CN106542745B - Low radiation coated glass and its laminated glass articles containing three layers of infrared reflecting layer - Google Patents
Low radiation coated glass and its laminated glass articles containing three layers of infrared reflecting layer Download PDFInfo
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- CN106542745B CN106542745B CN201610974451.4A CN201610974451A CN106542745B CN 106542745 B CN106542745 B CN 106542745B CN 201610974451 A CN201610974451 A CN 201610974451A CN 106542745 B CN106542745 B CN 106542745B
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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 especially 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, is set gradually outward on the glass baseplate surface: first medium layer, the first infrared reflecting layer, second dielectric layer, the second infrared reflecting layer, third dielectric layer, third infrared reflecting layer, outermost dielectric layer.The geometric thickness and optical thickness that the present invention is especially outermost dielectric layer by rationally designing the thickness of each film layer, on the one hand improve mechanical stability, can substantially reduce scuffing during following process, scratch trace；On the other hand the ability to bear to chemical corrosivity substance is enhanced；Meanwhile spectral technique index is improved, and its laminated glass articles maintains good color appearance feature, can satisfy the requirement of vehicle glass product.
Description
Technical field:
The present invention relates to Low emissivity (low-e) coated glasses used on coating film on glass field, the especially 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 technique:
As the promotion of the energy conservation and environmental awareness of people and the requirement to the comfort of vehicles seating are higher and higher,
Low emissivity (low-e) coated glass is applied on the vehicles more and more widely as transparent glass window, this is because low
Radiation film coating glass has the advantages that through visible light and reflects infrared ray, so as to significantly reduce air conditioning energy consumption and mention
The comfort level of high driver and passenger.Currently, the transparent glass window used on the vehicles is mostly using 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 one layer or multilayer,
Since silver (Ag) layer is easy to be corroded and aoxidizes, thus must the upper and lower of silver-colored (Ag) layer be all deposited with can penetrate it is visible
The transparent dielectric layer of light.In general, the low radiation coated glass with a silver layer is referred to as single silver low-radiation coated glass, have
The low radiation coated glass of two silver layers is referred to as double-silver low-emissivity coated glass, and there are three the low radiation coated glass of silver layer for tool
Referred to as Three-silver-layer low-radiation coated glass.
In practice, with the development of coating technique especially magnetron sputtering technique, it is more excellent to there is infrared reflection performance
Good Three-silver-layer low-radiation coated glass, the film structure of general Three-silver-layer low-radiation coated glass are glass substrate/inner medium layer/the
One silver layer/the first middle dielectric layer/the second silver layer/second middle dielectric layer/third silver layer/outermost dielectric layer, for being applied to
For Three-silver-layer low-radiation coated glass on the vehicles, film layer will also allow for withstanding up to 600~700 DEG C of high temperature
Heat treatment, and it is able to bear certain chemistry and mechanical damage, therefore farthest away from the outermost dielectric layer of glass substrate to silver layer
Protective effect be even more important.Now in the art, outermost dielectric layer generallys use the metal oxide that refractive index is 1.8~2.6
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 think if selects bigger thickness cannot obtain more neutrality appearance color and sufficiently high production efficiency.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, membrane system
Structure from glass substrate outward successively are as follows: 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) are Si3N4,
Its thicknesses of layers is 10~100nm.For above-mentioned low emissivity glass, it is found in use, manufacture and research process
The defects of there are still following disadvantages: 1, mechanical stability is insufficient, and scuffing, scratch are easy to produce during following process；2,
Chemical stability is insufficient, aqueous vapor, corrosive gas in air, not clean enough water, fingerprint etc. be easy to cause film layer by
Corrosion.These disadvantages reduce the yield rate of Three-silver-layer low-radiation coated glass in practice.
