WO2020016620A1 - Article optique à revêtement antireflet amélioré, et ses procédés de fabrication - Google Patents

Article optique à revêtement antireflet amélioré, et ses procédés de fabrication Download PDF

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Publication number
WO2020016620A1
WO2020016620A1 PCT/IB2018/000921 IB2018000921W WO2020016620A1 WO 2020016620 A1 WO2020016620 A1 WO 2020016620A1 IB 2018000921 W IB2018000921 W IB 2018000921W WO 2020016620 A1 WO2020016620 A1 WO 2020016620A1
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Prior art keywords
layer
equal
optical article
antireflective coating
optical
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PCT/IB2018/000921
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English (en)
Inventor
Delphine Passard
Christophe VALENTI
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Essilor International
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Priority to PCT/IB2018/000921 priority Critical patent/WO2020016620A1/fr
Publication of WO2020016620A1 publication Critical patent/WO2020016620A1/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
    • 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
    • C23C14/083—Oxides of refractory metals or yttrium
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/221—Ion beam deposition
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • G—PHYSICS
    • G02—OPTICS
    • G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
    • G02C7/00—Optical parts
    • G02C7/10—Filters, e.g. for facilitating adaptation of the eyes to the dark; Sunglasses

Definitions

  • the invention relates to an optical article, especially an ophthalmic lens, comprising an antireflective coating which strongly reduces reflection both in the visible region and in the UV- radiation range, while being able to develop no (or almost no) cosmetic defects over time, as well as to methods for making such an optical article.
  • a lens substrate such as an ophthalmic lens or lens blank
  • several coatings for imparting to the finished lens additional or improved optical or mechanical properties. These coatings are designated in general as functional coatings.
  • a lens substrate typically made of an organic glass material
  • an impact-resistant coating impact-resistant primer
  • an abrasion- and/or scratch- resistant coating hard coat
  • an anti-reflection coating and, optionally, an anti-fouling top coat.
  • Other coatings such as a polarized coating, a photochromic or a dyeing coating may also be applied onto one or both surfaces of the lens substrate.
  • An anti-reflection coating is defined as a coating, which improves the anti-reflective properties of an optical article when deposited at its surface. It reduces reflection of light at the interface article-air on a relatively wide band of the visible spectrum.
  • Anti-reflection coatings are well known and classically comprise a single-layer or multilayer stack of dielectric materials such as Si0 2 , SiO, Al 2 0 3 , MgF 2 , LiF, Si 3 N 4 , Ti0 2 , Zr0 2 , Nb 2 0 5 , Y 2 0 3 , Hf0 2 , Sc 2 0 3 , Ta 2 0 5 , Pr 2 0 3 , and mixtures thereof. They are generally inorganic by nature.
  • anti-reflection coatings preferably are multi-layer coatings comprising alternatively high refractive index layers (HI) and low refractive index layers (LI).
  • deposition of the anti-reflection coating (optionally comprising a sub-layer) has to be performed through moderate temperature processes so as to avoid deterioration of the substrate. Taking such precaution is useless in the case of mineral glass substrates.
  • the consequence of a lower temperature treatment is, generally, in the case of organic glass substrates, a lower durability of the AR coating.
  • organic glass substrates (either coated or uncoated) have a higher thermal expansion coefficient than inorganic materials constituting layers or sub-layers of the anti reflection coating. The consequence is that they lead to articles which may develop high stress. Such stress may generate naked eye visible cracks or exfoliation in the AR coating upon increasing temperature.
  • This phenomenon is particularly noticeable when the organic substrate is based on diethylene glycol bis(allyl carbonate) monomers, episulfide monomers (materials having a refractive index n > 1.70), or polythiourethane (materials having a refractive index n equal to or higher than 1.60).
  • the eyeglass undergoes mechanical deformations that may produce cracks in mineral interference coatings, in particular when the operation is not carried out with care.
  • thermal stresses heating of the frame
  • the anti-reflection coating may mar the field of view of the wearer and prevent the eyeglass from being sold.
  • scratches may appear. In mineral anti-reflection coatings, certain scratches lead to cracking, making the scratches more visible because of scattering of light.
  • a multilayer dielectric film such as an anti-reflection coating
  • Si0 2 /Al 2 0 3 mixtures instead of Si0 2 allows to decrease the stress in LI layers, and consequently the cracks appearance probability at the substrate surface.
