CN104290402A - Intermediate reflective three-silver LOW-E glass and preparation method thereof - Google Patents

Intermediate reflective three-silver LOW-E glass and preparation method thereof Download PDF

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Publication number
CN104290402A
CN104290402A CN201410563789.1A CN201410563789A CN104290402A CN 104290402 A CN104290402 A CN 104290402A CN 201410563789 A CN201410563789 A CN 201410563789A CN 104290402 A CN104290402 A CN 104290402A
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layer
rete
thickness
magnetron sputtering
znsno
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Inventor
杨永华
王玲
秦文锋
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Zhongshan Chuangke Scientific Research Technology Services Co Ltd
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Zhongshan Chuangke Scientific Research Technology Services Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/416—Reflective
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/42—Polarizing, birefringent, filtering

Abstract

The invention discloses intermediate reflective three-silver LOW-E glass which comprises a glass substrate, wherein fifteen film layers are sequentially compounded on the compound surface of the glass substrate adjacent to one another from inside to outside; the glass is characterized in that a Si3N4 layer is arranged on the first film layer, namely the innermost layer; the second film layer is a TiO2 layer; the third film layer is a ZnO layer; the fourth film layer is an Ag layer; the fifth film layer is a NiCrOx layer; the sixth film layer is a ZnSnO3 layer; the seventh film layer is a ZnO layer; the eighth film layer is an Ag layer; the ninth film layer is a NiCrOx layer; the tenth film layer is a ZnSnO3 layer; the eleventh film layer is a ZnO layer; the twelfth film layer is an Ag layer; the thirteenth film layer is a NiCr layer; the fourteenth film layer is a ZnSnO3 layer; and the outermost layer, namely the fifteenth layer, is a Si3N4 layer.

