WO2022070610A1 - Film conducteur transparent - Google Patents

Film conducteur transparent Download PDF

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Publication number
WO2022070610A1
WO2022070610A1 PCT/JP2021/029154 JP2021029154W WO2022070610A1 WO 2022070610 A1 WO2022070610 A1 WO 2022070610A1 JP 2021029154 W JP2021029154 W JP 2021029154W WO 2022070610 A1 WO2022070610 A1 WO 2022070610A1
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WIPO (PCT)
Prior art keywords
transparent conductive
conductive film
film
pen
sliding
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PCT/JP2021/029154
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English (en)
Japanese (ja)
Inventor
央 多々見
Original Assignee
東洋紡株式会社
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Application filed by 東洋紡株式会社 filed Critical 東洋紡株式会社
Priority to CN202180045394.0A priority Critical patent/CN115776942A/zh
Priority to JP2021549298A priority patent/JPWO2022070610A1/ja
Publication of WO2022070610A1 publication Critical patent/WO2022070610A1/fr

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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
    • B32B7/025—Electric or magnetic properties
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • 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

Definitions

  • the present invention relates to a transparent conductive film in which a transparent conductive film of a crystalline indium-tin composite oxide is laminated on a transparent plastic film base material, particularly a pen sliding durability when used for a resistance film type touch panel. It relates to a transparent conductive film having excellent heavy pressure durability and anti-glare property.
  • a transparent conductive film in which a transparent and low-resistance thin film is laminated on a transparent plastic base material is used for applications that utilize the conductivity, for example, flat panel displays such as liquid crystal displays and electroluminescence (EL) displays.
  • flat panel displays such as liquid crystal displays and electroluminescence (EL) displays.
  • EL electroluminescence
  • the transparent conductive thin film may be broken such as cracks and peeling.
  • a transparent conductive film having both excellent pen sliding durability and excellent pen heavy pressure durability.
  • anti-glare property is also required in order to prevent reflection of fluorescent lamps and the like on the image of the touch panel.
  • the conventional transparent conductive film realizes a transparent conductive film having excellent pen sliding durability by controlling the crystallinity of the indium-tin composite oxide.
  • the conventional transparent conductive film was insufficient when the pen heavy pressure durability test described later was carried out.
  • an object of the present invention is transparency that is excellent in pen sliding durability when used for a touch panel, is also excellent in pen heavy pressure durability, and can provide further excellent anti-glare property.
  • the purpose is to provide a conductive film.
  • the present invention has been made in view of the above circumstances, and the transparent conductive film of the present invention, which has been able to solve the above problems, has the following configuration.
  • 1. A transparent conductive film in which a transparent conductive film of an indium-tin composite oxide is laminated on one surface of a transparent plastic film substrate, and is a transparent conductive film of the transparent conductive film according to the following pen sliding durability test.
  • the ON resistance is 10 k ⁇ or less
  • the increase rate of the surface resistance value of the transparent conductive film of the transparent conductive film by the following pen heavy pressure test is 1.5 or less
  • the transparent conductive film on the transparent plastic film substrate A transparent conductive film having a 60 ° mirror surface gloss of 50% or more and 120% or less on the opposite surface to the side.
  • the transparent conductive film according to the present invention is used as one panel plate, and the other panel plate is an indium-tin composite oxide thin film having a thickness of 20 nm by a sputtering method on a glass substrate (tin oxide content: 10% by mass).
  • a transparent conductive thin film made of is used.
  • the two panel plates are arranged via epoxy beads having a diameter of 30 ⁇ m so that the transparent conductive thin films face each other, and the film side panel plate and the glass side panel plate are attached with double-sided tape having a thickness of 170 ⁇ m. , Make a touch panel.
  • a load of 2.5 N is applied to a polyacetal pen (tip shape: 0.8 mmR), and a linear sliding test of 180,000 reciprocations is performed on the touch panel.
  • a pen load is applied to the transparent conductive film surface according to the present invention.
  • the sliding distance is 30 mm and the sliding speed is 180 mm / sec.
  • the ON resistance resistance value when the movable electrode (film electrode) and the fixed electrode come into contact with each other
  • the transparent conductive film according to the present invention cut to 50 mm ⁇ 50 mm is used as one panel plate, and the other panel plate is an indium-tin oxide composite oxide thin film (tin oxide) having a thickness of 20 nm on a glass substrate by a sputtering method.
  • tin oxide indium-tin oxide composite oxide thin film
  • a transparent conductive thin film having a content of 10% by mass is used.
  • the two panel plates are arranged via epoxy beads having a diameter of 30 ⁇ m so that the transparent conductive thin films face each other, and the thickness is adjusted to 120 ⁇ m with double-sided tape.
  • a touch panel was made by pasting a board.
  • a load of 35 N is applied to a position 2.0 mm from the end of the double-sided tape with a pen made of polyacetal (tip shape 0.8 mmR), and linear sliding is performed 10 times (5 reciprocations) in parallel with the double-sided tape.
  • a pen load is applied to the transparent conductive film surface according to the present invention.
  • the sliding distance is 30 mm and the sliding speed is 20 mm / sec. Slide in a position where there are no epoxy beads.
  • the transparent conductive film is removed, the surface resistance (4 terminal method) at any 5 points of the sliding part is measured, and the average value is calculated.
  • the crystal grain size of the transparent conductive film of the indium-tin composite oxide is 10 to 100 nm, the crystallinity of the transparent conductive film of the indium-tin composite oxide is 20 to 80%, and the crystal size of the transparent conductive film of the indium-tin oxide is 20 to 80%.
  • the transparent conductive film contains 0.5 to 10% by mass of tin oxide, the thickness of the transparent conductive film of the indium-tin composite oxide is 10 to 30 nm, and the thickness of the transparent conductive film of the indium-tin composite oxide is three-dimensional.