  • the document US 2008/002260 describes an optical article having anti-reflection properties comprising a substrate having at least one main face coated with a multi-layer antireflection coating comprising a stack of at least one high refractive index layer and at least one low refractive index layer, wherein:
  • each low refractive index layer has a refractive index of 1.55 or less;
  • each high refractive index layer has a refractive index higher than 1.55 and does not comprise niobium pentoxide (Nb 2 0 5 );
  • said coated main face of the optical article has a mean luminous reflection factor Rv ⁇ 1 %;
  • the anti-reflection coating does not comprise a sub-layer comprising niobium (Nb), or (b) the anti-reflection coating comprises: at least one low refractive index layer having a physical thickness >100 nm which is not the outermost layer of the anti-reflection coating; and at least one high refractive index layer and at least one low refractive index layer, which are located above the low refractive index layer having a physical thickness 3100 nm and not being the outermost layer of the anti-reflection coating which is the furthest from the substrate, and the ratio R
  • the sum of the physical thicknesse s of the low refractive index layers of the anti - reflection coating sum of the physical thicknesse s of the high refractive index layers of the anti - reflection coating is higher than 2.1 , with the proviso that the layers of the anti-reflection coating taken into account for the calculation of said ratio RT are only the layers located above the low refractive index layer having a physical thickness 3100 nm and not being the outermost layer of the anti reflection coating which is the furthest from the substrate.
  • the particular multilayered interferential coating such as performed in this document improves the critical temperature of cracks appearance up to 98 to 1 10°C. However, even if this optical article is satisfactory, there is still a need to improve its robustness and its aesthetic appearance.
  • the aim of the present invention is thus to provide a new optical article, that avoids all or some of the aforementioned drawbacks.
  • Another aim of this invention is to provide a process of manufacturing the above defined article, which could be easily integrated into the classical manufacturing chain.
  • an optical article comprising a transparent substrate with a front main face and a rear main face, at least one of said main faces being coated with at least: a sub-layer with a main thick layer that is deposited in a vacuum chamber under a pre-determined pressure and a multilayered antireflective coating comprising at least one HI layer having a refractive index higher than or equal 1 .55, and at least one LI layer having a refractive index lower than 1.55, said multilayered antireflective coating - has a mean light reflection factor in the visible region R v , as defined in the ISO 13666:1998 Standard and measured in accordance with the ISO 8980-4, that is lower than or equal to 1.5 % for at least an angle of incidence lower than 35° and - a mean reflection factor Ruv between 280 nm and 380 nm, weighted by the function W(A) defined in the ISO 13666:1998 standard, that is equal to or lower than 5%, for an angle
  • the at least one HI layer comprises at least one material that is tantalum pentoxide (Ta 2 0 5 ), and
  • said multilayered antireflective coating comprises no cosmetic defects evaluated visually in transmission.
  • the optical article especially the ophthalmic lens according to the invention, comprises a transparent organic or mineral glass substrate coated with a multilayered antireflective coating possessing very good antireflective performances in the visible region and in the UV range, while guarantying both good aesthetics appearance (no or almost no cosmetic defects over time) and high robustness.
  • the optical article according to the invention has improved resistance to heat and temperature variations, i.e., a high critical temperature even after a long time, and is therefore an alternative to already known thermally resistant antireflective coated optical articles.
  • Such multilayered antireflective (AR) coating resistant to cracking would be particularly interesting if applied on the first face of a semi-finished lens, generally the front (convex) face, because it would then be possible to deposit by spin coating an AR coating on the second face of the lens (generally on the back side) followed by curing at elevated temperature without altering the AR on the front face.
  • AR antireflective
  • the optical article according to the invention has generally a critical temperature equal to or higher than 80°C, preferably higher than or equal to 90°C, without compromising the economic and/or industrial feasibility of its manufacture and without compromising their robustness properties and their aesthetic appearance.
  • the optical article according to the invention offers the advantage of having high critical temperature, without decreasing the optical and mechanical performances of said optical article, such as color and anti-reflection performances, cleanability, adhesion of the layers to the substrate, abrasion resistance and corrosion resistance.
  • the optical article has a good resistance to dipping in hot water followed by mechanical surface solicitations.
  • a multilayered antireflective coating comprising at least one HI layer having a refractive index higher than or equal 1.55, and at least one LI layer having a refractive index lower than 1.55, the at least one HI layer comprising at least one material that is tantalum pentoxide (Ta 2 0 5 ), that is performed by ion-beam assisted deposition (IAD) in which a predetermined anode current l A that is ranging from 1 to 4 A and a pre-determined anode voltage U A that is ranging from 80 to 200 V, are supplied, so as to form the stack S;
  • IAD ion-beam assisted deposition
  • the Applicant has discovered that specific experimental conditions during the deposition of the main thick layer of the sub-layer (such as the pressure) and during the deposition of the HI layer of the multilayered antireflective coating (such as the anode current l A or the anode voltage U A ), combined with the use of HI layer(s) made of tantalum pentoxide, enable to obtain in an easy manner an appropriate antireflective film coated onto a sublayer, and especially an appropriate antireflective coating comprising alternate HI and LI layers.
