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WO1997008357A1 - Revetement anti-reflechissant - Google Patents

Revetement anti-reflechissant Download PDF

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Publication number
WO1997008357A1
WO1997008357A1 PCT/US1996/014064 US9614064W WO9708357A1 WO 1997008357 A1 WO1997008357 A1 WO 1997008357A1 US 9614064 W US9614064 W US 9614064W WO 9708357 A1 WO9708357 A1 WO 9708357A1
Authority
WO
WIPO (PCT)
Prior art keywords
layer
index
refraction
refractive index
reflective coating
Prior art date
Application number
PCT/US1996/014064
Other languages
English (en)
Inventor
Eitan Zeira
Lee A. Batchelder
William A. Langille, Jr.
Original Assignee
Nashua Corporation
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 Nashua Corporation filed Critical Nashua Corporation
Publication of WO1997008357A1 publication Critical patent/WO1997008357A1/fr

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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
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G02B1/115—Multilayers
    • 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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides

Definitions

  • This invention relates to a three layer anti-reflective coating applied to optical lenses and other transparent substrates. More particularly, the invention relates to an anti-reflective coating which uses alloy targets specifically fabricated to produce coating layers having a desired index of refraction.
  • the layers of the anti-reflective coating generally comprise oxides of various elements deposited on the surface of a substrate by known techniques.
  • the deposition techniques can include physical vapor deposition techniques such as ablation, evaporation, and reactive and non-reactive sputtering.
  • U.S. Pat. No. 5,372,874 discloses the use of metal oxides in a three layer system
  • U.S. Pat. Nos. 5,216,542 and 5,279,722 disclose the use of oxides of metal alloys such as nickel-chromium and tin- ytterbium in four, five, and six layer anti-reflective coating systems.
  • the present invention concerns the development of a more efficient three layer anti-reflective coating.
  • a perfectly anti-reflecting three layer coating can be applied to an optical element such that the thicknesses of the first, second and third layers respectively satisfy the relationship
  • Equation 2 Equation 2
  • n 1; n 2 , and n 3 are the refractive indices of the respective layers, and no is the refractive index of air.
  • Such solutions include substituting two or more layers for one of the three layers in the coating to approximate the desired refractive indices.
  • indices of refraction that do not exist in available materials are simulated by combining two or more separate layers of materials such that the average of their indices approximates a desired index of refraction.
  • a further object of this invention is to provide for simplified manufacturing of optical lenses having an anti ⁇ reflective coating.
  • the present invention provides a three-layer anti ⁇ reflective coating for an optical lens.
  • the anti-reflective coating also can be used on camera or telescope lenses, automobile or building windows, television viewing surfaces, or other optically functional structures.
  • Each coating layer is made of a combination of materials designed to provide the coating with a desired index of refraction.
  • the invention combines two or more materials to form an alloy whose oxide deposit has anti-reflective properties not found in naturally occurring elements. For example, the invention permits the combination of two or more metals to form an alloy.
  • the oxide of the alloy approximates an index of refraction that does not exist in known elements.
  • the invention relates to an anti-reflective coating which includes a three layer stack deposited onto a substrate. Each layer is designed to have a specific index of refraction that approximates the relation of Equation (2) :
  • n 1 n 3 /n 2 ⁇ ( ⁇ n 0 )
  • n l f n 2 , and n 3 respectively, represent the refractive indices of the first, second, and third layers
  • n s represents the refractive index of the substrate
  • no is the refractive index of air.
  • the first and second layers are formed by reactively sputtering metal alloys in the presence of oxygen to obtain oxide deposits having a predetermined index of refraction.
  • the oxide deposits may be applied to the substrate by physical vapor deposition methods.
  • the third layer may be formed by reactive sputtering or by other methods. Any one of the three layers may be preselected, such that the other two layers are chosen based on the preselected layer.
  • the process of making the three stack (layer) anti ⁇ reflective coating includes selecting a substrate having a determinable index of refraction (n s ) .
  • a first coating layer is deposited on the substrate. If the third layer is the preselected layer, then the first coating layer, comprising an oxide deposit formed by reactively sputtering a metal alloy, is specifically designed to provide the oxide with a refractive index which approximates the relationship
  • n s is the refractive index of the substrate and n 3 represents the refractive index of a third coating layer.
  • a second coating layer is deposited onto the first layer using physical vapor deposition techniques.
  • the second layer can be reactively sputtered onto the first coating layer using a specially designed metal alloy target.
  • n 3 represents the refractive index of the third layer.
  • a third coating layer is deposited on the second layer by physical vapor deposition techniques.