Summary of the invention:
The technical problem to be solved by the present invention is to exist for above-mentioned Three-silver-layer low-radiation coated glass in the prior art
The disadvantages of mechanical stability is insufficient, chemical stability is insufficient and yield rate is not high provides one kind and contains 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 technical scheme adopted by the invention to solve the technical problem is that: it is low-emission coated containing three layers of infrared reflecting layer
Glass, including glass substrate, it is characterised in that: it is set gradually outward on the glass baseplate surface,
First medium layer, geometric thickness are 30~50nm；
First infrared reflecting layer, geometric thickness are 7~16nm；
Second dielectric layer, geometric thickness are 55~90nm；
Second infrared reflecting layer, geometric thickness are 7~16nm；
Third dielectric layer, geometric thickness are 55~90nm；
Third infrared reflecting layer, geometric thickness are 7~16nm；
Outermost dielectric layer, 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 of its mixture, or selected from Si, Al, Zr, Ti, Y, Hf, Nb, Ta metal nitride or nitrogen oxides and its mix
Close at least one of object.
Further, first infrared reflecting layer, the second infrared reflecting layer or third infrared reflecting layer be selected from silver, gold,
At least one of copper, aluminium 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 sublayer, ZnSnOx sublayer, ZnO sublayer, TiO2Son
Layer, SnO2Sublayer, WO3Sublayer, Bi2O3Sublayer, HfO2Sublayer and Nb2O5At least one of sublayer.
Further, when outermost dielectric layer includes Si3N4When sublayer, the Si3N4In sublayer doped with Al, Ni, Zr or
Hf。
Further, when outermost dielectric layer includes ZnO sublayer, in the ZnO sublayer doped with Al, Ga, Mo, Mg,
In, F or B.
Further, when outermost dielectric layer includes ZnSnOx sublayer, in the ZnSnOx sublayer doped with Al, Sb,
Mg, Ni or Y.
Further, the first medium layer, second dielectric layer or third dielectric layer be selected from Zn, Si, Sn, Ti, Nb, Zr,
At least one of 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 at least one of nitrogen oxides and its mixture.
Further, the first medium layer further includes the first ZnO sublayer, and the first ZnO sublayer is located at first medium
Between layer and the first infrared reflecting layer.
Further, the second dielectric layer further includes the 2nd ZnO sublayer, and the 2nd ZnO sublayer is located at second medium
Between layer and the second infrared reflecting layer.
Further, the third dielectric layer further includes the 3rd ZnO sublayer, and the 3rd ZnO sublayer is located at third medium
Between layer and third infrared reflecting layer.
Further, infrared between outermost dielectric layer and third infrared reflecting layer, and/or in third dielectric layer and second
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
Degree is 0.3~5nm, and the barrier layer is selected from Ni, Cr, Ti, Zn, Sn, Hf, Zr, Al metal and its metal of alloy, non-fully oxygen
Compound, non-fully at least one of nitride.
Meanwhile the present invention also provides a kind of laminated glass articles, including two blocks of glass and are clipped between two blocks of glass
Interbed, it is characterised in that: be selected from above-mentioned low radiation coated glass, the low radiation coated glass at least one piece in two blocks of glass
Plated film be located at close to middle layer one side.
The present invention has the following beneficial effects: due to taking above-mentioned technical proposal
Low radiation coated glass and its laminated glass articles of the present invention containing three layers of infrared reflecting layer, passes through conjunction
The thickness that reason designs each film layer is especially the geometric thickness and optical thickness of outermost dielectric layer, on the one hand improves mechanically stable
Property can substantially reduce scuffing during following process, scratch trace；On the other hand it enhances to chemical corrosivity substance
Ability to bear；Meanwhile spectral technique index is improved, and its laminated glass articles maintains good color appearance feature,
It can satisfy the requirement of vehicle glass product.