  • the surface roughness SRa is X
  • X is 1 to 100 nm
  • the three-dimensional surface roughness SRa on the transparent conductive film substrate opposite to the transparent conductive film side is Y
  • the transparent conductive film according to the first item which has a diameter of 70 to 270 nm. 3. 3.
  • the transparent conductive film according to any one of the above 1 to 4 which has a curable resin layer between a transparent conductive film of an indium-tin composite oxide and a transparent plastic film substrate.
  • the present invention it is possible to provide a transparent conductive film having both excellent pen sliding durability and excellent pen heavy pressure durability, and capable of providing further excellent anti-glare property.
  • the obtained transparent conductive film is extremely useful for applications such as a resistance film type touch panel.
  • the transparent conductive film of the present invention is a transparent conductive film in which a transparent conductive film of an indium-tin composite oxide is laminated on one surface of a transparent plastic film base material, and the following pen sliding durability test is performed.
  • the ON resistance of the transparent conductive film of the transparent conductive film is 10 k ⁇ or less, and the increase rate of the surface resistance value of the transparent conductive film of the transparent conductive film by the following pen heavy pressure test is 1.5 or less, and further transparent. It is preferable that the 60 ° mirror surface gloss of the surface of the plastic film substrate opposite to the transparent conductive film side is 50% or more and 120% or less.
  • the transparent conductive film according to the present invention is used as one panel plate, and the other panel plate is an indium-tin composite oxide thin film having a thickness of 20 nm by a sputtering method on a glass substrate (tin oxide content: 10% by mass).
  • a transparent conductive thin film made of is used.
  • the two panel plates are arranged via epoxy beads having a diameter of 30 ⁇ m so that the transparent conductive thin films face each other, and the film side panel plate and the glass side panel plate are attached with double-sided tape having a thickness of 170 ⁇ m. , Made a touch panel.
  • a load of 2.5 N was applied to a polyacetal pen (tip shape: 0.8 mmR), and a linear sliding test of 180,000 reciprocations was performed on the touch panel.
  • a pen load is applied to the transparent conductive film surface according to the present invention.
  • the sliding distance was 30 mm and the sliding speed was 180 mm / sec.
  • the ON resistance resistance value when the movable electrode (film electrode) and the fixed electrode came into contact with each other
  • a transparent conductive film obtained by cutting the transparent conductive film according to the present invention into a size of 50 mm ⁇ 50 mm is used as one panel plate, and the other panel plate is an indium-tin composite oxide having a thickness of 20 nm by a sputtering method on a glass substrate.
  • a transparent conductive thin film composed of a thin film (tin oxide content: 10% by mass) was used.
  • the two panel plates are arranged via epoxy beads having a diameter of 30 ⁇ m so that the transparent conductive thin films face each other, and the thickness is adjusted to 120 ⁇ m with double-sided tape.
  • a touch panel was made by pasting a board.
  • a load of 35 N is applied to a position 2.0 mm from the end of the double-sided tape with a pen made of polyacetal (tip shape 0.8 mmR), and linear sliding is performed 10 times (5 reciprocations) in parallel with the double-sided tape.
  • a pen load is applied to the transparent conductive film surface according to the present invention.
  • the sliding distance is 30 mm and the sliding speed is 20 mm / sec.
  • sliding is performed at a position where there are no epoxy beads.
  • the transparent conductive film is removed, the surface resistance (4 terminal method) at any 5 points of the sliding part is measured, and the average value is calculated.
  • the rate of increase in the surface resistance value is calculated by dividing the average value of the surface resistance values of the sliding portion by the surface resistance value of the non-sliding portion (measured by the 4-terminal method).
  • the transparent conductive film of the present invention is excellent in pen sliding durability and pen heavy pressure durability. Pen sliding durability and pen heavy pressure durability are contradictory properties.
  • the pen sliding durability will be described.
  • the transparent conductive film of indium-tin composite oxide having excellent pen sliding durability has a high crystallinity of the transparent conductive film and a large crystal grain size.
  • the degree of crystallinity and the crystal grain size will be described.
  • a high degree of crystallinity means a high proportion of crystals.
  • a large crystal grain size means a large circular or polygonal region observed under a transmission electron microscope.
  • a transparent conductive film with a high degree of crystallinity has a high proportion of hard crystals, and a transparent conductive film having a large crystal grain size has a large strain around the crystal grains. Excellent for.
  • the pen heavy pressure durability will be described.
  • a transparent conductive film of an indium-tin composite oxide having excellent pen heavy pressure durability needs to have a low crystallinity of the transparent conductive film, a small crystal grain size, and a small three-dimensional surface roughness of the transparent conductive film. be. The three-dimensional surface roughness will be described later.
  • a transparent conductive film having a low crystallinity has a high proportion of soft amorphous, and a transparent conductive film having a small crystal grain size has a small strain around the crystal grains.
  • the pen sliding durability and the pen heavy pressure durability are contradictory properties.
  • the pen sliding durability and the pen heavy pressure durability can be achieved at the same time by controlling the crystallinity and the crystal grain size of the transparent conductive film. A transparent conductive film having a transparent conductive film that achieves both pen sliding durability and pen heavy pressure durability will be described.
  • the ON resistance of the transparent conductive film of the transparent conductive film according to the pen sliding durability test is 10 k ⁇ or less, cracks, peeling, wear, etc. are suppressed with respect to the transparent conductive film even if continuous input is made to the touch panel with a pen. It is preferable because it is used.
  • the ON resistance may be 9.5 k ⁇ or less, more preferably 5 k ⁇ or less.
  • the ON resistance is 3 k ⁇ or less, may be 1.5 k ⁇ or less, and is preferably 1 k ⁇ or less. If the ON resistance is 0 k ⁇ , the pen sliding durability is very excellent, and in the present invention, the ON resistance can be 0 k ⁇ .