  • the third layer in this example has a known index of refraction (n 3 ) , and can comprise boron-doped silicon dioxide reactively sputtered onto the second layer.
  • another three layer stack may be deposited on the opposite interface of the substrate to eliminate reflection from that interface also.
  • Figure 1 is a cross-sectional view of a three layer coating formed in accordance with the teachings of this invention and applied to a substrate.
  • Figures 2 (a-b) are X-ray photoelectron spectroscopy (XPS) scans of titanium reactively sputtered with oxygen from a pure titanium target, and titanium reactively sputtered with oxygen from an alloy target comprising titanium and aluminum.
  • XPS X-ray photoelectron spectroscopy
  • Figures 3 (a-b) are XPS scans for aluminum reactively sputtered with oxygen from a pure aluminum target, and aluminum reactively sputtered with oxygen from an alloy target comprising aluminum and titanium.
  • Figures 4(a-c) are XPS scans of oxygen peaks from reactively sputtered layers of pure titanium, pure aluminum, and an alloy target comprising titanium and aluminum.
  • Figures 5(a-c) are XPS scans of carbon contaminants that exist in sputtered deposits of aluminum oxide (A1 2 0 3 ) , titanium dioxide (Ti0 2 ) , and an oxide sputtered from an alloy of titanium mixed with aluminum.
  • This invention relates to a process of forming and applying an anti-reflection coating to transparent or nontransparent substrates, and the formation of alloys for use in the coating system.
  • the substrate can include an optical, camera, or telescope lens; automobile or building windows; television viewing surfaces; or other optically similar structures. To reduce the reflective properties of the substrate, it is coated with an anti-reflective coating having a precise index of refraction.
  • the coating includes three layers.
  • the first coating layer is deposited directly on the surface of the substrate.
  • the second layer is deposited on the first layer, and the third layer is deposited on the second layer.
  • the first and second layers preferably are formed by separately depositing oxides of specially designed metal alloys on the substrate.
  • the alloys are custom designed such that their oxides provide an index of refraction which does not exist in naturally occurring elements.
  • the third layer preferably is formed of a material having a known index of refraction, any one of the three layers may be preselected such that the other two layers are chosen based on the preselected layer.
  • the third layer can have a low index of refraction and hardness and corrosion resistant properties.
  • the layers can be arranged in any order, and are not intended to be limited to the above description.
  • another three layer stack of the invention may be deposited on the opposite interface of the substrate to eliminate reflection from that interface.
  • the layers of the anti-reflective coating can be applied to the substrate using commonly known physical vapor deposition techniques such as ablation, evaporation, reactive and non- reactive sputtering, or other similar methods.
  • any index of refraction between the lowest and highest naturally available elements can be achieved by fabricating a metal alloy target.
  • the metal alloy target is designed to produce an oxide deposit having an index of refraction that is the resultant contribution of the refractive index of each element forming the alloy.
  • any combination of metals that produce a clear oxide, fluoride, or nitride can be used.
  • an alloy is produced from materials with higher and lower indices than the desired resultant index.
  • the resultant index is not a straight average of the two numbers, and before selecting an alloy, the sputtering rate of each element in the alloy target and of the oxide formed from the elements must be taken into consideration.
  • Figure 1 is a cross-sectional view of an embodiment of a three layer coating 10 applied to a substrate 12 in accordance with this invention.
  • the substrate 12 is an optical lens having an index of refraction (n s ) of 1.5.
  • the substrate 12 need not be limited to an optical lens, and may include any substrate onto which an anti-reflective coating is applied, such as glass, polycarbonate, or other materials.
  • the substrate 12 includes a front side 14 that faces an observer having a line of sight through the substrate 12 as shown.
  • An anti-reflective coating 10 is deposited on the front side 14 of the substrate 12.
  • the anti-reflective coating 10 includes three layers: a first layer 16 deposited directly onto the front surface 14 of the substrate 12; a second layer 18 formed directly on the first layer 16; and a third layer 20 formed on the second layer 18.
  • the index of refraction of each layer 16, 18, and 20 is determined by Equations (3) and (4) such that the indices of refraction approximate the relationship of Equation (2) .
  • Equation (2) if the material forming the third layer 20 is preselected, the index of refraction (n 3 ) of the third layer 20 is established as a known value. Consequently, the index of refraction of the first and second layers 16 and 18 is fixed by n 3 and n s , where n s is known.
  • the third layer 20 is boron- doped silicon dioxide (Si0 ) , which has an index of refraction, n 3 , of 1.502 measured at 550 nm.
  • the index of refraction, n 2/ of the second layer 18 is therefore determined using Equation (4) such that
  • the refractive index (ni) of the first layer 20 is established using Equation (3) :
  • the layers 16 and 18 may be chosen to form the layers 16 and 18 such that the resultant oxides deposited as layers 16 and 18 in a preferred embodiment provide indices of refraction of 1.840 and 2.256, respectively.
