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EP4255860A1 - Effet antireflet amélioré - Google Patents

Effet antireflet amélioré

Info

Publication number
EP4255860A1
EP4255860A1 EP21823295.7A EP21823295A EP4255860A1 EP 4255860 A1 EP4255860 A1 EP 4255860A1 EP 21823295 A EP21823295 A EP 21823295A EP 4255860 A1 EP4255860 A1 EP 4255860A1
Authority
EP
European Patent Office
Prior art keywords
glass article
oxide layer
cvd
oxide
layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP21823295.7A
Other languages
German (de)
English (en)
Inventor
Valérie FARINA
Eric Tixhon
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AGC Glass Europe SA
Original Assignee
AGC Glass Europe SA
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 AGC Glass Europe SA filed Critical AGC Glass Europe SA
Publication of EP4255860A1 publication Critical patent/EP4255860A1/fr
Pending legal-status Critical Current

Links

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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • 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
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/365—Coating different sides of a glass substrate

Definitions

  • the present invention relates to improved anti-reflective glazing, characterized through a visible light transmittance of at least 90% and a visible light reflectance of at most 1.0%.
  • the glazing of the invention is heat treatable and chemically and mechanically durable. Thanks to its properties, the glazing of the invention is suitable for applications involving monolithic glass substrates, laminated glass substrates and multiple glazing units. Applications are in automotive, building and house appliances.
  • the glass article of the invention is separating external and internal part of a building or of a closed system such a fridge.
  • Each glass surface is responsible for a light reflection.
  • a special coating is capable of decreasing this reflection at the surface between air and glass.
  • prior art disclose anti-reflective coating and by anti-reflective coating, we hereby mean a stack comprising a succession of high and low refractive index layers. A lot of solutions describes such successions of alternative high and low refractive index layers.
  • Such coatings may be deposited by any known method on the glass surface.
  • WO2016066994A1 discloses a glass substrate and a coating formed over the glass substrate which comprises a first oxide layer with a refractive index of at least 1.8 and a second oxide layer with a refractive index of at most 1.6, resulting in a visible light reflectance of at most 6.5%.
  • the two oxide layers are preferably deposited by CVD during the float glass process.
  • US20070236798A1 discloses a four layers reflecting stack (alternating high and low refractive index) deposited by Magnetron sputtering which allow an increase of at least 3 % of the light transmission thanks to a lower reflection.
  • AGC has develop a highly transparent product (EP3385236A1) with the same anti-reflective coating deposited on both main surfaces of the glass substrate, allowing a maximum of 2% visible light reflectance. Both coatings are deposited following a sputtering method. As can be seen very good results may be obtained in term of anti-reflective glass substrates.
  • This invention concerns anti-reflective coated article with enhanced anti- reflective effect.
  • the present invention is the result of an investigation concerning the possibility of combining CVD air side anti-reflective coating with PVD tin side anti-reflective coating and show how it is possible to improve the visible light transmission and decrease the visible light reflection.
  • Oxide layers of high and low refractive index material have been deposited on both side of a glass substrate. To optimize the thicknesses of the oxide layers, some simulations have been made and were indicating promising results. On a very surprising and still not understood way, it appears that the real optical parameters were far better than the simulated ones.
  • the anti-reflective coated article of the invention is far less impacted through a heating process. Namely, the difference between the reflected colour after tempering is less affected by the heating than the reflected colour of the double sides anti-reflected coating when both sides are PVD-coated. In other words, the coated article of the invention has a better matchability between heat treated and non-heat treated article. More particularly the colour variation in reflection expressed as AE* Rc is lower than 4.0, preferably lower than 3.5 and more preferably lower than 3.0.
  • the anti-reflective coated article of the invention comprises a glass substrate having two major surfaces, hereby called the air-side and the tin-side surfaces, those names referring to the float manufacturing process of the glass article.
  • the air-side is coated with a CVD coating and the tin-side is coated with a PVD coating.
  • Both coatings are designed to have anti-reflective properties and both coating are a succession of oxide layers with high refractive index and low refractive index.
  • the low refractive index layers comprise silicon oxide.
  • the CVD high refractive index layers comprise tin oxide or titanium oxide.
