US20170129806A1 - Cover glass - Google Patents

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Publication number
US20170129806A1
US20170129806A1 US15/404,609 US201715404609A US2017129806A1 US 20170129806 A1 US20170129806 A1 US 20170129806A1 US 201715404609 A US201715404609 A US 201715404609A US 2017129806 A1 US2017129806 A1 US 2017129806A1
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Prior art keywords
cover glass
glass
treatment
antireflection film
values
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Abandoned
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US15/404,609
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English (en)
Inventor
Kensuke Fujii
Shinji Kobune
Minoru Tamada
Hitoshi Mishiro
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AGC Inc
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Asahi Glass Co Ltd
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Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Assigned to ASAHI GLASS COMPANY, LIMITED reassignment ASAHI GLASS COMPANY, LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: TAMADA, MINORU, FUJII, KENSUKE, KOBUNE, SHINJI, MISHIRO, HITOSHI
Publication of US20170129806A1 publication Critical patent/US20170129806A1/en
Assigned to AGC Inc. reassignment AGC Inc. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: ASAHI GLASS COMPANY, LIMITED
Priority to US17/335,309 priority Critical patent/US20210284571A1/en
Abandoned legal-status Critical Current

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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
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
    • 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
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • 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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • 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
    • 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
    • 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
    • C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
    • 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
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • 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
    • C03C4/00—Compositions for glass with special properties
    • C03C4/18—Compositions for glass with special properties for ion-sensitive glass
    • 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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • C09D5/006—Anti-reflective coatings
    • 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
    • C09D5/1675—Polyorganosiloxane-containing compositions
    • 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
    • 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
    • G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
    • G02B27/0006—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00 with means to keep optical surfaces clean, e.g. by preventing or removing dirt, stains, contamination, condensation
    • 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
    • C03C2204/00—Glasses, glazes or enamels with special properties
    • 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
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/218—V2O5, Nb2O5, Ta2O5
    • 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
    • C03C2217/73—Anti-reflective coatings with specific characteristics
    • 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
    • C03C2217/73—Anti-reflective coatings with specific characteristics
    • C03C2217/734—Anti-reflective coatings with specific characteristics comprising an alternation of high and low refractive indexes
    • 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/154—Deposition methods from the vapour phase by sputtering
    • 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/31—Pre-treatment
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0268—Diffusing elements; Afocal elements characterized by the fabrication or manufacturing method

Definitions

  • the present invention relates to a cover glass.
  • a glass substrate surface is subjected to an antiglare treatment (AG treatment).
  • AG treatment antiglare treatment
  • a glass substrate surface is subjected to a chemical or physical surface treatment to form irregularities and this surface is then etched with, for example, hydrofluoric acid in order to arrange the surface shape (Patent Document 1).
  • the present inventors have found that the above problem(s) could be solved by the cover glass having no leach-out layer. That is, the present invention relates to the following cover glass.
  • cover glass according to any one of [1] to [8], further comprising an antifouling film disposed on the antireflection film, wherein a contact angle of water on a surface of the cover glass on the side where the antifouling film is present is 90° or larger.
  • FIG. 1A to FIG. 1D are a flowchart which shows steps of one embodiment of the production process in the present invention.
  • the cover glass of the present invention includes: a glass substrate having a convex and concave shape formed on at least one of surfaces thereof by an antiglare treatment; and an antireflection film disposed on the surface of the glass substrate, the surface having the convex and concave shape, and in the cover glass, a difference ⁇ a* in a* value between any two points within a surface of the glass on the side where the antireflection film is present and a difference ⁇ b* in b* value between any two points within the surface of the glass on the side where the antireflection film is present satisfy the following expression (1).
