WO2022014573A1 - Film optique équipé d'une couche antisalissure - Google Patents

Film optique équipé d'une couche antisalissure Download PDF

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Publication number
WO2022014573A1
WO2022014573A1 PCT/JP2021/026251 JP2021026251W WO2022014573A1 WO 2022014573 A1 WO2022014573 A1 WO 2022014573A1 JP 2021026251 W JP2021026251 W JP 2021026251W WO 2022014573 A1 WO2022014573 A1 WO 2022014573A1
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Prior art keywords
layer
antifouling layer
antifouling
optical film
inorganic oxide
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PCT/JP2021/026251
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English (en)
Japanese (ja)
Inventor
幸大 宮本
智剛 梨木
豊 角田
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日東電工株式会社
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Application filed by 日東電工株式会社 filed Critical 日東電工株式会社
Priority to CN202180049524.8A priority Critical patent/CN115812033B/zh
Priority to KR1020227045625A priority patent/KR102521712B1/ko
Priority to KR1020237011553A priority patent/KR102548030B1/ko
Priority to JP2022536377A priority patent/JP7185102B2/ja
Publication of WO2022014573A1 publication Critical patent/WO2022014573A1/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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • 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
    • B32B7/022—Mechanical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/12—Organic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G02B1/115—Multilayers
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14—Protective coatings, e.g. hard coatings
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/18—Coatings for keeping optical surfaces clean, e.g. hydrophobic or photo-catalytic films

Definitions

  • the present invention relates to an optical film with an antifouling layer.
  • an optical film with an antifouling layer is attached to the outer surface of a display such as a touch panel display on the image display side.
  • the optical film with an antifouling layer includes a transparent base material and an antifouling layer arranged on the outermost surface on one side of the transparent base material.
  • the antifouling layer suppresses the adhesion of contaminants such as hand grease on the display surface, and facilitates the removal of the adhered contaminants.
  • Patent Document 1 A technique relating to such an optical film with an antifouling layer is described in, for example, Patent Document 1 below.
  • the present invention provides an optical film with an antifouling layer, which is suitable for suppressing a decrease in antifouling property while ensuring peeling resistance in the antifouling layer.
  • the present invention [1] includes a transparent base material, a hard coat layer, an inorganic oxide base layer, and an antifouling layer in this order, and the antifouling layer is arranged on the inorganic oxide base layer. It is a dry coating film, and the elastic recovery rate measured by the nanoindentation method under the conditions of a temperature of 25 ° C. and a maximum indentation depth of 200 nm on the surface of the antifouling layer opposite to the inorganic oxide base layer.
  • the optical film with an antifouling layer is 76% or more.
  • the present invention [2] includes the optical film with an antifouling layer according to the above [1], wherein the antifouling layer has a thickness of 1 nm or more and 25 nm or less.
  • the present invention [3] includes the optical film with an antifouling layer according to the above [1] or [2], wherein the inorganic oxide base layer contains silicon dioxide.
  • the present invention [4] includes the optical film with an antifouling layer according to any one of the above [1] to [3], wherein the inorganic oxide base layer has a thickness of 50 nm or more.
  • the present invention [5] includes the optical film with an antifouling layer according to any one of the above [1] to [4], wherein the hard coat layer has a thickness of 1 ⁇ m or more and 50 ⁇ m or less.
  • the optical film with an antifouling layer of the present invention is a dry coating film in which the antifouling layer is arranged on the inorganic oxide base layer as described above.
  • Such a configuration is suitable for ensuring a high bonding force of the antifouling layer in the optical film with the antifouling layer, and therefore suitable for ensuring the peeling resistance of the antifouling layer.
  • the optical film with an antifouling layer has an elastic recovery measured by a nanoindentation method on the surface of the antifouling layer opposite to the inorganic oxide underlying layer under the conditions of a temperature of 25 ° C. and a maximum indentation depth of 200 nm. The rate is 76% or more.
  • Such a configuration is suitable for suppressing deterioration of the antifouling property of the antifouling layer against the wiping work on the antifouling layer.
  • the optical film F as an embodiment of the optical film with an antifouling layer of the present invention includes a transparent base material 11, a hard coat layer 12, an inorganic oxide base layer 13, and an antifouling layer. 14 and 14 are provided in this order toward one side of the thickness direction T.
  • the optical film F has a transparent base material 11, a hard coat layer 12, an adhesion layer 15, an inorganic oxide base layer 13, and an antifouling layer 14 on one side in the thickness direction T. Prepare in this order.
  • the optical film F has a shape that spreads in a direction (plane direction) orthogonal to the thickness direction T.
  • the transparent base material 11 is a transparent resin film having flexibility.