  • the ON resistance may be, for example, 3 k ⁇ or more, or 5 k ⁇ or more.
  • these upper and lower limits may be combined as appropriate.
  • the increase rate of the surface resistance value of the transparent conductive film of the transparent conductive film by the pen heavy pressure test is 1.5 or less.
  • the rate of increase in the surface resistance value is 1.2 or less, and particularly preferably 1.0 (no increase).
  • the rate of increase in the surface resistance value of the transparent conductive film according to the present invention is preferably 1.0 or more.
  • the ON resistance of the transparent conductive film of the transparent conductive film by the pen sliding durability test is 0.05 k ⁇ or more and 9.5 k ⁇ or less, and the transparent conductive film by the pen heavy pressure (durability) test.
  • the rate of increase in the surface resistance value of the transparent conductive film is 1.0 or more and 1.5 or less.
  • pen sliding durability and pen heavy pressure durability are usually contradictory properties. In the present invention, these two durability can be well-balanced within such a range.
  • cracks, peeling, wear, etc. can be suppressed against the transparent conductive film, and in addition, excellent durability is achieved against loads caused by pen sliding and pen heavy pressure. Can be shown.
  • the numerical range the range and the value described in the present specification can be selected.
  • the 60 ° mirror surface gloss on the transparent conductive film substrate opposite to the transparent conductive film side is 50% or more and 120% or less.
  • excellent antiglare property can be provided.
  • the 60 ° mirror surface gloss on the surface opposite to the transparent conductive film side is 100% or less.
  • the 60 ° mirror surface gloss on the surface opposite to the transparent conductive film side is 80% or less.
  • the sharpness of the image on the touch panel was judged by the total of the transmission image sharpness of the transparent conductive film.
  • the transmission image sharpness of the transparent conductive film was measured at a comb width of 0.125 mm, 0.25 mm, 0.5 mm, 1.0 mm, and 2.0 mm, and the transmission image sharpness of the transparent conductive film of each comb width was measured. When the total is 50% or more, the sharpness of the image on the touch panel is good, which is desirable.
  • "comb width” means an optical comb width which conforms to JIS-K7105.
  • the crystal grain size of the transparent conductive film of the indium-tin composite oxide is 10 to 100 nm, and the crystallinity of the transparent conductive film of the indium-tin composite oxide is 20 to 80%. It is preferable to have.
  • the crystal grain size of the transparent conductive film of the indium-tin composite oxide is 10 nm or more, the transparent conductive film becomes moderately hard due to the strain around the crystal grains of the transparent conductive film, so that the pen sliding durability is excellent.
  • the crystal grain size of the transparent conductive film of the indium-tin composite oxide is 30 nm or more.
  • the crystal grain size of the transparent conductive film of the indium-tin composite oxide is 100 nm or less, the transparent conductive film is not too hard due to the strain around the crystal grains of the transparent conductive film, so that the pen heavy pressure durability is improved. It is preferable because it is excellent. More preferably, the crystal grain size of the transparent conductive film of the indium-tin composite oxide is 90 nm or less. In one embodiment, the crystal grain size of the transparent conductive film of the indium-tin composite oxide is 30 nm or more and 95 nm or less, for example, 40 nm or more and 90 nm or less.
  • the crystallinity of the transparent conductive film of the indium-tin composite oxide is 20% or more, it becomes moderately hard due to the hard crystals occupying the transparent conductive film, and the pen sliding durability is excellent, which is preferable. More preferably, the crystallinity of the transparent conductive film of the indium-tin composite oxide is 25% or more. On the other hand, when the crystallinity of the transparent conductive film of the indium-tin composite oxide is 80% or less, the amount of hard crystals contained is large, but the transparent conductive film is not too hard, so that the pen heavy pressure durability is excellent. Therefore, it is preferable. In one embodiment, the crystallinity of the transparent conductive film of the indium-tin composite oxide is 25% or more and 78% or less, for example, 25% or more and 76% or less.
  • the transparent conductive film in the present invention preferably has an X of 1 to 100 nm, where X is the three-dimensional surface roughness SRa of the transparent conductive film.
  • X is 1 to 100 nm, the surface protrusions of the transparent conductive film are small, so that the amount of deformation of the surface protrusions is small when the pen heavy pressure test is performed, crack generation of the transparent conductive film is suppressed, and the transparent conductivity is further suppressed. Since the film has some surface protrusions, it is preferable because the film winding property can be maintained. More preferably, X is 1 to 80 nm. More preferably, X is 1 to 65 nm.
  • the transparent conductive film in the present invention is made of an indium-tin composite oxide, and preferably contains 0.5% by mass or more and 10% by mass or less of tin oxide.
  • Tin oxide in the indium-tin composite oxide corresponds to an impurity for indium oxide.
  • the inclusion of tin oxide impurities increases the melting point of the indium-tin composite oxide. That is, since the impurity content of tin oxide acts in the direction of inhibiting crystallization, it is an important factor having a strong correlation with crystallinity such as crystal grain size and crystallinity.
  • tin oxide is contained in an amount of 0.5% by mass or more, the surface resistance of the transparent conductive film becomes a practical level, which is preferable.
  • the tin oxide content is 1% by mass or more, and particularly preferably 2% by mass or more.
  • the tin oxide content is more preferably 8% by mass or less, further preferably 6% by mass or less, and particularly preferably 4% by mass or less.
  • the surface resistance of the transparent conductive film of the present invention is preferably 50 to 900 ⁇ / ⁇ , more preferably 50 to 600 ⁇ / ⁇ .
  • the thickness of the transparent conductive film is preferably 10 nm or more and 30 nm or less.
  • the thickness of the transparent conductive film is an important factor having a strong correlation with crystallinity such as crystal grain size and crystallinity.
  • the transparent conductive film does not have too many amorphous substances, and it is easy to give an appropriate crystal grain size and crystallinity to make a semi-crystalline state, which will be described later, and as a result, the pen slides. Durability is maintained and is preferable.
