EP4143143A1 - Matériau comportant un empilement a sous-couche dielectrique fine d'oxide a base de zinc et procédé de depôt de ce materiau - Google Patents
Matériau comportant un empilement a sous-couche dielectrique fine d'oxide a base de zinc et procédé de depôt de ce materiauInfo
- Publication number
- EP4143143A1 EP4143143A1 EP21732400.3A EP21732400A EP4143143A1 EP 4143143 A1 EP4143143 A1 EP 4143143A1 EP 21732400 A EP21732400 A EP 21732400A EP 4143143 A1 EP4143143 A1 EP 4143143A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- layer
- zinc
- zno
- dielectric
- functional 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
Links
- 239000011701 zinc Substances 0.000 title claims abstract description 71
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 71
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims description 10
- 238000000151 deposition Methods 0.000 title description 5
- 239000010410 layer Substances 0.000 claims abstract description 107
- 239000002346 layers by function Substances 0.000 claims abstract description 83
- 239000000758 substrate Substances 0.000 claims abstract description 62
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 31
- 239000010936 titanium Substances 0.000 claims abstract description 31
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 180
- 239000011787 zinc oxide Substances 0.000 claims description 86
- 238000000576 coating method Methods 0.000 claims description 46
- 239000011248 coating agent Substances 0.000 claims description 31
- 229910052709 silver Inorganic materials 0.000 claims description 28
- 239000004332 silver Substances 0.000 claims description 28
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 26
- 239000001301 oxygen Substances 0.000 claims description 26
- 229910052710 silicon Inorganic materials 0.000 claims description 26
- 239000010703 silicon Substances 0.000 claims description 26
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 25
- 239000006117 anti-reflective coating Substances 0.000 claims description 22
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 150000004767 nitrides Chemical class 0.000 claims description 18
- 230000005855 radiation Effects 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 17
- 238000011282 treatment Methods 0.000 claims description 15
- 239000012298 atmosphere Substances 0.000 claims description 13
- 239000011521 glass Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 8
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 8
- UVGLBOPDEUYYCS-UHFFFAOYSA-N silicon zirconium Chemical compound [Si].[Zr] UVGLBOPDEUYYCS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910003087 TiOx Inorganic materials 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 22
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 11
- 239000012300 argon atmosphere Substances 0.000 description 9
- 238000013532 laser treatment Methods 0.000 description 8
- 239000002356 single layer Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 230000002745 absorbent Effects 0.000 description 4
- 239000002250 absorbent Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 102200056507 rs104894175 Human genes 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910002065 alloy metal Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
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
- C03C17/36—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
-
- 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
- C03C17/361—Coatings of the type glass/metal/inorganic compound/metal/inorganic compound/other
-
- 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
- C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
-
- 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
- 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
- C03C17/3639—Multilayers containing at least two functional metal layers
-
- 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
- C03C17/3642—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 the multilayer coating containing a metal 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
- 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
- C03C17/3644—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 the metal being silver
-
- 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
- C03C17/3657—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 the multilayer coating having optical properties
- C03C17/366—Low-emissivity or solar control 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
- 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
- C03C17/3681—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 the multilayer coating being used in glazing, e.g. windows or windscreens
-
- 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
- C03C2217/90—Other aspects of coatings
- C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
- C03C2217/944—Layers comprising zinc oxide
Definitions
- MATERIAL CONTAINING A FINE DIELECTRIC ZINC-BASED OXIDE UNDERLAYMENT STACK AND PROCESS FOR DEPOSITING THIS MATERIAL
- the invention relates to a material comprising a glass substrate coated on one side with a stack of thin layers having reflection properties in the infrared and / or solar radiation having at least one metallic functional layer, in particular based on silver or containing metal alloy of silver and at least two antireflection coatings, said antireflection coatings each comprising at least one dielectric layer, said functional layer being placed between the two antireflection coatings.
- the single, or each, metallic functional layer is thus placed between two antireflection coatings each generally comprising several layers which are each made of a dielectric material of the nitride type, and in particular silicon nitride or silicon nitride. aluminum, or oxide. From an optical point of view, the purpose of these coatings which surround the or each metallic functional layer is to "antireflect" this metallic functional layer.