  • the ⁇ a* and the ⁇ b* should be determined by selecting any square portion of 10 cm 2 as a measuring range from the glass substrate, dividing the measuring range into 11 x 11 equal portions, examining all 100 intersections of equally dividing lines for a* values and b* values, determining a maximum value a* max of the a* values, a minimum value a* min of the a* values, a maximum value b* max of the b* values, and a minimum value b* min of the b* values, from the a* values and b* values, and taking the difference (a* max ⁇ a* min ) between the a* max and the a* min as the ⁇ a* and the difference (b* max ⁇ b* min ) between the b* max and the b* min as the ⁇ b*.
  • the glass composition of the extremely thin surface region can be determined, for example, by X-ray photoelectron spectroscopy (XPS).
  • the glass composition of the bulk part can be determined, for example, by XPS, X-ray fluorescence analysis (XRF), etc.
  • the thickness of the ion-exchange layer before the removal, i.e., the leach-out layer, as measured from the outermost surface of the glass substrate is preferably 10 nm or less, more preferably 8 nm or less, even more preferably 6 nm or less. It is also preferable that the thickness of the ion-exchange layer before the removal, i.e., the leach-out layer, should be larger than 1 nm. So long as the thickness of the leach-out layer before the removal is 10 nm or less, not only this leach-out layer can be efficiently removed, but also a suitable antiglare effect and even reflection properties can be finally obtained. So long as the thickness of the leach-out layer before the removal is larger than 1 nm, the minimum necessary antiglare effect and even reflection properties can be obtained. Such leach-out layer thicknesses are hence preferred.
  • any of glasses having various compositions can be utilized.
  • composition of the glass in the present invention is not particularly limited, but examples thereof include the following glass compositions.
  • the thickness of the glass is not particularly limited. However, in the case of performing a chemical strengthening treatment, the thickness of the glass is usually preferably 5 mm or less, more preferably 3 mm or less, from the standpoint of effectively conducting the treatment.
  • sand blasting in which a crystalline silicon dioxide powder, silicon carbide powder, or the like is blown against the surface of the glass substrate by compressed air or grinding with a brush equipped with bristles which have a crystalline silicon dioxide powder, silicon carbide powder, or the like adhered thereto and which have been moistened with water.
  • Examples of preferred methods for the etching include a method of immersing the glass substrate, as an object to be treated, in a solution which includes hydrogen fluoride as a main component.
  • This solution may contain an acid such as hydrochloric acid, nitric acid, or citric acid as a component other than hydrogen fluoride. Due to the inclusion of the acid, cationic components contained in the glass can be inhibited from reacting with the hydrogen fluoride and thereby locally causing a precipitation reaction, and the etching can hence be allowed to proceed evenly throughout the surface.
  • the cover glass of the present invention has an antireflection film disposed on the antiglare-treated surface of the glass substrate by performing an antireflection film treatment (referred to also as “AR treatment”).
  • AR treatment an antireflection film treatment
  • the cover glass of the present invention should have a luminous reflectance of 2% or less. So long as the luminous reflectance thereof is within that range, reflection in the cover glass surface can be sufficiently prevented.
  • the luminous reflectance is provided for in JIS Z8701. As the illuminant, illuminant D65 was used.
  • the printing treatment should be conducted between the antiglare treatment as step 1 and the antireflection film formation as step 4 and after the leach-out layer removal as step 3, in order to prevent the printed portion from being affected by the etching or other treatment for the leach-out layer removal.
  • This treatment for removing the leach-out layer does not result in elimination of the irregularities formed by the antiglare treatment.
  • An antireflection film 20 is further formed on the glass main surface 10 a from which the leach-out layer has been removed ( FIG. 1D ).
  • the leach-out described above also occurs simultaneously.
  • a relationship with etching rate is hence important. Specifically, it is preferred to use concentration and temperature conditions under which the etching rate is at least 1.5 times the rate of leach-out layer formation.
  • the etching rate is more preferably at least 2 times, even more preferably at least 2.5 times, the rate of leach-out layer formation.
  • Examples of methods for grinding with an abrasive material include a method in which a grinding fluid containing an abrasive material selected from calcium carbonate, cerium oxide, colloidal silica, and the like is used to grind the surface of the glass substrate.
