CN106542745A - Low radiation coated glass containing three layers of infrared reflecting layer and its laminated glass articles - Google Patents
Low radiation coated glass containing three layers of infrared reflecting layer and its laminated glass articles Download PDFInfo
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- CN106542745A CN106542745A CN201610974451.4A CN201610974451A CN106542745A CN 106542745 A CN106542745 A CN 106542745A CN 201610974451 A CN201610974451 A CN 201610974451A CN 106542745 A CN106542745 A CN 106542745A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3615—Coatings of the type glass/metal/other inorganic layers, at least one layer being non-metallic
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3626—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer one layer at least containing a nitride, oxynitride, boronitride or carbonitride
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- 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
- C03C17/3636—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 silicon, hydrogenated silicon or a silicide
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3639—Multilayers containing at least two functional metal layers
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3644—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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3649—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer made of metals other than silver
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3657—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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/216—ZnO
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/251—Al, Cu, Mg or noble metals
- C03C2217/252—Al
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
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Abstract
The present invention relates to the low radiation coated glass used on coating film on glass field, the particularly vehicles, more specifically a kind of high-durability contains the low radiation coated glass and its laminated glass articles of three layers of infrared reflecting layer.Low radiation coated glass containing three layers of infrared reflecting layer includes glass substrate, outwards sets gradually on the glass baseplate surface：First medium layer, the first infrared reflecting layer, second dielectric layer, the second infrared reflecting layer, the 3rd dielectric layer, the 3rd infrared reflecting layer, outermost dielectric layer.The present invention is particularly the geometric thickness and optical thickness of outermost dielectric layer by the thickness of each film layer of appropriate design, on the one hand improves mechanical stability, can substantially reduce scuffing during following process, scratch vestige；On the other hand enhance the ability to bear to chemical corrosivity material；Meanwhile, spectral technique index is improved, and its laminated glass articles maintains good color appearance feature, disclosure satisfy that the requirement of vehicle glass product.
Description
Technical field：
The present invention relates to Low emissivity (low-e) coated glass used on coating film on glass field, the particularly vehicles, more
Specifically a kind of high-durability contains the low radiation coated glass and its laminated glass articles of three layers of infrared reflecting layer.
Background technology：
The lifting realized with the energy-conserving and environment-protective of people and the requirement more and more higher of the comfortableness taken by the vehicles,
Low emissivity (low-e) coated glass is applied to more and more widely as transparent glass window on the vehicles, this is because low
Radiation film coating glass has through visible ray and the ultrared advantage of reflection, such that it is able to significantly reducing air conditioning energy consumption and carrying
High driver and the comfort level of passenger.At present, the transparent glass window for adopting on the vehicles mostly is silver layer as infrared external reflection
The Silver-based low emissivity coated glass of layer, the core material of Silver-based low emissivity coated glass is silver (Ag) layer of a layer or multilamellar,
As silver-colored (Ag) layer is easily corroded and aoxidizes, thus must the upper and lower of silver-colored (Ag) layer all deposited can pass through it is visible
The transparent dielectric layer of light.Generally, the low radiation coated glass with a silver layer is referred to as single silver low-radiation coated glass, has
The low radiation coated glass of two silver layers is referred to as double-silver low-emissivity coated glass, the low radiation coated glass with three silver layers
It is referred to as Three-silver-layer low-radiation coated glass.
In practice, as coating technique is particularly the development of magnetron sputtering technique, occur in that infrared reflection performance is more excellent
Good Three-silver-layer low-radiation coated glass, the film structure of general Three-silver-layer low-radiation coated glass is glass substrate/inner medium layer/the
One silver layer/the first middle dielectric layer/the second silver layer/the second middle dielectric layer/three silver layers/outermost dielectric layer, for being applied to
For Three-silver-layer low-radiation coated glass on the vehicles, its film layer will also allow for the high temperature for withstanding up to 600～700 DEG C
Heat treatment, and certain chemistry and mechanical damage can be born, thus farthest away from glass substrate outermost dielectric layer to silver layer
Protective effect be even more important.Now in the art, outermost dielectric layer generally adopt refractive index for 1.8～2.6 metal-oxide
Or metal nitride, and its geometric thickness is not higher than 100nm, in practice normally no higher than 70nm, this is because traditionally general
All over thinking if more neutral appearance color and sufficiently high production efficiency cannot be obtained from bigger thickness.Such as China
Patent CN102092959A discloses a kind of high-sunshade Three-silver-layer low-radiation coated glass containing three layers of compound anti-reflection layer, its membrane system
Structure is outwards followed successively by from glass substrate：Compound anti-reflection layer (1)/silver layer (1)/protective layer (1)/compound anti-reflection layer (2)/silver layer
(2)/protective layer (2)/compound anti-reflection layer (3)/silver layer (3)/protective layer (3)/dielectric layer (1), dielectric layer (1) is Si3N4,
Its thicknesses of layers is 10～100nm.For above-mentioned low emissivity glass, its using, manufacture and research process in be found
Yet suffer from following shortcoming：1st, mechanical stability is not enough, and the defects such as scuffing, scratch are easily produced during following process；2、
Chemical stability is not enough, the aqueous vapor, corrosive gas in air, and not enough the water of cleaning, fingerprint etc. are easily caused film layer and are subject to
Corrosion.These shortcomings reduce the yield rate of Three-silver-layer low-radiation coated glass in practice.