  • the first layer 16 is formed from an aluminum-zinc alloy, 94.35% aluminum and 5.65% zinc, reactively sputtered in the presence of oxygen to produce an oxide deposit having a refractive index of 1.840.
  • the second layer 18 is formed from a titanium-aluminum alloy, 98.27% titanium and 1.73% aluminum, reactively sputtered in the presence of oxygen to provide an oxide deposit with an index of refraction of 2.256.
  • the preferred method of depositing the coating 10 on the substrate 12 is reactive sputtering.
  • Sputtering is performed with a magnetron in a reactive gas environment composed of a discharge gas comprising argon (Ar) and a reactive gas comprising oxygen.
  • the argon gas is selectively fed into a sputtering gun to reduce oxidation of the target material.
  • the oxygen gas is fed directly into the sputtering chamber. Sputtering the base or target material in the reactive oxygen gas creates an oxide of the target material on the surface of a substrate placed in the sputtering chamber.
  • the first layer 16 is sputtered onto the substrate 12 using a target comprising an alloy of aluminum and titanium having the composition previously described.
  • the second layer 18 is reactively sputtered using a target alloy comprising titanium and zirconium as described above.
  • the third layer 20 is reactively sputtered onto the second layer 18 using a boron-doped silicon target.
  • the first, second, and third layers 16, 18, and 20 have an optical thickness (t 0 ) of ⁇ /4, ⁇ /2, and ⁇ /4 respectively, where ⁇ is approximately 550 nm.
  • the physical thickness of the first, second, and third layers 16, 18, and 20 is determined by the relationship
  • t 0 is the optical thickness and "n" represents the refractive index of the layer. Since the refractive index is a predetermined constant, its value is not affected by small variations in either the physical or optical thicknesses.
  • XPS X-ray photoelectron spectroscopy
  • XPS scans were performed on deposits of an aluminum- itanium alloy, Al 57 Ti 43 , a pure aluminum target, and a pure titanium target, all reactively sputtered in the presence of oxygen.
  • the XPS scans of the reactively sputtered aluminum- titanium alloy includes peaks which do not belong to either of the oxides of its constituent metals or the pure elements forming the alloy. These peaks indicate that the oxide of the sputtered alloy contained compounds other than aluminum oxide (A1 2 0 3 ) and titanium oxide (Ti0 2 ) .
  • Figure 2a is an XPS scan of the titanium peak from titanium oxide.
  • the binding energy of the titanium peak is shown as a single peak at 458.35 eV.
  • the published binding energy for titanium in Ti0 2 is 458.8 eV.
  • the difference in the binding energies is believed to be due to non-stoichiometry in the deposited film.
  • Figure 2b is an XPS scan of the titanium peak from the aluminum-titanium oxide sputtering. This scan shows the titanium element as having peaks at 458.4 and 458.0 eV. The peak at 458.4 eV is consistent with the binding energy of titanium oxide, but the peak at 458.0 eV is not a known binding energy for titanium or titanium oxide. The closest reported binding energy is 458.3 eV, which belongs to the metal titanates group (i.e., BaTi0 3 , PbTi0 3 , etc.). This extra peak at 458.0 eV is presumably due to the compounding of the titanium with aluminum and oxygen.
  • the metal titanates group i.e., BaTi0 3 , PbTi0 3 , etc.
  • Figure 3a is an XPS scan of the aluminum peak from the aluminum oxide sputtering.
  • the XPS scan shows two peaks, one at 74.0 eV and the other at 73.75 eV. This scan is within the range of published data which reports the binding energy of aluminum in aluminum oxide at about 74.1 eV ⁇ 0.3 eV.
  • Figure 3b is an XPS of the aluminum peak from the aluminum titanium oxide sputtering. This scan shows a peak at 73.7 eV and an inflection at 73.0 eV. The shift in the binding energy value of the aluminum in the aluminum-titanium oxide deposit is presumably due to the presence of an additional compound other than pure aluminum oxide in the deposit.
  • Figures 4(a-c) are XPS scans of the respective oxygen peaks from pure titanium, pure aluminum, and the alloy target deposits.
  • Figure 4a shows a scan of the oxygen peak from the titanium oxide (Ti0 2 ) sputtering. The scan shows a peak at approximately 529.4 eV, a value which is consistent with published data.
  • Figure 4b is an XPS scan of the oxygen peak from the aluminum oxide (A1 2 0 3 ) sputtering. This scan shows peaks at 536.85 eV, 530.45 eV and 530.25 eV. Again, the measured binding energies are consistent with published data.
  • Figure 4c shows an XPS scan of oxygen from the aluminum titanium oxide sputtering. This scan shows a number of peaks and inflections. For example, the scan shows peaks at 529.65, 530.5, 530.05 and 531.05 eV, and smaller inflections at 528.95, 529.3 and 531.4 eV.
  • the peaks and inflections shown in the sputtered aluminum titanium oxide are not consistent with known data for oxygen in aluminum oxide or titanium oxide. This information suggests the presence of other compounds.
  • each of the XPS scans were set-up to scan the compositions under analysis for contaminants.
  • Figures 5(a- c) are scans of the carbon contaminants that invariably exist on all surfaces. This scan was used as a marker to show that the XPS scans of the sputtered materials were not shifted in any way by the charging of the samples. Normal hydrocarbons have their carbon peak at 284.8 eV. It is clear from Figures 2-4 that the scans were not shifted.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
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Abstract

