CN110627374B - Amber middle-permeation low-reflection double-silver energy-saving coated glass and preparation method thereof - Google Patents
Amber middle-permeation low-reflection double-silver energy-saving coated glass and preparation method thereof Download PDFInfo
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- CN110627374B CN110627374B CN201910923967.XA CN201910923967A CN110627374B CN 110627374 B CN110627374 B CN 110627374B CN 201910923967 A CN201910923967 A CN 201910923967A CN 110627374 B CN110627374 B CN 110627374B
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- 239000011521 glass Substances 0.000 title claims abstract description 78
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 33
- 239000004332 silver Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000010410 layer Substances 0.000 claims abstract description 210
- 239000011241 protective layer Substances 0.000 claims abstract description 101
- 239000002346 layers by function Substances 0.000 claims abstract description 91
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 46
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 62
- 238000004544 sputter deposition Methods 0.000 claims description 40
- 239000007789 gas Substances 0.000 claims description 34
- 238000007747 plating Methods 0.000 claims description 33
- 229910052786 argon Inorganic materials 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 17
- 229910007717 ZnSnO Inorganic materials 0.000 claims description 16
- 238000002834 transmittance Methods 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000012495 reaction gas Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910004286 SiNxOy Inorganic materials 0.000 claims description 4
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000002310 reflectometry Methods 0.000 abstract description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 50
- 239000011787 zinc oxide Substances 0.000 description 25
- 239000000047 product Substances 0.000 description 14
- 239000010949 copper Substances 0.000 description 13
- 238000000151 deposition Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 238000001579 optical reflectometry Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019993 champagne Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 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
- 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
- C03C17/3644—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
- C03C17/3649—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
-
- 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
-
- 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
- C03C17/3684—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 for decoration purposes
-
- 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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- 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
The invention discloses amber middle-permeation low-reflection double-silver energy-saving coated glass and a preparation method thereof, wherein the amber middle-permeation low-reflection double-silver energy-saving coated glass comprises a glass substrate and a composite film layer plated on one side surface of the glass substrate, wherein the composite film layer comprises a first functional layer, a first medium protective layer, a second functional layer, a third functional layer, a first protective layer, a third medium protective layer, a fourth functional layer, a second protective layer and a fourth medium protective layer which are sequentially and adjacently compounded from inside to outside on a glass substrate; the first functional layer is an SSTZrOX layer; the preparation method adopts a magnetron sputtering process, and ten film layers are plated on the glass substrate adjacently in sequence from inside to outside. The amber middle-transmission low-reflection double-silver energy-saving coated glass reduces the reflectivity of a product through the collocation of the composite film layer structure and the film layer thickness, and the outdoor reflectivity is less than 7, so that light pollution is effectively prevented; the appearance of the coated glass is amber, and the appearance color of glass products on the market is enriched.
Description
Technical Field
The invention relates to the field of glass production, in particular to amber medium-transmittance low-reflection double-silver energy-saving coated glass and a preparation method thereof.
Background
The existing engineering glass product is basically blue-gray in appearance and single in color, so that the color of a building looks uniform, and people can easily feel aesthetic fatigue. Along with the increasingly strict requirements of Shanghai environment evaluation systems on the external reflection of LOW-E products for building curtain walls, the current Shanghai areas require more and more projects of curtain wall reflectivity lower than 9%, and the requirements of the products on the reflectivity lower than 9% are met, and the products are rich in appearance color, attractive and attractive, glossy and attractive. The existing color series products developed on the market generally have the problems of higher reflectivity and lower transmittance (the visible light transmittance is lower than 38%), and cannot meet the national standard requirements (the visible light transmittance of curtain walls is required to be higher than 40%), so that popularization cannot be realized, glass meeting the transmittance requirements and the reflectivity requirements needs to be developed, and the appearance colors of the low-reflectivity products can be enriched so as to meet different market requirements.
