the metal electrode 20, and the better the etchability of the transparent conductive thin film layer 12.
  • the formation method of the transparent metal oxide layer 13 can use conventionally well-known techniques, such as a vacuum evaporation method, sputtering method, or ion plating method. Moreover, the formation method of the transparent metal oxide layer 13 can mix the particle
  • the transparent metal oxide layer 13 is formed of particles 13 a having a particle diameter in the range of 20 to 800 nm by sputter deposition at a degree of vacuum of 2.5 to 20 Pa.
  • the metal electrode 20 As a material of the metal electrode 20, for example, an alloy or metal paste composed of a single element or two or more elements such as Cu, Ag, Al, Au, Ni, Ni / Cr, Cr, and Ti can be used.
  • the thickness of the metal electrode 20 is not particularly limited, but is usually 0.01 to 50 ⁇ m, preferably 0.02 to 25 ⁇ m.
  • a conventionally known method can be used to form the metal electrode 20.
  • a plating method, a vacuum evaporation method, a sputtering method can be used, and a printing and coating method can be used for the metal paste.
  • Ni, Cr, Ti, Mo, C, Au, Ag, and any of these alloys, or Cu may be provided under and over the metal electrode 20 for the purpose of protecting the metal electrode 20, if necessary.
  • Layers of Ni / Ni alloy or Cu / Cr alloy and layers of these oxides may be provided.
  • a hard coat layer or an antiglare layer may be provided on the side opposite to the ITO surface of the transparent conductive substrate 10 of the present invention on the ITO side.
  • a transparent adhesive layer or the like may be provided and attached to another substrate. Also good.
  • the ITO / transparent metal layer of the present invention may be provided on both sides of the PET.
  • the transparent conductive substrate 10 of the present embodiment can be used as a transparent electrode of a touch panel, an electrode for a solar cell, an electrode for an EL device, an electrode for a light emitting diode, a heater, or a substrate for electromagnetic wave / electrostatic shielding.
  • the transparent conductive substrate 10 of the present embodiment can be used as an upper electrode and / or a lower electrode of a resistive film type or capacitive type touch panel, and the touch panel is disposed on the front surface of a liquid crystal display
  • a display device having a touch panel function can be obtained.
  • the transparent conductive substrate 10 of this embodiment can be suitably used as a low resistance (surface resistance R: 100 to 5 ⁇ / ⁇ ) of a capacitive touch panel, and in particular as an electrode of a large projected capacitive touch panel. It can be used suitably.
  • the transparent conductive substrate 10 of the present embodiment can reflect electromagnetic waves and heat rays (infrared rays) by setting the surface resistance R to 10 ( ⁇ / ⁇ ) or less, a transparent electromagnetic wave reflecting material or a transparent material can be used. It can be used as an infrared reflector.
  • the transparent electromagnetic wave reflecting material can be used, for example, as a display window material of an electric device generating an electromagnetic wave or a window material for checking the inside of the device in order to prevent electromagnetic wave leakage from the inside of the electric device.
  • the transparent electromagnetic wave reflecting material can be used, for example, as a window material of a building or a housing in order to prevent electromagnetic wave penetration from the outside.
  • the transparent infrared reflective material can be used, for example, as a display window material of an electric device that generates infrared light or a window material for internal confirmation of the device, in order to prevent infrared leakage from the inside of the electric device.
  • the transparent infrared reflective material can be used, for example, as a window material of a building or a housing to prevent infrared penetration from the outside.
  • FIG. 2 is a schematic diagram which shows the cross section of the general electrostatic capacitance type touch panel using the transparent conductive base material in this embodiment.
  • the transparent conductive substrate 10 in the present embodiment is attached to the glass 30.
  • the glass 30 may be bonded to the transparent metal oxide layer 13 in addition to the case where the glass 30 is bonded to the substrate 11.
  • the position is detected by the charge change of the touch panel electrode surface.
  • FIG. 3 is a schematic view of a general projected capacitive touch panel using a transparent conductive substrate according to the present embodiment.
  • a capacitive touch panel can be configured using two transparent conductive substrates 10 in which a matrix-like conductive pattern is formed by the transparent conductive thin film layer 12. Since the conductive pattern formed on one of the transparent conductive substrates 10 is connected vertically, the vertical position is detected, and the conductive pattern formed on the other transparent conductive substrate 10 is connected horizontally. The lateral position can be detected and the intersection point can be recognized as the pressed position.
  • the ITO film (transparent conductive thin film layer 12) using a film substrate includes a crystallized (crystal) ITO film and an amorphous ITO film, which can be used as necessary.
  • Crystallized (Crystal) ITO film is formed by sputtering and vacuum evaporation of ITO film, followed by heating and annealing (usually 150 ° C or more, about 50 minutes) in air for the purpose of improving transparency and reducing resistance.
