WO2014119453A1 - 防汚膜付き透明基体 corps de base transparent avec film antisalissure - Google Patents

防汚膜付き透明基体 corps de base transparent avec film antisalissure Download PDF

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Publication number
WO2014119453A1
WO2014119453A1 PCT/JP2014/051291 JP2014051291W WO2014119453A1 WO 2014119453 A1 WO2014119453 A1 WO 2014119453A1 JP 2014051291 W JP2014051291 W JP 2014051291W WO 2014119453 A1 WO2014119453 A1 WO 2014119453A1
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WIPO (PCT)
Prior art keywords
transparent substrate
film
antifouling film
main surface
antifouling
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PCT/JP2014/051291
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English (en)
Japanese (ja)
Inventor
健輔 藤井
賢郎 宮村
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旭硝子株式会社
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Application filed by 旭硝子株式会社 filed Critical 旭硝子株式会社
Priority to KR1020157020526A priority Critical patent/KR101916507B1/ko
Priority to DE112014000613.0T priority patent/DE112014000613B4/de
Priority to KR1020177034773A priority patent/KR101916620B1/ko
Priority to CN201480006778.1A priority patent/CN104955783B/zh
Priority to JP2014559646A priority patent/JP5839134B2/ja
Publication of WO2014119453A1 publication Critical patent/WO2014119453A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • 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
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
    • C09D5/1662—Synthetic film-forming substance
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1681—Antifouling coatings characterised by surface structure, e.g. for roughness effect giving superhydrophobic coatings or Lotus effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/538—Roughness
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/77—Coatings having a rough surface

Definitions

  • the present invention relates to a transparent substrate with an antifouling film.
  • Patent Document 1 discloses a water-repellent glass in which a water-repellent layer is provided on the surface of a glass substrate having a concavo-convex shape as a transparent substrate having a surface subjected to antifouling treatment.
  • Patent Document 2 A method of making the surface shape of the film into a predetermined shape has been studied (for example, Patent Document 2).
  • Patent Document 2 has been developed for purposes such as windshield glass and window glass plate, and is not planned to be used as a transparent substrate for a display device or the like.
  • the water-repellent glass is used as a cover glass that is integrated with a cover member of a display device such as a liquid crystal display or a transparent electrode of a touch panel, ambient light is reflected because there is almost no anti-glare property, and the display part There was a problem that the visibility of was reduced.
  • the water-repellent glass of Patent Document 2 is a water-repellent glass that is planned to be used for a portion such as a window glass that has little chance of being touched by human hands. Durability was not sufficient for use as a substrate integrated with a cover member or touch panel that may be touched.
  • the present invention has been made in view of the above-mentioned problems of the prior art, and an object of the present invention is to provide a transparent substrate with an antifouling film having antiglare properties and improved durability of the antifouling film.
  • the present invention has a first main surface and a second main surface opposite to the first main surface, and an anti-glare process is applied to the surface of the first main surface.
  • a transparent substrate A fluorine-containing organosilicon compound film that is an antifouling film provided on the first main surface side of the transparent substrate, Provided is a transparent substrate with an antifouling film, wherein the antifouling film has a surface roughness RMS of 0.05 ⁇ m or more and 0.25 ⁇ m or less, and an average length RSm of elements of the roughness curve is 10 ⁇ m or more and 40 ⁇ m or less.
  • the transparent substrate with an antifouling film of the present embodiment has a first main surface and a second main surface opposite to the first main surface, and an anti-glare process on the surface of the first main surface. And a fluorine-containing organosilicon compound film that is an antifouling film provided on the first main surface side of the transparent substrate.
  • the antifouling film has a surface roughness RMS of 0.05 ⁇ m or more and 0.25 ⁇ m or less, and an average length RSm of elements of the roughness curve is 10 ⁇ m or more and 40 ⁇ m or less.
  • FIG. 1 schematically shows a cross-sectional view of a transparent substrate with an antifouling film of the present embodiment, and has a configuration in which an antifouling film 12 is disposed on the first main surface side of the transparent substrate 11. ing.
  • an antifouling film 12 is disposed on the first main surface side of the transparent substrate 11. ing.