- EP 718 250 It is known from European patent application No. EP 718 250 a previous configuration in which on the one hand a layer based on zinc oxide is located just under and in contact with the metallic functional layer, in the direction of the substrate, then a layer based on silicon nitride under and in contact with this layer based on zinc oxide and in which on the other hand a layer based on zinc oxide is located above, opposite the substrate , then a dielectric layer, for example based on silicon nitride, is located on and in contact with this layer based on zinc oxide.
- this radiation treatment of the stack does not structurally modify the substrate.
- the invention is based on the discovery of a particular configuration of layers surrounding a metallic functional layer which makes it possible to reduce the resistance per square at the same functional layer thickness, or even to reduce the functional layer thickness in order to obtain improved thermal properties, and this after a heat treatment of the material or a radiation treatment of the stack according to known techniques.
- An aim of the invention is thus to achieve the development of a new type of stack of layers with one or more functional layers, a stack which has, after heat treatment of the material or treatment of the stack with radiation, a low resistance per square (and therefore low emissivity), high light transmission, as well as uniformity of appearance, both in transmission and in reflection.
- the invention thus provides, in its broadest sense, a material according to claim 1.
- This material comprises a substrate coated on one side of a stack of thin layers having reflection properties in the infrared and / or solar radiation having at least one metallic functional layer, in particular based on silver or metallic alloy containing silver and at least two antireflection coatings, said antireflection coatings each comprising at least one dielectric layer, said functional layer being arranged between the two anti-reflective coatings, said material being remarkable:
- said anti-reflective coating located under said functional layer towards said substrate comprises:
- a zinc-based oxide sublayer, ZnO which is located under and in contact with said functional layer, with a physical thickness of said zinc-based ZnO oxide sublayer which is between 0, 3 and 4.4 nm, or even between 0.3 and 2.9 nm, or even between 0.5 and 2.4 nm, or even between 1.0 and 3.0 nm, or even between 1.5 and 2.4 nm ; and
- titanium-based oxide dielectric sublayer TiO x , which is located under and in contact with said zinc-based oxide sublayer ZnO, with a physical thickness of said oxide sublayer based on titanium TiOx which is between 5.0 and 50.0 nm, or even between 5.0 and 40.0 nm, or even between 12.0 and 33.0 nm;
- said anti-reflective coating located above said functional layer opposite said substrate comprises:
- a zinc-based oxide overlayer ZnO, which is located on and in contact with said functional layer, with a physical thickness of said zinc-based oxide ZnO overlayer which is between 2.0 and 10, 0 nm, or even between 2.0 and 8.0 nm, or even between 2.5 and 5.4 nm;
- Said zinc-based oxide sublayer is the very thin layer mentioned above: it has a thickness corresponding to a minimum of a mono-molecular layer of ZniOi and a maximum thickness of only a few nanometers.
- the zinc oxide is neither substoichiometric nor superstoichiometric, in order to have the lowest possible absorption coefficient in the visible range.
- Said zinc-based oxide sublayer, ZnO which is located under and in contact with said functional layer, may in particular have a physical thickness which is between 0.3 and 4.9 nm, or even between 0, 3 and 3.9 nm, or even between 0.3 and 2.9 nm; it may also have a physical thickness which is between 1.0 and 4.9 nm, or even between 1.0 and 3.9 nm, or even between 1.0 and 2.9 nm.
- Said titanium-based oxide dielectric sublayer, TiO x may have a physical thickness which is between 5.0 and 30.0 nm, or even between 5.0 and 20.0 nm, or even between 7.0 and 17.0 nm, or else 10.0 and 50.0 nm, or even between 10.0 and 40.0 nm, or even between 15.0 and 33.0 nm.
- Said stack may comprise a single metallic functional layer or may comprise two metallic functional layers, or three metallic functional layers, or four metallic functional layers; the metallic functional layers here are continuous layers.
