CN103857639A - 包含含有NiCu合金层的遮阳玻璃 - Google Patents
包含含有NiCu合金层的遮阳玻璃 Download PDFInfo
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- CN103857639A CN103857639A CN201280050645.5A CN201280050645A CN103857639A CN 103857639 A CN103857639 A CN 103857639A CN 201280050645 A CN201280050645 A CN 201280050645A CN 103857639 A CN103857639 A CN 103857639A
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- Prior art keywords
- layer
- window glass
- copper
- nickel
- lamination
- 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.)
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 50
- 239000000956 alloy Substances 0.000 title claims abstract description 50
- 229910003322 NiCu Inorganic materials 0.000 title description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 97
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 46
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052802 copper Inorganic materials 0.000 claims abstract description 41
- 239000010949 copper Substances 0.000 claims abstract description 41
- 239000011521 glass Substances 0.000 claims abstract description 37
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 239000005357 flat glass Substances 0.000 claims description 58
- 239000010410 layer Substances 0.000 claims description 56
- 238000003475 lamination Methods 0.000 claims description 47
- 239000002346 layers by function Substances 0.000 claims description 38
- 229910017083 AlN Inorganic materials 0.000 claims description 28
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 28
- 230000037072 sun protection Effects 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 19
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 17
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 17
- 229910052796 boron Inorganic materials 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 11
- 239000011241 protective layer Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000005496 tempering Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910001413 alkali metal ion Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000003989 dielectric material Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000000151 deposition Methods 0.000 description 15
