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WO2013051620A1 - Procédé de fabrication d'un objet doté d'un film antireflet - Google Patents

Procédé de fabrication d'un objet doté d'un film antireflet Download PDF

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Publication number
WO2013051620A1
WO2013051620A1 PCT/JP2012/075680 JP2012075680W WO2013051620A1 WO 2013051620 A1 WO2013051620 A1 WO 2013051620A1 JP 2012075680 W JP2012075680 W JP 2012075680W WO 2013051620 A1 WO2013051620 A1 WO 2013051620A1
Authority
WO
WIPO (PCT)
Prior art keywords
reflection film
low reflection
coating
substrate
roll
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2012/075680
Other languages
English (en)
Japanese (ja)
Inventor
義美 大谷
敏 本谷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AGC Inc
Original Assignee
Asahi Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Priority to PH1/2014/500695A priority Critical patent/PH12014500695A1/en
Priority to CN201280048487.XA priority patent/CN103842098A/zh
Priority to KR1020147008766A priority patent/KR20140088862A/ko
Publication of WO2013051620A1 publication Critical patent/WO2013051620A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • G02B1/111—Anti-reflection coatings using layers comprising organic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/28—Processes for applying liquids or other fluent materials performed by transfer from the surfaces of elements carrying the liquid or other fluent material, e.g. brushes, pads, rollers
    • 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
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • 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
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/25—Oxides by deposition from the liquid phase
    • 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
    • C09D201/00—Coating compositions based on unspecified macromolecular compounds
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/42—Gloss-reducing agents
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/69—Particle size larger than 1000 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2252/00—Sheets
    • 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
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/42—Coatings comprising at least one inhomogeneous layer consisting of particles only
    • 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
    • C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer

Definitions

  • the present invention relates to a method of manufacturing an article having a low reflection film on a substrate.
  • Articles having an antireflection function for the purpose of reducing external light reflection and improving light transmittance have been put into practical use.
  • a method for imparting an antireflection function a method of forming a low reflection film on a substrate by a wet coating method (spin coating method, spray coating method, roll coating method, etc.) is known.
  • the spin coating method is a method of applying a coating composition for forming a low reflection film on a substrate by centrifugal force by dropping the coating composition for forming a low reflection film on the substrate and rotating the substrate.
  • the spray coating method is a method of applying a coating composition for forming a low reflection film on a substrate by spraying the coating composition for forming a low reflection film from a spray head onto the substrate conveyed in a predetermined direction.
  • a coating composition for forming a low reflection film is applied onto a substrate by transferring the coating composition for forming a low reflection film on the surface of the coating roll onto the substrate conveyed in a predetermined direction. Is the method.
  • the spin coating method has the following problems. -When a base material becomes large, it will become difficult to rotate a base material. -The low reflective film tends to be thick at the periphery of the substrate, and the film thickness uniformity of the low reflective film is inferior. -Since the excess coating composition for forming a low reflection film is blown off from the substrate by centrifugal force, the amount of the coating composition for forming a low reflection film required is increased.
  • the spray coating method has the following problems. -Since it is necessary to reciprocate the spray head in the width direction of the base material, in order to form a low reflection film uniformly on a wide base material, a large number of spray heads are arranged along the transport direction of the base material. Or, it is necessary to slow down the conveying speed of the substrate. -Since there are many coating compositions for forming a low reflection film that do not adhere to the substrate and scatter in the atmosphere, the amount of coating composition for forming a low reflection film that is required increases.
  • a roll coating method is an example of a wet coating method that can handle a wide range of substrates, can relatively fasten the conveyance speed of the substrate, and requires a relatively small amount of the coating composition for forming a low reflection film. .
  • the roll coating method has the following problems. ⁇ Adjustment of the gap between the substrate and the coating roll is difficult, and the film thickness uniformity of the low reflective film is poor. When the viscosity of the coating composition for forming a low reflection film is low, it is difficult to form a low reflection film having an arbitrary film thickness that can be optically designed. That is, the film thickness controllability is poor.
  • the following method has been proposed as a roll coating method capable of forming a metal oxide film having a uniform film thickness.
  • the concentration of the metal compound in the coating composition (as oxide) is 0.1 to 10% by mass
  • the viscosity of the coating composition is 0.1 to 100 mPa ⁇ s
  • the rotation speed of the coating roll is 2 to 55 m / min
  • the substrate transport speed is 1 to 30 m / min
  • the rotation speed of the coating roll is higher than the substrate transport speed (see Patent Document 1).
  • the present invention can deal with a wide range of substrates, can relatively fast the conveyance speed of the substrate, requires a relatively small amount of coating composition, relatively short drying or baking time and application time, A method for producing an article with a low-reflection film that can form a low-reflection film having a uniform film thickness and is easy to form a low-reflection film having an arbitrary film thickness that can be optically designed (that is, excellent in film thickness controllability) provide.
  • the method for producing an article with a low reflection film of the present invention is a method for producing an article having a low reflection film on a substrate, and the method comprises a reverse roll coater on the substrate conveyed in a predetermined direction.
  • the coating composition is applied by a coating roll to form the low reflection film, and the dispersion medium (a) and fine particles (b) dispersed in the dispersion medium (a) are formed as the coating composition.
