WO2019130841A1 - 光透過性導電フィルム、その製造方法、調光フィルム、および、調光部材 - Google Patents

光透過性導電フィルム、その製造方法、調光フィルム、および、調光部材 Download PDF

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Publication number
WO2019130841A1
WO2019130841A1 PCT/JP2018/041344 JP2018041344W WO2019130841A1 WO 2019130841 A1 WO2019130841 A1 WO 2019130841A1 JP 2018041344 W JP2018041344 W JP 2018041344W WO 2019130841 A1 WO2019130841 A1 WO 2019130841A1
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Prior art keywords
film
light
transmitting conductive
conductive film
light transmitting
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PCT/JP2018/041344
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English (en)
French (fr)
Japanese (ja)
Inventor
望 藤野
智剛 梨木
秀行 米澤
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日東電工株式会社
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Priority to CN201880084061.7A priority Critical patent/CN111527570B/zh
Priority to JP2019502028A priority patent/JP7264807B2/ja
Priority to KR1020207014151A priority patent/KR102633881B1/ko
Publication of WO2019130841A1 publication Critical patent/WO2019130841A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/023—Optical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • 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
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
    • E06B9/24—Screens or other constructions affording protection against light, especially against sunshine; Similar screens for privacy or appearance; Slat blinds
    • 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 light transmitting conductive film, a method of manufacturing the same, and a light control film and a light control member including the same.
  • Patent Document 1 proposes a film provided with two transparent conductive resin substrates and a light control layer sandwiched between two transparent conductive resin substrates. (See, for example, Patent Document 1).
  • the light control film of Patent Document 1 enables light control by adjusting absorption and scattering of light passing through the light control layer by application of an electric field.
  • a transparent conductive resin substrate of such a light control film a film in which a transparent electrode made of indium tin complex oxide (ITO) is laminated on a supporting substrate such as a polyester film is adopted.
  • ITO indium tin complex oxide
  • the light control film may be used by being attached to a large glass (for example, a window glass of 1 to 10 m 2 ) or the like. Specifically, a light control film of substantially the same size as the glass is disposed on a glass via a thermosetting or hot melt adhesive or the like, and the light control film is heated or cured by heating or melting. Stick to glass.
  • a large glass for example, a window glass of 1 to 10 m 2
  • a light control film of substantially the same size as the glass is disposed on a glass via a thermosetting or hot melt adhesive or the like, and the light control film is heated or cured by heating or melting. Stick to glass.
  • the light control film after sticking has a defect that it shrinks more than the state before heating due to heating. As a result, the light control film is not attached to the glass (particularly, the peripheral end). This non-sticking point is conspicuous as the area of the target glass increases.
  • An object of the present invention is to provide a light transmitting conductive film which can be attached to the entire surface of an object, a method of manufacturing the same, a light control film, and a light control member.
  • the present invention [1] is a light transmitting conductive film extending in a first direction and a second direction orthogonal to the first direction, comprising a base film and a light transmitting conductive layer, and the light
  • a thermomechanical analysis step of raising the temperature of the permeable conductive film from 20 ° C. to 160 ° C. and then decreasing the temperature to 20 ° C.
  • dimensional change before and after the analysis step in the first direction, and the second direction The dimensional change before and after the analysis step in includes both light-transmissive electrically conductive films that exhibit swelling.
  • the light-transmitting conductive film is heated from 20 ° C. to 150 ° C. and then cooled to 20 ° C. according to JIS C 2151.
  • Both the dimensional change before and after the heating step and the dimensional change before and after the heating step in the second direction indicate contraction, and the absolute value of the dimensional change rate before and after the heating step in the first direction,
  • the light transmissive conductive film as described in [1] whose absolute value of the dimensional change before and behind the said heating process in the said 2nd direction is both less than 0.35%.
  • the base film includes the light transmitting conductive film described in [1] or [2], which is a film heat-treated in an air environment.
  • the present invention [4] includes the light transmitting conductive film according to any one of [1] to [3], wherein the base film is a polyester film.
  • the present invention [5] comprises a first light-transmitting conductive film, a light control function layer, and a second light-transmitting conductive film in order, and the first light-transmitting conductive film and / or the first light-transmitting conductive film
  • the light transmitting conductive film of No. 2 includes a light control film which is the light transmitting conductive film according to any one of [1] to [4].
  • the present invention [6] includes a light control member including a protective member and the light control film described in [5] attached to the protective member.
  • the present invention [7] is a method for producing the light transmitting conductive film according to any one of [1] to [4], which comprises the steps of heating a substrate film in the air environment, and then A method for producing a light transmitting conductive film, comprising the step of providing a light transmitting conductive layer on the base film in a state where the base film is cooled to 5 ° C. or less.
  • both the dimensional change in the first direction and the dimensional change in the second direction show expansion.
  • the light transmitting conductive film of the present invention expands more than the state before heating. Therefore, it can prevent that the surface of the edge part of a target object is exposed, and a transparent conductive film can be stuck on the whole surface of a target object.
  • the light transmissive conductive film of the same size as a target object can be stuck on a target object by cut
  • the end can be effectively used as a wiring installation area.
