CN113443836B - A glass mirror capable of being tempered off-site and a preparation method thereof - Google Patents
A glass mirror capable of being tempered off-site and a preparation method thereof Download PDFInfo
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- CN113443836B CN113443836B CN202010223327.0A CN202010223327A CN113443836B CN 113443836 B CN113443836 B CN 113443836B CN 202010223327 A CN202010223327 A CN 202010223327A CN 113443836 B CN113443836 B CN 113443836B
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- 239000011521 glass Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000010410 layer Substances 0.000 claims abstract description 250
- 229910052751 metal Inorganic materials 0.000 claims abstract description 72
- 239000002184 metal Substances 0.000 claims abstract description 72
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 42
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 35
- 239000011241 protective layer Substances 0.000 claims abstract description 32
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 239000011651 chromium Substances 0.000 claims abstract description 23
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 19
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 157
- 229910052786 argon Inorganic materials 0.000 claims description 75
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 53
- 239000001301 oxygen Substances 0.000 claims description 53
- 229910052760 oxygen Inorganic materials 0.000 claims description 53
- 238000004544 sputter deposition Methods 0.000 claims description 38
- 229910000838 Al alloy Inorganic materials 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 22
- 238000005477 sputtering target Methods 0.000 claims description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical group [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000005341 toughened glass Substances 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical group O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 28
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 26
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 15
- 239000010936 titanium Substances 0.000 abstract description 15
- 229910052719 titanium Inorganic materials 0.000 abstract description 14
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 12
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 12
- 238000002310 reflectometry Methods 0.000 abstract description 9
- 239000003963 antioxidant agent Substances 0.000 abstract 1
- 230000003078 antioxidant effect Effects 0.000 abstract 1
- 238000007747 plating Methods 0.000 description 19
- 229910001120 nichrome Inorganic materials 0.000 description 16
- 230000008569 process Effects 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000005496 tempering Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000010955 niobium Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000002519 antifouling agent Substances 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material 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
- 230000007935 neutral effect Effects 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000001228 spectrum 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
- C03C17/3639—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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明提供了一种可异地钢化的玻璃镜及其制备方法，涉及建筑镀膜玻璃技术领域。本发明提供的玻璃镜包括玻璃基片、从内向外依次设置在所述玻璃基片上的增强反射层、金属层和保护层；所述增强反射层为从内向外依次设置的氧化铌层和氧化硅层或为从内向外依次设置的氧化钛层和氧化硅层，增强反射层的总厚度为80～170nm；所述金属层为镍铬合金层、金属钛层或金属铬层，金属层的厚度为30～75nm；所述保护层包括氧化硅层、氧化铌层、氧化钛层和氮化硅层中的一层或两层，保护层的厚度为40～80nm。本发明提供的玻璃镜抗氧化能力强、使用寿命长，无污染，膜层牢固度高、安全，可进行异地钢化加工；还具有高的反射率；且制备过程简便。
The present invention provides a glass mirror that can be tempered off-site and a preparation method thereof, and relates to the technical field of architectural coated glass. The glass mirror provided by the present invention comprises a glass substrate, an enhanced reflection layer, a metal layer and a protective layer arranged on the glass substrate in sequence from the inside to the outside; the enhanced reflection layer is a niobium oxide layer and a silicon oxide layer arranged in sequence from the inside to the outside or a titanium oxide layer and a silicon oxide layer arranged in sequence from the inside to the outside, and the total thickness of the enhanced reflection layer is 80 to 170 nm; the metal layer is a nickel-chromium alloy layer, a metal titanium layer or a metal chromium layer, and the thickness of the metal layer is 30 to 75 nm; the protective layer comprises one or two layers of a silicon oxide layer, a niobium oxide layer, a titanium oxide layer and a silicon nitride layer, and the thickness of the protective layer is 40 to 80 nm. The glass mirror provided by the present invention has strong antioxidant ability, long service life, no pollution, high film firmness, safety, can be tempered off-site; it also has high reflectivity; and the preparation process is simple.