  • the rotational speed of the coating roll when applying the composition that is, the peripheral speed.
  • “rotational speed” means the peripheral speed) is made slower than the transport speed of the substrate.
  • the coating composition preferably further contains a terpene derivative (d) dissolved or dispersed in the dispersion medium (a).
  • the amount of the terpene derivative (d) is preferably 0.01 to 2 parts by mass with respect to 1 part by mass of the solid content of the coating composition.
  • the solid content concentration of the coating composition is preferably 1 to 9% by mass.
  • the mass ratio of the fine particles (b) to the binder (c) is preferably 10/90 to 95/5.
  • the conveying speed of the substrate is preferably 3 to 20 m / min.
  • the rotation speed of the coating roll is preferably 0.28 times or more and 0.98 times or less the conveyance speed of the base material.
  • the surface hardness (JIS-A standard) of the coating roll is preferably 10 to 70. It is preferable that the base material is a template glass having a satin pattern on at least one surface.
  • the substrate conveyance speed can be relatively fast, the amount of the coating composition required is relatively small, and drying Or, the baking time and the coating time are relatively short, a low reflection film having a uniform film thickness can be formed, and it is easy to form a low reflection film having an arbitrary film thickness that can be optically designed, that is, excellent in film thickness controllability. .
  • FIG. 1 is a cross-sectional view showing an example of an article with a low reflection film obtained by the production method of the present invention.
  • the article 1 with a low reflection film has a base material 2 and a low reflection film 3 formed on the surface of the base material 2.
  • Examples of the material for the substrate 2 include glass, metal, resin, silicon, wood, paper, and the like.
  • Examples of the glass include soda lime glass, borosilicate glass, aluminosilicate glass, alkali-free glass, and mixed alkali glass.
  • Examples of the resin include polyethylene terephthalate, polycarbonate, triacetyl cellulose, polymethyl methacrylate, and the like.
  • a satin-patterned template glass having an uneven surface is preferable.
  • the soda lime glass ie, high transparency
  • blue plate glass used for ordinary window glass or the like
  • Transmission glass commonly called white plate glass
  • the white plate glass is expressed in terms of mass percentage based on oxide, SiO 2 : 65 to 75%, Al 2 O 3 : 0 to 10%, CaO: 5 to 15%, MgO: 0 to 15%, Na 2 O: 10 ⁇ 20%, K 2 O: 0 to 3%, Li 2 O: 0 to 5%, Fe 2 O 3 : 0 to 3%, TiO 2 : 0 to 5%, CeO 2 : 0 to 3%, BaO: 0 to 5%, SrO: 0 to 5%, B 2 O 3 : 0 to 15%, ZnO: 0 to 5%, ZrO 2 : 0 to 5%, SnO 2 : 0 to 3%, SO 3 : 0 to It is preferable to have a composition of 0.5%.
  • the base material 2 is non-alkali glass, it is expressed in terms of mass percentage on the basis of oxide, SiO 2 : 39 to 70%, Al 2 O 3 : 3 to 25%, B 2 O 3 : 1 to 30% MgO: 0 to 10%, CaO: 0 to 17%, SrO: 0 to 20%, BaO: 0 to 30%.
  • the base material 2 is a mixed alkali glass, it is expressed in terms of mass percentage on the basis of oxide, SiO 2 : 50 to 75%, Al 2 O 3 : 0 to 15%, MgO + CaO + SrO + BaO + ZnO: 6 to 24%, Na It is preferable to have a composition of 2 O + K 2 O: 6 to 24%.
  • the substrate 2 may have a functional layer 5 on the surface of the substrate body 4.
  • the functional layer 5 include an undercoat layer, an adhesion improving layer, and a protective layer.
  • the undercoat layer functions as an alkali barrier layer or a wide band low refractive index layer.
  • the undercoat layer is preferably a layer formed by applying an undercoat coating composition containing a hydrolyzate of alkoxysilane (sol-gel silica, that is, a silica precursor by a sol-gel method) on a substrate.
  • sol-gel silica that is, a silica precursor by a sol-gel method
  • the undercoat layer may be baked in advance or may remain wet.
  • the application temperature (that is, the substrate temperature during application) is preferably room temperature to 80 ° C., and the firing temperature of the applied coating film is 30 to 700 ° C. is preferable.
  • the thickness of the undercoat layer is preferably 10 to 500 nm.
  • the low-reflection film 3 is a single-layer film containing a binder (c) or a fired product thereof and fine particles (b), which is formed by applying a coating composition coating solution described later once. preferable.
  • the binder is a hydrolyzate of alkoxysilane
  • the low reflection film 3 is a film in which the fine particles (b) are dispersed in a matrix made of a calcined product of the alkoxysilane hydrolyzate (SiO 2 ).
  • the binder is resin
  • the low reflection film 3 is a film in which fine particles (b) are dispersed in a matrix made of resin.
  • the film thickness of the low reflection film 3 is preferably 50 to 300 nm, more preferably 80 to 200 nm. If the film thickness of the low reflection film 3 is 50 nm or more, light interference occurs and antireflection performance is exhibited. If the film thickness of the low reflective film 3 is 300 nm or less, the film can be formed without generating cracks.
