WO2020255947A1 - 透明導電性フィルム - Google Patents

透明導電性フィルム Download PDF

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Publication number
WO2020255947A1
WO2020255947A1 PCT/JP2020/023553 JP2020023553W WO2020255947A1 WO 2020255947 A1 WO2020255947 A1 WO 2020255947A1 JP 2020023553 W JP2020023553 W JP 2020023553W WO 2020255947 A1 WO2020255947 A1 WO 2020255947A1
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Prior art keywords
transparent conductive
conductive layer
base material
less
conductive film
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PCT/JP2020/023553
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English (en)
French (fr)
Japanese (ja)
Inventor
才将 西森
智剛 梨木
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日東電工株式会社
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Priority to KR1020217032205A priority Critical patent/KR20220021450A/ko
Publication of WO2020255947A1 publication Critical patent/WO2020255947A1/ja

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    • 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
    • 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

Definitions

  • the present invention relates to a transparent conductive film, and more particularly to a transparent conductive film preferably used for optical applications.
  • a transparent conductive film in which a transparent conductive layer made of indium tin oxide composite oxide (ITO) is formed in a desired electrode pattern has been used for optical applications such as touch panels.
  • ITO indium tin oxide composite oxide
  • Such a transparent conductive film usually includes a base material and a transparent conductive layer in this order.
  • the base material if a relatively thick glass base material is used as the base material, the flexibility is lowered. Therefore, from the viewpoint of improving the flexibility, it is considered to use a polymer film as the base material.
  • ITO indium gallium oxide
  • azudepo crystallization crystallized (also referred to as "azudepo crystallization") at the same time as the film formation. It is known that such azudepo crystallization can lower the surface resistance value of the transparent electrode layer as compared with crystallization after forming an amorphous film once.
  • the film since the film is formed by raising the temperature of the substrate to a high temperature, the polymer film cannot be used from the viewpoint of the heat resistance of the polymer film.
  • Patent Document 1 when thin glass is used as the base material and the transparent electrode layer is crystallized at a high temperature, transparent conductive oxidation occurs due to the difference in linear expansion coefficient between the thin glass and the transparent conductive oxide layer. There is a problem that the material layer curls.
  • the present invention is to provide a transparent conductive film capable of suppressing curling.
  • the present invention [1] includes a glass base material and a transparent conductive layer in this order, the thickness of the glass base material is 150 ⁇ m or less, the transparent conductive layer is crystalline, and the residual stress of the transparent conductive layer. However, it is a transparent conductive film having a value of ⁇ 100 MPa or more and 100 MPa or less.
  • the present invention [2] includes the transparent conductive film according to claim 1, wherein the surface resistance value of the transparent conductive layer is 10 ⁇ / ⁇ or less.
  • the transparent conductive layer contains the transparent conductive film according to the above [1] or [2], which contains a metal oxide.
  • the present invention [4] includes the transparent conductive film according to the above [3], wherein the metal oxide is an indium tin composite oxide.
  • the transparent conductive film of the present invention includes a glass base material and a transparent conductive layer in this order, and the thickness of the glass base material is 150 ⁇ m or less. Therefore, it is excellent in flexibility.
  • the transparent conductive layer is crystalline. Therefore, the surface resistance value can be lowered. Further, in this transparent conductive film, the residual stress of the transparent conductive layer is -100 MPa or more and 100 MPa or less. Therefore, curl can be suppressed.
  • FIG. 1 shows a cross-sectional view of an embodiment of the transparent conductive film of the present invention.
  • the vertical direction of the paper surface is the vertical direction (thickness direction)
  • the upper side of the paper surface is the upper side (one side in the thickness direction)
  • the lower side of the paper surface is the lower side (the other side in the thickness direction).
  • the horizontal direction and the depth direction of the paper surface are plane directions orthogonal to the vertical direction. Specifically, it conforms to the direction arrows in each figure.
  • the transparent conductive film 1 has a film shape (including a sheet shape) having a predetermined thickness, extends in a plane direction orthogonal to the thickness direction, and has a flat upper surface and a flat lower surface.
  • the transparent conductive film 1 is, for example, a component such as a touch panel base material or an electromagnetic wave shield provided in an image display device, that is, it is not an image display device. That is, the transparent conductive film 1 is a component for manufacturing an image display device or the like, and is a device that does not include an image display element such as an OLED module, is distributed as a single component, and can be industrially used.
  • the transparent conductive film 1 includes a glass base material 2 and a transparent conductive layer 3 in this order. More specifically, the transparent conductive film 1 includes a glass base material 2 and a transparent conductive layer 3 arranged on the upper surface (one side in the thickness direction) of the glass base material 2.