Description
Technical Field
The invention relates to the technical field of building coated glass, in particular to a glass mirror capable of being tempered in different places and a preparation method thereof.
Background
The existing glass mirror reflection mainly depends on an aluminized film or a silver film on the surface of glass, but the two metals are easy to oxidize in the atmosphere and have short service life. In order to protect the aluminum film or silver film on the surface of the glass, a layer of thick protective paint is sprayed on the outer side of the film layer, the paint is harmful to human health and causes atmospheric pollution, and due to the existence of the protective paint, the glass mirror is not tempered, so that the strength of the glass mirror is low, the safety risk is brought, and once the glass mirror is damaged, the damage to personnel is possibly brought.
Disclosure of Invention
In view of the above, the present invention aims to provide a glass mirror capable of being tempered in different places and a preparation method thereof. The glass mirror provided by the invention has the advantages of strong oxidation resistance, long service life, no pollution, high film firmness and safety, and can be subjected to remote tempering processing.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a glass mirror capable of being tempered in different places, which comprises a glass substrate, an enhanced reflection layer, a metal layer and a protection layer, wherein the enhanced reflection layer, the metal layer and the protection layer are sequentially arranged on the glass substrate from inside to outside;
The enhanced reflection layer is a niobium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside or a titanium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, and the total thickness of the enhanced reflection layer is 80-170 nm;
The metal layer is a nickel-chromium alloy layer, a metal titanium layer or a metal chromium layer, and the thickness of the metal layer is 30-75 nm;
The protective layer comprises one or two layers of a silicon oxide layer, a niobium oxide layer, a titanium oxide layer and a silicon nitride layer, and the thickness of the protective layer is 40-80 nm.
Preferably, when the enhanced reflection layer is a niobium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, the thicknesses of the niobium oxide layer and the silicon oxide layer are independently 30-85 nm.
Preferably, when the enhanced reflection layer is a titanium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, the thickness of the titanium oxide layer and the thickness of the silicon oxide layer are independently 30-85 nm.
Preferably, the molar ratio of nickel to chromium of the nichrome in the metal layer is 20:80.
Preferably, when the protective layer includes two layers, the protective layer is a silicon oxide layer and a niobium oxide layer which are sequentially disposed from inside to outside, or a titanium oxide layer and a silicon oxide layer which are sequentially disposed from inside to outside, or a niobium oxide layer and a silicon oxide layer which are sequentially disposed from inside to outside, or a silicon oxide layer and a titanium oxide layer which are sequentially disposed from inside to outside.
Preferably, when the protective layer includes two layers of a silicon oxide layer, a niobium oxide layer, a titanium oxide layer, and a silicon nitride layer, each single layer thickness of the two layers is independently 20 to 50nm.
The invention provides a preparation method of the remotely tempered glass mirror, which comprises the following steps:
and sputtering the reinforced reflecting layer, the metal layer and the protective layer on the glass substrate from inside to outside by adopting a magnetron sputtering method to obtain the glass mirror capable of being tempered in different places.
Preferably, the vacuum degree of the sputtering is 1.0X10 -4Pa～5.0×10-7 Pa.
Preferably, when sputtering the niobium oxide layer, the sputtered sputtering target is a Nb 2O5 target, the sputtering gas is argon and oxygen, and the volume ratio of the argon to the oxygen is 1:0.1;
when sputtering the silicon oxide layer, the sputtered sputtering target is a silicon-aluminum alloy target, sputtering gas is argon and oxygen, and the volume ratio of the argon to the oxygen is 1:1;
When the titanium oxide layer is sputtered, the sputtered sputtering target is a TiO 2 target, sputtering gas is argon and oxygen, and the volume ratio of the argon to the oxygen is 1:0.1;
when a nichrome layer is sputtered, the sputtered sputtering target is a nichrome target, and the sputtering gas is argon;
when the metal titanium layer is sputtered, the sputtered sputtering target is a metal titanium target, and the sputtering gas is argon;
When sputtering a metal chromium layer, the sputtered sputtering target is a metal chromium target, and the sputtering gas is argon;
when the silicon nitride layer is sputtered, the sputtered sputtering target is a silicon-aluminum alloy target, sputtering gas is argon and nitrogen, and the volume ratio of the argon to the nitrogen is 1.2:1;
The molar ratio of silicon to aluminum in the silicon-aluminum alloy target is 98:2, and the molar ratio of nickel to chromium in the nichrome target is 20:80.
