WO2012095380A1 - Solar control glazing - Google Patents

Solar control glazing Download PDF

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Publication number
WO2012095380A1
WO2012095380A1 PCT/EP2012/050218 EP2012050218W WO2012095380A1 WO 2012095380 A1 WO2012095380 A1 WO 2012095380A1 EP 2012050218 W EP2012050218 W EP 2012050218W WO 2012095380 A1 WO2012095380 A1 WO 2012095380A1
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WO
WIPO (PCT)
Prior art keywords
layer
glazing
functional layer
glazing according
thickness
Prior art date
Application number
PCT/EP2012/050218
Other languages
French (fr)
Inventor
Laurent Dusoulier
Original Assignee
Agc Glass Europe
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
Priority to EP11150586 priority Critical
Priority to EP11150586.3 priority
Application filed by Agc Glass Europe filed Critical Agc Glass Europe
Publication of WO2012095380A1 publication Critical patent/WO2012095380A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10009Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin characterized by the number, the constitution or treatment of glass sheets
    • B32B17/10036Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheet
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10165Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin particular functional features of the laminated glazing
    • B32B17/10174Coatings of a metallic or dielectric material on a constituent layer of glass or polymer
    • B32B17/1022Metallic coatings
    • B32B17/10229Metallic layers sandwiched by dielectric layers
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3626Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer one layer at least containing a nitride, oxynitride, boronitride or carbonitride
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3649Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer made of metals other than silver
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3657Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having optical properties
    • C03C17/366Low-emissivity or solar control coatings
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3681Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating being used in glazing, e.g. windows or windscreens
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/78Coatings specially designed to be durable, e.g. scratch-resistant

Abstract

The present invention relates to solar control glazings comprising on at least one of the faces of a glass substrate a system of layers comprising at least one infrared-reflecting functional layer and dielectric layers surrounding the infrared-reflecting layer, the infrared-reflecting layer being a metallic layer of tungsten, the system comprising, between the substrate and the functional layer, at least one layer of aluminium nitride or of silicon nitride, and a layer of silicon nitride on top of the functional layer.

Description

solar control glazing

The present invention relates to solar control glazing consisting of a glass substrate carrying a system of thin layers, at least one thin layer providing these solar control properties. A functional layer associated dielectric layers which function in particular to adjust the reflective properties, coloring and protection against mechanical or chemical alterations of the glazing properties. The glazing according to the invention are intended to fill the buildings such as motor vehicles. According to these uses certain required properties may differ as explained below.

The functionality of solar control glass are multiple. For automotive concerning, in particular passenger compartment warming prevention exposed to solar radiation when it is sufficiently intense, while maintaining an appropriate light transmission. In other words the energy transmission of the glazing, TE should be as low as possible while maintaining a light transmission TL adequate. The glass must have a ratio TL / TE as high as possible. This ratio is designated as constituting the selectivity of the glazing.

The considered energy transmission comprises both the direct transmission. It also includes the energy re-emitted towards the passenger compartment after absorption by the substrate and the layer system.

The particular car windows must also participate in the establishment of temperature control conditions in winter time avoiding the energy loss to the outside of the cockpit. The glazing must also exhibit low- emissive properties. They oppose the issuance of energetic radiation from the cockpit. In the smooth ÉTAB nt of these properties, automotive glazing are subject to rules that set minimum light transmission guaranteeing adequate vision through these windows. The windshield, and to a lesser hovel side windows at the driver must have a high transmission.

The invention relates to the windows where the light transmission is not subject to the choice of manufacturers and their customers. These cover glass surfaces increasingly important, particularly with regard to glass roofs, but also the appropriate glasses and rear side windows.

The light transmission of the glazing in question may be limited to less than 20% and even less, in particular as regards the roof. But if the characteristics of these glasses are relatively less stringent at least with regard to their light transmission, the other properties do not offer the same facilities.

glazing for buildings significant feature is the ability to produce glass that could withstand heat treatments without their particular color in reflection is changed significantly. The goal is to have windows side by side heat-treated and others that have not been without color differences are obvious.

In the following description, the optical properties are defined for the substrate glass which is glass "float" ordinary clear 4mm thick. The choice of substrate of course works on these properties. For the ordinary clear glass light transmission under 4mm, in the absence of layer is approximately 90% and reflection 8%. The measurements are made according to EN 410.