  • the thickness of the transparent conductive film is more preferably 13 nm or more, more preferably 16 nm or more.
  • the thickness of the transparent conductive film is 30 nm or less, the crystal grain size of the transparent conductive film is not too large, the crystallinity is not too high, the semi-crystalline state is easily maintained, and the pen heavy pressure durability is maintained. It is preferable that the sex is maintained. It is more preferably 28 nm or less, still more preferably 25 nm or less.
  • the transparent conductive film in the present invention has excellent antiglare when Y is 70 to 270 nm, where Y is the three-dimensional surface roughness SRa of the surface of the transparent plastic film substrate opposite to the transparent conductive film side. It is desirable because it can provide sex. The larger the value of Y, the better the anti-glare property. More preferably, Y is 90 nm or more. More preferably, Y is 130 nm or more. Further, when the value of Y is 270 nm or less, the sharpness of the image on the touch panel is good, which is preferable.
  • the transparent conductive film in the present invention does not peel off even when the adhesion test (JIS K5600-5-6: 1999) is carried out on the transparent conductive film surface.
  • the transparent conductive film that does not peel off in the adhesion test is a transparent conductive film that is in close contact with a layer that is in contact with the transparent conductive film, such as a transparent plastic substrate or a curable resin layer. Even if continuous input is performed, cracks, peeling, wear, etc. are suppressed on the transparent conductive film, and even if a stronger force than expected for normal use is applied, cracks, peeling, etc. are suppressed on the transparent conductive film. preferable.
  • the transparent conductive film in the present invention is cracked or peeled when a bending resistance test (JIS K5600-5: 1: 1999) is performed on the transparent conductive film side of the transparent conductive film and the bent portion is observed with a 10-fold loupe.
  • a bending resistance test JIS K5600-5: 1: 1999
  • the mandrel diameter at which this occurs is smaller than 20 mm.
  • the layer in contact with the transparent conductive film does not crack when the pen heavy pressure test is performed, and the transparent conductive film does not crack, which is preferable. More preferably, it is 18 mm or less.
  • the value of the bending resistance test may be 1 mm or more, for example, 8 mm or more and 10 mm or more.
  • the value of the bending resistance test is 13 mm or more, and may be 15 mm or more.
  • the layer in contact with the transparent conductive film does not crack when the pen heavy pressure test is performed, and the transparent conductive film does not crack, which is preferable. Further, it becomes possible to provide a transparent conductive film having both excellent pen sliding durability and excellent pen heavy pressure durability.
  • the thickness of the transparent plastic film base material is preferably in the range of 100 to 250 ⁇ m, more preferably 130 to 220 ⁇ m.
  • the thickness of the plastic film is 100 ⁇ m or more, the mechanical strength is maintained, the deformation with respect to the pen input when used for a touch panel is small, and the pen sliding durability and the pen heavy pressure durability are excellent, which is preferable.
  • the thickness is 250 ⁇ m or less, when it is used for a touch panel, it is not necessary to particularly increase the load for positioning by pen input, which is preferable.
  • the transparent conductive film in the present invention preferably has a curable resin layer between the transparent conductive film and the plastic film base material.
  • the presence of the curable resin layer can increase the adhesion of the transparent conductive film and disperse the force applied to the transparent conductive film, so that cracks, peeling, wear, etc. are suppressed with respect to the transparent conductive film in the pen sliding test. Further, it is preferable because cracks and peeling are suppressed with respect to the transparent conductive film in the pen heavy pressure test.
  • the crystallinity of the transparent conductive film in the present invention is neither too high nor too low (such crystallinity is referred to as semi-crystalline or semi-crystalline). It is very difficult to make the transparent conductive film stable and semi-crystalline. This is because the state of being stopped in the middle of the rapid phase change from amorphous to crystalline is semi-crystalline.
  • the production method for obtaining the transparent conductive film of the present invention is not particularly limited, and for example, the following production methods can be preferably exemplified.
  • the sputtering method is preferably used as a method for forming a transparent conductive film of a crystalline indium-tin composite oxide on at least one surface of a transparent plastic film substrate.
  • the hydrogen atom-containing gas (hydrogen, ammonia, hydrogen + argon mixed gas, etc., which is not particularly limited as long as it contains hydrogen atoms, but water is excluded) is described below by the mass flow controller in the film forming atmosphere.
  • Indium-tin composite oxide using a sintered target of indium-tin composite oxide containing 0.5 to 10% by mass of tin oxide, with the film temperature during sputtering set to 0 ° C. or lower.
  • the thickness of the transparent conductive film is adjusted to be 10 to 30 nm, and the transparent conductive film is placed on a transparent plastic film having a three-dimensional surface roughness SRa of the transparent conductive film of indium-tin composite oxide of 1 to 100 nm.
  • the hydrogen atom-containing gas has the effect of inhibiting the crystallization of the transparent conductive film in the film forming atmosphere during sputtering.
  • the value of (hydrogen gas flow rate) ⁇ (inert gas flow rate + hydrogen gas flow rate) ⁇ 100 (may be simply described as hydrogen concentration) is 0.01 to 3. It is desirable that it is 0.00%.
  • the hydrogen concentration is, for example, 0.01% or more and 2.00%, and may be 0.01% or more and 1.00% or less. When the hydrogen concentration is within such a range, it can contribute to leading to good results in both the pen sliding durability test ON resistance value and the pen heavy pressure durability test, for example.
  • the inert gas examples include helium, neon, argon, krypton, xenon and the like.
  • a gas outlet is arranged so that the hydrogen atom-containing gas can be sprayed uniformly in the direction perpendicular to the longitudinal direction of the film roll when the hydrogen atom-containing gas is precisely flowed in the film formation atmosphere by the mass flow controller. By doing so, it is difficult to form a transparent conductive film in which high and low crystalline parts are mixed, and it is easy to obtain a uniform semi-crystalline transparent conductive film.