- 230000005855 radiation Effects 0.000 description 12
- 238000000576 coating method Methods 0.000 description 9
- 238000001755 magnetron sputter deposition Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 6
- 229910052804 chromium Inorganic materials 0.000 description 6
- 239000011651 chromium Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 238000007669 thermal treatment Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910018054 Ni-Cu Inorganic materials 0.000 description 3
- 229910018481 Ni—Cu Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004453 electron probe microanalysis Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000881 Cu alloy Chemical class 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000003984 copper intrauterine device Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Classifications
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- 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
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- 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
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- 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
- C03C17/3613—Coatings of type glass/inorganic compound/metal/inorganic compound/metal/other
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- 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
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- 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
- C03C17/3649—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 made of metals other than silver
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- 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
- C03C17/3652—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 coating stack containing at least one sacrificial layer to protect the metal from oxidation
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/74—UV-absorbing coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
- Y10T428/12542—More than one such component
- Y10T428/12549—Adjacent to each other
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
- Y10T428/12597—Noncrystalline silica or noncrystalline plural-oxide component [e.g., glass, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
- Y10T428/2495—Thickness [relative or absolute]
- Y10T428/24967—Absolute thicknesses specified
- Y10T428/24975—No layer or component greater than 5 mils thick
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
- Y10T428/264—Up to 3 mils
- Y10T428/265—1 mil or less
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- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Laminated Bodies (AREA)
- Optical Filters (AREA)
Abstract
具有遮阳性质的窗玻璃,包含玻璃基底,在其上沉积叠层,所述叠层包含由合金组成的层,所述合金包含镍和铜,其中铜的原子百分比为大于1%且小于25%,并且其中镍的原子百分比为大75%且小于99%。
Description
本发明涉及玻璃基板或制品领域,特别是用于建筑的窗玻璃类型,在其表面处包含赋予其遮阳性质的薄层类型涂层。此类窗玻璃还可以应用于汽车领域。术语窗玻璃对本发明目的而言理解为是指由一个或多个玻璃基板组成的玻璃产品,特别是简单窗玻璃(simples
vitrages)、双层窗玻璃(doubles vitrages)、三层窗玻璃(triples vitrages)等等。
此类窗玻璃具有通过吸收和通过反射作用于入射日光辐射的薄层的叠层。它们统称为“遮阳玻璃”。它们尤其用于日光防护(日光防护功能)或尤其用于提供乘客舱或住宅的绝热(低辐射功能)。
术语日光防护,由此对本发明的目的而言理解为是指窗玻璃限制由住宅或乘客舱外部穿过该窗玻璃进入内部的能量流,特别是红外(IR)辐射的能力。
术语低辐射率理解为是指具有至少一个赋予其小于50%、或甚至小于40%的法向辐射率εn的官能层的窗玻璃,该辐射率由下列等式规定:
εn = 1 – Rn,
其中Rn是该窗玻璃的沿法向的反射系数(根据国际标准ISO 10292的附录A)。
通常,本说明书中提出的所有光与能量特性根据涉及测定建筑用玻璃中所用窗玻璃的光、太阳能与能量特性的国际标准ISO 9050(2003)和ISO 10292(1994)以及欧洲标准EN 410(1998)和EN 673(1998)中描述的原则与方法获得。
此外,与玻璃基底结合,这些涂层必须是审美上令人愉悦的,也就是说,具有该叠层的窗玻璃在投射和反射方面必须具有足够中性色度(colorimétrie neutre)以免干扰使用者或者具有特别是在建筑领域中所需的浅蓝色或浅绿色的色度。这些涂层通常地通过最简单的CVD类沉积技术或目前最通常通过真空溅射沉积技术(本领域中通常也称为磁控溅射)沉积,特别是当该涂层由连续层的复杂叠层组成时,其厚度不超过几纳米或几十纳米。
通常,薄层叠层尤其因一个或多个活性层(在本说明书中称为官能层)的固有性质而具有遮阳性质。术语活性层或官能层由此理解为是指明显作用于穿过所述窗玻璃的阳光流的层。此类活性层以已知方式可以主要以红外辐射反射模式或主要以红外辐射吸收模式起作用。通常,如前面已经解释的那样,这些日光防护层部分通过反射和部分通过吸收起作用。
特别地,目前销售的表现最好的叠层混入了至少一个银类型的金属功能层,其基本上以反射大部分入射的IR(红外)辐射的模式起作用。它们的法向辐射率不超过几个百分比。这些叠层由此主要用作用于建筑物隔热的低辐射率(或低e)窗玻璃。但是,这些层对水分非常敏感,因此只能用于双层窗玻璃,在其面2上以保护其免受水分侵袭。本发明的叠层不包含此类银类型层,或金或铂类型的层或仅为可忽略的量,特别是以不可避免的杂质形式。
例如如申请WO 01/21540中所述,在本领域中也已经报道了具有日光防护功能的其它金属层,包括Nb、Ta或W类型或这些金属的氮化物类型的功能层。在此类层中,太阳辐射此时主要被该功能层非选择性地吸收,也就是说IR辐射(即,其波长为大约780 nm至2500 nm)和可见光辐射(其波长为大约380 nm至780 nm)被不加区别地吸收。在此类窗玻璃中,法向辐射率εn的值通常较高。仅仅当该功能层相对较厚时才能获得较低的辐射率值,特别是对金属铌而言至少20 nm。由于这种层的非选择性吸收,此类窗玻璃的光透射系数必然非常低,通常远低于30。最后,考虑到此类特性,使用此类叠层不可能出现结合相对低的法向辐射率(通常低于30%,特别是大约25%或甚至20%)并同时保持足够高的透光率(也就是说通常大于30%)的遮阳玻璃。
专利公开EP 747 329 B2描述了叠层,其功能层由纯镍组成。由于镍是铁磁性金属,已经证明了通过磁控溅射类型的常规沉积技术(其包括使用磁场力溅射待沉积的金属靶)以工业规模沉积层形式的镍是非常困难和昂贵的。
为了避免该问题,专利EP 747 329 B2表示可能使用主要包含镍和铬的合金,Ni的比例为至少10原子%。
申请EP 067 257 A1另外描述了作为日光防护功能层使用以1至25重量%镍与75至99重量%铜的比例包含镍和铜的合金。
