WO2024043120A1 - 誘電体多層膜付き基板およびその製造方法 - Google Patents

誘電体多層膜付き基板およびその製造方法 Download PDF

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Publication number
WO2024043120A1
WO2024043120A1 PCT/JP2023/029281 JP2023029281W WO2024043120A1 WO 2024043120 A1 WO2024043120 A1 WO 2024043120A1 JP 2023029281 W JP2023029281 W JP 2023029281W WO 2024043120 A1 WO2024043120 A1 WO 2024043120A1
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Prior art keywords
refractive index
film
substrate
dielectric multilayer
film layer
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PCT/JP2023/029281
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English (en)
French (fr)
Japanese (ja)
Inventor
英明 高星
友志 新江
泰永 西川
晃男 藤原
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AGC Inc
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Asahi Glass Co Ltd
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Priority to CN202380060759.6A priority Critical patent/CN119731562A/zh
Priority to JP2024542757A priority patent/JPWO2024043120A1/ja
Publication of WO2024043120A1 publication Critical patent/WO2024043120A1/ja
Priority to US19/046,758 priority patent/US20250180784A1/en
Anticipated expiration legal-status Critical
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/023—Optical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • 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
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/285—Interference filters comprising deposited thin solid films
    • 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
    • C03C2217/212—TiO2
    • 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
    • C03C2217/213—SiO2
    • 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
    • C03C2217/228—Other specific oxides
    • 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
    • C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering

Definitions

  • the present invention relates to a substrate with a dielectric multilayer film and a method for manufacturing the same.
  • Patent Document 1 discloses a configuration in which a dielectric multilayer film is provided on a substrate, and the dielectric multilayer film has a plurality of low refractive index layers, high refractive index layers, and antireflection layers from the surface. There is.
  • Patent Document 2 discloses that a light-transmitting layer including a plurality of first dielectric layers made of silicon oxide and a plurality of second dielectric layers made of titanium oxide on the surface of a substrate made of a light-transmitting material.
  • An optical filter member with a membrane is disclosed.
  • Patent Document 3 listed below has an inorganic thin film consisting of multiple layers on a substrate, and the inorganic thin film has a plurality of layers of silicon oxide and a plurality of metal oxide layers laminated, and the An optical article is disclosed in which the oxide is a metal oxide containing at least one of zirconium, tantalum, and titanium, and has a surface roughness of 0.55 nm or more and 0.70 nm or less.
  • Patent Document 4 listed below discloses a visible light mirror that includes a mirror stack layer portion on a substrate that includes a layer of a dielectric material made of alternately laminated layers of Ta 2 O 5 and SiO 2 .
  • Patent Document 5 discloses a polarizing beam splitter in which a high refractive index dielectric film made of a high refractive index material and a low refractive index dielectric film made of a low refractive index material are alternately laminated on a base material.
  • Ta2O5 , TiO2 , HfO2 , ZrO2 , LaTiXOY , Y2O3 are exemplified as high refractive index dielectric films
  • SiO2 , MgF2 are exemplified as low refractive index dielectric films. Illustrated.
  • Patent Document 6 listed below describes an antireflection film consisting of a multilayer film in which a total of 14 to 17 layers are laminated on a substrate surface from the substrate side to the air side based on alternating layers of film types TiO 2 and SiO 2 . is disclosed.
  • a technique is also known in which a transparent antireflection film having a dielectric multilayer film is installed on the front surface of an image display device in order to prevent external light from being reflected on the screen.
  • a dielectric multilayer film is formed on a substrate by sputtering (see Patent Documents 1 to 2, 5 to 6, etc.)
  • the resulting dielectric multilayer film has high residual stress, causing warping and peeling.
  • reducing film stress is important for stabilizing long-term properties.
  • an object of the present invention is to provide a substrate with a dielectric multilayer film with reduced film stress and a method for manufacturing the same.
  • a substrate with a dielectric multilayer film comprising a dielectric multilayer film on the substrate
  • the dielectric multilayer film includes a first dielectric multilayer film and a second dielectric multilayer film stacked in this order from the substrate side
  • the first dielectric laminated film is formed by alternately stacking the same number of first high refractive index film layers containing TiO 2 and first low refractive index film layers containing SiO 2 in this order from the substrate side
  • the second dielectric laminated film includes, from the substrate side, a second high refractive index film layer containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer containing SiO 2 alternately in this order.
  • the first low refractive index film layer located farthest from the substrate has a thickness of 30 nm or more;
  • Substrate with dielectric multilayer film (2)
  • Substrate with multilayer film. (5) The total layer of the first high refractive index film layer, the first low refractive index film layer, the second high refractive index film layer, and the second low refractive index film layer in the dielectric multilayer film.
  • the dielectric multilayer film-coated substrate according to (5) wherein the total number of layers is six.
  • the dielectric multilayer film includes, in order from the substrate side: a first high refractive index film layer a1 containing TiO 2 ; a first low refractive index film layer b1 containing SiO 2 ; a first high refractive index film layer a2 containing TiO 2 ; a first low refractive index film layer b2 containing SiO 2 ; a second high refractive index film layer a3 containing Ta 2 O 5 or Nb 2 O 5 ; a second low refractive index film layer b3 containing SiO 2 ;
  • the dielectric multilayer film-coated substrate according to (6) above which has the following.