  • the coated article of the invention is a class A product, as defined in the norm EN 1096-2, being as a consequence a durable coated article and also meaning that the PVD coating does not contain silver layer. This is true for the article before and after heat treatment. This means that it is possible to perform a heat treatment on the coated article of the invention when necessary.
  • anti-reflective coating we mean a coating such that the measurement of visible light reflection made on the coated article is at least 1 % lower, preferably at least 1.5% lower and more preferably at least 2% lower than the reflection measured on the uncoated same glass article. This effect is verified on both sides.
  • the measurement of the visible light reflection is at least 2% lower, preferably at least 2.5% lower and more preferably at least 3% lower than the measurement of the visible light reflection of the corresponding single side anti-reflective coated article.
  • CVD coating we mean a coating deposited during the float glass process involving gaseous, powder or sprayed precursors that are chemically transformed during deposition on glass at temperature greater than 400°C.
  • CVD oxide layer we mean an oxide layer deposited by a CVD process. Any CVD process known in the art is convenient for manufacturing the CVD-coating of the invention, such as an online or an offline process. For example WO2010107998 gives good non limiting examples for the CVD online process and is incorporated here in its entirety by reference. The CVD offline process is also possible, though more expensive.
  • PVD coating we refer to the well-known deposition process involving plasma sputtering of a target in high vacuum atmosphere.
  • PVD oxide layer we mean an oxide layer deposited by a PVD process. Any sputtering process is suitable to build the anti-reflective coating of the invention. Alternatively, part or all of the PVD coating may also be made through a process known in the art as a PECVD process.
  • temperable coated article we mean that the coated article after having been heat treated at a temperature greater than 600°C for more than 2 minutes and less than 10 minutes, has not been altered. Namely, no marks, scratches or cracks, nor corrosion traces should be observed on the coated product after tempering. Time and duration for the heat treatment are adjusted in a known way depending the glass thickness.
  • the optical properties of the samples are measured with a spectrophotometer Perkin Elmer Lamdba 950 with an integrating sphere of 150 mm diameter.
  • the visible transmittance and visible reflectance performances are expressed according to the standard EN 410 (2011).
  • the integrated values visible transmittance (Tv) and reflectance (R) are determined with a D65 illuminant defined by the CIE standard and at a solid observer angle of 2°.
  • the other properties (L*, a*, b*) are also measured with a D65 illuminant but at a solid observer angle of 10°.
  • the external reflectance (measured from a point outside the building or outside the enclosed system) is represented by R ou t and the internal reflectance (measured from a point inside the building or the enclosed system) is represent by Rin.
  • R ou t The external reflectance (measured from a point outside the building or outside the enclosed system) is represented by R ou t and the internal reflectance (measured from a point inside the building or the enclosed system) is represent by Rin.
  • AL* is the difference in colour coordinates L* before and after heat treatment
  • Aa* is the difference in colour coordinates a* before and after heat treatment
  • Ab* is the difference in colour coordinates b* before and after heat treatment.
  • the AE* value may be calculated for the colour in transmission or reflection.
  • the refractive index n is calculated from the light spectrum wavelength at 550 nm.
  • low refractive index oxide layer we mean an oxide layer which refractive index is not greater than 1 .8, preferably not greater than 1 .7 and more preferably not greater than 1 .6.
  • high refractive index oxide layer we mean an oxide layer which refractive index is not smaller than 1.7, more preferably not smaller than 1.8 and more preferably not smaller than 1.9.
  • Fig 1a shows the first embodiment of the invention
  • Fig 1b shows the first embodiment of the invention in combination with the fourth embodiment.
  • Fig 2a shows the second embodiment of the invention
  • Fig 2b shows the second embodiment of the invention in combination with the fourth embodiment.
  • Fig 3a shows the third embodiment of the invention
  • Fig 3b shows the third embodiment of the invention in combination with the fourth embodiment.
  • Fig 4a shows a combination of the second and the third embodiments of the invention
  • Fig 4b shows a combination of the second, the third and the fourth embodiments of the invention.
  • the substrate is an inorganic soda-lime glass from a float process.
  • the substrate is a clear glass or an extra clear glass.
  • the clear glass has a composition characterized by an iron content expressed in weight percent of Fe O3 which is at most 0.1 %. This value drops to at most 0.015% for the extra clear glass.
  • the glass substrate of the invention has a thickness that is greater than 1 mm, preferably greater than 1.5 mm and more preferably greater than 2 mm.
  • the thickness of the glass substrate of the invention is at most 20 mm, preferably at most 15 mm and more preferably at most 10 mm.
  • the thickness of the glass substrate is comprised between 3 and 6 mm.
  • a 4 mm clear glass substrate has a light transmittance of about 90.5%.