Description

Three silver medal LOW-E glass and preparation methods are reflected in one
[technical field]
The present invention relates to a kind of coated glass, be more particularly in one, reflect three silver medal LOW-E glass, the invention still further relates to a kind of preparation method of glass.
[background technology]
Glass plays key player in the production and life in the present age, and glass is all used in the many places of the door and window automotive window of building and windshield etc., brings a lot of convenience to production and life.Middle reflecting glass demand is also very large, but existing middle reflecting glass sunlight transmitance is low, and reflectivity is high, and shading coefficient is high.
[summary of the invention]
The present invention seeks to overcome the deficiencies in the prior art, provide a kind of transmitance high, reflectivity is low, the middle reflection three silver medal LOW-E glass that shading coefficient is little.The present invention also provides a kind of preparation method of middle reflection three silver medal LOW-E glass.
The present invention is achieved by the following technical solutions:
Reflect three silver medal LOW-E glass in one, include glass substrate 1, the composite surface of described glass substrate 1 is adjacent to from inside to outside be successively compounded with 15 retes, it is characterized in that: wherein the first rete and innermost layer are Si 3n 4layer the 21, second rete is TiO 2layer 22, third membrane layer is ZnO layer 23, and the 4th rete is Ag layer the 24, five rete is NiCrO xlayer 25, layer 6 film is ZnSnO 3layer the 26, seven rete is ZnO layer 27, and the 8th rete is Ag layer the 28, nine rete is NiCrO xlayer the 29, ten rete is ZnSnO 3layer the 210, the 11 rete is ZnO layer 211, and the 12 rete is Ag layer 212, and the 13 rete is NiCr layer 213, and the 14 rete is ZnSnO 3layer 214, outermost layer the 15 rete is Si 3n 4layer 215, the Si of described first rete 3n 4the thickness of layer 21 is 8 ~ 15nm, outermost layer the 15 rete Si 3n 4the thickness of layer 215 is 15 ~ 25nm, and layer 6 film is ZnSnO 3the thickness of layer 26 is 78 ~ 85nm, and the tenth rete is ZnSnO 3the thickness of layer 210 is 95 ~ 100nm, and the 14 rete is ZnSnO 3layer 214, thickness is 15 ~ 25nm.
In as above, reflection three silver medal LOW-E glass, is characterized in that the TiO of described second rete 2the thickness of layer 22 is 8 ~ 15nm.
Reflection three silver medal LOW-E glass in as above, it is characterized in that the thickness of described third membrane layer ZnO layer 23 is 15 ~ 20nm, the thickness of the 7th rete ZnO layer 27 is 15 ~ 25nm, and the 11 rete is the thickness of ZnO layer 211 is 8 ~ 14nm.
Reflection three silver medal LOW-E glass in as above, it is characterized in that the thickness of described 4th rete Ag layer 24 is 2 ~ 5nm, the 8th rete is the thickness of Ag layer 28 is 5 ~ 10nm, and the 12 rete is the thickness of Ag layer 212 is 5 ~ 10nm.
In as above, reflection three silver medal LOW-E glass, is characterized in that described 5th rete NiCrO xthe thickness of layer 25 is 1 ~ 3nm, the 9th rete NiCrO xthe thickness of layer 29 is 2 ~ 5nm.
In as above, reflection three silver medal LOW-E glass, is characterized in that the thickness of the 13 rete NiCr layer 213 is 0.5 ~ 2nm.
Prepare a method for above-mentioned middle reflection three silver medal LOW-E glass, it is characterized in that comprising the steps:
(1) magnetron sputtering Si 3n 4layer, makes reacting gas sputtering semi-conducting material SiAl weight ratio Si:Al=90:10 with interchange intermediate frequency power supply, nitrogen, density 96%;
(2) magnetron sputtering TiO 2layer, sputters ceramic titanium target with interchange intermediate frequency power supply;
(3) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(4) magnetron sputtering Ag layer, sputters by AC power;
(5) magnetron sputtering NiCrO xlayer, does reacting gas with nitrogen, oozes a small amount of oxygen, sputter with dc source;
(6) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(7) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(8) magnetron sputtering Ag layer, sputters by AC power;
(9) magnetron sputtering NiCrO xlayer, does reacting gas with nitrogen, oozes a small amount of oxygen, sputter with dc source;