The invention provides a glass mirror capable of being tempered in different places, which comprises a glass substrate, and an enhanced reflection layer, a metal layer and a protective layer which are sequentially arranged on the glass substrate from inside to outside, wherein the enhanced reflection layer is a niobium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside or a titanium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, the total thickness of the enhanced reflection layer is 80-170 nm, the metal layer is a nichrome layer, a metal titanium layer or a metal chromium layer, the thickness of the metal layer is 30-75 nm, the protective layer comprises one layer or two layers of a silicon oxide layer, a niobium oxide layer, a titanium oxide layer and a silicon nitride layer, and the thickness of the protective layer is 40-80 nm. The glass mirror provided by the invention replaces a common aluminum film or silver film with the nickel-chromium alloy layer, the metal titanium layer or the metal chromium layer, has the functions of increasing the density and enhancing the hardness, and remarkably prolongs the service life of the glass mirror; the invention uses one or two layers of silicon oxide layer, niobium oxide layer, titanium oxide layer and silicon nitride layer as protective layers to replace the conventional protective paint, which is pollution-free and can better protect the metal layer, in the toughening process, the glass body is heated to about 700 ℃ and needs to be rapidly cooled, the protective layers can ensure the bonding strength with the metal layer in the toughening process, can effectively isolate the corrosion of oxygen to the metal layer, and the material characteristics of the protective layers are not changed. Therefore, the glass mirror provided by the invention has the advantages of strong oxidation resistance, long service life, no pollution, high strength, safety, capability of performing remote tempering processing, and high reflectivity and brightness.
The invention provides a preparation method of the glass mirror capable of being tempered in different places, which is simple and convenient to operate and easy for large-scale production.
Drawings
FIG. 1 is a block diagram of a remotely tempered glass mirror according to the present invention, wherein a 1-glass substrate, a 2-enhanced reflective layer, a 3-metal layer, and a 4-protective layer are provided.
Detailed Description
The invention provides a glass mirror capable of being tempered in different places, which comprises a glass substrate, an enhanced reflection layer, a metal layer and a protection layer, wherein the enhanced reflection layer, the metal layer and the protection layer are sequentially arranged on the glass substrate from inside to outside;
The enhanced reflection layer is a niobium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside or a titanium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, and the total thickness of the enhanced reflection layer is 80-170 nm;
The metal layer is a nickel-chromium alloy layer, a metal titanium layer or a metal chromium layer, and the thickness of the metal layer is 30-75 nm;
The protective layer comprises one or two layers of a silicon oxide layer, a niobium oxide layer, a titanium oxide layer and a silicon nitride layer, and the thickness of the protective layer is 40-80 nm.
The glass mirror capable of being tempered in different places comprises a glass substrate. The present invention is not particularly limited, and glass substrates known to those skilled in the art, such as a normal glass substrate and an ultrawhite glass substrate, may be used.
The glass mirror capable of being tempered in different places comprises an enhanced reflection layer arranged on the glass substrate. In the invention, the total thickness of the enhanced reflection layer is preferably 98-144 nm. In the invention, when the enhanced reflection layer is a niobium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, the thicknesses of the niobium oxide layer and the silicon oxide layer are preferably 30-85 nm, more preferably 30-72 nm independently, and when the enhanced reflection layer is a titanium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, the thicknesses of the titanium oxide layer and the silicon oxide layer are preferably 30-85 nm, more preferably 30-72 nm independently. The invention firstly sets a niobium oxide layer or a titanium oxide layer on the glass substrate, then sets a silicon oxide layer, and the formed enhanced reflection layer has the characteristics of enhancing reflection and improving brightness.