  • annealing usually 150 ° C or more, about 50 minutes
  • the amorphous ITO film is formed by sputtering and vacuum evaporation of the ITO film, and is not annealed. Two types of films will be described below with reference to examples.
  • the double-sided hard coat PET film base material was used for the purpose of the haze increase prevention of the PET film base material at the time of annealing.
  • the total light transmittance of the double-sided hard-coated PET film substrate is about 91%, and the temperature of the film substrate at the time of sputter deposition is normal temperature. Moreover, the usual magnetron electrode method was used for the sputtering method here.
  • Example 2 (crystallization (crystal) ITO film)
  • a Si target was used on the ITO film, and a SiO 2 film having a thickness of about 70 nm was formed by sputter deposition under a vacuum degree of about 10 Pa in an Ar gas atmosphere containing about 3% of O 2 gas.
  • a film crystallized ITO film was formed in the same manner as in Example 1 except for the above.
  • Example 3 (Crystallized (Crystalline) ITO Film) The degree of vacuum at the time of Si sputter deposition on the ITO film was 5 Pa. A film crystallized ITO film was formed in the same manner as in Example 1 except for the above.
  • Example 4 crystal (crystallization (crystal) ITO film)
  • the degree of vacuum at the time of sputter deposition of Si on the ITO film was set to 2.5 Pa.
  • a film crystallized ITO film was formed in the same manner as in Example 1 except for the above.
  • Example 2 The degree of vacuum at the time of Si sputter deposition on the ITO film was 0.4 Pa.
  • a film crystallized ITO film was formed in the same manner as in Example 1 except for the above. When the crystallized ITO film was formed, curling occurred in the base material, and a crack was generated in the deposited film, so that it was not possible to form the intended transparent conductive base material 10.
  • Example 3 The vacuum degree at the time of Si sputter deposition on the ITO film was set to 1 Pa. A film crystallized ITO film was formed in the same manner as in Example 1 except for the above. When the crystallized ITO film was formed, curling occurred in the base material, and a crack was generated in the deposited film, so that it was not possible to form the intended transparent conductive base material 10.
  • Example 5 (amorphous ITO film)
  • the degree of vacuum is 0.1 to 0.9 Pa (in Ar gas atmosphere containing about 1% of O 2 gas)
  • Ar gas atmosphere containing about 1% of O 2 gas
  • a Si target is used on the ITO film, and a SiO 2 film with a thickness of about 95 nm is formed by sputter deposition at a degree of vacuum of 5 to 20 Pa (about 10 Pa) in an Ar gas atmosphere containing about 3% of O 2 gas.
  • the total light transmittance of the PET film substrate at this time was about 90%.
  • Example 6 (amorphous ITO film)
  • the degree of vacuum at the time of sputtering using a Si target was 5 Pa.
  • a target amorphous ITO film substrate was formed in the same manner as in Example 5 except for the above.
  • Example 7 (amorphous ITO film)
  • the degree of vacuum at the time of sputtering using a Si target was 2.5 Pa.
  • a target amorphous ITO film substrate was formed in the same manner as in Example 5 except for the above.
  • Example 5 The degree of vacuum at the time of Si sputter deposition on the ITO film was 0.4 Pa. An amorphous ITO film substrate was formed in the same manner as in Example 5 except for the above.
  • Example 6 The vacuum degree at the time of Si sputter deposition on the ITO film was set to 1 Pa. An amorphous ITO film substrate was formed in the same manner as in Example 5 except for the above.
  • Total light transmittance The total light transmittance of the transparent conductive film was measured using Suga Test Instruments Co., Ltd. HGM-2DP.
  • Etching test of ITO film Using a nitric acid-based ITO etching solution, measure the time until the ITO film is etched (visual and electrical resistance of the film surface is> 10E ⁇ 6 ⁇ / ⁇ ) at liquid temperatures of 20 ° C and 50 ° C. did. In addition, what can not be etched in 40 minutes was displayed as> 40 minutes, and it was judged that etching was not possible. Whether or not the etching was possible was also confirmed with other etching solutions such as sulfuric acid type, hydrochloric acid type and oxalic acid type.
  • the above transparent conductive film is cut into 1 cm width, and two Cu electrodes (10 mm width, about 180 nm thickness) by ordinary sputter deposition are formed so that the distance between the electrodes is 1 cm, both The resistance Rb between the electrodes was measured by the two-terminal method.
  • Index matching between ITO film and substrate The ITO film was partially etched using the transparent conductive film prepared in this example and the comparative example, and the surface reflectance of the surface of the transparent metal oxide layer and the surface of the etched portion (PET film substrate) was measured for each light wavelength ⁇ , 400 nm, 550 nm, and 660 nm.
  • a measured value is a value also including the reflectance of the vapor deposition opposite surface (substrate back surface).