- the stack comprises several metallic functional layers
- at least the first functional layer, closest to the substrate, and more preferably each functional layer is according to the previous indication, with:
- said anti-reflective coating located under and in contact with each functional layer which comprises, in the direction of said substrate:
- a zinc-based oxide sublayer, ZnO which is located under and in contact with said functional layer, with a physical thickness of said zinc-based ZnO oxide sublayer which is between 0, 3 and 4.4 nm, or even between 0.3 and 2.9 nm, or even between 0.5 and 2.4 nm, or even between 1.0 and 3.0 nm, or even between 1.5 and 2.4 nm ; and
- titanium-based oxide dielectric sublayer TiO x which is located under and in contact with said zinc-based oxide sublayer, ZnO, with a physical thickness of said titanium-based oxide TiO x dielectric sublayer which is between 5.0 and 50.0 nm, or even between 5.0 and 40.0 nm, or even between 12.0 and 33 , 0 nm;
- a zinc-based oxide overlayer ZnO, which is located on and in contact with said functional layer, with a physical thickness of said zinc-based oxide ZnO overlayer which is between 2.0 and 10, 0 nm, or even between 2.0 and 8.0 nm, or even between 2.5 and 5.4 nm; and - a dielectric overlayer which is located on said zinc based oxide overlayer ZnO, and preferably a silicon nitride dielectric overlayer, SÎ3N4.
- Said metallic functional layer, or each metallic functional preferably has a physical thickness which is between 6.5 and 22.0 nm, or even between 9.0 and 16.0 nm, or even between 9.5 and 12.4 nm .
- a metallic functional layer preferably comprises, at least 50% in atomic percentage, at least one of the metals chosen from the list: Ag, Au, Cu, Pt; one, more, or each metallic functional layer is preferably silver.
- metal layer within the meaning of the present invention, it should be understood that the layer does not contain oxygen or nitrogen.
- dielectric layer within the meaning of the present invention, it should be understood that from the point of view of its nature, the layer is “non-metallic”, that is to say that it comprises oxygen or nitrogen, or both. In the context of the invention, this term means that the material of this layer has an n / k ratio over the entire visible wavelength range (from 380 nm to 780 nm) equal to or greater than 5.
- n denotes the real refractive index of the material at a given wavelength and the coefficient k represents the imaginary part of the refractive index at a given wavelength, or absorption coefficient; the ratio n / k being calculated at a given wavelength identical for n and for k.
- the term “in contact” means that no layer is interposed between the two layers considered.
- the term “based on” means that for the composition of this layer, the reactive elements oxygen or nitrogen, or both if they are both present, are not considered and the element is not reactive (eg silicon or zinc or titanium) which is indicated as constituting the base, is present at more than 85 atomic% of the total of the unreactive elements in the layer.
- This expression thus includes what is commonly referred to in the technique under consideration as "doping, while the doping element, or each doping element, may be present in an amount of up to 10 atomic%, but without the total being dopant does not exceed 15 atomic% of the non-reactive elements.
- This notion of "based on also covers a complete composition,” consisting of the reactive element or of the reactive elements, that is to say "en.
- said antireflection coating located under said functional layer and / or said antireflection coating located above said functional layer does not include any layer in the metallic state. Indeed, it is not desired that such a layer can react, and in particular oxidize, during the treatment.
- said antireflection coating located under said functional layer and / or said antireflection coating located above said functional layer does not include any absorbent layer;
- absorbent layer within the meaning of the present invention, it should be understood that the layer is a material exhibiting an average k coefficient, over the entire visible wavelength range (from 380 nm to 780 nm), greater than 0, 5 and exhibiting an electrical resistivity in the bulk state (as known in the literature) which is greater than 10 5 Q.cm. In fact, it is not desirable for such a layer to be able to react, and in particular to oxidize, during the treatment.
- said titanium-based oxide dielectric sublayer is a titanium-based oxide dielectric sublayer
- TiO x does not contain nitrogen. It can be in T1 ⁇ 2.
- said antireflection coating comprises a primary dielectric sub-layer of silicon-based nitride S1 3 N 4 which is located under and in contact with said sub-layer of titanium-based oxide TiO x , with a physical thickness of said primary dielectric sub-layer of silicon-based nitride S13N4 which is between 5.0 and 50.0 nm, or even between 10.0 and 40.0 nm, or even between 15.0 and 20.0 nm .