The content of the invention：
The technical problem to be solved is present for above-mentioned Three-silver-layer low-radiation coated glass of the prior art
The shortcomings of mechanical stability deficiency, chemical stability deficiency and not high yield rate, there is provided a kind of to contain three layers of infrared reflecting layer
Low radiation coated glass, while also providing a kind of laminated glass articles containing the low radiation coated glass.
The present invention solves its technical problem and is adopted the technical scheme that：Containing the low-emission coated of three layers of infrared reflecting layer
Glass, including glass substrate, it is characterised in that：Outwards set gradually on the glass baseplate surface,
First medium layer, its geometric thickness are 30～50nm；
First infrared reflecting layer, its geometric thickness are 7～16nm；
Second dielectric layer, its geometric thickness are 55～90nm；
Second infrared reflecting layer, its geometric thickness are 7～16nm；
3rd dielectric layer, its geometric thickness are 55～90nm；
3rd infrared reflecting layer, its geometric thickness are 7～16nm；
Outermost dielectric layer, its geometric thickness be 150～200nm, optical thickness be 300～360nm, refractive index be 1.7～
2.6, the material of the outermost dielectric layer be selected from Zn, Sn, Ti, Nb, Zr, Hf, Mg, Ni, In, Al, Ga, W, Bi metal-oxide and
At least one in its mixture, or be selected from Si, Al, Zr, Ti, Y, Hf, Nb, Ta metal nitride or nitrogen oxides and its mix
At least one in compound.
Further, first infrared reflecting layer, the second infrared reflecting layer or the 3rd infrared reflecting layer selected from silver, gold,
At least one in copper, aluminum and its alloy.
Further, the geometric thickness of the outermost dielectric layer is 155～175nm, and optical thickness is 310～350nm.
Further, the outermost dielectric layer includes Si3N4Sublayer, AlN sublayers, ZnSnOx sublayers, ZnO sublayers, TiO2Son
Layer, SnO2Sublayer, WO3Sublayer, Bi2O3Sublayer, HfO2Sublayer and Nb2O5At least one of sublayer.
Further, when outermost dielectric layer includes Si3N4During sublayer, the Si3N4In sublayer doped with Al, Ni, Zr or
Hf。
Further, when outermost dielectric layer include ZnO sublayers when, in the ZnO sublayers doped with Al, Ga, Mo, Mg,
In, F or B.
Further, when outermost dielectric layer include ZnSnOx sublayers when, in the ZnSnOx sublayers doped with Al, Sb,
Mg, Ni or Y.
Further, the first medium layer, second dielectric layer or the 3rd dielectric layer selected from Zn, Si, Sn, Ti, Nb, Zr,
At least one in Hf, Mg, Ni, In, Al, Ga, W, Bi metal-oxide and its mixture, or selected from Si, Al, Zr, Ti, Y,
Hf, Nb, Ta metal nitride or nitrogen oxides and its at least one in mixture.
Further, the first medium layer also includes a ZnO sublayers, and a ZnO sublayers are located at first medium
Between layer and the first infrared reflecting layer.
Further, the second dielectric layer also includes the 2nd ZnO sublayers, and the 2nd ZnO sublayers are located at second medium
Between layer and the second infrared reflecting layer.
Further, the 3rd dielectric layer also includes the 3rd ZnO sublayers, and the 3rd ZnO sublayers are located at the 3rd medium
Between layer and the 3rd infrared reflecting layer.
