EP3016916A2 - Substrat verrier revetu d'un empilement a reflexion diffusante et transmission speculaire - Google Patents
Substrat verrier revetu d'un empilement a reflexion diffusante et transmission speculaireInfo
- Publication number
- EP3016916A2 EP3016916A2 EP14790126.8A EP14790126A EP3016916A2 EP 3016916 A2 EP3016916 A2 EP 3016916A2 EP 14790126 A EP14790126 A EP 14790126A EP 3016916 A2 EP3016916 A2 EP 3016916A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- thickness
- layer
- substrate according
- stack
- silicon nitride
- 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.)
- Ceased
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
- C03C17/3429—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 at least one of the coatings being a non-oxide coating
- C03C17/3435—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 at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
-
- 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
- C03C17/36—Surface 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
- C03C17/3602—Surface 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
- C03C17/3626—Surface 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
-
- 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
- C03C2218/32—After-treatment
- C03C2218/328—Partly or completely removing a coating
Definitions
- the present invention relates to thin functional layers in particular deposited by reduced pressure processes such as cathode sputtering, especially magnetron assisted, on glass, for the automobile or building.
- the aim of the present invention is to provide thin layers of easy, reproducible and homogeneous preparation and implementation in their diffusive reflection and specular transmission properties, and more able to coexist with other functionalities currently offered on products.
- glassmakers such as low-emissivity, solar control, hydrophobia, etc.
- the invention which, accordingly, relates to a non-rough glass substrate coated with a stack of thin layers, characterized in that said stack ends with a layer of mixed zinc oxide and tin (sometimes called SnZnO x in the following) with a thickness of between 15 and 60 nm, then with a layer of silicon nitride (Si 3 N 4 ) with a thickness of between 20 and 100 nm, peeled from place to place of said mixed oxide layer so as to form delamination blisters of size between 1 and 20 ⁇ .
- a layer of mixed zinc oxide and tin sometimes called SnZnO x in the following
- Si 3 N 4 silicon nitride
- the fact that the stack ends with the two characteristic layers does not exclude the presence of a thin additional layer just above the silicon nitride layer, for example a thin layer hydrophilic or hydrophobic.
- optical effect produced is therefore substantially equivalent to that described for the layers deposited on Satinovo® mentioned above, but the embodiment makes it possible to very significantly reduce the costs by eliminating the planarization and laminated steps.
- Another advantage is that of depositing other functional layers below the SnZnOx layer so as to combine a reflective diffusing appearance with properties such as low emissivity, as well as being able to use omnidirectional antireflective stacks. by diffusion. It is possible to vary the thickness of the SnZnO x and Si 3 N 4 layers within a reasonable limit so as to adjust the color in the most appropriate range for a given application.
- the thickness of said mixed oxide layer is at least 20 nm
- the thickness of said mixed oxide layer is at most equal to 50 nm
- the thickness of said silicon nitride layer is at least 40 nm
- the thickness of said silicon nitride layer is at most equal to 60 nm;
- said stack is low-emissive (in English: low-e); this property is provided by the stack underlying said mixed oxide layer;
- said stack is antireflective; the antireflection is omnidirectional due to the reflective diffusing nature of the blistered silicon nitride layer, but the omnidirectional antireflexion can be improved by arranging a stack of appropriate layers under said mixed oxide layer;
- said stack has the solar control property; this property is provided by the stack underlying said mixed oxide layer;
- said stack is hydrophilic or hydrophobic; this property is provided by a functional layer deposited on top of said silicon nitride layer.
- the subject of the invention is also a process for manufacturing the substrate described above, characterized in that it comprises the operations consisting in
- sputtering in particular magneto-assisted sputtering, onto a non-rough glass substrate coated or not with at least one thin layer, a zinc and tin mixed oxide layer whose oxygen content is lower than that of completely saturating the oxidation process of these two metals at once (which is often described as substoichiometry), and thickness of between 15 and 60 nm, then a layer of silicon nitride with a thickness of between 20 and 100 nm and having an intrinsic compressive stress of at least 1 GPa, then at
- the oxygen sub-stoichiometry is obviously obtained by the proportion or flow rate used in the oxygen deposition process.
- the high compressive intrinsic stress is obtained by the total pressure of the gases in the deposition chamber and the proportion of nitrogen N 2 on the total of these gases.
- the minimum compressive intrinsic stress of 1 GPa is necessary for the formation of blisters of size and aspect ratio adapted to provide the desired optical function. If the intrinsic compressive stress is too low, blistering does not occur.
- the thermal cycle of this process is calibrated so as to cause segregation of the tin and zinc phases in the mixed oxide, which has the effect of destabilizing the SnZnOx-Si 3 N 4 interface and of inducing the formation of delamination blisters.
- micron size (1 -20 ⁇ ) on the upper layer of Si 3 N 4 which relaxes its highly compressive stress.
- the defects constituted by these blisters are at the origin of a diffusing aspect in reflection while maintaining a transmission largely free of blur (absence quantifiable by a measure of clarity> 93% on which we return in the continuation).