  • the center value (the value between the maximum value and the minimum value) of the ratio of the water pressure to the inert gas in the film formation atmosphere at the time of sputtering onto a film roll is 1.0 ⁇ 10.
  • Controlled to -4 to 2.0 ⁇ 10 -3 and the difference between the maximum and minimum values of the ratio of the water pressure to the inert gas in the film formation atmosphere during sputtering from the start of film formation to the end of film formation.
  • the uniformity of the crystallinity of the transparent conductive film is maintained over the entire length of the film.
  • the amount of water released from the film when forming a transparent conductive film is small, such as the following bombarding process and the following limitation of the height difference of the unevenness of the end face of the film roll, so that the amount of water is uniform over the entire length of the film. If it is released, precise control of the water content becomes unnecessary, which is preferable.
  • the central value of the ratio of the water pressure to the inert gas depends somewhat on the content of tin oxide in the transparent conductive film of the indium-tin composite oxide and the thickness of the transparent conductive film.
  • the center value of the ratio of the water pressure to the inert gas is set low within the above range. It is desirable to do.
  • the center value of the ratio of the water pressure to the inert gas is within the above range. It is desirable to set it higher.
  • FIG. 5 shows a schematic diagram of an example of a sputtering apparatus preferably used in the present invention, in which the traveling film 1 partially contacts the surface of the center roll 2 and travels.
  • An indium-tin sputtering target 4 is installed via the chimney 3, and a thin film of indium-tin composite oxide is deposited and laminated on the surface of the film 1 running on the center roll 2.
  • the temperature of the center roll 2 is controlled by a temperature controller (not shown).
  • the film temperature is 0 ° C. or lower, the release of impurity gases such as water and organic gas from the film, which disperses the crystallinity of the transparent conductive film, can be suppressed, so that the film is transparent from the start of film formation to the end of film formation. It is preferable because the crystallinity of the conductive film is easily made uniform.
  • the center value of the ratio of the water pressure to the inert gas in the film forming atmosphere during sputtering (the value between the maximum value and the minimum value) is 1.0 ⁇ 10 -4 to 2 It is desirable that it is 0.0 ⁇ 10 -3 .
  • the ratio of the water pressure to the inert gas in the film forming atmosphere during sputtering is in the above range, it is desirable because the inhibition of the crystallinity of the transparent conductive film by the hydrogen atom-containing gas effectively acts.
  • the main purpose of this manufacturing method is to eliminate the influence of water-induced crystallinity, which is a factor that disperses the crystallinity of the transparent conductive film, as much as possible, and to control the crystallinity with a hydrogen-containing gas.
  • the first reason is that when a film is formed on a plastic film by sputtering, the film is heated and water is released from the film, so that the amount of water in the film formation atmosphere increases and the ultimate vacuum is measured. Since it increases more than the amount of water at the time, it is more accurate to express it with the amount of water at the time of film formation than to express it with the degree of ultimate vacuum.
  • the second reason is the case of a device that puts in a large amount of transparent plastic film.
  • the film is charged in the form of a film roll.
  • water easily drains from the outer layer of the roll, but water does not easily drain from the inner layer of the roll.
  • the film roll is stopped, but the film roll runs during film formation, and the inner layer of the film roll containing a large amount of water is unwound, so that the moisture in the film formation atmosphere This is because the amount increases and the amount of water increases from the amount of water when the ultimate vacuum degree is measured.
  • it when controlling the amount of water in the film-forming atmosphere, it is possible to preferably cope with it by observing the ratio of the water pressure to the inert gas in the film-forming atmosphere during sputtering.
  • the bombarding step is to generate plasma by applying a voltage and discharging with only an inert gas such as argon gas or a mixed gas of a reactive gas such as oxygen and an inert gas flowing. .. Specifically, it is desirable to bombard the film by RF sputtering with a SUS target or the like. Since the film is exposed to plasma by the bombarding process, water and organic components are released from the film, and the amount of water and organic components released from the film when forming a transparent conductive film is reduced, so that the film is formed from the start of film formation. It is preferable because the crystallinity of the transparent conductive film up to the end is easily made uniform. Further, since the layer in contact with the transparent conductive film is activated by the bombard process, the adhesion of the transparent conductive film is improved, which is desirable because the pen sliding durability and the pen heavy pressure durability are improved.
  • an inert gas such as argon gas or a mixed gas of a reactive gas such as oxygen and an inert gas flowing. .
  • the film roll for forming a transparent conductive film preferably has a height difference of 10 mm or less between the most convex portion and the most concave portion on the roll end face. If it is 10 mm or less, the crystal of the transparent conductive film from the start of film formation to the end of film formation will be less uneven in the way water and organic components are discharged from the end face of the film when the film roll is put into the sputtering apparatus. It is preferable because the properties are easily made uniform.
  • the method of forming a transparent conductive film of a crystalline indium-tin composite oxide on at least one surface of a transparent plastic film substrate it is desirable to introduce oxygen gas during sputtering.
  • oxygen gas is introduced during sputtering, there is no problem due to lack of oxygen in the transparent conductive film of the indium-tin composite oxide, the surface resistance of the transparent conductive film is low, and the total light transmittance is high, which is preferable. Therefore, it is desirable to introduce oxygen gas during sputtering in order to bring the surface resistance and total light transmittance of the transparent conductive film to a practical level.
  • the total light transmittance of the transparent conductive film of the present invention is preferably 70 to 95%.
  • the transparent conductive film of the present invention is formed by laminating a transparent conductive film of an indium-tin composite oxide on a transparent plastic film substrate, and then in an atmosphere containing oxygen at 80 to 200 ° C. and 0.1 to 1. It is desirable that it has been heat-treated for 12 hours. When the temperature is 80 ° C. or higher, it is easy to take measures to slightly increase the crystallinity so as to make the pen semi-crystalline state, and the pen sliding durability is improved, which is preferable. When the temperature is 200 ° C. or lower, the flatness of the transparent plastic film is ensured, which is preferable.
