WO2011149694A1 - Échange d'ions de verre à revêtement antireflet ar et procédé associé - Google Patents

Échange d'ions de verre à revêtement antireflet ar et procédé associé Download PDF

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Publication number
WO2011149694A1
WO2011149694A1 PCT/US2011/036608 US2011036608W WO2011149694A1 WO 2011149694 A1 WO2011149694 A1 WO 2011149694A1 US 2011036608 W US2011036608 W US 2011036608W WO 2011149694 A1 WO2011149694 A1 WO 2011149694A1
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WO
WIPO (PCT)
Prior art keywords
glass
coating
ion
ions
compressive stress
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Application number
PCT/US2011/036608
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English (en)
Inventor
Jiangwei Feng
Xavier Gerard Lafosse
Mike Xu Ouyang
Yawei Sun
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Corning Incorporated
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Publication of WO2011149694A1 publication Critical patent/WO2011149694A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • 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
    • 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
    • G02B1/12—Optical coatings produced by application to, or surface treatment of, optical elements by surface treatment, e.g. by irradiation
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/73—Anti-reflective coatings with specific characteristics
    • C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
    • 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
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes

Definitions

  • the present disclosure relates to a process for making a strengthened glass having an anti-reflective ("AR") coating there and to the glass made according to the process. More particularly, the disclosure relates a process for depositing an anti-reflective coating on a glass and chemically strengthening the glass by ion-exchange after placement of the anti-reflective coating.
  • AR anti-reflective
  • Glasses may be chemically strengthened using an ion-exchange process.
  • metal ions that are present in a region at or near the surface of a glass are exchanged for larger metal ions, typically by immersion of the glass in a molten salt bath.
  • the presence of the larger ions in the glass strengthens the glass by creating a compressive stress in a region near the surface.
  • a tensile stress is induced within a central region of the glass to balance the compressive stress.
  • AR coatings can be deposited on the surface glass substrates by numerous methods, for example, the sol-gel method and vacuum deposition methods such as convention deposition (“CD” )in which the materials to be deposited are heated to the molten state by either a resistance heating method or electron bombardment (an e-beam), chemical vapor deposition (“CVD”), ion-assisted deposition (“IAD”) which is similar to CD with the added feature that the film being deposited is bombarded with energetic ions of an inert gas (e.g., argon) during the deposition plus some ionized oxygen when oxide films are being deposited ( to improve film
  • CD convention deposition
  • CVD chemical vapor deposition
  • IAD ion-assisted deposition
  • sol-gel coating is an attractive alternative coating technology for the mass production of consumer products.
  • the sol-gel method utilizes that low cost materials and equipment, and operates at or near room temperatures (for example, 18-25°C) and ambient pressures.
  • the sol-gel coating in general requires curing, which is accomplished by either applying heat energy[D. Chen, "Anti-reflection coatings made by sol-gel process: a review," Solar Energy Materials & Solar Cells, Vol. 68 (2001), pp. 313-336], to evaporate residual organics and other liquid compounds of the solution from the adhered layer; by curing in an ammoniacal atmosphere [U.S. Patent No. 7,642, 199 and EP Patent No.
  • UV curing U.S. Patent No. 6,942,924 and article by P. Belleville et al, "A UV cured sol-gel broadband antireflective and scratch-resistance coating for CRT", So-Gel Optics V, Proceedings ofSPIE, Vol. 3943 (2000), pp.67 - 71] to densify the coating structure.
  • high temperature curing especially curing at temperature above approximately 300°C can compromise an
  • ion-exchanged glass 's high damage resistance results from ion-exchange process, which generates high compressive stress by exchanging, for example, sodium ion from glass with potassium ion from KNO 3 bath, by causing relaxation of the compressive stress.
  • IOX ion-exchanged
  • Another factor of concern with sol-gel coating is that an "edge effect" from sol-gel coating process can cause a coating area of
  • the present disclosure is directed to a method for producing anti-reflection (AR) and/or anti-glare (AG) coated, ion-exchanged glass articles produced by a process including providing a sheet of a selected glass material having
  • glasses containing sodium and or lithium can be ion-exchanged by potassium ions or cesium ions.