  • the difference ( ⁇ R) in reflectance between the transparent metal oxide layer surface and the etched portion for each wavelength is 4% or less, it is difficult to distinguish visually, so the index matching property is considered to be good. More preferably, the difference in reflectance ( ⁇ R) is 2% or less.
  • Example 1 As also shown in the photographs of FIG. 6 to FIG. 8, in the SiO x layer on the ITO film, particles having a particle diameter of about 190 nm are dispersed at an average spacing of about 890 nm. The coverage of the ITO film surface by the SiO x layer was about 2%. As a result, the contact resistance between the Ag paste electrode and the ITO film, and the contact resistance between the vapor deposition Cu electrode and the ITO film were both good at zero. In the case of the Ag paste electrode, Comparative Example 4 in which the Ag paste electrode was directly formed on the ITO film showed that there is a contact resistance (about 5 ⁇ ) unique to the Ag paste in which Ag particles are dispersed.
  • Example 2 In this example, a SiO 2 layer was formed on the ITO film. The surface observation with a scanning electron microscope was equivalent to FIG. From this, the shape and dispersion of the SiO 2 layer on the ITO film are the same as in Example 1. The same effect as in Example 1 was also obtained on the coverage of the ITO film surface by the SiO 2 layer, the contact resistance between the electrodes, the etching property, and the scratch resistance. In addition, the total light transmittance was also improved as high as 91%.
  • Example 3 In the present example, the Si sputter conditions of Example 1 were changed. According to scanning electron microscopy, in the SiO x layer, particles having a particle size of about 100 nm were dispersed at an average spacing of about 190 nm. The coverage of the ITO film surface with the SiO x layer increased to about 20%. From this, it was found that the contact resistance between the Ag paste electrode and the ITO increases by 1 ⁇ (about 20%) and the etching time also increases (about 20%), but it is still within the practical range. It was also confirmed that etching could be performed with other etching solutions. On the other hand, the scratch resistance (Rb / RO) was good with almost no change at 1.0. In addition, the total light transmittance was also improved as high as 91%. In addition, if the coverage of the ITO film surface is about 20% or less, the surface resistance RO of the ITO film can be measured by a four-terminal measuring device.
  • Example 4 In the present example, the Si sputter conditions of Example 1 were changed. According to scanning electron microscopy, in the SiO x layer, particles of about 80 nm in diameter were dispersed at an average spacing of about 50 nm. The coverage of the ITO film surface with the SiO x layer increased to about 60%. From this, it was found that the contact resistance between the Ag paste electrode and the ITO increases by 5 ⁇ , and the etching time also increases by about twice, but it is still within the practical range. It was also confirmed that etching could be performed with other etching solutions. On the other hand, the scratch resistance (Rb / RO) was good with almost no change at 1.0. In addition, the total light transmittance was also improved as high as 91%.
  • Example 2 In Example 1, the degree of vacuum at the time of sputter deposition of Si was changed to 0.4 Pa and 1 Pa, respectively. Except for this, a crystal ITO film substrate was formed in the same manner. In any case, curling and cracking of the deposited film occurred during heating and curing after sputter deposition (both of the curling and cracking of Comparative Example 2 were larger than those of Comparative Example 3), and the desired amorphous ITO film substrate It turned out that it can not create.
  • SiO x film thickness as thick as approximately 90 nm, and predicted since the SiO 2 film of Comparative Examples 5 and 6 created in the same vacuum degree is a continuous film, SiO x film of this comparative example also is a continuous film It can be predicted. From this, it was found from the results of Examples 1 and 3 that in the case of 160 ° C. high temperature curing, the SiO x film could not form the intended amorphous ITO film substrate unless it was a discontinuous film.
  • Example 5 (amorphous ITO film substrate)
  • the surface observation by scanning electron microscopy was similar to the photographs shown in FIG. 6 to FIG.
  • the particle size, interval dispersion, coverage, etc. of the SiO 2 layer on the ITO film were the same as in Examples 1 and 2.
  • the coverage of the ITO film surface with the SiO 2 layer was also found to be about 2% as well.
  • the contact resistance between the Ag paste and the vapor deposition Cu electrode and the ITO film, the etching property of the ITO film, the scratch resistance and the like were also good as in the above example.
  • an amorphous ITO film reduced in resistance (40 ⁇ / ⁇ ) can be formed by increasing the film thickness of ITO to about 90 nm, and a PET film substrate is formed by forming a SiO 2 layer about 95 nm thick on the ITO film.
  • the total light transmittance could be improved as high as about 90.5%.
  • the high temperature annealing (crystallization) step for reducing the resistance is not necessary. From this, it is not necessary to consider the thermal damage of the film substrate to be used, and there is an advantage that a wide range of substrates can be used without particularly requiring an expensive haze preventing substrate, a high heat resistant substrate and the like.