  • the material of the transparent base material 11 include polyester resin, polyolefin resin, polystyrene resin, acrylic resin, polycarbonate resin, polyether sulfone resin, polysulfone resin, polyamide resin, polyimide resin, cellulose resin, norbornene resin, and polyallylate resin. And polyvinyl alcohol resin.
  • the polyester resin include polyethylene terephthalate (PET), polybutylene terephthalate, and polyethylene naphthalate.
  • Polyolefin resins include, for example, polyethylene, polypropylene, and cycloolefin polymers (COPs).
  • the cellulose resin include triacetyl cellulose (TAC).
  • the transparent base material 11 one selected from the group consisting of polyester resin, polyolefin resin, and cellulose resin is used from the viewpoint of transparency and strength, and more preferably, it is composed of PET, COP, and TAC. One selected from the group is used.
  • the surface of the transparent substrate 11 on the hard coat layer 12 side may be surface-modified.
  • Examples of the surface modification treatment include corona treatment, plasma treatment, ozone treatment, primer treatment, glow treatment, and coupling agent treatment.
  • the thickness of the transparent substrate 11 is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, and further preferably 20 ⁇ m or more.
  • the thickness of the transparent base material 11 is preferably 300 ⁇ m or less, more preferably 200 ⁇ m or less, from the viewpoint of handleability.
  • the total light transmittance (JIS K 7375-2008) of the transparent base material 11 is preferably 80% or more, more preferably 90% or more, still more preferably 95% or more. Such a configuration is suitable for ensuring the transparency required for the optical film F when the optical film F is provided on the surface of a display such as a touch panel display.
  • the total light transmittance of the transparent substrate 11 is, for example, 100% or less.
  • the hard coat layer 12 is arranged on one surface of the transparent base material 11 in the thickness direction T.
  • the hard coat layer 12 is a layer for making it difficult for scratches to be formed on the exposed surface (upper surface in FIG. 1) of the optical film F.
  • the hard coat layer 12 is a cured product of the curable resin composition.
  • the curable resin contained in the curable resin composition include polyester resin, acrylic resin, urethane resin, acrylic urethane resin, amide resin, silicone resin, epoxy resin, and melamine resin. These curable resins may be used alone or in combination of two or more. From the viewpoint of ensuring high hardness of the hard coat layer 12, an acrylic urethane resin is preferably used as the curable resin.
  • examples of the curable resin composition include an ultraviolet curable resin composition and a thermosetting resin composition.
  • an ultraviolet curable resin composition is preferably used from the viewpoint of helping to improve the production efficiency of the optical film F because it can be cured without heating at a high temperature.
  • the UV curable resin composition contains at least one selected from the group consisting of UV curable monomers, UV curable oligomers, and UV curable polymers.
  • Specific examples of the ultraviolet curable resin composition include the composition for forming a hard coat layer described in JP-A-2016-179686.
  • the curable resin composition may contain fine particles.
  • the formulation of the fine particles in the curable resin composition is useful for adjusting the hardness, adjusting the surface roughness, adjusting the refractive index, and imparting antiglare property in the hard coat layer 12.
  • the fine particles include metal oxide particles, glass particles, and organic particles.
  • Materials for the metal oxide particles include, for example, silica, alumina, titania, zirconia, calcium oxide, tin oxide, indium oxide, cadmium oxide, and antimony oxide.
  • Materials for organic particles include, for example, polymethylmethacrylate, polystyrene, polyurethane, acrylic-styrene copolymers, benzoguanamines, melamines, and polycarbonates.
  • the thickness of the hard coat layer 12 is preferably 1 ⁇ m or more, more preferably 3 ⁇ m or more, still more preferably 5 ⁇ m or more, from the viewpoint of ensuring the hardness of the surface of the antifouling layer 14 by ensuring the hardness of the hard coat layer 12.
  • the thickness of the hard coat layer 12 is preferably 50 ⁇ m or less, more preferably 40 ⁇ m or less, still more preferably 35 ⁇ m or less, and particularly preferably 30 ⁇ m or less, from the viewpoint of ensuring the flexibility of the optical film F.
  • the surface of the hard coat layer 12 on the adhesion layer 15 side may be surface-modified.
  • Examples of the surface modification treatment include plasma treatment, corona treatment, ozone treatment, primer treatment, glow treatment, and coupling agent treatment. From the viewpoint of ensuring a high adhesion between the hard coat layer 12 and the adhesion layer 15, the surface of the hard coat layer 12 on the adhesion layer 15 side is preferably plasma-treated.
  • the adhesion layer 15 is a layer for ensuring the adhesion of the inorganic oxide layer (in the present embodiment, the inorganic oxide base layer 13) to the transparent base material 11.