  • the ion-exchange can be done in a single step or in a plurality of steps using one or more ion-exchange baths of the same of different composition.
  • Na/Li ions in a glass can be exchanged using a K-ion containing bath in a first step and a K/Cs ion containing bath in a second step; or a both baths can contain K-ions.
  • an advantage of the method described herein, in which the IOX is carried out after formation of the AR coating, including curing, is that maximum compressive stress is obtained.
  • an ion-exchanged glass is AR coated after the ion-exchange has been carried out it is necessary to carefully control any curing of the AR coating. Temperatures above 300°C are to be avoided because above this temperature relaxation of the compressive stress generated by ion-exchange, which is what strengthens the glass, is relaxed. The result is that the compressive stress is diminished and there is a loss of impact and shock resistance.
  • the glass can be ion -exchanged to achieve high compressive stress without significant loss of AR properties.
  • 3- and 4-layer AR-coated glass that is subsequently ion-exchanged produces AR/IOV glass that has a compressive stress greater than 620 MPa and depth of layer greater than 23 ⁇ .
  • the compressive stress is greater than 660 MPa and the depth of layer is greater than 30 ⁇ .
  • the compressive stress is greater than 700 MPa and the depth of layer is greater than 35 ⁇ .
  • the compressive stress is greater than 720 MPa and the depth of layer is greater than 38 ⁇ .
  • Figures la and lb are schematic illustrating the main process steps of the existing and the present disclosure processes, respectively, for sol gel/AR coating to produce AR coated, chemically strengthened glass articles.
  • Figure 2 a is a graph illustrating the IOX effect on single layer AR coating reflectance.
  • Figure 2b is a graph illustrating the IOX effect on four layer sol-gel AR coating reflectance.
  • Figure 2c is a graph illustrating the IOX effect on three layer sol-gel AR coating reflectance.
  • Figure 3 is a chart illustrating the IOX effect on compressive stress and K ion diffusion depth for the various AR coated ion-exchanged glasses of Table 1.
  • Figure 4 is a graph illustrating the K and Na depth profiles of ion-exchanged glass as obtained by electron microprobe analysis (EPMA).
  • Figure 5a illustrates the discoloration of a glass sample due to reaction with the IOX salt because the sol-gel AR coating was not thoroughly cured prior to IOX.
  • Figure 5b illustrates a sol-gel AR coating that was properly curd before IOX.
  • an AR coating is used to exemplify the disclosure.
  • anti-glare coatings can be applied according to what is disclosed herein. Both anti-glare and anti-reflective treatments represent ways to improve or optimize readability. However, they accomplish this in different ways.
  • Anti-glare coatings use a diffusion mechanism to breakup light from an external source (for example, the sun or room lighting) reflected from the surface of an article. Anti-reflection deals with both internal and external sources that are transmitted through a display window.
  • the index of refraction difference or materials in the layers (air/solid or solid/solid) between the layers creates transitional phase differences that increase the amount of light that is reflected. These reflections are cumulative and can "wash out" the display, making the image unreadable without increasing the light output of the display, which is undesirable because this requires increasing the power to the display, and for portable display items the power increase will lead to shorted battery life between recharging or replacement.
  • FIG. l a is a schematic illustrating the main steps of existing sol-gel methods/processes 10 for preparing AR-coated, ion-exchanged glass.
  • the method 10 involves the step sequence of ion-exchanging 12 a provided glass, cleaning 14 the ion-exchanged glass, sol-gel coating 16 the cleaned ion-exchanged glass and curing the sol-gel coat, and cutting and trimming 18 the cured sol-gel coating.
  • a glass containing exchangeable ions such as Li and/or Na ions is ion-exchanged, replacing the Li and/or Na ions with larger ions, for example, K ions.
  • the glass is cleaned and coated with a sol-gel AR coating mixture that may then be dried to partially remove fluids and cured to form an AR coating on the surface of the ion-exchanged glass.
  • the curing can be done thermally, but care must be taken so that the curing temperature is not done at a temperature at which the compressive stress within the ion-exchanged glass is relaxed. If such relaxation does occur the glass loses some part of the strength attain by the ion-exchange process.