The glass mirror capable of being tempered in different places comprises a metal layer arranged on the reinforced reflecting layer, wherein the metal layer is a nichrome layer, a metal titanium layer or a metal chromium layer. In the invention, the thickness of the metal layer is preferably 49-70 nm, and the molar ratio of nickel to chromium of the nichrome in the metal layer is 20:80. The invention replaces the common aluminum film or silver film with the nickel-chromium alloy layer, the metal titanium layer or the metal chromium layer, has the functions of increasing the density and enhancing the hardness, and obviously prolongs the service life of the glass mirror.
The glass mirror capable of being tempered in different places comprises a protective layer arranged on the metal layer. In the present invention, when the protective layer includes two layers, the protective layer is preferably a silicon oxide layer and a niobium oxide layer which are sequentially arranged from inside to outside, a titanium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, a niobium oxide layer and a silicon oxide layer which are sequentially arranged from inside to outside, or a silicon oxide layer and a titanium oxide layer which are sequentially arranged from inside to outside. In the invention, the total thickness of the protective layer is 40-80 nm, preferably 50-60 nm. In the present invention, when the protective layer includes two layers of a silicon oxide layer, a niobium oxide layer, a titanium oxide layer, and a silicon nitride layer, each single layer thickness of the two layers is independently preferably 20 to 50nm, more preferably 25 to 30nm. The invention uses one or two layers of silicon oxide layer, niobium oxide layer, titanium oxide layer and silicon nitride layer as protective layers to replace conventional protective paint, which not only has no pollution, but also can better protect metal layer, so that the glass mirror has the characteristics of oxidation resistance and long service life.
The glass mirror provided by the invention has the advantages of strong oxidation resistance, long service life, no pollution, high strength, safety, capability of performing remote tempering processing, and high reflectivity and brightness.
The invention provides a preparation method of the remotely tempered glass mirror, which comprises the following steps:
and sputtering the reinforced reflecting layer, the metal layer and the protective layer on the glass substrate from inside to outside by adopting a magnetron sputtering method to obtain the glass mirror capable of being tempered in different places.
The present invention is not particularly limited to the apparatus used in the magnetron sputtering method, and may be a magnetron sputtering apparatus known to those skilled in the art. The specific operation method of the magnetron sputtering method is not particularly required, and the operation method well known to those skilled in the art can be adopted. In the present invention, the vacuum degree of the sputtering is preferably 1.0X10 -4Pa～5.0×10-7 Pa, more preferably 5.0X10 -5 Pa.
In the embodiment of the invention, the sputtering target is preferably a Nb 2O5 target, the sputtering gas is preferably argon and oxygen, the volume ratio of the argon to the oxygen is preferably 1:0.1, the introducing amounts of the argon and the oxygen are preferably 500sccm and 50sccm respectively, in the sputtering process, argon atoms of the argon impact the Nb 2O5 target on the target position in an ionized state, and Nb 2O5 is sputtered to form a niobium oxide layer after being deposited, and a small amount of oxygen is supplemented because part of niobium oxide loses oxygen atoms in the sputtering process.
In the present invention, when sputtering a silicon oxide layer, the sputtered sputtering target is preferably a silicon aluminum alloy target, and the sputtering gas is preferably argon and oxygen. In the embodiment of the invention, the molar ratio of silicon to aluminum in the silicon-aluminum alloy target is preferably 98:2, the volume ratio of argon to oxygen is preferably 1:1, and the inflow amounts of the argon and the oxygen are preferably 500sccm respectively. In the sputtering process, argon atoms of argon impact silicon-aluminum alloy on a target position in an ionization state, si atoms in the silicon-aluminum alloy are sputtered out and are oxidized into silicon oxide by oxygen, and a silicon oxide layer is formed after deposition (the aluminum content in the silicon-aluminum alloy target is very low, the aluminum oxide content is usually negligible in the oxidation process, and the aluminum oxide content in a film layer is very low and hardly acts).