  • the thickness of the transparent conductive film 1 is, for example, 200 ⁇ m or less, preferably 150 ⁇ m or less, and for example, 20 ⁇ m or more, preferably 30 ⁇ m or more.
  • the glass base material 2 is a transparent base material for ensuring the mechanical strength of the transparent conductive film 1. That is, the glass base material 2 supports the transparent conductive layer 3.
  • the glass base material 2 has a film shape.
  • the glass base material 2 is arranged on the entire lower surface of the transparent conductive layer 3 so as to come into contact with the lower surface of the transparent conductive layer 3.
  • the glass base material 2 has flexibility and is formed of transparent glass.
  • glass examples include non-alkali glass, soda glass, borosilicate glass, aluminosilicate glass and the like.
  • the thickness of the glass substrate 2 is 150 ⁇ m or less, preferably 120 ⁇ m or less, and more preferably 100 ⁇ m or less. Further, for example, it is 10 ⁇ m or more, preferably 50 ⁇ m or more. When the thickness of the glass base material 2 is not more than the above upper limit, the flexibility is excellent. Further, when the thickness of the glass base material 2 is at least the above lower limit, the mechanical strength is excellent and damage during transportation can be suppressed.
  • the thickness of the glass base material 2 can be measured using a dial gauge (manufactured by PEACOCK, "DG-205").
  • the total light transmittance (JIS K 7375-2008) of the glass base material 2 is, for example, 80% or more, preferably 85% or more.
  • the transparent conductive layer 3 is a transparent layer that is crystalline and exhibits excellent conductivity.
  • the transparent conductive layer 3 has a film shape.
  • the transparent conductive layer 3 is arranged on the entire upper surface of the glass base material 2 so as to be in contact with the upper surface of the glass base material 2.
  • the material of the transparent conductive layer 3 for example, at least one selected from the group consisting of In, Sn, Zn, Ga, Sb, Ti, Si, Zr, Mg, Al, Au, Ag, Cu, Pd, and W.
  • Examples include metal oxides containing the above metals. The metal oxide may be further doped with the metal atoms shown in the above group, if necessary.
  • the transparent conductive layer 3 include indium-containing oxides such as indium tin oxide composite oxide (ITO), and antimony-containing oxides such as antimony tin composite oxide (ATO).
  • ITO indium tin oxide composite oxide
  • ATO antimony tin composite oxide
  • ITO indium tin oxide composite oxide
  • ITO indium tin oxide composite oxide
  • ITO antimony tin composite oxide
  • ITO indium tin oxide composite oxide
  • ATO antimony tin composite oxide
  • the tin oxide (SnO 2 ) content is preferably 0.5% by mass or more, for example, with respect to the total amount of tin oxide and indium oxide (In 2 O 3 ). Is 3% by mass or more, and is, for example, 15% by mass or less, preferably 13% by mass or less.
  • the tin oxide content is at least the above lower limit, the durability of the ITO layer can be further improved.
  • the content of tin oxide is not more than the above upper limit, crystal conversion of the ITO layer can be facilitated, and transparency and stability of resistivity can be improved.
  • the "ITO” in the present specification may be a composite oxide containing at least indium (In) and tin (Sn), and may contain additional components other than these.
  • additional component include metal elements other than In and Sn, and specifically, Zn, Ga, Sb, Ti, Si, Zr, Mg, Al, Au, Ag, Cu, Pd, W and Fe. , Pb, Ni, Nb, Cr, Ga and the like.
  • the transparent conductive layer 3 is crystalline.
  • the transparent conductive layer 3 is crystalline, the surface resistivity described later can be lowered.
  • the transparent conductive film 1 is immersed in hydrochloric acid (20 ° C., concentration 5% by mass) for 15 minutes, then washed with water and dried, and then the surface on the transparent conductive layer 3 side. It can be determined by measuring the resistance between terminals between terminals with respect to about 15 mm. In the transparent conductive film 1 after immersion, washing with water, and drying, when the resistance between terminals between 15 mm is 10 k ⁇ or less, the transparent conductive layer is crystalline, while when the resistance exceeds 10 k ⁇ , the transparent conductivity is transparent. Layer 3 is amorphous.
  • the surface resistivity of the upper surface of the transparent conductive layer 3 is, for example, 30 ⁇ / ⁇ or less, preferably 10 ⁇ / ⁇ or less, and for example, 1 ⁇ / ⁇ or more.
  • the surface resistivity can be measured by the 4-terminal method in accordance with JIS K7194.