申请GB 1309881描述了包含功能层的透明窗玻璃,所述功能层主要含有铜和5至15重量%的镍。
本发明的目的由此是提供包含多层叠层的窗玻璃,所述叠层赋予其如前所述的遮阳性质,也就是说通常大于30%、优选大于或等于40%的光透过率TL,和小于30%、或甚至小于25%的法向辐射率,所述叠层长期有效,尤其是当其直接放置在该窗玻璃暴露于建筑物或乘客舱内部或甚至外部的面上时。本发明的另一目的是提供日光防护窗玻璃,其所述叠层能够经受热处理如回火、弯曲或更通常在更高温度下的热处理而不会损失其光学和能量性质。特别地,装有本发明的层的窗玻璃尤其在透射或在反射方面具有并在热处理后保持基本中性的颜色或不是非常强烈的蓝-绿色调,如特别是在建筑领域所需的那样。术语中性色彩或蓝-绿色调对本发明的目的而言在LAB色度系统(L*,a*,b*)中理解为是指a*和b*的值小于或接近10并且优选为负值。
本发明的窗玻璃还能够通过在极大程度上有利于光波(也就是说大约380至780
nm的波长)的透射并限制其波长大于780 nm的红外辐射的透过来选择穿过其的辐射。
根据本发明,由此能够保持该窗玻璃所保护的房间或乘客舱的强照明,同时尽量减少进入其中的热的量。
根据另一方面,本发明的窗玻璃还因所用层的低辐射性质能够限制建筑内部与外部之间的热交换而具有隔热性质。
根据本发明的另一优点,装有本发明的叠层的窗玻璃与具有日光防护性质的其它已知窗玻璃,尤其是包含银-基叠层的窗玻璃相比可以简单地制造。
此外,其是防潮和耐刮擦的。因此,其有时可以有利地以简单窗玻璃(单一玻璃基底)形式使用,该叠层有利地转向要保护的建筑物或乘客舱的内部面。
更具体而言,本发明涉及具有遮阳性质的窗玻璃,其包含至少一个玻璃基底,在该玻璃基底上沉积层的叠层,所述叠层包含由合金组成的层,该合金包含镍和铜或由镍和铜组成,其中铜的原子百分比大于1%且小于25%,并且其中镍的原子百分比大于75%且小于99%。由包含镍和铜的合金所组成的所述层是该叠层的功能层,也就是说,其是该窗玻璃的遮阳性质的来源,或者是所述性质的至少主要部分。
根据本发明的优选实施方案,其当然可以在适当情况下组合在一起:
- 在该合金中铜的原子百分比为2%至20%,例如5%至10%或2%至5%,
- 在该合金中镍的原子百分比为80%至95%,
- 所述功能层的厚度为5至25纳米,优选10至20纳米,
- 该合金仅由镍和铜组成,其它元素仅以不可避免的杂质的形式存在,
- 该叠层由以下层按顺序组成,从玻璃基底表面开始:
- 一个或多个用于保护该功能层以抵抗碱金属离子由玻璃基底迁移的下层,具有总计5至150 nm的几何厚度,
- 所述功能层由所述合金组成,包含镍和铜或由镍和铜组成,
- 一个或多个用于保护该功能层以抵抗来自空气中的氧的上层,特别是在如回火或退火的热处理过程中,所述层具有总计5至150 nm的几何厚度,
- 该下保护层和上保护层选自任选掺杂有Al、Zr或B的氮化硅、氮化铝AlN、氧化锡、锌或锡的混合氧化物SnyZnzOx、氧化硅SiO2、未掺杂的氧化钛TiO2以及氧氮化硅SiOxNy,
- 该叠层按顺序包含下列层,从玻璃基底表面开始:
- 厚度为5至150 nm、优选30至70 nm的氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的下层,
- 所述功能层由所述合金组成,包含镍和铜或由镍和铜组成,
- 厚度为5至150 nm、优选30至70 nm氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的上层,
- 如前所述,该叠层包含至少两个由所述合金组成的功能层,所述合金包含镍和铜或由镍和铜组成,所述层各自在叠层中通过至少一个介电材料的中间层彼此分隔,
- 所述中间层包含选自任选掺杂有Al、Zr或B的氮化硅、氮化铝AlN、氧化锡、锌或锡的混合氧化物SnyZnzOx、氧化硅SiO2、未掺杂的氧化钛TiO2、以及氧氮化硅SiOxNy的材料的至少一个层,
- 该叠层按顺序包含下列层,从玻璃基底表面开始:
- 厚度为5至150 nm、优选30至70 nm的氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的下层,
- 由所述合金组成的第一功能层,所述合金如前所述包含镍和铜或由镍和铜组成,所述功能层的厚度特别为5至25 nm,优选5至10 nm,
- 厚度为5至150 nm、优选5至50 nm、非常特别为5至15 nm的包含选自任选掺杂有Al、Zr或B的氮化硅、氮化铝AlN、氧化锡、锌或锡的混合氧化物SnyZnzOx、氧化硅SiO2、未掺杂的氧化钛TiO2、以及氧氮化硅SiOxNy,优选任选掺杂有Al、Zr或B的氮化硅的材料的至少一个层的中间层,
- 由所述合金组成的第二功能层,所述合金如前所述包含镍和铜或由镍和铜组成,所述功能层的厚度特别为5至25 nm,优选5至10 nm,
- 厚度为5至150 nm、优选30至70 nm的氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的上层,