  • the exact maximum temperature for thermal curing may vary from glass-to-glass composition, but it is typically below 350°C and preferably below 300°C. After the sol-gel AR coating has been cured, the coated glass may then be cut and trimmed to the desired size.
  • UV curing in place of thermal curing avoids overheating the coated substrate, but problem is that cutting and trimming after coating an IOXed glass can introduce microcracks into the cut or trimmed surfaces, and these microcracks can grow during use and result in a cracked or broken glass in the final product.
  • Figure lb is a schematic illustrating the main steps of the process 20 of the present disclosure for preparing AR-coated, ion-exchanged glass.
  • the method 20 involves the step sequence of cleaning 22 a non-ion-exchanged glass, sol-gel coating 24 the cleaned glass and curing the sol-gel coat, cutting and trimming 26 the cured sol-gel coating, and ion-exchanging 28 the coated, cut and trimmed glass.
  • a glass containing exchangeable ions such as Li and/or Na ions is cleaned 22, coated with a sol-gel AR coating, and the AR coating on the glass is either thermally cured or UV cured 14. In one embodiment the coating is UV cured.
  • the coated glass is cut and trimmed into the desired size and any necessary edge finishing such as grinding or lapping is carried out.
  • the sized, and edge finished glass is placed in an ion-exchange medium to exchange ions such as Li and/or Na for larger ions such K ions.
  • the glass is cleaned and any additional process steps, for example without limitation, printing features (e.g., logos or writings) on the surface of the glass or applying oleophobic and/or hydrophobic coatings to the glass, can carried out. In this process the glass all surfaces are ion-exchanged and strengthened.
  • the cured sol-gel AR coating should have sufficient hardness so that it is not marred, for example, by scratches, during subsequent procedures involving, for example without limitation, cutting, lapping, trimming, ion-exchange, cleaning and so forth.
  • One simple way to determine whether the coating has sufficient hardness is to conduct a "pencil hardness" test of the coating. The pencil hardness test can also be used to determine the hardness of the coating after the AR coated glass has been ion-exchanged.
  • the pencil hardness test uses a grades set of pencils of hardness 9H (the hardest), 8H, 7H, 6H, 5H, 4H, 3H, 2H, F, HB, B, 2B, 3B, 4B, 5B, 6B, 7B, 8B and 9B (the softest).
  • the letter “H” and “B” stand for "hardness” and “blackness,” respectively.
  • the pencil material consists of clay and graphite. Hardness increases with increasing clay content and blackness decreases. Thus, for all pencils, the more clay the harder the pencil.
  • the test surface should be clean and free of any dirt and loose residuum from the AR and/or IOX process.
  • the pencil test is simple and easy to perform, gives uniform results and is dependable because the pencils are uniform in their grading.
  • To perform the test select a pencil and make a line at least 1 -inch ( ⁇ 2.5cm) along the surface of the test piece. If the pencil leaves a scratch, use the next softer pencil and repeat the process.
  • the number of the first pencil that does not make a scratch after the use of a pencil that does make a scratch is considered the "pencil hardness" of the coating. For example, if an AR (only) coated piece is pencil tested and a 3H pencil leaves a scratch, but a 2H pencil does not leave a scratch, the pencil hardness of the coating is 2H. Any coating that is not scratched by a 9H pencil is considered to have a 9H hardness rating.
  • Pencil testing was carried out on a series of samples that were AR coated and ion-exchanged.
  • the AR coatings were 1 -layer, 3 -layer and 4-layer coatings that were deposited using a sol-gel consisting of, for example without limitation, S1O2, AI2O 3 , T1O2 and/or transition metal oxides, for example without limitation, the oxides of Ti, Hf, Gd, and Zr.
  • the sol-gel can be made using known methods, for example without limitation, using an alkoxide of Si and/or Ti in an acidic alcoholic medium that contains alkali metal salts (generally the chloride, nitrate or acetates) of Ti and/or Al or others metals.
  • the sol-gel can be thixotropic or non-thixotropic and it can be applied as one or a plurality of layers by dipping, spraying or other means known in the art.
  • the coating can be applied by spraying the sol-gel on the desired side or by protecting the side that is to be uncoated using a protective material, for example, a removable polymer film, and applying the coating to the desired side by dipping.