  • specific experimental conditions during the deposition of the main thick layer of the sub-layer such as the pressure
  • the HI layer of the multilayered antireflective coating such as the anode current l A or the anode voltage U A
  • the Applicant has found that from at least a specific mineral oxide that is tantalum pentoxide for forming at least one HI layer of the multilayered antireflective coating and from specific experimental conditions (pressure, anode current and anode voltage) and deposition processes (evaporation under vacuum with or without ion-beam assisted deposition), it is possible to form a multilayered antireflective coating having an improved critical temperature, a reduced weakness to crazing and/or cracking, while having excellent antireflective and robustness properties, while being easy to implement.
  • specific experimental conditions pressure, anode current and anode voltage
  • deposition processes evaporation under vacuum with or without ion-beam assisted deposition
  • the invention also relates to a method of optimizing the manufacture of an optical article comprising a transparent substrate with a front main face and a rear main face, at least one of said main faces being coated with at least a multilayered antireflective coating comprising at least one HI layer having a refractive index higher than or equal 1 .55, and at least one LI layer having a refractive index lower than 1.55, the at least one HI layer comprising at least one material that is tantalum pentoxide (Ta20 5 ),
  • said method of optimizing comprising the following steps:
  • the deposition of the at least one HI layer is performed by ion beam assisted deposition (IAD) in which the pre-determined anode current l A and the pre-determined anode voltage U A are supplied, so as to form the stack S;
  • IAD ion beam assisted deposition
  • the Applicant has developed a method of optimizing the manufacture of an optical article, such as the one described above.
  • a method, or a step in a method that“comprises,”“has,”“contains,” or“includes” one or more steps or elements possesses those one or more steps or elements, but is not limited to possessing only those one or more steps or elements.
  • the coating on a substrate or deposited onto a substrate is in direct contact with this substrate.
  • the multilayered antireflective coating according to the invention may be formed on at least one of the main faces of a bare substrate, i.e. an uncoated substrate, or at least one of the main faces of the substrate already coated with one or more functional coatings, such as an anti-abrasion coating.
  • the rear (or the inner or Concave or CC) face of the substrate is intended to mean the face which, when using the article, is the nearest from the wearer’s eye. It is generally a concave face.
  • the front face of the substrate (or Convex or CX), is the face which, when using the article, is the most distant from the wearer’s eye. It is generally a convex face.
  • cosmetic appearance means that there is no, or almost no, cosmetic defects over time evaluated visually in transmission and is preferably measured under an arc lamp.
  • Tc critical temperature
  • transmittances/transmissions are measured at the center of the optical article for a thickness ranging from 0.7 to 2 mm, preferably from 0.8 to 1 .5 mm, at an angle of incidence ranging from 0° to 15°, preferably 0°.
  • the light transmitted refers to light arriving on the front main face of the optical article and that went through the lens.
  • the "luminous reflectance" noted R v is such as defined in the ISO 13666:1998 Standard, and measured in accordance with the ISO 8980-4, i.e. this is the weighted spectral reflection average over the whole visible spectrum between 380 and 780 nm.
  • R v is usually measured for an angle of incidence lower than 17°, typically of 15°, but can be evaluated for any angle of incidence.
  • R(A) represents the lens spectral reflection factor at a given wavelength
  • W(A) represents a weighting function equal to the product of the solar spectrum irradiance Es(A) and the efficiency relative spectral function S(A).
  • this factor may be measured at an angle of incidence that ranges from 30° to 45° on the rear face.
  • Figure 1 shows a graph obtained thanks to the Minilab software with the experiment conditions of example 1 with a pressure of 10 4 mBar (a) and 1.2.10 4 mBar (b).
  • the preferred substrates according to the invention are for instance the substrates obtained from MR6®, MR7®, MR8®, MR10®, MR174 ® resins and Trivex® product or polycarbonate.
  • a polycarbonate is intended to mean either homopolycarbonates or copolycarbonates and block copolycarbonates
  • This pretreatment is generally carried out under vacuum. It may be carried out through bombardment with energetic and/or reactive species, for example an ion beam (ion pre-cleaning or I PC) or an electron beam, a corona discharge treatment, a glow discharge treatment, a UV treatment or treatment in a vacuum plasma, generally an oxygen or argon plasma. It may also be carried out through an acidic or basic surface treatment and/or a treatment with solvents (water or organic solvent(s)). Several of these treatments may be combined. By virtue of these cleaning treatments, the cleanliness and the reactivity of the surface of the substrate are optimized.