  • the film thickness of the low reflection film 3 is measured by a reflection spectral film thickness meter.
  • the reflectance of the low reflective film 3 is the lowest value (so-called bottom reflectance) in the wavelength range of 300 to 1200 nm, preferably 2.6% or less, and more preferably 1.0%.
  • a coating liquid of a coating composition which will be described later, is applied onto a substrate 2 conveyed in a predetermined direction by a coating roll of a reverse roll coater,
  • the low reflection film 3 is formed by baking or drying and curing as necessary.
  • FIG. 3 is a schematic diagram illustrating an example of a reverse roll coater.
  • the reverse roll coater 10 is disposed with a predetermined gap above the conveyor belt 12 such that the rotation axis direction is orthogonal to the traveling direction of the conveyor belt 12 and a conveyor belt 12 that conveys the substrate 2 in a predetermined direction.
  • a coating roll 14 that rotates in a direction opposite to the direction of travel of the conveyor belt 12; and is disposed downstream of the coating roll 14 in the direction of travel of the transport belt 12, and with a predetermined indentation thickness with respect to the coating roll 14
  • a doctor roll 16 also referred to as a metalling roll
  • a backup roll that is disposed below the coating roll 14 via the conveyor belt 12 so as to be in contact with the conveyor belt 12 and rotates in the same direction as the traveling direction of the conveyor belt 12
  • a first doctor blade 22 arranged to contact the surface of the upper half of the doctor roll 16 so as to be formed between the first roll 16 and the surface of the coating roll 14 not transferred to the substrate 2.
  • a second doctor blade 24 disposed so as to contact the surface of the coating roll 14 is provided.
  • a plurality of conveyance rolls may be arranged in the conveyance direction of the base material 2 so that the rotation axis direction is orthogonal to the traveling direction of the conveyance belt 12.
  • the coating composition 20 is applied on the surface of the substrate 2 as described below, and a coating film is formed.
  • the coating composition 20 is supplied to the surface of the doctor roll 16 from above the doctor roll 16.
  • a predetermined amount of the coating composition 20 adheres to the surface of the doctor roll 16 and moves between the doctor roll 16 and the first doctor blade 22 toward the coating roll 14 as the doctor roll 16 rotates.
  • the coating composition 20 that could not pass between the doctor roll 16 and the first doctor blade 22 is separated from the doctor roll 16. It collects between the first doctor blade 22 and a liquid reservoir is formed.
  • the coating composition 20 adhered to the surface of the doctor roll 16 and moved to the coating roll 14 side moves to the surface of the coating roll 14 while maintaining a predetermined amount between the coating roll 14 and the doctor roll 16. To do. At this time, since the transfer of the coating composition 20 is regulated by the doctor roll 16, the coating composition 20 that could not pass between the coating roll 14 and the doctor roll 16 is between the coating roll 14 and the doctor roll 16. And a liquid reservoir is formed. The coating composition 20 transferred to the surface of the coating roll 14 moves to the side of the conveyor belt 12 as the coating roll 14 rotates.
  • the coating composition 20 adhered to the surface of the coating roll 14 and moved toward the conveying belt 12 has a predetermined amount based on the gap between the conveying belt 12 and the coating roll 14 and the thickness of the substrate 2. It moves to the surface of the material 2 and a coating film is formed. At this time, the coating composition 20 that has not moved to the surface of the base material 2 moves to the second doctor blade 24 side with the rotation of the coating roll 14 while adhering to the surface of the coating roll 14. The second doctor blade 24 scrapes the surface of the coating roll 14.
  • the doctor roll 16 Since the first doctor blade 22 and the second doctor blade 24 are provided in each of the doctor roll 16 and the coating roll 14, the doctor roll 16 does not move from the surface of the doctor roll 16 to the surface of the coating roll 14.
  • the coating roll 14 As the coating roll 14, a rubber lining roll lined with rubber is usually used.
  • the surface hardness (JIS-A standard) of the coating roll 14 is preferably 10 to 70, more preferably 20 to 50. If the hardness is 10 or more, it is easy to control the film thickness of the coating film of the coating composition 20 applied on the substrate 2. If the hardness is 70 or less, even if a template glass is used as the substrate 2, the surface of the coating roll 14 can follow the irregularities on the surface of the template glass, and the coating film thickness of the coating composition 20 can be reduced. Easy to make uniform.
  • the rotational speed (that is, the peripheral speed) of the coating roll 14 is made slower than the conveying speed of the substrate 2.
  • the rotation speed of the coating roll 14 is preferably 0.28 times or more of the transport speed of the base material 2 and 0.98 times or less of the transport speed of the base material 2 from the viewpoint of further excellent film thickness controllability. More preferably, it is 0.35 times or more of the transport speed of the base material 2 and 0.90 times or less of the transport speed of the base material 2.
  • the rotation speed of the coating roll 14 is made faster than the conveyance speed of the base material 2, but in the present invention, a specific coating composition described later is used.
  • a specific coating composition described later is used.