Further, it is infrared with second between outermost dielectric layer and the 3rd infrared reflecting layer, and/or in the 3rd dielectric layer
Barrier layer is set between reflecting layer, and/or between second dielectric layer and the first infrared reflecting layer, and the geometry of the barrier layer is thick
Spend for 0.3～5nm, the barrier layer is selected from Ni, Cr, Ti, Zn, Sn, Hf, Zr, Al metal and its metal of alloy, non-fully oxygen
At least one in compound, non-fully nitride.
Meanwhile, the present invention also provides a kind of laminated glass articles, including two blocks of glass and is clipped between two blocks of glass
Interbed, it is characterised in that：In two blocks of glass, at least one piece is selected from above-mentioned low radiation coated glass, the low radiation coated glass
Plated film be located near intermediate layer one side.
Due to taking above-mentioned technical proposal, which has the advantages that the present invention：
Low radiation coated glass containing three layers of infrared reflecting layer of the present invention and its laminated glass articles, by closing
The thickness of each film layer of reason design is particularly the geometric thickness and optical thickness of outermost dielectric layer, on the one hand improves mechanically stable
Property, scuffing during following process, scratch vestige can be substantially reduced；On the other hand enhance to chemical corrosivity material
Ability to bear；Meanwhile, spectral technique index is improved, and its laminated glass articles maintains good color appearance feature,
Disclosure satisfy that the requirement of vehicle glass product.
Description of the drawings：
Fig. 1 is the film layer structure schematic diagram of the low radiation coated glass containing three layers of infrared reflecting layer of the present invention；
It is ZnO that Fig. 2 is outermost dielectric layer:Its ZnSnOx thicknesses of layers and normal incidence reflection colour during Al 8nm/ZnSnOx
Coordinate graph of a relation；
It is ZnO that Fig. 3 is outermost dielectric layer:Its ZnSnOx thicknesses of layers and 60 ° of incidence reflection colors during Al 8nm/ZnSnOx
Coordinate graph of a relation；
Fig. 4 is one embodiment structural representation of laminated glass articles of the present invention；
Fig. 5 is another example structure schematic diagram of laminated glass articles of the present invention；
Fig. 6 is the transmitted light spectrogram of embodiment of the present invention 1 and comparative example 1；
Fig. 7 is the reflectance spectrum figure of embodiment of the present invention 1 and comparative example 1；
In figure：1, first medium layer；2, the first infrared reflecting layer；3, second dielectric layer；4, the second infrared reflecting layer；5, the
Three dielectric layers；6, the 3rd infrared reflecting layer；7, outermost dielectric layer；8, the first barrier layer；9, the second barrier layer；10, the 3rd intercepts
Layer；100, glass substrate；101, inner layer glass substrate；102, intermediate layer；103, glass outer substrate；104, it is low-emission coated.
Specific embodiment：
Present disclosure is described further below in conjunction with accompanying drawing, do not fill it is bright in the case of described thicknesses of layers
It is geometric thickness；Wherein, the refractive index value of film layer is the refractive index value at 550nm wavelength, and the optical thickness of film layer is
The product of the geometric thickness of refractive index and film layer at 550nm wavelength.
As shown in figure 1, the low radiation coated glass containing three layers of infrared reflecting layer of the present invention, including glass substrate
100, it is characterised in that：Outwards set gradually on 100 surface of the glass substrate,
First medium layer 1, its geometric thickness are 30～50nm；
First infrared reflecting layer 2, its geometric thickness are 7～16nm；
Second dielectric layer 3, its geometric thickness are 55～90nm；
Second infrared reflecting layer 4, its geometric thickness are 7～16nm；
3rd dielectric layer 5, its geometric thickness are 55～90nm；
3rd infrared reflecting layer 6, its geometric thickness are 7～16nm；
Outermost dielectric layer 7, its geometric thickness be 150～200nm, optical thickness be 300～360nm, refractive index be 1.7～
2.6, the material of the outermost dielectric layer 7 is selected from Zn, Sn, Ti, Nb, Zr, Hf, Mg, Ni, In, Al, Ga, W, Bi metal-oxide
And its at least one in mixture, or be selected from Si, Al, Zr, Ti, Y, Hf, Nb, Ta metal nitride or nitrogen oxides and its
At least one in mixture.