At present, many production researches on champagne-colored series coated glass exist, but the visible light reflectivity is high, light pollution is easy to cause, and market requirements cannot be met, for example, the invention patent application with publication number of CN106904842A discloses champagne-colored double-silver low-emissivity coated glass, and the color range of a 6mm single glass surface is as follows: r is more than or equal to 14.5 and less than or equal to 17, a is more than or equal to 2 and less than or equal to 2.5,7, b is more than or equal to 8. For example, patent application publication No. CN207468490U discloses champagne-colored double-silver Low-E glass, wherein the reflectance of a single glass surface is about 16%, the color a x g is about 7, and the color b x g is about 28, and the reflectance of the products related to the above two patents is relatively high, and the light pollution is easily caused.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides amber medium-transmittance low-reflection double-silver energy-saving coated glass and a preparation method thereof, which are used for enriching glass colors and reducing reflectivity, and the technical scheme is as follows:
the invention provides amber middle-permeation low-reflection double-silver energy-saving coated glass which comprises a glass substrate and a composite film layer plated on one side surface of the glass substrate, wherein the composite film layer comprises a first functional layer, a first medium protective layer, a second functional layer, a third functional layer, a first protective layer, a third medium protective layer, a fourth functional layer, a second protective layer and a fourth medium protective layer which are sequentially and adjacently compounded from inside to outside on a glass substrate; the first functional layer is an SSTZrOX layer, and the thickness of the SSTZrOX layer is 3.5-5nm.
Further, the first dielectric protection layer is an AZO layer, the second dielectric protection layer is a ZnO layer, and the third dielectric protection layer is a ZnO/ZnSnO layer.
Further, the thickness of the AZO layer is 7-9nm, the thickness of the ZnO layer is 26-34nm, and the total thickness of the ZnO/ZnSnO layer is 38-46nm.
Further, the fourth dielectric protection layer is Si 3 N 4 A composite layer of any one or any plurality of layers of SiNxOy, siOx, tiOx, saidThe thickness of the fourth dielectric protective layer is 15-25nm.
Further, the second functional layer and the fourth functional layer are Ag layers, and the third functional layer is a Cu layer.
Further, the thickness of the second functional layer is 9-10nm, the thickness of the third functional layer is 3-4nm, and the thickness of the fourth functional layer is 4.5-5.5nm.
Further, the first protective layer and the second protective layer are any one layer or any multi-layer composite layer in CrNxOy, crNx, niCrNx, niCrNxOy, niCr; the thickness of the first protective layer is 1.5-2nm, and the thickness of the second protective layer is 1-2nm.
The invention also provides a preparation method of the amber middle-permeation low-reflection double-silver energy-saving coated glass, which comprises the following steps: a magnetron sputtering process is adopted, and a first functional layer of 3.5-5nm, a first dielectric protective layer of 7-9nm, a second dielectric protective layer of 26-34nm, a second functional layer of 9-10nm, a third functional layer of 3-4nm, a first protective layer of 1.5-2nm, a third dielectric protective layer of 38-46nm, a fourth functional layer of 4.5-5.5nm, a second protective layer of 1-2nm and a fourth dielectric protective layer of 15-25nm are plated on a glass substrate adjacently in sequence from inside to outside.