The presence of my system layers can cause color problems. Most often manufacturers require that windows offer both transmitted and reflected as neutral a color as possible and therefore gray appearance. slightly green or blue colorations are possible. The layer systems, in particular the dielectric layers flanking the functional layers are chosen, natures, indices and thicknesses, in particular to control these colorations.

The automotive glazing, in theory can be many to give them a better ownership of particular thermal insulation. In fact these achievements are exceptional. The vast majority of these windows consists of single glazing is monolithic or laminated. In both cases, the emissive bas character is expressed properly, the ys te medecouchesest necessarily on a face that is not immune to mechanical and chemical stresses. The systems in question must therefore have very good resistance to these possible attacks.

In practice to limit the risk of tampering, the layer systems are normally on the side of the window facing the passenger. But even in this position they must offer a very good mechanical strength.

layer systems according to the invention still have to lend to formatted glazing. Those used in vehicles are particularly subject to heat treatment during forming, especially the bending of glass sheets, or during quenching for imparting particular their enhanced mechanical properties. The layers used in the invention must withstand these treatments without their properties are degraded. Treatments of this type require temperatures that exceed 600 ° C during ten minutes. Subject to these temperatures the layers should retain their qualities. Defects often caused during such treatments are the appearance of iridescence, change in light transmission, and especially the formation of a more or less sail. In practice glazing subjected to these treatments must not develop a veil that would be greater than 1% or even greater than 0.5%. In applications requiring extensive glazing to have to f Porte transm iss ion lum ine use, the c ho ix s couc he s functional requires that they be particularly transparent. The most common is to select one or more metal layers of very small thickness. One or more silver layers disposed between dielectric layers that (the) protect and minimize both reflection and adjust neutrality. The layer systems obtained in the set have to limit some particular mechanical fragility, even in the presence of specific protective layers.

For panes which do not require high light transmission, and possibly even where transmission must remain low, the choice of layer systems offer greater diversity.

The prior art provides glazing comprising metallic functional layers or metal alloys, nitrides or oxy-nitrides of various metals and in particular NiCr, Mo, W, Ta, Co-Cr, Al, Nb, Zr. To allow these metal layers in particular have good mechanical strength, it is also proposed to provide dielectric layers known to be relatively hard. In this area the most common layers are those of silica, SiO 2, and silicon nitride, Si 3 N 4.

Earlier proposals meet at least part of the requirements of the intended use of glazing according to the invention. It remains the necessities of improvement particularly from the standpoint of strength, but also resistance to thermal treatments.

A proposal of the invention is to form on a glass substrate, a layer system comprising at least the following layers:

- a relatively absorbent layer based on tungsten or tungsten alloyed with one or more metals from the group comprising: Ti, Nb, Zr, Ta, and Cr; - a layer of aluminum nitride or silicon nitride, which layer is located between the glass substrate and the absorber layer to tungsten-based;

- a layer of silicon nitride located above the absorbing layer.

The functional layers preferably are tungsten-based thick enough to limit light transmission but also simultaneously to reduce significantly the energy transmission. The thickness of this layer is preferably between 50 and 600 A and particularly preferably from 100 to 450Â.

The aluminum nitride layers or silicon nitride arranged between the substrate and the functional layer, the functional layer protect against tampering thereof by the diffusion of especially ions substrate in thermal processing operations. In a protective aluminum nitride layers are particularly efficient. These layers co ntr ib ue nt aus if the establishment of the optical properties and in particular the colorimetric characteristics.

Preferably these layers of aluminum nitride or silicon nitride have a thickness between 100 and 500Å, and preferably between 150 and 400A.

The thicknesses of the silicon nitride layers simultaneously used to adjust the level of the glass on the side of the reflection and its coloration in reflection. This thickness also operates on the system's resistance to external attacks, in particular to mechanical attack.

But it should be noted that the resistance does not increase uniformly with the thickness of the layer. If a minimum is required too great an increase is not favorable.

Preferably the silicon nitride layer has a thickness between 900A and 100 and preferably between 200 and 650A. When tungsten is alloyed with one or more other metals thereof are more than 20 atomic% of the whole, and preferably at most 10 atomic%

the layer systems used according to the invention may further comprise additional layers that contribute in particular to the stability of the functional layer and also improving the consistency of this layer. One way of improvement is to deposit on the functional layer and in contact therewith, a thin metallic layer of zirconium, tantalum or niobium. A layer of the same type or different, can also be located under the functional layer and also in contact with this layer.