- said antireflection coating comprises a primary dielectric sublayer of silicon-zirconium nitride Si x N y Zrz which is located under and in contact with said sublayer of titanium-based oxide TiO x , with a physical thickness of said primary dielectric sub-layer of silicon-zirconium nitride Si x N y Zrz which is between 5.0 and 50.0 nm, or even between 10.0 and 40.0 nm, or even between 15.0 and 20.0 nm.
- Said zinc-based oxide underlayer ZnO and / or said zinc-based oxide ZnO overlay is preferably made of zinc oxide ZnO doped with aluminum, that is to say that it does not contain any element other than Zn, Al and O.
- said antireflection coating located under said functional layer further comprises a dielectric intermediate sub-layer located between said dielectric sub-layer of silicon-based nitride S13N4 and said face, this dielectric intermediate sub-layer being oxidized (c 'that is to say comprising oxygen) and preferably comprising a mixed oxide of zinc and tin.
- said antireflection coating located above said functional layer further comprises a dielectric intermediate overlayer situated between said zinc-based oxide overlayer ZnO and said dielectric overlayer, this dielectric intermediate overlayer being oxidized and preferably comprising a titanium oxide.
- the present invention also relates to a multiple glazing comprising a material according to the invention, and at least one other substrate, the substrates being held together by a frame structure, said glazing forming a separation between an exterior space and an interior space. , in which at least one interleaving gas blade is disposed between the two substrates.
- Each substrate can be clear or colored. At least one of the substrates, in particular, can be made of glass colored in the mass. The choice of the type of coloring will depend on the level of light transmission and / or the colorimetric appearance desired for the glazing once its manufacture has been completed.
- a substrate of the glazing, in particular the substrate carrying the stack can be bent and / or tempered after the deposition of the stack. It is preferable in a multiple glazing configuration that the stack is arranged so as to be turned towards the side of the interlayer gas knife.
- the glazing can also be a triple glazing consisting of three sheets of glass separated two by two by a gas layer.
- the substrate carrying the stack may be on face 2 and / or on face 5, when it is considered that the incident direction of sunlight passes through the faces in increasing order of their number. .
- the present invention also relates to a process for obtaining or manufacturing a material comprising a glass substrate coated on one face with a stack of thin layers with reflection properties in the infrared and / or in the infrared.
- solar radiation comprising at least one metallic functional layer, in particular based on silver or a metal alloy containing silver and two anti-reflection coatings, said anti-reflection coatings each comprising at least one dielectric layer, said functional layer being arranged between the two anti-reflective coatings, said method comprising the following steps, in order:
- the deposition on one face of said substrate of a stack of thin layers with reflection properties in the infrared and / or in solar radiation comprising at least one functional metallic layer, in particular based on silver or on a metallic alloy containing silver and at least two anti-reflective coatings, in order to form a material according to the invention, then
- Said treatment is preferably carried out in an atmosphere not comprising oxygen.
- Said ZnO zinc-based oxide sublayer is preferably deposited from a ceramic target comprising ZnO and in an atmosphere not comprising oxygen or comprising at most 10.0% oxygen.
- FIG. 1 illustrates a structure of a functional monolayer stack according to the invention, the functional layer being deposited directly on an oxide sublayer based on zinc ZnO and directly under an oxide sublayer based on zinc ZnO , the stack being illustrated during processing using a radiation producing source;
- FIG. 2 illustrates a structure of a functional bilayer stack according to the invention, each functional layer being deposited directly on an oxide sublayer based on zinc ZnO and directly under an oxide sublayer based on zinc ZnO , the stack being illustrated during processing using a radiation producing source;
- FIG. 3 illustrates double glazing incorporating a stack according to the invention
- FIG. 4 illustrates a triple glazing incorporating two stacks according to the invention
- - [Fig. 5] and [Fig. 6] illustrate the resistance per square R, in ohms per square, of the stacks of a first series of examples, respectively before and after a laser treatment, as a function of the thickness of an oxide sublayer based on zinc ZnO 129;
- FIG. 7 and FIG. 8 illustrate the solar factor of a second set of examples as a function of the thickness of a zinc oxide ZnO 129 undercoat after laser treatment
- FIG. 9 illustrates the solar factor of a third series of examples as a function of the thickness of a zinc oxide ZnO 129 undercoat after laser treatment.