Further, (1) magnetron sputtering a first functional layer: plating a first functional layer SSTZrOX layer on a glass substrate by adopting a magnetron sputtering process, and sputtering a zirconium-doped stainless steel target Fe by using an alternating-current intermediate-frequency power supply and oxygen as reactive gases: zr=80:20, argon oxygen flow ratio 650SCCM-750SCCM:850SCCM-950SCCM;
(2) Magnetron sputtering a first dielectric protection layer: plating a first dielectric protection layer AZO layer on the first functional layer SSTZrOX layer by adopting a magnetron sputtering process, sputtering a ceramic AZO target by using an intermediate frequency alternating current power supply, and using pure argon as sputtering gas, wherein the argon flow ratio is 1400SCCM-1600SCCM;
(3) Magnetron sputtering a second dielectric protection layer: plating a second dielectric protective layer ZnO layer on the first dielectric protective layer AZO layer by using a magnetron sputtering process, sputtering by using an alternating current power supply, and using argon and oxygen as sputtering gases, wherein the gas flow ratio is 650-750SCCM:950-1050SCCM;
(4) Magnetron sputtering a second functional layer: plating a second functional layer Ag layer on the ZnO layer of the second dielectric protective layer by adopting a magnetron sputtering process, sputtering a pure Ag target by using a direct current power supply, and using argon as sputtering gas, wherein the flow rate of the argon is 1100SCCM-1300SCCM;
(5) Magnetron sputtering a third functional layer: plating a third functional layer Cu layer on the second functional layer Ag layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, and taking argon as a process gas, wherein the gas flow is 1100SCCM-1300SCCM;
(6) Magnetron sputtering a first protective layer: plating a first protective layer CrNxOy layer on the third functional layer Cu layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, taking nitrogen as a reaction gas, and infiltrating a small amount of oxygen;
(7) Magnetron sputtering a third dielectric protection layer: plating a third dielectric protective layer ZnO/ZnSnO layer on the first protective layer CrNxOy layer by adopting a magnetron sputtering process, sputtering a Zn/ZnSn target by using an alternating-current medium-frequency power supply and using argon and oxygen as reaction gases, wherein the argon and oxygen flow ratio is 650SCCM-750SCCM:950SCCM-1050SCCM;
(8) Magnetron sputtering a fourth functional layer: plating a fourth functional layer Ag layer on the third dielectric protective layer ZnO/ZnSnO layer by adopting a magnetron sputtering process, and sputtering by using a direct current power supply, wherein the gas flow is 1100SCCM-1300SCCM;
(9) Magnetron sputtering a second protective layer: plating a second protective layer CrNxOy layer on the fourth functional layer Ag layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, taking nitrogen as a reaction gas, and infiltrating a small amount of oxygen;
(10) Magnetron sputtering a fourth dielectric protection layer, and plating a fourth dielectric protection layer Si on the second protection layer CrNxOy layer by adopting a magnetron sputtering process 3 N 4 The layer is formed by sputtering a silicon-aluminum target by using an alternating-current medium-frequency power supply and using argon and nitrogen as reactive gases, wherein the mass percentage of silicon to aluminum is 90:10, and the flow ratio of argon to nitrogen is 650SCCM-750SCCM:850SCCM-950SCCM.
Further, the SSTZrOX layer has a thickness of 3.98nm, the AZO layer has a thickness of 8nm, the ZnO layer has a thickness of 30.2nm, the Ag layer has a thickness of 9.45nm, the Cu layer has a thickness of 3.65nm, the CrNxOy layer has a thickness of 1.98nm, the ZnO/ZnSnO layer has a thickness of 42.1nm, and the Ag layer has a thickness of 9.45nmIs 5.20nm thick, the CrNxOy layer is 1.39nm thick, the Si 3 N 4 The thickness of the layer was 20.5nm.
The technical scheme provided by the invention has the following beneficial effects:
a. the amber medium-transmission low-reflection double-silver energy-saving coated glass developed by the invention has the appearance of amber, and can enrich the appearance color of glass products in the market;
b. the amber middle-permeation low-reflection double-silver energy-saving coated glass reduces the reflectivity of a product by matching a composite film layer structure with the film layer thickness, and the visible light reflectivity outside a chamber of the product is less than 7;
c. the amber low-transmittance and low-reflection double-silver energy-saving coated glass developed by the invention has beautiful and beautiful color, can achieve the transmittance meeting the requirements of laws and regulations, and can effectively reduce the visible light reflectivity and prevent the light pollution phenomenon.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a side view of amber mid-transmission low-reflection double-silver energy-saving coated glass provided by an embodiment of the invention;
FIG. 2 is a graph of test results of a glass surface visible light reflection curve of amber mid-transmission low-reflection double-silver energy-saving coated glass provided by the embodiment of the invention;
fig. 3 is a graph of test results of visible light reflection curves of film surfaces of amber mid-transmission low-reflection double-silver energy-saving coated glass provided by the embodiment of the invention.