Revêtement anti-réfléchissant en trois couches dont chacune est une combinaison de matières conçue pour conférer à ce revêtement un indice de réfraction déterminé. Ce revêtement fait appel à deux matières ou plus pour constituer un alliage dont le dépôt d'oxyde présente des caractéristiques anti-réfléchissantes qui ne se rencontrent pas dans ces éléments à l'état natif. Chaque couche est conçue pour présenter un indice spécifique de réfraction correspondant sensiblement à la relation n1n3/n2 = X(nsn0), dans laquelle n1, n2 et n3 correspondent respectivement aux indices de réfraction des première, deuxième et troisième couches. Dans le présent cas, ns représente l'indice de réfraction du substrat et n0 représente l'indice de réfraction de l'air. Les première et deuxième couches sont réalisées par diffusion par réaction d'alliages métalliques en présence d'oxygène pour obtenir des dépôts d'oxyde présentant un indice de réfraction prédéterminé. Les dépôts d'oxyde peuvent être appliqués sur le substrat par déposition en phase vapeur.
PCT/US1996/014064 1995-08-30 1996-08-27 Revetement anti-reflechissant WO1997008357A1 (fr)

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US52096695A 1995-08-30 1995-08-30
US08/520,966 1995-08-30

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WO1997008357A1 true WO1997008357A1 (fr) 1997-03-06

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1020738A1 (fr) * 1999-01-14 2000-07-19 Sumitomo Chemical Company, Limited Revêtement antiréfléchissant à trois couches contenant une première couche d' une résine liante avec des particules ultrafines
WO2001057579A3 (fr) * 2000-02-02 2002-02-21 3M Innovative Properties Co Revetement anti-reflet a trois couches pour un ecran tactile
US6436541B1 (en) * 1998-04-07 2002-08-20 Ppg Industries Ohio, Inc. Conductive antireflective coatings and methods of producing same
WO2004026782A1 (fr) 2002-09-14 2004-04-01 Schott Ag Systemes de couches contenant une couche d'oxyde de titane-aluminium
WO2004067791A3 (fr) * 2003-01-28 2004-11-25 Philips Intellectual Property Aluminium-oxyde de titane transparent et/ou oxyde d'aluminium recouvert d'une structure rutile
WO2004087985A3 (fr) * 2003-03-28 2005-01-20 Ppg Ind Ohio Inc Substrats recouverts de melanges de materiaux en titane et en aluminium, procedes de fabrication desdits substrats, et cibles cathodiques de metaux titane et aluminium
EP1074907A4 (fr) * 1998-04-24 2005-11-16 Nissha Printing Ecran tactile
US11685688B2 (en) 2018-10-22 2023-06-27 Mimsi Materials Ab Glazing and method of its production