  • the kind of the inert gas in the chamber is not particularly limited, and any of various inert gases including argon and helium can be used.
  • fluorine-containing organosilicon compounds are stored in the form of a mixture with a solvent, such as a fluorochemical solvent, for the purpose of, for example, inhibiting the deterioration due to reaction with atmospheric moisture.
  • a solvent such as a fluorochemical solvent
  • this organosilicon compound may adversely affect the durability and other properties of the thin film obtained therefrom.
  • a fluorine-containing organosilicon compound which has undergone a solvent removal treatment before being heated in a heating vessel or a fluorine-containing organosilicon compound which has not been diluted with a solvent should be used in this embodiment.
  • a fluorine-containing organosilicon compound solution having a solvent concentration of preferably 1 mol % or less, more preferably 0.2 mol % or less. It is especially preferred to use a fluorine-containing organosilicon compound containing no solvent.
  • Examples of the solvents usable for storing the fluorine-containing organosilicon compound include perfluorohexane, m-xylene hexafluoride (C 6 H 4 (CF 3 ) 2 ), hydrofluoropolyethers, and HFE 7200/7100 (trade names; manufactured by Sumitomo 3M Ltd.; HFE 7200 is represented by C 4 F 9 C 2 H 5 and HFE 7100 is represented by C 4 F 9 OCH 3 ).
  • a treatment for removing the solvent from a solution of a fluorine-containing organosilicon compound in a fluorochemical solvent can be accomplished, for example, by evacuating a vessel which contains the solution of a fluorine-containing organosilicon compound.
  • a treatment for removing the solvent can also be conducted after the solution of a fluorine-containing organosilicon compound is introduced into the heating vessel of a deposition device for antifouling film deposition, by evacuating the heating vessel at room temperature before the heating vessel is heated. It is also possible to remove the solvent beforehand with an evaporator or the like before introduction into the heating vessel.
  • the fluorine-containing organosilicon compound should be immediately introduced into the heating vessel of the deposition device for antifouling film deposition. It is preferable that after the introduction, the inside of the heating vessel should be made vacuum or replaced with an inert gas, e.g., nitrogen or a rare gas, thereby removing the atmosphere (air) contained in the heating vessel. It is more preferable that the storage container and the heating vessel of the production device should have been connected to each other by a valved pipeline so that the compound can be introduced from the storage container into the heating vessel without coming into with the air.
  • an inert gas e.g., nitrogen or a rare gas
  • DRAGONTRAIL registered trademark
  • This substrate was subsequently immersed in an alkali solution (SUN WASH TL-75, manufactured by Lion Corp.) for 4 hours to remove a leach-out layer present in the surfaces.
  • the amount of the leach-out layer removed was calculated from the glass weights respectively measured before and after the treatment for leach-out layer removal and from the surface area and density of the glass.
  • an antireflection film was deposited on the surface which had undergone the antiglare treatment, in the following manner.
  • pulse sputtering was conducted using a niobium oxide target (trade name, NBO Target; manufactured by AGC Ceramics Co., Ltd.) under the conditions of a pressure of 0.3 Pa, frequency of 20 kHz, power density of 3.8 W/cm 2 , and inversion pulse width of 5 ⁇ sec, while introducing thereinto a mixed gas obtained by mixing argon gas with 10% by volume oxygen gas, thereby forming a high-refractive-index layer made of niobium oxide (niobia) and having a thickness of 13 nm on that surface of the glass substrate which had undergone the antiglare treatment.
  • a niobium oxide target trade name, NBO Target; manufactured by AGC Ceramics Co., Ltd.
  • pulse sputtering was conducted using a niobium oxide target (trade name, NBO Target; manufactured by AGC Ceramics Co., Ltd.) under the conditions of a pressure of 0.3 Pa, frequency of 20 kHz, power density of 3.8 W/cm 2 , and inversion pulse width of 5 ⁇ sec, while introducing a mixed gas obtained by mixing argon gas with 10% by volume oxygen gas, thereby forming a high-refractive-index layer made of niobium oxide (niobia) and having a thickness of 115 nm on the low-refractive-index layer.