Wherein, the reference numerals include: 1-glass substrate, 2-composite film layer, 21-first functional layer, 22-first dielectric protective layer, 23-second dielectric protective layer, 24-second functional layer, 25-third functional layer, 26-first protective layer, 27-third dielectric protective layer, 28-fourth functional layer, 29-second protective layer, 30-fourth dielectric protective layer.
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and the claims of the present invention and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that the embodiments of the invention described herein may be implemented in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, apparatus, article, or device that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed or inherent to such process, method, article, or device.
Glass products with a transmittance between 40% and 60%, referred to as intermediate products; the low reflection referred to in this patent means that the visible reflectance is less than 7.
In one embodiment of the invention, an amber middle-permeation low-reflection double-silver energy-saving coated glass and a preparation method thereof are provided, and the specific structure is shown in fig. 1, and the energy-saving coated glass comprises a glass substrate 1 and a composite film layer 2 plated on one side surface of the glass substrate 1, wherein the composite film layer 2 comprises a first functional layer 21, a first medium protective layer 22, a second medium protective layer 23, a second functional layer 24, a third functional layer 25, a first protective layer 26, a third medium protective layer 27, a fourth functional layer 28, a second protective layer 29 and a fourth medium protective layer 30 which are adjacently compounded in sequence from inside to outside on a glass substrate.
The method comprises the following steps:
the first functional layer, namely the innermost layer, is an SSTZrOX layer, namely a zirconium-doped oxidized stainless steel layer, the refractive index of the film layer is improved during reactive sputtering by doping zirconium in the stainless steel, the refractive index of the film layer can reach about 2.0, the transmittance of a product is further improved, and the film layer can be used for adjusting an amber color layer, so that an amber effect can be obtained. The SSTZrOX layer has a thickness of 3.5-5nm.
The first dielectric protection layer 22 is an AZO layer, namely an aluminum doped zinc oxide layer, which can improve the flatness of the film layer, and is a ZnO, ag, cu layer which is used as a pad to reduce the emissivity, and the thickness of the AZO layer is 7-9nm.
The second dielectric protection layer 23 is a ZnO layer, the thickness of the ZnO layer is 26-34nm,
the second functional layer 24 is an Ag layer, which can effectively reduce emissivity, the thickness of the second functional layer 24 is 9-10nm,
the third functional layer 25 is a Cu layer, i.e. a metallic copper layer, which can improve the transmission color of the film layer and reduce the emissivity, and the thickness of the Cu layer is 3-4nm; the Cu layer has the function of improving energy-saving performance and improving the permeation color of the product.
The first protective layer 26 is any one layer or any multi-layer composite layer in CrNxOy, crNx, niCrNx, niCrNxOy, niCr, so that the wear resistance and oxidation resistance of the film layer can be improved, the silver layer and the copper layer are protected from oxidation, preferably a CrNxOy chromium oxynitride layer, and the thickness of the first protective layer 26 is 1.5-2nm.
The third dielectric protective layer 27 is a ZnO/ZnSnO layer, and can be used for controlling and adjusting the color of the film, and the total thickness of the ZnO/ZnSnO layer is 38-46nm.
The fourth functional layer 28 is an Ag layer, namely a metallic silver layer, is a functional layer, has good conductivity, can effectively reduce the emissivity of the film layer, has the effects of environmental protection and energy saving, and has the thickness of 4.5-5.5nm.
The second protective layer 29 is any one layer or any multi-layer composite layer in CrNxOy, crNx, niCrNx, niCrNxOy, niCr, preferably CrNxOy, namely a chromium oxynitride layer, for improving the wear resistance and oxidation resistance of the film, and the thickness of the second protective layer 29 is 1-2nm.
The fourth dielectric protection layer 30 is Si as the outermost layer 3 N 4 Any one or any multiple of the layers SiNxOy, siOx, tiOx, preferably Si 3 N 4 Layers, i.e. silicon nitride layers, si 3 N 4 The layer is a very hard material, improves the physical properties and scratch resistance of the film, ensures that the whole plating layer has good mechanical durability, and is arranged on the outermost layer as a first barrier for protecting the whole film; the thickness of the fourth dielectric protection layer 30 is 15-25nm.