Wherein, outermost dielectric layer 7 is used to protect its other film layer between glass substrate 100, each by appropriate design
The thickness of film layer is particularly the geometric thickness and optical thickness of outermost dielectric layer 7, it is possible to increase the heat stability of membrane system, chemistry are steady
Qualitative and mechanical stability, so as to realize high-durability, and can make final laminated glass articles have neutral color
Reflection appearance.Preferably, the outermost dielectric layer 7 includes Si3N4Sublayer, AlN sublayers, ZnSnOx sublayers, ZnO sublayers, TiO2Son
Layer, SnO2Sublayer, WO3Sublayer, Bi2O3Sublayer, HfO2Sublayer and Nb2O5At least one of sublayer, namely the outermost medium
Layer 7 can be Si3N4Sublayer, AlN sublayers, ZnSnOx sublayers, ZnO sublayers, TiO2Sublayer, SnO2Sublayer, WO3Sublayer, Bi2O3Son
Layer, HfO2Sublayer or Nb2O5Sublayer, it is also possible to which the sublayer more than any two-layer or two-layer in by above-mentioned sublayer is constituted.
Meanwhile, here with outermost dielectric layer 7 as ZnO:It is durable that Al/ZnSnOx citings illustrate height of the present invention
Property the laminated glass articles that constitute of low radiation coated glass there is the reflection appearance of neutral color, wherein ZnO:Al is represented and is doped with
The ZnO sublayers of Al, ZnO:The thickness of Al is 8nm, increases to 400nm from traditional 20nm by changing the thickness of ZnSnOx,
The normal incidence reflection colour and 60 ° of incidence reflection colors of final laminated glass articles are measured respectively, so as to assess ZnSnOx films
Impact of the change of thickness degree to the low angle and high angle reflection colour of its laminated glass articles.In Fig. 2 and Fig. 3, a+ represents red
Color, a- represent green, and b+ represents yellow, and b- represents blueness；It is in coordinate system, more more shallow to the close expression color of coordinate origin,
Otherwise then represent that color is deeper.
As can be seen that when the thickness of ZnSnOx is 40nm (in traditional Three-silver-layer low-radiation coated glass from Fig. 2 and Fig. 3
The typical thickness of ZnSnOx) when, the reflection colour of the low angle of its laminated glass articles and 60 degree is green and lavender respectively；
When being even up to hundreds of nanometers with the increase of the thickness of ZnSnOx, in most thickness ranges, its laminated glass articles
Reflection colour inaesthetic color is presented, for example as can be seen from Figure 2 the thickness of ZnSnOx be 80nm when its interlayer glass
The normal incidence reflection colour of glass product is dark green, and during 120nm, the normal incidence reflection colour of its laminated glass articles is in yellow,
During 180nm, the normal incidence reflection colour of its laminated glass articles is dark green；Or high angle observation and low angle when observing are in
Existing significant color distortion, such as the normal incidence reflection colour of its laminated glass articles when the thickness of ZnSnOx is 180nm in Fig. 2
It is dark green, and 60 ° of incidence reflection colors of its laminated glass articles are presented aobvious when in Fig. 3, the thickness of ZnSnOx is 180nm
What is write is light blue.Based on this, due to the front as the transparent glass window on the vehicles, particularly automobile, skylight, rear shelves or
Side window often requires that the colored appearance for having neutrality or certain pleasant when observing in low angle and high angle, such as bluish-green
Color, light blue or bluish violet, the thickness of traditional ZnSnOx have practical value, but simply increase the thickness of ZnSnOx then very
It is difficult to obtain the laminated glass articles with practical value.Conversely, in the present invention, the thickness by each film layer of appropriate design is special
The geometric thickness and optical thickness of outermost dielectric layer 7, such as the thickness of the ZnSnOx illustrated in Fig. 2 and Fig. 3 be 155nm, 160
When its laminated glass articles normal incidence reflection colour in pale blue green, 60 ° of incidence reflection colors are in muted color；Now, when
When the thickness of ZnSnOx is 155nm or 160nm, the geometric thickness of corresponding outermost dielectric layer 7 is 163nm or 168nm, optics thickness
Spend for 334nm or 344nm.It is visible with reference to Fig. 2 and Fig. 3, ZnSnOx thickness be 155nm or 160nm near, exist one it is thick
Degree scope, can make its laminated glass articles reflection colour when low angle and high angle are observed basically identical and have to make us pleased
The thickness in two dotted ellipse regions in happy appearance color, i.e. Fig. 2 and Fig. 3, the geometric thickness of preferred outermost dielectric layer 7 is
150～175nm, optical thickness is 310～340nm, and the thickness of outermost dielectric layer 7 is arranged on what the membrane system in the range of this built
Laminated glass product has great practical value.It must be noted that the thickness of outermost dielectric layer 7 is arranged except with reference to conventional three silver medals
Outside the technical scheme that mentality of designing and the present invention are provided, even if carrying out to the thickness of other dielectric layer film layers and infrared reflecting layer
Global optimization is arranged, and can not obtain the qualified laminated glass articles of spectral technique index and color characteristics.