  • the light control film of the present invention comprises the light transmitting conductive film of the present invention, it can be attached to the entire surface of an object.
  • the light control function can be provided on the entire surface of the protective member.
  • the manufacturing method of the present invention can obtain a light transmitting conductive film which can be stuck to the entire surface of an object.
  • FIG. 1A-B show an embodiment of the light transmitting conductive film of the present invention
  • FIG. 1A shows a cross-sectional view
  • FIG. 1B shows a perspective view
  • FIG. 2 shows a perspective view of the process of manufacturing the light transmitting conductive film shown in FIG. 1A
  • FIG. 3 shows a cross-sectional view of a light control film provided with the light transmitting conductive film shown in FIG. 1A
  • 4A to 4E are process diagrams for producing a light control member using the light control film shown in FIG. 2
  • FIG. 4A is a process of preparing a protective member
  • FIG. 4B is a thermosetting process for the protective member.
  • FIG. 4C is a step of arranging the light control film on the thermosetting adhesive layer
  • FIG. 4D is a step of heat curing the thermosetting adhesive layer
  • FIG. 4E is a light control film. The step of cutting is shown.
  • the paper thickness direction is the front-rear direction (first direction)
  • the front side of the sheet is the front side (one side in the first direction)
  • the rear side is the rear side (the other side in the first direction).
  • the left-right direction of the drawing is the left-right direction (width direction, second direction orthogonal to the first direction)
  • the left side of the drawing is the left side (one side of the second direction)
  • the right side of the drawing is the right (second side of the second direction).
  • the vertical direction in the drawing is the vertical direction (the thickness direction, the third direction orthogonal to the first direction and the second direction)
  • the upper side in the drawing is the upper side (one side in the thickness direction, one side in the third direction)
  • the lower side in the drawing is the lower side (the other side in the thickness direction, the other side in the third direction). Specifically, it conforms to the directional arrow in each figure.
  • the light transmissive conductive film 1 is, for example, a film used as a light control film as an example of a light control element, a light control member, a light control device, etc. (Light transmitting conductive film for light).
  • the light transmitting conductive film 1 has a film shape (including a sheet shape) having a predetermined thickness, as shown in FIG. 1, and is in a predetermined direction (longitudinal direction and left and right direction) orthogonal to the vertical direction (thickness direction). , And has a flat upper surface (one surface in the thickness direction) and a flat lower surface (the other surface in the thickness direction).
  • the light transmitting conductive film 1 is, for example, one component of a light control film 4 (described later, refer to FIG. 3), a light control member 6 (described later, refer to FIG. 4E), and a light control device (described later). It is not a light film 4 or the like. That is, the light transmitting conductive film 1 is a component for producing the light control film 4 or the like, does not include the light control function layer 5 or the like, and is a device which can be distributed alone and can be industrially used.
  • the light transmitting conductive film 1 includes the base film 2 and the light transmitting conductive layer 3 in order. That is, the light transmitting conductive film 1 includes the base film 2 and the light transmitting conductive layer 3 disposed on the upper side of the base film 2.
  • the light transmitting conductive film 1 is composed only of the base film 2 and the light transmitting conductive layer 3. Each layer will be described in detail below.
  • the base film 2 is a lowermost layer of the light transmitting conductive film 1 and is a support material for securing the mechanical strength of the light transmitting conductive film 1. Moreover, the base film 2 is a support material which has light transmittance and flexibility. The base film 2 supports the light transmitting conductive layer 3.
  • the base film 2 has a film shape (including a sheet shape).
  • the base film 2 is made of, for example, a polymer film.
  • the material of the polymer film include polyester resins such as polyethylene terephthalate (PET), polybutylene terephthalate and polyethylene naphthalate, for example, (meth) acrylic resins (acrylic resins and / or methacrylic resins) such as polymethacrylates, for example And olefin resins such as polyethylene, polypropylene and cycloolefin polymers, such as polycarbonate resin, polyether sulfone resin, polyarylate resin, melamine resin, polyamide resin, polyimide resin, cellulose resin, polystyrene resin, norbornene resin and the like.
  • polyester resins such as polyethylene terephthalate (PET), polybutylene terephthalate and polyethylene naphthalate
  • acrylic resins acrylic resins and / or methacrylic resins
  • olefin resins such as polyethylene, polypropylene
  • the base film 2 is preferably a polyester film formed of a polyester resin from the viewpoint of light transmittance, heat resistance, mechanical strength and the like, and more preferably a polyethylene terephthalate film.
  • the base film 2 is preferably a stretched film, and more preferably a biaxially stretched film, from the viewpoint of further excellent heat resistance and mechanical strength.
  • the base film 2 is preferably a film heat-treated under an air environment as described later, and more preferably a biaxially stretched film heat-treated under an air environment.
  • a base film 2 When such a base film 2 is used, the stress existing inside the base film 2 is relieved, so when the light transmitting conductive film 1 is attached to the object by heating, the light transmitting conductive film 1 is used. Contraction can be prevented.
  • the total light transmittance (JIS K-7105) of the base film 2 is, for example, 80% or more, preferably 85% or more, and for example, 100% or less, preferably 95% or less.