  • doctor roll As the doctor roll 16, a metal roll whose surface is made of metal or a rubber lining roll lined with rubber is usually used.
  • the doctor roll 16 preferably has a plurality of grooves formed on the surface from the viewpoint of easily holding the coating composition 20 on the surface of the doctor roll 16. From the viewpoint of making the film thickness uniform, it is more preferable that a lattice-like groove is formed on the surface.
  • the indentation thickness of the doctor roll 16 with respect to the coating roll 14 (this indentation thickness is the coating roll with respect to the tangent in the state where the coating roll 14 and the doctor roll 16 are not pushed by the doctor roll 16 when the coating roll 14 and the doctor roll 16 are disposed.
  • the doctor roll is pushed in by a rubber lining on the surface of the roller), and is preferably 0.1 to 1.0 mm, more preferably 0.3 to 0.9 mm. If the indentation thickness is within this range, it is easy to make the film thickness of the coating composition 20 applied onto the substrate 2 uniform, and the coating film of the coating composition 20 applied onto the substrate 2. Easy to control the film thickness.
  • the gap between the conveyor belt 12 and the coating roll 14 is appropriately adjusted according to the thickness of the base material 2, the film thickness of the coating composition 20 applied on the base material 2, and the like.
  • the conveying speed of the substrate 2 is preferably 3 to 20 m / min, and more preferably 5 to 15 m / min. If the conveyance speed of the base material 2 is 3 m / min or more, the productivity is improved. If the conveyance speed of the base material 2 is 20 m / min or less, it is easy to control the film thickness of the coating film of the coating composition 20 applied on the base material 2.
  • the coating temperature (this coating temperature refers to the temperature of the substrate when applied to the substrate surface) is preferably room temperature to 80 ° C., more preferably room temperature to 60 ° C.
  • the drying or baking temperature of the coating film of the coating composition is preferably 30 ° C. or higher, and may be appropriately determined according to the material of the substrate 2, the fine particles (b) or the binder (c).
  • the drying or firing temperature is 30 ° C. or higher and the heat resistant temperature of the resin or lower, but this temperature is sufficient. An antireflection effect is obtained.
  • the firing temperature is preferably 30 ° C.
  • the baking process of the low reflective film 3 and the physical strengthening process of glass can be combined.
  • the glass is heated to near the softening temperature.
  • the firing temperature is set in the range of about 600 ° C. to about 700 ° C.
  • the firing temperature is usually preferably equal to or lower than the heat distortion temperature of the substrate 2.
  • the lower limit of the firing temperature is determined according to the formulation of the coating composition 20. Since the polymerization proceeds to some extent even in natural drying, it is theoretically possible to set the drying or calcination temperature to a temperature setting near room temperature if there is no restriction on time.
  • the coating composition 20 includes a dispersion medium (a), fine particles (b) dispersed in the dispersion medium (a), and a binder (c) dissolved or dispersed in the dispersion medium (a).
  • the terpene derivative (d) dissolved or dispersed in the dispersion medium (a) may be contained, and other additives may be further contained as necessary.
  • the coating composition 20 includes, for example, mixing a fine particle (b) dispersion, a binder (c) solution, and an additional dispersion medium (a), a terpene derivative (d), and other additives as necessary. It is prepared by.
  • the viscosity of the coating composition 20 as the coating solution is 1.0 to 10.0 mPa ⁇ s, and preferably 2.0 to 5.0 mPa ⁇ s. If the viscosity of the coating composition 20 is 1.0 mPa ⁇ s or more, it is easy to control the film thickness of the coating film of the coating composition 20 applied on the substrate 2. If the viscosity of the coating composition 20 is 10.0 mPa ⁇ s or less, the drying or baking time and the coating time are shortened. The viscosity of the coating composition 20 is measured with a B-type viscometer.
  • the solid content concentration of the coating composition 20 is preferably 1 to 9% by mass, and more preferably 2 to 6% by mass. If the solid content concentration is 1% by mass or more, the film thickness of the coating film of the coating composition 20 can be reduced, and the film thickness of the finally obtained low reflection film 3 can be made uniform. If solid content concentration is 9 mass% or less, it will be easy to make uniform the film thickness of the coating film of the coating composition 20 apply
  • the solid content of the coating composition 20 means the sum of the fine particles (b) and the binder (c) (however, in the case where the binder (c) is a hydrolyzate of alkoxysilane, the SiO 2 equivalent solid content concentration).
  • the amount of the terpene derivative (d) is preferably 0.01 to 2 parts by mass, more preferably 0.03 to 1 part by mass with respect to 1 part by mass of the solid content of the coating composition 20.
  • the amount of the terpene derivative (d) is 0.01 parts by mass or more, the antireflection effect is sufficiently higher than that when the terpene derivative (d) is not added.
  • the terpene derivative (d) is 2 parts by mass or less, the strength of the low reflection film 3 is good.
  • the mass ratio of the fine particles (b) to the binder (c) is preferably 10/90 to 95/5, more preferably 70/30 to 90/10.
  • fine particles (b) / binder (c) is 95/5 or less, the adhesion between the low reflective film 3 and the substrate 2 is sufficiently high.