  • the adhesion layer 15 is arranged on one surface of the hard coat layer 12 in the thickness direction T.
  • Examples of the material of the adhesion layer 15 include metals such as silicon, indium, nickel, chromium, aluminum, tin, gold, silver, platinum, zinc, titanium, tungsten, zirconium, and palladium, and two or more alloys of these metals. And the oxides of these metals are mentioned.
  • both the adhesion to both the organic layer (specifically, the hard coat layer 12) and the inorganic oxide layer (specifically, the inorganic oxide base layer 13 in this embodiment) and the transparency of the adhesion layer 15 are compatible.
  • the material of the adhesion layer 15 indium tin oxide (ITO) or silicon oxide (SiOx) is preferably used.
  • SiOx having a smaller oxygen content than the stoichiometric composition is preferably used, and more preferably SiOx having x of 1.2 or more and 1.9 or less is used. ..
  • the thickness of the adhesion layer 15 is preferably 1 nm or more and 10 nm or less from the viewpoint of ensuring the adhesion between the hard coat layer 12 and the inorganic oxide base layer 13 and the transparency of the adhesion layer 15. ..
  • the inorganic oxide base layer 13 is a layer for ensuring peeling resistance in the antifouling layer 14.
  • Examples of the material of the inorganic oxide base layer 13 include silicon dioxide (SiO 2 ) and magnesium fluoride, and silicon dioxide is preferably used.
  • the thickness of the inorganic oxide base layer 13 is preferably 50 nm or more, more preferably 65 nm or more, still more preferably 80 nm or more, and particularly preferably 90 nm or more, from the viewpoint of ensuring the peeling resistance of the antifouling layer 14.
  • the thickness of the inorganic oxide base layer 13 is, for example, 300 nm or less.
  • the antifouling layer 14 is a layer having an antifouling function.
  • the antifouling layer 14 is arranged on one surface of the inorganic oxide base layer 13 in the thickness direction T.
  • the antifouling layer 14 has a surface 14a (outer surface) on one side in the thickness direction T.
  • the antifouling function of the antifouling layer 14 includes a function of suppressing the adhesion of contaminants such as hand grease to the exposed surface of the film when the optical film F is used, and a function of facilitating the removal of the adhered contaminants.
  • Examples of the material of the antifouling layer 14 include organic compounds containing a fluorine group.
  • an alkoxysilane compound having a perfluoropolyether group is preferably used.
  • Examples of the alkoxysilane compound having a perfluoropolyether group include a compound represented by the following general formula (1).
  • R 1 is a linear or branched alkyl fluoride group in which one or more hydrogen atoms in the alkyl group are replaced with a fluorine atom (for example, the number of carbon atoms is 1 or more and 20 or less).
  • R 2 represents a structure containing at least one repeating structure of a perfluoropolyether (PFPE) group, and preferably represents a structure containing two repeating structures of a PFPE group.
  • the repeating structure of the PFPE group include a repeating structure of a linear PFPE group and a repeating structure of a branched PFPE group.
  • the repeating structure of the linear PFPE group for example, a structure represented by- (OC n F 2n) p- (n represents an integer of 1 or more and 20 or less, and p is an integer of 1 or more and 50 or less. Represented. The same shall apply hereinafter).
  • Examples of the repeating structure of the branched PFPE group include a structure represented by-(OC (CF 3 ) 2 ) p- and a structure represented by-(OCF 2 CF (CF 3 ) CF 2 ) p-. Can be mentioned.
  • the repeating structure of the PFPE group is preferably a repeating structure of a linear PFPE group, and more preferably- (OCF 2 ) p- and-(OC 2 F 4 ) p- .
  • R 3 represents an alkyl group having 1 or more and 4 or less carbon atoms, and preferably represents a methyl group.
  • X represents an ether group, a carbonyl group, an amino group, or an amide group, and preferably represents an ether group.
  • M represents an integer of 1 or more. Further, m represents an integer of preferably 20 or less, more preferably 10 or less, still more preferably 5 or less.
  • the compound represented by the following general formula (2) is preferably used.
  • q represents an integer of 1 or more and 50 or less
  • r represents an integer of 1 or more and 50 or less
  • alkoxysilane compound having a perfluoropolyether group may be used alone or in combination of two or more.
  • the antifouling layer 14 is a film (dry coating film) formed by the dry coating method.
  • the dry coating method include a sputtering method, a vacuum vapor deposition method, and a CVD method.
  • the antifouling layer 14 is preferably a film (vacuum-film-deposited film) formed by a vacuum-deposited method.