- the thermal cycle, the degree of oxidation of SnZnO x and the stress level of Si 3 N 4 make it possible to control the size of diffusing blisters, which could be used to generate various diffusing visual aspects.
- the layer having to undergo an intense thermal process to generate the diffusing effect it is possible to use it for bending or tempering the glass on which it is deposited, which opens the possibility of uses in the automobile.
- said silicon nitride layer is intended to be oriented towards the outside of a building or a transport vehicle, especially as a transparent automotive roof, glass facade or lighter; from the outside, this substrate may for example have a similar appearance to that of a metallized body, or adapted to that of the building;
- said silicon nitride layer is intended to be oriented towards the interior of a building or a transport vehicle, especially as a low-emission automotive roof antireflective, antireflective windshield or low-emission building glazing;
- the operating conditions are recorded in the following table.
- the layer SnZnO x is substoichiometric in oxygen, in fact a prior calibration shows that the films deposited with 17 sccm of oxygen and are transparent, indicating that the oxidation reactions of Sn and Zn in the plasma are saturated and there are no more unoxidized metallic species, whereas those deposited with less than 17 sccm of oxygen in the plasma give rise to significant absorptions of light, absorptions which correspond to the presence of unoxidized metallic species at the same time. within the layer.
- the intrinsic compressive stress of the Si 3 N 4 layer measured by mechanical profilometry with the DekTak apparatus from Veeco, is 1.1 GPa.
- the whole is subjected to annealing at 650 ° C for 12 minutes in a radiative oven without forced convection of the manufacturer Nabertherm.
- the low-emissive stack thus obtained is diffusing in reflection.
- the perception of a clear image through the glazing is related to the lack of diffusion of the light passing through the glazing.
- This sharpness can be quantified using the parameter called clarity, measurable using specialized devices such as the Hazegard + manufactured by BYK-Gardner.
- the Hazegard + manufactured by BYK-Gardner.
- the result of the measurement is 98.5% indicating a specular transmission.
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
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1356433A FR3008088B1 (fr) | 2013-07-02 | 2013-07-02 | Substrat verrier revetu d'un empilement a reflexion diffusante et transmission speculaire |
PCT/FR2014/051686 WO2015001248A2 (fr) | 2013-07-02 | 2014-07-01 | Substrat verrier revetu d'un empilement a reflexion diffusante et transmission speculaire |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3016916A2 true EP3016916A2 (fr) | 2016-05-11 |
Family
ID=49510266
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP14790126.8A Ceased EP3016916A2 (fr) | 2013-07-02 | 2014-07-01 | Substrat verrier revetu d'un empilement a reflexion diffusante et transmission speculaire |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP3016916A2 (fr) |
FR (1) | FR3008088B1 (fr) |
WO (1) | WO2015001248A2 (fr) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012110823A1 (fr) * | 2011-02-17 | 2012-08-23 | Pilkington Group Limited | Carreau de verre à couche pouvant être traité thermiquement |
WO2013083827A1 (fr) * | 2011-12-08 | 2013-06-13 | Von Ardenne Anlagentechnik Gmbh | Système stratifié de couleur stable, réfléchissant les ir et transparent et son procédé de fabrication, unité de verre |
WO2014191472A2 (fr) * | 2013-05-30 | 2014-12-04 | Agc Glass Europe | Vitrage à faible émissivité |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006067102A2 (fr) * | 2004-12-21 | 2006-06-29 | Glaverbel | Feuille de verre portant un empilage multi-couches |
GB0823501D0 (en) * | 2008-12-24 | 2009-01-28 | Pilkington Group Ltd | Heat treatable coated glass pane |
FR2971060B1 (fr) | 2011-01-31 | 2013-08-09 | Saint Gobain | Element transparent a reflexion diffuse |
-
2013
- 2013-07-02 FR FR1356433A patent/FR3008088B1/fr not_active Expired - Fee Related
-
2014
- 2014-07-01 EP EP14790126.8A patent/EP3016916A2/fr not_active Ceased
- 2014-07-01 WO PCT/FR2014/051686 patent/WO2015001248A2/fr active Application Filing
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012110823A1 (fr) * | 2011-02-17 | 2012-08-23 | Pilkington Group Limited | Carreau de verre à couche pouvant être traité thermiquement |
WO2013083827A1 (fr) * | 2011-12-08 | 2013-06-13 | Von Ardenne Anlagentechnik Gmbh | Système stratifié de couleur stable, réfléchissant les ir et transparent et son procédé de fabrication, unité de verre |
WO2014191472A2 (fr) * | 2013-05-30 | 2014-12-04 | Agc Glass Europe | Vitrage à faible émissivité |
Non-Patent Citations (1)
Title |
---|
See also references of WO2015001248A2 * |
Also Published As
Publication number | Publication date |
---|---|
FR3008088B1 (fr) | 2015-07-17 |
WO2015001248A2 (fr) | 2015-01-08 |
FR3008088A1 (fr) | 2015-01-09 |
WO2015001248A3 (fr) | 2015-03-26 |
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