  • the at least one HI layer comprises at least one material selected from the group consisting of tantalum pentoxide (Ta 2 0 5 ) and preferably is constituted of tantalum pentoxide (Ta 2 0 5 ), and
  • a layer of an antireflective coating is said to be a low refractive index layer (LI) when its refractive index is lower than 1.55, preferably lower than or equal to 1 .50, more preferably lower than or equal to 1.48.
  • Said LI layer preferably has a refractive index higher than 1.1.
  • the other HI layer (s) may be traditional high refractive index layer, that is well known in the art. It generally comprises one or more metal oxides such as, without limitation, zirconia (Zr0 2 ), titanium dioxide (Ti0 2 ), alumina (Al 2 0 3 ), tantalum pentoxide (Ta 2 0 5 ), neodymium oxide (Nd 2 0 5 ), praseodymium oxide (Pr 2 0 3 ), praseodymium titanate (PrTi0 3 ), lanthanum oxide (La 2 0 3 ), niobium oxide (Nb 2 0 5 ), yttrium oxide (Y 2 0 3 ).
  • Zr0 2 zirconia
  • Ti0 2 titanium dioxide
  • alumina Al 2 0 3
  • tantalum pentoxide Ta 2 0 5
  • neodymium oxide Nd 2 0 5
  • Pr 2 0 3 praseodymium oxide
  • the first HI layer is deposited in a vacuum chamber by ion beam assisted deposition (IAD) with a pre-determined anode current l A ranging from 1 to 4 A.
  • IAD ion beam assisted deposition
  • U A pre-determined anode voltage
  • a pre-determined anode current l A ranging from 1 to 4 A includes the followings values and any intervals between them: 1 ; 1.5 ; 2; 2.5 ; 3 ; 3.5 ; 4 and “a pre determined anode voltage U A ranging from 80 to 200 V” includes the followings values and any intervals between them: 80; 90; 100; 1 10; 120; 130; 140; 150; 160; 170; 180; 190; 200.
  • said pre-determined anode current l A ranges from 2 to 3 A;
  • LI layers are also well known and may comprise, without limitation, Si0 2 , MgF 2 , ZrF 4 , AIF 3 , and their combinations, preferably Si0 2 , which contributes to increase the thermal resistance of the antireflection coating.
  • the LI layers may further contain materials with a high refractive index, provided the refractive index of the resulting layer is lower than 1.55.
  • a sub-layer comprising at least a main thick layer or thick sub-layer (or adhesion layer) is intended to mean a relatively thick coating, used in order to improve the mechanical properties such as the abrasion resistance and/or the scratch resistance of said AR coating and/or so as to reinforce its adhesion to the substrate or to the underlying coating.
  • the sub-layer should have a thickness that is sufficient for promoting the abrasion resistance of the antireflective coating, but preferably not to such an extent that a light absorption could be caused, which, depending on the sub-layer nature, could significantly reduce the relative transmission factor t n .
  • Its thickness is generally lower than 300 nm, more preferably lower than 200 nm, and is generally higher than 90 nm, more preferably higher than 100 nm and may be ranging from 90 to 300 nm.
  • a sub-layer of the single-layer type will be preferably used.
  • These additional layers are preferably thin layers, which function aims at limiting the reflections at the sub-layer / underlying coating interface or sub-layer / substrate interface, as appropriate.
  • a multilayered sub-layer preferably comprises, in addition to the main thick layer, a layer with a high refractive index and with a thickness lower than or equal to 80 nm, more preferably lower than or equal to 50 nm and most preferably lower than or equal to 30 nm.
  • a layer with a high refractive index is directly contacting the substrate with a high refractive index or the underlying coating with a high refractive index, as appropriate.
  • this embodiment may be used even if the substrate (or the underlying coating) has a refractive index lower than 1.55.
  • the main thick layer of the sub-layer (either of the single-layered or multilayered type) is deposited under vacuum at a predetermined pressure that is preferably ranging from 0.4 10 4 mbar to 1 .5 10 4 mbar, preferably from 0.5 10 4 mbar to 1 .3 10 4 mbar.
  • the anti reflective coating does not comprise any layer with a thickness higher than or equal to 20 nm, preferably higher than 15 nm, based on tin oxide.
  • a plurality of indium oxide-based layers are present in the antireflective coating, their total thickness is preferably lower than 20 nm, more preferably lower than 15 nm.
  • an indium oxide-based layer is intended to mean a layer comprising at least 50% by weight of indium oxide relative to the layer total weight.