Preferably, in order to further optimize film performance, outermost dielectric layer 7 can be worked as comprising Si3N4It is during sublayer, described
Si3N4Doped with Al, Ni, Zr or Hf in sublayer.Equally, when outermost dielectric layer 7 includes ZnO sublayers, mix in the ZnO sublayers
It is miscellaneous to have Al, Ga, Mo, Mg, In, F or B；When outermost dielectric layer 7 include ZnSnOx sublayers when, in the ZnSnOx sublayers doped with
Al, Sb, Mg, Ni or Y.
Wherein, first infrared reflecting layer 2, the second infrared reflecting layer 4 or 6 major function of the 3rd infrared reflecting layer are to use
In reflection infrared ray, reduce infrared ray and transmit from low radiation coated glass, so first infrared reflecting layer 2, second is red
The film material of outer reflective layer 4 or the 3rd infrared reflecting layer 6 can select any material for being capable of reflecting infrared energy, for example
At least one of (but being not limited to) in silver, gold, copper, aluminum and its alloy, is preferably the conjunction of silver or argentiferous in the present invention
The alloy of gold, wherein argentiferous is preferably the alloy of silver and at least one of gold, aluminum, copper in the present invention.In the enforcement of the present invention
Silver has been selected in example, radiance can have effectively been reduced, heat-proof quality has been improved.
Wherein, the first medium layer 1, second dielectric layer 3 or the 3rd dielectric layer 5 can reduce the anti-of visible region
Penetrate, suitable growth basis is provided for infrared reflecting layer and keep the high-temperature stability of infrared reflecting layer.Also, first medium layer
1 due to 100 directly contact of glass substrate, additionally it is possible to intercept Na atoms in glass substrate 100, oxygen atom and other impurities former
Intrusion of the son to infrared reflecting layer is destroyed, and for enough adhesions are provided between low radiation film and glass substrate 100.It is excellent
Selection of land, the first medium layer 1, second dielectric layer 3 or the 3rd dielectric layer 5 selected from selected from Zn, Si, Sn, Ti, Nb, Zr, Hf, Mg,
At least one in Ni, In, Al, Ga, W, Bi metal-oxide and its mixture, or selected from Si, Al, Zr, Ti, Y, Hf, Nb,
Ta metal nitrides or nitrogen oxides and its at least one in mixture.Further, the first medium layer 1 also includes the
One ZnO sublayers 11, a ZnO sublayers 11 are located between first medium layer 1 and the first infrared reflecting layer 2.Similarly, it is described
Second dielectric layer 3 also includes the 2nd ZnO sublayers 31, and the 2nd ZnO sublayers 31 are located at second dielectric layer 3 and the second infrared external reflection
Between layer 4.Meanwhile, the second dielectric layer 5 also includes the 2nd ZnO sublayers 51, and the 2nd ZnO sublayers 51 are located at second medium
Between layer 5 and the second infrared reflecting layer 6.
Alternatively, the 3rd barrier layer 10 is set between outermost dielectric layer 7 and the 3rd infrared reflecting layer 6, and/or the 3rd
Second barrier layer 9 is set between dielectric layer 5 and the second infrared reflecting layer 4, and/or in second dielectric layer 3 and the first infrared external reflection
First barrier layer 8 is set between layer 2, the geometric thickness of first barrier layer 8, the second barrier layer 9 and the 3rd barrier layer 10 is
0.3～5nm, first barrier layer 8, the second barrier layer 9 and the 3rd barrier layer 10 are selected from Ni, Cr, Ti, Zn, Sn, Hf, Zr, Al
At least one in metal Deng metal and its alloy, non-fully oxide, non-fully nitride.
Laminated glass articles of the present invention as shown in Figure 4 and Figure 5, including two blocks of glass and be clipped in two blocks of glass it
Between intermediate layer 102, two blocks of glass are respectively inner layer glass substrate 101 and glass outer substrate 103；In the diagram, glass outer
It is low that one side on substrate 103 near intermediate layer 102 arranges the glass outer of low-emission coated 104, i.e. this laminated glass articles
Radiation film coating glass；In Figure 5, the one side on inner layer glass substrate 101 near intermediate layer 102 arranges low-emission coated 104,
Be this laminated glass articles inner layer glass be low radiation coated glass.Thus, the laminated glass articles of present invention protection, including
Two blocks of glass and the intermediate layer 102 being clipped between two blocks of glass, wherein, in two blocks of glass at least one piece selected from above-described low
Radiation film coating glass, the plated film of the low radiation coated glass are located at the one side near intermediate layer 102.