- Figures 1 to 4 the proportions between the thicknesses of the different layers or the different elements are not strictly observed in order to facilitate their reading.
- FIG. 1 illustrates a structure of a functional monolayer stack 14 according to the invention deposited on a face 29 of a transparent glass substrate 30, in which the single functional layer 140, in particular based on silver or an alloy metal containing silver, is disposed between two antireflection coatings, the underlying antireflection coating 120 located below the functional layer 140 towards the substrate 30 and the overlying antireflection coating 160 disposed above the functional layer 140 opposite the substrate 30.
- These two antireflection coatings 120, 160 each comprise at least one dielectric layer 125, 127, 129; 161, 163, 165.
- said antireflection coating 120 located under said functional layer 140 towards said substrate 30 comprises:
- a zinc-based oxide sublayer, ZnO 129 which is located under and in contact with said functional layer 140, with a physical thickness of said zinc oxide-based sublayer ZnO 129 which is between 0.3 and 4.4 nm, or even between 0.3 and 2.9 nm, or even between 0.5 and 2.4 nm; and
- TiO x 127 which is located under and in contact with said zinc-based oxide sublayer, ZnO 129, with a physical thickness of said dielectric sublayer of titanium-based oxide TiO x 127 which is between 5.0 and 50.0 nm, or even between 5.0 and 40.0 nm, or even between 12.0 and 33.0 nm; it may be between 10.0 and 50.0 nm, or even between 10.0 and 40.0 nm, or even between 15.0 and 33.0 nm;
- said anti-reflective coating 160 located above said functional layer 140 opposite said substrate 30 comprises:
- a zinc-based oxide overlayer ZnO 161 which is located on and in contact with said functional layer 140, with a physical thickness of said zinc-based oxide overlayer, ZnO 161 which is between 2.0 and 10.0 nm, or even between 2.0 and 8.0 nm, or even between 2.5 and 5.4 nm;
- a dielectric overlayer 165 which is located on said zinc-based oxide overlayer, ZnO 161 and, preferably a silicon-based nitride dielectric overlayer, S13N 4 .
- FIG. 2 illustrates a structure of a functional bilayer stack 14 according to the invention deposited on a face 29 of a transparent glass substrate 30, in which the functional layers 140, 180, in particular based on silver or on metal alloy containing silver, are disposed between two antireflection coatings, the underlying antireflection coating 120 located below the functional layer 140 closest to the face 29 of the substrate 30, the intermediate antireflection coating 160 is located between the two functional layers and the overlying 200 anti-reflective coating arranged above the functional layer 180 furthest from the face 29 of the substrate 30.
- These three antireflection coatings 120, 160, 200 each comprise at least one dielectric layer 125, 127, 129; 161, 165, 167, 169; 201, 205.
- said anti-reflective coating located under and in contact with each functional layer 140, 180 comprises, in the direction of said substrate:
- a primary dielectric sublayer of silicon-based nitride S13N4 125, 165 which is located under and in contact with said sublayer of titanium-based oxide TiO x , respectively 127, 167, with a physical thickness of said primary dielectric sublayer of silicon-based nitride S13N4 which is between 5.0 and 50.0 nm, or even between 10.0 and 40.0 nm, or even between 15.0 and 20.0 nm;
- said anti-reflective coating located above and in contact with each functional layer comprises, opposite said substrate:
- a zinc-based oxide overlayer ZnO 161, 201 which is located on and in contact with said functional layer, with a physical thickness of said zinc-based oxide ZnO overlayer which is between 2.0 and 10.0 nm, or even between 2.0 and 8.0 nm, or even between 2.5 and 5.4 nm;
- a dielectric overlayer 205 which is located on said zinc-based oxide overlayer ZnO 201, and preferably this dielectric overlayer is silicon-based nitride, S13N 4 .
- Functional layer 140 is located directly over the underlying anti-reflective coating 120 and directly below the anti-reflective coating 160 overlying: there is no underblocking coating located between the underlying antireflection coating 120 and functional layer 140 or overblocking coating located between functional layer 140 and antireflection coating 160. There is no overblocking coating located between functional layer 140 and antireflection coating 160. The same is preferably true for the other functional layers which may be present: it is in direct contact with the antireflection coating located directly below and the antireflection coating located directly above.