  • the material of the transparent substrate 11 is not particularly limited, and various transparent substrates that transmit at least visible light can be used. Examples thereof include various materials such as a plastic substrate and a glass substrate. Among them, the transparent substrate is preferably a glass substrate from the viewpoints of transparency and strength. In this case, the type of glass is not particularly limited, and various types of glass such as alkali-free glass, soda lime glass, and aluminosilicate glass can be used. Among these, soda lime glass is preferably used from the viewpoint of adhesion to a layer (film) provided on the upper surface.
  • the transparent substrate 11 is a glass substrate
  • a tempered glass substrate for example, “Dragon Trail (registered trademark)” obtained by chemically strengthening aluminosilicate glass.
  • the chemical strengthening treatment refers to a treatment of substituting alkali ions (for example, sodium ions) having a small ionic radius on the glass surface with alkali ions (for example, potassium ions) having a large ionic radius.
  • alkali ions for example, sodium ions
  • the glass containing sodium ions can be chemically strengthened by treating with a molten salt containing potassium ions.
  • the composition of the compressive stress layer on the surface of the glass substrate after such chemical strengthening treatment is slightly different from the composition before chemical strengthening treatment, but the composition of the substrate deep layer portion is almost the same as the composition before chemical strengthening treatment.
  • the conditions for chemical strengthening are not particularly limited, and can be selected according to the type of glass used for chemical strengthening and the required degree of chemical strengthening.
  • the molten salt for performing the chemical strengthening treatment may be selected according to the glass substrate subjected to chemical strengthening.
  • examples thereof include alkali sulfates and alkali chlorides such as potassium nitrate, sodium sulfate, potassium sulfate, sodium chloride and potassium chloride. These molten salts may be used alone or in combination of two or more.
  • the heating temperature of the molten salt is preferably 350 ° C. or higher, and more preferably 380 ° C. or higher. Moreover, 500 degrees C or less is preferable and 480 degrees C or less is more preferable.
  • the heating temperature of the molten salt By setting the heating temperature of the molten salt to 350 ° C. or higher, it is possible to prevent chemical strengthening from becoming difficult due to a decrease in the ion exchange rate. Moreover, decomposition
  • the time for bringing the glass substrate into contact with the molten salt is preferably 1 hour or longer and more preferably 2 hours or longer in order to give sufficient compressive stress.
  • the time for bringing the glass substrate into contact with the molten salt is preferably 1 hour or longer and more preferably 2 hours or longer in order to give sufficient compressive stress.
  • productivity falls and a compressive stress value falls by relaxation, 24 hours or less are preferable and 20 hours or less are more preferable.
  • the shape of the transparent substrate is not particularly limited, and various shapes of transparent substrates can be used.
  • the transparent substrate 11 has the first main surface 11A and the second main surface 11B facing the first main surface 11A.
  • the first main surface 11A is subjected to an antiglare process for forming a desired uneven shape.
  • the RMS which is the surface roughness of the first main surface 11A is 0.05 ⁇ m or more and 0.25 ⁇ m or less
  • the RSm which is the average length of the elements of the roughness curve of the first main surface 11A is 10 ⁇ m or more and 40 ⁇ m or less. It is preferable that By setting it as such a range, the surface roughness RMS of the antifouling film described later and the average length RSm of the elements of the roughness curve can be set as desired ranges.
  • the surface roughness RMS is the average depth of irregularities from the reference surface (here, the substrate surface before the surface treatment). In addition, it is also called a root mean square roughness and may be represented by Rq.
  • the average length RSm of the elements of the roughness curve is a length obtained by averaging the lengths on the reference surface where irregularities for one period are generated in the roughness curve included in the reference length taken on the reference surface. is there.
  • the surface roughness RMS ( ⁇ m) and the average length RSm of the elements of the roughness curve can be measured by a method based on the method defined in JIS B 0601 (2001).
  • the surface characteristics of the first main surface 11A have the above characteristics.
  • the durability of the antifouling film is particularly improved as compared with a conventional transparent substrate with an antifouling film.
  • the antifouling film is formed on the first main surface side of the transparent substrate, and the antifouling film traces the surface shape of the transparent substrate, the antifouling film surface has the same surface roughness characteristics as the transparent substrate. Have.
  • the first main surface 11A of the transparent substrate satisfies the above-mentioned definition, it is compared with a conventionally used transparent substrate that has been subjected to an antiglare process in which RMS exceeds 0.25 ⁇ m or RSm exceeds 40 ⁇ m.