  • the transparent conductive film 1 can be suitably used for a large touch panel or the like.
  • the residual stress of the transparent conductive layer 3 is -100 MPa or more, preferably -50 MPa or more, more preferably -30 MPa or more, still more preferably -10 MPa or more, and 100 MPa or less, preferably 60 MPa or less. It is preferably 10 MPa or less, more preferably -5 MPa or less.
  • Negative residual stress means residual stress in the compression direction
  • positive residual stress means residual stress in the extension direction
  • the residual stress can be obtained by the X-ray diffraction method, which will be described in detail in Examples described later.
  • the residual stress can be obtained in accordance with the method for measuring residual stress in JP-A-2017-106124.
  • the residual stress which will be described in detail later, is adjusted to the above range by adjusting the amount of reactive gas introduced later, the film formation pressure described later, and the substrate temperature described later within a predetermined range. ..
  • the thickness of the transparent conductive layer 3 is, for example, 15 nm or more, preferably 30 nm or more, more preferably 100 nm or more, and for example, 300 nm or less, preferably 250 nm or less, more preferably 150 nm or less.
  • the thickness of the transparent conductive layer 3 can be measured by observing the cross section of the transparent conductive film 1 using, for example, a transmission electron microscope. 4. Method for Producing Transparent Conductive Film In order to manufacture the transparent conductive film 1, for example, in the roll-to-roll step, the transparent conductive layer 3 is provided on the upper surface of the glass base material 2.
  • the transparent conductive layer 3 is provided on the upper surface of the glass base material 2 while the long glass base material 2 is sent out from the delivery roll and conveyed to the downstream side in the transport direction, and the conductive film is formed by the winding roll. Take up 1. The details will be described below.
  • a long glass base material 2 wound around a delivery roll is prepared, and the glass base material 2 is conveyed so as to be wound around a take-up roll.
  • the transport speed is, for example, 0.1 m / min or more, preferably 0.2 m / min or more, and for example, 1.0 m / min or less, preferably 0.5 m / min or less.
  • the glass base material 2 can be dust-removed and cleaned by solvent cleaning, ultrasonic cleaning, or the like.
  • the transparent conductive layer 3 is provided on the upper surface of the glass base material 2.
  • the transparent conductive layer 3 is formed on the upper surface of the glass base material 2 by a dry method.
  • the dry method examples include a vacuum deposition method, a sputtering method, an ion plating method, and the like.
  • a sputtering method is used.
  • the transparent conductive layer 3 which is a thin film and has a uniform thickness can be formed.
  • the target and the adherend are placed facing each other in the vacuum chamber, gas is supplied and a voltage is applied from the power source to accelerate the gas ions and irradiate the target with the target surface.
  • the target material is ejected from the surface of the adherend, and the target material is laminated on the surface of the adherend.
  • Examples of the sputtering method include a bipolar sputtering method, an ECR (electron cyclotron resonance) sputtering method, a magnetron sputtering method, and an ion beam sputtering method. Preferred is the magnetron sputtering method.
  • examples of the target material include the above-mentioned metal oxides constituting the transparent conductive layer 3, and preferably ITO.
  • the tin oxide concentration of ITO is, for example, 0.5% by mass or more, preferably 3% by mass or more, and for example, 15% by mass or less, preferably 15% by mass or less. , 13% by mass or less.
  • the gas examples include an inert gas such as Ar. Further, if necessary, a reactive gas such as oxygen gas can be used in combination.
  • the introduction ratio of the reactive gas to the inert gas (hereinafter referred to as the amount of the reactive gas introduced) is, for example, 0.1% by volume or more, preferably 1% by volume or more, and for example, 10% by volume. Hereinafter, it is preferably 3% by volume or less, more preferably less than 2.5% by volume.
  • the atmospheric pressure during sputtering (hereinafter referred to as film formation pressure) is, for example, 1 Pa or less, preferably 0.5 Pa or less, and for example, 0.1 Pa or more, preferably 0.2 Pa or more. is there.
  • the power supply may be, for example, any of a DC power supply, an AC power supply, an MF power supply, and an RF power supply, or may be a combination thereof.
  • the glass base material 2 is preheated to a high temperature before sputtering.
  • the particles forming the transparent conductive layer 3 on the surface of the glass base material 2 are placed in a high energy state and can be crystallized (azudepo crystallization) at the same time as the film formation by sputtering.
  • the heating temperature of the glass substrate 2 (hereinafter referred to as the substrate temperature) is, for example, 350 ° C. or higher, and for example, 600 ° C. or lower, preferably 550 ° C. or lower.