Detailed description of the invention:
Fig. 1 is the film layer structure schematic diagram of the low radiation coated glass of the present invention containing three layers of infrared reflecting layer；
Fig. 2 is outermost dielectric layer when being ZnO:Al 8nm/ZnSnOx its ZnSnOx thicknesses of layers and normal incidence reflection colour
Coordinate relational graph；
Fig. 3 is outermost dielectric layer when being ZnO:Al 8nm/ZnSnOx its ZnSnOx thicknesses of layers and 60 ° of incident reflection colours
Coordinate relational graph；
Fig. 4 is one embodiment structural schematic diagram 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 1 and comparative example 1 of the present invention；
Fig. 7 is the reflectance spectrum figure of embodiment 1 and comparative example 1 of the present invention；
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, third infrared reflecting layer；7, outermost dielectric layer；8, the first barrier layer；9, the second barrier layer；10, third barrier
Layer；100, glass substrate；101, inner layer glass substrate；102, middle layer；103, glass outer substrate；104, it is low-emission coated.
Specific embodiment:
Below in conjunction with attached drawing, the content of the present invention will be further explained, the thicknesses of layers in the case where not filling bright situation
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 of the present invention containing three layers of infrared reflecting layer, including glass substrate
100, it is characterised in that: it is set gradually outward on 100 surface of glass substrate,
First medium layer 1, geometric thickness are 30~50nm；
First infrared reflecting layer 2, geometric thickness are 7~16nm；
Second dielectric layer 3, geometric thickness are 55~90nm；
Second infrared reflecting layer 4, geometric thickness are 7~16nm；
Third dielectric layer 5, geometric thickness are 55~90nm；
Third infrared reflecting layer 6, geometric thickness are 7~16nm；
Outermost dielectric layer 7, 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 of mixture, or selected from Si, Al, Zr, Ti, Y, Hf, Nb, Ta metal nitride or nitrogen oxides and its
At least one of mixture.
Wherein, outermost dielectric layer 7 is each by rationally designing for protecting its other film layer between glass substrate 100
The thickness of film layer is especially the geometric thickness and optical thickness of outermost dielectric layer 7, and thermal stability, the chemistry that can be improved membrane system are steady
Qualitative and mechanical stability 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 sublayer, ZnSnOx sublayer, ZnO sublayer, TiO2Son
Layer, SnO2Sublayer, WO3Sublayer, Bi2O3Sublayer, HfO2Sublayer and Nb2O5At least one of sublayer namely the outermost medium
Layer 7 can be Si3N4Sublayer, AlN sublayer, ZnSnOx sublayer, ZnO sublayer, TiO2Sublayer, SnO2Sublayer, WO3Sublayer, Bi2O3Son
Layer, HfO2Sublayer or Nb2O5Sublayer can also be made of any two layers or two layers or more of sublayer in above-mentioned sublayer.
It meanwhile being herein that be illustrated height of the present invention durable for ZnO:Al/ZnSnOx citing with outermost dielectric layer 7
Property low radiation coated glass constitute laminated glass articles have neutral color reflection appearance, wherein ZnO:Al expression be doped with
The ZnO sublayer of Al, ZnO:Al with a thickness of 8nm, the thickness by changing ZnSnOx increases to 400nm from traditional 20nm,
The normal incidence reflection colour and 60 ° of incident reflection colours for measuring final laminated glass articles respectively, to assess ZnSnOx film
Influence of the change of thickness degree to the low angle and high angle reflection colour of its laminated glass articles.A+ is represented red in Fig. 2 and Fig. 3
Color, a- represent green, and b+ represents yellow, and b- represents blue；It is more more shallow to the close expression color of coordinate origin in coordinate system,
It is on the contrary then indicate that color is deeper.