  • the structure in which the material of the antifouling layer 14 contains an alkoxysilane compound having a perfluoropolyether group and the antifouling layer 14 is a dry coating film (preferably a vacuum-deposited film) is an inorganic oxide underlayer. It is suitable for ensuring a high bonding force of the antifouling layer 14 with respect to 13, and therefore suitable for ensuring the peeling resistance of the antifouling layer 14.
  • the high peel resistance of the antifouling layer 14 helps to maintain the antifouling function of the antifouling layer 14.
  • the elastic recovery rate of the surface 14a of the antifouling layer 14 measured by the nanoindentation method under the conditions of a temperature of 25 ° C. and a maximum indentation depth of 200 nm is 76% or more, preferably 80% or more, more preferably. It is 81.5% or more, more preferably 85% or more.
  • Such a configuration is suitable for suppressing the deterioration of the antifouling property of the antifouling layer 14 against the wiping work on the antifouling layer 14.
  • the elastic recovery rate of the surface 14a of the antifouling layer 14 is preferably 100% or less, more preferably 95% or less. Such a configuration is suitable for ensuring the flexibility of the antifouling layer 14, and therefore suitable for ensuring the flexibility of the optical film F.
  • the nanoindentation method is a technique for measuring various physical properties of a sample on a nanometer scale.
  • the nanoindentation method is carried out in accordance with ISO14577.
  • the process of pushing the indenter into the sample set on the stage (load application process) and the process of pulling out the indenter from the sample after that (unloading process) are carried out, and during a series of processes,
  • the load acting between the indenter and the sample and the relative displacement of the indenter with respect to the sample are measured (load-displacement measurement). This makes it possible to obtain a load-displacement curve. From this load-displacement curve, it is possible to obtain various physical properties of the measurement sample based on nanometer-scale measurement.
  • a nanoindenter (trade name "Triboindenter”, manufactured by Hysitron) can be used.
  • the measurement mode is single indentation measurement
  • the measurement temperature is 25 ° C
  • the indenter used is a Berkovich (triangular pyramid) type diamond indenter
  • the maximum indentation depth maximum indentation depth of the indenter with respect to the measurement sample in the load application process.
  • the displacement H1) is 200 nm
  • the pushing speed of the indenter is 20 nm / sec
  • the withdrawal speed of the indenter from the measurement sample in the unloading process is 20 nm / sec.
  • the maximum load Pmax (the load acting on the indenter at the maximum displacement H1) and the contact projection area Ap (the projected area of the contact area between the indenter and the sample at the maximum load).
  • the amount of plastic deformation H2 on the sample surface after the unloading process (the depth of the recess maintained on the sample surface after the indenter is separated from the sample surface) can be obtained.
  • the hardness of the surface 14a of the antifouling layer 14 at 25 ° C. measured by the nanoindentation method is preferably 1.05 GPa or more, more preferably 1.1 GPa or more, still more preferably 1.15 GPa or more, still more preferable. Is 1.2 GPa or more, particularly preferably 1.25 GPa or more, and particularly preferably 1.3 GPa or more. Such a configuration is suitable for suppressing the deterioration of the antifouling property of the antifouling layer 14 against the wiping work on the antifouling layer 14. The hardness of the surface 14a of the antifouling layer 14 at 25 ° C.
  • measured by the nanoindentation method is preferably 30 GPa or less, more preferably 20 GPa or less, still more preferably 15 GPa or less.
  • Such a configuration is suitable for ensuring the flexibility of the antifouling layer 14, and therefore suitable for ensuring the flexibility of the optical film F.
  • the water contact angle (pure water contact angle) of the surface 14a of the antifouling layer 14 is preferably 110 ° or more, preferably 111 ° or more, more preferably 112 ° or more, still more preferably 113 ° or more, and particularly preferably 113 ° or more. It is 114 ° or more.
  • the configuration in which the water contact angle on the surface 14a is as high as this is suitable for realizing high antifouling property in the antifouling layer 14.
  • the water contact angle is, for example, 130 ° or less.
  • the water contact angle is determined by forming water droplets (droplets of pure water) having a diameter of 2 mm or less on the surface 14a (exposed surface) of the antifouling layer 14 and measuring the contact angle of the water droplets with respect to the surface 14a. ..
  • the water contact angle of the surface 14a is determined by, for example, adjusting the composition of the antifouling layer 14, the roughness of the surface 14a, the composition of the hard coat layer 12, and the roughness of the surface of the hard coat layer 12 on the antifouling layer 14 side. , Can be adjusted.
  • the thickness of the antifouling layer 14 is preferably 1 nm or more, more preferably 3 nm or more, further preferably 5 nm or more, and particularly preferably 7 nm or more. Such a configuration is suitable for achieving the above-mentioned surface hardness in the antifouling layer 14.