  • the total thickness of the antireflection coating is lower than 1 micrometer, more preferably lower than or equal to 800 nm and even more preferably lower than or equal to 500 nm.
  • the total thickness of the antireflection coating is typically higher than 100 nm, preferably higher than 150 nm.
  • the sub-layer has a physical thickness ranging from 75 nm to 250 nm, especially from 80 nm to 200 nm and typically from 100 to 180 nm and the multilayered antireflective coating comprises at least two HI layers and two LI layers and has especially, in the direction moving away from the substrate, the followings structure:
  • a first HI layer having a physical thickness ranging from 10 to 30 nm, preferably from 15 to 20nm and typically from 17 to 22 nm;
  • a first LI layer having a physical thickness ranging from 10 to 35 nm, preferably from 15 to 30 nm and typically from 16 to 25 nm;
  • a second HI layer having a physical thickness ranging from 80 to 105 nm, preferably from 85 to 100 nm and typically from 88 to 95 nm;
  • a second LI layer having a physical thickness ranging from 60 to 90 nm, preferably from 65 to 85 nm and typically from 70 to 78 nm.
  • the present invention provides hence an antireflective coating with an improved conception, comprising a stack made of thin layers, the thicknesses and materials of which have been selected so as to obtain satisfactory antireflective performances both in the visible region and eventually in the ultraviolet region, while having both improved heat resistance, esthetic appearance and robustness properties.
  • the deposition of the LI layer(s) of the multilayered AR coating and of the sub-layer are conducted by evaporation under vacuum.
  • the deposition of the HI layer(s) of the multilayered AR coating are conducted by evaporation under vacuum with ion gun assistance (IAD),
  • the multilayered antireflective coating of the invention has improved robustness properties and heat resistance properties.
  • the multilayered antireflective coating has an optical robustness corresponding to the standard deviation of hue “ah” as defined in the international colorimetric CIE L * a * b * (1976) for an angle of incidence (Q) of 15° that is lower than or equal to 12°, preferably lower than or equal to 10°, in particular lower than or equal to 8°.
  • a standard deviation of hue “ah” lower than or equal to 12 includes the followings values and any intervals between them: 0; 0.5 ; 1 ; 1.5 ; 2; 2.5 ; 3 ; 3.5 ; 4 ; 4.5 ; 5 ; 5.5 ; 6 ;6.5 ;7 ;7.5 ;8 ;8.5 ;9 ;9.5 ;10 ;10.5 ; 1 1 ; 11 .5 ; 12.
  • the standard deviation of hue“ah” corresponds to the formula below and is measured such as explained in the experimental part (standard deviation of 500 values of hue generated by the Mac Leod software) :
  • the optical article has a critical temperature Tc equal to or higher than 80°C.
  • a critical temperature Tc equal to or higher than 80°C. includes the followings values and any intervals among them: 80; 81 ; 82; 83; 84; 85; 86; 87; 88; 89; 90; 91 ; 92; 93; 94; 95; 96; 97; 98; 99; 100; 101 ; 102; 103; 104; 105; 106; 107; 108; 109; 1 10; 1 11 ; 1 12; 1 13; 114; 115; 116; 1 17; 1 18; 1 19; 120; 121 ; 122; 123; 124; 125; etc.
  • the optical article has a critical temperature equal to or higher than 81 °C, preferably equal to or higher than 85°C, more preferably equal to or higher than 90°C, especially equal to or higher than 93°C and typically equal to or higher than 100°C.
  • Tc is measured as explained in the experimental part below, for instance at one month after the preparation of the optical article.
  • an optical article preferably an ophthalmic lens according to the invention comprises a substrate that is successively coated on its rear face with an impact-resistant primer layer, an anti-abrasion and scratch-resistant layer, an anti-UV, antireflective coating according to the invention, and with a hydrophobic and/or oleophobic coating, or with a hydrophilic coating which provides antifog properties, or an antifog precursor coating.
  • the ophthalmic lens according to the invention is preferably an ophthalmic lens for spectacles (spectacle lens), or a blank for ophthalmic lenses.
  • the lens may be a polarized lens, a photochromic lens or a solar lens, which may be tinted or not, be corrective, or not.
  • the front face of the substrate of the optical article may be successively coated with an impact-resistant primer layer, an abrasion-resistant layer and/or a scratch-resistant layer, an antireflective coating which may be, or not, an anti-UV antireflective coating according to the invention, and with a hydrophobic and/or oleophobic coating.
  • the optical article according to the invention does not absorb in the visible or not much, which means, in the context of the present application, that its transmission factor in the visible range x v , also called relative transmission factor in the visible range, is higher than 90%, more preferably higher than 95%, even more preferably higher than 96% and most preferably higher than 97%.