From in Fig. 2 and Fig. 3 as can be seen that when ZnSnOx is with a thickness of 40nm (in traditional Three-silver-layer low-radiation coated glass
The typical thickness of ZnSnOx) when, the low angle of laminated glass articles and 60 degree of reflection colour are green and lavender respectively；
When being even up to hundreds of nanometers with the increase of the thickness of ZnSnOx, in most thickness ranges, laminated glass articles
Reflection colour inaesthetic color is presented, such as can be seen from Figure 2 ZnSnOx with a thickness of its interlayer glass when 80nm
The normal incidence reflection colour of glass product is dark green, and the normal incidence reflection colour of its laminated glass articles is in yellow when 120nm,
The normal incidence reflection colour of its laminated glass articles is dark green when 180nm；Or it is in when high angle observation and low angle observation
Now significant color difference, for example, in Fig. 2 ZnSnOx the normal incidence reflection colour with a thickness of its laminated glass articles when 180nm
It is dark green, and the incident reflection colour presentation of 60 ° with a thickness of its laminated glass articles when 180nm of ZnSnOx is aobvious in Fig. 3
What is write is light blue.Based on this, due to as the front of the transparent glass window on the vehicles, especially automobile, skylight, rear shelves or
Side window, which is often required that in low angle and high angle observation, neutral or certain pleasant colored appearance, 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
Hardly possible obtains the laminated glass articles with practical value.On the contrary, in the present invention, it is special by the thickness for rationally designing each film layer
The geometric thickness and optical thickness of outermost dielectric layer 7, for example, ZnSnOx shown in Fig. 2 and Fig. 3 with a thickness of 155nm, 160
When its laminated glass articles normal incidence reflection colour in pale blue green, 60 ° of incident reflection colours are in neutrality color；At this point, working as
ZnSnOx with a thickness of 155nm or 160nm when, the geometric thickness of corresponding outermost dielectric layer 7 is 163nm or 168nm, optics is thick
Degree is 334nm or 344nm.In conjunction with Fig. 2 and Fig. 3 as it can be seen that there are a thickness near ZnSnOx is with a thickness of 155nm or 160nm
Range is spent, its laminated glass articles reflection colour when low angle and high angle are observed can be made almost the same and had to make us pleased
The geometric thickness of the thickness in two dotted ellipse regions in happy appearance color, i.e. Fig. 2 and Fig. 3, preferably outermost dielectric layer 7 is
150~175nm, optical thickness are 310~340nm, the membrane system building of the thickness setting of outermost dielectric layer 7 within this range
Laminated glass product has great practical value.It must be noted that the thickness setting of outermost dielectric layer 7 is in addition to referring to conventional three silver medals
Outside mentality of designing and technical solution provided by the invention, even if the film thickness to other dielectric layer film layers and infrared reflecting layer carries out
Global optimization setting, and the qualified laminated glass articles of spectral technique index and color characteristics cannot be obtained.
It preferably, can include Si when outermost dielectric layer 7 in order to advanced optimize film performance3N4It is described when sublayer
Si3N4Doped with Al, Ni, Zr or Hf in sublayer.Equally, it when outermost dielectric layer 7 includes ZnO sublayer, is mixed in the ZnO sublayer
It is miscellaneous to have Al, Ga, Mo, Mg, In, F or B；When outermost dielectric layer 7 includes ZnSnOx sublayer, in the ZnSnOx sublayer 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 third infrared reflecting layer are to use
In reflection infrared ray, reduces infrared ray and transmitted from low radiation coated glass, so first infrared reflecting layer 2, second is red
The film material of outer reflective layer 4 or third infrared reflecting layer 6 can select any material for capableing of reflecting infrared energy, such as
(but being not limited to) is selected from least one of silver, gold, copper, aluminium and its alloy, is in the present invention preferably silver-colored or argentiferous conjunction
Gold, wherein the alloy of argentiferous is preferably the alloy of silver at least one of gold, aluminium, copper in the present invention.In implementation of the invention
Silver has been selected in example, can be effectively reduced radiance, has improved heat-proof quality.
Wherein, the first medium layer 1, second dielectric layer 3 or third dielectric layer 5 can reduce the anti-of visible light region
It penetrates, provide suitable growth basis for infrared reflecting layer and keep the high-temperature stability of infrared reflecting layer.Also, first medium layer
1 with glass substrate 100 due to directly contacting, additionally it is possible to which Na atom, oxygen atom and the other impurities obstructed in glass substrate 100 are former
Son destroys the intrusion of infrared reflecting layer, and enough adhesion strengths 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 third dielectric layer 5 be selected from selected from Zn, Si, Sn, Ti, Nb, Zr, Hf, Mg,
At least one of 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 at least one of nitrogen oxides and its mixture.Further, the first medium layer 1 further includes
One ZnO sublayer 11, the first ZnO sublayer 11 are located between first medium layer 1 and the first infrared reflecting layer 2.Similarly, described
Second dielectric layer 3 further includes the 2nd ZnO sublayer 31, and the 2nd ZnO sublayer 31 is located at second dielectric layer 3 and the second infrared external reflection
Between layer 4.Meanwhile the second dielectric layer 5 further includes the 2nd ZnO sublayer 51, the 2nd ZnO sublayer 51 is located at second medium
Between layer 5 and the second infrared reflecting layer 6.