(10) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(11) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(12) magnetron sputtering Ag layer, sputters by AC power;
(13) magnetron sputtering NiCr layer, the metal sputtering of reacting gas of deciding with dc source, argon gas;
(14) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(15) magnetron sputtering Si 3n 4layer, makes reacting gas sputtering semi-conducting material SiAl weight ratio Si:Al=90:10 with interchange intermediate frequency power supply, nitrogen, density 96%.
Compared with prior art, the present invention has the following advantages:
1, this glass utilizes Si 3n 4make basement membrane and teleblem, make rete have good caking property and preferably mechanical strength, utilize TiO 2improve the light transmittance of glass, and with the smooth rete of ZnO, make TiO 2film smooth surface, improves the conductance of later stage silverskin.
2, this glass transmission rate T (through the luminous flux of transparent or semitransparent body and the percentage of its incident flux) >=60%; Reflectivity≤15, shading coefficient SC≤0.38.This glass radiance≤0.03, radiance is the ratio of heat commensurate area black matrix radiations heat energy under identical temperature, the same terms of the unit are radiation of object.Radiance definition is the ability of object absorption or reflecting heat.The radiance of glass is more close to zero, and its heat-insulating property is better.
3, this glass colour manifests silver gray, a*=-3, b*=-6.
[accompanying drawing explanation]
Fig. 1 is structural representation of the present invention.
[detailed description of the invention]
Reflect three silver medal LOW-E glass in one, include glass substrate 1, the composite surface of described glass substrate 1 is adjacent to from inside to outside be successively compounded with 15 retes, wherein the first rete and innermost layer are Si 3n 4layer the 21, second rete is TiO 2layer 22, third membrane layer is ZnO layer 23, and the 4th rete is Ag layer the 24, five rete is NiCrO xlayer 25, layer 6 film is ZnSnO 3layer the 26, seven rete is ZnO layer 27, and the 8th rete is Ag layer the 28, nine rete is NiCrO xlayer the 29, ten rete is ZnSnO 3layer the 210, the 11 rete is ZnO layer 211, and the 12 rete is Ag layer 212, and the 13 rete is NiCr layer 213, and the 14 rete is ZnSnO 3layer 214, outermost layer the 15 rete is Si 3n 4layer 215.
Described innermost layer Si 3n 4layer 21, i.e. silicon nitride layer; Si 3n 4be a kind of adamantine material, improve film hardness and avoid bad atom deeply to destroy silver layer film plating layer, at high temperature heat resistance is better to make whole rete, and mechanicalness is better, it ensures whole coating and has good mechanical endurance.Si 3n 4the thickness of layer 21 is 8 ~ 15nm, nm is nanometer, 1m=10 9nm.
Described second layer TiO 2layer 22, i.e. titanyl compound---titanium dioxide.Adopt the TiO of high index of refraction n=2.5 2being the light transmittance in order to improve glass, reducing the surface resistance of silver layer, reduce the consumption of silver, produce light scattering after LOW-E heat treatment can being reduced again, and glass is neutral color, TiO 2film surface unusual light, thus improves the conductance of silverskin.TiO 2the thickness of layer is 8 ~ 15nm.
Described third layer ZnO layer 23, i.e. zinc oxide film is antireflecting metal oxide layer, improves the conductance of silverskin further simultaneously.Zinc oxide ZnO can be used as flux, reduces the sintering temperature of glass, and as glass coating, reflected infrared ray while allowing visible ray pass through, to reach insulation or heat insulation effect.ZnO layer thickness is 15 ~ 20nm.
Described 4th layer of Ag layer 24, i.e. metallic silver layer, argent provides lower radiance, plays environmental protection and energy saving; Thickness is 2 ~ 5nm.
The NiCrO of described 5th rete xlayer 25; i.e. nickel oxide layers of chrome, nickel oxide layers of chrome, in order to protect silverskin further, is subject to etch to avoid silverskin at reactive sputtering process; also to increase so-called " barrier layer " in thin silverskin one or both sides, for coating, there is very good chemical resistance and mechanical performance.Thickness is 1 ~ 3nm.
Described layer 6 ZnSnO 3layer 26, i.e. zinc oxide tin layers, improves the transmitance of glass, ZnSnO 3thickness be 78 ~ 85nm.