  • the fine particle (b) / binder (c) is 10/90 or more, the antireflection effect is sufficiently high.
  • Dispersion medium (a) examples include water, alcohols (methanol, ethanol, isopropanol, butanol, diacetone alcohol, etc.), ketones (acetone, methyl ethyl ketone, methyl isobutyl).
  • Ketones ethers (tetrahydrofuran, 1,4-dioxane, etc.), cellosolves (methyl cellosolve, ethyl cellosolve, etc.), esters (methyl acetate, ethyl acetate, etc.), glycol ethers (ethylene glycol monoalkyl ether, etc.) And nitrogen-containing compounds (N, N-dimethylacetamide, N, N-dimethylformamide, N-methylpyrrolidone and the like), sulfur-containing compounds (dimethylsulfoxide and the like) and the like.
  • the dispersion medium (a) is preferably selected as appropriate according to the substrate 2 or the binder (c).
  • an alcohol-based dispersion medium containing a solvent for example, a nitrogen-containing compound capable of dissolving the polycarbonate is preferable.
  • an alcohol-based dispersion medium containing a solvent capable of dissolving polyethylene terephthalate such as dichloromethane
  • the binder (c) is polyester, acrylic resin, silicone resin or the like is used as the binder (c), and as the dispersion medium (a) when the binder (c) is polyester, ethyl acetate or the like is used. Is preferred.
  • Fine particles (b) examples include at least one selected from the group consisting of metal oxide fine particles, metal fine particles, pigment-based fine particles, and resin fine particles.
  • the material of the metal oxide fine particles Al 2 O 3 , SiO 2 , SnO 2 , TiO 2 , ZrO 2 , ZnO, CeO 2 , Sb-containing SnO X (ATO), Sn-containing In 2 O 3 (ITO), and Suitable materials include at least one selected from the group consisting of RuO 2 .
  • SiO 2 is suitable as a material for the low reflection film 3 because it has a low refractive index, and is particularly preferable.
  • the metal fine particle material include metals such as Ag and Ru, alloys such as AgPd and RuAu, and the like.
  • the pigment-based fine particles include inorganic pigments such as titanium black and carbon black, and organic pigments.
  • the resin fine particle material include polystyrene and melanin resin.
  • Examples of the shape of the fine particles (b) include a spherical shape, an elliptical shape, a needle shape, a plate shape, a rod shape, a conical shape, a cylindrical shape, a cubic shape, a rectangular shape, a diamond shape, a star shape, and an indefinite shape.
  • the fine particles (b) may be hollow, perforated, or communicating holes.
  • the fine particles (b) may be present in a state where each fine particle is independent, each fine particle may be linked in a chain shape, or each fine particle may be aggregated.
  • the fine particles (b) those having the above-mentioned shapes may be mixed.
  • the fine particles (b) may be used alone or in combination of two or more.
  • the average aggregate particle diameter of the fine particles (b) is preferably 1 to 1000 nm, more preferably 3 to 500 nm, and even more preferably 5 to 300 nm. When the average aggregate particle diameter of the fine particles (b) is 1 nm or more, the antireflection effect is sufficiently high. If the average aggregate particle diameter of the fine particles (b) is 1000 nm or less, the haze of the low reflective film 3 can be kept low.
  • the average aggregate particle diameter of the fine particles (b) is an average aggregate particle diameter of the fine particles (b) in the dispersion medium (a), and is measured by a dynamic light scattering method. In the case of monodispersed fine particles (b) in which no aggregation is observed, the average aggregate particle size is equal to the average primary particle size.
  • the low reflection film 3 in the present invention exhibits an antireflection effect by the voids selectively formed around the fine particles (b), and therefore the material of the fine particles (b) is not necessarily of a low refractive index (for example, SiO 2 2 ) need not be used. Therefore, it is possible to form the low reflection film 3 having both the various characteristics of the fine particles (b) and the antireflection effect. For example, when the material of the fine particles (b) is SiO 2 , the refractive index of the low reflective film 3 can be further lowered, so that the low reflective film 3 having a sufficiently low reflectance can be formed.
  • the low reflection film 3 having both conductivity and / or infrared shielding property and antireflection effect can be formed.
  • the material of the fine particles (b) is CeO 2 or ZnO
  • the low reflection film 3 having both the ultraviolet absorption and the antireflection effect can be formed.
  • the material of the fine particles (b) is TiO 2 having a high refractive index
  • the low reflection film 3 can be formed with a single layer coating which has not been considered in the past. Therefore, the hydrophilic and antibacterial properties of TiO 2
  • the low reflection film 3 having both properties and an antireflection effect can be formed.
  • the material of the fine particles (b) is an organic pigment or an inorganic pigment
  • a colored low reflection film 3 can be formed, and a colored filter having an antireflection function can be manufactured.
  • binder (c) examples include a hydrolyzate of alkoxysilane (sol-gel silica, that is, a silica precursor by a sol-gel method), a resin (for example, a thermoplastic resin, a thermosetting resin, or an ultraviolet curable resin). .
  • the binder (c) is preferably selected as appropriate according to the substrate 2. As the binder (c) when the substrate 2 is glass, a hydrolyzate of alkoxysilane is preferable.