In order to illustrate in greater detail and more support to cogency the inventive point of the present invention, some embodiments are now enumerated detailed
Illustrate.
Embodiment 1-3
Low radiation coated glass containing three layers of infrared reflecting layer of the present invention, it is set forth below for embodiment in
Three infrared reflecting layers are silver layer, namely Three-silver-layer low-radiation coated glass, now enumerate embodiment 1～3 and corresponding comparative example 1
～2 are compared explanation technical solution of the present invention in spectrum, machinery, improvement effect chemically and thermally in stability.
With the white glass of sodium-calcium-silicate float glass process that thickness is 2.1 millimeters as glass substrate, through cutting, edging, washing and dry
After the operation such as dry, coated film deposition is carried out into magnetron sputtering plating line, background vacuum is higher than 6 × 10-4Pa, on the glass substrate
It is sequentially depositing film layer as shown in Table 1 and Table 2.In these film layers in addition to Ag is deposited using pulse direct current sputtering flat target, remaining
Film layer is deposited using medium frequency reactive sputtering rotary target in oxidizing atmosphere or nitriding atmosphere, by controlling the work(on each target
The control of rate, gas ratio and movement velocity obtains the film layer of suitable thickness.
Table 1：Comparative example 1-2 and embodiment 1-3 film layer structure
Automobile laminated safety glass production technology of the low radiation coated glass that plated film in table 1 is completed according to standard, example
Such as include big or small slice pairing, high-temperature molding and close the techniques such as piece, be finally made laminated glass articles of the present invention.Meanwhile,
With reference to ISO9050：2003 and D65 (10 degree) canonical measures and its dominant spectral index of calculating, as a result as shown in table 2.
Table 3：The dominant spectral index of the laminated glass articles that comparative example 1-2 and embodiment 1-2 are obtained
Wherein：TL is visible transmission ratio；Tds is the direct transmittance of sunlight；Tts is total solar energy transmittance；RL is
Visible light reflectance；Rds is the direct reflectivity of sunlight；L*a*b* is color space coordinate.
Contrasted from table 1, the outermost dielectric layer thickness for differring primarily in that embodiment 1 of comparative example 1 and embodiment 1 reaches
To 157nm, its optical thickness is about 321nm, and 1 optical design of comparative example is according to traditional design theory, and its dielectric layer combines 1 film
Thick is 37.7nm, and its optical thickness is about 76nm.The first medium layer 1 of comparative example 1 and embodiment 1, second dielectric layer 3 and the 3rd
The thickness of dielectric layer 5 has all reached preferable spectral target and neutral appearance through optimization.As seen from Table 2, comparative example 1
The spectral targets such as Tds, Rds and Tts are poor, fail to reach higher product standard (such as Tds≤35%, Tts≤41%)；Knot
Close Fig. 6 and Fig. 7 analyses to obtain, embodiment 1 can reach preferable spectral target, be embodied near infrared band (780-1200nm) model
There is in enclosing higher infrared external reflection ability.It can be seen that technical solution of the present invention can be issued to preferably in silver thickness thinner case
Spectral target, it is and poor according to the three-silver low radiation coated laminated glass spectral target of traditional design theory.
Meanwhile, the embodiment 2 and contrast 2 of Tables 1 and 2 are analyzed and can be obtained：The three-silver low radiation plated film of traditional structure
Increasing Ag layer gross thickness (35.8nm) in the comparative example 2 of laminated glass as far as possible and optimizing each film layer causes laminated glass to have conjunction
The spectrum and colour index of lattice；Comparatively speaking, the laminated glass embodiment 2 of the three silverskin system scheme constructses that the present invention is provided exists
Equal spectral target is reached just in the case of Ag layers gross thickness only 31.8nm.TL is guaranteed in embodiment 3>70% and just entering
Penetrate and under the premise of 60 degree of incidence reflection Color Neutrals, increase Ag layer gross thickness (36.1nm) as far as possible, resulting key technology refers to
The mark such as index such as Tds, Rds and Tts is superior to comparative example 2, it can be seen that the three-silver low radiation plating that technical solution of the present invention is provided
Film laminated glass, with than the more preferable spectral technique index of traditional three-silver low radiation coated laminated glass.
Below, to embodiment 1-3 and comparative example 1-2 mechanical performance, heat stability and chemical stability are estimated, and
Acquired results are recorded in table 3.