Described layer 7 ZnO layer 27, i.e. zinc oxide film, ZnO layer thickness is 15 ~ 25nm.
Described 8th layer of Ag layer 28, i.e. metallic silver layer, thickness is 5 ~ 10nm.
The NiCrO of described 9th rete xlayer 29, i.e. nickel oxide layers of chrome, thickness is 2 ~ 5nm.
Described ten layer of ZnSnO 3layer 210, i.e. zinc oxide tin layers, ZnSnO 3thickness be 95 ~ 100nm.
Described eleventh floor ZnO layer 211, i.e. zinc oxide film, ZnO layer thickness is 8 ~ 14nm.
Described Floor 12 Ag layer 212, i.e. metallic silver layer, thickness is 5 ~ 10nm.
Described 13 layer of NiCr layer 213, i.e. nickel chromium triangle metal level, as protective layer and the levelling blanket of Ag layer, improves the oxidation that oxidation resistent susceptibility prevents Ag layer.The thickness of NiCr layer is 0.5 ~ 2nm.
Described 14 layer of ZnSnO 3layer 214, i.e. zinc oxide tin layers, ZnSnO 3thickness be 15 ~ 25nm.
Described outermost layer Si 3n 4layer 215, i.e. silicon nitride layer; It ensure whole coating and there is good mechanical endurance.Si 3n 4film is very hard, and scratch resistance, and its hardness is three times of glass, is TiO 2two times; Si 3n 4refractive index be 2.05, absorptivity is almost nil, so it is fit closely as the top layer of Low-e coating.Si 3n 4the thickness of layer is 15 ~ 25nm.
Prepare a method for above-mentioned middle reflection three silver medal LOW-E glass, comprise the steps:
(1) magnetron sputtering Si 3n 4layer, makes reacting gas sputtering semi-conducting material SiAl weight ratio Si:Al=90:10 with interchange intermediate frequency power supply, nitrogen, density 96%;
(2) magnetron sputtering TiO 2layer, sputters ceramic titanium target with interchange intermediate frequency power supply;
(3) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(4) magnetron sputtering Ag layer, sputters by AC power;
(5) magnetron sputtering NiCrO xlayer, does reacting gas with nitrogen, oozes a small amount of oxygen, sputter with dc source;
(6) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(7) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(8) magnetron sputtering Ag layer, sputters by AC power;
(9) magnetron sputtering NiCrO xlayer, does reacting gas with nitrogen, oozes a small amount of oxygen, sputter with dc source;
(10) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(11) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(12) magnetron sputtering Ag layer, sputters by AC power;
(13) magnetron sputtering NiCr layer, the metal sputtering of reacting gas of deciding with dc source, argon gas;
(14) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(15) magnetron sputtering Si 3n 4layer, makes reacting gas sputtering semi-conducting material SiAl weight ratio Si:Al=90:10 with interchange intermediate frequency power supply, nitrogen, density 96%.
Middle reflection three silver medal LOW-E glass improves a lot on solar properties, and three layers of silverskin can make emissivity drop to very low value, and namely heat transfer coefficient drops to low value; And it is while reduction solar energy, still can keep very high visible light transmissivity, so three silver medal LOW-E coating have good selective in solar properties.
LOW-E glass is also called low radiation coated glass.
This glass utilizes TiO 2the surface resistance of silver layer can be reduced, reduce the consumption of silver, produce light scattering after LOW-E heat treatment can being reduced again, Si 3n 4make teleblem and counterdie, improve film hardness and avoid bad atom deeply to destroy silver layer film plating layer, at high temperature heat resistance is better to make whole rete, and mechanicalness is better, has the characteristic to visible ray high transmission and centering far infrared high reverse--bias.
This glass transmission rate T (through the luminous flux of transparent or semitransparent body and the percentage of its incident flux) >=60%; Reflectivity≤15, shading coefficient SC≤0.38.This glass radiance≤0.03, radiance is the ratio of heat commensurate area black matrix radiations heat energy under identical temperature, the same terms of the unit are radiation of object.Radiance definition is the ability of object absorption or reflecting heat.The radiance of glass is more close to zero, and its heat-insulating property is better.
This glass colour manifests silver gray, a*=-3, b*=-6.