In the present invention, when the titanium oxide layer is sputtered, the sputtered sputtering target is preferably a TiO 2 target, the sputtering gas is preferably argon and oxygen, the volume ratio of the argon to the oxygen is preferably 1:0.1, and in the embodiment of the present invention, the inflow amounts of the argon and the oxygen are preferably 500sccm and 50sccm, respectively. In the sputtering process, argon atoms of argon impact TiO 2,TiO2 on a target in an ionization state to be sputtered and deposited to form a titanium oxide layer, and part of titanium oxide loses oxygen atoms in the sputtering process, so that a small amount of oxygen is supplemented.
In the present invention, when the nichrome layer is sputtered, the sputtered sputtering target is preferably a nichrome target, and the sputtering gas is preferably argon. In the present invention, the molar ratio of nickel to chromium in the nichrome target is preferably 20:80. In the embodiment of the invention, the argon gas is preferably introduced in an amount of 1000sccm. In the sputtering process, argon atoms of argon impact the nichrome on the target in an ionization state, ni atoms and Cr atoms in the nichrome are sputtered, and a nichrome layer is formed after deposition.
In the present invention, when the metallic titanium layer is sputtered, the sputtered sputtering target is a metallic titanium target and the sputtering gas is argon gas. In the present invention, the argon gas is preferably introduced in an amount of 1000sccm. In the sputtering process, argon atoms of argon impact metal titanium on a target in an ionization state, the titanium atoms are sputtered, and a metal titanium layer is formed after deposition.
In the present invention, when the metal chromium layer is sputtered, the sputtered sputtering target is a metal chromium target and the sputtering gas is argon gas. In the present invention, the argon gas is preferably introduced in an amount of 1000sccm. In the sputtering process, argon atoms of argon impact metal chromium on a target in an ionization state, and the chromium atoms are sputtered out to form a metal chromium layer after deposition.
In the present invention, when the silicon nitride layer is sputtered, the sputtered sputtering target is preferably a silicon aluminum alloy target, and the sputtering gas is preferably argon and nitrogen. In the embodiment of the invention, the molar ratio of silicon to aluminum in the silicon-aluminum alloy target is preferably 98:2, the volume ratio of argon to nitrogen is preferably 1.2:1, and the inflow amounts of the argon and the oxygen are preferably 600sccm and 500sccm respectively. In the sputtering process, argon atoms of argon impact silicon-aluminum alloy on a target position in an ionization state, si atoms in the silicon-aluminum alloy are sputtered out to encounter nitrogen to form silicon nitride, and a silicon nitride layer is formed after deposition (the aluminum content in the silicon-aluminum alloy target is very low, the aluminum nitride content is negligible in the nitriding process generally, and the aluminum nitride content in a film layer is very low and hardly acts).
The preparation method of the glass mirror capable of being tempered in different places is simple and convenient to operate and easy to produce in large scale.
The present invention provides a glass mirror capable of being tempered in different places and a method for manufacturing the same, which are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Placing a glass substrate into a chamber of a magnetron sputtering device, pumping the chamber to a vacuum degree of 1.0X10 -4 Pa, firstly plating a first target-niobium oxide target (Nb 2O5), adding argon and oxygen with a volume ratio of 1:0.1 (argon 500sccm and oxygen 50 sccm), and then plating a second target-silicon-aluminum alloy target (Si and Al molar ratio is 98:2), adding argon and oxygen with a volume ratio of 1:1 (argon 500sccm and oxygen 500 sccm), wherein the thickness of the film is 70nm, and forming an enhanced reflecting layer on the glass substrate;
plating a third target-nichrome target (the molar ratio of Ni to Cr is 20:80) on the enhanced reflecting layer, adding pure argon (1000 sccm), and forming a metal layer on the enhanced reflecting layer, wherein the thickness of the film layer is 70 nm;
Plating a fourth target-silicon aluminum alloy target (the molar ratio of Si to Al is 98:2) on the metal layer, adding argon and oxygen with the volume ratio of 1:1 (argon 500sccm and oxygen 500 sccm), and the thickness of the film layer of 20nm, plating a fifth target-niobium oxide target (Nb 2O5), adding argon and oxygen with the volume ratio of 1:0.1 (argon 500sccm and oxygen 50 sccm), and forming a protective layer on the metal layer with the thickness of 20nm, thereby finally obtaining the glass mirror capable of being tempered in different places.