  • the haze (JIS K-7105) of the base film 2 is, for example, 2.0% or less, preferably 1.8% or less, more preferably 1.5% or less, still more preferably 1.2% or less And, for example, 0.1% or more.
  • the thickness of the base film 2 is, for example, 2 ⁇ m or more, preferably 50 ⁇ m or more, more preferably 100 ⁇ m or more, and for example, 300 ⁇ m or less, preferably 250 ⁇ m or less. If the thickness of the base film 2 is not less than the above lower limit, more moisture contained in the polymer film can be imparted to the light transmitting conductive layer 3 when the light transmitting conductive layer 3 is formed, so the light transmitting conductive layer The crystallization of 3 can be suppressed. Therefore, the amorphous property of the light transmissive conductive layer 3 can be maintained. In addition, when the thickness of the base film 2 is equal to or more than the above lower limit, the strength of the light transmitting conductive film 1 is excellent.
  • the thickness of the base film 2 can be measured, for example, using a film thickness meter.
  • a separator or the like may be provided on the lower surface of the base film 2.
  • the light transparent conductive layer 3 is a transparent conductive layer that can be patterned by etching in a later step as necessary.
  • the light transmitting conductive layer 3 has a film shape (including a sheet shape), and is disposed on the entire upper surface of the base film 2 so as to be in contact with the upper surface of the base film 2.
  • the material of the light transmitting conductive layer 3 is, 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, W
  • a metal oxide containing one kind of metal can be mentioned.
  • the metal oxide may further be doped with the metal atoms shown in the above group, as needed.
  • the light-transmissive conductive layer 3 examples include indium-based conductive oxides such as indium tin complex oxide (ITO), and antimony-based conductive oxides such as antimony tin complex oxide (ATO). .
  • the light transmitting conductive layer 3 contains an indium-based conductive oxide, and more preferably contains indium tin complex oxide (ITO), from the viewpoint of being able to ensure excellent conductivity and light transmission. That is, the light transmissive conductive layer 3 is preferably an indium-based conductive oxide layer, more preferably an ITO layer.
  • the content of tin oxide (SnO 2 ) is, for example, 0.5 mass% or more with respect to the total amount of tin oxide and indium oxide (In 2 O 3 ) , Preferably 3% by mass or more, more preferably 8% by mass or more, more preferably 10% by mass, and for example, 25% by mass or less, preferably 15% by mass or less, more preferably It is 13% by mass or less. If content of a tin oxide is more than the said lower limit, crystallization can be suppressed more reliably, implement
  • ITO 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, Fe , Pb, Ni, Nb, Cr, Ga and the like.
  • the light transmitting conductive layer 3 may be either crystalline or amorphous (amorphous), but is preferably amorphous, more specifically, preferably an amorphous ITO layer. is there. If the light transmitting conductive layer 3 is amorphous, it is excellent in crack resistance and scratch resistance, and therefore excellent in processability. That is, when the light transmitting conductive film 1 is attached to an object to be attached (for example, a protective member such as a glass described later), the generation of cracks and scratches generated in the light transmitting conductive film 1 is suppressed can do. Therefore, the external appearance and the characteristic of the light transmissive conductive film 1 stuck can be maintained favorably.
  • the light transmitting conductive layer 3 is amorphous or crystalline after being dipped in hydrochloric acid (concentration 5 mass%) at 20 ° C. for 15 minutes. It can be judged by washing with water, drying and measuring the resistance between terminals of about 15 mm.
  • hydrochloric acid concentration 5 mass%
  • the resistance between terminals in the light-transmissive conductive layer is 10 k ⁇ or more
  • the light transmitting conductive layer is assumed to be amorphous.
  • the surface resistance value of the light transmitting conductive layer 3 is, for example, 1 ⁇ / sq or more, preferably 10 ⁇ / sq or more, and for example, 200 ⁇ / sq or less, preferably 100 ⁇ / sq or less, more preferably, It is 85 ⁇ / ⁇ or less. If the surface resistance value of the light transmitting conductive layer 3 is in the above range, good electric drive can be realized even when used as a large light control device.
  • the specific resistance value of the light transmitting conductive layer 3 is, for example, 6 ⁇ 10 ⁇ 4 ⁇ ⁇ cm or less, preferably 5.5 ⁇ 10 ⁇ 4 ⁇ ⁇ cm or less, more preferably 5 ⁇ 10 ⁇ 4 ⁇ ⁇ cm. or less, more preferably 4.8 ⁇ 10 ⁇ 4 ⁇ ⁇ cm or less, and for example, 3 ⁇ 10 ⁇ 4 ⁇ ⁇ cm or more, preferably 3.5 ⁇ 10 ⁇ 4 ⁇ ⁇ cm or more More preferably, it is 4.0 ⁇ 10 ⁇ 4 ⁇ ⁇ cm or more. If the specific resistance value of the light transmitting conductive layer 3 is not more than the above upper limit, good electric drive can be realized even when used as a large light control device. In addition, when the specific resistance value is equal to or more than the above lower limit, the amorphousness of the light transmitting conductive layer 3 can be more reliably maintained.