Claims (7)

1. reflect three silver medal LOW-E glass in one kind, include glass substrate (1), the composite surface of described glass substrate (1) is adjacent to be compounded with 15 retes from inside to outside successively, it is characterized in that: wherein the first rete and innermost layer are Si 3n 4layer (21), the second rete is TiO 2layer (22), third membrane layer is ZnO layer (23), and the 4th rete is Ag layer (24), and the 5th rete is NiCrO xlayer (25), layer 6 film is ZnSnO 3layer (26), the 7th rete is ZnO layer (27), and the 8th rete is Ag layer (28), and the 9th rete is NiCrO xlayer (29), the tenth rete is ZnSnO 3layer (210), the 11 rete is ZnO layer (211), and the 12 rete is Ag layer (212), and the 13 rete is NiCr layer (213), and the 14 rete is ZnSnO 3layer (214), outermost layer the 15 rete is Si 3n 4layer (215), the Si of described first rete 3n 4the thickness of layer (21) is 8 ~ 15nm, outermost layer the 15 rete Si 3n 4the thickness of layer (215) is 15 ~ 25nm, and layer 6 film is ZnSnO 3the thickness of layer (26) is 78 ~ 85nm, and the tenth rete is ZnSnO 3the thickness of layer (210) is 95 ~ 100nm, and the 14 rete is ZnSnO 3layer (214), thickness is 15 ~ 25nm.
2. middle reflection three silver medal LOW-E glass according to claim 1, is characterized in that the TiO of described second rete 2the thickness of layer (22) is 8 ~ 15nm.
3. middle reflection three silver medal LOW-E glass according to claim 1, the thickness that it is characterized in that described third membrane layer ZnO layer (23) is 15 ~ 20nm, the thickness of the 7th rete ZnO layer (27) is 15 ~ 25nm, and the 11 rete is the thickness of ZnO layer (211) is 8 ~ 14nm.
4. middle reflection three silver medal LOW-E glass according to claim 1, the thickness that it is characterized in that described 4th rete Ag layer (24) is 2 ~ 5nm, 8th rete is the thickness of Ag layer (28) is 5 ~ 10nm, and the 12 rete is the thickness of Ag layer (212) is 5 ~ 10nm.
5. middle reflection three silver medal LOW-E glass according to claim 1, is characterized in that described 5th rete NiCrO xthe thickness of layer (25) is 1 ~ 3nm, the 9th rete NiCrO xthe thickness of layer (29) is 2 ~ 5nm.
6. middle reflection three silver medal LOW-E glass according to claim 1, is characterized in that the thickness of the 13 rete NiCr layer (213) is 0.5 ~ 2nm.
7. prepare a method for the middle reflection three silver medal LOW-E glass described in claim 1-6 any one, it is characterized in that comprising the steps:
(1) magnetron sputtering Si 3n 4layer, makes reacting gas sputtering semi-conducting material SiAl weight ratio Si:Al=90:10 with interchange intermediate frequency power supply, nitrogen, density 96%;
(2) magnetron sputtering TiO 2layer, sputters ceramic titanium target with interchange intermediate frequency power supply;
(3) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(4) magnetron sputtering Ag layer, sputters by AC power;
(5) magnetron sputtering NiCrO xlayer, does reacting gas with nitrogen, oozes a small amount of oxygen, sputter with dc source;
(6) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(7) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(8) magnetron sputtering Ag layer, sputters by AC power;
(9) magnetron sputtering NiCrO xlayer, does reacting gas with nitrogen, oozes a small amount of oxygen, sputter with dc source;
(10) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(11) magnetron sputtering ZnO layer, sputters ceramic Zn target with midfrequent AC power supply, for Ag layer makes place mat;
(12) magnetron sputtering Ag layer, sputters by AC power;
(13) magnetron sputtering NiCr layer, the metal sputtering of reacting gas of deciding with dc source, argon gas;
(14) magnetron sputtering ZnSnO 3layer, with midfrequent AC electric current sputtering ZnSn weight ratio Zn:Sn=48 ~ 52:48 ~ 52;
(15) magnetron sputtering Si 3n 4layer, makes reacting gas sputtering semi-conducting material SiAl weight ratio Si:Al=90:10 with interchange intermediate frequency power supply, nitrogen, density 96%.
CN201410563789.1A 2014-10-18 2014-10-18 Intermediate reflective three-silver LOW-E glass and preparation method thereof Pending CN104290402A (en)

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CN109650743A (en) * 2019-01-17 2019-04-19 吴江南玻华东工程玻璃有限公司 Through the grey three silver medal LOW-E glass of crystal and preparation method thereof of color neutrality
CN110418710A (en) * 2016-12-20 2019-11-05 墨西哥平板玻璃可变资本股份有限公司 Low emissivity coatings for glass baseplate

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* Cited by examiner, † Cited by third party
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CN110418710A (en) * 2016-12-20 2019-11-05 墨西哥平板玻璃可变资本股份有限公司 Low emissivity coatings for glass baseplate
CN108218253A (en) * 2018-01-11 2018-06-29 中建材光电装备（太仓）有限公司 A kind of high-permeability, tempered three silver medal Low-E glass and preparation method thereof
CN108218253B (en) * 2018-01-11 2020-12-11 中建材光电装备（太仓）有限公司 High-permeability tempered three-silver Low-E glass and preparation method thereof
CN109650743A (en) * 2019-01-17 2019-04-19 吴江南玻华东工程玻璃有限公司 Through the grey three silver medal LOW-E glass of crystal and preparation method thereof of color neutrality

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Application publication date: 20150121