Optionally, third barrier layer 10 is set between outermost dielectric layer 7 and third infrared reflecting layer 6, and/or in third
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 third barrier layer 10 is
0.3~5nm, first barrier layer 8, the second barrier layer 9 and third barrier layer 10 are selected from Ni, Cr, Ti, Zn, Sn, Hf, Zr, Al
Equal metals and its metal of alloy, non-fully oxide, non-fully at least one of 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 middle layer 102, two blocks of glass are respectively inner layer glass substrate 101 and glass outer substrate 103；In Fig. 4, glass outer
Close to the one side setting low-emission coated 104 of middle layer 102 on substrate 103, i.e. the glass outer of this laminated glass articles is low
Radiation film coating glass；In Fig. 5, it is arranged low-emission coated 104 close to the one side of middle layer 102 on inner layer glass substrate 101,
I.e. the inner layer glass of this laminated glass articles is low radiation coated glass.The laminated glass articles that the present invention protects as a result, including
Two blocks of glass and the middle 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 close to middle layer 102.
In order to be described in more detail and more support to convincingness inventive point of the invention, it is detailed now to enumerate some embodiments
It illustrates.
Embodiment 1-3
Low radiation coated glass of the present invention containing three layers of infrared reflecting layer, 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 Examples 1 to 3 and corresponding comparative example 1
~2 make a comparison description improvement effect of the technical solution of the present invention in spectrum, machinery, chemical and thermal stability.
Using the white glass of sodium-calcium-silicate float glass process with a thickness of 2.1 millimeters as glass substrate, by cutting, edging, washing and baking
After the processes 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 using pulse direct current sputtering flat target deposition, remaining
Film layer is deposited in oxidizing atmosphere or nitriding atmosphere using medium frequency reactive sputtering rotary target, by controlling the function on each target
Rate, gas ratio and movement velocity control to obtain 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 conjunction piece technique, is finally made laminated glass articles of the present invention.Meanwhile
Referring to ISO9050:2003 and D65 (10 degree) canonical measure and its dominant spectral index is calculated, the results are shown in Table 2.
Table 3: the dominant spectral index for 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.
It is compared by table 1 it is found that the main distinction of comparative example 1 and embodiment 1 is that the outermost dielectric layer film thickness of embodiment 1 reaches
To 157nm, optical thickness is about 321nm, and 1 optical design of comparative example combines 1 film according to its dielectric layer of traditional design theory
Thickness is 37.7nm, and optical thickness is about 76nm.The first medium layer 1 of comparative example 1 and embodiment 1, second dielectric layer 3 and third
The film thickness of dielectric layer 5 all has been subjected to optimization and has reached preferable spectral target and neutral appearance.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
Closing Fig. 6 and Fig. 7 analysis can obtain, and embodiment 1 can reach preferable spectral target, be embodied near infrared band (780-1200nm) model
There is stronger infrared external reflection ability in enclosing.It can be seen that technical solution of the present invention can reach preferable under silver thickness thinner case
Spectral target, and it is poor according to the three-silver low radiation coated laminated glass spectral target of traditional design theory.