  • the thickness of the light transmitting conductive layer 3 is, for example, 10 nm or more, preferably 30 nm or more, more preferably 50 nm or more, and for example, 200 nm or less, preferably 150 nm or less, more preferably 100 nm or less is there.
  • the thickness of the light transmitting conductive layer 3 can be measured, for example, by cross-sectional observation using a transmission electron microscope.
  • the method for producing the light transmitting conductive film 1 includes, for example, a preheating step of heating the base film 2 in the atmospheric environment, and then cooling the base film 2 to 5 ° C. or less. And a conductive layer disposing step of providing the light transmitting conductive layer 3.
  • the method of producing the light transmitting conductive film 1 is preferably carried out by a roll-to-roll method, as shown in FIG.
  • the base film 2 is prepared.
  • the base film 2 wound in a roll shape is used long in the transport direction (for example, the first direction).
  • the biaxially stretched base film 2 is prepared from the viewpoint of mechanical strength, heat resistance, and light transmittance.
  • the base film 2 is heated in the air environment. That is, before providing the light transmitting conductive layer 3, the base film 2 is heated.
  • the heating of the base film 2 is preferably carried out by a roll-to-roll method, for example, after the base film 2 wound into a long roll is drawn out and transported while being heated in the atmospheric environment, Roll it into a long roll again.
  • the heating temperature is, for example, 100 ° C. or more, preferably 130 ° C. or more, more preferably 150 ° C. or more, and for example, 220 ° C. or less, preferably 200 ° C. or less, more preferably 180 ° C. or less is there.
  • the heating temperature is a set temperature of heating equipment (for example, an IR heater or a heating roll) for heating the base film 2.
  • the heating time is, for example, 0.3 minutes or more, preferably 0.5 minutes or more, more preferably 1 minute or more, and for example, 10 minutes or less, preferably 5 minutes or less. If the heating time is equal to or less than the above-described upper limit, generation of excess precipitates (such as oligomers) from the base film 2 can be suppressed, and the reduction in transparency and the increase in haze of the base film 2 can be suppressed. it can. Moreover, if heating time is more than the said minimum, the residual stress of the base film 2 can be fully relieved, and the thermal contraction at the time of sticking of the transparent conductive film 1 can be suppressed more reliably. .
  • the light transmissive conductive layer 3 is formed on the upper surface of the base film 2 by, for example, a dry process.
  • a vacuum evaporation method, sputtering method, ion plating method etc. are mentioned, for example.
  • a sputtering method is mentioned.
  • a target and an adherend are disposed opposite to each other in a chamber (film forming chamber) of a vacuum device, gas is supplied and voltage is applied to accelerate gas ions and irradiate the target.
  • the target material is repelled from the target surface, and the target material is laminated on the adherend surface.
  • Examples of the sputtering method include bipolar sputtering, ECR (electron cyclotron resonance) sputtering, magnetron sputtering, and ion beam sputtering.
  • a magnetron sputtering method is mentioned.
  • the power source used for the sputtering method may be, for example, any of a direct current (DC) power source, an alternating current medium frequency (AC / MF) power source, a high frequency (RF) power source, and a high frequency power source on which a direct current power source is superimposed.
  • DC direct current
  • AC / MF alternating current medium frequency
  • RF high frequency
  • the above-mentioned metal oxide which comprises the transparent conductive layer 3 is mentioned.
  • a target made of ITO is used.
  • the content of tin oxide (SnO 2 ) in the target is, for example, 0.5% by mass or more, preferably 3% by mass or more, more preferably, relative to the total amount of tin oxide and indium oxide (In 2 O 3 ). 8% by mass or more, more preferably more than 10% by mass, and for example, 25% by mass or less, preferably 15% by mass or less, more preferably 13% by mass or less.
  • the sputtering is preferably performed under vacuum, and the pressure is, for example, 1.0 Pa or less, preferably 0.5 Pa or less, more preferably 0.2 Pa or less, and for example, 0.01 Pa It is above.
  • an inert gas such as Ar may be mentioned.
  • reactive gas such as oxygen gas is used in combination.
  • the ratio of the flow rate of reactive gas to the flow rate of inert gas is, for example, 0.1 / 100 or more and 5/100 or less.
  • the temperature of the base film 2 in forming the light transmitting conductive layer 3 is 5 ° C. or less, preferably less than 0 ° C., more preferably ⁇ 3 ° C. or less, and for example, ⁇ 40 ° C. or more, Preferably, it is ⁇ 20 ° C. or higher.
  • the temperature of the base film 2 exceeds the above upper limit, the base film 2 is stretched in the transport direction by the tension in the transport direction, and stress remains in the base film 2 of the light transmitting conductive film 1 obtained.
  • the light transmitting conductive film 1 is attached to an object, there is a possibility of heat shrinkage.
  • the lower surface of the base film 2 is brought into contact with a cooling device (for example, a cooling roll) or the like.
  • a cooling device for example, a cooling roll
  • the film forming roll and the nip roll can be cooled to form a cooling roll.
  • the temperature of the base film 2 is a set temperature of the cooling device.