- 该叠层还包含用于该功能层的补充性保护层,该保护层由选自Ti、Mo、Al的金属或包含这些元素的至少一种的合金组成,所述补充性保护层与该功能层接触并分别在其顶部和底部上放置,并具有大约1 nm至大约5 nm的几何厚度。所述补充性保护层优选由Ti组成。
制造日光防护窗玻璃的方法包括例如下列步骤:
- 制造玻璃基底,
- 通过磁控真空溅射技术在玻璃基底上沉积叠层,在惰性气体如氩气的剩余气氛中通过溅射由镍和铜的合金组成的靶获得日光防护功能层,该合金中铜的原子百分比为1%至25%,特别为5%至20%。
术语“仅包含”对本说明书的目的而言理解为是指构成该功能层的合金唯一或非常主要地包含元素铜和镍,其它元素由此仅仅以非常次要的浓度存在,该浓度对该材料的所需性质没有或实际上没有影响。术语“不可避免的杂质”由此理解为是指由于这些杂质存在于初始使用的铜和镍的来源中或由于沉积该镍和铜层的方法,在该镍和铜合金中某些额外元素,特别是金属元素的存在不能避免。通常,被认为是合金中杂质的元素各自的原子比例为小于1原子%、优选小于0.5原子%和非常优选小于0.1原子%。
下面的实施例仅通过例示给出并且不在任意所述方面中限制本发明的范围。出于比较的目的,下面的实施例的所有叠层在同样的Planilux®玻璃基底上合成。根据公知的常规磁控溅射真空沉积技术沉积该叠层的所有层。
实施例
1
(根据本发明):
在本发明的该实施例中,根据常规磁控管技术在本申请人的公司所销售的Planilux®类型的玻璃基底上沉积的是由下列层依次组成的叠层:
玻璃/ Si3N4
/ Ni80Cu20* / Si3N4
(52 nm)
(15 nm) (54 nm)
* 80原子%的镍,20原子%的铜
通过磁控溅射技术由包含大约80原子%的镍和大约20原子%的铜的合金所组成的靶起始获得由NiCu制成的功能金属层。在通过磁控管溅射技术沉积该层的过程中没有什么困难。
通过最终获得的层的Castaing微探针分析(也称为EPMA或电子探针显微分析)和SIMS(二次粒子质谱法)验证了最终获得的金属层的组成基本对应于初始靶的组成。
随后对具有其叠层的基底施以热处理,所述热处理由以下步骤组成:在650℃下加热8分钟,接着回火。该处理代表了如果该窗玻璃必须被回火时后者所经受的条件。
对本发明的窗玻璃测量的是在热处理之前和之后的光透射系数TL与法向辐射率,根据前述标准。
实施例
2
(根据本发明):
在本发明的该实施例中,根据磁控管技术由镍和铜的合适合金靶在Planilux®类型的玻璃基底上沉积的是由下列层依次组成的叠层:
玻璃 / Si3N4
/ Ni93Cu7 / Si3N4
(52 nm) (15 nm) (54 nm)
不考虑合金中高浓度的镍,在通过磁控管溅射技术沉积该层的过程中没有什么困难。
实施例
3
(对比):
以与实施例1相同的方式进行该实施例,并通过磁控溅射技术获得基本相同的叠层,除了用于沉积功能层的靶之外——根据专利EP
747 329 B2,实施例22的教导,这一次该靶由镍和铬的合金组成。
更具体而言,根据常规磁控管技术在Planilux®类型的相同玻璃基底上沉积的是由下列层依次组成的叠层:
玻璃 / Si3N4
/ Ni80Cr20* / Si3N4
(52 nm) (15 nm) (54 nm)
* 80原子%的镍,20原子%的铬
获得的由NiCr制成的功能金属层由80原子%的镍和20原子%的铬组成。
实施例
4
(对比):
在该对比例中,为了获得如公开文本EP 0 067 257中所述的遮阳玻璃,根据相同的磁控管技术在Planilux®类型的玻璃基底上沉积的是下列叠层,其活性层,即作用于穿过所述窗玻璃的日光辐射的层,是Ni-Cu合金层,其铜比例占绝大多数:
玻璃 / Si3N4
/ Ni25Cu75* / Si3N4
(55 nm) (15 nm) (50 nm)
* 25原子%的镍,75原子%的铬
对本发明的实施例1和2的样品和对比例3和4的样品进行的测量的值集中在下表1中:
实施例
5
至
9
:
为了验证根据前述实施例沉积的功能层的化学耐受性,仍通过磁控管技术在预先沉积在该玻璃表面上的10 nm氮化硅亚层上沉积相同的各种合金组合物。该功能层的厚度对各样品均为10 nm。随后在基底上进行前述水解试验,并在暴露4天和60天后测量该层的薄层电阻的变化。在下表2中给出了结果:
比较表1至2中报道的数据证实了与使用本发明的功能层相关的优点与优越性。
特别是:
通过比较表1中报道的数据,很显然,本发明的包含功能层的窗玻璃具有能量隔绝性质与光性质之间的最佳折衷,也就是说,最高的优值(TL/εN)。
更特别低,比较本发明的实施例1或2与为了比较给出的实施例3显示,本发明的具有由NiCu合金组成的功能层的窗玻璃与包含镍与铬的相应合金层的已知窗玻璃相比具有优异的光学性质。此外,在表1中观察到,该窗玻璃的系数εN对具有本发明的功能层的窗玻璃来说明显较低,同时光透过率TL更高。
具有对比例4的叠层的窗玻璃(其中功能层由主要包含铜的Ni-Cu合金组成)具有接近本发明的窗玻璃的优值。但是,表2中报道的数据表明,此类层不能确保长期有效,其耐水解性过低。
根据另一优点,本发明的日光防护叠层(其活性层基于Ni-Cu合金,其厚度相对较小,即大约10至20纳米)可以极为简单和廉价地制造,尤其是通过磁控溅射真空沉积技术:的确,小厚度的合金层能够在生产率方面产生不小的增益,因为沉积室中基底的运行速度与所述层的所需厚度直接相关。