Meanwhile the embodiment of Tables 1 and 22 and comparison 2 are analyzed and can be obtained: the three-silver low radiation plated film of traditional structure
Increasing Ag layers of overall thickness (35.8nm) in the comparative example 2 of laminated glass as far as possible and optimizing each film layer makes laminated glass have conjunction
The spectrum and colour index of lattice；In comparison, the laminated glass embodiment 2 of three silverskin provided by the invention system scheme constructs exists
Ag layers of overall thickness just reach same spectral target in the case where there was only 31.8nm.Ensure TL > 70% in embodiment 3 and just enters
It penetrates and increases Ag layers of overall thickness (36.1nm) as far as possible under the premise of 60 degree of incident reflection colours neutrality, obtained key technology refers to
Mark such as Tds, Rds and Tts index is superior to comparative example 2, it can be seen that the three-silver low radiation plating that technical solution of the present invention provides
Film laminated glass has spectral technique index more better than traditional three-silver low radiation coated laminated glass.
In the following, the mechanical performance of embodiment 1-3 and comparative example 1-2, thermal stability and chemical stability are assessed, and
Acquired results are recorded in table 3.
In terms of thermal stability, due to the low radiation coated glass in table 1 under same heat treatment process appearance, sheet resistance without aobvious
Difference is write, therefore assesses its thermal stability difference by measuring mist degree.
Mechanical properties, the main ability investigated film layer and bear frictional dissipation, including friction assessment and Taper mill by hand
Consumption assessment.Wherein friction assessment is rubbed on film surface repeatedly using the clean cotton for dipping in alcohol, finger pressing by hand, and one back and forth
Friction is denoted as 1 time, and continuous friction 40 times is scored as follows according to the destruction situation of film surface:
1 point dabs i.e. demoulding
2 points firmly wipe demoulding
3 points of slight demouldings
4 points, without demoulding, only slightly scratch
5 points of film surface appearances are good, and no macroscopic destroys
For heat-treatment sample, also using on straight line abrasion instrument, load 1N/cm is set2, with non-dust cloth dip in mud into
Row abrasion, reciprocal 200 back and forth, and the mist degree after measuring 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
Seen from table 3, it is steady to present preferable heat for the embodiment 1 of technical solution of the present invention, embodiment 2 and embodiment 3
Qualitative, film surface does not occur presentation quality deterioration, situations such as level of haze is lower after high-temperature heat treatment, on the whole with comparative example 1, right
Ratio 2 is suitable, it is seen that technical solution membrane system thermal stability provided by the invention and three traditional silverskin system thermal stability are suitable.
Seen from table 3, the film layer after the embodiment 1 of technical solution of the present invention, embodiment 2 and the heat treatment of embodiment 3 is in
Existing excellent abrasion performance property, the embodiment 1 of technical solution of the present invention and embodiment 2 are shown lower in the case of same abrasion
The degree of wear.
Similarly, the film layer after being heat-treated shows excellent resisting salt fog corrosion property, in the case of same salt air corrosion
Embodiment 1, embodiment 2 and the embodiment 3 of technical solution of the present invention show good corrosion ability to bear, especially through excessively high
Warm the glass of processing.When the comparative example 1 and 2 coated glass of comparative example of traditional design have already appeared significant corrosion, tool
Only there is corrosion failure dot in the embodiment 1 and embodiment 2 and embodiment 3 for having thicker outermost dielectric layer.
In short, 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 has better light while high-temperature stability is suitable
Compose performance indicator and machinery, chemical durability.
Present invention embodiment enumerated above is describing film layer structure and corresponding film material, while embodiment
It only lists a part, and such as specific depositing operation, parameter, more embodiments and is fabricated to low radiation coated glass
The concrete technology and parameter of laminated glass articles do not describe, it is to be appreciated that these parts not described are all that this field is general
Known to logical technical staff, therefore the part not described does not influence 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
It has been described in detail, but the present invention is by the limitation of specific embodiments described above content, so all according to this hair
Any improvement, equivalent modifications and the replacement etc. that bright technical essential carries out, belong to the scope of protection of the invention.