  • the thickness of the coating can be varied.
  • the AR coating has a thickness in the range of 50-nm to 350nm.
  • the AR coating has a thickness in the range of lOOnm to 250nm.
  • the AR sol-gel coating After the AR sol-gel coating has been applied to the desired surface or surfaces it is cured in an oxygen containing atmosphere (for example, air or air admixed with additional oxygen) either thermally or by UV curing.
  • Thermal curing is typically carried out for a selected time in the range of 20 minutes to 12 hours at a temperature in the range of 150°C to either 600°C or below the softening point of the glass, whichever is lower.
  • the thermal curing is carried out at a temperature in the range of 350°C to 600°C for a time in the range of 1 hour to 5 hours.
  • thermal curing can be carried out at lower temperatures in the presence of ozone (O 3 ), for example, thermal curing at a temperature in the range of 170°C to250°C in the presence of a selected amount of ozone to promote the burning of any organic residue.
  • O 3 ozone
  • Table 1 summarizes the pencil hardness for the samples that were AR coated and then IOXed.
  • test results indicate that after ion-exchange the hardness of the surface increased when ion-exchange was carried out after the glass had been AR coated using a sol-gel.
  • the AR coatings can be either a single layer coating or a multilayer coating.
  • Figures 2a to 2c show optical performance, reflectance versus wavelength, test results for a series of glass articles in which the AR coating was applied, as a sol-gel, either before or after ion-exchange.
  • Tables 2a to 2c describe the samples of 1 -layer, 3 -layer and 4-layer AR coated, IOXed glass whose optical performance, measured as reflectance versus wavelength, were evaluated. In all cases ion-exchange was carried out after the AR coating was fully cured.
  • Tables 2a to 2c correspond to Figures 2a to 2c, respectively.
  • Figures 2a to 2c shows the IOX effect on the optical performance of different layer AR coatings.
  • Figure 2(a) is the single layer AR coating optical performance. The order of the samples is given on both sides of minimal reflectance. The minimal reflectance at either 490nn or 535nm wavelength was degraded from 0.4% to 0.5% and is believed due to an IOX process-induced densification of AR sol-gel structure. Different IOX processes have different impact on AR coating reflectance.
  • Figure 2(b) and 2(c) are represent the 4- and 3 -layer sol-gel coatings after IOX, respectively, and show both reflectance shift or deformation, which again shows that the IOX process impacts the
  • Figure 3 is a graph illustrating the optically measured compressive stress and K-ion depth of layer after IOX on AR coated Gorilla ® glass. It indicates that different sol-gel AR coatings (1-, 3-, and 4-layer), cured at selected times and temperatures, respond differently to IOX process. For example, single layer sol-gel AR has fast diffusion rate than multilayer AR coated glass and leads to a shorter IOX time. In addition, Figure 3 suggests that it is feasible to optimize the IOX process to meet selected target Compressive Stress (CS) and Depth of Layer (DOL) on an AR coated Gorilla ® glass. Table 5 describes the each glass sample represented by the numerals,
  • Figure 4 is a graph illustrating electron microprobe analysis ("EPMA") measured K and Na ions depth profile on Gorilla ® glass that was AR coated first, then IOX afterwards; the result confirms that the optically measured DOL on AR coated glass is convincing.
  • EPMA electron microprobe analysis
  • any glass composition capable of being ion-exchanged can be used in accordance with this disclosure, Such glass, or glass-ceramic, composition contain smaller ions, typically Na and Li ions that can be exchanged by larger ions, for example by K, Rb and Cs ions.
  • Such glass compositions include soda lime, alkali aluminosilicate and alkali aluminoborosilicate glasses.
  • An example without limitation of an alkali aluminosilicate glass is one described in the commonly assigned U.S. Patent Application Publication No.
  • 2010/0009154 that can be used in the present disclosure is one having the approximate composition: 66 mol% Si0 2 ; 14 mol% Na 2 0; 10 mol% A1 2 0 3 ; 0.6 mol% B 2 0 3 ; 2.5 mol% K 2 0; 5.7 mol% MgO; 0.6 mol% CaO; 0.2 mol% Sn0 2 ; and 0.02 mol% Zr0 2 .