这次还对根据实施例1制备的样品测量的是根据下列测试进行的叠层的耐水解性(气候模拟):
在封闭室中,对具有叠层的窗玻璃施以苛刻的湿度与温度条件(50℃下95%的相对湿度),总持续时间为28天,以导致其加速老化。对未经受最终热处理的实施例1的第一样品和最后在620℃下加热8分钟的第二样品进行该测试。
在试验开始前、随即在测试8天、20天和28天后测量该叠层的法向辐射率。
在试验的第8天、20天和28天结束时检测到测得的法向辐射率的初始值没有改变。
前面的耐久性试验表明,此类叠层可以无难度地在简单窗玻璃的面2上沉积,其不具有被化学作用(水分)或甚至机械作用(叠层的摩擦)劣化的风险。
在退火与回火之前和之后在透射和反射(外侧)方面测量实施例1的窗玻璃的L*,
b*, a*系统的色度特性。
下表3中报道了测得的数据:
表3中报道的数据显示了具有本发明的叠层的窗玻璃的理想色度性质:实施例1的参数a*和b*在透射和反射方面均相对较低。此类色度性质导致窗玻璃的中性色彩或并不非常强烈的蓝-绿色彩,如建筑领域目前所需的那样。
在L*, a*, b*色度系统中和在法向入射下,与热处理相关的透射方面该玻璃的色彩变化用常规使用并由下列等式定义的量值ΔE来量化:
申请人进行的测试均表明,对于本发明的窗玻璃,所述量值ΔE总是小于3,通常小于2,这证明了涂有此类叠层的基底可以经受热处理和任选随后的回火,而不会显著改变其光学性质,特别是其被感知的色彩。
Claims (12)
1.具有遮阳性质的窗玻璃,包含至少一个玻璃基底,在所述玻璃基底上沉积叠层,所述叠层包含由合金组成的层,所述合金包含镍和铜,在该合金中铜的原子百分比大于1%且小于25%,并且其中镍的原子百分比大于75%且小于99%。
2.如权利要求1所要求保护的日光防护窗玻璃,其中该合金中铜的原子百分比为5%至20%。
3.如权利要求1所要求保护的日光防护窗玻璃,其中该合金中镍的原子百分比为80%至95%。
4.如前述权利要求之一所要求保护的日光防护窗玻璃,其中所述功能层的厚度为5至25纳米,优选10至20纳米。
5.如前述权利要求之一所要求保护的日光防护窗玻璃,其中该合金仅包含镍、铜和不可避免的杂质。
6.如前述权利要求之一所要求保护的日光防护窗玻璃,其中该叠层由以下层按顺序组成,从玻璃基底表面开始:
- 一个或多个用于保护该功能层以抵抗碱金属离子由玻璃基底迁移的下层,具有总计5至150 nm的几何厚度,
-由所述合金组成的所述功能层,
- 一个或多个用于保护该功能层以抵抗来自空气中的氧的上层,特别是在如回火或退火的热处理过程中,所述层具有总计5至150 nm的几何厚度。
7.如前述权利要求所要求保护的日光防护窗玻璃,其中下保护层和上保护层选自任选掺杂有Al、Zr或B的氮化硅、氮化铝AlN、氧化锡、锌或锡的混合氧化物SnyZnzOx、氧化硅SiO2、未掺杂的氧化钛TiO2以及氧氮化硅SiOxNy。
8.如前述权利要求之一所要求保护的日光防护窗玻璃,其中该叠层按顺序包含下列层,从玻璃基底表面开始:
- 厚度为5至150 nm、优选30至70 nm的氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的下层,
- 由所述合金组成的所述功能层,
- 厚度为5至150 nm、优选30至70 nm氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的上层。
9.如前述权利要求之一所要求保护的日光防护窗玻璃,其中该叠层包含至少两个由所述合金组成的功能层,所述合金包含镍和铜或由镍和铜组成,所述层各自在叠层中通过至少一个介电材料的中间层彼此分隔。
10.如前述权利要求所要求保护的日光防护窗玻璃,其中所述中间层包含选自任选掺杂有Al、Zr或B的氮化硅、氮化铝AlN、氧化锡、锌或锡的混合氧化物SnyZnzOx、氧化硅SiO2、未掺杂的氧化钛TiO2、以及氧氮化硅SiOxNy的材料的至少一个层。
11.如前述权利要求所要求保护的日光防护窗玻璃,其中该叠层按顺序包含下列层,从玻璃基底表面开始:
- 厚度为5至150 nm、优选30至70 nm的氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的下层,
- 基本上由所述合金组成的第一功能层,所述合金包含镍和铜或由镍和铜组成,
- 厚度为5至150 nm的包含选自任选掺杂有Al、Zr或B的氮化硅、氮化铝AlN、氧化锡、锌或锡的混合氧化物SnyZnzOx、氧化硅SiO2、未掺杂的氧化钛TiO2、以及氧氮化硅SiOxNy,优选任选掺杂的氮化硅的材料的至少一个层的中间层,
- 基本由所述合金组成的第二功能层,所述合金包含镍和铜或由镍和铜组成,
- 厚度为5至150 nm、优选30至70 nm的氮化铝AlN或任选掺杂有Al、Zr或B的氮化硅的上层。
12.如前述权利要求之一所要求保护的日光防护窗玻璃,其中该叠层还包含金属保护层,所述金属选自Ti、Mo、Al或包含这些元素的至少一种的合金,所述层与该功能层接触并在其顶部和底部上放置,各保护层具有大约1 nm至大约5 nm的几何厚度。