  • alkoxysilane examples include tetraalkoxysilane (tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetrabutoxysilane, etc.), alkoxysilane having a perfluoropolyether group (perfluoropolyether triethoxysilane, etc.), perfluoroalkyl.
  • Group-containing alkoxysilane perfluoroethyltriethoxysilane, etc.
  • vinyl group-containing alkoxysilane vinyltrimethoxysilane, vinyltriethoxysilane, etc.
  • epoxy group-containing alkoxysilane (2- (3,4-epoxycyclohexyl), etc.
  • hydrolysis of the alkoxysilane is performed using water or an acid or alkali as a catalyst at least 4 times mol of alkoxysilane.
  • the acid include inorganic acids (HNO 3 , H 2 SO 4 , HCl, etc.) and organic acids (formic acid, oxalic acid, monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, etc.).
  • the alkali include ammonia, sodium hydroxide, potassium hydroxide and the like.
  • the catalyst is preferably an acid from the viewpoint of long-term storage, and the catalyst is preferably one that does not hinder the dispersion of the fine particles (b).
  • the terpene means a hydrocarbon having a composition of (C 5 H 8 ) n (where n is an integer of 1 or more) having isoprene (C 5 H 8 ) as a structural unit.
  • the terpene derivative means terpenes having a functional group derived from terpene.
  • the terpene derivative (d) includes those having different degrees of unsaturation.
  • the terpene derivative (d) is preferably a terpene derivative having a hydroxyl group and / or a carbonyl group in the molecule from the viewpoint of the antireflection effect of the low reflective film 3, and the hydroxyl group, aldehyde group (—CHO), keto group in the molecule.
  • a terpene derivative having at least one functional group selected from the group consisting of (—C ( ⁇ O) —), an ester bond (—C ( ⁇ O) O—), and a carboxy group (—COOH) is more preferable. More preferred are terpene derivatives having in the molecule at least one functional group selected from the group consisting of a hydroxyl group, an aldehyde group and a keto group.
  • terpene derivative (d) examples include terpene alcohols (for example, ⁇ -terpineol, terpinene 4-ol, L-menthol, ( ⁇ ) citronellol, myrtenol, nerol, borneol, farnesol, phytol, etc.), terpene aldehyde (for example, citral) , ⁇ -cyclocitral, perilaldehyde, etc.), terpene ketone (eg, ( ⁇ ) camphor, ⁇ -ionone, etc.), terpene carboxylic acid (eg, citronellic acid, abietic acid, etc.), terpene ester (eg, terpinyl acetate) , Menthyl acetate, etc.).
  • terpene alcohol is preferable.
  • a terpene derivative (d) may be used individually by 1 type, and may use 2 or more types together.
  • additives examples include surfactants for improving leveling properties, and metal compounds for improving durability of the low reflective film 3.
  • surfactant include silicone oil and acrylic.
  • a zirconium chelate compound, a titanium chelate compound, an aluminum chelate compound and the like are preferable.
  • the zirconium chelate compound include zirconium tetraacetylacetonate and zirconium tributoxy systemate.
  • the viscosity of the coating composition is 10 mPa ⁇ s or less, which is a relatively low viscosity, so the drying or baking time and coating time are compared. Short.
  • the rotation speed of the coating roll of the reverse roll coater is made slower than the conveyance speed of the substrate. Therefore, even if the viscosity of the coating composition is relatively low, it is possible to form a low reflection film having a uniform film thickness, and it is easy to form a low reflection film having an arbitrary film thickness that can be optically designed. . That is, the film thickness controllability is excellent.
  • the coating composition described above includes the dispersion medium (a), the fine particles (b), and the binder (c) as described above, a low reflection having an antireflection effect by the reverse roll coater method.
  • Films can be formed at low cost and at relatively low temperatures. That is, when the low reflection film is formed by the reverse roll coating method unique to the present invention using the coating composition described above, voids are selectively formed around the fine particles (b) in the low reflection film. Improves the antireflection effect. For example, when the film thickness is thick and non-uniform, the terpene is not volatilized uniformly during firing, and voids are not formed as intended.
  • the terpene volatilizes efficiently and smoothly during firing, the portion where the terpene was present remains as a void, and the volume of the void increases, so the antireflection effect is increased.
  • the article with a low reflection film described above has a high antireflection effect because it has a high antireflection effect, can be produced at low cost, and has a coating film that can be formed even at a relatively low temperature.
  • the base material that can be used when manufacturing the article is not so limited, and can be manufactured at a relatively low cost.
  • Examples 1 to 4 are examples, and examples 5 and 6 are comparative examples.
  • the average primary particle diameter of the fine particles was calculated by converting from the specific surface area measured by the BET method and the volume of the spherical particles assuming that the spherical particles were uniformly dispersed in the carrier.
  • the average aggregate particle size of the fine particles was measured using a dynamic light scattering particle size analyzer (manufactured by Nikkiso Co., Ltd., Microtrac UPA).
  • viscosity The viscosity of the coating composition was measured using a B-type viscometer (manufactured by Toki Sangyo Co., Ltd., MODEL BL) after adjusting the liquid temperature to 25 ° C. in a thermostatic bath.