  • the dielectric multilayer film in order from the substrate side, a first high refractive index film layer a1 containing TiO 2 with a film thickness of 20 nm or less; a first low refractive index film layer b1 containing SiO 2 with a film thickness of 30 nm or more and 50 nm or less; a first high refractive index film layer a2 containing TiO 2 with a film thickness of 10 nm or more and 50 nm or less; a first low refractive index film layer b2 containing SiO 2 with a film thickness of 30 nm or more and 50 nm or less; a second high refractive index film layer a3 containing Ta 2 O 5 or Nb 2 O 5 with a film thickness of 15 nm or more and 50 nm or less, and a second low refractive index film layer b3 containing SiO 2 with a film thickness of 75 nm or more and 105 nm or less;
  • the dielectric multilayer film-coated substrate according to (1) or (2) wherein the substrate includes at least one of glass and resin.
  • a second high refractive index film layer containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer containing SiO 2 are alternately stacked in this order on the first dielectric laminated film in equal numbers. , forming a second dielectric stack; A method for manufacturing a substrate with a dielectric multilayer film, wherein the first low refractive index film layer located farthest from the substrate in the first dielectric multilayer film has a thickness of 30 nm or more.
  • a substrate with a dielectric multilayer film with reduced film stress it is possible to provide a substrate with a dielectric multilayer film with reduced film stress and a method for manufacturing the same.
  • FIG. 1 is a cross-sectional view schematically showing a configuration example of a dielectric multilayer film-coated substrate according to an embodiment of the present invention.
  • FIG. 2 is a cross-sectional view schematically showing a particularly preferable configuration example of the dielectric multilayer film-coated substrate according to the embodiment of the present invention.
  • FIG. 3 is a graph showing the film thickness of the dielectric multilayer film produced in the example.
  • FIG. 4 is a graph showing the film stress of the dielectric multilayer film produced in the example.
  • having another layer, film, etc. on the main surface of a substrate or on a film such as a dielectric multilayer film means that the other layer, film, etc. is on the main surface, layer, or film.
  • the present invention is not limited to an embodiment in which a layer or a film is provided in the upper direction of the layer, but is not limited to an embodiment in which a layer, a film, or the like is provided in the upper direction.
  • FIG. 1 is a cross-sectional view schematically showing a configuration example of a dielectric multilayer film-coated substrate according to an embodiment of the present invention.
  • the dielectric multilayer film is formed by laminating a first dielectric laminated film 10 and a second dielectric laminated film 20 in this order on a substrate S.
  • the dielectric multilayer film has a first portion made of the first dielectric laminated film 10 and a second portion made of the second dielectric laminated film 20 on the substrate S in this order.
  • the first dielectric laminated film 10 has a first high refractive index film layer 101 containing TiO 2 and a first low refractive index film layer 102 containing SiO 2 alternately stacked in this order from the substrate S side.
  • the alternating stacking can be repeated multiple times.
  • the number of first high refractive index film layers 101 and first low refractive index film layers 102 in the first dielectric laminated film 10 is the same.
  • a high refractive index film layer means a dielectric film having a refractive index higher than the refractive index of the substrate
  • a low refractive index film layer means a dielectric film having a refractive index lower than that of the high refractive index layer. refers to a dielectric film having a constant
  • the second dielectric laminated film 20 includes, from the substrate S side, a second high refractive index film layer 201 containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer 202 containing SiO 2 .
  • the layers are alternately stacked in sequence, and this alternate stacking can be repeated multiple times.
  • the number of second high refractive index film layers 201 and second low refractive index film layers 202 in the second dielectric laminated film 20 is the same.
  • the first low refractive index film layer 1022 located farthest from the substrate S has a thickness of 30 nm or more.
  • the dielectric multilayer film is made up of the same number of high refractive index film layers and low refractive index film layers stacked alternately in this order from the substrate S side.
  • the first layer is a high refractive index film layer and the final layer is a low refractive index film layer, so that the film stress of the dielectric multilayer film can be reduced, and the luminous reflectance described below can be reduced. (SCI Y) can also be reduced.
  • the first high refractive index film layer 101 may contain a high refractive index material other than TiO 2 . In that case, a high refractive index material with higher film stress than Ta 2 O 5 and Nb 2 O 5 is preferable. However, from the viewpoint of achieving the effects of the present invention, the first high refractive index film layer 101 does not contain Ta 2 O 5 or Nb 2 O 5 . That is, "the second high refractive index film layer 201 containing Ta 2 O 5 or Nb 2 O 5 " does not exist in the first dielectric laminated film 10.
  • the second high refractive index film layer 201 may contain a high refractive index material other than Ta 2 O 5 or Nb 2 O 5 . In that case, a high refractive index material with lower film stress than TiO 2 is preferable. However, from the viewpoint of achieving the effects of the present invention, the second high refractive index film layer 201 does not contain TiO 2 . That is, in the second dielectric laminated film 20, "the first high refractive index film layer 101 containing TiO 2 " does not exist.