  • a 4 mm glass substrate with the extra clear composition has a light transmittance of about 91.7% and a reflectance value of about 8%
  • the anti-reflective coated article with enhanced anti-reflective effect of the invention comprises a substrate with two main surfaces, each of the main surface being coated with an anti-reflective coating.
  • the so-called air-side of the substrate which is the upward main surface during the float process, is coated through a CVD on-line process with at least 3 CVD oxides layers, those at least 3 CVD oxide layers being characterized by a succession of low and high refractive index (first embodiment).
  • the first and third CVD oxide layers have both a low refractive index and the second CVD oxide layer is characterized by a high refractive index, said high refractive index being higher than the refractive index of both first and third CVD oxide layers.
  • the said first CVD oxide layer is the layer which is the nearest layer of the substrate, the second CVD oxide layer is deposited between first and third oxide layers.
  • the at least 3 CVD oxide layers may be deposited through an offline process and speaking of CVD oxide layer means equally a layer deposited by an online process or an offline process.
  • At least one of the CVD oxide layer may be replaced by at least one PVD or at least one PECVD oxide layer.
  • at least one of the CVD oxide layer is replaced by at least one PVD or at least one PECVD layer, it is the third (or last) CVD oxide layer.
  • the resulting CVD coated substrate is characterized by a lower reflectance than the uncoated corresponding glass substrate.
  • the reflectance of the CVD coated substrate is at least 1 % lower, preferably at least 1 .5% lower and more preferably at least 2% lower than the uncoated substrate.
  • the CVD low refractive index oxide layers are based on silica and they may contain other elements such as carbon, hydrogen, nitrogen, tin, boron and phosphorus.
  • the CVD high refractive index oxide layers is chosen from a titanium based oxide, a tin based oxide layer or mixture of both.
  • a titanium based oxide In order to attain the requested low reflectance, not only the nature but also the thickness of each layer must be adjusted.
  • the Table 2 illustrate the composition of the CVD coating of the invention. Without any other precision and for the whole text, values are given in nm and are geometric thicknesses.
  • a supplementary CVD oxide layer with a high refractive index is deposited under the first CVD oxide layer of the stack described in the table 2.
  • the refractive index of said supplementary CVD oxide layer is at least 1.7, preferably at least 1.8 and more preferably at least 1.9.
  • said supplementary CVD oxide layer comprises titanium oxide, tin oxide or mixture thereof.
  • the thickness of said supplementary CVD oxide layer is comprised between 5 and 35 nm, preferably between 8 and 30 nm.
  • none of the oxide layers that are deposited on the air side of the glass substrate is a conductive oxide layer such as for example a doped tin oxide or a doped zinc oxide layer.
  • the second CVD oxide layer of the stack described in the table 2 is a transparent conductive oxide layer.
  • the transparent conductive oxide layer of this third embodiment is a doped tin oxide layer.
  • the doping element is chosen from fluoride, antimony or mixture thereof.
  • This third embodiment allows to add a low-emissive property to the anti- reflective coated article.
  • This supplementary CVD oxide layer may also be deposited on the glass surface of the second embodiment.
  • the supplementary CVD oxide layer of the second embodiment is also a doped tin oxide layer.
  • the CVD coated article is characterized by an emissivity that is at most 0.20 and allow to reach a II value of at most 1.6 for a standard DGU configuration (16 mm gap fill with 90% argon, 4 mm glass) when the coated article of the invention is used in a double glazing unit.
  • the CVD coated article of the third embodiment is characterized by an emissivity that is at most 0.15 and allow to reach a II value of at most 1 .5 for a standard DGU configuration (16 mm gap fill with 90% argon, 4 mm glass).
  • the CVD coated article of the third embodiment is characterized by an emissivity that is at most 0.10 and allow to reach a U value of at most 1.3 for a standard DGU configuration (16 mm gap fill with 90% argon, 4 mm glass).
  • the third CVD oxide layer is replaced by a low refractive index oxide layer that is deposited by an offline PVD or PECVD process.
  • the low refractive index oxide layer deposited by an offline PVD or PECVD process is a single silica-based layer or a combined double silica based layer in which the two silica-based part are different in composition.
  • any or both of the silica-based layer deposited by an offline PVD or PECVD process may contain aluminium or zirconium.
  • the second part of the double silica based layer contains 0 to 45 weight % of zirconium oxide.
  • the reflectance of the CVD coated substrate is at most 7%, preferably at most 6.5% and more preferably at most 6%.
  • the resulting CVD coated substrate is then transferred in a magnetron coating installation and the uncoated main surface of the CVD coated substrate is conducted through the magnetron line under the targets where at least 4 PVD oxide layers are deposited on the so called tin-side of the substrate, the side which is opposite to the CVD coated surface.