  • RMS exceeds 0.25 ⁇ m or RSm exceeds 40 ⁇ m.
  • the fine unevenness of the first main surface of the transparent substrate it means that the pitch between the concave portions is reduced and the area of the convex portions is increased.
  • the surface of the antifouling film also has the same surface shape.
  • the surface of the transparent substrate with the antifouling film that is, when a finger or the like comes into contact with the antifouling film, the area of the convex portion of the antifouling film that comes into contact with the finger or the like is compared with the conventional transparent substrate with the antifouling film. It is getting bigger. For this reason, it is estimated that the force applied to the surface (antifouling film) part of the transparent substrate with antifouling film is dispersed by fingers, etc., the pressure applied to the antifouling film can be reduced, and peeling and abrasion of the antifouling film can be suppressed Is done.
  • RSm that is the average length of the elements of the roughness curve, that is, the smaller the pitch of the recesses, the greater the contact area with the finger and the more the durability.
  • an etching process using a photomask or the like needs to be performed. From the viewpoint of cost, it can be preferably created if RSm is 10 ⁇ m or more. For this reason, it is preferable to use the transparent base
  • the RMS which is the surface roughness of the first main surface 11A is more preferably 0.08 ⁇ m or more and 0.20 ⁇ m or less, and the RSm which is the average length of the elements of the roughness curve is 15 ⁇ m or more and 35 ⁇ m or less. It is more preferable. By satisfying these parameters, it is possible to further improve the durability of the antifouling film.
  • the anti-glare processing method for forming a transparent substrate having such surface characteristics is not particularly limited, and a method of performing surface treatment on the first main surface to form desired irregularities can be used.
  • the frost treatment can be performed, for example, by immersing a transparent substrate, which is an object to be processed, in a mixed solution of hydrogen fluoride and ammonium fluoride and chemically treating the immersion surface.
  • a chemical treatment method for example, a so-called sand blast treatment in which crystalline silicon dioxide powder, silicon carbide powder or the like is sprayed onto the surface of the transparent substrate with pressurized air, crystalline silicon dioxide powder, silicon carbide, etc. It is also possible to use a method based on physical treatment such as polishing a brush to which powder or the like is adhered with water dampened with water.
  • microcracks on the surface of the object to be treated are unlikely to occur, and mechanical strength is unlikely to decrease. It can preferably be used as a method of applying.
  • the glass surface is chemically etched in order to adjust the surface shape.
  • the haze can be adjusted to a desired value depending on the etching amount, cracks generated by sandblasting or the like can be removed, and glare can be suppressed.
  • etching a method of immersing a transparent substrate as an object to be processed in a solution containing hydrogen fluoride as a main component is preferably used.
  • Components other than hydrogen fluoride may include hydrochloric acid, nitric acid, citric acid, and the like. By containing these, it can suppress that the alkaline component and hydrogen fluoride which are contained in glass react, and local precipitation reaction arises, and can make etching progress uniformly in a surface.
  • the characteristics of the second main surface 11B of the transparent substrate are not particularly limited, and have the same surface roughness RMS as the first main surface and RSm that is the average length of the elements of the roughness curve. Can also be processed.
  • a transparent electrode for a touch panel can be formed on the second main surface 11B of the transparent substrate.
  • a transparent electrode for a touch panel can be formed on the second main surface 11B of the transparent substrate.
  • membrane 12 is formed in the 1st main surface 11A side of the transparent base
  • the antifouling film 12 can be composed of a fluorine-containing organosilicon compound.
  • the fluorine-containing organosilicon compound used in this embodiment is not particularly limited as long as it imparts antifouling properties, water repellency, and oil repellency.
  • Examples of such a fluorine-containing organosilicon compound include a fluorine-containing organosilicon compound having one or more groups selected from the group consisting of a polyfluoropolyether group, a polyfluoroalkylene group, and a polyfluoroalkyl group.
  • the polyfluoropolyether group is a divalent group having a structure in which polyfluoroalkylene groups and etheric oxygen atoms are alternately bonded.
  • fluorine-containing organosilicon compound having one or more groups selected from the group consisting of a polyfluoropolyether group, a polyfluoroalkylene group and a polyfluoroalkyl group include the following general formulas (I) to (V): The compound etc. which are represented by these are mentioned.