  • the factor x v should be understood as defined by the international normalized definition (ISO 13666:1998 Standard) and is measured in accordance with the ISO 8980-3 Standard. It is defined in the wavelength range of from 380 to 780 nm.
  • the light absorption of the article coated according to the invention is lower than or equal to 1 %.
  • the invention also relates to a process for manufacturing an optical article, comprising at least the following steps:
  • a multilayered antireflective coating comprising at least one HI layer having a refractive index higher than or equal 1.55, and at least one LI layer having a refractive index lower than 1.55, the at least one HI layer comprising at least one material selected from the group consisting of tantalum pentoxide (Ta20 5 ), that is performed by ion beam assisted deposition (IAD) in which a pre-determined anode current l A that is ranging from 1 to 4 A and a pre-determined anode voltage U A that is ranging from 80 to 200 V, are supplied, so as to form the stack S;
  • IAD ion beam assisted deposition
  • the first HI layer of the multilayered AR coating made of at least Ta 2 0 5 or constituted of Ta 2 0 5 is deposited by ion-assisted deposition (IAD). More precisely, this HI layer is deposited by evaporation under vacuum assisted by bombarding the surface to be treated with ions. This deposition method enables indeed to increase the compression of this layer and therefore its refractive index.
  • the other HI layer(s) is (are) also deposited by IAD. IAD does not require any heating of the substrates, which is interesting for coating heat-sensitive substrates such as glass or plastic substrates.
  • the IAD operation may be performed by means of an ion gun (the Commonwealth of the type Mark II for example), where ions are particles composed of gas atoms from which one or more electron(s) is or are extracted. It does preferably consist in bombarding the surface to be treated with oxygen ions.
  • Other ionized gases may be used either combined with oxygen, or not, as for example argon, nitrogen, in particular a mixture of 0 2 and argo n according to a volume ratio ranging from 2:1 to 1 :2.
  • a pre-determined anode current l A ranging from 1 to 4 A includes the followings values and any intervals between them: 1 ; 1.5 ; 2; 2.5 ; 3 ; 3.5 ; 4 and “a pre determined anode voltage U A ranging from 80 to 200 V” includes the followings values and any intervals between them: 80; 90; 100; 1 10; 120; 130; 140; 150; 160; 170; 180; 190; 200.
  • said first HI layer of the multilayered AR coating is deposited in a vacuum chamber by ion beam assisted deposition (IAD) with a current density typically ranging from to 10 mA/cm 2 to 200 mA/cm 2 , preferably from 30 to 100 mA/cm 2 on the activated surface and typically under a residual pressure in the empty chamber which may vary from 6.1 O 5 mbar to 1 ,3 .10 4 mbar, preferably from 8.10 5 mbar to 1 ,3.10 4 mbar.
  • IAD ion beam assisted deposition
  • all the HI layers of said multilayered antireflective coating are deposited in a vacuum chamber by ion beam assisted deposition (IAD) with the pre-determined anode current l A and the pre-determined anode voltage U A.
  • IAD ion beam assisted deposition
  • the experimental conditions are as follows:
  • said pre-determined main thick layer of sub-layer pressure ranges from 0.4 c 10 4 mbar to 1 .5 x 10 4 mbar, preferably from 0.5 c 10 4 mbar to 1.3 c 10 4 mbar;
  • said pre-determined anode current l A ranges from 2 to 3 A;
  • Such a process avoids heating the substrate, which is particularly interesting in the case of organic glasses.
  • Vacuum methods for the deposition of the different layers of the AR stack, especially the LI layers, and the sublayer include: i) evaporation; ii) spraying with an ion beam; iii) cathode sputtering; iv) plasma assisted chemical vapor deposition. These techniques are described in detail in "Thin Film Processes” and “Thin Film Processes II,” Vossen & Kern, Ed., Academic Press, 1978 and 1991 respectively. The particularly recommended technique is vacuum evaporation.
  • the optional electrically conductive layer which generally is a HI layer of the antireflection stack, may be deposited according to any appropriate method, for example by vacuum evaporation, preferably under ion assistance (IAD: Ion Assisted Deposition), or by a sputtering technique.
  • IAD Ion Assisted Deposition
  • the IAD method comprises packing said layer with heavy ions while it is being formed, so as to increase its density, adhesion and refractive index. It requires an ion plasma in a gas atmosphere, such as argon and/or oxygen.
  • I PC Ion pre-cleaning
  • the optical article to be coated with the AR coating of the present invention may be a finished lens or a semi-finished lens.
  • One of its main faces may have previously been coated with an appropriate coating stack (anti-reflection, hard coat, primer coating, impact resistant coating, etc.).