  • the thickness of the antifouling layer 14 is preferably 25 nm or less, more preferably 20 nm or less, still more preferably 18 nm or less. Such a configuration is suitable for realizing the above-mentioned water contact angle in the antifouling layer 14.
  • the optical film F is produced by preparing the transparent base material 11 and then sequentially forming the hard coat layer 12, the adhesion layer 15, and the antifouling layer 14 on the transparent base material 11, for example, in a roll-to-roll method. can.
  • the hard coat layer 12 can be formed, for example, by applying a curable resin composition on the transparent substrate 11 to form a coating film, and then curing the coating film.
  • the curable resin composition contains an ultraviolet-type resin
  • the coating film is cured by irradiation with ultraviolet rays.
  • the curable resin composition contains a thermosetting resin
  • the coating film is cured by heating.
  • the exposed surface of the hard coat layer 12 formed on the transparent base material 11 is surface-modified, if necessary.
  • plasma treatment for example, argon gas is used as the inert gas.
  • the discharge power in the plasma processing is, for example, 10 W or more, and for example, 10000 W or less.
  • the inorganic oxide base layer 13 is formed by forming a material by a dry coating method.
  • the dry coating method include a sputtering method, a vacuum vapor deposition method, and a CVD method, and a sputtering method is preferably used.
  • a negative voltage is applied to the target placed on the cathode while introducing gas into the sputtering chamber under vacuum conditions.
  • a glow discharge is generated to ionize the gas atom, the gas ion collides with the target surface at high speed, the target material is ejected from the target surface, and the ejected target material is deposited on a predetermined surface.
  • reactive sputtering is preferable as the sputtering method.
  • a metal target is used as the target, and a mixed gas of an inert gas such as argon and oxygen (reactive gas) is used as the above-mentioned gas.
  • Examples of the power supply for carrying out the sputtering method include a DC power supply, an AC power supply, an RF power supply, and an MFAC power supply (AC power supply having a frequency band of several kHz to several MHz).
  • the discharge voltage in the sputtering method is, for example, 200 V or more, and is, for example, 1000 V or less.
  • the film forming pressure in the sputtering chamber where the sputtering method is carried out is preferably 0.01 Pa or more, more preferably 0.05 Pa or more, and further preferably 0.1 Pa or more. Such a configuration is preferable from the viewpoint of forming the antifouling layer 14 in which the material is densely deposited. Further, the film forming pressure is, for example, 2 Pa or less from the viewpoint of discharge stability.
  • the antifouling layer 14 is formed by forming, for example, an organic compound containing a fluorine group on the inorganic oxide base layer 13 by a dry coating method.
  • a dry coating method include a vacuum vapor deposition method, a sputtering method, and a CVD method, and a vacuum vapor deposition method is preferably used.
  • the optical film F can be manufactured as described above.
  • the optical film F is used with the transparent base material 11 side bonded to the adherend via, for example, an adhesive.
  • the adherend include a transparent cover arranged on the image display side of a display such as a touch panel display.
  • the optical film F is a dry coating film in which the antifouling layer 14 is arranged on the inorganic oxide base layer 13.
  • Such a configuration is suitable for ensuring a high bonding force of the antifouling layer 14 in the optical film F, and is therefore suitable for ensuring the peeling resistance of the antifouling layer 14.
  • the high peel resistance of the antifouling layer 14 helps to maintain the antifouling function of the antifouling layer 14.
  • the elastic recovery rate of the surface 14a of the antifouling layer 14 measured by the nanoindentation method under the conditions of a temperature of 25 ° C. and a maximum indentation depth of 200 nm is 76% or more as described above. It is preferably 80% or more, more preferably 81.5% or more, still more preferably 85% or more.
  • Such a configuration is suitable for suppressing the deterioration of the antifouling property of the antifouling layer 14 against the wiping work on the antifouling layer 14.
  • the optical film F is suitable for suppressing the deterioration of the antifouling property while ensuring the peeling resistance in the antifouling layer 14.
  • the optical film F may include a layer having a predetermined optical function (optical functional layer).
  • optical functional layer includes a plurality of layers, it is preferable that the layer on the surface of the antifouling layer 14 side of such an optical functional layer also serves as the above-mentioned inorganic oxide base layer 13.
  • FIG. 2 shows a case where the optical film F includes an optical functional layer 20 between the adhesion layer 15 and the antifouling layer 14.
  • the optical functional layer 20 has a layer that also serves as an inorganic oxide base layer 13 on the surface of the antifouling layer 14 side.
  • the optical functional layer 20 is arranged on one surface of the adhesion layer 15 in the thickness direction T.