  • Rf is a linear polyfluoroalkyl group having 1 to 16 carbon atoms (alkyl group such as methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, etc.), and X is hydrogen An atom or a lower alkyl group having 1 to 5 carbon atoms (eg, methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, etc.), R1 is a hydrolyzable group (eg, amino group, alkoxy group) Or a halogen atom (for example, fluorine, chlorine, bromine, iodine, etc.), m is an integer of 1 to 50, preferably 1 to 30, n is an integer of 0 to 2, preferably 1 to 2, and p is 1 to It is an integer of 10, preferably 1-8.
  • alkyl group such as methyl group, ethyl group, n-propy
  • Examples of the compound represented by the general formula (II) include n-trifluoro (1,1,2,2-tetrahydro) propylsilazane (n-CF 3 CH 2 CH 2 Si (NH 2 ) 3 ), n-heptafluoro. Examples thereof include (1,1,2,2-tetrahydro) pentylsilazane (nC 3 F 7 CH 2 CH 2 Si (NH 2 ) 3 ).
  • q ′ is an integer of 1 or more, preferably 1-20.
  • Examples of the compound represented by the general formula (III) include 2- (perfluorooctyl) ethyltrimethoxysilane (n—C 8 F 17 CH 2 CH 2 Si (OCH 3 ) 3 ).
  • R f2 is — (OC 3 F 6 ) s — (OC 2 F 4 ) t — (OCF 2 ) u — (s, t and u are each independently an integer of 0 to 200)
  • R 2 and R 3 each independently represents a monovalent hydrocarbon group having 1 to 8 carbon atoms (for example, methyl group, ethyl group, n-propyl group). Group, isopropyl group, n-butyl group and the like.
  • X 2 and X 3 are independently hydrolyzable groups (for example, amino group, alkoxy group, acyloxy group, alkenyloxy group, isocyanate group, etc.) or halogen atoms (for example, fluorine atom, chlorine atom, bromine atom, iodine atom)
  • D and e are independently an integer of 1 to 2
  • c and f are independently an integer of 1 to 5 (preferably 1 to 2)
  • a and b are independently 2 or 3 is there.
  • s + t + u is preferably 20 to 300, and more preferably 25 to 100.
  • R 2 and R 3 are more preferably a methyl group, an ethyl group, or a butyl group.
  • the hydrolyzable group represented by X 2 or X 3 is more preferably an alkoxy group having 1 to 6 carbon atoms, particularly preferably a methoxy group or an ethoxy group. Further, a and b are each preferably 3.
  • v is an integer of 1 to 3
  • w, y and z are each independently an integer of 0 to 200
  • h is 1 or 2
  • i is an integer of 2 to 20.
  • X 4 is a hydrolyzable group
  • R 4 is a linear or branched hydrocarbon group having 1 to 22 carbon atoms
  • k is an integer of 0 to 2.
  • w + y + z is preferably 20 to 300, and more preferably 25 to 100.
  • i is more preferably 2 to 10.
  • X 4 is preferably an alkoxy group having 1 to 6 carbon atoms, more preferably a methoxy group or an ethoxy group.
  • R 4 is more preferably an alkyl group having 1 to 10 carbon atoms.
  • fluorine-containing organosilicon compound having one or more groups selected from the group consisting of a commercially available polyfluoropolyether group, polyfluoroalkylene group and polyfluoroalkyl group, KP-801 (trade name, Shin-Etsu Chemical Co., Ltd.) KY178 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.), KY-130 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.), OPTOOL (registered trademark) DSX and OPTOOL AES (both trade names, manufactured by Daikin) and the like can be preferably used.
  • KP-801 trade name, Shin-Etsu Chemical Co., Ltd.
  • KY178 trade name, manufactured by Shin-Etsu Chemical Co., Ltd.
  • KY-130 trade name, manufactured by Shin-Etsu Chemical Co., Ltd.
  • OPTOOL registered trademark
  • DSX and OPTOOL AES both trade names, manufactured by Daikin
  • fluorine-containing organosilicon compounds are stored in a mixture with a solvent such as a fluorinated solvent in order to suppress deterioration due to reaction with moisture in the atmosphere. If it is subjected to the film forming process as it is, the durability of the obtained thin film may be adversely affected.
  • the fluorine-containing organosilicon compound that has been subjected to the solvent removal treatment before heating in the heating container, or the fluorine-containing organosilicon that has not been diluted with the solvent (no solvent added) It is preferable to use a compound.