  • the 4 PVD oxide layers are characterized by a succession of high and low refractive index.
  • the first and third PVD oxide layers of the stack have a refractive index that is at least 1.8, preferably at least 1.9.
  • the second and third PVD oxide of the stack have a refractive index that is at most 1 .8, preferably at most 1 .7.
  • the PVD low refractive index oxide layers are based on silica and they may contain other elements, as for example aluminium and zirconium.
  • the silica PVD low refractive index layer contains aluminium, preferably the aluminium weight proportion is at most 12% (Al ratio related to the total Al and Si content).
  • the silica PVD low refractive index layer contains zirconium, preferably the zirconium weight proportion is at most 28% (Zr ratio related to the total Zr and Si content).
  • the PVD high refractive index oxide layers are based on titanium.
  • the PVD high refractive index oxide layers are a mixed oxide comprising titanium oxide and zirconium oxide.
  • the mixed oxide has a weight composition of TiO2/ZrO2 (TZO) comprised between 50/50 and 75/25. More preferably the mixed oxide layer comprising titanium oxide and zirconium oxide has a weight composition of TiO2/ZrO2: 65/35.
  • TiO2/ZrO2 TiO2/ZrO2
  • the table 3 illustrates the composition of the PVD coating of the invention.
  • the first PVD oxide layer is the layer which is closest to the glass substrate.
  • the second, third and fourth oxide layers are deposited successively above the first oxide layer.
  • the PVD high refractive layers are based on both titanium and zirconium since the presence of zirconium oxide keeps a better appearance after heat treatment (see for example EP3385236A1).
  • the fourth PVD oxide layer of the stack described in the table 3 is a combination of 2 successive silica-based oxide layers.
  • the upper layer is a mixture of silicon oxide and zirconium oxide (SiZrO x ) with a content of at most 45 weight% of zirconium oxide and at least 55 weight% of silicon oxide.
  • SiZrO x zirconium oxide
  • another silicon oxidebased layer is deposited. This other silicon oxide based layer is deposited from a silicon target that contains from 0 to 12 weight% of aluminium.
  • the SiO x layer has a thickness comprised between 50 and 80 nm and the SiZrOx has a thickness comprised between 10 and 40 nm.
  • At least one of the oxide layer of the stack described in the table 3 is deposited through a PECVD process, following well known practice of the art.
  • the PVD coated surface together with the CVD coated surface are characterized by a very low reflectance value, this reflectance value being lower than the one expected by the previous simulation study.
  • the resulting reflectance of the double side coated substrate of the invention is at most 1.2%, preferably at most 1.1 % and more preferably at most 1.0%. These values are the ones measured after heat treatment (670°C, 3 min for 4mm glass).
  • the simulation study has been made following an usual manner known by the man in the art. Simulation is using mathematical modelling to obtain simulated values characterizing a glazing without the necessity of building or prototyping a sample. This is made by using a database of glazing components and material properties, allowing to determine according to international standards, glazing specifications, ranging from optical properties (solar energy, visible light, colour appearance) to thermal properties (U-value, solar factor). More particularly the Transfer Matrix Method is a commonly used tool in Optics. Transmittance and reflectance are calculated for each interface in the glazing as well as attenuation in each component. The theory behind this calculation is described in literature (L.A.A. Petterson, J. of Appl. Phys.
  • the coated glass article of the invention has on both sides a class A coating, which is conform to the norm EN 1096-2 2012E.
  • PVD stack On the tin-side of the coated substrates of the 6 examples of the invention, a PVD stack has been deposited.
  • the PVD stack was the same for all examples and has the following structure:
  • R1 visible reflectance measured on the article with only the CVD coating
  • R2 visible reflectance measured on the article with both CVD and PVD coating
  • R3 visible reflectance simulated (see ⁇ [0047]) for the article with both CVD and PVD coatings.
  • the relation between the measured value of reflectance and the simulated value is given through the ratio R2 divided by R3. As can be seen this ratio is at maximum 0.71 (instead of 1 for an ideal simulation), showing that the measured value is at most 71 % of the simulated value.
  • the last row indicates the measured visible light transmission (Tv) of the coated article of the invention (coated on both sides).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention concerne un article en verre qui est revêtu des deux côtés d'un revêtement antireflet et caractérisé par une très faible réflectance de la lumière visible et une transmittance de la lumière visible élevée. Le côté air est revêtu par un procédé de dépôt chimique en phase vapeur (CVD) et le côté étain est revêtu par un procédé de dépôt physique en phase vapeur (PVD).
EP21823295.7A 2020-12-04 2021-12-03 Effet antireflet amélioré Pending EP4255860A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP20212010 2020-12-04
PCT/EP2021/084221 WO2022117846A1 (fr) 2020-12-04 2021-12-03 Effet antireflet amélioré