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1005867A (fr) * 1947-10-10 1952-04-16 Physikalisches Untersuchungsla Procédé de production d'enduits ou revêtements réducteurs de la réflexion
FR2293719A1 (fr) * 1974-12-05 1976-07-02 Leybold Heraeus Gmbh & Co Kg Procede de preparation de systemes multicouches permettant d'attenuer les reflets, par un effet d'interferences, et les elements optiques prepares par ce procede
DE3434583A1 (de) * 1983-09-20 1985-04-11 Olympus Optical Co., Ltd., Tokio/Tokyo Reflexvermindernde beschichtung fuer ein optisches bauteil und verfahren zu ihrer ausbildung
WO1993004993A1 (fr) * 1991-09-03 1993-03-18 Viratec Thin Films, Inc. Revetement antireflet electroconducteur attenuant la lumiere

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1005867A (fr) * 1947-10-10 1952-04-16 Physikalisches Untersuchungsla Procédé de production d'enduits ou revêtements réducteurs de la réflexion
FR2293719A1 (fr) * 1974-12-05 1976-07-02 Leybold Heraeus Gmbh & Co Kg Procede de preparation de systemes multicouches permettant d'attenuer les reflets, par un effet d'interferences, et les elements optiques prepares par ce procede
DE3434583A1 (de) * 1983-09-20 1985-04-11 Olympus Optical Co., Ltd., Tokio/Tokyo Reflexvermindernde beschichtung fuer ein optisches bauteil und verfahren zu ihrer ausbildung
WO1993004993A1 (fr) * 1991-09-03 1993-03-18 Viratec Thin Films, Inc. Revetement antireflet electroconducteur attenuant la lumiere

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6436541B1 (en) * 1998-04-07 2002-08-20 Ppg Industries Ohio, Inc. Conductive antireflective coatings and methods of producing same
EP1074907A4 (fr) * 1998-04-24 2005-11-16 Nissha Printing Ecran tactile
EP1020738A1 (fr) * 1999-01-14 2000-07-19 Sumitomo Chemical Company, Limited Revêtement antiréfléchissant à trois couches contenant une première couche d' une résine liante avec des particules ultrafines
WO2001057579A3 (fr) * 2000-02-02 2002-02-21 3M Innovative Properties Co Revetement anti-reflet a trois couches pour un ecran tactile
WO2004026782A1 (fr) 2002-09-14 2004-04-01 Schott Ag Systemes de couches contenant une couche d'oxyde de titane-aluminium
CN1323045C (zh) * 2002-09-14 2007-06-27 肖特股份公司 层系统
US7713638B2 (en) 2002-09-14 2010-05-11 Schott Ag Layer system
WO2004067791A3 (fr) * 2003-01-28 2004-11-25 Philips Intellectual Property Aluminium-oxyde de titane transparent et/ou oxyde d'aluminium recouvert d'une structure rutile
US7550208B2 (en) 2003-01-28 2009-06-23 Koninklijke Philips Electronics N.V. Transparent titanium oxide-aluminum and/or aluminum oxide coating with rutile structure
WO2004087985A3 (fr) * 2003-03-28 2005-01-20 Ppg Ind Ohio Inc Substrats recouverts de melanges de materiaux en titane et en aluminium, procedes de fabrication desdits substrats, et cibles cathodiques de metaux titane et aluminium
AU2004225545B2 (en) * 2003-03-28 2008-08-14 Ppg Industries Ohio, Inc. Substrates coated with mixtures of titanium and aluminum materials, methods for making the substrates, and cathode targets of titanium and aluminum metal
US11685688B2 (en) 2018-10-22 2023-06-27 Mimsi Materials Ab Glazing and method of its production
US12006250B2 (en) 2018-10-22 2024-06-11 Mimsi Materials Ab Glazing and method of its production

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