  • the atmosphere (in the chamber) at the time of sputtering is preferably hydrated, and the ratio of the moisture gas to the sputtering pressure (total pressure) (partial pressure of moisture gas (Pa) / sputtering pressure (Pa)) is, for example, 0.006 or more, preferably 0.008 or more, more preferably 0.01 or more, and for example, 0.3 or less, preferably 0.1 or less, more preferably 0.07 or less, More preferably, it is 0.05 or less.
  • the light transmitting conductive film 1 including the base film 2 and the light transmitting conductive layer 3 is obtained.
  • the light transmissive conductive layer 3 at this time is amorphous.
  • the total thickness thereof is, for example, 2 ⁇ m or more, preferably 20 ⁇ m or more, and for example, 300 ⁇ m or less, preferably 200 ⁇ m or less.
  • thermomechanical analysis process (the above analysis process; hereinafter abbreviated as "TMA") is performed, in which the temperature of the light transmitting conductive film 1 is increased from 20 ° C to 160 ° C and then decreased to 20 ° C.
  • TMA thermomechanical analysis process
  • the longitudinal length at 20 ° C. before implementation of TMA is L 1
  • the longitudinal length at 20 ° C. after implementation of TMA is L 1 ′
  • left and right at 20 ° C. before implementation of TMA the left-right length at 20 ° C. after direction length was conducted L 2
  • TMA as L 2 '
  • dimensional change [Delta] L 1 in the longitudinal direction the dimensional change rate [Delta] L 2 in the lateral direction
  • in-plane dimensional change The ratio R is expressed by the following equation.
  • ⁇ L 1 ⁇ (L 1 ′ ⁇ L 1 ) / L 1 ⁇ ⁇ 100 (%)
  • ⁇ L 2 ⁇ (L 2 ′ ⁇ L 2 ) / L 2 ⁇ ⁇ 100 (%)
  • R ⁇ ( ⁇ L 1 ) 2 + ( ⁇ L 2 ) 2 ⁇ 1/2 (%)
  • the dimensional change of shows expansion "means that the dimensional change rate ⁇ L 2 shows a positive value.
  • the load to be applied to the light transmitting conductive film 1 is 19.6 mN, and the size of the light transmitting conductive film 1 (measurement sample) at the time of measurement is 20 mm long side (direction of load application) The short side is 3 mm.
  • Other conditions apply to the example.
  • the transport direction (MD direction) for transporting the base film 2 is the front-rear direction (first direction), and the orthogonal direction (TD direction) orthogonal to the transport direction is the left-right direction (first Two directions) (see FIG. 2).
  • the dimensional change rate ⁇ L 1 is, for example, more than 0%, preferably 0.10% or more, and for example, 0.50% or less.
  • the dimensional change rate ⁇ L 2 is, for example, more than 0%, preferably 0.10% or more, and for example, 0.50% or less.
  • the in-plane dimensional change rate R is, for example, 0.55% or less, preferably 0.50 or less, more preferably 0.40% or less, and still more preferably 0.30% or less.
  • At least one of the absolute value of the dimensional change rate ⁇ M 1 before and after and the absolute value of the dimensional change rate ⁇ M 2 before and after heating in the left-right direction is less than 0.35%, preferably 0.30% or less, more preferably , 0.20% or less.
  • the absolute value of ⁇ M 1 and the absolute value of ⁇ M 2 are both less than 0.35%, preferably 0.30% or less, more preferably 0.20% or less.
  • the method according to JIS C 2151 is a method of heating the light transmitting conductive film 1 in a state where a load such as a tensile load is not applied to the light transmitting conductive film 1.
  • the longitudinal length at 20 ° C. before performing the heating step is M 1
  • the longitudinal length at 20 ° C. after performing the heating step is M 1 ′ before performing the heating step
  • the lateral change length at 20 ° C. is M 2
  • the lateral change length at 20 ° C. after the heating process is M 2 ′
  • the dimensional change rate ⁇ M 1 in the front-rear direction, and the dimensional change rate ⁇ M in the lateral direction 2 is shown by the following formula.
  • the dimensional change rate ⁇ M 1 exceeds ⁇ 0.35%, preferably ⁇ 0.30% or more, more preferably ⁇ 0.25% or more, and for example, less than 0.35%. Preferably, it is 0.30% or less, more preferably 0.20% or less.
  • the dimensional change rate ⁇ M 2 exceeds ⁇ 0.35%, preferably ⁇ 0.20% or more, more preferably ⁇ 0.10% or more, and for example, less than 0.35% Preferably, it is 0.20% or less, more preferably 0.10% or less.
  • At least one of a dimensional change before and after the heating step in the front-rear direction and a dimensional change before and after the heating step in the left-right direction (second direction) indicates contraction.
  • Both the dimensional change before and after the heating process in the front-rear direction and the dimensional change before and after the heating process in the left-right direction (second direction) indicate contraction.
  • the dimensional change of the heating step before and after in the longitudinal direction showing a shrinkage is that the dimensional change rate .DELTA.M 1 takes a negative value.
  • the dimensional change before and after the heating process in the lateral direction indicates contraction means that the dimensional change rate ⁇ M 2 shows a negative value.