  • the first dielectric laminated film 10 includes the first high refractive index film layer 101 containing TiO 2 and the first low refractive index film layer 102 containing SiO 2 alternately in this order from the substrate S side. Laminated on.
  • the second dielectric laminated film 20 also includes, from the substrate S side, a second high refractive index film layer 201 containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer 202 containing SiO 2 . are alternately stacked in this order.
  • the total number of layers of the first high refractive index film layer, the first low refractive index film layer, the second high refractive index film layer, and the second low refractive index film layer in the dielectric multilayer film is From the viewpoint of further reducing membrane stress, the number of layers is preferably 4 or more and 12 or less. Further, the total number of layers is more preferably 4 or more, further preferably 6 or more, more preferably 10 or less, and even more preferably 8 or less. It is particularly preferable that the total number of layers is six.
  • the total number of layers of the first high refractive index film layer 101 and the first low refractive index film layer 102 in the first dielectric multilayer film 10 is determined from the viewpoint of further reducing the film stress of the dielectric multilayer film. It is preferable that the number of layers is 2 or more and 8 or less. Further, the total number of layers is more preferably two or more, and more preferably six or less. It is particularly preferable that the total number of layers is four.
  • the total number of layers of the second high refractive index film layer 201 and the second low refractive index film layer 202 in the second dielectric laminated film 20 is determined from the viewpoint of further reducing the film stress of the dielectric multilayer film. It is preferable that the number of layers is 2 or more and 8 or less. Further, the total number of layers is more preferably 2 or more, more preferably 8 or less, even more preferably 6 or less, and even more preferably 4 or less. It is particularly preferable that the total number of layers is two.
  • the first low refractive index film layer 102 (1022) located farthest from the substrate S in the first dielectric multilayer film 10 has a thickness of 30 nm. That's all. From the viewpoint of further reducing the film stress of the dielectric multilayer film, the thickness is preferably 30 nm or more and 50 nm or less. The thickness is more preferably 45 nm or less, and even more preferably 40 nm or less.
  • the first low refractive index film layer located farthest from the substrate S is, in other words, "the first low refractive index film layer in contact with the second dielectric laminated film”.
  • the refractive index and film thickness that can reproduce the reflection spectrum can be determined by a computer using the refractive index dispersion and film thickness as variables from the actual reflection spectrum.
  • the above steps can be carried out using commercially available software, such as TF-Calc (manufactured by Hulinx) or OptiLayer (manufactured by K-One).
  • the film thickness can also be estimated by observing the cross-sectional structure using a scanning electron microscope and measuring the thickness of layers with different contrasts. In this case, since resolution is important, it is preferable to measure the viewing angle so that the entire laminated structure can be confirmed, and to use the average of measurements at a plurality of points or more. It is more preferable to use the average of measurements at five or more points.
  • a second low refractive index film layer located farthest from the substrate S of the second dielectric multilayer film 20 is preferably 75 nm or more and 105 nm or less.
  • the thickness is more preferably 80 nm or more, more preferably 100 nm or less, and even more preferably 95 nm or less.
  • the first high refractive index film layer located farthest from the substrate S in the first dielectric multilayer film 10 in the form of FIG.
  • the thickness T1 of the refractive index film layer a2) and the second high refractive index film layer located closest to the substrate side of the second dielectric laminated film (high refractive index film layer in the form of FIG. 2 described later)
  • the ratio of thickness T2 (T1/T2) in a3) is preferably 0.7 or more and 1.4 or less.
  • the ratio (T1/T2) is more preferably 1 or more, further preferably 1.2 or more, and even more preferably 1.3 or more.
  • the total thickness of the dielectric multilayer film is preferably 300 nm or less, more preferably 250 nm or less.
  • the film stress of the dielectric multilayer film is suppressed in this embodiment.
  • the internal stress of a dielectric film changes depending on the gas pressure during film formation, but from the viewpoint of film density, it is necessary to lower the pressure of the sputtering gas (generally Ar) during film formation.
  • the pressure of the sputtering gas generally Ar
  • the dielectric film basically has compressive stress, but the magnitude of the stress differs depending on the type of material.
  • the present invention is not limited in any way by this reason.
  • FIG. 2 is a cross-sectional view schematically showing a substrate with a dielectric multilayer film according to an embodiment of the present invention in the particularly preferred form described above.
  • the dielectric multilayer film-coated substrate 2 includes a first dielectric multilayer film 10 and a second dielectric multilayer film 20 laminated in this order on a substrate S, and the first dielectric multilayer film 10 is , from the substrate S side, a first high refractive index film layer a1 containing TiO2 , a first low refractive index film layer b1 containing SiO2 , a first high refractive index film layer a2 containing TiO2 , and a first high refractive index film layer a2 containing SiO2. 1 low refractive index film layer b2 are laminated in this order.
  • the second dielectric laminated film 20 includes, from the substrate S side, a second high refractive index film layer a3 containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer b3 containing SiO 2 . They are stacked in order.
  • the first low refractive index film layer b2 located farthest from the substrate S has a thickness of 30 nm or more.
  • dielectric multilayer film-attached substrate 2 shown in FIG. 2 a total of six dielectric multilayer films are provided on the substrate S.