  • the sodium in this glass can be exchanged with potassium, rubidium, or cesium to produce a region of high compressive stress near the surface and a region under central tension in the interior or central region of a glass part.
  • lithium lithium
  • sodium sodium
  • potassium sodium
  • cesium sodium
  • the lithium can be then be exchanged with sodium, potassium, rubidium, or cesium to obtain a high surface compressive stress and an interior volume under tension.
  • one or more of the ions in the glass must be replaced by an ion in the salt solution that has a higher atomic number; for example, sodium replaces lithium in the glass, potassium replaces sodium and/or lithium in the glass, rubidium replaces potassium and/or sodium and/or lithium in the glass and so forth.
  • the disclosure is directed to a chemically strengthened glass article comprising a glass article having a first and a second face and a selected thickness, the glass article having at compressive outer layers extending for a selected depth into said first and second faces and an tensile inner layer formed between said compressive layers, and a selected coating on at least one of the first and second faces of said glass article.
  • the coating is selected from the group consisting of an anti-reflection and anti-glare coating, and said coating contains at least 5 wt% potassium oxide.
  • the selected coating contains at least 10 wt% potassium oxide.
  • the selected coating can be a multilayer coating consisting of 2-4 layers.4.
  • the chemically strengthened glass according to claim 1 wherein said selected coating has a thickness in the range of 50nm to 350nm. In one embodiment the selected coating has a thickness in the range of lOOnm to 250nm. In one embodiment the glass, after coating and ion-exchange has a compressive stress of at least 620 MPa and a depth of layer of at least 23 ⁇ . In another embodiment the glass has a compressive stress of at least 660 MPa and a depth of layer of at least 30 ⁇ .8. In a further embodiment the glass has a compressive stress of at least 700 MPa and a depth of layer of at least 35 ⁇
  • the resulting ion-exchanged glass has been found to contain at least 5 wt% potassium oxide in the AR coating.
  • the amount of potassium ions in the AR coating is at least 10 wt% potassium oxide. This is due for example, to migration of sodium ions (and/or lithium ions) that enter the AR coating layer through migration from the glass into the AR coating.
  • the migrated sodium (and/or lithium) ions are then ion-exchanged by for potassium ions in the ion-exchange bath.
  • the resulting exchange of ions in the AR coating imparts an additional hardness to the cured AR coating.
  • the disclosure is accordingly directed to a method for making a chemically strengthened glass article having a selected coating thereon.
  • the method comprises providing a shaped glass article of a selected composition having a first and second face and a selected thickness, the glass article containing sodium and/or lithium ions; applying a selected sol-gel coating to the first and second faces of said glass article; curing the sol-gel on the surfaces of said article by a method selected from the group consisting of thermal curing and UV curing; providing a ion-exchange bath containing selected alkali metal ions larger than lithium and/or sodium ions, and ion-exchanging lithium and/or sodium ions in the selected coating and in the glass with said selected alkali metal ions larger than lithium and/or sodium, said ion-exchange replacement of ions extending through the selected coating and to a selected depth from the surface of said first and selected faces to thereby generate a compressive stress.
  • the sol-gel coating is selected from the group consisting of anti-reflection and anti-glare coating, and the coating, after ion-exchange, contains, as the oxide, at least 5 wt% of the alkali metal ions larger than lithium and/or sodium ion.
  • the selected coating can be a 1 -layer coating or a 2-4 multilayer anti-reflective or anti-glare coating having a thickness in the range of 50nm to 350nm. In one embodiment of the method that applied coating has a thickness in the range of ⁇ to 250 ⁇ .
  • the ion-exchange is carried for a time such that the glass has a compressive stress of at least 620 MPa and a depth of layer of at least 23 ⁇ .
  • the ion-exchange is carried out such that the glass has a compressive stress of at least 660 MPa and a depth of layer of at least 30 ⁇ . In a further embodiment the ion-exchange is carried out such that the glass has a compressive stress of at least 700 MPa and a depth of layer of at least 35 ⁇ .