  • the haze (JIS K-7105) of the light transmitting conductive film 1 is, for example, 2.0% or less, preferably 1.8% or less, more preferably 1.5% or less, further preferably 1.2. % Or less and, for example, 0.1% or more. If the haze of the light transmitting conductive film 1 is in the above range, it can be suitably used as a light transmitting conductive film for light control.
  • the light transmitting conductive film 1 can be etched as needed to pattern the light transmitting conductive layer 3 into a predetermined shape.
  • the method of manufacturing the light control film 4 includes, for example, a step of manufacturing two light transmitting conductive films 1 and a step of sandwiching the light control functional layer 5 between the two light transmitting conductive films 1.
  • two light transmitting conductive films 1 are manufactured.
  • one light transmissive conductive film 1 can be cut and processed to prepare two light transmissive conductive films 1.
  • the two light transmitting conductive films 1 are a first light transmitting conductive film 1A and a second light transmitting conductive film 1B.
  • the light control function layer 5 is formed on the upper surface (surface) of the light transmitting conductive layer 3 in the first light transmitting conductive film 1A by, for example, a wet method.
  • a liquid crystal composition or a solution thereof is applied to the upper surface of the light transmitting conductive layer 3 in the first light transmitting conductive film 1A to form a coating film.
  • the liquid crystal composition is not limited as long as it can be used for light control applications, and may be known ones, and examples thereof include liquid crystal dispersion resins described in JP-A-8-194209.
  • the second light transmitting conductive film 1B is laminated on the upper surface of the coating film so that the light transmitting conductive layer 3 of the second light transmitting conductive film 1B and the coating are in contact with each other.
  • the coating film is sandwiched between the two light transmitting conductive films 1, that is, the first light transmitting conductive film 1A and the second light transmitting conductive film 1B.
  • the coating film is subjected to an appropriate treatment (for example, heat drying treatment, photocuring treatment) as necessary to form the light control function layer 5.
  • the light control function layer 5 is disposed between the light transmitting conductive layer 3 of the first light transmitting conductive film 1A and the light transmitting conductive layer 3 of the second light transmitting conductive film 1B.
  • the light control film 4 provided in order with the 1st light transmissive conductive film 1A, the light control function layer 5, and the 2nd light transmissive conductive film 1B is obtained.
  • the method of manufacturing the light control member 6 includes, for example, a step of forming the thermosetting adhesive layer 8 on the protective member 7, a step of arranging the light control film 4 on the thermosetting adhesive layer 8, and a thermosetting adhesive
  • the process of heat-hardening the agent layer 8 and the process of cutting the light control film 4 are provided.
  • the protective member 7 is an object to which the light control film 4 is attached, and examples thereof include window glass, partitions, and interiors.
  • a hard transparent plate having appropriate mechanical strength and thickness is used, and examples thereof include a glass plate, a reinforced plastic plate (for example, a polycarbonate resin), and the like.
  • thermosetting adhesive layer 8 is formed on the protective member 7.
  • a liquid thermosetting adhesive composition is applied to the entire upper surface (surface) of the protective member 7.
  • thermosetting adhesive composition an epoxy-type thermosetting adhesive composition, an acryl-type thermosetting adhesive composition, etc. are mentioned, for example.
  • thermosetting adhesive composition can employ
  • Examples of the application method include a method using an applicator, potting, cast coating, spin coating, roll coating and the like.
  • the light control film 4 is disposed on the thermosetting adhesive layer 8. That is, the light control film 4 is disposed on the upper surface of the protective member 7 via the thermosetting adhesive layer 8.
  • the light control film 4 is disposed so as to have substantially the same size as the protective member 7. Specifically, the light control film 4 is cut so as to have substantially the same size (length in the same longitudinal direction and length in the same left-right direction) as the protective member 7, and then, the light control film 4 is adjusted with the peripheral edge of the protective member 7
  • the light control film 4 is disposed on the upper surface of the thermosetting adhesive layer 8 so as to coincide with the peripheral edge of the light film 4 when projected in the vertical direction.
  • thermosetting adhesive layer 8 is heat-cured.
  • the heating temperature is, for example, 80 ° C. or more, preferably 100 ° C. or more, and for example, 180 ° C. or less, preferably 160 ° C. or less.
  • the heating time is, for example, 5 minutes or more, preferably 20 minutes or more, more preferably 30 minutes or more, and for example, 600 minutes or less, preferably 300 minutes or less.
  • the heat curing may be carried out in the atmospheric environment or in a vacuum environment, and an appropriate pressure may be applied.
  • the light control film 4 attached to the protective member 7 is cooled to room temperature (5 to 35 ° C.).
  • thermosetting adhesive layer 8 is thermosetted to form the adhesive layer 8a.
  • the light control film 4 is attached (fixed) to the protective member 7 via the adhesive layer 8a.
  • the light transmitting conductive film 1, and by extension, the light control film 4 expand in the surface direction side (longitudinal direction and left and right direction), and the end portion (protruding portion 9) of the light control film 4 is a protective member 7. Project laterally from the edge of the That is, the peripheral edge of the light control film 4 is located outward of the peripheral edge of the protective member 7.
  • the light control film 4 is cut. That is, the end of the light control film 4 is cut in the vertical direction, and the protruding portion 9 of the light control film 4 is removed.