Example 2
Placing a glass substrate into a chamber of a magnetron sputtering device, pumping the chamber to a vacuum degree of 1.0X10 -4 Pa, firstly plating a first titanium oxide target (TiO 2), adding argon and oxygen with a volume ratio of 1:0.1 (argon 500sccm and oxygen 50 sccm), and a film thickness of 35nm, then plating a second target-silicon-aluminum alloy target (Si and Al molar ratio of 98:2), adding argon and oxygen with a volume ratio of 1:1 (argon 500sccm and oxygen 500 sccm), and a film thickness of 70nm, thereby forming an enhanced reflection layer on the glass substrate;
Plating a third target-nichrome target (the molar ratio of Ni to Cr is 20:80) on the enhanced reflecting layer, adding pure argon (1000 sccm), and forming a metal layer on the enhanced reflecting layer, wherein the thickness of the film layer is 70 nm;
Plating a fourth target-silicon aluminum alloy target (the molar ratio of Si to Al is 98:2) on the metal layer, adding argon and oxygen with the volume ratio of 1:1 (argon 500sccm and oxygen 500 sccm), and the thickness of the film layer of 20nm, plating a fifth target-niobium oxide target (Nb 2O5), adding argon and oxygen with the volume ratio of 1:0.1 (argon 500sccm and oxygen 50 sccm), and forming a protective layer on the metal layer with the thickness of 20nm, thereby finally obtaining the glass mirror capable of being tempered in different places.
Example 3
Placing a glass substrate into a chamber of a magnetron sputtering device, pumping the chamber to a vacuum degree of 1.0X10 -4 Pa, firstly plating a first niobium oxide target (Nb 2O5), adding argon and oxygen with a volume ratio of 1:0.1 (argon 500sccm and oxygen 50 sccm), and a film thickness of 35nm, then plating a second target-silicon-aluminum alloy target (Si and Al molar ratio of 98:2), adding argon and oxygen with a volume ratio of 1:1 (argon 500sccm and oxygen 500 sccm), and a film thickness of 70nm, thereby forming an enhanced reflection layer on the glass substrate;
Plating a third target-nichrome target (the molar ratio of Ni to Cr is 20:80) on the enhanced reflecting layer, adding pure argon (1000 sccm), controlling the thickness of the film layer to be 70nm, and forming a metal layer on the enhanced reflecting layer;
Plating a fourth target-silicon-aluminum alloy target (the molar ratio of Si to Al is 98:2) on the metal layer, adding argon and nitrogen with the volume ratio of 1.2:1 (argon 600sccm and oxygen 500 sccm), forming a protective layer on the metal layer, and finally obtaining the glass mirror capable of being tempered in different places.
Example 4
Placing a glass substrate into a chamber of a magnetron sputtering device, pumping the chamber to a vacuum degree of 1.0X10 -4 Pa, firstly plating a first niobium oxide target (Nb 2O5), adding argon and oxygen with a volume ratio of 1:0.1 (argon 500sccm and oxygen 50 sccm), and a film thickness of 35nm, then plating a second target-silicon-aluminum alloy target (Si and Al molar ratio of 98:2), adding argon and oxygen with a volume ratio of 1:1 (argon 500sccm and oxygen 500 sccm), and a film thickness of 70nm, thereby forming an enhanced reflection layer on the glass substrate;
plating a third target-metal titanium target (Ti) on the enhanced reflection layer, adding pure argon (1000 sccm), and forming a metal layer on the enhanced reflection layer, wherein the thickness of the film layer is 60 nm;
Plating a fourth target-silicon aluminum alloy target (the molar ratio of Si to Al is 98:2) on the metal layer, adding argon and oxygen with the volume ratio of 1:1 (argon 500sccm and oxygen 500 sccm), and the thickness of the film layer of 20nm, plating a fifth target-niobium oxide target (Nb 2O5), adding argon and oxygen with the volume ratio of 1:0.1 (argon 500sccm and oxygen 50 sccm), and forming a protective layer on the metal layer with the thickness of 20nm, thereby finally obtaining the glass mirror capable of being tempered in different places.