  • the form shown in FIG. 2 is particularly preferable from the viewpoint that the film stress of the dielectric multilayer film can be further reduced and the luminous reflectance (SCI Y) can also be reduced.
  • the thickness of the first high refractive index film layer a1 containing TiO 2 is preferably 20 nm or less, more preferably 3 nm or more and 15 nm or less.
  • the thickness of the first high refractive index film layer a1 is more preferably 10 nm or less.
  • the thickness of the first low refractive index film layer b1 containing SiO 2 is preferably 30 nm or more and 50 nm or less.
  • the thickness of the first low refractive index film layer b1 is more preferably 35 nm or more, more preferably 45 nm or less, and even more preferably 40 nm or less.
  • the thickness of the first high refractive index film layer a2 containing TiO 2 is preferably 10 nm or more and 50 nm or less.
  • the thickness of the first high refractive index film layer a2 is more preferably 15 nm or more, even more preferably 20 nm or more, and more preferably 45 nm or less, even more preferably 40 nm or less.
  • the thickness of the first low refractive index film layer b2 containing SiO 2 is preferably 30 nm or more and 50 nm or less.
  • the thickness of the first low refractive index film layer b2 is preferably 30 nm or more, preferably 50 nm or less, more preferably 45 nm or less, and even more preferably 40 nm or less. Note that the first low refractive index film layer b2 containing SiO 2 corresponds to the first low refractive index film layer located farthest from the substrate.
  • the thickness of the second high refractive index film layer a3 containing Ta 2 O 5 or Nb 2 O 5 is preferably 15 nm or more and 50 nm or less.
  • the thickness of the second high refractive index film layer a3 is more preferably 20 nm or more, even more preferably 30 nm or more, and more preferably 45 nm or less, even more preferably 40 nm or less.
  • the thickness of the second low refractive index film layer b3 containing SiO 2 is preferably 75 nm or more and 105 nm or less.
  • the thickness of the second low refractive index film layer b3 is more preferably 80 nm or more, more preferably 100 nm or less, and even more preferably 95 nm or less.
  • the substrate of this embodiment any conventionally known substrate such as glass or resin film can be used.
  • the refractive index of the substrate is preferably 1.4 or more and 1.7 or less. If the refractive index of the substrate is within the above range, reflection at the bonding surface can be sufficiently suppressed when a display, a touch panel, or the like is optically bonded.
  • the refractive index of the substrate is more preferably 1.45 or more, still more preferably 1.47 or more, and more preferably 1.65 or less, still more preferably 1.6 or less.
  • the substrate preferably contains at least one of glass and resin.
  • the type of glass is not particularly limited, and glasses having various compositions can be used.
  • the glass preferably contains quartz or sodium, and preferably has a composition that can be strengthened by molding or chemical strengthening treatment. Specific examples include quartz glass, aluminosilicate glass, soda lime glass, borosilicate glass, alkali-free glass, lead glass, alkali barium glass, aluminoborosilicate glass, and the like. Note that in this specification, when a substrate includes glass, the substrate is also referred to as a glass substrate.
  • the thickness of the glass substrate is not particularly limited, but is usually preferably 5 mm or less, more preferably 3 mm or less, and even more preferably 1.5 mm or less. Moreover, it is usually 0.2 mm or more.
  • the glass substrate is preferably chemically strengthened glass. This increases the strength of the dielectric multilayer film coated substrate.
  • chemical strengthening is performed after providing an anti-glare layer and before forming a dielectric multilayer film (multilayer film).
  • the type of resin is not particularly limited, and resins having various compositions can be used.
  • the resin is preferably a thermoplastic resin or a thermosetting resin, such as polyvinyl chloride resin, polyethylene resin, polypropylene resin, polystyrene resin, polyvinyl acetate resin, polyester resin, polyurethane resin, cellulose resin, acrylic resin, etc.
  • Resin AS (acrylonitrile-styrene) resin, ABS (acrylonitrile-butadiene-styrene) resin, fluorine resin, thermoplastic elastomer, polyamide resin, polyimide resin, polyacetal resin, polycarbonate resin, modified polyphenylene ether resin, polyethylene terephthalate resin, poly Examples include butylene terephthalate resin, polylactic acid resin, cyclic polyolefin resin, polyphenylene sulfide resin, and the like.
  • cellulose resins are preferred, and examples include triacetyl cellulose resins, polycarbonate resins, and polyethylene terephthalate resins. These resins may be used alone or in combination of two or more. It is particularly preferred that the resin comprises at least one resin selected from polyethylene terephthalate, polycarbonate, acrylic, silicone and triacetylcellulose.
  • a substrate when a substrate includes resin, the substrate is also referred to as a resin substrate.
  • the shape of the resin substrate is not particularly limited, and examples include a film shape and a plate shape, but a film shape is preferable from the viewpoint of scattering prevention.
  • the thickness is not particularly limited, but is preferably 20 to 250 ⁇ m, more preferably 40 to 188 ⁇ m.
  • the thickness is not particularly limited, but is usually preferably 5 mm or less, more preferably 3 mm or less, and even more preferably 1.5 mm or less. Moreover, it is usually 0.2 mm or more.