By using a relatively thin additional metal layer optical properties are substantially unchanged, but the resistance of the assembly, in particular to the heat treatment is further improved. PREFERABLY additional elacouchede has a thickness between 10 and 70A, and particularly preferably from 20 to 50Â.

The presence of additional layers of zirconium, in particular allows preventing the occurrence of defects in the regularity of the layer, defects that take the form of what is referred to as "pin-holes". The reason for the occurrence of these defects is not well understood. It seems related to a reaction of the functional layer during heat treatment bending or toughening type. Whatever the origin of these defects, their presence is particularly detrimental to the aesthetics of glass that they are more absorbent. In this case the defects appear by contrast as so many distinct points of light.

The glazing according to the invention find various applications by adapting their properties by adjusting layers and in particular of their thicknesses.

As an indication, the functional layer controls the light and energy transmission. More functional layer is thick more it absorbs and reflects. For the applications contemplated these layers with the light transmission is relatively reduced. She does not normally exceed 50%, but can be as low as 4% for thicker layers.

The dielectric layers, particularly the top layer including order reflection of the system. In known manner the alternating layers of high and low index refraction, possible to control the reflection. The thickness of the layers is also a factor. Within the limits of the thicknesses indicated above, increasing the thickness of the silicon nitride layer located above the functional layer, reduces the intensity of the reflection from the glass side as the side layer.

For the most common applications, including "automotive" applications, the reflection should be kept relatively low. It is normally below 30% and most usually less than 20% and can be as low as 4%.

A key feature of the glazing according to the invention remains their ability to limit energy transmission. This solar radiation, and consequently of limiting warming space sunny, so as to limit the use of air conditioning means, be it buildings or vehicles. It is also conversely, when the space in question is hotter than the exterior, to avoid excessive heat loss through the glazing.

Protection against solar radiation is quantified by the "solar factor" (FS or g) which corresponds to the value of the actual energy transmitted through the glazing and reemitted that inward after being absorbed by the glazing. The solar factor of the glazing according to the invention is usually not greater than 30% and preferably not more than 20%.

The presence of the layer system according to the invention is also useful for avoiding heat loss. The measurement of this property called emissivity is performed according to EN 12898. A suitable choice of thickness of the layers allows to obtain according to the invention a normal emissivity glazing which is not greater than 0.35 and advantageously less than 0.20.

The colorations of the glazings, whose control depends not only on the nature of the layers but also their combined thicknesses are advantageously maintained relatively neutral. In practice color perception is even less sensitive than the reflections and transmissions are low. Nevertheless it remains favorite to keep the colors as inconspicuous as possible and especially to avoid the reflection stains pulling yellow or red. In the CIELAB system, for illuminant D65 at an angle of 10 °, colorings in question correspond to values ​​a * and b * as close as possible to 0, and especially in the a * that are not positive.

If the light transmission is not very high, some defects are less noticeable. This is the case of the veil ( "haze") that may develop during vigorous heat treatments glazing of the type of the invention. It is still preferable that the glass in question, with or without thermal treatment are virtually no veil, or that it is extremely limited. The choice of the invention layer systems leads to particularly resistant glazings to heat treatment, in particular when these systems include a layer of aluminum nitride between the glass substrate and the functional layer.

In the pratiq ue cho ix of layers my system is lon the invention keeps the sail to values ​​below 1% (corresponding to the percentage of scattered light measured in accordance with ASTM 1003-61 O), and advantageously a value less than 0.5% after a heat treatment which leads the coated glazing at 650 ° C and maintained at that temperature for 10 minutes.

Heat treatments of bending / toughening type, with regard to the optical and especially coloring properties, may also induce more or less significant changes. It is best to minimize these variations so that heat-treated or not the windows have a virtually unchanged appearance.

Traditionally measuring variations is carried out from the coordinates of the CIELAB system. It is expressed by the term denoted ΔΕ expression corresponding to the formula:

ΔΕ = (U * 2 * 2 + Aa + Ab * 2) 1/2

Changes made by the glazing according to the invention during treatment type 650 ° C for 10 minutes remain below 3 and even below 2.