  • the heating time of the glass substrate 2 is, for example, 10 seconds or more, preferably 20 seconds or more, and for example, 120 seconds or less, preferably 60 seconds or less.
  • the above-mentioned reactive gas introduction amount, film formation pressure, and substrate temperature are adjusted to the above-mentioned predetermined range. ..
  • the amount of reactive gas introduced is, for example, 1% by volume or more and 3% by volume or less
  • the film formation pressure is, for example, It is 0.2 Pa or more and 0.5 Pa or less.
  • the amount of reactive gas introduced is, for example, 1.5% by volume or more and less than 2.5% by volume, and the film formation pressure is, for example. , 0.1 Pa or more and 0.5 Pa or less.
  • the amount of reactive gas introduced is, for example, 2.5% by volume or more and 3.5% by volume or less, and the film formation pressure is, for example. , 0.1 Pa or more and 0.2 Pa or less.
  • the residual stress of the transparent conductive layer 3 described above can be adjusted within the predetermined range described above.
  • the transparent conductive layer 3 is cooled.
  • the transparent conductive layer 3 is formed on the upper surface of the glass base material 2, and the transparent conductive film 1 including the glass base material 2 and the transparent conductive layer 3 in this order can be obtained.
  • the thickness of the obtained transparent conductive film 1 is, for example, 2 ⁇ m or more, preferably 20 ⁇ m or more, and for example, 100 ⁇ m or less, preferably 50 ⁇ m or less. 5.
  • the transparent conductive film 1 includes a glass base material 2 and a transparent conductive layer 3 in this order, and the thickness of the glass base material 2 is 150 ⁇ m or less. Therefore, it is excellent in flexibility.
  • the transparent conductive layer 3 is crystalline. Therefore, the surface resistance value can be lowered.
  • the residual stress of the transparent conductive layer 3 is -100 MPa or more and 100 MPa or less.
  • the temperature of the base material is raised in order to sufficiently crystallize the transparent conductive layer 3.
  • the transparent conductive layer 3 may curl due to the difference in linear expansion coefficient between the glass substrate 2 and the transparent conductive layer 3.
  • the transparent conductive film 1 is composed of the glass base material 2 and the transparent conductive layer 3, but an intermediate layer may be interposed between the glass base material 2 and the transparent conductive layer 3.
  • the intermediate layer includes a hard coat layer.
  • the hard coat layer is a protective layer for suppressing the occurrence of scratches on the glass base material 2 when the transparent conductive film 1 is manufactured. Further, the hard coat layer is a scratch-resistant layer for suppressing the occurrence of scratches on the transparent conductive layer 3 when the transparent conductive film 1 is laminated.
  • the hard coat layer is formed from, for example, a hard coat composition.
  • the hard coat composition contains a resin component.
  • the resin component examples include curable resin, thermoplastic resin (for example, polyolefin resin) and the like.
  • the hard coat composition can also contain particles.
  • the particles include organic particles such as crosslinked acrylic particles and inorganic particles such as silica particles.
  • the thickness of the hard coat layer is, for example, 0.1 ⁇ m or more, preferably 0.5 ⁇ m or more, and for example, 10 ⁇ m or less, preferably 3 ⁇ m or less.
  • the thickness of the hard coat layer can be calculated, for example, based on the wavelength of the interference spectrum observed using an instantaneous multi-photometric system (for example, "MCPD2000" manufactured by Otsuka Electronics Co., Ltd.).
  • an optical adjustment layer can be mentioned.
  • the optical adjustment layer is transparent in order to ensure excellent transparency of the transparent conductive film 1 while suppressing the pattern visibility of the transparent conductive layer 3 and suppressing reflection at the interface in the transparent conductive film 1.
  • This is a layer for adjusting the optical properties (for example, refractive index) of the conductive film 1.
  • the optical adjustment layer is formed from, for example, an optical adjustment composition.
  • the optical adjustment composition contains the above resin component and the above particles.
  • the thickness of the optical adjustment layer is, for example, 5 nm or more, preferably 10 nm or more, and for example, 200 nm or less, preferably 100 nm or less.
  • the thickness of the optical adjustment layer can be calculated, for example, based on the wavelength of the interference spectrum observed using an instantaneous multi-photometric system.
  • the transparent conductive film 1 may have a hard coat layer or an optical adjustment layer interposed between the glass base material 2 and the transparent conductive layer 3, and the transparent conductive film 1 may be formed with the glass base material 2.
  • a hard coat layer and an optical adjustment layer may be interposed between the transparent conductive layer 3.