  • the resin substrate may be provided on the glass substrate, for example.
  • an adhesive layer can also be provided between the substrate and the dielectric multilayer film.
  • the type of adhesive layer is not particularly limited, and may be an organic layer made of resin or the like or an inorganic layer. Each case will be explained in detail below.
  • the organic layer is preferably a resin layer containing a predetermined resin.
  • the type of resin forming the resin layer is not particularly limited, and examples thereof include silicone resin, polyimide resin, acrylic resin, polyolefin resin, polyurethane resin, and fluororesin. It is also possible to use a mixture of several types of resin. Among these, silicone resins, polyimide resins, and fluororesins are preferred.
  • the thickness of the organic layer is not particularly limited, but is preferably 1 to 100 ⁇ m, more preferably 5 to 30 ⁇ m, and even more preferably 7 to 20 ⁇ m. When the thickness of the organic layer is within the above range, the substrate and the dielectric multilayer film will have sufficient adhesion.
  • the organic layer may contain a leveling agent.
  • the type of leveling agent is not particularly limited, but typical examples include fluorine-based leveling agents.
  • the material constituting the inorganic layer is not particularly limited, but preferably includes at least one selected from the group consisting of oxides, nitrides, oxynitrides, carbides, carbonitrides, silicides, and fluorides.
  • oxides preferably metal oxides
  • nitrides preferably metal nitrides
  • oxynitrides preferably metal oxynitrides
  • Si Si, Hf, Zr, Ta, Ti, and Y.
  • Nb Na, Co, Al, Zn, Pb, Mg, Bi, La, Ce, Pr, Sm, Eu, Gd, Dy, Er, Sr, Sn, In and Ba.
  • Examples include nitrides, nitrides, and oxynitrides.
  • silicon nitride oxide SiN x O y
  • titanium oxide TiO 2
  • indium oxide In 2 O 3
  • indium cerium oxide ICO
  • tin oxide SnO 2
  • zinc oxide ZnO
  • gallium oxide Ga 2 O 3
  • indium tin oxide ITO
  • indium zinc oxide IZO
  • zinc tin oxide ZTO
  • gallium-doped zinc oxide GZO
  • carbides preferably metal carbides
  • carbonitrides preferably metal carbonitrides
  • Examples include carbonates and carbonates.
  • silicon carbide oxide (SiCO) may be used.
  • the carbide may be a so-called carbon material, for example, a carbide obtained by sintering a resin component such as a phenol resin.
  • silicide examples include silicides of one or more elements selected from Mo, W, and Cr.
  • fluoride preferably metal fluoride
  • fluorides of one or more elements selected from Mg, Y, La, and Ba examples include magnesium fluoride (MgF 2 ).
  • the thickness of the inorganic layer is not particularly limited, but from the viewpoint of adhesion between the substrate and the dielectric multilayer film, it is preferably 5 to 5000 nm, more preferably 10 to 500 nm.
  • the surface roughness (Ra) of the surface of the inorganic layer in contact with the dielectric multilayer film is preferably 2.0 nm or less, more preferably 1.0 nm or less.
  • the lower limit is not particularly limited, but 0 is most preferable. Within the above range, the adhesion to the dielectric multilayer film will be better.
  • Ra is measured according to JIS B 0601 (revised in 2001).
  • the adhesive layer may be a plasma polymerized film.
  • the materials forming the plasma polymerized film include fluorocarbon monomers such as CF4 , CHF3 , CH3F , methane, ethane, propane, ethylene, propylene, acetylene, benzene, toluene, C Examples include hydrocarbon monomers such as 4H8 , hydrogen, SF6, and the like. Particularly preferred is a plasma polymerized membrane made of fluorocarbon monomer or hydrocarbon monomer. These may be used alone or in combination of two or more types.
  • the thickness of the plasma polymerized film is preferably 1 to 100 nm, more preferably 1 to 50 nm, and even more preferably 1 to 10 nm.
  • At least one of an anti-glare layer and a hard coat layer may be provided on the surface of the substrate in this embodiment on the side where the dielectric multilayer film is provided.
  • the anti-glare layer has an uneven shape on one side, which causes external scattering or internal scattering, thereby increasing the haze value and imparting anti-glare properties.
  • a conventionally known anti-glare layer can be used, for example, an anti-glare layer composition comprising at least a particulate substance that itself has anti-glare properties dispersed in a solution in which a polymer resin as a binder is dissolved. It may be composed of.
  • the anti-glare layer can be formed by applying the anti-glare layer composition, for example, to one main surface of the substrate.
  • particulate substances having anti-glare properties include inorganic fine particles such as silica, clay, talc, calcium carbonate, calcium sulfate, barium sulfate, aluminum silicate, titanium oxide, synthetic zeolite, alumina, and smectite, as well as styrene resin. , urethane resin, benzoguanamine resin, silicone resin, acrylic resin, and the like.
  • a conventionally known hard coat layer can be used, and for example, it may be composed of a hard coat layer composition containing a polymer resin described below.
  • the hard coat layer can be formed by applying the hard coat layer composition, for example, to one main surface of a transparent substrate such as a substrate.