Publications (1)

Publication Number Publication Date
EP4255860A1 true EP4255860A1 (fr) 2023-10-11

Family

ID=73726730

Family Applications (1)

Application Number Title Priority Date Filing Date
EP21823295.7A Pending EP4255860A1 (fr) 2020-12-04 2021-12-03 Effet antireflet amélioré

Country Status (3)

Country Link
EP (1) EP4255860A1 (fr)
CN (1) CN116745249A (fr)
WO (1) WO2022117846A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2025012228A1 (fr) * 2023-07-13 2025-01-16 Agc Glass Europe Verre revêtu résistant à la corrosion

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0313029D0 (en) * 2003-06-06 2003-07-09 Pilkington Plc Coated glass
FR2869897B1 (fr) * 2004-05-10 2006-10-27 Saint Gobain Substrat a revetement photocatalytique
FR2898295B1 (fr) * 2006-03-10 2013-08-09 Saint Gobain Substrat transparent antireflet presentant une couleur neutre en reflexion
US20070236798A1 (en) 2006-04-05 2007-10-11 Shelestak Larry J Antireflective coating and substrates coated therewith
SG173911A1 (en) 2009-03-18 2011-09-29 Agc Flat Glass Na Inc Thin film coating and method of making the same
CN117486501A (zh) 2014-10-31 2024-02-02 皮尔金顿集团有限公司 减反射的涂覆的玻璃制品
JP6657872B2 (ja) 2015-12-03 2020-03-04 Ａｇｃ株式会社 反射防止膜付きガラス板
GB201910988D0 (en) * 2019-08-01 2019-09-18 Pilkington Group Ltd Touchenable coated substrate

Also Published As

Publication number Publication date
WO2022117846A1 (fr) 2022-06-09
CN116745249A (zh) 2023-09-12

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