  • the concentration of the solvent contained in the fluorine-containing organosilicon compound solution is preferably 1 mol% or less, more preferably 0.2 mol% or less. It is particularly preferable to use a fluorine-containing organosilicon compound that does not contain a solvent.
  • Examples of the solvent used for storing the fluorine-containing organosilicon compound include perfluorohexane, metaxylene hexafluoride (C 6 H 4 (CF 3 ) 2 ), hydrofluoropolyether, HFE7200 / 7100 (trade name, manufactured by Sumitomo 3M Ltd., HFE7200 is represented by C 4 F 9 C 2 H 5 , and HFE 7100 is represented by C 4 F 9 OCH 3 ).
  • the removal treatment of the solvent (solvent) from the fluorine-containing organosilicon compound solution containing the fluorine-based solvent can be performed, for example, by evacuating a container containing the fluorine-containing organosilicon compound solution.
  • the time for evacuation is not limited because it varies depending on the exhaust capacity of the exhaust line, the vacuum pump, etc., the amount of the solution, etc. For example, it may be about 10 hours or more.
  • the method of forming the antifouling film of this embodiment is not particularly limited, but it is preferable to form the film by vacuum deposition using the above materials.
  • the solvent removal treatment is performed by evacuating the heating container at room temperature after introducing the fluorine-containing organosilicon compound solution into the heating container of the film forming apparatus for forming the antifouling film and before raising the temperature. You can also. Further, the solvent can be removed beforehand by an evaporator or the like before being introduced into the heating container.
  • the fluorine-containing organosilicon compound having a small or no solvent content is more likely to be deteriorated by contact with the atmosphere as compared with the one containing the solvent.
  • storage containers for fluorine-containing organosilicon compounds with low (or no) solvent content should be replaced with an inert gas such as nitrogen and sealed, and exposed to the atmosphere when handled. It is preferable to shorten the contact time.
  • the fluorine-containing organosilicon compound into a heating container of a film forming apparatus for forming an antifouling film immediately after opening the storage container.
  • transduction it is preferable to remove the air
  • the storage container and the heating container are more preferably connected by a pipe with a valve so that the storage container (storage container) can be introduced into the heating container of the present manufacturing apparatus without coming into contact with the atmosphere.
  • the present invention is not limited to this.
  • a so-called deposition pellet in which a certain amount of a fluorine-containing organosilicon compound is impregnated with a porous metal (for example, tin or copper) or a fibrous metal (for example, stainless steel) is commercially available.
  • a method of using this for example, Surf Clear manufactured by Canon Optron.
  • the antifouling film can be easily formed using the amount of pellets corresponding to the capacity of the vapor deposition apparatus and the required film thickness as the vapor deposition source.
  • the surface roughness RMS is 0.05 ⁇ m or more and 0.25 ⁇ m or less, and the average length RSm of the elements of the roughness curve is 10 ⁇ m or more and 40 ⁇ m or less.
  • the surface roughness RMS is more preferably 0.08 ⁇ m or more and 0.20 ⁇ m or less, and the average length RSm of the elements of the roughness curve is more preferably 15 ⁇ m or more and 35 ⁇ m or less.
  • an adhesion layer may be inserted between the transparent substrate and the antifouling film.
  • the adhesion layer When the adhesion layer is inserted, it may be formed in advance on the first main surface of the transparent substrate before forming the antifouling film.
  • a silicon oxide film is preferably used as the adhesion layer.
  • the film thickness is 2 nm to 50 nm, preferably 5 nm to 20 nm.
  • the haze of the transparent substrate with an antifouling film according to this embodiment is preferably 2% or more and 30% or less. If the haze is 2% or more, the reflection of light can be confirmed visually and compared with a substrate that has not been antiglare processed, but if it exceeds 30%, the light will be diffusely reflected. This is because, when used as a substrate integrated with a cover member or a touch panel of the display device, the display visibility of the display device is lowered. Further, the haze of the transparent substrate with an antifouling film of the present embodiment is more preferably 15% or more and 27% or less.
  • the haze in the above range indicates that the transparent substrate with the antifouling film of this embodiment has sufficient antiglare properties, and can be more preferably used as a substrate integrated with a cover member or a touch panel of a display device or the like. .