  • the transparent conductive film 1 has an optical adjustment layer interposed between the glass base material 2 and the transparent conductive layer 3, and more preferably, the transparent conductive film 1 is the glass base material 2 and the transparent conductive layer 3.
  • the transparent conductive film 1 is composed of the glass base material 2 and the transparent conductive layer 3 without interposing a hard coat layer and an optical adjustment layer between the two.
  • the transparent conductive film 1 uses the glass base material 2 as the base material, the space between the glass base material 2 and the transparent conductive layer 3 is compared with the case where the polymer film is used as the base material. It has excellent adhesion and permeability without the intervention of an intermediate layer (particularly a hard coat layer).
  • Example 1 As a glass base material, a long transparent glass base material (thickness 50 ⁇ m, manufactured by Nippon Electric Glass Co., Ltd., “G-Leaf”) wound in a roll shape was prepared.
  • This transparent glass base material was set on a delivery roll, delivered at a transport speed of 0.27 m / min, passed through a sputtering device (target portion), and wound on a take-up roll.
  • An ITO layer transparent conductive layer
  • An ITO layer transparent conductive layer having a thickness of 130 nm was formed on the upper surface of the glass substrate by the DC sputtering method.
  • Sputtering was carried out in a vacuum atmosphere at an atmospheric pressure (deposition pressure) of 0.3 Pa into which 98% of argon gas and 2% of oxygen gas (that is, 2% by volume of oxygen gas introduced) were introduced.
  • the discharge output was 3 kW.
  • As the target a sintered body of 87.5% by mass of indium oxide and 12.5% by mass of tin oxide was used.
  • an infrared heater heating unit
  • the heater temperature base material temperature
  • the glass base material was heated for 25 seconds.
  • Example 2 to Example 4 and Comparative Example 1 to Comparative Example 4 A transparent conductive film was produced in the same manner as in Example 1 except that the substrate temperature, the film forming pressure, and the amount of oxygen gas introduced were changed according to Table 1. 2.
  • the integrated time (exposure time) at each measurement angle was 100 seconds.
  • the crystal lattice spacing d of the ITO film is calculated from the peak (peak of the (622) plane of ITO) angle 2 ⁇ of the obtained diffraction image and the wavelength ⁇ of the X-ray source, and the lattice strain ⁇ is calculated based on d. Calculated.
  • the following formula (1) and the following formula (2) were used in the calculation.
  • d 0 is a value obtained from the ICDD (The International Center for Diffraction Data) database.
  • the above X-ray diffraction measurement was performed for each of the angles ⁇ formed by the film surface normal and the ITO crystal plane normal at 45 °, 50 °, 55 °, 60 °, 65 °, 70 °, 77 °, and 90 °. This was carried out and the lattice strain ⁇ at each ⁇ was calculated.
  • the angle ⁇ formed by the film surface normal and the ITO crystal plane normal was adjusted by rotating the sample around the TD direction as the center of rotation.
  • the residual stress ⁇ in the in-plane direction of the ITO film was obtained by the following equation (3) from the slope of a straight line plotting the relationship between sin 2 ⁇ and the lattice strain ⁇ .
  • E is the Young's modulus of ITO (116 GPa) and ⁇ is the Poisson's ratio (0.35).
  • the obtained residual stress is shown in Table 1.
  • Table 1 Amount of curl First, the transparent conductive film was cut into a width of 100 mm and a length of 100 mm, and the cut transparent conductive film was placed on a smooth table. Next, the distance at which the vertices of each corner of the cut transparent conductive film were floating from the table was measured, and the average value of the four vertices was calculated and used as the curl amount. The results are shown in Table 1.
  • the transparent conductive film of the present invention is suitably used in optical applications.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Non-Insulated Conductors (AREA)
  • Laminated Bodies (AREA)
  • Physical Vapour Deposition (AREA)
PCT/JP2020/023553 2019-06-21 2020-06-16 透明導電性フィルム WO2020255947A1 (ja)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013115125A1 (ja) * 2012-02-02 2013-08-08 株式会社カネカ 透明電極付き基板の製造方法

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JP5903820B2 (ja) 2011-09-28 2016-04-13 凸版印刷株式会社 透明導電性フィルムの製造方法及びタッチパネルの製造方法
KR20170008196A (ko) 2014-05-20 2017-01-23 닛토덴코 가부시키가이샤 투명 도전성 필름 및 그 제조 방법
JP6278241B2 (ja) 2014-08-29 2018-02-14 日本電気硝子株式会社 膜付きガラス基板の製造方法

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WO2013115125A1 (ja) * 2012-02-02 2013-08-08 株式会社カネカ 透明電極付き基板の製造方法

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