- the antireflection coating 160 located above the single metallic functional layer in Figure 1 may terminate by an end protective layer (not illustrated), called an “overcoat” in English, which is the layer of the stack which is furthest from the face 29.
- the antireflection coating 120 may include a primary dielectric sublayer of silicon nitride S13N4 125 which is located under and in contact with said sublayer of titanium based oxide TiO x 127, with a physical thickness of said sublayer.
- primary dielectric layer of silicon-based nitride S13N4 125 which is between 5.0 and 50.0 nm, or even between 10.0 and 40.0 nm, or even between 15.0 and 20.0 nm
- the antireflection coating 120 may comprise a primary dielectric sub-layer of silicon-zirconium nitride Si x N y Zrz 125 'which is located under and in contact with said sub-layer of titanium-based oxide TiO x 127, with a physical thickness of said primary dielectric sub-layer of silicon-zirconium nitride Si x N y Zrz 125 'which is between 5.0 and 50.0 nm, or even between 10.0 and 40.0 nm, or even between 15, 0
- the antireflection coating 120 may also include a primary dielectric nitride sublayer which is over part of its thickness based on silicon-zirconium Si x N y Zrz and on another part of its thickness based on silicon S13N4.
- a stack of thin layers can be used in a multiple glazing 100 providing a separation between an exterior space ES and an interior space IS; this glazing may have a structure:
- this glazing is then made up of two substrates 10, 30 which are held together by a structure of frame 90 and which are separated from each other by an intermediate gas blade 15;
- this glazing is then made up of three substrates 10, 20, 30, separated two by two by an intermediate gas layer 15, 25, the whole being held together by a frame structure 90 .
- the stack 14 of thin layers can be positioned on face 3 (on the innermost sheet of the building, considering the incident direction of the sunlight entering the building and on its face facing the strip. gas), that is to say on an interior face 29 of the substrate 30 in contact with the intermediate gas sheet 15, the other face 31 of the substrate 30 being in contact with the interior space IS.
- face 3 on the innermost sheet of the building, considering the incident direction of the sunlight entering the building and on its face facing the strip. gas
- the stack 14 of thin layers can be positioned on face 3 (on the innermost sheet of the building, considering the incident direction of the sunlight entering the building and on its face facing the strip. gas), that is to say on an interior face 29 of the substrate 30 in contact with the intermediate gas sheet 15, the other face 31 of the substrate 30 being in contact with the interior space IS.
- one of the substrates has a laminated structure.
- FIG. 4 there are two stacks of thin layers, preferably identical:
- a stack 14 of thin layers is positioned on face 2 (on the outermost sheet of the building considering the incident direction of sunlight entering the building and on its face facing the gas layer), c 'that is to say on an interior face 11 of the substrate 10 in contact with the intermediate gas layer 15, the other face 9 of the substrate 10 being in contact with the exterior space ES; - and a stack 26 of thin layers is positioned on face 5 (on the innermost sheet of the building considering the incident direction of sunlight entering the building and on its face facing the gas layer), that is to say on an interior face 29 of the substrate 30 in contact with the intermediate gas sheet 25, the other face 31 of the substrate 30 being in contact with the interior space IS.
- a first series of examples has been produced on the basis of the stacking structure illustrated in FIG. 1 with, starting from surface 29, only the following layers, in this order: - a primary dielectric sublayer of silicon-based nitride S1 3 N 4 125 with a physical thickness of 10 nm, deposited from a silicon target doped with aluminum, at 92% by weight of silicon and 8% by weight of aluminum in an atmosphere at 45% nitrogen on the total nitrogen and argon and under a pressure of 1, 5.10 3 mbar;
- a titanium-based oxide dielectric sublayer TiO x 127 with a physical thickness of 10.0 nm, deposited from a titanium target in an atmosphere with 5% oxygen out of the total d oxygen and argon and under a pressure of 2.10 3 mbar;
- a zinc-based oxide sublayer, ZnO 129 of variable physical thickness, from 1.0 nm to 8.0 nm, deposited from a ceramic target consisting of 49 atomic% of zinc and 49 atomic% oxygen and doped with 2% aluminum, in an argon atmosphere and under a pressure of 2.10 3 mbar;
- a zinc-based oxide overcoat ZnO 161 with a physical thickness of 5.0 nm, deposited from a ceramic target consisting of 49 atomic% of zinc and 49 atomic% of oxygen and doped with l 2% aluminum, in an argon atmosphere and under a pressure of 2.10 3 mbar;
- FIG. 5 The resistance per square R of this stack as a function of the thickness of the zinc-based oxide sublayer ZnO 129 without any heat treatment is illustrated in FIG. 5.