  • the optical functional layer 20 is an antireflection layer for suppressing the reflection intensity of external light. That is, the optical film F is an antireflection film with an antifouling layer in this modification.
  • the optical functional layer 20 (antireflection layer) has a high refractive index layer having a relatively large refractive index and a low refractive index layer having a relatively small refractive index alternately in the thickness direction.
  • the net reflected light intensity is attenuated by the interference action between the reflected light at the plurality of interfaces in the plurality of thin layers (high refractive index layer, low refractive index layer) contained in the same layer.
  • an interference effect for attenuating the reflected light intensity can be exhibited by adjusting the optical film thickness (product of the refractive index and the thickness) of each thin layer.
  • the optical functional layer 20 as such an antireflection layer includes a first high refractive index layer 21, a first low refractive index layer 22, and a second high refractive index layer 23.
  • the first high-refractive index layer 21 and the second high-refractive index layer 23 are each made of a high-refractive index material having a refractive index of preferably 1.9 or more at a wavelength of 550 nm.
  • high refractive index materials include, for example, niobium oxide (Nb 2 O 5 ), titanium oxide, zirconium oxide, tin-doped indium oxide (ITO), and antimony.
  • Dope tin oxide (ATO) is mentioned, and niobium oxide is preferably used.
  • the optical film thickness (product of refractive index and thickness) of the first high refractive index layer 21 is, for example, 20 nm or more, and is, for example, 55 nm or less.
  • the optical film thickness of the second high-refractive index layer 23 is, for example, 60 nm or more, and for example, 330 nm or less.
  • the first low refractive index layer 22 and the second low refractive index layer 24 are each made of a low refractive index material having a refractive index of preferably 1.6 or less at a wavelength of 550 nm.
  • examples of the low refractive index material include silicon dioxide (SiO 2 ) and magnesium fluoride, and silicon dioxide is preferably used. As described above, SiO 2 and magnesium fluoride are also preferable as materials for the inorganic oxide base layer 13.
  • the optical film thickness of the first low refractive index layer 22 is, for example, 15 nm or more, and is, for example, 70 nm or less.
  • the optical film thickness of the second low refractive index layer 24 is, for example, 100 nm or more, and is, for example, 160 nm or less.
  • the first high refractive index layer 21, the first low refractive index layer 22, and the second high refractive index layer 23 can each be formed by forming a material by a dry coating method.
  • the second low refractive index layer 24, which also serves as the inorganic oxide base layer 13, is formed by forming a material by a dry coating method.
  • the dry coating method include a sputtering method, a vacuum vapor deposition method, and a CVD method, and a sputtering method is preferably used.
  • the sputtering method reactive sputtering is preferable from the viewpoint of the film forming speed.
  • the conditions of the sputtering method are the same as those described above as the conditions of the sputtering method relating to the formation of the inorganic oxide base layer 13.
  • the antifouling layer 14 is a dry coating film arranged on the second low refractive index layer 24 (inorganic oxide base layer 13).
  • the elastic recovery rate of the surface 14a of the antifouling layer 14 measured by the nanoindentation method under the conditions of a temperature of 25 ° C. and a maximum indentation depth of 200 nm is 76 as described above. % Or more, preferably 80% or more, more preferably 81.5% or more, still more preferably 85% or more.
  • Such an optical film F is suitable for suppressing a decrease in antifouling property while ensuring peeling resistance in the antifouling layer 14.
  • the present invention will be specifically described below with reference to examples.
  • the present invention is not limited to the examples.
  • the specific numerical values such as the compounding amount (content), the physical property value, the parameter, etc. described below are the compounding amounts corresponding to them described in the above-mentioned "form for carrying out the invention” (forms for carrying out the invention). It can be replaced with the upper limit (numerical value defined as “less than or equal to” or “less than”) or lower limit (numerical value defined as "greater than or equal to” or “greater than or equal to”) such as content), physical property value, and parameter.
  • a hard coat layer was formed on one side of a polyethylene terephthalate (PET) film (thickness 50 ⁇ m) as a transparent substrate (hard coat layer forming step).
  • PET polyethylene terephthalate
  • a butyl acetate solution (trade name "Unidic 17-806") of a mixture of an ultraviolet curable monomer and an oligomer (containing urethane acrylate as a main component), a solid content concentration of 80% by mass, manufactured by DIC, Inc.
  • this coating film was dried by heating and then cured by irradiation with ultraviolet rays.
  • the heating temperature was 90 ° C. and the heating time was 60 seconds.
  • a high-pressure mercury lamp was used as a light source, ultraviolet rays having a wavelength of 365 nm were used, and the integrated irradiation light amount was set to 300 mJ / cm 2 .