The glazing according to the invention can be part of double glazing in which case the layer system may be disposed in the space between the two glass sheets, which limits the risks of particular mechanical alteration. However one of the significant characteristics of layer systems proposed for the glazing according to the invention is their both mechanical and chemical resistance. This strength is such that they can be used with the layer system exposed without further protection. In the latter case the glazing unit may as well consist of a single sheet of glass, the layer systems are applied on one side of this sheet. It can also be a laminated glazing comprising two sheets of glass, or more, the sheets being joined together by interlayers of thermoplastic material according to the conventional techniques in this field.

In these applications on a single glass layer system is not protected from the environment. Even in the case of laminated glazing, the layers are on an external face so that they can play their role in controlling energy transmission.

When the preferred feature is the bas-emissive nature of the pane, the layer system is preferably arranged on the side facing inside the vehicle or building. This position leads to the reflection of the largest infrared rays. For vehicles this position leads the layer on the side facing the passenger compartment. In this position the layer system resists even better than the stress, especially for fixed glazing (roof, window ...) are relatively limited.

The glazing according to the invention carrying the layer systems are tested in particular for their chemical resistance properties by following the standard test EN1096-2. Is the ss is co mp o rd nt systematically a moisture resistance test (10 days in a climatic chamber) and a chemical resistance test (neutral salt spray for 10 days). In addition the mechanical strength is checked with a wet friction test ( "AWRT" to "automatic wet rub test"). This test is performed with a circular head Teflon coated with a cotton cloth (Adsol ref. 40700004). This head is moved over the layer under a load of 1050g. Cotton is kept moist throughout the test with deionized water. The oscillation frequency is 60 to 90 per minute. Any alterations of the layer are observed.

All samples of the invention successfully pass these tests.

The following examples of panes according to the invention are given by way of illustration. These windows are for preparing roofs for motor vehicles. In these applications the windows are used either monolithic or in laminated form. In all cases the layers are arranged on the side facing the passenger compartment.

The tests are conducted on sheets of clear glass 3,85mm thick for single glazing and 2.1mm thick for those used in the composition of laminated glazing.

The sheets on which the layers are deposited can also be colored glasses. It is also possible to combine the glass sheets used, some are colored some not, or in the case of laminated glazing interlayers using either colorless or colored. The combinations of these elements possible in particular to modify the colorful aspects of glazing concerned. Choosing a colored glass can not only change the transmission but also appropriate energy absorption. The colored interlayer presence mainly affects the color appearance of the glazing.

Laminated glazing may also have the usual additional features in this area. Especially glazings can be made so as to provide a limitation of noise pollution. For this purpose, the most common, without increasing the thickness of the glasses concerned, is to use laminated structures including interlayers having a larger plasticity than traditional laminated.

Examples of glazing according to the invention are given below.

The functional and dielectric layers are applied by a sputtering technique ( "sputtering") under conventional conditions for this type of technique.

The dielectric layers of aluminum nitride, or silicon are produced from metallic targets in an atmosphere consisting of a mixture of argon (30-70%) and nitrogen (70-30%) at a total pressure of 4mTorr (0,53Pa). Optionally, a small amount of oxygen may be introduced during deposition. The tungsten layer as any layers of zirconium are deposited from metal cathodes in single argon atmosphere.

The following systems are produced. The layers are in the order, from left to right, starting from the glass. The approximate thicknesses are expressed in angstroms.

The samples are determined, the light transmission TL and the reflection side of the layers with the colorimetric coordinates L *, a *, b *. The angle at which these measurements are made is 2 ° to the transmission and reflection, and 10 ° for the colorimetric coordinates, and the illuminant is D65.

The samples were also subjected to a heat treatment comprising holding at 670 ° C for 7 minutes. The same parameters are given in lower line for these samples processed. Changes in transmission, reflection and ΔΕ are also given in the following table. In this table the AIN and SiN numerals denote nitrides without representing a chemical formula, provided that the products obtained are not necessarily strictly stoichiometric, but are those obtained in the deposition conditions indicated and are neighbors stoichiometric products.