  • the process of the invention presents many advantages. For example, its implementation requires no modification of the original tweaking of the traditional process for depositing an AR coating, no modification of the deposition apparatus, no various additional equipments.
  • the invention also relates to a method of optimizing the manufacture of an optical article comprising a transparent substrate with a front main face and a rear main face, at least one of said main faces being coated with at least a multilayered anti reflective coating comprising at least one HI layer having a refractive index higher than or equal 1 .55, and at least one LI layer having a refractive index lower than 1 .55,
  • said method of optimizing comprising the following steps:
  • the multilayered antireflective coating the deposition of which is performed by ion beam assisted deposition (IAD) in which the pre-determined anode current l A and the pre-determined anode voltage U A are supplied, so as to form the stack S;
  • IAD ion beam assisted deposition
  • said optical performances are further selected from: transparency, abrasion properties thanks to the ISTM Bayer Test, optical losses, cosmetic defects, adhesion thanks to the nx10 blow test.
  • the transparency T v (%) as defined by the international normalized standard ISO 8980-3 measured at a wavelength ranging from 380 to 780 nm is higher than or equal to 90 %, preferably 95 %;
  • the ISTM Bayer value is higher than or equal to 9, preferably 10 according to ASTM Standard F735-81 ;
  • n_10 blows value is higher than 12;
  • the cosmetic defects evaluated visually in transmission preferably under an arc lamp.
  • step (c) is implemented through a computer means, such as a computer with the analyzing program using the Minitab software from Minitab Inc.
  • Fig.1 shows the ideal process window for different parameters, such as Tc at one week, Tc at one month, cosmetic defect, and ISTM Bayer value for a predetermined pressure (1 x 10-4 mBar; Fig.1 (a) or 1.2x 10-4 mBar; Fig.1 (b)) and as function of different predetermined values of anode current l A (A) and of anode voltage U A (V).
  • Tc time at one week
  • Tc at one month a predetermined pressure
  • Fig.1 (b) as function of different predetermined values of anode current l A (A) and of anode voltage U A (V).
  • Tc, ISTM Bayer value and cosmetic defect are entered in the software.
  • optical articles used in the examples were semi-finished MR7 ® round lenses surfaced to a power of (-4.00) diopters and a diameter of 75 mm, coated with a hard coat layer of refractive index 1 ,6 (Elis Mithril 1 .6 hardcoat) and coated on its front face with an sub-layer made of Si0 2 .
  • the layers of the antireflective coating were deposited without heating the substrates by evaporation under vacuum (evaporation source: electron gun) in a Syrus 3 AR coater.
  • the deposition frame is a Leybold 1 104 machine fitted with an electron gun (ESV14 (8kV)) for evaporating oxides, and provided with an ion gun (Commonwealth Mark II) for the deposition of all the HI Layer of the multilayered AR coating by IAD and the electrically conductive layer made of Sn0 2 and for the preliminary phase to prepare the surface of the substrate (I PC).
  • ESV14 8kV
  • ion gun Commonwealth Mark II
  • the ionized gas was Argon for I PC and 0 2 for IAD for both Sn0 2 & Ta 2 0 5 .
  • the thickness of the layers was controlled by means of a quartz microbalance.
  • the spectral measurements were effected on a variable incidence-spectrophotometer Perkin-Elmer Lambda 850 with an URA accessory (Universal Reflectance Accessory).
  • the method for making optical articles comprises the step of:
  • the Bayer abrasion test is a standard test used to determine the abrasion resistance of curved/lens surfaces. Determination of the Bayer value was performed in accordance with the standards ASTM F 735-94 (Standard Test Method for Abrasion Resistance of Transparent Plastics and Coatings Using Oscillating Sand Method) and ISO CD 15258 (Bayer Abrasion test for ophthalmic lenses), with a higher Bayer value meaning a higher abrasion resistance. Per this test, a coated lens is mounted and held tightly using clamps on the bottom of a tray next to an uncoated CR-39 ® reference lens of similar curvature, diameter, thickness and diopter.
  • abrasive powder (sand) of specified grain size is poured evenly over the lenses and the tray, and the tray is oscillated at a period of 100 cycles/minutes for two minutes. Oscillation is achieved using a motor that is connected to an oscillating plate through a revolving wheel.
  • the coated lens and the reference are then removed and the haze and transmittance of both the reference and coated sample are measured with a Haze Guard Plus meter, in accordance with ASTM D1003-00, before and after the test has been performed.
  • the results are expressed as a calculated ratio of the standard CR-39 ® test lens to the coated lens (haze gain caused by the abrading sand).
  • the Bayer value is set to 1 for the reference CR-39 ® lens. Only fresh sand is used for each measurement.