  • HC hard coat layer
  • the surface of the HC layer of the PET film with the HC layer was plasma-treated in a vacuum atmosphere of 1.0 Pa by a roll-to-roll type plasma processing device.
  • argon gas was used as the inert gas, and the discharge power was set to 780 W.
  • an adhesion layer and an inorganic oxide base layer were sequentially formed on the HC layer of the PET film with the HC layer after the plasma treatment (sputter film formation step).
  • an indium tin oxide (ITO) layer having a thickness of 2.0 nm as an adhesion layer and an inorganic oxide are placed on the HC layer of the PET film with an HC layer by a roll-to-roll type sputter film forming apparatus.
  • Two layers of SiO having a thickness of 165 nm as a base layer were sequentially formed.
  • an ITO target was used, an argon gas as an inert gas and 10 parts by volume of oxygen gas as a reactive gas with respect to 100 parts by volume of the argon gas were used, and the discharge voltage was set to 350 V.
  • the pressure in the film chamber was set to 0.4 Pa, and the ITO layer was formed by MFAC sputtering.
  • a Si target is used, 100 parts by volume of argon gas and 30 parts by volume of oxygen gas are used, the discharge voltage is 350 V, the film formation pressure is 0.3 Pa, and SiO 2 is formed by MFAC sputtering. Formed a layer.
  • an antifouling layer was formed (antifouling layer forming step). Specifically, an antifouling layer having a thickness of 12 nm was formed on the inorganic oxide base layer by a vacuum vapor deposition method using an alkoxysilane compound containing a perfluoropolyether group as a vapor deposition source.
  • the vapor deposition source is a solid content obtained by drying "KY1903-1" (perfluoropolyether group-containing alkoxysilane compound, solid content concentration 20% by mass) manufactured by Shin-Etsu Chemical Co., Ltd.
  • the heating temperature of the vapor deposition source in the vacuum vapor deposition method was 260 ° C.
  • the optical film of Example 1 includes a resin film, a hard coat layer, an adhesion layer, an inorganic oxide base layer, and an antifouling layer in this order toward one side in the thickness direction.
  • Example 2 The optical film of Example 2 was produced in the same manner as the optical film of Example 1 except that the thickness of the HC layer was 10 ⁇ m instead of 5 ⁇ m.
  • Example 3 Optical of Example 3 in the same manner as the optical film of Example 1 except that the thickness of the HC layer was changed to 10 ⁇ m instead of 5 ⁇ m and the thickness of the inorganic oxide base layer was changed to 100 nm instead of 165 nm. A film was made.
  • Example 4 The optical film of Example 4 was produced in the same manner as the optical film of Example 1 except that the film forming pressure at the time of forming the inorganic oxide base layer was 0.1 Pa instead of 0.3 Pa.
  • Example 5 Similar to the optical film of Example 1 except that the thickness of the HC layer was changed to 10 ⁇ m instead of 5 ⁇ m, and the film forming pressure at the time of forming the inorganic oxide base layer was changed to 0.1 Pa instead of 0.3 Pa. The optical film of Example 5 was produced.
  • Example 6 The optical film of Example 6 was produced in the same manner as the optical film of Example 1 except that the thickness of the antifouling layer was 8 nm instead of 12 nm.
  • Example 7 The optical film of Example 7 was produced in the same manner as the optical film of Example 1 except that the thickness of the antifouling layer was 6 nm instead of 12 nm.
  • Example 8 The optical film of Example 8 was produced in the same manner as the optical film of Example 1 except that the thickness of the antifouling layer was 16 nm instead of 12 nm.
  • Comparative Example 1 was carried out in the same manner as the optical film of Example 1 except that the thickness of the HC layer was changed to 10 ⁇ m instead of 5 ⁇ m and the thickness of the inorganic oxide base layer was changed to 30 nm instead of 165 nm. An optical film was produced.
  • the load-displacement measurement by the nanoindentation method was performed on the surface of the antifouling layer of each of the optical films of Examples 1 to 8 and Comparative Example 1. Specifically, first, a measurement sample (5 mm ⁇ 5 mm) was cut out from the optical film. Next, using a nano indenter (trade name "Triboindenter", manufactured by Hysitron), load-displacement measurement of the surface of the antifouling layer in the measurement sample was performed in accordance with ISO14577, and a load-displacement curve was obtained.
  • a nano indenter trade name "Triboindenter”, manufactured by Hysitron
  • the measurement mode is single indentation measurement
  • the measurement temperature is 25 ° C
  • the indenter used is a Berkovich (triangular pyramid) type diamond indenter
  • the maximum indentation depth maximum indentation depth of the indenter with respect to the measurement sample during the load application process.