  • the transparent substrate with an antifouling film of the present embodiment it is possible to provide a transparent substrate with an antifouling film having antiglare properties and improved durability of the antifouling film.
  • a configuration in which a low reflection film is further provided in the first embodiment will be described. Since other configurations are the same as those described in the first embodiment, they are omitted here.
  • the low-reflection film can suppress the reflection of light on the surface of the transparent substrate with the antifouling film, so that the antiglare property can be further improved.
  • the antiglare property can be further improved.
  • when used as a cover member of a display device it is possible to suppress the reflection of ambient light and further improve the display visibility of the display device.
  • the material of the low reflection film is not particularly limited, and various materials can be used as long as the material can suppress reflection.
  • the low reflective film can be configured by laminating a high refractive index layer and a low refractive index layer.
  • the high-refractive index layer and the low-refractive index layer may each include one layer, but may include two or more layers. When two or more high refractive index layers and low refractive index layers are included, it is preferable that the high refractive index layers and the low refractive index layers are alternately laminated.
  • the low reflection film is preferably a laminate in which a plurality of films (layers) are laminated.
  • the laminate preferably has a total of 2 or more and 6 or less layers, more preferably 2 or more and 4 or less layers.
  • the laminate here is preferably a laminate in which a high refractive index layer and a low refractive index layer are laminated as described above, and the total number of layers of the high refractive index layer and the low refractive index layer is the above. A range is preferable.
  • the materials of the high refractive index layer and the low refractive index layer are not particularly limited, and can be selected in consideration of the required degree of antireflection, productivity, and the like.
  • Examples of the material constituting the high refractive index layer include niobium oxide (Nb 2 O 5 ), titanium oxide (TiO 2 ), zirconium oxide (ZrO 2 ), silicon nitride (SiN), and tantalum oxide (Ta 2 O 5 ).
  • niobium oxide Nb 2 O 5
  • titanium oxide TiO 2
  • zirconium oxide ZrO 2
  • silicon nitride SiN
  • tantalum oxide Ta 2 O 5
  • silicon oxide (SiO 2 ) can be preferably used as a material constituting the low refractive index layer.
  • the low reflection film is more preferably a laminate of a niobium oxide layer and a silicon oxide layer.
  • the place where the low reflection film is provided is not particularly limited, and can be disposed on the first main surface 11A and / or the second main surface 11B of the transparent substrate. . It is particularly preferable to provide the first main surface 11A of the transparent substrate.
  • the low reflection film 13 and the fluorine-containing organosilicon compound coating 12 are laminated in this order on the surface of the first main surface 11A of the transparent substrate 11 (from the first main surface side). It is more preferable.
  • the low reflection film 13 and the fluorine-containing organic silicon compound film (antifouling film) 12 are laminated on the first main surface 11A of the transparent substrate, whereby the low reflection film 13 is also peeled off. It is preferable because it can prevent and improve durability.
  • the silicon oxide film is preferably used.
  • the uppermost layer of the low reflection film is also silicon oxide as in the above example, the low reflectivity and the effect of the adhesion layer can be achieved at the same time. Therefore, this is a preferable configuration.
  • the low reflection film 13 has a configuration in which two layers 131 and 132 are stacked.
  • the present invention is not limited to such a configuration, and a configuration in which a plurality of layers are further stacked as described above. You can also.
  • the haze is preferably 2% or more and 30% or less, and preferably 15% or more and 27% or less for the same reason described in the first embodiment. More preferred.
  • the transparent substrate with an antifouling film having a low reflection film has been described.
  • the antiglare property can be further improved by having such a configuration. For this reason, it can be more preferably used in applications that require anti-glare properties such as a cover device of a display device and a substrate integrated with a touch panel.
  • Examples 1 to 4 are examples, and examples 5 to 7 are comparative examples.
  • (1) Evaluation Method A method for evaluating the characteristics of the transparent substrate with an antifouling film obtained in Examples 1 to 7 below will be described below.
  • (Surface shape measurement) About the surface shape of the antifouling film of the sample after forming the antifouling film used in Examples 1 to 7, using a laser microscope (manufactured by Keyence Corporation, trade name: VK-9700), a planar profile at a magnification of 50 times was measured. Then, from the obtained planar profile, values of the surface roughness RMS and the average length RSm of the roughness curve elements were obtained based on JIS B 0601 (2001).