- These examples of the first series were then subjected to a treatment of laser consisting here of a scrolling of the substrate 30 at a speed of 4 m / min under a laser line 20 of 0.08 mm wide, 11.6 mm long and of total power of 433 W with the laser line oriented perpendicular to the face 29 and in the direction of the stack 14, that is to say by placing the laser line above of the stack, as visible in FIG. 1 (the right black arrow illustrating the orientation of the light emitted).
- the resistance per square R of these stacks after this treatment is illustrated in FIG. 6. It has thus been observed that the resistance per square of the stacks with the dielectric sub-layer of titanium-based oxide TiO x 127 and the sub-layer of very fine zinc oxide ZnO 129, between 0.3 and 5.0 nm, and preferably between 0.3 and 4.9 nm, or even between 0.3 and 3.9 nm, was surprisingly good with a laser treatment. Such a situation makes it possible in a first approach to increase the solar factor at constant functional layer thickness, or even in a second approach to decrease the thickness of the functional layer to further increase the solar factor without modifying the resistance per square previously obtained. . To confirm this effect, a second series of examples was carried out on the basis of the stacking structure illustrated in FIG. 1 with, starting from surface 29, only the following layers, in this order:
- a dielectric titanium-based oxide sublayer TiO x 127 with a physical thickness varying between approximately 26.5 nm and approximately 21.6 nm, deposited from a titanium target in an atmosphere at 5% oxygen out of the total of oxygen and argon and under a pressure of 2.10 3 mbar;
- a zinc-based oxide sublayer ZnO 129 of variable physical thickness, from 1.0 nm to 6.0 nm, deposited from a ceramic target consisting of 49 atomic% zinc and 49 atomic% of oxygen and doped with 2% aluminum, in an argon atmosphere and under a pressure of 2.10 3 mbar;
- a dielectric overlayer 163 comprising titanium dioxide T1 ⁇ 2, of a physical thickness varying between about 10.2 nm and about 10.7 nm, deposited from a titanium target in an atmosphere with 10% oxygen out of the total oxygen and argon and under a pressure of 2.10 3 mbar - a dielectric overlay 165 of silicon-based nitride S13N4, with a physical thickness varying between about 24.7 nm and about 25.1 nm, deposited from a silicon target doped with aluminum, at 92% by weight of silicon and 8% by weight of aluminum in an atmosphere containing 45% nitrogen on the total nitrogen and argon and under a pressure of 2.10 3 mbar.
- the interior substrate 30 of this double glazing is coated on its interior face 29 facing the intermediate gas layer 15, with an insulating coating 14 consisting of the functional single-layer stack described above: the functional single-layer stack is thus in face called "face
- the table in figure 7 summarizes the exact thickness of layers 127, 129, 163 and 165, in nm, for the six examples of zinc-based oxide sublayer ZnO 129, with a physical thickness varying from 1 , 0 nm to 6.0 nm.
- the last line of the table in FIG. 7, as well as in FIG. 8 illustrate the change on the ordinate of the solar factor, g, in percent, as a function of the thickness, ti29, in nanometers of this sub-layer of oxide at zinc base ZnO 129 on the abscissa, this solar factor being measured immediately after the laser treatment of the two substrates 10, 30, then their integration to form the double glazing.
- the solar factor is thus improved when the zinc oxide ZnO 129 sublayer is between 0.03 and 5.0 nm.
- the solar factor is increased here, in the double glazing configuration, by 0.9% by decreasing the thickness of the zinc-based oxide sub-layer ZnO 129 from 6.0 nm to 1.0 nm.