The glass mirrors prepared in examples 1 to 4 were subjected to performance test before and after tempering under the conditions of 680 to 700 ℃ heating temperature, 240 to 270 seconds heating time, cooling air pressure of 1.8KPa/cm 2, and cooling time of 160 to 200 seconds, and the performance test results are shown in Table 1:
table 1 results of Performance test of the glass mirror prepared in examples 1 to 4 before and after tempering
| Experimental details | Example 1 | Example 2 | Example 3 | Example 4 |
| Reflectivity before tempering% | 73.2 | 73.5 | 73.4 | 65.2 |
| Reflectivity after tempering is% | 71.4 | 58 | 62 | 52 |
| Salt spray test after tempering | Grade 10 | Grade 10 | Level 8 | Level 8 |
| Hundred grid test before tempering | 5B | 5B | 5B | 5B |
| Hundred grid test after tempering | 5B | 4B | 4B | 4B |
In Table 1, the reflection detecting instrument used for measuring the reflectivity is a GSTR spectrum transreflective on-line scanning measuring system, and the reflectivity test result shows that the reflectivity of the glass mirror is higher after being toughened, which indicates that the glass mirror provided by the invention can be toughened with good toughening effect;
According to the salt spray test, the standards are GB/6458-86 (neutral salt spray test standard) and GB/T6461-2002 (the grades of samples and test pieces on a metal substrate and after corrosion tests of other inorganic coating layers), the test time is 950 hours, and the glass mirror provided by the invention can be toughened through the salt spray test, and the service life of the toughened glass mirror is longer (more than 8 grades are qualified and 10 grades are excellent);
According to the hundred grid test of GB/9286-1998 (hundred grid test standard), the glass mirror provided by the invention has better firmness before and after tempering, and can effectively protect the metal reflecting layer (5B is judged to be excellent and 4B is qualified).
The embodiment shows that the glass mirror provided by the invention has the advantages of strong oxidation resistance, long service life, high film firmness, safety, capability of performing remote tempering processing, no pollution and high reflectivity.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
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| CN114879284A (en) * | 2022-05-05 | 2022-08-09 | 广东轻工职业技术学院 | Anti-dazzle light reflecting mirror plated by sputtering method |
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| CN106068467A (en) * | 2013-09-18 | 2016-11-02 | 玻璃与陶瓷研究有限公司卢森堡中心 | Dielectric mirror |
| CN110395914A (en) * | 2019-06-27 | 2019-11-01 | 福建西河卫浴科技有限公司 | It is a kind of can tempering two-sided chromium mirror |
| CN212025201U (en) * | 2020-03-26 | 2020-11-27 | 沙河市峰禾玻璃科技有限公司 | Glass mirror capable of being tempered in different places |
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| CN107098598B (en) * | 2017-04-25 | 2020-07-28 | 江苏秀强玻璃工艺股份有限公司 | Glass for increasing blue chroma of printed decorative glass based on film coating method and preparation method thereof |
| CN208632388U (en) * | 2018-08-08 | 2019-03-22 | 台玻天津玻璃有限公司 | One kind can tempering half mirror |
| CN109539998A (en) * | 2018-12-05 | 2019-03-29 | 陕西理工大学 | A kind of nanometer gap measuring device and method based on light-intensity test |
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| CN106068467A (en) * | 2013-09-18 | 2016-11-02 | 玻璃与陶瓷研究有限公司卢森堡中心 | Dielectric mirror |
| CN110395914A (en) * | 2019-06-27 | 2019-11-01 | 福建西河卫浴科技有限公司 | It is a kind of can tempering two-sided chromium mirror |
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