  • the selected alkali metal ions larger than lithium and/or sodium ions are selected from the group consisting of potassium, rubidium and cesium ions, and mixtures thereof.

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  • Engineering & Computer Science (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention porte sur un procédé de fabrication d'articles en verre, ayant subi un échange d'ions à revêtement antireflet AR ou AG, fabriqués par un procédé comprenant l'utilisation d'une feuille d'un matériau en verre choisi ayant des ions pouvant subir un échange d'ions, le nettoyage de la feuille de verre, le revêtement du verre avec une matière de revêtement sol-gel, le séchage du mélange de revêtement sur la feuille de verre, le durcissement du revêtement afin d'obtenir un verre ayant un revêtement adhérent sur celui-ci et l'échange d'ions des ions pouvant subir un échange d'ions présents dans la feuille de verre et dans le revêtement sur celle-ci par des ions de plus grande taille afin de former ainsi au moins une couche ayant subi un échange d'ions dans ledit verre et de conférer une contrainte de compression dans le verre pour de cette manière le renforcer. Dans un exemple, dans le verre à revêtement antireflet AR et/ou AG ayant subi un échange d'ions la contrainte de compression dans le verre est d'au moins 660 MPa et la profondeur de la couche est d'au moins 30 µm. Dans un autre exemple, la contrainte de compression est d'au moins 700 MPa et la profondeur de la couche est d'au moins 35 µm.
PCT/US2011/036608 2010-05-26 2011-05-16 Échange d'ions de verre à revêtement antireflet ar et procédé associé WO2011149694A1 (fr)

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WO2013078039A1 (fr) * 2011-11-23 2013-05-30 Corning Incorporated Verre et stratifiés de verre renforcés présentant une résistance asymétrique au choc
KR20130084864A (ko) * 2012-01-18 2013-07-26 삼성코닝정밀소재 주식회사 강화 유리 제조방법 및 이에 의해 제조되는 강화 유리
WO2013116420A1 (fr) * 2012-02-01 2013-08-08 Corning Incorporated Procédé de production de constance de la contrainte de compression dans du verre dans un procédé par échange d'ions
WO2013106629A3 (fr) * 2012-01-13 2013-11-07 Corning Incorporated Articles en verre résistant à la réflexion et leurs procédés de fabrication et d'utilisation
CN103979800A (zh) * 2014-03-31 2014-08-13 广州视睿电子科技有限公司 防眩钢化玻璃及其制备方法
WO2014190014A1 (fr) * 2013-05-23 2014-11-27 Corning Incorporated Stratifies de verre-film dotes d'une resistance a la rupture regulee
DE102014013527A1 (de) * 2014-09-12 2016-03-17 Schott Ag Verfahren zur Herstellung eines beschichteten, chemisch vorgespannten Glassubstrats mit Antifingerprint-Eigenschaften sowie das hergestellte Glassubstrat
DE102014013550A1 (de) 2014-09-12 2016-03-31 Schott Ag Beschichtetes chemisch vorgespanntes flexibles dünnes Glas
CN103979800B (zh) * 2014-03-31 2016-11-30 广州视睿电子科技有限公司 防眩钢化玻璃及其制备方法
DE102015213075A1 (de) * 2015-07-13 2017-01-19 Schott Ag Asymmetrisch aufgebaute, auf beiden Oberflächenseiten chemisch vorgespannte Dünnglasscheibe, Verfahren zu deren Herstellung sowie deren Verwendung
WO2017041307A1 (fr) * 2015-09-11 2017-03-16 Schott Glass Technologies (Suzhou) Co. Ltd. Procédé de production d'un article de verre trempé comportant un revêtement fonctionnel durable, et article de verre trempé comportant un revêtement fonctionnel durable