  • examples of polymer resins used as binders for anti-glare layers and hard coat layers include polyester resins, acrylic resins, acrylic urethane resins, polyester acrylate resins, polyurethane acrylate resins, epoxy acrylate resins, and urethane resins.
  • Polymer resins including resins and the like can be used.
  • the substrate with a dielectric multilayer film in this embodiment may further include an antifouling film (also referred to as "Anti Finger Print (AFP) film”) on the dielectric multilayer film from the viewpoint of protecting its outermost surface. good.
  • the antifouling film can be made of, for example, a fluorine-containing organosilicon compound.
  • the fluorine-containing organosilicon compound can be used without particular limitation as long as it can impart stain resistance, water repellency, and oil repellency; for example, it can be selected from the group consisting of polyfluoropolyether groups, polyfluoroalkylene groups, and polyfluoroalkyl groups. Examples include fluorine-containing organosilicon compounds having one or more groups.
  • the polyfluoropolyether group is a divalent group having a structure in which polyfluoroalkylene groups and ether oxygen atoms are alternately bonded.
  • 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.), KY-185 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.), Optool (registered trademark) DSX and Optool AES (all trade names, manufactured by Daikin), etc. can be preferably used.
  • the antifouling film is provided on the dielectric multilayer film.
  • a dielectric multilayer film is provided on both of the two main surfaces of the substrate, an antifouling film can be formed on both dielectric multilayer films, but an antifouling film can be formed on only one of the main surfaces.
  • a structure in which dirt films are laminated may also be used. This is because the antifouling film only needs to be provided at a location that may come into contact with human hands, and can be selected depending on the intended use.
  • the dielectric multilayer film-coated substrate in this embodiment may include an adhesive layer on the main surface of the transparent substrate on the side on which the dielectric multilayer film is not provided, of the two main surfaces.
  • the dielectric multilayer film-coated substrate is attached to, for example, an image display device via an adhesive layer.
  • the adhesive layer can be formed using a conventionally known adhesive composition, such as an optically clear adhesive (OCA) or an optically clear resin (OCR) such as a UV curable resin. It will be done.
  • OCA and OCR include, for example, acrylic polymers, silicone polymers, polyesters, polyurethanes, polyamides, polyvinyl ethers, vinyl acetate/vinyl chloride copolymers, modified polyolefins, epoxy systems, fluorine systems, rubber systems such as natural rubber, synthetic rubber, etc.
  • the adhesive layer preferably has a luminous transmittance of 90% or more, preferably 91% or more, and 92% or more, as measured by a spectrophotometer according to the provisions of JIS Z 8709 (1999). It is more preferable that When the transmittance of the adhesive layer is within the above range, visibility of, for example, an image display device is not impaired.
  • the luminous reflectance (SCI Y) of the outermost surface of the dielectric multilayer film is 4% or less. If the luminous reflectance (SCI Y) is within the above range, when used in an image display device, the effect of preventing reflection of external light on the screen is high.
  • the luminous reflectance (SCI Y) is more preferably 2% or less, particularly preferably 1% or less.
  • the luminous reflectance (SCI) can be reduced by adjusting the balance between the thicknesses of the high refractive index film layer and the low refractive index film layer to generate optical interference and suppress reflected light.
  • the dielectric multilayer film-coated substrate of this embodiment can be suitably used as an antireflection film for displays, touch panels, and the like.
  • a method for manufacturing a substrate with a dielectric multilayer film according to an embodiment of the present invention includes: A dielectric multilayer film including a first dielectric multilayer film and a second dielectric multilayer film is provided on the substrate, On the substrate, a first high refractive index film layer containing TiO 2 and a first low refractive index film layer containing SiO 2 are alternately stacked in the same number in this order to form a first dielectric laminated film. , A second high refractive index film layer containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer containing SiO 2 are alternately stacked in this order on the first dielectric laminated film in equal numbers. , forming a second dielectric stack.
  • Lamination of each of the above layers can be performed using a known film forming method such as a dry film forming process such as a CVD method, a sputtering method, or a vacuum evaporation method, or a wet film forming process such as a spray method or a dipping method.
  • a dry film forming process such as a CVD method, a sputtering method, or a vacuum evaporation method
  • a wet film forming process such as a spray method or a dipping method.
  • a dry film forming process is preferred, and a sputtering method is particularly preferred.
  • Examples of the sputtering method include methods such as magnetron sputtering, pulse sputtering, AC sputtering, and digital sputtering.
  • a magnet in magnetron sputtering, a magnet is installed on the back surface of a dielectric material that serves as a base material to generate a magnetic field, and gas ion atoms collide with the surface of the dielectric material and are ejected, resulting in sputtering with a thickness of several nanometers. It is a film forming method that can form a continuous film of a dielectric material that is an oxide or nitride of the dielectric material.
  • digital sputtering uses the same process of first forming an extremely thin metal film by sputtering and then oxidizing it by irradiating it with oxygen plasma, oxygen ions, or oxygen radicals. This method repeatedly forms a thin film of metal oxide in a chamber.