  • the displacement H1) was set to 200 nm
  • the pushing speed of the indenter was set to 20 nm / sec
  • the withdrawal speed of the indenter from the measurement sample in the unloading process was set to 20 nm / sec.
  • the maximum load Pmax (the load acting on the indenter at the maximum displacement H1)
  • the contact projected area Ap (the projected area of the contact area between the indenter and the sample at the maximum load)
  • the amount of plastic deformation H2 on the sample surface after the unloading process (the depth of the recess maintained on the sample surface after the indenter is separated from the sample surface) was obtained.
  • Table 1 shows these surface hardness (GPa) and elastic recovery rate (%).
  • ⁇ Water contact angle> The water contact angle on the surface of the antifouling layer was examined for each of the optical films of Examples 1 to 8 and Comparative Example 1. First, water droplets were formed on the surface of the antifouling layer of the optical film by dropping about 1 ⁇ L of pure water. Next, the angle formed by the surface of the water droplet on the surface of the antifouling layer and the surface of the antifouling layer was measured. A contact angle meter (trade name "DMo-501", manufactured by Kyowa Interface Science Co., Ltd.) was used for the measurement. The measurement results are shown in Table 1 as the initial water contact angle ⁇ 0.
  • ⁇ Eraser sliding test> For each of the optical films of Examples 1 to 8 and Comparative Example 1, the degree of deterioration of the antifouling property on the surface of the antifouling layer by passing through the eraser sliding test was investigated. Specifically, first, a sliding test was carried out in which the eraser was reciprocated while sliding the eraser against the surface of the antifouling layer of the optical film (first eraser sliding test). In this test, an eraser ( ⁇ 6 mm) manufactured by Minoan was used, the load of the eraser on the surface of the antifouling layer was 1 kg / 6 mm ⁇ , and the sliding distance of the eraser on the surface of the antifouling layer (one way in reciprocating movement) was 20 mm.
  • the sliding speed of the eraser was set to 40 rpm, and the number of times the eraser was reciprocated with respect to the surface of the antifouling layer was set to 3000 reciprocations.
  • the water contact angle of the eraser sliding portion on the surface of the antifouling layer of the optical film was measured by the same method as the initial measurement method of the water contact angle ⁇ 0.
  • the measurement results are shown in Table 1 as the water contact angle ⁇ 1 after the first eraser sliding test.
  • FIG. 3 is a graph in which the elastic recovery rate and the water contact angle ⁇ 2 of each of the optical films of Examples 1 to 8 and Comparative Example 1 are plotted.
  • the horizontal axis represents the elastic recovery rate (%), and the vertical axis represents the water contact angle ⁇ 2 (°).
  • plots E1 to E8 represent measurement results in Examples 1 to 8
  • plot C1 represents measurement results in Comparative Example 1.
  • Each of the optical films of Examples 1 to 8 undergoes an eraser sliding test (first eraser sliding test, second eraser sliding test) as compared with the optical film of Comparative Example 1, and is an antifouling layer.
  • the degree of decrease in water contact angle on the surface is significantly small, and therefore the decrease in antifouling property is significantly small (on the surface of the antifouling layer, the smaller the decrease in water contact angle, the smaller the decrease in antifouling property).
  • the optical film with an antifouling layer of the present invention can be applied to, for example, an antireflection film with an antifouling layer, a transparent conductive film with an antifouling layer, and an electromagnetic wave shielding film with an antifouling layer.
  • Optical film (optical film with antifouling layer) 11 Transparent base material 12 Hard coat layer 13 Inorganic oxide base layer 14 Antifouling layer 14a Surface 15 Adhesive layer 20 Optical functional layer 21 First high refractive index layer 22 First low refractive index layer 23 Second high refractive index layer 24 2 Low refractive index layer

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Abstract

Selon la présente invention, le film optique (F) équipé d'une couche antisalissure est pourvu d'un matériau de base transparent (11), d'une couche de revêtement dur (12), d'une couche d'apprêt en oxyde inorganique (13) et d'une couche antisalissure (14) dans l'ordre indiqué. La couche antisalissure (14) est une membrane de revêtement à sec située sur la couche d'apprêt en oxyde inorganique (13). La recouvrance élastique mesurée par un procédé de nano-indentation à une température de 25 °C et une profondeur d'indentation maximale de 200 nm dans une surface (14a) sur le côté opposé de la couche d'apprêt en oxyde inorganique (13) dans la couche antisalissure (14) est d'au moins 76 %.
PCT/JP2021/026251 2020-07-13 2021-07-13 Film optique équipé d'une couche antisalissure WO2022014573A1 (fr)

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