US20170233287A1 (en) * 2014-09-12 2017-08-17 Schott Ag Coated glass substrate or glass ceramic substrate with resistant multifunctional surface properties, method for production thereof, and use of thereof
JP2017178634A (ja) * 2016-03-28 2017-10-05 フクビ化学工業株式会社 高反射防止強化ガラスの製造方法
US10071933B2 (en) 2013-03-15 2018-09-11 Schott Glass Technologies (Suzhou) Co. Ltd. Chemically toughened flexible ultrathin glass
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CN112379472A (zh) * 2020-11-13 2021-02-19 上海卫星装备研究所 一种低吸辐比的光学太阳反射镜及其制备方法
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WO2013078039A1 (fr) * 2011-11-23 2013-05-30 Corning Incorporated Verre et stratifiés de verre renforcés présentant une résistance asymétrique au choc
WO2013106629A3 (fr) * 2012-01-13 2013-11-07 Corning Incorporated Articles en verre résistant à la réflexion et leurs procédés de fabrication et d'utilisation
KR20130084864A (ko) * 2012-01-18 2013-07-26 삼성코닝정밀소재 주식회사 강화 유리 제조방법 및 이에 의해 제조되는 강화 유리
KR101714423B1 (ko) * 2012-01-18 2017-03-09 코닝정밀소재 주식회사 강화 유리 제조방법 및 이에 의해 제조되는 강화 유리
WO2013116420A1 (fr) * 2012-02-01 2013-08-08 Corning Incorporated Procédé de production de constance de la contrainte de compression dans du verre dans un procédé par échange d'ions
US10071933B2 (en) 2013-03-15 2018-09-11 Schott Glass Technologies (Suzhou) Co. Ltd. Chemically toughened flexible ultrathin glass
WO2014190014A1 (fr) * 2013-05-23 2014-11-27 Corning Incorporated Stratifies de verre-film dotes d'une resistance a la rupture regulee
CN103979800A (zh) * 2014-03-31 2014-08-13 广州视睿电子科技有限公司 防眩钢化玻璃及其制备方法
CN103979800B (zh) * 2014-03-31 2016-11-30 广州视睿电子科技有限公司 防眩钢化玻璃及其制备方法
DE102014013527A1 (de) * 2014-09-12 2016-03-17 Schott Ag Verfahren zur Herstellung eines beschichteten, chemisch vorgespannten Glassubstrats mit Antifingerprint-Eigenschaften sowie das hergestellte Glassubstrat
DE102014013550A1 (de) 2014-09-12 2016-03-31 Schott Ag Beschichtetes chemisch vorgespanntes flexibles dünnes Glas
US20170233287A1 (en) * 2014-09-12 2017-08-17 Schott Ag Coated glass substrate or glass ceramic substrate with resistant multifunctional surface properties, method for production thereof, and use of thereof
CN115521063A (zh) * 2014-11-04 2022-12-27 康宁股份有限公司 深层非易碎应力曲线及其制造方法
US20170015584A1 (en) * 2015-07-13 2017-01-19 Schott Ag Asymmetrically structured thin glass sheet that is chemically strengthened on both surface sides, method for its manufacture as well as use of same
DE102015213075A1 (de) * 2015-07-13 2017-01-19 Schott Ag Asymmetrisch aufgebaute, auf beiden Oberflächenseiten chemisch vorgespannte Dünnglasscheibe, Verfahren zu deren Herstellung sowie deren Verwendung
CN108025962A (zh) * 2015-09-11 2018-05-11 肖特玻璃科技(苏州)有限公司 用于生产具有耐用功能性涂层的钢化玻璃制品的方法及具有耐用功能性涂层的钢化玻璃制品
WO2017041307A1 (fr) * 2015-09-11 2017-03-16 Schott Glass Technologies (Suzhou) Co. Ltd. Procédé de production d'un article de verre trempé comportant un revêtement fonctionnel durable, et article de verre trempé comportant un revêtement fonctionnel durable
CN108025962B (zh) * 2015-09-11 2021-04-30 肖特玻璃科技(苏州)有限公司 用于生产具有耐用功能性涂层的钢化玻璃制品的方法及具有耐用功能性涂层的钢化玻璃制品
JP2017178634A (ja) * 2016-03-28 2017-10-05 フクビ化学工業株式会社 高反射防止強化ガラスの製造方法
US20200283335A1 (en) * 2017-11-16 2020-09-10 Hewlett-Packard Development Company, L.P. Protective panels with anti-glare coating
CN112379472A (zh) * 2020-11-13 2021-02-19 上海卫星装备研究所 一种低吸辐比的光学太阳反射镜及其制备方法

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