  • a niobium oxide target trade name, NBO Target; manufactured by AGC Ceramics Co., Ltd.
  • any 10 cm 2 -square portion within the glass substrate was selected as a measuring range, and this measuring range was divided into 11 ⁇ 11 equal portions.
  • the 100 intersections in the resultant lattice pattern on the substrate were examined for color in the following manner.
  • the spectral reflectance of that surface of the substrate which was on the side where the antireflection treatment had been performed was measured with a spectrophotometric colorimeter (Type CM-2600d, manufactured by Konica Minolta) in the SCI mode, and a luminous reflectance (color indexes a* and b* as provided for in JIS Z8729) was determined form the value of spectral reflectance.
  • the back surface of the glass to be subjected to this measurement was painted in black in order to eliminate reflection from the back surface, which had undergone neither the antiglare treatment nor the antireflection treatment.
  • the heating vessel which contained the composition for forming fluorine-containing organosilicon compound film was heated to 270° C. After the temperature of the heating vessel had reached 270° C., the heated state was maintained for 10 minutes until the temperature became stable.
  • the feeding of the starting material through the nozzle was stopped. Thereafter, the optical part produced was taken out of the vacuum chamber.
  • a cover glass was produced in the same manner as in Example 1, except that the etching treatment period in the antiglare treatment step (1) in Example 1 was changed to 20 minutes to thereby regulate the haze to 4%, that the period of immersion in the alkali solution in the leach-out layer removal step (3) in Example 1 was changed to 8 hours, and that the antireflection film formation step (4) in Example 1 was conducted by the following method.
  • An antireflection film was deposited on the surface which had undergone the antiglare treatment, in the following manner.
  • pulse sputtering was conducted using a silicon target under the same conditions as in Example 1, thereby forming a low-refractive-index layer made of silicon oxide (silica) and having a thickness of 90 nm on the high-refractive-index layer.
  • a cover glass was produced in the same manner as in Example 1, except that the etching treatment period in the antiglare treatment step (1) in Example 1 was changed to 10 minutes to thereby regulate the haze to 10%, that the leach-out layer removal step (3) in Example 1 was conducted by calcium carbonate washing under the following conditions, and that the antireflection film formation step (4) in Example 1 was conducted by the method used in Example 3.
  • a calcium-carbonate abrasive material having an average particle diameter of 1.6 ⁇ m (particle size distribution, 0.1 ⁇ m to 50 ⁇ m) was used as an aqueous solution (slurry) having a concentration of 20% by weight to grind one surface of the substrate with a nylon brush at a grinding pressure of 30 to 50 kPa and a conveying speed of 55 mm/sec, in an amount of about 1 nm.
  • a cover glass was produced in the same manner as in Example 1, except that the leach-out layer removal step (3) in Example 1 was conducted by cerium oxide washing under the following conditions and that the antireflection film formation step (4) in Example 1 was conducted under the following conditions.
  • Cerium oxide washing A cerium-oxide abrasive material having an average particle diameter of 1.2-1.8 ⁇ m, an aqueous solution (slurry) having a concentration of 4 Be, and a suede pad were used to grind one surface of the substrate 20 times at a grinding pressure of 0.113 MPa and a conveying speed of 20 mm/sec, in an amount of about 1 ⁇ m.
  • niobium oxide targets (trade name, NBO Target; manufactured by AGC Ceramics Co., Ltd.) at a pressure of 0.3 Pa, frequency of 40 kHz, and power density of 3.8 W/cm 2 , while introducing thereinto a mixed gas obtained by mixing argon gas with 10% by volume oxygen gas.
  • a high-refractive-index layer made of niobium oxide (niobia) and having a thickness of 11 nm was formed on that surface of the glass substrate which had undergone the antiglare treatment.