The further explanation is as follows: the x and y are positive numbers, the protective layer can protect the functional layer from damage, and the medium protective layer can not only protect the functional layer, but also regulate the color.
The invention also provides a method for preparing the amber middle-permeation low-reflection double-silver energy-saving coated glass, which comprises the following steps: a magnetron sputtering process is adopted, and a first functional layer 21 with the thickness of 3.5-5nm, a first dielectric protective layer 22 with the thickness of 7-9nm, a second dielectric protective layer 23 with the thickness of 26-34nm, a second functional layer 24 with the thickness of 9-10nm, a third functional layer 25 with the thickness of 3-4nm, a first protective layer 26 with the thickness of 1.5-2nm, a third dielectric protective layer 27 with the thickness of 38-46nm, a fourth functional layer 28 with the thickness of 4.5-5.5nm, a second protective layer 29 with the thickness of 1-2nm and a fourth dielectric protective layer 30 with the thickness of 15-25nm are plated on a glass substrate 1 adjacently from inside to outside.
The color of each film layer can be regulated, and the finally prepared amber medium-transmittance low-reflection double-silver energy-saving coated glass can be amber (amber comprises light yellow, light golden, lemon yellow, orange yellow, brown yellow, champagne and the like) under the combined action of all film layers, and the amber can be debugged only if the thickness of each film layer is within the range. The amber middle-transmission low-reflection double-silver energy-saving coated glass provided by the invention can adjust the reflectivity to be below 7 through a specific film structure and a specific proportion (film thickness), can effectively reduce light pollution caused by a building, and can even be said to be basically free of light pollution.
The following are specific examples.
Example 1
The structure of the composite film layer 2 on the surface of the glass substrate is as follows: the inner layer of the first functional layer 21 is SSTZrOX, the first dielectric protective layer 22 is AZO, the second dielectric protective layer 23 is ZnO, the second functional layer 24 is Ag, the third functional layer 25 is Cu, the first protective layer 26 is CrNxOy, the third dielectric protective layer 27 is ZnO/ZnSnO, the fourth functional layer 28 is Ag, the second protective layer 29 is CrNxOy, and the fourth dielectric protective layer 30 is Si 3 N 4 A layer.
The thickness of each film layer in the composite film layer 2 is 3.98nm, 8nm, 30.2nm, 9.45nm, 3.65nm, 1.98nm, 42.1nm, 5.20nm, 1.39nm and 20.5nm in sequence.
The preparation method of the amber middle-permeation low-reflection double-silver energy-saving coated glass in the embodiment comprises the following steps:
(1) Plating a first functional layer on a glass substrate (the thickness of the selected glass substrate is 6 mm) by adopting a magnetron sputtering process, and sputtering a zirconium-doped stainless steel target Fe by using an alternating-current intermediate-frequency power supply and oxygen as reaction gases: zr=80:20, argon oxygen flow ratio 650SCCM-750SCCM:850SCCM-950SCCM, argon oxygen flow ratio is preferably 700SCCM:900SCCM, depositing an SSTZrOX layer with a film thickness of 3.98nm, and determining the film forming quality by the argon-oxygen flow ratio in the step;
(2) Plating a first dielectric protection layer AZO layer on the first functional layer SSTZrOX layer by adopting a magnetron sputtering process, sputtering a ceramic AZO target by using an intermediate frequency alternating current power supply, using pure argon as sputtering gas, wherein the argon flow ratio is 1400SCCM-1600SCCM, the argon flow ratio is preferably 1500SCCM, depositing an AZO layer with the thickness of 8nm, and performing sputtering of ZnO, ag, cu layers as a bedding;
(3) Plating a second dielectric protective layer ZnO layer on the first dielectric protective layer AZO layer by adopting a magnetron sputtering process, sputtering by using an alternating current power supply, and sputtering by using Ar and O 2 The gas is used as sputtering gas, and the gas flow ratio is 650-750SCCM:950-1050SCCM, gas flow ratio of 700SCCM:1000SCCM, depositing ZnO layer with film thickness of 30.2 nm;