In terms of heat stability, due to the low radiation coated glass in table 1 under equal Technology for Heating Processing outward appearance, sheet resistance without aobvious
Difference is write, therefore its thermal stability difference is assessed by measuring mist degree.
Mechanical properties, it is main to investigate the ability that film layer bears frictional dissipation, including manual friction is assessed and Taper grinds
Consumption assessment.Using the clean cotton for dipping in ethanol, finger is pressed against on face and rubs repeatedly, and one back and forth for wherein manual friction assessment
Friction is designated as 1 time, continuous friction 40 times, is scored according to the destruction situation of face as follows：
1 point dabs i.e. demoulding
2 points firmly wipe demoulding
3 points of slight demouldings
4 points without demoulding, only slight scuffing
5 points of face outward appearances are good, destroy without macroscopic
For heat-treatment sample, also using on straight line abrasion instrument, load 1N/cm is set2, mud is dipped in non-dust cloth enter
Row abrasion, reciprocal 200 back and forth, determines the mist degree after its abrasion, calculates its increment value.
In terms of chemical stability, the low radiation coated glass in table 1 is exposed to 170 under corrosive neutral salt spray atmosphere
Hour, assess its cosmetic variation.
Table 3：Comparative example 1-4 and embodiment 1-4 heat treatment, mechanically and chemically stability assessment
From table 3, it is steady that the embodiment 1 of technical solution of the present invention, embodiment 2 and embodiment 3 present preferably heat
It is qualitative, after high-temperature heat treatment face there is not presentation quality deterioration, situations such as level of haze is relatively low, on the whole with comparative example 1, right
Ratio 2 is suitable, it is seen that the technical scheme membrane system heat stability and three traditional silverskin system heat stability that the present invention is provided is suitable.
From table 3, the film layer after the embodiment 1 of technical solution of the present invention, 3 heat treatment of embodiment 2 and embodiment is in
Existing excellent abrasion performance property, in the case of equal abrasion, the embodiment 1 and embodiment 2 of technical solution of the present invention shows lower
The degree of wear.
Similarly, the film layer after heat treatment presents excellent resisting salt fog corrosion property, in the case of equal salt air corrosion
The embodiment 1 of technical solution of the present invention, embodiment 2 and embodiment 3 show good corrosion ability to bear, especially through height
The glass that warm is processed.When significantly corroding have occurred in the comparative example 1 and 2 coated glass of comparative example of traditional design, tool
Only there is corrosion failure point in the embodiment 1 and embodiment 2 and embodiment 3 for having thicker outermost dielectric layer.
In a word, based on above-mentioned comparative example 1, comparative example 2 and embodiment 1, the measurement of embodiment 2 and embodiment 3, analysis, ratio
Compared with, it is seen that the low radiation coated glass provided in technical solution of the present invention, there is while high-temperature stability is suitable more preferable light
Spectrum performance indications and machinery, chemical durability.
Present invention embodiment enumerated above is describing film layer structure and corresponding film material, while embodiment
Only list a part, and such as specific depositing operation, parameter, more embodiments and low radiation coated glass is fabricated to
The concrete technology and parameter of laminated glass articles is not described, it is to be appreciated that it is general that these parts not described are all this area
Known to logical technical staff, therefore the part not described does not affect invention which is intended to be protected.
Low radiation coated glass and its laminated glass articles of the above content to three layers of infrared reflecting layer of the present invention
Have been described in detail, but the present invention is not limited to by specific embodiments described above content, so all according to this
Any improvement, equivalent modifications and replacement that bright technical essential is carried out etc., belongs to the scope of protection of the invention.
Claims (13)
1. the low radiation coated glass containing three layers of infrared reflecting layer, including glass substrate, it is characterised in that：In the glass base
Outwards set gradually in plate surface,
First medium layer, its geometric thickness are 30～50nm；
First infrared reflecting layer, its geometric thickness are 7～16nm；
Second dielectric layer, its geometric thickness are 55～90nm；
Second infrared reflecting layer, its geometric thickness are 7～16nm；
3rd dielectric layer, its geometric thickness are 55～90nm；
3rd infrared reflecting layer, its geometric thickness are 7～16nm；
Outermost dielectric layer, its geometric thickness are 150～200nm, and optical thickness is 300～360nm, and refractive index is 1.7～2.6,
The material of the outermost dielectric layer is selected from Zn, Sn, Ti, Nb, Zr, Hf, Mg, Ni, In, Al, Ga, W, Bi metal-oxide and its mixes
At least one in compound, or it is selected from Si, Al, Zr, Ti, Y, Hf, Nb, Ta metal nitride or nitrogen oxides and its mixture
In at least one.
2. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：Described
One infrared reflecting layer, the second infrared reflecting layer or the 3rd infrared reflecting layer in silver, gold, copper, aluminum and its alloy at least one
Kind.
3. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：It is described most
The geometric thickness of outer dielectric layer is 155～175nm, and optical thickness is 310～350nm.
4. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：It is described most
Outer dielectric layer includes Si3N4Sublayer, AlN sublayers, ZnSnOx sublayers, ZnO sublayers, TiO2Sublayer, SnO2Sublayer, WO3Sublayer,
Bi2O3Sublayer, HfO2Sublayer and Nb2O5At least one of sublayer.
5. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 4, it is characterised in that：Work as outermost
Dielectric layer includes Si3N4During sublayer, the Si3N4Doped with Al, Ni, Zr or Hf in sublayer.
6. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 4, it is characterised in that：Work as outermost
When dielectric layer includes ZnO sublayers, doped with Al, Ga, Mo, Mg, In, F or B in the ZnO sublayers.
7. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 4, it is characterised in that：Work as outermost
When dielectric layer includes ZnSnOx sublayers, doped with Al, Sb, Mg, Ni or Y in the ZnSnOx sublayers.
8. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：Described
One dielectric layer, second dielectric layer or the 3rd dielectric layer are golden selected from Zn, Si, Sn, Ti, Nb, Zr, Hf, Mg, Ni, In, Al, Ga, W, Bi
At least one in category oxide and its mixture, or it is selected from Si, Al, Zr, Ti, Y, Hf, Nb, Ta metal nitride or nitrogen oxygen
At least one in compound and its mixture.
9. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：Described
One dielectric layer also includes a ZnO sublayers, and a ZnO sublayers are located between first medium layer and the first infrared reflecting layer.
10. the low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：It is described
Second dielectric layer also includes the 2nd ZnO sublayers, the 2nd ZnO sublayers be located at second dielectric layer and the second infrared reflecting layer it
Between.
11. low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：It is described
3rd dielectric layer also includes the 3rd ZnO sublayers, the 3rd ZnO sublayers be located at the 3rd dielectric layer and the 3rd infrared reflecting layer it
Between.
12. low radiation coated glass containing three layers of infrared reflecting layer according to claim 1, it is characterised in that：Most
Between outer dielectric layer and the 3rd infrared reflecting layer, and/or between the 3rd dielectric layer and the second infrared reflecting layer, and/or
Barrier layer is set between second medium layer and the first infrared reflecting layer, and the geometric thickness of the barrier layer is 0.3～5nm, the resistance
Interlayer be selected from Ni, Cr, Ti, Zn, Sn, Hf, Zr, Al metal and its metal of alloy, non-fully oxide, non-fully in nitride
At least one.
A kind of 13. laminated glass articles, including two blocks of glass and the intermediate layer being clipped between two blocks of glass, it is characterised in that：Two
In block glass, at least one piece is selected from the low radiation coated glass described in claim 1-12 any one, the low-emission coated glass
The plated film of glass is located at the one side near intermediate layer.
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| CN109467320A (en) * | 2018-04-27 | 2019-03-15 | 福耀玻璃(湖北)有限公司 | A kind of on-line coating and film-removing technology of shield glass |
| CN110790516A (en) * | 2019-10-23 | 2020-02-14 | 天津耀皮汽车玻璃有限公司 | Double-sided coated automobile front windshield sandwich glass capable of guaranteeing shooting and recording definition of electronic eyes |
| CN113682007A (en) * | 2021-08-23 | 2021-11-23 | 福耀玻璃工业集团股份有限公司 | Laminated glass with transparent conductive layer and preparation method thereof |
| CN114538792A (en) * | 2022-01-28 | 2022-05-27 | 福建省万达汽车玻璃工业有限公司 | Low-emissivity coated glass with double infrared reflecting layers, laminated glass and vehicle |
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Effective date of registration: 20200928 Address after: 300000 Tianjin city Xiqing District Zhangjiawo Town, Anfu Road No. 13 Patentee after: TIANJIN HONGDE AUTOMOBILE GLASS Co.,Ltd. Address before: Acer Road, Fuqing city Fuzhou City, Fujian Province town 350301 Fuyao Industrial Zone II Patentee before: FUYAO GLASS INDUSTRY GROUP Co.,Ltd. |