  • the transparent plastic film base material used in the present invention is a film obtained by melt-extruding or solution-extruding an organic polymer into a film, and if necessary, stretching, cooling, and heat-fixing in the longitudinal direction and / or the width direction.
  • the organic polymers include polyethylene, polypropylene, polyethylene terephthalate, polyethylene-2,6-naphthalate, polypropylene terephthalate, polybutylene terephthalate, nylon 6, nylon 4, nylon 66, nylon 12, polyimide, polyamideimide, and polyether.
  • organic polymers polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate, polyethylene-2,6-naphthalate, syndiotactic polystyrene, norbornene-based polymer, polycarbonate, polyarylate and the like are suitable. Further, these organic polymers may be copolymerized with a small amount of a monomer of another organic polymer, or may be blended with another organic polymer.
  • the transparent plastic film substrate used in the present invention has surface activity of the film such as corona discharge treatment, glow discharge treatment, flame treatment, ultraviolet irradiation treatment, electron beam irradiation treatment, ozone treatment, etc., as long as the object of the present invention is not impaired. It may be subjected to a chemical discharge treatment.
  • the transparent conductive film adheres strongly to the curable resin layer and the force applied to the transparent conductive film can be dispersed. It is preferable because cracks, peeling, abrasion, etc. are suppressed with respect to the film, and cracks, peeling, etc. are suppressed with respect to the transparent conductive film in the pen heavy pressure test. Further, when a transparent conductive film is formed on the surface of the curable resin layer having an uneven surface, the true contact area when the transparent conductive thin film comes into contact with the glass during the pen sliding test is reduced, so that the glass surface is reduced.
  • the slipperiness between the transparent conductive film and the transparent conductive film will be improved and the pen sliding durability will be improved, the winding property of the film roll will be improved, and the anti-Newton ring property will be improved.
  • the curable resin layer may be applied to both surfaces of the transparent plastic film base material. When the three-dimensional surface roughness SRa of the curable resin layer opposite to the surface on which the transparent conductive film is formed is Y, it is preferable that Y is 70 to 270 nm. Details of the curable resin layer are described below.
  • the curable resin preferably used in the present invention is not particularly limited as long as it is a resin that can be cured by applying energy such as heating, ultraviolet irradiation, electron beam irradiation, etc., and is a silicone resin, an acrylic resin, a methacrylic resin, or an epoxy resin. , Melamine resin, polyester resin, urethane resin and the like. From the viewpoint of productivity, it is preferable to use an ultraviolet curable resin as a main component.
  • Such an ultraviolet curable resin is synthesized from, for example, a polyfunctional acrylate resin such as acrylic acid or methacrylic acid ester of polyhydric alcohol, diisocyanate, polyhydric alcohol and hydroxyalkyl ester of acrylic acid or methacrylic acid.
  • a polyfunctional acrylate resin such as acrylic acid or methacrylic acid ester of polyhydric alcohol, diisocyanate, polyhydric alcohol and hydroxyalkyl ester of acrylic acid or methacrylic acid.
  • examples thereof include a polyfunctional urethane acrylate resin and the like.
  • monofunctional monomers such as vinylpyrrolidone, methylmethacrylate, and styrene can be added to these polyfunctional resins to copolymerize them.
  • a discharge treatment method in which a glow or corona discharge is applied to increase the number of carbonyl groups, carboxyl groups, and hydroxyl groups, and an acid or alkali to increase polar groups such as amino groups, hydroxyl groups, and carbonyl groups.
  • Examples include a chemical treatment method for processing.
  • the ultraviolet curable resin is usually used by adding a photopolymerization initiator.
  • a photopolymerization initiator a known compound that absorbs ultraviolet rays to generate radicals can be used without particular limitation, and such photopolymerization initiators include, for example, various benzoins, phenylketones, and benzophenones. The kind etc. can be mentioned.
  • the amount of the photopolymerization initiator added is usually preferably 1 to 5 parts by mass per 100 parts by mass of the ultraviolet curable resin.
  • inorganic particles and organic particles in combination with the curable resin layer, which is the main constituent component, in the curable resin layer.
  • the curable resin layer which is the main constituent component
  • Examples of the inorganic particles include silica and the like.
  • Examples of the organic particles include polyester resin, polyolefin resin, polystyrene resin, and polyamide resin.
  • a resin that is incompatible with the curable resin in combination with the curable resin that is the main component it is also preferable to use a resin that is incompatible with the curable resin in combination with the curable resin that is the main component.
  • a resin that is incompatible with the curable resin in combination with the curable resin of the matrix phase separation occurs in the curable resin and the incompatible resin can be dispersed in the form of particles.
  • the dispersed particles of the incompatible resin can form irregularities on the surface of the curable resin and improve the surface roughness in a wide area.
  • incompatible resin examples include polyester resin, polyolefin resin, polystyrene resin, and polyamide resin.
  • the mixing ratio when inorganic particles are used in the curable resin layer directly under the transparent conductive film is shown.
  • the amount of the inorganic particles is preferably 0.1 to 20 parts by mass, more preferably 0.1 to 15 parts by mass, and particularly preferably 0.1 to 12 parts by mass per 100 parts by mass of the ultraviolet curable resin.
  • the blending amount is 0.1 to 20 parts by mass per 100 parts by mass of the ultraviolet curable resin, the convex portions formed on the surface of the curable resin layer are not too small, and three-dimensional surface roughness can be effectively imparted.
  • the amount of deformation of the surface protrusions is reduced, cracks in the transparent conductive film are suppressed, high-definition images can be provided, and the transparent conductive film has some surface protrusions, so the film is wound. It is preferable because it can maintain the removability.