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FR1159542A FR2981646B1 (fr) | 2011-10-21 | 2011-10-21 | Vitrage de controle solaire comprenant une couche d'un alliage nicu |
FR1159542 | 2011-10-21 | ||
PCT/FR2012/052363 WO2013057425A1 (fr) | 2011-10-21 | 2012-10-17 | Vitrage de controle solaire comprenant une couche d'un alliage nicu |
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BR (1) | BR112014008474B1 (zh) |
EA (1) | EA025184B1 (zh) |
ES (1) | ES2560834T3 (zh) |
FR (1) | FR2981646B1 (zh) |
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FR3005313B1 (fr) * | 2013-05-03 | 2016-05-27 | Saint Gobain | Vitrage de controle solaire comprenant une couche d'un alliage de zinc et de cuivre |
FR3011836B1 (fr) * | 2013-10-10 | 2015-10-23 | Saint Gobain | Vitrage de controle thermique |
CN103614696B (zh) * | 2013-11-07 | 2016-02-03 | 中山市创科科研技术服务有限公司 | 一种耐腐蚀薄膜的制备方法 |
US10539726B2 (en) * | 2015-09-01 | 2020-01-21 | Vitro Flat Glass Llc | Solar control coating with enhanced solar control performance |
FR3048243B1 (fr) * | 2016-02-26 | 2018-03-16 | Saint-Gobain Glass France | Vitrage de controle solaire comprenant une couche d'un alliage nicucr |
US11472373B2 (en) | 2017-04-17 | 2022-10-18 | 3E Nano Inc. | Energy control coatings, structures, devices, and methods of fabrication thereof |
CN111646709B (zh) * | 2020-05-08 | 2023-05-16 | 台玻太仓工程玻璃有限公司 | 一种低辐射可钢化镀膜玻璃 |
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MX2014004436A (es) | 2014-05-28 |
PL2768784T3 (pl) | 2016-06-30 |
JP6092882B2 (ja) | 2017-03-08 |
US20140255721A1 (en) | 2014-09-11 |
WO2013057425A1 (fr) | 2013-04-25 |
EP2768784B1 (fr) | 2015-12-30 |
AU2012324663B2 (en) | 2016-06-30 |
EA201490841A1 (ru) | 2014-07-30 |
KR101996693B1 (ko) | 2019-07-04 |
KR20140088522A (ko) | 2014-07-10 |
ES2560834T3 (es) | 2016-02-23 |
CN103857639B (zh) | 2017-05-03 |
US8889260B2 (en) | 2014-11-18 |
FR2981646B1 (fr) | 2013-10-25 |
EP2768784A1 (fr) | 2014-08-27 |
BR112014008474B1 (pt) | 2021-01-05 |
BR112014008474A2 (pt) | 2017-04-11 |
FR2981646A1 (fr) | 2013-04-26 |
AU2012324663A1 (en) | 2014-06-05 |
JP2015505789A (ja) | 2015-02-26 |
MX340161B (es) | 2016-06-29 |
EA025184B1 (ru) | 2016-11-30 |
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