(4) Plating a second functional layer Ag layer on the ZnO layer of the second dielectric protective layer by adopting a magnetron sputtering process, sputtering a pure Ag target by using a direct current power supply, using argon as sputtering gas, wherein the flow rate of the argon is 1100SCCM-1300SCCM, the flow rate of the argon is preferably 1200SCCM, and depositing an Ag layer with the film thickness of 9.45 nm;
(5) Plating a third functional layer Cu layer on the second functional layer Ag layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, using argon as a process gas, wherein the gas flow is 1100SCCM-1300SCCM, the gas flow is preferably 1200SCCM, and depositing a Cu layer with the film thickness of 3.65 nm;
(6) Plating a first protective layer CrNxOy layer on the third functional layer Cu layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, taking nitrogen as reaction gas, penetrating a small amount of oxygen, and depositing a CrNxOy layer with the film thickness of 1.98 nm;
(7) Plating a third dielectric protective layer ZnO/ZnSnO layer on the first protective layer CrNxOy layer by adopting a magnetron sputtering process, sputtering a Zn/ZnSn target by using an alternating-current medium-frequency power supply and using argon and oxygen as reaction gases, wherein the argon and oxygen flow ratio is 650SCCM-750SCCM:950SCCM-1050SCCM, argon oxygen flow ratio is preferably 700SCCM:1000SCCM, and ZnO/ZnSnO layer with film thickness of 42.1nm is deposited;
(8) Plating a fourth functional layer Ag layer on the ZnO/ZnSnO layer of the third dielectric protective layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, wherein the gas flow is 1100SCCM-1300SCCM, the gas flow is 1200SCCM, and depositing the Ag layer with the film thickness of 5.20 nm;
(9) Plating a second protective layer CrNxOy layer on the fourth functional layer Ag layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, taking nitrogen as reaction gas, penetrating a small amount of oxygen, and depositing a CrNxOy layer with the film thickness of 1.39 nm;
(10) Plating a fourth medium protective layer on the second protective layer CrNxOy layer by adopting a magnetron sputtering process, sputtering a silicon-aluminum target by using an alternating-current medium-frequency power supply and using argon and nitrogen as reactive gases, wherein the mass percentage of silicon-aluminum is 90:10, and the flow ratio of argon to nitrogen is 650SCCM-750SCCM:850SCCM-950SCCM, argon nitrogen flow ratio is preferably 700SCCM:900SCCM, si with a deposited film thickness of 20.5nm 3 N 4 A layer. The metal aluminum Al is used for increasing the conductivity of raw materials in the magnetron sputtering process, and does not participate in the reaction, and the conductivity of the non-metal semiconductor silicon Si is extremely poor, such as not adoptedIncreasing the conductivity by mixing metallic aluminum and Al will not be able to successfully perform magnetron sputtering of Si 3 N 4 A layer.
The amber mid-transmission low-reflection double-silver energy-saving coated Glass prepared in the embodiment is subjected to reflectivity test, the test result of the visible light reflection curve of the Glass surface is shown in fig. 2, the test result of the visible light reflection curve of the film surface is shown in fig. 3 (in fig. 2 and 3, reflection is the reflectivity, wavelength is the wavelength, glass side is the Glass surface, coating side is the film surface; two curves are shown in fig. 2 and 3, one is the theoretical curve, the other is the actual curve, and the actual reflection curve is the result of the coaction when each film layer reaches a certain thickness), and the explanation of the Glass surface and the film surface is as follows: the glass comprises two surfaces which are arranged up and down oppositely, one surface is a film plating surface (namely an energy-saving LOW-E film), the other surface is a glass surface (or a tin surface), a spectrum curve which is reflected by the front view of the glass surface is a glass surface curve (namely a reflection diagram of the outside of the glass chamber facing visible light), and a spectrum curve which is reflected by the front view of the film plating surface is a film surface curve. The curves of fig. 2 and 3 can be quantified by a measuring instrument, giving the following table 1.