  • niobium oxide targets (trade name, NBO Target; manufactured by AGC Ceramics Co., Ltd.) at a pressure of 0.3 Pa, frequency of 40 kHz, and power density of 3.8 W/cm 2 , while introducing a mixed gas obtained by mixing argon gas with 10% by volume oxygen gas, thereby forming a high-refractive-index layer made of niobium oxide (niobia) and having a thickness of 120 nm on the low-refractive-index layer.
  • NBO Target manufactured by AGC Ceramics Co., Ltd.
  • AC sputtering was conducted using two silicon targets at a pressure of 0.3 Pa, frequency of 20 kHz, and power density of 3.8 W/cm 2 , while introducing a mixed gas obtained by mixing argon gas with 40% by volume oxygen gas, thereby forming a low-refractive-index layer made of silicon oxide (silica) and having a thickness of 95 nm.
  • a cover glass was produced in the same manner as in Example 2, except that the leach-out layer removal in Example 2 was conducted by immersing the substrate in a 13.4% by weight solution of hydrochloric acid for 3 hours, rinsing this substrate with pure water, and subsequently immersing the substrate in 10% aqueous NaOH solution for 4 hours.
  • a cover glass was produced in the same manner as in Example 8, except that the chemical strengthening treatment in Example 8 was omitted.
  • a cover glass was produced in the same manner as in Example 1, except that the leach-out layer removal step (3) in Example 1 was replaced by pure-water cleaning conducted under the following conditions.
  • Pure-water cleaning Pure water was introduced into an immersion tank, and the substrate was immersed therein. An ultrasonic wave of 40 kHz was propagated thereto to clean the substrate for 10 minutes. Thereafter, the substrate was immersed in pure water heated at 60° C., and was then pulled out gradually and dried thereby.
  • a cover glass was produced in the same manner as in Example 3, except that the leach-out layer removal step (3) in Example 3 was replaced by plasma cleaning conducted under the following conditions.
  • a cover glass was produced in the same manner as in Comparative Example 1, except that the antiglare treatment (frosting treatment) in Example 1 was omitted.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 Example 6
  • Example 7 Glass DT DT DT DT DT DT DT DT DT DT DT DT DT (un- DT strengthened) Size (mm ⁇ mm) 150 ⁇ 250 150 ⁇ 250 400 ⁇ 600 150 ⁇ 250 150 ⁇ 250 150 ⁇ 250 150 ⁇ 250 150 ⁇ 250
  • Frosting treatment conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted conducted
  • Example 10 Example 11 Example 12
  • Example 1 Example 2
  • Example 2 Glass DT DT DT (un- DT DT DT strengthened) strengthened) Size (mm ⁇ mm) 150 ⁇ 250 150 ⁇ 250 150 ⁇ 250 150 ⁇ 250 400 ⁇ 600 150 ⁇ 250 150 ⁇ 250

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  • General Physics & Mathematics (AREA)
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US15/404,609 2014-07-16 2017-01-12 Cover glass Abandoned US20170129806A1 (en)

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CN115724592A (zh) * 2022-10-11 2023-03-03 广东山之风环保科技有限公司 一种家居触控面板玻璃ag效果蒙砂液及其制备方法
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JP7059512B2 (ja) * 2017-03-06 2022-04-26 Ａｇｃ株式会社 液晶表示装置
JP2018197183A (ja) * 2017-05-23 2018-12-13 Ａｇｃ株式会社 ガラス物品、および表示装置
KR101987834B1 (ko) * 2018-01-17 2019-06-12 주식회사 셀코스 컬러유리 및 그 제조방법
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DE112015003283B4 (de) 2018-05-03
DE112015003283T5 (de) 2017-04-06
US20210284571A1 (en) 2021-09-16
TWI615277B (zh) 2018-02-21
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KR101889667B1 (ko) 2018-08-17
CN106536440A (zh) 2017-03-22

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