  • the film thickness of the low-reflection film is measured with a spectral reflectance film thickness meter (manufactured by Otsuka Electronics Co., Ltd., FE3000), and measured with a curve obtained from the dispersion formula of nk Couchy by the least square method. It was measured by fitting the reflected curve. Moreover, the film thickness of the low reflection film was measured at four locations, and the average value and the difference (variation) between the maximum value and the minimum value were determined.
  • the reflectance is the bottom reflectance in the wavelength range of 300 to 1200 nm (that is, the lowest value in the wavelength range of 300 to 1200 nm).
  • a spectrophotometer manufactured by JASCO Corporation, V670
  • a spectrophotometer Otsuka Electronics Co., Ltd., instantaneous multi-photometry system MCPD-3000
  • Linear SiO 2 fine particle dispersion (b-1)) Product name: “Snowtex OUP” manufactured by Nissan Chemical Industries, Ltd., solid content concentration in terms of SiO 2 : 15.5% by mass, average primary particle size: 10 to 20 nm, average aggregated particle size: 40 to 100 nm.
  • Coating compositions (B) and (C) were prepared in the same manner as the coating composition (A) except that the formulation shown in Table 1 was changed. The composition and viscosity are shown in Table 1.
  • Template glass made by Asahi Glass Co., Ltd., trade name: “Solite” (template glass with a low iron content and high permeability soda lime glass (white plate glass), with a satin pattern on the surface), size : 100 mm x 100 mm, thickness: 3.2 mm), polishing and washing the textured surface of the template glass with an aqueous cerium oxide dispersion, rinsing the cerium oxide with water, rinsing with ion-exchanged water, and drying I let you.
  • Solite template glass with a low iron content and high permeability soda lime glass (white plate glass), with a satin pattern on the surface), size : 100 mm x 100 mm, thickness: 3.2 mm
  • polishing and washing the textured surface of the template glass with an aqueous cerium oxide dispersion, rinsing the cerium oxide with water, rinsing with ion-exchanged water, and drying I let you.
  • the above template glass is preheated in a preheating furnace (VTR-115, manufactured by ISUZU), and the reverse roll coater is applied to the satin pattern surface on the template glass in a state where the glass surface temperature of the template glass is kept at 30 ° C.
  • the coating composition (A) was applied with a coating roll (manufactured by Sanwa Seiki Co., Ltd.). The application conditions were as follows. Substrate transport speed: 13.8 m / min, Rotating speed of coating roll: 9.0 m / min Doctor roll rotation speed: 9.0 m / min, Gap between coating roll and conveyor belt: 2.9 mm, Indentation thickness between coating roll and doctor roll: 0.6 mm.
  • the coating roll a rubber lining roll lined with a rubber (ethylene propylene diene rubber) having a surface hardness (JIS-A standard) of 30 was used.
  • a metal roll having lattice-like grooves formed on the surface thereof was used. Thereafter, it was baked in the atmosphere at 500 ° C. for 30 minutes to obtain an article on which a low reflective film was formed. The article was evaluated. The results are shown in Table 2.
  • Example 2 An article on which a low reflection film was formed was obtained in the same manner as in Example 1 except that the coating composition and application conditions were changed to the coating composition and application conditions shown in Table 2. The article was evaluated. The results are shown in Table 2.
  • Example 6 A template glass kept at 30 ° C. by a preheating furnace is set on a stand in a booth where a spray coating robot (manufactured by Kawasaki Robotics Co., Ltd., JE005F) is installed, and a paint composition ( X) was applied. Thereafter, it was baked in the atmosphere at 500 ° C. for 30 minutes to obtain an article on which a low reflective film was formed. The article was evaluated. The results are shown in Table 2.
  • a spray coating robot manufactured by Kawasaki Robotics Co., Ltd., JE005F
  • Example 1 it can be seen that the low reflection film having the target film thickness is formed, the film thickness variation of the low reflection film is small, and the uniformity is good. Moreover, although the conveyance speed was changed in Example 2 and Example 3 and the rotation speed was also changed, a uniform film was obtained in the same manner. Also, a uniform film was obtained in the same manner as in Example 4 in which the ratio of the fine particles to the binder was changed. In Example 5, since the rotation speed of the coating roll was made faster than the conveying speed of the substrate, a low reflection film having a target film thickness could not be obtained. In Example 6, since the low reflection film was formed by the spray coating method, the variation in the film thickness of the low reflection film became large.
  • An article with a low reflection film obtained by the production method of the present invention is an article having an antireflection function for the purpose of reducing external light reflection or improving light transmittance, for example, a cover glass of a solar cell, a display (LCD, PDP, organic EL, CRT, SED, etc.), their front plates, vehicle (car, train, aircraft, etc.) window glass, residential window glass, touch panel cover glass, etc.
  • a cover glass of a solar cell for example, a cover glass of a solar cell, a display (LCD, PDP, organic EL, CRT, SED, etc.), their front plates, vehicle (car, train, aircraft, etc.) window glass, residential window glass, touch panel cover glass, etc.