  • the blending ratio when inorganic particles are used in the curable resin layer on the surface opposite to the surface on which the transparent conductive film is formed is shown.
  • the amount of the inorganic particles blended is preferably 12.5 to 48 parts by mass, more preferably 17 to 48 parts by mass, and particularly preferably 25.5 to 48 parts by mass per 100 parts by mass of the ultraviolet curable resin.
  • the amount is 12.5 to 48 parts by mass per 100 parts by mass of the ultraviolet curable resin, the size of the unevenness formed on the surface of the curable resin layer becomes appropriate, and excellent antiglare properties can be provided, which is preferable.
  • the above-mentioned ultraviolet curable resin, photopolymerization initiator, and resin incompatible with inorganic particles, organic particles, and ultraviolet curable resin are dissolved in a common solvent to prepare a coating liquid.
  • the solvent used is not particularly limited, and is, for example, an alcohol solvent such as ethyl alcohol and isopropyl alcohol, an ester solvent such as ethyl acetate and butyl acetate, and dibutyl ether and ethylene glycol monoethyl ether.
  • Ketone-based solvents such as ether-based solvents, methylisobutylketone, cyclohexanone and the like, aromatic hydrocarbon-based solvents such as toluene, xylene, solventnaphtha and the like can be used alone or in combination.
  • the concentration of the resin component in the coating liquid can be appropriately selected in consideration of the viscosity and the like according to the coating method.
  • the ratio of the total amount of the ultraviolet curable resin, the photopolymerization initiator, and the high molecular weight polyester resin in the coating liquid is usually 20 to 80% by mass.
  • other known additives such as a silicone-based leveling agent may be added to the coating liquid, if necessary.
  • the prepared coating liquid is coated on a transparent plastic film substrate.
  • the coating method is not particularly limited, and conventionally known methods such as a bar coat method, a gravure coat method, and a reverse coat method can be used.
  • the solvent of the coated coating liquid is evaporated and removed in the next drying step.
  • the high molecular weight polyester resin uniformly dissolved in the coating liquid becomes particles and precipitates in the ultraviolet curable resin.
  • the plastic film is irradiated with ultraviolet rays to crosslink and cure the ultraviolet curable resin to form a curable resin layer.
  • the high-molecular-weight polyester resin particles are fixed in the hard coat layer, and protrusions are formed on the surface of the curable resin layer to improve the surface roughness in a wide area.
  • the thickness of the curable resin layer is preferably in the range of 0.1 to 15 ⁇ m. It is more preferably in the range of 0.5 to 10 ⁇ m, and particularly preferably in the range of 1 to 8 ⁇ m. When the thickness of the curable resin layer is 0.1 ⁇ m or more, sufficient protrusions are formed, which is preferable. On the other hand, if it is 15 ⁇ m or less, the productivity is good and preferable.
  • the three-dimensional center surface average surface roughness SRa is defined in ISO 25178, and is a three-dimensional surface shape measuring device Bartscan (R5500H-M100 manufactured by Ryoka System Co., Ltd. (measurement conditions: wave mode, measurement wavelength 560 nm,). The three-dimensional center plane average surface roughness SRa was obtained using an objective lens 10 times)). The number of measurements was set to 5, and the average value thereof was calculated. Here, the first decimal place in nm is rounded off.
  • the three-dimensional surface roughness SRa of the transparent conductive film is X
  • the three-dimensional surface roughness SRa of the surface of the transparent plastic film substrate opposite to the transparent conductive film side is Y.
  • FIGS. 1 to 4 show an example of a method for certifying the longest part of a crystal grain at the time of measurement. That is, the longest part is certified by the length of the straight line that can measure the largest particle size of each crystal grain.
  • Thickness (film thickness) of transparent conductive film A film sample piece on which a transparent conductive thin film layer was laminated was cut into a size of 1 mm ⁇ 10 mm and embedded in an epoxy resin for an electron microscope. This was fixed to a sample holder of an ultramicrotome, and a thin section having a cross section parallel to the short side of the embedded sample piece was prepared. Next, a photograph was taken at a site where the thin film of this section was not significantly damaged, using a transmission electron microscope (JEM-2010, manufactured by JEOL) at an acceleration voltage of 200 kV and a bright field of view at an observation magnification of 10,000 times. The film thickness was calculated from the photographs taken.
  • JEM-2010 manufactured by JEOL
  • the transparent conductive film according to the present invention is used as one panel plate, and the other panel plate is an indium-tin composite oxide thin film having a thickness of 20 nm on a glass substrate by a sputtering method.
  • a transparent conductive thin film having a tin oxide content (10% by mass) was used.
  • a touch panel was produced by arranging these two panel plates via epoxy beads having a diameter of 30 ⁇ m so that the transparent conductive thin films face each other. Next, a load of 5.0 N was applied to a polyacetal pen (tip shape: 0.8 mmR), and a linear sliding test of 180,000 reciprocations was performed on the touch panel.
  • the sliding distance was 30 mm and the sliding speed was 180 mm / sec.
  • the ON resistance resistance value when the movable electrode (film electrode) and the fixed electrode came into contact with each other
  • the ON resistance is preferably 10 k ⁇ or less.
  • the films in each comparative example were used instead of the transparent conductive film according to the present invention.
  • a transparent conductive film obtained by cutting the transparent conductive film according to the present invention into a size of 50 mm ⁇ 50 mm is used as one panel plate, and the thickness of the other panel plate is increased by sputtering on a glass substrate.
  • a transparent conductive thin film made of a 20 nm indium-tin oxide composite oxide thin film (tin oxide content: 10% by mass) was used.
  • the two panel plates are arranged via epoxy beads having a diameter of 30 ⁇ m so that the transparent conductive thin films face each other, and the thickness is adjusted to 120 ⁇ m with double-sided tape.