  • the heat resistance test is performed one month after preparation of the lenses.
  • the prepared lenses were put into an oven preheated to a selected temperature, and were left there for 1 hour. They were removed from the oven and visually evaluated by reflection in terms of the presence of cracks under a desk lamp.
  • This experiment was performed at different temperatures, starting from 50 °C and raising the heating temperature in 10°C increments. The temperature was measured, at which the lenses could not withstand the heat treatment and were cracked after 1 hour. This temperature is given as the critical temperature in the tables below. When several lenses have been tested, the critical temperature mentioned is the average value.
  • the test called R-17 used for the inspection is in fact the transmission test described in detail in W02006136757 (Protocole of measurement of optical defects) which is incorporated herein by reference.
  • Inspection with an arc lamp is carried out by using a BT XL 75/ LIS//Lamp made by Bulbtronics Inc.
  • nx10 blow test A qualitative test was carried out using the procedure known as the "nx10 blow test.” This procedure makes it possible to evaluate adhesion of a film deposited on a substrate, such as an ophthalmic lens. The test was performed such as described in international patent application WO 99/49097.
  • This software is able to generate graphs for a predetermined pressure: at 10 4 mbar (see Fig.1 (a)) and at 1.2 .10 4 mbar (see Fig.1 (b)).
  • These graphs Fig.1 (a) and Fig.1 (b) show the ideal window process of the anode current“l A ” and the anode voltage“U A ” for a predetermined pressure.
  • the optimized pressure during the deposition of the sub-layer is 1.2.10 4 mbar and the optimized anode current“l A ” is 3A and the anode voltage“U A ” is 130V during the deposition of the HI layers and the electrically conductive layer.
  • the tested lens has the following characteristics (table 3):
  • Lens 1 has been reproduced by varying another parameter such as the ionized gas during the IAD deposition (introduction of 0 2 ) for two substrates (Orma® obtained through (co)polymerization of the diethyleneglycol bis allyl carbonate) and MR7®.
  • another parameter such as the ionized gas during the IAD deposition (introduction of 0 2 ) for two substrates (Orma® obtained through (co)polymerization of the diethyleneglycol bis allyl carbonate) and MR7®.
  • the tested structure is as follow (see table 4):
  • This table 5 shows that the presence/absence of the gas (0 2 ) during the deposition of the HI layers has no influence on the optical characteristics of the obtained lens (good optical performances).
  • This table 6 shows that these two substrates enable to obtain good optical characteristics.
  • the robustness of the predetermined antireflective coating corresponds to the standard deviation of hue angle, also called“hue” or“h” of these 500 iterations.
  • table 9 shows that the lens according to the invention has an improved robustness as compared to the lens of the prior art document.

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Abstract

La présente invention concerne un article optique comprenant un substrat transparent présentant une face principale avant et une face principale arrière, la face principale avant et/ou la face principale arrière étant revêtues au moins : d'une sous-couche comprenant une couche épaisse principale qui est déposée dans une chambre à vide sous une pression prédéfinie et un revêtement antireflet multicouche comprenant au moins une couche HI ayant un indice de réfraction supérieur ou égal à 1,55, et au moins une couche LI ayant un indice de réfraction inférieur à 1,55, ledit revêtement antireflet multicouche ayant un facteur de réflexion de lumière moyen dans la région visible Rv qui est inférieur ou égal à 1,5 % en ce qui concerne au moins un angle d'incidence inférieur à 35° et un facteur de réflexion moyen Ruv compris entre 280 nm et 380 nm, pondéré par la fonction W(A) définie dans la norme ISO 13666:1998, qui est inférieur ou égal à 5 %, en ce qui concerne un angle d'incidence dans la plage de 20° à 50°, ladite couche HL comprenant au moins un matériau choisi dans le groupe constitué par le pentoxyde de tantale (Ta205), et ledit revêtement antireflet multicouche ne comportant pas de défauts de fabrication apparents évalués visuellement en transmission.
PCT/IB2018/000921 2018-07-18 2018-07-18 Article optique à revêtement antireflet amélioré, et ses procédés de fabrication WO2020016620A1 (fr)

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EP3182177A1 (fr) * 2015-12-18 2017-06-21 ESSILOR INTERNATIONAL (Compagnie Générale d'Optique) Couches composites à indice élevé pour des empilements anti-réfléchissants
EP3203274A1 (fr) * 2016-02-04 2017-08-09 ESSILOR INTERNATIONAL (Compagnie Générale d'Optique) Lentille ophtalmique comprenant un mince revêtement antireflet avec une très faible réflexion dans ce qui est visible

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