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Abstract

La présente invention concerne un procédé de fabrication d'un objet doté d'un film antireflet, grâce auquel on forme un film antireflet qui va permettre de manipuler un substrat de grande largeur, d'avoir une vitesse d'acheminement relativement rapide du substrat, un volume relativement faible du composé d'enduction nécessaire, un temps de séchage, de cuisson et/ou d'application relativement court et une épaisseur uniforme, et d'avoir en outre une très grande facilité de contrôle de l'épaisseur. On forme ainsi, très facilement, un film antireflet dont l'épaisseur peut être conçue de façon arbitraire par voie optique. Pour former, sur un substrat (2) qui est acheminé dans un sens indiqué, un film antireflet par application d'un composé d'enduction (20) au moyen d'un rouleau d'enduction (14) d'un dispositif de rouleau d'induction inverse (10), on rend la vitesse de rotation du rouleau d'enduction (14) inférieure à la vitesse d'acheminement du substrat (2), le composé d'enduction (20) comprenant un milieu de dispersion (a), de fines particules (b) dispersées dans le milieu de dispersion (a), et un liant (c) dissout ou dispersé dans le milieu de dispersion (a), avec une viscosité de 1 à 10 mPa•s.
PCT/JP2012/075680 2011-10-03 2012-10-03 Procédé de fabrication d'un objet doté d'un film antireflet Ceased WO2013051620A1 (fr)

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PH1/2014/500695A PH12014500695A1 (en) 2011-10-03 2012-10-03 Method of manufacturing object with low reflection film
CN201280048487.XA CN103842098A (zh) 2011-10-03 2012-10-03 带低反射膜的物品的制造方法
KR1020147008766A KR20140088862A (ko) 2011-10-03 2012-10-03 저반사막구비 물품의 제조 방법

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WO2015046260A1 (fr) * 2013-09-30 2015-04-02 旭硝子株式会社 Procédé de fabrication d'un substrat sur lequel est fixé un film poreux
JP2016109333A (ja) * 2014-12-04 2016-06-20 日本電気硝子株式会社 調理器用トッププレート及びその製造方法
WO2017150132A1 (fr) * 2016-02-29 2017-09-08 富士フイルム株式会社 Procédé de fabrication de stratifié, verre pourvu d'un film antireflet et module pour cellule solaire
KR20190076596A (ko) * 2017-12-22 2019-07-02 주식회사 엘지화학 저굴절 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
KR20190076599A (ko) * 2017-12-22 2019-07-02 주식회사 엘지화학 저반사 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
KR20190076598A (ko) * 2017-12-22 2019-07-02 주식회사 엘지화학 메조포러스 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
CN110280439A (zh) * 2019-07-29 2019-09-27 广东省新材料研究所 涂布辊、其应用及制备方法
CN114744068A (zh) * 2022-03-30 2022-07-12 天津南玻节能玻璃有限公司 一种光伏建筑一体化组件及其制备方法

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CN107265877A (zh) * 2017-08-03 2017-10-20 李郑松 一种抗酸碱玻璃涂层的制备方法
KR101890902B1 (ko) * 2017-08-24 2018-08-22 (주)경진테크 적외선 차단 강화유리 제조방법
GB2567238B (en) * 2017-10-09 2020-01-08 Surrey Nanosystems Ltd Paint with low light reflectivity

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WO2015046260A1 (fr) * 2013-09-30 2015-04-02 旭硝子株式会社 Procédé de fabrication d'un substrat sur lequel est fixé un film poreux
JP2016109333A (ja) * 2014-12-04 2016-06-20 日本電気硝子株式会社 調理器用トッププレート及びその製造方法
WO2017150132A1 (fr) * 2016-02-29 2017-09-08 富士フイルム株式会社 Procédé de fabrication de stratifié, verre pourvu d'un film antireflet et module pour cellule solaire
JPWO2017150132A1 (ja) * 2016-02-29 2018-09-13 富士フイルム株式会社 積層体の製造方法、反射防止膜付ガラス及び太陽電池モジュール
KR20190076598A (ko) * 2017-12-22 2019-07-02 주식회사 엘지화학 메조포러스 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
KR20190076599A (ko) * 2017-12-22 2019-07-02 주식회사 엘지화학 저반사 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
KR20190076596A (ko) * 2017-12-22 2019-07-02 주식회사 엘지화학 저굴절 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
KR102267504B1 (ko) 2017-12-22 2021-06-21 주식회사 엘지화학 메조포러스 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
KR102267506B1 (ko) 2017-12-22 2021-06-21 주식회사 엘지화학 저굴절 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
KR102267503B1 (ko) 2017-12-22 2021-06-21 주식회사 엘지화학 저반사 실리카 코팅층을 포함하는 광학 부재의 제조방법 및 이를 이용하여 제조된 광학 부재
CN110280439A (zh) * 2019-07-29 2019-09-27 广东省新材料研究所 涂布辊、其应用及制备方法
CN114744068A (zh) * 2022-03-30 2022-07-12 天津南玻节能玻璃有限公司 一种光伏建筑一体化组件及其制备方法
CN114744068B (zh) * 2022-03-30 2024-03-19 天津南玻节能玻璃有限公司 一种光伏建筑一体化组件及其制备方法

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