  • the surface uneven structure substantially traces the surface shape of the transparent substrate as it is. Therefore, the surface shape of the transparent substrate (on the surface on which the antifouling film is formed) is considered to be equivalent.
  • permeation haze was measured for samples after the antifouling film was formed. The haze measurement was performed using a haze meter (manufactured by Suga Test Instruments Co., Ltd., model: HZ-V3).
  • Rubbing durability (wear resistance) test) was conducted on the antifouling film of the sample according to the following procedure.
  • the antifouling films of Examples 1 to 7 were subjected to a rubbing test according to the following procedure.
  • the steel wool # 0000 was attached to the surface of a flat metal indenter having a bottom surface of 10 mm ⁇ 10 mm, and a friction member for rubbing the sample was obtained.
  • a rubbing test was carried out using the above-mentioned friction element with a plane abrasion tester triple type (manufactured by Daiei Kagaku Seiki Co., Ltd., model: PA-300A). Specifically, first, the indenter is attached to a wear tester so that the bottom surface of the indenter contacts the antifouling film surface of the sample, and a weight is placed so that the load on the friction element is 1000 g, the average speed is 6400 mm / min, one way Reciprocated at 40 mm. The test was performed so that one reciprocation was counted as one rubbing and the number of rubbing was 1000.
  • a plane abrasion tester triple type manufactured by Daiei Kagaku Seiki Co., Ltd., model: PA-300A.
  • the water contact angle of the antifouling film is measured by dropping 1 ⁇ L of pure water onto the antifouling film using an automatic contact angle meter (manufactured by Kyowa Interface Science Co., Ltd., model: DM-501) and measuring the contact angle. Was done. In the measurement, each sample was measured at 10 locations on the antifouling film surface, and the average value was taken as the water contact angle after the durability test of the sample.
  • an automatic contact angle meter manufactured by Kyowa Interface Science Co., Ltd., model: DM-501
  • a glass substrate (trade name: Dragon Trail (registered trademark) manufactured by Asahi Glass Co., Ltd.) subjected to chemical strengthening treatment is used as a transparent substrate, and a predetermined frost treatment is performed on the first main surface of the glass substrate.
  • a glass substrate (hereinafter referred to as a transparent substrate A) was used.
  • an antifouling film was formed on the first main surface of the transparent substrate A by the following procedure.
  • a fluorine-containing organosilicon compound manufactured by Shin-Etsu Chemical Co., Ltd., trade name: KY-185
  • a heating vessel was degassed with a vacuum pump for 10 hours or more, and the solvent in the solution was removed to obtain a composition for forming a fluorine-containing organosilicon compound film.
  • the heating container containing the composition for forming the fluorine-containing organosilicon compound film was heated to 270 ° C. After reaching 270 ° C., that state was maintained for 10 minutes until the temperature stabilized.
  • the film thickness is measured with a quartz crystal monitor installed in a vacuum chamber, and film formation is performed until the film thickness of the fluorine-containing organosilicon compound film formed on the transparent substrate A reaches 10 nm. went. *
  • the extracted transparent substrate A on which the fluorine-containing organosilicon compound film was formed was placed on a hot plate with the film surface facing upward, and heat-treated in the atmosphere at 150 ° C. for 60 minutes.
  • Example 2 Using a glass substrate (trade name: Dragon Trail (registered trademark) manufactured by Asahi Glass Co., Ltd.) subjected to chemical strengthening treatment as a transparent substrate, and using a transparent substrate B subjected to frost treatment on the first main surface of the glass substrate An antifouling film was formed on the first main surface of the transparent substrate B in the same manner as in Example 1 except that. The obtained transparent substrate with an antifouling film was evaluated in the same manner as in Example 1. The results are shown in Table 1.
  • Example 3 Using a glass substrate (trade name: Dragon Trail (registered trademark) manufactured by Asahi Glass Co., Ltd.) subjected to chemical strengthening treatment as a transparent substrate, and using a transparent substrate C subjected to frost treatment on the first main surface of the glass substrate An antifouling film was formed on the first main surface of the transparent substrate C in the same manner as in Example 1 except that. The obtained transparent substrate with an antifouling film was evaluated in the same manner as in Example 1. The results are shown in Table 1. [Example 4] On the transparent substrate A, a low reflection film was formed as follows.