  • the film-forming molecules are metal when deposited on the substrate, it is presumed that the film is more ductile than when the film is deposited using a metal oxide. Therefore, even with the same energy, rearrangement of film-forming molecules is likely to occur, resulting in a dense and smooth film.
  • a substrate with a dielectric multilayer film comprising a dielectric multilayer film on the substrate
  • the dielectric multilayer film includes a first dielectric multilayer film and a second dielectric multilayer film stacked in this order from the substrate side
  • the first dielectric laminated film is formed by alternately stacking the same number of first high refractive index film layers containing TiO 2 and first low refractive index film layers containing SiO 2 in this order from the substrate side
  • the second dielectric laminated film includes, from the substrate side, a second high refractive index film layer containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer containing SiO 2 alternately in this order.
  • the first low refractive index film layer located farthest from the substrate has a thickness of 30 nm or more;
  • Substrate with dielectric multilayer film (2)
  • the dielectric multilayer film includes, in order from the substrate side: a first high refractive index film layer a1 containing TiO 2 ; a first low refractive index film layer b1 containing SiO 2 ; a first high refractive index film layer a2 containing TiO 2 ; a first low refractive index film layer b2 containing SiO 2 ; a second high refractive index film layer a3 containing Ta 2 O 5 or Nb 2 O 5 ; a second low refractive index film layer b3 containing SiO 2 ;
  • the dielectric multilayer film-coated substrate according to (6) above which has the following.
  • the dielectric multilayer film in order from the substrate side, a first high refractive index film layer a1 containing TiO 2 with a film thickness of 20 nm or less; a first low refractive index film layer b1 containing SiO 2 with a film thickness of 30 nm or more and 50 nm or less; a first high refractive index film layer a2 containing TiO 2 with a film thickness of 10 nm or more and 50 nm or less; a first low refractive index film layer b2 containing SiO 2 with a film thickness of 30 nm or more and 50 nm or less; a second high refractive index film layer a3 containing Ta 2 O 5 or Nb 2 O 5 with a film thickness of 15 nm or more and 50 nm or less, and a second low refractive index film layer b3 containing SiO 2 with a film thickness of 75 nm or more and 105 nm or less;
  • (11) A method for manufacturing a substrate with a dielectric multilayer film, comprising a dielectric multilayer film including a first dielectric multilayer film and a second dielectric multilayer film on the substrate, On the substrate, a first high refractive index film layer containing TiO 2 and a first low refractive index film layer containing SiO 2 are alternately stacked in the same number in this order to form a first dielectric laminated film.
  • a second high refractive index film layer containing Ta 2 O 5 or Nb 2 O 5 and a second low refractive index film layer containing SiO 2 are alternately stacked in this order on the first dielectric laminated film in equal numbers. , forming a second dielectric stack; A method for manufacturing a substrate with a dielectric multilayer film, wherein the first low refractive index film layer located farthest from the substrate in the first dielectric multilayer film has a thickness of 30 nm or more.
  • Examples 1 to 3 are examples, and Examples 4 to 8 are comparative examples.
  • ⁇ Film thickness measurement> The reflectance at each wavelength was measured using a spectrophotometer (manufactured by Shimadzu Corporation, product name: SolidSpec3700), and the refractive index dispersion and film thickness were used as variables from the obtained actual reflection spectrum. The thickness of each film was determined using .
  • the luminous reflectance (SCI Y) is determined by measuring the luminous reflectance of the outermost surface of the dielectric multilayer film using a spectrophotometer (manufactured by Shimadzu Corporation, product name: SolidSpec3700) using the method specified in JIS Z 8722 (2009). ).
  • Example 1 A dielectric multilayer film-coated substrate of Example 1 was produced by the following method.
  • the dielectric multilayer film coated substrate of Example 1 has the layer structure shown in FIG. That is, the substrate 2 with a dielectric multilayer film has a first dielectric laminated film 10 and a second dielectric laminated film 20 laminated in this order on a substrate S.
  • the first dielectric laminated film 10 includes, from the substrate S side, a first high refractive index film layer a1 containing TiO2 , a first low refractive index film layer b1 containing SiO2 , and a first high refractive index film containing TiO2 .
  • Layer a2 and first low refractive index film layer b2 containing SiO 2 were laminated in this order.
  • the second dielectric laminated film 20 has a second high refractive index film layer a3 containing Ta 2 O 5 and a second low refractive index film layer b3 containing SiO 2 stacked in this order from the substrate S side.
  • the dielectric multilayer film coated substrate 2 of Example 1 has a total of six dielectric laminated films provided on the substrate S. This will be explained in detail below.
  • a quartz substrate synthetic recycled material, manufactured by Sanei Optical Co., Ltd.
  • a refractive index of 1.46 and a diameter of 150 mm x 0.5 mm was used.
  • the pre-evacuation pressure was set to 10 -4 Pa or less, and reactive sputtering was performed using a DC magnetron and oxygen gas under a pressure atmosphere of 0.1 Pa using Ar gas during film formation.
  • a first high refractive index film layer a1 containing TiO 2 with a thickness of 10 nm was provided.
  • the preliminary evacuation pressure is set to 10 ⁇ 4 Pa or less, and DC is applied under the conditions of a pressure atmosphere of 0.1 Pa using Ar gas during film formation.