  • Example 6 amorphous ITO film substrate
  • the degree of vacuum at the time of sputter deposition of the SiO 2 layer was changed to 5 Pa.
  • the surface observation results were the same as in Example 3, and the coverage of the SiO 2 layer was also about 20%. Other characteristics were also good as in the other examples.
  • Comparative example 4 In this comparative example, only the ITO film without the SiO 2 layer was used. The total light transmittance in this case was as low as 79%, much worse than the PET film substrate (about 90%). In addition, the scratch resistance (Rb / RO) is 2.0, and the ITO film is easily scratched. As a result of the above, there is a need for improvement. The other properties were the same as in Comparative Example 1.
  • Example 4 In Example 4, the degree of vacuum at the time of sputter deposition of Si was changed to 0.4 Pa and 1 Pa, respectively. Except for this, an amorphous ITO film substrate was formed by the same method. As a result of surface observation, the SiO 2 film was a completely continuous film, and the coverage of the SiO 2 film was about 100%. The surface resistance of the ITO film of the present substrate could not be measured by the four-terminal measurement method. Moreover, even if it uses Ag paste electrode and vapor deposition Cu electrode, contact resistance is as high as 1 * 10E6 ((ohm)), and it can not use it for the use which requires an electrode. Moreover, it turned out that the etching by etching liquid is also practically impossible. In addition, it was not able to etch also by other etching liquid.
  • Example 7 the Si sputter conditions of the fifth embodiment are changed.
  • the SiO 2 layer particles of about 80 nm in diameter were dispersed at an average spacing of about 60 nm.
  • the coverage of the ITO film surface with the SiO 2 layer increased to about 50%. From this, it was found that the contact resistance between the Ag paste electrode and the ITO increases by 3 ⁇ , and the etching time also increases by about twice, but it is still within the practical range. It was also confirmed that etching could be performed with other etching solutions.
  • the scratch resistance (Rb / RO) was good with almost no change at 1.0. In addition, the total light transmittance was also improved as high as 90.5%.

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Abstract

L'invention concerne un substrat conducteur transparent qui comprend une couche de film mince conductrice (12) et une couche d'oxyde métallique transparente (13) qui sont stratifiées, dans cet ordre, sur une surface ou les deux surfaces d'un substrat (11), la couche d'oxyde métallique transparente (13) comprenant des particules diffusées (13a). On obtient ainsi un substrat conducteur transparent doté d'un haut niveau de conductivité entre une couche de film mince transparent renfermant de l'oxyde d'étain et d'indium (ITO) ou analogue et une électrode comprenant un métal, une pâte métallique, ou analogue. En outre, le substrat conducteur transparent selon l'invention est hautement transparent, doté d'une bonne performance d'adaptation d'indice, d'une bonne résistance à l'abrasion et d'une bonne aptitude à la gravure.
PCT/JP2014/004104 2013-09-10 2014-08-06 Substrat conducteur transparent et procédé de fabrication de substrat conducteur transparent Ceased WO2015037182A1 (fr)

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WO2017196022A1 (fr) * 2016-05-09 2017-11-16 엘지이노텍(주) Élément électroluminescent
JP2018098024A (ja) * 2016-12-13 2018-06-21 パイオニア株式会社 発光装置
JP2020001232A (ja) * 2018-06-27 2020-01-09 ロック技研工業株式会社 Ｉｔｏフィルム及び透明導電性フィルム
WO2020122150A1 (fr) * 2018-12-12 2020-06-18 日東電工株式会社 Film d'adaptation d'impédance pour absorbeur d'ondes radio, film avec film d'adaptation d'impédance pour absorbeur d'ondes radio, absorbeur d'ondes radio, et stratifié pour absorbeur d'ondes radio
CN116345179A (zh) * 2023-05-31 2023-06-27 鹏城实验室 具有对高频通信信号智能调控功能的透明窗及其制造方法

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TWI738433B (zh) * 2020-01-09 2021-09-01 致伸科技股份有限公司 光源模組以及具有光源模組的電子裝置
JP7434598B2 (ja) * 2020-10-30 2024-02-20 株式会社クレハ 透明導電圧電フィルムおよびタッチパネル
CN114501970A (zh) * 2022-02-22 2022-05-13 深圳市乐工新技术有限公司 电磁屏蔽材料、溅射镀膜装置及电磁屏蔽材料的制作方法

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WO2020122150A1 (fr) * 2018-12-12 2020-06-18 日東電工株式会社 Film d'adaptation d'impédance pour absorbeur d'ondes radio, film avec film d'adaptation d'impédance pour absorbeur d'ondes radio, absorbeur d'ondes radio, et stratifié pour absorbeur d'ondes radio
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CN116345179B (zh) * 2023-05-31 2023-08-18 鹏城实验室 具有对高频通信信号智能调控功能的透明窗及其制造方法

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