Table 1 color values of amber mid-transmission low-reflection double-silver energy-saving coated glass of this example
As is clear from Table 1, the reflectance of the glass surface was 6.55, the reflectance of the film surface was 5.15, and the reflectance was 7 or less; the glass of this color value exhibits an amber color. The visible light transmittance is 46.05, and high visible light transmittance indicates that the light is more natural, so that the illumination cost is reduced; the reduced reflectivity reduces light pollution. a and b are psychological colourimetry, +a represents red, +a represents green, +b represents yellow, -b represents blue, a represents the degree of redness and greenness of transmitted light, b represents the degree of transmission of clear yellow and blueness, R is an abbreviation for reflectivity, R% represents the percentage of reflection of light, and T% is the percentage of transmission of visible light.
In other embodiments, the first protective layer may be any one of CrNx, niCrNx, niCrNxOy, niCr; the fourth dielectric protection layer may be any one of SiNxOy, siOx, tiOx.
The amber middle-permeation low-reflection double-silver energy-saving coated glass developed by the invention has the appearance of amber, is beautiful and glossy, is extremely attractive, and can enrich the appearance color of glass products on the market. The reflectivity of the amber middle-permeation low-reflection double-silver energy-saving coated glass provided by the invention is regulated to be below 7, so that the light pollution caused by a building can be effectively reduced, and even the environment is basically free of light pollution. The amber middle-permeation low-reflection double-silver energy-saving coated glass developed by the invention has beautiful and beautiful color, can effectively reduce visible light reflectivity and prevent light pollution while reaching the transmittance meeting the requirements of laws and regulations, and can be applied to different areas and different requirements.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (4)
1. The amber middle-transmission low-reflection double-silver energy-saving coated glass is characterized by comprising a glass substrate (1) and a composite film layer (2) plated on one side surface of the glass substrate (1), wherein the composite film layer (2) comprises a first functional layer (21), a first medium protective layer (22), a second medium protective layer (23), a second functional layer (24), a third functional layer (25), a first protective layer (26), a third medium protective layer (27), a fourth functional layer (28), a second protective layer (29) and a fourth medium protective layer (30) which are sequentially and adjacently compounded on the glass substrate from inside to outside; the first functional layer (21) is SSTZrO X A layer of SSTZrO X The thickness of the layer is 3.5-5nm; the first dielectric protection layer (22) is an AZO layer, the second dielectric protection layer (23) is a ZnO layer, and the third dielectric protection layer (27) is a ZnO/ZnSnO layer; the thickness of the AZO layer is 7-9nm, the thickness of the ZnO layer is 26-34nm, and the total thickness of the ZnO/ZnSnO layer is 38-46nm;
the fourth medium is protectedThe protective layer (30) is Si 3 N 4 Any one layer or any multiple layers of composite layers in SiNxOy, siOx, tiOx, wherein the thickness of the fourth medium protective layer (30) is 15-25nm;
the second functional layer (24) and the fourth functional layer (28) are Ag layers, and the third functional layer (25) is a Cu layer;
the thickness of the second functional layer (24) is 9-10nm, the thickness of the third functional layer (25) is 3-4nm, and the thickness of the fourth functional layer is 4.5-5.5nm;
the first protective layer (26) and the second protective layer (29) are any one layer or any multi-layer composite layer in CrNxOy, crNx, niCrNx, niCrNxOy, niCr; the thickness of the first protective layer (26) is 1.5-2nm, and the thickness of the second protective layer (29) is 1-2nm.
2. A method for preparing the amber mid-transmission low-reflection double-silver energy-saving coated glass according to claim 1, which is characterized by comprising the following steps:
a magnetron sputtering process is adopted, and a first functional layer of 3.5-5nm, a first dielectric protective layer of 7-9nm, a second dielectric protective layer of 26-34nm, a second functional layer of 9-10nm, a third functional layer of 3-4nm, a first protective layer of 1.5-2nm, a third dielectric protective layer of 38-46nm, a fourth functional layer of 4.5-5.5nm, a second protective layer of 1-2nm and a fourth dielectric protective layer of 15-25nm are plated on a glass substrate adjacently in sequence from inside to outside.