  • a touch panel was made by pasting a board.
  • a load of 35 N is applied to a position 2.0 mm from the end of the double-sided tape with a pen made of polyacetal (tip shape 0.8 mmR), and linear sliding is performed 10 times (5 reciprocations) in parallel with the double-sided tape.
  • a pen load is applied to the transparent conductive film surface according to the present invention.
  • the sliding distance is 30 mm and the sliding speed is 20 mm / sec.
  • sliding is performed at a position where there are no epoxy beads.
  • the transparent conductive film is removed, the surface resistance (4 terminal method) at any 5 points of the sliding part is measured, and the average value is calculated.
  • the four terminals When measuring the surface resistance, arrange the four terminals in a direction perpendicular to the sliding portion so that the sliding portion comes between the second terminal and the third terminal.
  • the rate of increase in the surface resistance value is calculated by dividing the average value of the surface resistance values of the sliding portion by the surface resistance value of the non-sliding portion (measured by the 4-terminal method).
  • the films in each comparative example were used instead of the transparent conductive film according to the present invention.
  • the transparent plastic film base material used in Examples and Comparative Examples is a biaxially oriented transparent PET film having easy-adhesive layers on both sides (manufactured by Toyobo Co., Ltd., A4340, thickness is shown in Table 1).
  • As the curable resin layer 100 parts by mass of a photopolymerization initiator-containing acrylic resin (Seika Beam (registered trademark) EXF-01J, manufactured by Dainichi Seika Kogyo Co., Ltd.) and silica particles (Snowtex ZL, manufactured by Nissan Chemical Co., Ltd.) are shown.
  • this coating liquid is hereinafter referred to as coating liquid A).
  • the prepared coating liquid was applied using a Meyer bar so that the thickness of the coating film was 5 ⁇ m.
  • the coating film was cured by irradiating with ultraviolet rays (light intensity: 300 mJ / cm 2 ) using an ultraviolet irradiation device (UB042-5AM-W type manufactured by Eye Graphics). .. Further, the curable resin layer was provided on both sides of the transparent plastic base material.
  • Examples 1 to 8 Each example level was carried out as follows under the conditions shown in Table 1. The film was placed in a vacuum chamber and evacuated to 1.5 ⁇ 10 -4 Pa. Next, after the introduction of oxygen, argon was introduced as the inert gas and hydrogen gas was introduced as the hydrogen-containing gas at the concentrations shown in Table 1 to bring the total pressure to 0.6 Pa. Power was applied to an indium-tin oxide composite oxide sintering target or an indium oxide sintered target containing no tin oxide at a power density of 3 W / cm 2 , and a transparent conductive film was formed by a DC magnetron sputtering method. The film thickness was controlled by changing the speed at which the film passed over the target.
  • the ratio of the water pressure to the inert gas in the film formation atmosphere during sputtering was measured using a gas analyzer (Transpector XPR3 manufactured by Inficon).
  • a gas analyzer Transpector XPR3 manufactured by Inficon.
  • Table 1 shows the temperature at the center of the maximum and minimum temperatures from the start of film formation to the end of film formation on the film roll as the center value.
  • the film on which the transparent conductive film was formed and laminated was subjected to the heat treatment shown in Table 1 and then measured. The measurement results are shown in Table 1.
  • Comparative Examples 1 to 9 A transparent conductive film was prepared and evaluated in the same manner as in Example 1 under the conditions shown in Table 1. However, Comparative Example 7 does not have a curable resin layer. However, in Comparative Example 8, the thickness of the coating film of the curable resin layer was adjusted to be 20 ⁇ m. The results are shown in Table 2.
  • the transparent conductive films shown in Examples 1 to 8 are excellent in pen sliding durability, pen heavy pressure durability, and antiglare property, and have all the characteristics. ..
  • Comparative Examples 1 to 9 cannot satisfy all of the pen sliding durability, the pen heavy pressure durability, and the anti-glare property.
  • a transparent conductive film having excellent pen sliding durability, pen heavy pressure durability, and anti-glare property can be produced, which is extremely useful for applications such as a resistance film type touch panel. ..

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Abstract

Le problème décrit par la présente invention est de fournir un film conducteur transparent excellent en termes de durabilité de frappe de stylo, de durabilité de mise sous pression de poids de stylo et de propriétés antireflet lorsqu'il est utilisé pour un écran tactile. La solution selon l'invention porte sur un film conducteur transparent dans lequel une membrane conductrice transparente qui est un oxyde composite indium-étain est stratifiée sur une surface d'un matériau de base de film plastique transparent, la résistance à l'état passant de la membrane conductrice transparente du film conducteur transparent dans un test de durabilité de frappe de stylo n'étant pas supérieure à 10 kΩ ; le taux d'augmentation de la valeur de résistance de surface de la membrane conductrice transparente du film conducteur transparent dans un test de durabilité de mise sous pression de poids de stylo n'est pas supérieur à 1,5 ; et un brillant spéculaire à 60° de la surface sur le côté opposé à la membrane conductrice transparente sur le matériau de base de film plastique transparent est compris entre 50 % et 120 %.
PCT/JP2021/029154 2020-09-29 2021-08-05 Film conducteur transparent WO2022070610A1 (fr)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002050230A (ja) * 2000-08-03 2002-02-15 Toyobo Co Ltd 透明導電性フィルム、透明導電性シートおよびタッチパネル
JP2002343150A (ja) * 2001-05-22 2002-11-29 Mitsui Chemicals Inc 透明導電性フィルム及びその製造方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002050230A (ja) * 2000-08-03 2002-02-15 Toyobo Co Ltd 透明導電性フィルム、透明導電性シートおよびタッチパネル
JP2002343150A (ja) * 2001-05-22 2002-11-29 Mitsui Chemicals Inc 透明導電性フィルム及びその製造方法

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