  • positioned on the upper surface of the adhesive bond layer 8a is obtained.
  • the protection member 7 and the light control film 4 have substantially the same size. That is, when projected in the vertical direction, the peripheral edge of the protective member 7 coincides with the peripheral edge of the light control film 4.
  • the light control member 6 is used as, for example, an electrically driven light control device (not shown) by mounting a wiring (not shown), a power supply (not shown) and a control device (not shown) .
  • the electric drive type includes an electric field drive type and a current drive type.
  • the electric field drive type light control device the light transmission conductive layer 3 in the first light transmission conductive film 1A and the light transmission conductive layer in the second light transmission conductive film 1B by the wiring and the power supply A voltage is applied to 3 and thereby an electric field is generated between them. Then, the above-described electric field is controlled based on the control device, whereby the light control function layer 5 located between them is in an oriented state or an irregular state to transmit or block the light ( Or scatter).
  • thermomechanical analysis process TMA
  • the dimensional change in the front-rear direction and the dimensional change in the left-right direction Both show swelling. Therefore, when it sticks by heating with respect to the protection member 7 (object), it expand
  • the light transmission conductive film 1 and the light control film 4 of substantially the same size as the protective member 7 are attached by cutting the protruding part 9 of the light transmission conductive film 1 and the light control film 4. be able to.
  • the light control member 6 using the light control film 4 has a light control function on the entire surface of the protective member 7 (particularly also at the end portion) since the light control film 4 is attached to the entire surface of the protective member 7 Can.
  • the light transmitting conductive layer 3 is directly disposed on the upper surface of the base film 2, but for example, although not shown, it functions on the upper surface and / or the lower surface of the base film 2. Layers can be provided.
  • the light transmitting conductive film 1 includes the base film 2, the functional layer disposed on the upper surface of the base film 2, and the light transmitting conductive layer 3 disposed on the upper surface of the functional layer.
  • the light transmitting conductive film 1 includes the base film 2, the light transmitting conductive layer 3 disposed on the upper surface of the base film 2, and the functional layer disposed on the lower surface of the base film 2. It can be equipped. Also, for example, the functional layer and the light transmitting conductive layer 3 can be provided in this order on the upper side and the lower side of the base film 2.
  • Examples of the functional layer include an easy adhesion layer, an undercoat layer, and a hard coat layer.
  • the easy adhesion layer is a layer provided to improve the adhesion between the base film 2 and the light transmitting conductive layer 3.
  • the undercoat layer is a layer provided to adjust the reflectance and the optical hue of the light transmitting conductive film 1.
  • the hard coat layer is a layer provided to improve the abrasion resistance of the light transmitting conductive film 1.
  • the light control member 6 including the adhesive layer 8a and the light control film 4 on the upper surface of the protective member 7 is shown, but for example, although not shown, on the upper surface of the light control film 4. Furthermore, the adhesive layer 8a and the protective member 7 may be provided in order.
  • the end 9 of the light control film 4 positioned outside the peripheral edge of the protective member 7 is cut as shown by the phantom line in FIG. 4D.
  • part of the end 9 may be left without being cut to any size.
  • a part of the end 9 is, for example, a wire for connecting the light transmitting conductive layer 3 in the first light transmitting conductive film 1A (or the second light transmitting conductive film 1B) to a power supply. Can be used as an area (wiring installation area) etc.
  • a wire may be disposed in advance on the outer peripheral portion of the light transmitting conductive layer 3 of the light control film 4.
  • the manufacturing method of the light control member 6 is sticking the light control film 4 to the protection member 7 using the thermosetting adhesive layer 8, as an adhesive layer, it is heated. It may be adhesive as long as it is not limited to a thermosetting adhesive layer.
  • the light control film 4 may be attached to the protective member 7 using a heat melting adhesive. That is, in the method of manufacturing the light control member 6, for example, a step of forming a heat-meltable adhesive layer on the protective member 7, a step of arranging the light-control film 4 on a heat-meltable adhesive layer, and a heat-meltable adhesive The method may include the steps of heating and melting the agent layer and cutting the light control film 4.
  • a sheet made of a heat-meltable adhesive composition is laminated on the entire top surface of the protective member 7.
  • thermoplastic resin compositions such as ethylene vinyl acetate composition, polyolefin composition, polyamide composition, polyester composition, polypropylene composition, polyurethane composition, etc. Can be mentioned. These may be used alone or in combination of two or more.
  • hot-melt adhesive compositions are used, for example, as hot-melt adhesives.
  • the heating temperature of the heat-meltable adhesive layer is, for example, the same as the heating temperature of the thermosetting adhesive layer 8 described above.
  • the light transmitting conductive film 1) is exemplified as the light transmitting conductive film, for example, the light transmitting conductive film may be applied to uses other than for light control. it can.
  • the light transmitting conductive film is provided, for example, in an optical device such as an image display device (LCD, organic EL).
  • the light transmitting conductive film is used as a touch panel substrate.
  • an optical type such as an ultrasonic type, an electrostatic capacity type, and a resistive film type can be mentioned, and in particular, it is suitably used for an electrostatic capacity type touch panel.