  • a first low refractive index film layer b1 containing SiO 2 with a thickness of 40 nm was provided by reactive sputtering using a magnetron and oxygen gas.
  • sufficient vacuum evacuation is performed on the first low refractive index film layer b1, the preliminary evacuation pressure is set to 10 ⁇ 4 Pa or less, and DC is applied under the conditions of a pressure atmosphere of 0.1 Pa using Ar gas during film formation.
  • a first high refractive index film layer a2 containing TiO 2 with a thickness of 30 nm was provided by reactive sputtering using a magnetron and oxygen gas. Subsequently, sufficient vacuum evacuation is performed on the first high refractive index film layer a2, the preliminary evacuation pressure is set to 10 -4 Pa or less, and DC is applied under the conditions of a pressure atmosphere of 0.1 Pa using Ar gas during film formation.
  • a first low refractive index film layer b2 containing SiO 2 with a thickness of 30 nm was provided by reactive sputtering using a magnetron and oxygen gas. In this way, the first dielectric laminated film 10 was provided.
  • a second high refractive index film layer a3 containing Ta 2 O 5 having a thickness of 30 nm was provided by reactive sputtering using a DC magnetron and oxygen gas under conditions of 1 Pa.
  • sufficient vacuum evacuation is performed on the second high refractive index film layer a3, the preliminary evacuation pressure is set to 10 -4 Pa or less, and a DC magnetron is applied to the second high refractive index film layer a3 under the condition of a pressure atmosphere of 0.1 Pa using Ar gas during film formation.
  • a second low refractive index film layer b3 containing SiO 2 with a thickness of 85 nm was provided by reactive sputtering using oxygen gas.
  • the second dielectric laminated film 20 was provided on the first dielectric laminated film 10, and the substrate with the dielectric multilayer film of Example 1 was produced.
  • Example 2 Example 2
  • Example 8 Example 1 was repeated except that the layer structure and film thickness of the dielectric multilayer film were changed as shown in Table 1.
  • the substrates with dielectric multilayer films of Examples 1 to 3 have a first dielectric multilayer film and a second dielectric multilayer film laminated in this order on the substrate, and the first dielectric multilayer film is In the laminated film, a first high refractive index film layer containing TiO 2 and a first low refractive index film layer containing SiO 2 are alternately laminated in this order from the substrate side, and the first dielectric film layer in the first dielectric laminated film is The number of high refractive index film layers and the first low refractive index film layer is the same, and the second dielectric laminated film has a second high refractive index film containing Ta 2 O 5 or Nb 2 O 5 from the substrate S side.
  • the film layer and the second low refractive index film layer containing SiO 2 are alternately laminated in this order, and the number of the second high refractive index film layer and the second low refractive index film layer in the second dielectric laminated film is the same.
  • the first low refractive index film layer located farthest from the substrate has a thickness of 30 nm or more, so film stress is reduced and warping and peeling can be sufficiently suppressed. I understand that.
  • Example 4 the film stress increased because the second high refractive index film layer containing Ta 2 O 5 or Nb 2 O 5 was not provided.
  • Example 5 the film stress increased because the first high refractive index film layer containing TiO 2 was not provided.
  • Example 6 the film stress increased because the first low refractive index film layer was not provided on the side farthest from the substrate in the first dielectric laminated film.
  • Example 7 and 8 the film stress increased because the thickness of the first low refractive index film layer located farthest from the substrate was less than 30 nm.

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Publication number Priority date Publication date Assignee Title
JP2002014203A (ja) * 2000-06-30 2002-01-18 Canon Inc 反射防止膜及びそれを用いた光学部材
JP2002040237A (ja) * 2000-07-19 2002-02-06 Minolta Co Ltd 多層光学薄膜
JP2006171332A (ja) * 2004-12-15 2006-06-29 Nippon Electric Glass Co Ltd 反射防止膜
JP2011237472A (ja) * 2010-05-06 2011-11-24 Konica Minolta Opto Inc 撮像用レンズ
JP2012118536A (ja) * 2009-10-09 2012-06-21 Seiko Epson Corp 光学物品、光学物品の製造方法、電子機器
JP2022072420A (ja) * 2020-10-29 2022-05-17 キヤノン株式会社 光学素子、光学系、および、光学機器

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Publication number Priority date Publication date Assignee Title
JP2002014203A (ja) * 2000-06-30 2002-01-18 Canon Inc 反射防止膜及びそれを用いた光学部材
JP2002040237A (ja) * 2000-07-19 2002-02-06 Minolta Co Ltd 多層光学薄膜
JP2006171332A (ja) * 2004-12-15 2006-06-29 Nippon Electric Glass Co Ltd 反射防止膜
JP2012118536A (ja) * 2009-10-09 2012-06-21 Seiko Epson Corp 光学物品、光学物品の製造方法、電子機器
JP2011237472A (ja) * 2010-05-06 2011-11-24 Konica Minolta Opto Inc 撮像用レンズ
JP2022072420A (ja) * 2020-10-29 2022-05-17 キヤノン株式会社 光学素子、光学系、および、光学機器

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