Figure imgf000013_0001

The properties of these examples are summarized in the following table:

Transmission reflection layer side

TL L * a * b * ATL ΔΕ Rc L * a * b * ARc ΔΕ

13.5 43.5 -0.1 -0.3 43.6 71 8 0.3 3.5

13.6 43.7 -0.1 -0.1 0.1 0.2 43.4 71, 7 -0.3 3.2 -0.2 0.4

25.6 57.7 -0.1 -0.1 32.2 64.3 -0.5 0.4

25.8 57.8 -0.1 0.3 0.2 0.3 32.6 63.9 -0.5 0.4 -0.6 0.5

26.8 58.8 0.0 1 1 29.8 61 5 0.4 1 0

27.1 56.9 0.0 1 2 0.3 0.3 29.3 61 -0.4 0 1 0 -0.5 0.5

56.9 0.0 24.8 1: 9 36.1 66.7 -0.7 -2.6

25.5 57.2 0.0 2.0 0.4 0.4 35.3 66.1 -0.6 -2.5 -0.8 0.6

25.8 57.8 -0.5 0.3 29.9 61 5 2.2 -0.1

-0.2 63.4 32.2 1 6 6.3 5.7 26.9 58.9 -0.4 0.4 -3.0 3.2

-0.5 25.6 57.6 1 1 34.5 65.4 -0.3 -1, 6

35.0 65.7 -0.2 2.0 9.5 8.2 30.4 62.1 -0.7 -2.9 -4.1 3.6 In the examples of layer systems, those the first dielectric is nitride "aluminum (examples 1-4) changes in transmittance, reflectance and AE are less than those observed with the system (examples 5-6) having a lower dielectric layer of silicon nitride. before glazing and after thermal treatment of the first four tests are less sensitive to these treatments.

The emissivity of the samples 1 and 3 amounted respectively to 0, 197 and 0.374. This emissivity is a function of the thickness of the functional layer based on tungsten, and decreases as the thickness of this layer increases.

The following tests are carried out on a layer system comprising in addition on both sides of the functional layer of tungsten, a thin layer of zirconia. The systems are:

Figure imgf000014_0001

The presence of additional layers of zirconium improves the stability of the absorbent layer of tungsten. The properties of the samples are determined as above and the results given in the table below: Transmission Reflection layers side

TL L * a * b * ATL ΔΕ Rc L * a * b * ARc ΔΕ

10.5 38.8 0.5 -1 0 71 43.9 9 0.1 8.9

9.9 37.7 -0.4 -0.7 -0.6 1, 1 44.2 72.1 0.2 8.3 0.3 0.7

3.1 20.1 0.6 4.9 37.7 67.4 2.3 14.7

2.9 19.3 0.6 4.5 -0.2 0.9 39.1 68.4 2.1 13.8 1, 3 1, 4

16.7 47.9 0.5 12.7 13.1 42.9 -0.2 -33.4

17.1 48.4 -ο, ι 11 4 0.4 1 12.8 42.5 5 1, 9 -34.6 -0.2 2.5

Before and after thermal treatment (640 ° C for 5 minutes), the emissivity and solar factor of the previous samples are as follows:

Figure imgf000015_0001

Other samples are products whose composition is as follows:

Figure imgf000015_0002

Example 14 is carried out on a strongly absorbing gray glass which has a thickness of 4mm under a transmission of 17%. Unlike previous samples Te glass thickness is 2.1 mm in this case. Compared to other samples the light transmission is reduced accordingly. This type of glass is particularly intended for the use of automobile roofs for which the transmission is still very small.

The properties of the samples after annealing at 640 ° C for lOmn are as follows:

Transmission reflection layer side

TL L * a * b * Rc L * a * b *

10 16.1 47.0 -2.8 2.2 11 8 40.5 15.6 5.7

11 20.7 52.5 -2.5 6.2 7.4 33.4 19.1 -24.5

12 20.8 52.5 -2.2 8.7 7.2 33.6 15.0 -34.5

13 20.2 51, 7 -1, 0 11, 3 8,8 7,7 -38.4 37.3

14 8.4 34.5 -0.9 9.0 10.9 41, 1 2.8 -39, 1

Claims

REVEN dications 1. Solar control glazing comprising at least one of the faces of a glass substrate a layer system comprising at least one functional layer reflecting infrared and dielectric layers flanking the infrared reflecting layer, characterized in that the infrared reflective layer is a metal layer of tungsten or tungsten alloy with at least one metal of the group comprising: Ti, Nb, Zr, Ta, Cr, the system comprising between the substrate and the functional layer at least one layer of nitride or aluminum silicon nitride, and a layer of silicon nitride above the functional layer.
2. Glazing according to claim 1 wherein a metallic layer of zirconium, tantalum or niobium is disposed above the functional layer and directly in contact with the functional layer.
3. Glazing according to claim 2 wherein a metal layer of zirconium, tantalum or niobium is disposed under the functional layer and directly in contact with the functional layer.
4. Glazing according to one of the preceding claims wherein the thickness of the functional layer has a thickness of 50 to 600A, preferably from 100 to 450Â.
5. Glazing according to claim 4 wherein the thickness of the silicon nitride layer placed in the system above the functional layer has a thickness of 100 to 900A, preferably from 200 to 650A.
6. Glazing according to claim 4 or claim 5 wherein the aluminum nitride layer or silicon nitride between the substrate and the functional layer has a thickness of 100 to 500Å, and preferably from 150 to 400A.
7. Glazing according to claim 2 or claim 3 wherein the layer of zirconium, tantalum or niobium has a thickness of 10 to 70A, and preferably from 20 to 50Â.
8. Glazing according to one of the preceding claims wherein the thickness of the functional layer is selected so that the light transmission for a glass consisting of clear 4 mm thick substrate is at most equal to 50%.
9. Glazing according to claim 8 wherein the thickness of the dielectric layers is chosen so that the glass side or side reflection layers, is not greater than 30% and preferably not greater than 20%.
10. Glazing according to claim 8 or claim 9 wherein the thicknesses of the layers are such that the solar factor is not greater than 30% and preferably not more than 20%.
January 1. Glazing according to claim 10 wherein the normal emissivity not greater than 0.35 and preferably have greater than 0.20.
12. Glazing according to one of claims 4 to 7, the color variation:
ΔΕ = (U * 2 * 2 + Aa + Ab * 2) 1/2
when subjected to a temperature of 650 ° C for 10 minutes, is not greater than 3 and preferably not greater than 2.
13. Motor vehicle roof comprising at least one glazing according to one of the preceding claims, wherein the layer system is on the exposed face towards the passenger compartment.
14. A roof according to claim 13, consisting of a laminated assembly comprising two glass sheets joined by means of a thermoplastic interlayer, the glazing having the functional layer system being situated towards the vehicle interior.
PCT/EP2012/050218 2011-01-11 2012-01-09 Solar control glazing WO2012095380A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP11150586 2011-01-11
EP11150586.3 2011-01-11

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
KR1020137020387A KR20140003527A (en) 2011-01-11 2012-01-09 Solar control glazing
EP12700469.5A EP2663537A1 (en) 2011-01-11 2012-01-09 Solar control glazing
JP2013548806A JP2014503461A (en) 2011-01-11 2012-01-09 Solar control plate glass
BR112013017791A BR112013017791A2 (en) 2011-01-11 2012-01-09 glass with solar control
CN201280005226XA CN103391905A (en) 2011-01-11 2012-01-09 Solar control glazing

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WO2012095380A1 true WO2012095380A1 (en) 2012-07-19

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EP (1) EP2663537A1 (en)
JP (1) JP2014503461A (en)
KR (1) KR20140003527A (en)
CN (1) CN103391905A (en)
BR (1) BR112013017791A2 (en)
WO (1) WO2012095380A1 (en)

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JP2016513061A (en) * 2013-02-14 2016-05-12 エージーシー グラス ユーロップ Solar control glazing
WO2014125081A1 (en) * 2013-02-14 2014-08-21 Agc Glass Europe Solar control glazing
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WO2014207171A1 (en) * 2013-06-27 2014-12-31 Agc Glass Europe Solar protection glazing
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JP2017507874A (en) * 2013-12-13 2017-03-23 エージーシー グラス ユーロップAgc Glass Europe Glass of the vehicle roof
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WO2015119490A1 (en) * 2014-02-10 2015-08-13 Vidrio Plano De Mexico, S.A. De C.V. Coating with solar control properties for a glass substrate
WO2016012323A1 (en) 2014-07-25 2016-01-28 Agc Glass Europe Heating glazing unit
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EP2977202A1 (en) 2014-07-25 2016-01-27 AGC Glass Europe Heating glass
EP3106304A1 (en) * 2015-06-19 2016-12-21 AGC Glass Europe Laminated glazing
WO2016202617A1 (en) * 2015-06-19 2016-12-22 Agc Glass Europe Laminated glazing

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KR20140003527A (en) 2014-01-09
BR112013017791A2 (en) 2016-10-11
EP2663537A1 (en) 2013-11-20
CN103391905A (en) 2013-11-13
JP2014503461A (en) 2014-02-13

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