- the solar factor is particularly favorable for a thickness of ZnO 129 zinc-based oxide sublayer between 1.0 and 3.0 nm, or even between 1.5 and 2.4 nm.
- a dielectric titanium-based oxide sublayer TiO x 127 with a physical thickness varying between approximately 32.2 nm and approximately 28.2 nm, deposited from a titanium target in an atmosphere at 5% oxygen out of the total of oxygen and argon and under a pressure of 2.10 3 mbar 4;
- a zinc-based oxide sublayer ZnO 129 of variable physical thickness, from 1.0 nm to 6.0 nm, deposited from a ceramic target consisting of 49 atomic% zinc and 49 atomic% of oxygen and doped with 2% aluminum, in an argon atmosphere and under a pressure of 2.10 3 mbar; a functional metallic layer 140 based on silver, and even here precisely in silver, with a physical thickness of 10 nm, deposited from a metallic target in silver, in an argon atmosphere and under a pressure of 2.10 3 mbar;
- a dielectric overlayer 163 comprising titanium dioxide T1 ⁇ 2, with a physical thickness varying between approximately 5.7 nm and approximately 5.0 nm, deposited from a titanium target in an atmosphere with 10% oxygen on the total of oxygen and argon and under a pressure of 2.10 3 mbar
- the two outer substrates 10, 30 of this triple glazing are each coated, on its inner face 11, 29 facing the intermediate gas layer 15, 25, with an insulating coating 14, 26 consisting of the functional monolayer stack described. above: the functional monolayer stacks are thus on faces called "face 2 and" face 5).
- the central substrate 20 of this triple glazing is not coated with any coating on any of these faces.
- the table in figure 9 summarizes the exact thickness of layers 125, 127, 129, 163 and 165, in nm, for the six examples of zinc-based oxide underlayer ZnO 129, of varying physical thickness. from 1.0 nm to 6.0 nm.
- the last line of the table in FIG. 9, as well as in FIG. 10, illustrate the change on the y-axis of the solar factor, g, in percent, as a function of the thickness, ti29, in nanometers of this sub-layer of oxide at zinc base ZnO 129 on the abscissa, this solar factor being measured immediately after the laser treatment of the two substrates 10, 30, then their integration to form the triple glazing.
- the solar factor is thus improved when the zinc oxide ZnO 129 sublayer is between 0.03 and 5.0 nm.
- the solar factor is increased here, in the triple glazing configuration, by 0.4% by decreasing the thickness of the zinc-based oxide ZnO 129 undercoat from 6.0 nm to 1.0 nm.
- the solar factor is particularly favorable for a sub-layer thickness of zinc oxide ZnO 129 between 1.0 and 3.0 nm, or even between 1.5 and 2.4 nm.
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Abstract
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FR2004310A FR3109776B1 (fr) | 2020-04-30 | 2020-04-30 | Materiau comportant un empilement a sous-couche dielectrique fine d’oxide a base de zinc et procede de depot de ce materiau |
PCT/FR2021/050738 WO2021219961A1 (fr) | 2020-04-30 | 2021-04-28 | Materiau comportant un empilement a sous-couche dielectrique fine d'oxide a base de zinc et procede de depot de ce materiau |
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FR2728559B1 (fr) | 1994-12-23 | 1997-01-31 | Saint Gobain Vitrage | Substrats en verre revetus d'un empilement de couches minces a proprietes de reflexion dans l'infrarouge et/ou dans le domaine du rayonnement solaire |
FR2858816B1 (fr) * | 2003-08-13 | 2006-11-17 | Saint Gobain | Substrat transparent comportant un revetement antireflet |
FR2946639B1 (fr) * | 2009-06-12 | 2011-07-15 | Saint Gobain | Procede de depot de couche mince et produit obtenu. |
FR2981346B1 (fr) * | 2011-10-18 | 2014-01-24 | Saint Gobain | Procede de traitement thermique de couches d'argent |
FR3021310B1 (fr) * | 2014-05-23 | 2022-11-18 | Saint Gobain | Substrat muni d'un empilement a couche metallique partielle, vitrage et procede. |
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