  • Example 1 A polyethylene terephthalate (PET) film (thickness 188 ⁇ m, biaxially stretched film) elongated in the first direction (conveying direction, MD) was prepared as a light transmitting base film.
  • PET polyethylene terephthalate
  • the PET film was heated at 170 ° C. for 1 minute in the atmosphere by roll-to-roll method (pre-heating).
  • the heated PET film was placed in a roll-to-roll type sputtering apparatus, and a light transmitting conductive layer made of amorphous ITO with a thickness of 65 nm was formed by DC magnetron sputtering.
  • the temperature of the PET film was set to ⁇ 5 ° C. as the sputtering condition.
  • As a target a sintered body of 12% by mass of tin oxide and 88% by mass of indium oxide was used.
  • Comparative Example 1 A light transmitting conductive film was produced in the same manner as in Example 1 except that the PET film was not preheated.
  • Comparative example 3 The temperature of the PET film in sputtering is set to 140 ° C., the water content is set to 0.005, and after the formation of the light transmitting conductive layer, post heating is further performed under the conditions of 170 ° C. for 2 minutes in the air. In the same manner as in Comparative Example 2, a light transmitting conductive film was produced.
  • the thickness of the PET film was measured using a film thickness meter (manufactured by Ozaki Mfg. Co., Ltd., device name “digital dial gauge DG-205”).
  • the thickness of the ITO layer was measured by cross-sectional observation using a transmission electron microscope (manufactured by Hitachi, Ltd., device name "HF-2000").
  • TMA thermal mechanical analysis
  • the measurement sample is set in a thermomechanical analyzer ("TMA / SS71000" manufactured by SAI Technology Inc.), and the temperature is raised from 20 ° C to 160 ° C for each of the MD direction and the TD direction, and further lowered to 20 ° C. The dimensional change rate was measured.
  • TMA / SS71000 manufactured by SAI Technology Inc.
  • the dimensional change rate ⁇ L 1 (%) in the MD direction is “ ⁇ (L was calculated by the equation of 1 '-L 1) / L 1 ⁇ ⁇ 100 (%) ".
  • the dimensional change rate ⁇ L 2 (%) in the TD direction is “ ⁇ (L 2 '-L 2) / L 2 ⁇ was calculated by the equation of ⁇ 100 (%) ".
  • the in-plane dimensional change rate R of the whole measurement sample was calculated by the equation “ ⁇ ( ⁇ L 1 ) 2 + ( ⁇ L 2 ) 2 ⁇ 1/2 ”.
  • thermomechanical analysis The conditions for thermomechanical analysis were as follows.
  • Measurement mode Pull method Load: 19.6 mN Heating rate: 10 ° C / min Measurement atmosphere: Air (flow rate 200 ml / min) Chucking distance: 10 mm (3) Measurement of dimensional change rate according to JIS C 2151
  • the light transmitting conductive films of Examples and Comparative Examples were 10 cm in MD direction (first direction) and 10 cm in TD direction (direction orthogonal to MD direction, second direction) The sample was prepared by cutting into The temperature at this time was 20 ° C.
  • the sample was heated at 150 ° C. for 30 minutes in a hot air oven according to JIS C 2151 and then cooled to 20 ° C.
  • the dimensional change rate after this high temperature treatment was measured for each of the MD direction and the TD direction.
  • the dimensional change rate ⁇ M 1 (%) in the MD direction M 1 ′ ⁇ M 1 ) / M 1 ⁇ ⁇ 100 (%) ”.
  • the dimensional change rate ⁇ M 2 (%) in the TD direction is “ ⁇ (M 2 '-M 2) / M 2 ⁇ was calculated by the equation of ⁇ 100 (%) ".
  • thermosetting resin (acrylic adhesive) was applied to the entire surface of a commercially available glass plate (length 30 cm in the front-rear direction, length 25 cm in the left-right direction). Then, the transparent conductive films of the example and each comparative example of the same size as the glass plate are prepared, and each transparent conductive film is composed of the peripheral edge of the glass plate and the peripheral edge of the transparent conductive film. To be consistent, it was placed on top of the thermosetting adhesive and then heated at 150 ° C. for 60 minutes under atmospheric conditions. Thereby, the transparent conductive film was stuck on the glass plate.
  • Example 1 since the light transmitting conductive film attached was slightly expanded in the longitudinal direction and in the lateral direction as compared to the glass plate, the expanded film end portion is cut to obtain the entire glass plate. It can be seen that a light transmitting conductive film of the same size as the glass plate can be stuck.
  • the light transmitting conductive film attached is shrunk by heating at the time of attachment, and the light transmitting conductive film can not be attached to the peripheral end of the glass plate.
  • the transparent conductive film of the Example and each comparative example was heated on the conditions of 80 degreeC and 20 hours in air
  • the light transmitting conductive film of the present invention can be applied to various industrial products, and is suitably used, for example, as a light control film provided in a light control member, a touch panel substrate provided in an image display device, etc. .

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PCT/JP2018/041344 2017-12-28 2018-11-07 光透過性導電フィルム、その製造方法、調光フィルム、および、調光部材 WO2019130841A1 (ja)

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