Claims (11)
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
It is set gradually outward in plate surface,
First medium layer, geometric thickness are 30~50nm；
First infrared reflecting layer, geometric thickness are 7~16nm；
Second dielectric layer, geometric thickness are 55~90nm；
Second infrared reflecting layer, geometric thickness are 7~16nm；
Third dielectric layer, geometric thickness are 55~90nm；
Third infrared reflecting layer, geometric thickness are 7~16nm；
Outermost dielectric layer, geometric thickness are 150~200nm, and optical thickness is 300~360nm, and refractive index is 1.7~2.6,
The outermost dielectric layer includes ZnSnOx sublayer, doped with Al, Sb, Mg, Ni or Y in the ZnSnOx sublayer；
The outermost dielectric layer also includes Si3N4Sublayer, AlN sublayer, ZnO sublayer, TiO2Sublayer, SnO2Sublayer, WO3Sublayer,
Bi2O3Sublayer, HfO2Sublayer and Nb2O5At least one of sublayer.
2. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: described
One infrared reflecting layer, the second infrared reflecting layer or third infrared reflecting layer in silver, gold, copper, aluminium and its alloy at least one
Kind.
3. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, 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 according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: when outermost
Dielectric layer includes Si3N4When sublayer, the Si3N4Doped with Al, Ni, Zr or Hf in sublayer.
5. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: when outermost
When dielectric layer includes ZnO sublayer, doped with Al, Ga, Mo, Mg, In, F or B in the ZnO sublayer.
6. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: described
One dielectric layer, second dielectric layer or third dielectric layer are selected from Zn, Si, Sn, Ti, Nb, Zr, Hf, Mg, Ni, In, Al, Ga, W, Bi gold
Belong at least one of oxide, or in Si, Al, Zr, Ti, Y, Hf, Nb, Ta metal nitride or nitrogen oxides extremely
Few one kind.
7. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: described
One dielectric layer further includes the first ZnO sublayer, and the first ZnO sublayer is between first medium layer and the first infrared reflecting layer.
8. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: described
Second medium layer further includes the 2nd ZnO sublayer, and the 2nd ZnO sublayer is between second dielectric layer and the second infrared reflecting layer.
9. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: described
Three dielectric layers further include the 3rd ZnO sublayer, and the 3rd ZnO sublayer is between third dielectric layer and third infrared reflecting layer.
10. the low radiation coated glass according to claim 1 containing three layers of infrared reflecting layer, it is characterised in that: most
Between outer dielectric layer and third infrared reflecting layer, and/or between third 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
Metal of the interlayer selected from Ni, Cr, Ti, Zn, Sn, Hf, Zr, Al metal and its alloy, non-fully oxide, non-fully in nitride
At least one.
11. a kind of laminated glass articles, including two blocks of glass and the middle layer being clipped between two blocks of glass, it is characterised in that: two
Low radiation coated glass described in claim 1-10 any one, the low-emission coated glass are selected from least one piece in block glass
The plated film of glass is located at the one side close to middle layer.
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| 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 |
| CN114538792B (en) * | 2022-01-28 | 2024-02-27 | 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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| CN101875536A (en) * | 2009-12-31 | 2010-11-03 | 中航三鑫股份有限公司 | Coated glass and manufacture method thereof |
| CN102807330A (en) * | 2012-08-24 | 2012-12-05 | 福耀玻璃工业集团股份有限公司 | Low-emissivity film-coated glass high in infrared reflection and sandwich glass product thereof |
| CN103072341A (en) * | 2013-01-22 | 2013-05-01 | 福耀玻璃工业集团股份有限公司 | Low-emissivity coated glass and sandwich glass product thereof |
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| WO2008060453A2 (en) * | 2006-11-09 | 2008-05-22 | Agc Flat Glass North America, Inc. | Optical coating with improved durability |
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| CN101875536A (en) * | 2009-12-31 | 2010-11-03 | 中航三鑫股份有限公司 | Coated glass and manufacture method thereof |
| CN102807330A (en) * | 2012-08-24 | 2012-12-05 | 福耀玻璃工业集团股份有限公司 | Low-emissivity film-coated glass high in infrared reflection and sandwich glass product thereof |
| CN103072341A (en) * | 2013-01-22 | 2013-05-01 | 福耀玻璃工业集团股份有限公司 | Low-emissivity coated glass and sandwich glass product thereof |
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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. |