  • Pulse sputtering was performed under the conditions of 0.8 W / cm 2 and inversion pulse width of 5 ⁇ sec to form a high refractive index layer made of niobium oxide (niobium) having a thickness of 13 nm on the first main surface of the transparent substrate A.
  • niobium oxide target manufactured by AGC Ceramics, trade name: NBO target
  • Pulse sputtering was performed under the conditions of 8 W / cm 2 and inversion pulse width of 5 ⁇ sec, and a high refractive index layer made of niobium oxide (niobium) having a thickness of 110 nm was formed on the low refractive index layer.
  • pulse sputtering was performed under the condition of a pulse width of 5 ⁇ sec to form a low refractive index layer made of silicon oxide (silica) having a thickness of 90 nm.
  • Example 5 The obtained transparent substrate with an antifouling film was evaluated in the same manner as in Example 1. The results are shown in Table 1.
  • Example 5 Using a glass substrate (trade name: Dragon Trail (registered trademark) manufactured by Asahi Glass Co., Ltd.) subjected to chemical strengthening treatment as a transparent substrate, and using a transparent substrate D subjected to frost treatment on the first main surface of the glass substrate An antifouling film was formed on the first main surface of the transparent substrate D in the same manner as in Example 1 except that.
  • the obtained transparent substrate with an antifouling film was evaluated in the same manner as in Example 1. The results are shown in Table 1.
  • Example 6 Using a glass substrate (trade name: Dragon Trail (registered trademark) manufactured by Asahi Glass Co., Ltd.) that has been chemically strengthened as a transparent substrate, and using a transparent substrate E that is frosted on the first main surface of the glass substrate An antifouling film was formed on the first main surface of the transparent substrate E in the same manner as in Example 1 except that.
  • the obtained transparent substrate with an antifouling film was evaluated in the same manner as in Example 1. The results are shown in Table 1.
  • Example 7 A low reflection film and an antifouling film were formed in the same manner as in Example 4 except that the same transparent substrate D as in Example 5 was used as the transparent substrate, and the obtained transparent substrate with an antifouling film was the same as in Example 1. Evaluation was performed. The results are shown in Table 1.
  • the antifouling film has water repellency, and when the water contact angle is small as described above, it indicates that the antifouling film is peeled off and worn. Therefore, in Examples 5 to 7, it can be seen that the antifouling film is peeled off and worn.
  • Examples 1 to 4 have appropriate anti-glare properties from the haze value.

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Abstract

L'invention fournit un corps de base transparent avec film antisalissure qui possède : un corps de base transparent qui possède une première face principale ainsi qu'une seconde face principale s'opposant à la première, et à la surface de la première face principale duquel un usinage antireflet est exécuté ; et un revêtement de composé de silicium organique comprenant une fluorine constituant un film antisalissure agencé côté de ladite première face principale dudit corps de base transparent. Ce corps de base transparent avec film antisalissure présente une rugosité de surface (RMS) dudit film antisalissure supérieure ou égale à 0,05µm et inférieure ou égale à 0,25µm, et une longueur moyenne (RSm) d'un élément de sa courbe de rugosité, est supérieure ou égale à 10µm et inférieure ou égale à 40µm.
PCT/JP2014/051291 2013-01-30 2014-01-22 防汚膜付き透明基体 corps de base transparent avec film antisalissure WO2014119453A1 (fr)

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DE112014000613.0T DE112014000613B4 (de) 2013-01-30 2014-01-22 Transparenter Grundkörper mit Belag-hemmender Beschichtung
KR1020177034773A KR101916620B1 (ko) 2013-01-30 2014-01-22 방오막이 형성된 투명 기체
CN201480006778.1A CN104955783B (zh) 2013-01-30 2014-01-22 带防污膜的透明基体
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KR20170137223A (ko) 2017-12-12
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CN108129032B (zh) 2020-11-03
DE112014000613T5 (de) 2015-10-29
TW201434775A (zh) 2014-09-16
DE112014000613B4 (de) 2019-05-29
JP2016052992A (ja) 2016-04-14
CN104955783A (zh) 2015-09-30
TWI596069B (zh) 2017-08-21
KR20150112972A (ko) 2015-10-07
KR101916507B1 (ko) 2018-11-07
JP5839134B2 (ja) 2016-01-06
KR101916620B1 (ko) 2018-11-07
JP6075435B2 (ja) 2017-02-08
JPWO2014119453A1 (ja) 2017-01-26

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