3. The preparation method of the amber medium-transmittance low-reflection double-silver energy-saving coated glass according to claim 2, which is characterized in that,
(1) Magnetron sputtering a first functional layer: plating a first functional layer SSTZrO on a glass substrate by using a magnetron sputtering process X The layer is formed by sputtering a zirconium doped stainless steel target Fe by using an alternating current intermediate frequency power supply and oxygen as reaction gases: zr=80:20, argon oxygen flow ratio 650SCCM-750SCCM:850SCCM-950SCCM;
(2) Magnetron sputtering a first dielectric protection layer: SSTZrO in the first functional layer by using a magnetron sputtering process X Plating on the layerSputtering a ceramic AZO target by using an intermediate frequency alternating current power supply, and using pure argon as sputtering gas, wherein the argon flow ratio is 1400SCCM-1600SCCM;
(3) Magnetron sputtering a second dielectric protection layer: plating a second dielectric protective layer ZnO layer on the first dielectric protective layer AZO layer by using a magnetron sputtering process, sputtering by using an alternating current power supply, and using argon and oxygen as sputtering gases, wherein the gas flow ratio is 650-750SCCM:950-1050SCCM;
(4) Magnetron sputtering a second functional layer: plating a second functional layer Ag layer on the ZnO layer of the second dielectric protective layer by adopting a magnetron sputtering process, sputtering a pure Ag target by using a direct current power supply, and using argon as sputtering gas, wherein the flow rate of the argon is 1100SCCM-1300SCCM;
(5) Magnetron sputtering a third functional layer: plating a third functional layer Cu layer on the second functional layer Ag layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, and taking argon as a process gas, wherein the gas flow is 1100SCCM-1300SCCM;
(6) Magnetron sputtering a first protective layer: plating a first protective layer CrNxOy layer on the third functional layer Cu layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, taking nitrogen as a reaction gas, and infiltrating a small amount of oxygen;
(7) Magnetron sputtering a third dielectric protection layer: plating a third dielectric protective layer ZnO/ZnSnO layer on the first protective layer CrNxOy layer by adopting a magnetron sputtering process, sputtering a Zn/ZnSn target by using an alternating-current medium-frequency power supply and using argon and oxygen as reaction gases, wherein the argon and oxygen flow ratio is 650SCCM-750SCCM:950SCCM-1050SCCM;
(8) Magnetron sputtering a fourth functional layer: plating a fourth functional layer Ag layer on the third dielectric protective layer ZnO/ZnSnO layer by adopting a magnetron sputtering process, and sputtering by using a direct current power supply, wherein the gas flow is 1100SCCM-1300SCCM;
(9) Magnetron sputtering a second protective layer: plating a second protective layer CrNxOy layer on the fourth functional layer Ag layer by adopting a magnetron sputtering process, sputtering by using a direct current power supply, taking nitrogen as a reaction gas, and infiltrating a small amount of oxygen;
(10) Magnetron sputtering a fourth dielectric protection layer, and plating a fourth dielectric protection layer Si on the second protection layer CrNxOy layer by adopting a magnetron sputtering process 3 N 4 The layer is formed by sputtering a silicon-aluminum target by using an alternating-current medium-frequency power supply and using argon and nitrogen as reactive gases, wherein the mass percentage of silicon to aluminum is 90:10, and the flow ratio of argon to nitrogen is 650SCCM-750SCCM:850SCCM-950SCCM.
4. The method for preparing amber medium-transmittance low-reflection double-silver energy-saving coated glass according to claim 3, wherein the SSTZrO X The thickness of the layer is 3.98nm, the thickness of the AZO layer is 8nm, the thickness of the ZnO layer is 30.2nm, the thickness of the Ag layer is 9.45nm, the thickness of the Cu layer is 3.65nm, the thickness of the CrNxOy layer is 1.98nm, the thickness of the ZnO/ZnSnO layer is 42.1nm, the thickness of the Ag layer is 5.20nm, the thickness of the CrNxOy layer is 1.39nm, and the thickness of the Si layer is 3 N 4 The thickness of the layer was 20.5nm.
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